Home

Operating Instructions METTLER TOLEDO DL77 / DL70ES / DL67

1. Order No Peripherals Mettler Toledo balances with data output AG AM PM AT AX AB PB PR Adapter cable for balances with options 03 011 and 040 between option and cable 214101 42931 Converter cable for SARTORIUS balances RS CL CL RS 106024 Connection cable for AX AM PM AT balances 214103 LC CL cable for AG AB PB PR balances 229130 Sample Changer Rondo 60 Double cable connecting DL77 with two Rondo 60 s51108305 Sampler system Sampler system QUANTO aliquot QUANTO direct Olivetti Artjet printer EU version 51190985 US version 51190986 TBox control of external devices via TTL I O DR42 09 2002 METTLER TOLEDO DL77 DL70ES DL67 11 37 Accessories Order No Connection cable RS232C for computer DTE 9 pin female 201508 Connection cable RS232C for computer terminal DTE 25 pin female 201507 LabX professional titration software incl Operating Instructions English 51106300 German 51106302 LabX multi titration software incl Operating Instructions English 51106310 German 51106312 Miscellaneous 5 RS option 2 RS232C DCE interfaces plus 1 sensor input 25690 incl the Operating Instructions RS232C Description Interface English 709165 6 Temperature option 2 inputs fo
2. fade out the titration with EXIT in the selection menu confirm Interrupt with RUN press lt index T gt and select with the aid of the Cursor keys gt between e the last measured value pair e the last five tabulated values with the aid of the arrow key you can follow the table of measured values back to the initial values however e the selected titration curve c If you wish to view the table of measured values or the titration curve once again at the end of a method press lt index T gt see Note b 3 30 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Stirrer 3 10 Stirrer You can change the stirrer speed during a currently running or interrupted method see Sections 3 3 and 3 4 If you confirm Stirrer with RUN the following parameter mask appears example Stirrer Speed 80 Status On If you change the speed and confirm it with RUN the stirrer then stirs at the specified speed until the next Sample or Stir function If you wish to switch off the stirrer select Status with SEL gt Off lt remains switched off e until the next Sample or Stir function or e until you select status On 02 93 METTLER DL77 DL70ES DL67 3 31 Records ANALYSIS 3 11 Records With the aid of this function you can generate an additional record on the printer at the end of every sample determination For this you must interrupt the method see Section 3 4 If you select this menu the
3. 100 conversion constant cx t Example 1 You determine the titer of a 0 1 mol L NaOH solution with potassium hydro gen phthalate M 204 2 g mol and weigh in 0 1954 g The predispensing should be 80 of the absolute mL consumption You enter the number 80 You expect a titer of 1 Enter the number 1 The conversion constant for the titer calculation is M 1000 z Select this formula from the recommendation menu 80 1 0 1954 g V 400 0 2042 g mol 0 1 mol L 7 665 mL are predispensed with these entries 8 28 METTLER DL77 DL70ES DL67 02 93 Examples of formulae Example 2 Example 3 Example 4 You determine the content of 0 085 g NaCl M 58 44 g mol with 0 1 mol L AgNQx titer 0 992 The predispensing should be 85 of the absolute mL consumption Enter the number 85 You expect a nominal content of 100 Enter the number 100 The conversion constant for this content determination is M 10 z Select this formula from the recommendation menu 85 100 0 085 g V 00 5 844 g mol 0 0992 mol L 12 46 mL AgNO3 are predispensed with these entries You determine the content in g of 5 mL of a KOH solution M 56 11 g mol with 0 1 mol L HCI titer 0 981 The predispensing should be 90 of the absolute mL consumption Enter the number 90 You expect a nominal content of 5 g KOH L Enter the number 5 The conversion constant for this content determination is M z Sel
4. 1 Modify 2 Start Modify press 1 You are shown the parameter mask 1 Select the sample changer ST20 1 or ST20 2 If you confirm the selection with RUN you can start dispensing Start press 2 or RUN If you press lt index F gt 5 8 2 when e g in the main menu you can start the dispensing process immediately e The relay at the DISPENSER output closes for 0 5 s thereby starting the dispensing You can repeat the process with RUN To obtain the Auxiliary functions menu again press lt index F gt 4 20 METTLER DL77 DL70ES DL67 02 93 AUXILIARY FUNCTIONS Auxiliary instrument 4 6 Auxiliary instrument With the aid of this function you can control a pump a dispenser an electromagnetic valve or a relay attached to an auxiliary output of the titrator There is no need to install these auxiliary instruments if you do not include them in a method If you press function number 6 in one of the other menus lt index F gt then 6 you are shown the following menu 1 Time controlled 2 Manual 4 6 1 Time controlled If the auxiliary instrument has to perform its function at a certain time press function number 1 If you press 6 1 in the Auxiliary functions menu you are immediately shown the selection menu 1 Modify 2 Start Modify press 1 You are shown the parameters whose value or name you can change If you press lt index F gt 611 when e g in the main menu you are shown the
5. Set up original cabling configuration Error messages 1 Ifyou select Memory copy with Titrator 1 or 2 while methods and or auxiliary functions are active and or methods are stored in the method list under ANALYSIS the following appears Command not possible Terminate all actions Delete all methods in method list ANALYSIS Confirm the error message with RUN terminate all activities with RESET and or press lt Index A gt lt Index B gt and delete the methods from the appropriate list Return to the documentation menu with lt Index D gt 5 10 METTLER DL77 DL70ES DL67 02 93 DOCUMENTATION Memory copy 2 If errors appear during the storage operation Titrator 2 shows the following message Computer Sequenc rror Order code Error code E033 E037 E054 Confirm the message with RUN Error code E033 User data memory full Error code E037 Working data memory full too many resources in a block Error code E054 RESET has been pressed on the titrator which receives the data 02 93 METTLER DL77 DL70ES DL67 5 11 USER LEVEL Contents Page 6 USER LEVEL conca pulento 6 3 02 93 METTLER DL77 DL70ES DL67 6 1 USER LEVEL 6 USER LEVEL In the Installation menu under Routine level you have blocked the menus that should be inaccessible to employees see Section 1 9 6 With the aid of this menu you can implement this selection You are shown
6. etc 3 Enter Ri i index see Use of indexes Section 8 2 4 Enter the minimum slope mV unit e g 53 5 Enter the maximum slope mV unit e g 61 Notes a The stored buffer values types a b and c apply to the specified temperature If you calibrate at another temperature these buffer values will be temperature corrected automatically and recorded on the printout b You have specified 3 MERCK Titrisol buffers in a calibration method first buffer pH 4 second buffer pH 7 third buffer pH 9 When you measure these 3 solutions the order is immaterial If you measure only 2 solutions however you must measure the first and second buffer pH 4 and pH 7 in that order otherwise you will obtain wrong calibration data If you measure with buffer solutions whose values you have entered under point 2d you must keep to the order defined there c If inapH calibration with e g these 3 buffer types you obtain a slope that exceeds the limits you defined the calibration data of the appropriate sensor are not entered The error message Data not acquired appears on the record 02 93 METTLER DL77 DL70ES DL67 2 73 Calibration EDITOR Example of a calibration method Sample TITLE You define only the number of samples that is the number of buffers which you use to calibrate the gt d electrode e g n 3 You can leave all other para meters as they are the titrator ignores them SAMPLE
7. Delete all methods in method list ANALYSIS Confirm the error message with RUN terminate all activities with RESET and or press lt Index A gt lt Index B gt and de lete the methods from the appropriate list Press lt Index M gt and again select REMOTE CONTROL 03 99 METTLER DL77 DL70ES DL67 7 3 REMOTE CONTROL To follow the entries and commands of the computer on the titrator display you can use the following keys and key combinations Arrow keys RUN EXIT Index M Index A Index B Index S Index T tLlidd Main menu Method list of Analysis menu A Method list of Analysis menu B Sample data list Display of the active function of a current method To switch off the remote control when you have finished select Off in the REMOTE CONTROL menu 7 4 METTLER DL77 DL70ES DL67 02 93 Communication Titrator lt gt Computer 7 1 Communication between titrator and computer 7 1 1 Overview If you have attached and installed a computer the titrator is able to receive and process data in a specific format from this external device or send data to the outside world You can attach all devices which fulfill the specifications described below Possible devices include any type of computer from the simple hand held computer up to a mainframe The titrator can thus also be integrated in relatively large systems In Section 7 1 2 we refer to the use of the syst
8. Dynamic Titrant addition sionistas 2 55 End eieiei dru 2 56 VENENO mireasa annaia naasia aa 2 57 Maximum Eegenheeten Ee 2 57 2 3 12 4 LEARN EQP Learn titration equivalence point determination 2 58 2 3 12 5 LEARN EP Learn titration end point determination sssssseeeeseeeenenennne 2 60 2 3 13 PT EN einiino endai etege dale 2 62 2 3 14 leegent 2 66 2 3 15 Auxiliary VANS E 2 70 2 3 16 A AAE Ee 2 71 2 3 17 Cala sene ita 2 72 2 3 18 SEN 2 75 2 3 19 le RE 2 77 2 3 20 SYNG eea SO O A 2 81 2 2 METTLER DL77 DL70ES DL67 02 93 EDITOR 2 EDITOR In this menu you develop titration methods which you can store You can modify or delete these methods or print them out Acomplete titration method comprises sample preparation dispensing of auxiliary solutions stirring and waiting times the titration itself calculation of the result and statistics and a record In the titrator these substages are defined as functions that are executed in succession in an analysis Within a method you can not only modify these functions but also cut them out of the defined sequence and hence delete them or paste them in at a different place You can also add a new function to a method Virtually all functions can occur more than once in a method see Section 8 5 1 List of all functions Title Sample Stir Measure Temperature Instruction Dispense Pump Rinse Conditioning Auxiliary instrument Ti
9. It stores for instance titrant names with the corresponding concentrations it knows that it must terminate the titration after an equivalence point has been found it rinses burettes and can provide records of stored data on an attached printer We call the listing of these various tasks a menu Each task is subdivided further If you select a task from the main menu you are shown a new set of tasks the submenu from which you can select another task We refer to this as a menu tree when the main menu branches into submenus and these in turn into additional submenus 4 METTLER DL77 DL70ES DL67 05 99 Introduction 02 93 METTLER DL77 DL70ES DL67 5 Introduction 6 METTLER DL77 DL70ES DL67 02 93 Key combinations Rapid menu change with key combinations Inthe Tutorial you have already become acquainted with several key combinations which you can employ to obtain a certain menu immediately Using these keys you can reduce the number of keystrokes before and during the titrations considerably The key combinations consist of the index key and a letter key which must be pressed simultaneously Key combi nations exist to e jump from a submenu into the main menu or from a submenu into that of another branch or to e trigger commands for the burette or the printer see below Ifyou press akey combination in a submenu the DL70 stores all changes that you have made up to this point in the menu The selector bar
10. T gt functions of the current method see above e lt index S gt sample data list see Section 3 7 3 16 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Interrupt method 3 4 Interrupt current method If you select Interrupt in the selection menu Method the titrator discontinues the function it is currently processing The following selection menu appears DL77 DL70ES DL67 see Section see Section Method Method Add 31 3 1341 Continue see below Continue see below Sample data a Sample data 3 7 Display 3 9 Display 3 9 Stirrer 3 10 Stirrer 3 10 Records 3 11 Records SCH Calculations 3 12 Calculations 3 12 Method data 3 8 Method data 3 8 Modify method 3 6 Modify method 3 6 Reevaluationa gt 35 Reevaluation gt 3 5 Record data 3 8 1 Record data 3 8 1 a If you interrupt a METTLER method the menus Modify method and Reevaluation are missing This also applies to methods stored only in the computer see Method ID Section 3 1 b Reevaluation appears only when you interrupt a user method during a Titration EQP function for which a possible predispensing has been completed You can select or execute all menus or commands of the selection menu To continue titration confirm Continue with RUN The functions Titration pH mV stat Dispense Measure or Temperature are continued from the point at which they were interrupted Caution The remaining functions are r
11. v lt lt Q1 gt Q2 _ gt D Formula Constant Unit 1st Calculation function R1 Q1 C1 m for C1 M 10 z 2nd Calculation function R2 Q2 C2 m for C2 60 01 1000 1 ppm 3rd Calculation function R3 Q3 C3 m for C3 53 5 1 mg g Notes a You must enter the molar mass M and the equivalent number z of the 2nd and 3rd Calculation functions as numeric values or insert as Hj if you have stored these as auxiliary values see Section 1 6 M and z are defined in the Sample function only for the calculation of the first equivalence point see Section 2 3 2 Ifyou do not know the number of the equivalence points instead of defining indexes for Q you can have Q identified by a condition e g Q 200 lt EPOT lt 300 means that the Q used for the calculation is that whose equivalence point potential lies between 200 and 300 mV If the titrator finds 2 equivalence points in this region it calculates the first one see also Section 8 6 4 2 68 METTLER DL77 DL70ES DL67 02 93 EDITOR Calculation Notes c The titrator stores results until you start a new titration method or switch off the titrator If you terminate a titration with RESET all data recorded up to this point are evaluated Non calculable results R are then set to zero 0 If you were to abort the above titration shortly before the attainment of the second equivalence point for instance you would receive the result R1
12. 03 03 METTLER TOLEDO DL77 DL70ES DL67 11 2 Technical data 11 2 10 Memory Data base EPROM METTLER methods User data memory EEPROM Customer methods installation and analysis data Memory for approx 50 standard methods 11 2 11 Attachment possibilities for peripherals Balance Serial by bit current loop data interface for all METTLER balances with data output CL 03 011 012 016 017 018 040 A converter cable is available for SARTORIUS balances CL RS RS CL Printer RS232C interface for various commercial graphics printers with RS232C interface with XON XOFF protocol Sample Changer Attachment also via RS232C interface available as option Computer Attachment also via RS232C interface RS232C interface Pin assignment of the socket of the titrator and the connectors or sockets of the available cables Connection socket of the titrator Computer DTE Cables with ME No 200495 201507 201508 25 pin 25 pin 9 pin male female female Shielding 4 1 4 TxD 2 2 3 RxD 3 3 2 GND 7 7 5 DSR 6 6 6 DTR 20 20 4 RTS 4 7 CTS 5 8 11 22 METTLER TOLEDO DL77 DL70ES DL67 03 03 Technical data Null modem Connector RS232 for 2 printer cables Connections Shielding TxD RxD GND DSR DTR D sub sockets 25 pin both female 1 1 2 gt e 2 3 3 e 7 6 gt 6 Sp as gt 20 Additional connections in the connector are all
13. 61 15 RSD 0 5 Titration with two component reagent EPA of the first Titration function 20 mV Drift 40 ug min 1 0704 RSD 0 9 9 94 my RSD 0 4 Titer determination with sodium tartrate n 2 Titration 10 uL water ne 5 xI XI 10 14 METTLER DL77 DL70ES DL67 02 93 Contents Page 11 1 Installation instructions for the titrator oooononccccnnnnoniccccnnnoninananannn rn nnnnn anar 11 3 11 1 1 inserting the DUETS den cado dietas 11 3 11 1 2 DV1001 DV1005 DV1010 DV1020 bure tes usaste 11 5 VEZI Equipping te burata lloraba ass 11 6 RN Derne ee Buroo eiee E E A EE eNi 11 7 11 1 2 3 Mointaining the burette e ln EE 11 8 RRE e li Rue 11 9 11 1 3 Equipping the titration Sii id 11 10 11 1 4 Rear view of the titrator sra 11 12 11 1 5 Power supply voltage DEET Banos EECH 11 14 11 1 6 Inserting aN GT UE 11 15 11 1 7 Setting and inserting a temperature Option AAA 11 16 11 1 8 Inserting a user data memory IC aa aio dol a 11 18 11 2 Technical dolar rs 11 19 11 2 1 Meet SYSTEM si cis 11 19 11 2 2 PURITY OULD UNS A 11 20 11 2 3 Burete drive MA Ee EE Ee 11 20 11 2 4 liarla EE 11 20 11 2 5 Propeller Ida 11 20 11 2 6 ele 11 21 11 2 7 DIS dt ias Act 11 21 11 2 8 TITO MOS rd da Si Rae 11 21 11 2 9 A SN 11 22 A A ue 11 22 11 2 11 Attachment possibilities for peripherals oonnnninnnnninnnnooooooooooccncccncnoninininininano 11 23 A A a geen en eee a a er one 11 24 11 3 PIC CESS ONIOS canina EA 11 25 11
14. A only DL77 only DL77 only if sample changer is installed only if temperature option has been built in Sample data list for the current method example Display of the method function for the current method Titration function active METTLER DL77 DL70ES DL67 02 93 INSTALLATION Contents Page 1 INSTALLATION 10 c catsio riscos gege 1 3 1 1 TANIS AP 1 4 AA A 1 4 11 2 MOIY E 1 4 1 1 3 AdO erea A 1 8 1 2 EE 1 9 1 2 1 Deli ae eet a a E EE a EARE EAE 1 10 122 MOI oseminte aa aa aaa a aaa 1 10 1 2 3 PUN EE 1 14 1 3 Temperature Sensors oocooooocccccccccccooconcnonccnnnnnnncnonnnnnnnnnnnnncnncnnnnnnnccnnnnncnnns 1 15 1 4 Auxiliary reagents civil 1 17 1 4 1 A T 1 17 1 4 2 Modi ti 1 17 1 4 3 e A E A o 1 18 1 5 Auxiliary instruments iia 1 20 1 5 1 Dell 1 20 1 5 2 MOAI E 1 20 1 5 3 e A A NO AIE A A A EE T 1 21 1 6 fe VIN vale Seea eiii it 1 23 1 7 Titration stands oir 1 25 1 8 E oori nr ee eee renee rr 1 28 1 8 1 A 1 28 1 8 2 Balanco E 1 30 1 8 3 Eege 1 32 1 8 4 Sample E Le E 1 35 02 93 METTLER DL77 DL70ES DL67 1 1 INSTALLATION Page 1 9 DISCO ACO TT 1 36 1 9 1 Format date time airada ncaa cede nectendneucsedte eege eet 1 36 1 9 2 Enter date time ii 1 36 1 9 3 Language ms EE E A E eee 1 37 1 9 4 Record header occcococccococccccconccnnnnonnnnnnnonnnononnnnnnnnnnnnnnnnnnnnnnnnnonnnonnnnnnnnnnnnnnnos 1 37 1 9 5 BD wl EE 1 37 1 9 6 Routine level ME 1 38 1 9 7 A A 1 39 1 9 8 Analysis paramete
15. C F or K of the Pt sensor used Dispense function VDISP Total dispensed volume in mL QDISP Total dispensed amount of substance in mmol 02 93 METTLER DL77 DL70ES DL67 8 3 List of designations Titration function ET1 Initial potential of the measured solution before the first titrant addition in mV or in the installed unit of the sensor used ET2 Potential following Dose 1 Predispensing 1 or Predispensing in mV or in the installed unit of the sensor used Titration mode DOS EQP and EP ET3 Potential following Dose 2 or Predispensing 2 in mV or in the installed unit of the sensor used Titration mode DOS and EQP E mV ET3 ET3 ET2 b ET1 a V mL a mL or nominal content dispensing b dispensing to a potential c dispensing to the slope of the curve 8 4 METTLER DL77 DL70ES DL67 02 93 List of designations Titration function VEQ Titrant consumption in mL up to the equivalence or end point the equivalence points are numbered consecutively Q Titrant consumption in mmol up to the equivalence or end point the equivalence points are numbered consecutively VEX Calculated excess of the titrant in equivalence point or end point titrations in mL QEX Calculated excess of the titrant in equivalence point or end point titrations in mmol EPOT Calculated equivalence point potential of the equivalence or end point VEQ in mV or in the installed unit of the sensor used EHNV Calculated half neutralization
16. Combined pH electrode for titrations in aqueous solutions Combined pH electrode for small volumes in small titration vessels in aqueous solutions Combined glass electrode with movable sleeve frit for titrations in nonaqueous solutions Combined glass electrode with movable sleeve frit for titrations in aqueous solutions Combined glass electrode with sleeve frit for titrations in aqueous solutions Combined platinum ring electrode for redox titrations Combined silver ring electrode for argentometric titrations Order No DG111 SC DG101 SC DG113 SC DG114 SC DG115 SC DM140 SC DM141 SC Phototrode incl power supply untable length 70 cm for color indicated titrations Transmission measurement at 555 nm green DP550 Transmission measurement at 660 nm red DP660 11 34 METTLER TOLEDO DL77 DL70ES DL67 09 2002 Accessories Order No lon selective measuring electrodes e Fluoride ISE DX219 51089931 e Chloride ISE DX235 51089933 e Nitrate ISE DX262 51089934 e Sodium ISE DX223 51089930 e Potassium ISE DX239 51089932 e Lithium ISE DX207 51107673 e Ammonia GSE DX217 51107677 e Ammonium ISE DX218 51107679 e Magnesium ISE DX224 51107684 e Cyanide ISE DX226 51107681 e Sulfide ISE DX232 51107675 e Calcium ISE DX240 51107683 Copper ll ISE DX264 51107678 e Bromide ISE DX280 51107671 e Fluoroborate ISE DX287 51107676 e Silver ISE DX308 51107682 e Cadmium ISE DX312 5110767
17. Dosing pump manual ony nan Os W NP Dispenser 4 5 1 Lift If you wish to change the lift position press function number 1 If you press 5 1 in the Auxiliary functions menu you are immediately shown the selection menu 1 Modify 2 Start Modify press 1 You are shown the parameter mask 1 Select the sample changer ST20 1 or ST20 2 If you confirm the selection with RUN you can change the lift position Start press 2 or RUN If you press lt index F gt 5 1 2 when e g in the main menu you can change the lift position immediately e If the lift is in the topmost position in moves to the middle position e If itis in the middle position it moves to the lowest position e If it is in the lowest position it returns to the topmost position To obtain the Auxiliary functions menu again press lt index F gt 4 16 METTLER DL77 DL70ES DL67 02 93 AUXILIARY FUNCTIONS Sample changer 4 5 2 Turntable forward If you wish to move the turntable forward press function number 2 If you press 5 2 in the Auxiliary functions menu you are immediately shown the selection menu 1 Modify 2 Start Modify press 1 You are shown the parameter mask 1 Select the sample changer ST20 1 or ST20 2 2 Enter the number of positions the turntable should move forward If you confirm the entry with RUN you can move the turntable Start press 2 or RUN If you know what number is stored for the positions
18. ID1 B233 1 Molar mass M 40 00 Equivalent number z 1 Temperature sensor Manual 02 93 METTLER DL77 DL70ES DL67 2 13 Title EDITOR 2 3 Functions All functions whose parameters you wish to modify have to be selected by the operation described under Sections 2 1 and 2 2 The following explanations of all functions and their parameters thus take place under the command Modify function see above represen tation of menu tree 2 3 1 Title This function serves to identify the titration method It must always be first in a method and is the only function that can occur only once in a method You need to define its parameters You call up the stored method in question using the method identification The function has no significance for the progress of the titration 1 Enter the method ID letters and or number max 4 characters e g B101 2 Enter a title for the method e g NaCl in butter 3 Date and time are entered here automatically when you save a new or modified method You can neither clear nor overwrite this information Notes a You must adhere to the upper case or lower case notation of the identification during entries otherwise the titrator outputs an error message b You can not use any method identifications that start with upper case M as they are reserved for METTLER methods c Asterisks and question marks are not allowed in the method identification 2 14 METTLER DL77
19. Installed are Sample data Current sample Aux 1 Stand 1 Sample No 1 1 Sensor 1 DG111 SC D2 No 1 1 Drive 3 0 1 mol L NaOH Volume U mL 5 0 Method 1D1 M001 HCI Minimum mL 4 0 ID2 Maximum mL 6 0 Correction factor f 1 0 3 4 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Executing a method DL77 DL70ES Menu sequence until the start of a method with RUN and or EXIT Method Method Add y Y RUN Method entry ma Method ID M001 User MM Data entry Method data Sample function No 1 Sample data Sample data Sample data 1D1 HCI Sample No 1 1 Sample No 1 2 Sample No 1 3 Number samples 3 ID2 etc etc Titration stand Stand 1 Volume U mL 5 0 gt gt Temperature C 25 0 Minimum mL 4 0 Temperature sensor Manual Maximum mL 6 0 Molar mass M 36 46 Correction factor f 1 0 Equivalent number z 1 EXIT Method Method ay M001 MM Add Start Sample data Method data Cut Record data Method Start M001 MM Single method List once List continuous Y Installed are Sample data Current Sample Aux 1 Stand 1 Sample No 1 11 Sensor 1 DG111 SC D2 dl No 1 1 Drive 3 0 1 mol L NaOH Volume U mL 5 0 Method ID1 M001 HCI Minimum mL 4 0 ID2 Maximum mL 6 0 Correction factor f 1 0 DL77 On the right side of each mask possibly in the side bar
20. Section 11 1 4 and Technical data Section 11 2 1 The RS option has an additional low resistance sensor input the temperature option an additional high resistance sensor input see Sections 11 1 6 and 11 1 7 Depending on the installation manner the low resistance input may for example be either sensor 3 or sensor 4 See Rear view of the titrator Section 11 1 4 and Technical data Section 11 2 1 4 Enter the zero point of the sensor The zero point of a sensor is the measured value at which it displays O mV potential zero point of electrode assembly e For the zero point of a pH electrode this is pHo with unit pH e For the zero point of an ion selective electrode this is pMg with the unit pM or pXo with the unit pX e The zero point of the phototrode is normally 0 T 100 T 1000 mV e The zero point of a conductivity cell is normally 0 uS cm or 0 mS cm 02 93 METTLER DL77 DL70ES DL67 1 11 Sensors INSTALLATION 5 Enter the slope of the sensor The slope of a sensor is the potential change in mV per unit of measurement e For the slope of a pH electrode the unit is mV pH e For the slope of an ion selective electrode the unit is mV pM or mV pX e The slope of a phototrode is normally 10 mV T e For the slope of a conductivity cell the unit is mV uS cm or mV mS cm 6 Enter the temperature The actual calibration temperature is either e defined by you when starting a calibration method see Sect
21. Select record Yes or No Yes the measured values are recorded 6 Enter At s e g 10 A measured value will be recorded every 10 seconds If you confirm one of the parameters with RUN you can measure the temperature of the solution Start press 2 or RUN e The titrator starts to measure the temperature of the solution The measured values appear on the display and are recorded To stop the measurement confirm the mask with RUN and press 3 4 14 METTLER DL77 DL70ES DL67 02 93 AUXILIARY FUNCTIONS Temperature To obtain the Auxiliary functions menu again press lt index F gt Note Ifyou continue the measurement butinthe meantime wish to process other menus quit the display with the appropriate key combination index letter Printout of the mea sured values continues To follow the measured values later on the display press lt index F gt 4 4 02 93 METTLER DL77 DL70ES DL67 4 15 Sample changer AUXILIARY FUNCTIONS 4 5 Sample changer With the aid of this function you control the sample changer titration stand ST201 or ST20 2 and its attached auxiliary units DL70ES DL67 You cannot select ST20 2 as a second sample changer can not be con nected If you press function number 5 in one of the other menus lt index F gt then 5 you are shown the following menu Lift Turntable forward Turntable backward Rinsing pump Rinsing pump manual Dosing pump
22. and the ST20 you can e g when in the main menu immediately move the turntable forward with lt index F gt 5 2 2 e The turntable moves forward by the specified number of positions To obtain the Auxiliary functions menu again press lt index F gt 4 5 3 Turntable backward If you wish to move the turntable backward press function number 3 If you press 5 3 in the Auxiliary functions menu you are shown the selection menu immediately 1 Modify 2 Start Modify press 1 You are shown the parameter mask 1 Select the sample changer ST20 1 or ST20 2 2 Enter the number of positions the turntable should move backward If you confirm the entry with RUN you can move the turntable 02 93 METTLER DL77 DL70ES DL67 4 17 Sample changer AUXILIARY FUNCTIONS Start press 2 or RUN If you know what number is stored for the positions and the ST20 you can e g when in the main menu immediately move the turntable backward with lt index F gt 5 3 2 e The turntable moves backward by the specified number of positions To obtain the Auxiliary functions menu again press lt index F gt 4 5 4 Rinsing pump If you wish to perform rinsing for a certain time press function number 4 If you press 5 4 in the Auxiliary functions menu you are immediately shown the selection menu 1 Modify 2 Start Modify press 1 You are shown the parameter mask If you press lt index F gt 5 4 1 when e g in the
23. but not R2 and R3 02 93 METTLER DL77 DL70ES DL67 2 69 Auxiliary value EDITOR 2 3 15 Auxiliary value Auxiliary value is an assignment function The result R or Ri or its calculated mean value xor x i or a raw result of the titration method is assigned to the auxiliary value Hj and entered automatically with the date in the auxiliary value memory see Section 1 6 and Use of Indexes Section 8 2 20 auxiliary value memories are available As an auxiliary value you can store for instance e the blank value of a titration with the formula H5 x example e araw result determined under the Dispense Measure Temperature Titration and pH mV stat functions with the formula H6 VEQ example You can call up these auxiliary values for the functions e Titration value for EPS values for buffer potentials P1 and P2 e pH mV stat value for EPS and e Calculation 1 Enter an identification text e g Blank of DMF 2 Enter the formula H Hj x x i if you determine the auxiliary value with more than one sample n gt 1 and in this case the calculated mean value is assigned to the Auxiliary value Enter the formula H Hj R Ri only if you determine the auxiliary value with one sample n 1 Enter the formula H Hj E only if a Measure function precedes the Auxiliary value function As a formula you can also enter for instance H Hj x i QDISP or H Hj VTOT 1 5 3
24. g within the limits specified in the Sample function or have it trans ferred by an attached balance see Section 3 1 1 Sample preparation weigh in CaCl and add 40 mL deion H20 4 You can not change the minimum and maximum values specified in the Sample function 5 For every sample you can enter a value which will be calculated if you incorporate fin the formula of the Calculation function Example Each sample has a different known moisture content which can be compensat ed by incorporation of factor f 1st sample moisture content 4 gt f 0 96 gt R Q C m f 2nd sample moisture content 3 gt f 0 97 gt R Q C m f Once you have confirmed the entries with RUN you will be shown the sample data mask for the second then the third sample in order to enter the weight before the following selection menu appears 02 93 METTLER DL77 DL70ES DL67 3 7 Executing a method ANALYSIS DL77 DL70ES DL67 see Section see Section Method Method Add 3 1 3 13 1 Load 3 1 3 13 1 Start 3 1 3 1 4 3 13 3 Start 3 1 4 Sample data 3 7 Sample data 3 7 Method data 3 8 Method data 3 8 Cut 3 12 2 1 Cut 3 12 2 1 Record data 3 8 1 Record data 3 8 1 You can select all menus or execute all commands of this selection menu before starting the method Caution DL67 If you now confirm Load the titrator will automatically load the same method Modified method data and entered sam
25. isco ache races ineditos 3 23 3 8 Method data E 3 26 3 8 1 Record data smiesne a aa Ne Meee aa a A AE 3 27 3 9 INTE 3 28 3 9 1 PUG TOROS A 3 29 3 9 2 A A 3 30 3 10 A EE 3 31 3 11 FROG ORS suioiicnncconn tea 3 32 3 12 Calculations o ae cece eeccccee eee eeeeeeeeaeeeeeeeeceaaeeeeeeeseeeeeeeeeeeeeeeeeaas 3 34 02 93 METTLER DL77 DL70ES DL67 3 1 ANALYSIS Page 3 13 Method NSt st accio 3 35 3 13 1 Filling the method list cuina isis ENEE 3 35 3 13 2 Modifying the methodi list ascuas ant 3 36 o T EE 3 36 3 13 22 Paste senian ae E S 3 36 3 13 3 Processing the meibod et 3 37 Se Single A PPP 3 37 3 13 32 LIST A AA 3 37 3 13 33 List continu OU aeeie E E EEE 3 40 3 14 Parallel titrations with the DL77 ooooooooooccccccncnicicicoconccononancccncnnnanannrnncnnnn 3 42 3 14 1 N tes on EE Ke 3 43 3 14 2 Changing the Analysis menus ENEE 3 44 3 15 Sample series with 2 sample changers ooooooocnnoccccccccccocccnancnincnanannncno 3 45 3 2 METTLER DL77 DL70ES DL67 02 93 ANALYSIS 3 ANALYSIS Under this menu you perform the titration with a selected method The necessary data are stored as a method in the EDITOR and as resources in INSTALLATION You prepare your sample titrate and receive the result You have the possibility to effect entries during the titration or to interrupt it to modify parameter values of the method You can enter the methods you wish to run with the sample data weight or volume in advance the titrator
26. the value for the maximum volume or the potential value for the titration termination if this termination criterion has been specified within the method With an EP titration you can modify for instance the time for the delay if the titrant addition Continuous has been specified in the method 3rd example pH mV stat function If you interrupt the method during this function you can modify for example the value for the control range the volume for the minimum consumption or the time for the specified termination criteria You can not change the numeric parameter values of the Sample function 3 22 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Sample data 3 7 Sample data You can enter the weight or volume the 1D2 and the correction factor for all samples of the methods stored in the method list before and during a current method see also Section 3 1 2 Notes on method and sample data mask Before starting a method Select the method in the method list not valid for the DL67 Select Sample data from the selection menu The sample data list appears During a current method Press lt index S gt The sample data list of the current method appears see example of a pH stating on the following page No ID2 Wt vol 1 1 0 0000 g 1 2 0 0000 g I 3 0 0000 g You may enter the identification ID2 and the correction factor f whereas you must enter the weight or volume for each individual sample s
27. 0 eren Tel td Petes so e EE EN E s S D Ema Tel estas sas EE 100 0 Thres hold exis divi EEN NEE o e a 10 0 aximum volume mi sri seras bie wae a 10 Termination after n EQPS Yes MS scale Seis a eee ow ed ws Bp p ee 1 Evaluation procedure o o ooo ooo o oo Standard 2 58 METTLER DL77 DL70ES DL67 02 93 EDITOR Titration LEARN EQP The titrator always titrates the entire volume of the burette used Thus you must select the weight volume of your sample in accordance with the burette volume The titrator calculates the parameters from the response behavior of the sensor the shape of the titration curve and with due consideration of the burette volume used You thus always obtain e the relative limits AV min AV max of the dynamic titrant addition DYN and e the parameters of the measure mode EQU If the titrator finds more than one equivalence point it calculates the parameters for the one with the steepest jump Ifthe titrator finds no equivalence point it interrupts the method You are shown an error mes sage see Section 3 4 Notes a Since the titrator immediately stores the parameters of the titration mode EQP you can titrate a series of samples with the same content n gt 1 in the Sample function The statistics calculation then discards the result of the first sample b If your method has several Titration functions you can select LEARN EQP or LEARN EP for each titratio
28. 1 1 2 Menu tree Auxiliary reagents H20 250 mL min Aux 2 gt CH30H 250 mL min Aux 2 ho CHCI 250 mL min Aux 2 l etc Auxiliary reagent parameters Name H20 Dispensing rate mL min 250 Auxiliary output Aux 2 Enter new name or select menu with SEL i rate Select another auxiliary output with SEL gt entry from recommendation e Selection Delete The auxiliary reagent Modify is deleted Add Reagent names H20 CH3OH CHCl etc Aux reagent Aux 1 Aux 2 Aux 3 ST20 DOSE ST20 RINSE 02 93 METTLER DL77 DL70ES DL67 1 19 Auxiliary instruments INSTALLATION 1 5 Auxiliary instruments When you select this menu you are shown the installed auxiliary units with the specified parameter auxiliary output Auxiliary instruments can be pumps dispensers valves or relays that have a 24 V connector They are controlled by the titrator the actual function of the units is unknown to the titrator Pump Aux 3 Dispenser Aux 3 Valve Aux 3 If you select pump for instance the list is masked on the right by a selection menu containing the following commands Delete Modify Add 1 5 1 Delete Position the selector bar on this command and confirm with RUN The mask of the selection menu disappears the auxiliary unit pump is deleted Note You can also delete an auxiliary instrument directly from the list by pressing th
29. 1 40 METTLER DL77 DL70ES DL67 02 93 EDITOR Contents Page 2 EDITOR ended 2 3 2 1 Select MICU NOS ccoo coccion ia dadas 2 5 Zils A A 2 6 2 1 2 A A IA 2 7 2 1 3 MOAI A O III 2 7 2 2 Select functions tE 2 8 2 2 1 EE 2 8 2 2 2 COPY ere aeee EEE AA E EAE AEE 2 8 2 2 3 EE 2 8 2 2 4 LEE 2 9 2 2 5 o eege 2 10 2 2 6 Savo method A A EE EEA EA 2 11 2 3 e TE 2 14 2 3 1 UE cas 2 14 2 3 2 Sanlucar a t Eegegeg 2 15 2 3 3 Mas 2 18 2 3 4 MESS rr AA AA A AA A AAA 2 20 2 3 5 Ener en ner rete rn mena E aE ee etre nCre ten 2 22 2 3 0 NS E EE 2 23 2 3 7 BA eee 2 24 2 3 8 int E 2 25 2 3 9 el 2 26 2 3 10 RS OO Tute e EE 2 27 2 3 11 Auxiliary instrument sora tis 2 31 2 3 12 A A EE AN 2 32 2 3 12 1 DOS Titration mode dispensing cccccoococccccnnnnnncnanoncncconnnncnncnnnnnonannnoccnnnos 2 34 02 93 METTLER DL77 DL70ES DL67 2 1 EDITOR Page 2 3 12 2 EQP Titration mode equivalence point determination ooococccnnnniccnncnnn 2 36 Predispensing ascitis iaa 2 39 DYN Titrant addition PP e 2 40 INC littant adaton E 2 41 EQU Measure mode 2 42 TFIX Measure mode tarro tt 2 44 Threshold Equivalence point recognition EE 2 45 EQP range Equivalence point recogniton EN 2 49 Termination criteria secrinaininidcn darte 2 51 Eval ation Criteria o ie 2 51 23 123 EP Titration mode end point determination oi sccccccccenccissiecencececestiectennenseees 2 53 a A o ee 2 53 Continuous Titrant adoos aras 2 54
30. 2 2 DG111 SC pH Sensor 1 Combined pH electrode aqueous medium DG101 SC pH Sensor 1 Combined pH electrode for small volumes in a small titration vessel aqueous medium DG113 SC mV Sensor 1 Combined glass electrode with movable sleeve frit nonaqueous medium DG114 SC mV Sensor 1 Combined glass electrode with movable sleeve frit aqueous medium DG115 SC mV Sensor 1 Combined glass electrode with sleeve frit aqueous medium DM140 SC mV Sensor 2 Combined platinum ring electrode redox titrations DM141 SC mV Sensor 2 Combined silver ring electrode argentometry DM142 mV Sensor 1 Double pin platinum electrode voltametry DP550 T Sensor 2 Phototrode transmission measurements at 550 nm DP660 T Sensor 2 Phototrode transmission measurements at 660 nm DL67 Only sensor DG111 SC is stored in the DL67 You can however add sensors to the list see Section 1 2 3 Note There is no need to install a reference electrode as it is part of the installed measuring electrode at input sensor 1 The input for the reference electrode is marked see Sec tion 11 1 4 If you select DG111 SC for instance the list is masked on the right by a selection menu containing the following commands Delete Modify Add 02 93 METTLER DL77 DL70ES DL67 1 9 Sensors INSTALLATION 1 2 1 Delete Position the selector bar on this command and confirm with RUN T
31. 2 51 explanation 8 22 SEL key 1 5 2 10 Selection menu 1 5 Send mode 1 33 Sensor s adding 1 14 auxiliary function 4 12 deleting 1 10 installing 1 14 menu tree 1 13 modifying 1 10 overview 1 9 Sensor input s adjusting 4 24 calibration data 1 12 for glass electrodes 1 9 1 11 for phototrodes 1 9 1 11 for temperature sensors 1 15 RS option 1 11 temperature option 1 11 Series see sample or method series resp Single method 3 37 Slope sensor calculation 2 72 entry through calibration 1 12 explanation 1 12 pH calibration 2 73 theoretical value 1 12 Software version 4 Speed entering 1 26 2 18 modifying 3 31 srel rel standard deviation 2 75 8 8 ST20A ST20 sample changer 1 35 ST20 1 ST20 2 1 25 Standard evaluation procedure equivalence point recognition 2 45 evaluation criteria 2 51 explanation 8 20 Stand 1 2 1 25 Standard deviation 2 75 Start end character 1 33 Statistics function 2 75 12 8 METTLER DL77 DL70ES DL67 02 93 Index Status remote control 7 3 stirrer 3 31 Steepest jump only 2 51 Stir function 2 18 Stirrer analysis menu 3 31 auxiliary function 4 11 Stirrer connection 1 26 Stop bits printer 1 29 system 1 32 Stop for reevaluation 2 52 Submethods 8 34 Sync function 2 81 Synchronization mode 2 81 System 1 32 T temperature 2 22 8 3 t titer 2 71 8 8 t max end point titration 2 55 equivalence point titration 2 42 measure function 2 21 pH mV stat fun
32. 2nd Titration function The equivalence point with a potential value closest to 100 will be determined Titrant consumption up to the 1st equivalence point of the 1st Titration function The equivalence point lying closest to the buffer potential P1 will be determined Titrant consumption up to the 1st equivalence point of the 1st Titration function The equivalence point lying closest to the auxiliary value stored under H11 will be determined Titrant consumption up to the 1st equivalence point of the 1st Titration function The equivalence point lying within the range of the buffer potential P1 and 300 mV will be determined 02 93 METTLER DL77 DL70ES DL67 8 31 Examples of methods 8 7 Examples of methods Note Numerous applications performed with the DL70 titrator predecessor to the DL70ES are available in brochures see Section 11 3 2 8 7 1 Series titration with functions that the titrator performs before the actual sample addition HE The Sample and Statistics functions are the identifiers for the loop of a series y SAMPLE Sample You specify all parameters After starting the method you confirm the sample data mask with RUN y without entering the weight volume DISPENSE i WM Dispense The specified volume of a titrant should be Y added MEASURE Measure The titrator should acquire the measured value Y E in accordance with the s
33. 3 1 A O Ennn Eeee 11 27 11 3 2 Optional accessories terri Uta 11 28 03 03 METTLER TOLEDO DL77 DL70ES DL67 11 1 METTLER TOLEDO DL77 DL7OES DL67 03 03 Installation instructions 11 1 Installation instructions for the titrator The aim of the following descriptions and drawings is to help you assemble the individual parts of the titrator and become acquainted with all interfaces and inputs and outputs for electrodes and stirrer The titrator must be disconnected from all voltage sources before you remove the baseplate Risk of electric shock 11 1 1 Inserting the burette drive Plug connection 1a of ribbon cable 1 both connections are identical into connector 2 of the burette drive Place the burette drive on the third opening of the instrument press ribbon cable 1 downward slightly to allow it to be led through the lower hous ing slot later and fasten with screw 3 Note Please place the burette drive on the 3rd opening For the first titration which you perform according to the instructions given in the tutorial the 3rd burette drive is defined in the method 03 03 METTLER TOLEDO DL77 DL7OES DL67 11 3 Installation instructions Lay the titrator on its side and undo the 4 screws to remove the baseplate Plug connection 1 of the ribbon cable of the bu rette drive into the third connector 2c of the digi tal board 3 4 is the analog board 5 is the p
34. 3 7 Manual titration interrupting 4 10 modifying 4 9 starting 4 10 terminating 4 10 Maximum evaluation procedure equivalence point recognition 2 45 evaluation criteria 2 51 explanation 8 23 Maximum volume end point titration 2 57 pH mV stat function 2 64 termination criterium 2 50 titration mode DOS 2 34 Mean value 2 75 Measure function 2 20 Measure mode EQP titration 2 42 Measured values displaying 3 29 storage 2 64 8 25 Measurement points measured values for equivalence point recognition 2 45 2 59 maximum number titration fct 8 25 Memory copy computer titrator 5 7 titrator 1 titrator 2 5 9 titrator computer 5 8 Menu explanation 4 Menu change with key combinations 7 Menu sequences example for sample data entry 3 11 method M001 3 4 3 5 Menu tree explanation 4 Menu trees auxiliary functions 4 4 auxiliary instruments 1 21 auxiliary reagents 1 19 auxiliary values 1 24 editor menu 2 12 2 13 equivalence point titration 2 37 overview DL77 5 sensors 1 13 system with computer 1 34 temperature sensors 1 16 titrants 1 7 titration function 2 33 titration stands 1 27 Method ANALYSIS adding 3 6 cutting 3 36 deleting 3 36 executing 3 4 fading out 3 16 interrupting 3 17 loading 3 6 3 8 modifying 3 21 pasting 3 36 recording 3 32 restarting 3 14 starting 3 8 terminating 3 15 time acquisition 3 13 02 93 METTLER DL77 DL70ES DL67 12 5 Index Method EDITOR copying 2 7 deleting 2 7 explanati
35. DISPENSER Select this command when you wish to add an auxiliary instrument to the list You can also add an auxiliary instrument directly to the list by pressing the lt gt plus key You are always shown the following mask Name Auxiliary output Aux 3 1 Select the name from the recommendation menu or enter the name of the device you wish to install 02 93 METTLER DL77 DL70ES DL67 Auxiliary instruments INSTALLATION Note If you install several auxiliary instruments with the same name you must provide each one with a different flag to allow the titrator to distinguish between them e g Pump 2 2 Select the auxiliary output from the selection menu The auxiliary instrument with the appropriate parameters is installed when you quit the parameter mask with EXIT see the appropriate description at the end of Section 1 1 2 1 22 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Auxiliary values 1 6 Auxiliary values When you select this menu you are shown 20 auxiliary value memories H1 H20 You can assign results of a titration such as blank values and potentials to these memories using the Auxiliary value function These are then entered automatically here together with the date see Section 2 3 15 Auxiliary value 1 H1 Auxiliary value 2 H2 etc You can also enter numeric values here as an auxiliary value and you can then call up these under different functions As auxiliary value H1 the Z
36. DL67 02 93 EDITOR Record 2 3 19 Record With the aid of this function you determine what data should be recorded where Notes a If in your method a Record function follows the Statistics function the titrator records only the selected parameters of the last sample of a titration If you add a Record function before the Statistics function the titrator records the selected parameters of all samples see following le Note 2 3 b If your method has two or more Titration functions and you would like to have a record of the table of measured values and curve of the first second or third titration a Record function must follow the Titration function as the titrator stores only the measured values of the last Titration function see Examples of methods Section 8 7 2 The titrator stores the raw results of all functions up to the titration of the next sample within a loop see Section 8 5 7 Output unit 1 8 1 In the selection menu choose between Printer Computer Printer Computer Printer is stored as the default parameter the printer you have installed see Section If you have not installed a printer and or computer the function can not be executed However you can leave it in the method since in this case it neither triggers an error message nor influences the titration If you have installed a printer and or computer but have not connected it or switched iton e the titrator waits unt
37. DL70ES DL67 02 93 EDITOR Sample 2 3 2 Sample With the aid of this function you determine the parameters that are needed for the entry of the sample data such as weight or volume and whether the temperature of the sample should be meaured Parameters of the mask Number samples Titration stand Entry type a Molar mass M Equivalent number z Temperature sensor 1 Enter the number of samples n You can change n before and after the start of the method see Section 3 1 A parameter value of n 3 for instance tells you that you have to titrate at least three samples e g in a titer determination 2 Select the titration stand at which you wish to determine the samples from the selection menu see Section 1 7 You can change the titration stand before the start of the method see Section 3 1 3 Select the type of entry from the selection menu a Weight m Enter the lower weight limit g Enter the upper weight limit g b Volume U Enter the lower volume limit mL Enter the upper volume limit mL The actual weight or volume are not entered until the samples are prepared or the titrator requests the amount after the start of the method see Section 3 1 If you violate this specified upper or lower limit you will be given a notice c Fixed volume U Enter the volume mL You can not change this entry before the start of the method 02 93 METTLER DL77 DL70ES DL67
38. EDITOR Titration EQP INC 2 b Relative Enter AV min dosVol refers to the volume already dispensed in other words the minimum set increment increases during the course of the titration Enter AV max buVol refers to the burette volume and remains constant Note If no predispensing takes place the titrator calculates and dispenses first two volume increments relative to 10 of the burette volume INC The volume increment added by the titrator remains constant 1 Enter AV mL e g 0 1 E mV AE 4 AE13 Aus V mL AV1i2 AVia AV constant 02 93 METTLER DL77 DL70ES DL67 2 41 Titration EQP EQU EDITOR Selection menu Measure mode You can select the equilibrium controlled EQU or time controlled TFIX measured value acquisition This determines the waiting time between addition of the increments Using EQU the waiting time is variable using TFIX itis constant You can not decide the optimum measure mode for your method until you know the reaction time of the components and the response time of the sensor used EQU Before the titrator accepts a measured value equilibrium must be established in the solution The following parameters are responsible for the equilibrium AE potential change of the solution At within a time Time limits between the increments are the parameters t min minimum time t max maximum time As soon as the potential change of the solution is smaller than the s
39. M014 M015 M016 MKF1 MKF2 MKF3 MKF4 List of the METTLER methods Acid Content Titer of NaOH 0 1 mol L Titer of HCI 0 1 mol L Calibration pH Electrode Titer of HCIO4 0 1 mol L Titer of AgNO3 0 1 mol L Titer of EDTA 0 1 mol L Titer of Fe ll 0 1 mol L Titer Na2S203 0 1 mol L Titer of TBAH 0 1 mol L Titer 1 2 H2SO4 0 1 mol L Titer of CPC 0 01 mol L Titer of KMnO4 0 1 mol L Titer of EGTA 0 1 mol L Titer Ce SO4 2 0 1 mol L Titer of 1 2 lo 0 1 mol L KF Titration KF Drift Determination KF Standby Titration KF Titer with Na Tartrate 10 4 METTLER DL77 DL70ES DL67 02 93 Karl Fischer methods 10 2 Water determination according to Karl Fischer You can use the titrator for the reliable determination of the water content of substances when it is greater than 2 mg H20 per sample 10 2 1 Safety measures All Karl Fischer reagents are readily inflammable solutions They are toxic e Do not inhale and avoid skin contact e On skin contact immediately wash off with copious amounts of water e On eye contact immediately irrigate with copious amounts of water then consult a physician 10 2 2 Startup You will find general explanations regarding burettes and titration stand in Section 11 1 This section deals only with specific points Accessories The Karl Fischer accessories are listed in Section 11 3 page 11 36 Burette In METTLER methods MKF1 MKF4 a5 mL burette is instal
40. None 4 Select the number of data bits with SEL 7 bits or 8 bits 5 Select the number of stop bits with SEL 1 stop bit or 2 stop bits Terminal You can use a terminal of the tyoe DEC VT340 or DEC VT241 as acolor terminal As a B W terminal a DEC VT330 or DEC VT240 terminal can be used The cable with order number 201507 can be used as connection cable see Section 11 3 Accessories The terminal should be configured as follows e Baud rate 4800 or 9600 baud e Parity even e Number data bits 8 e Number stop bits 1 1 32 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Peripherals You will find additional information regarding configuration of the terminal and keyboard operation in Section 7 2 Computer The computer requires an RS232C interface DTE The baud rate parity number of data bits and number of stop bits are freely selectable The cables with order numbers 201507 25 pin or 201508 9 pin can be used as connection cable see Section 11 3 Accessories If you have installed a computer you must confirm the line Instrument type Computer with RUN to define the following parameters Character set Select the relevant parameter value with SEL ASCII or DL ASCII The standard character set HEX 20 to HEX 7E for text output to the computer is used DL The character set in the titrator is used Caution If you select DL you must define 8 for the number of data bits Send mode Se
41. Routine level You are shown the following parameter mask Installation Open The user has access to this menu If he should not access it press SEL gt Blocked Editor Open The useris allowedto develop modify delete and print out methods in the Editor menu If he should be allowed to only print out the stored methods press SEL gt Blocked Documentation Open The user has access to this menu If he should not access it press SEL gt Blocked Analysis Modify parameters Open The user is allowed to modify the parameters of the current method in the Analysis menu If he should not be allowed to do so press SEL gt Blocked When you now select Routine in the USER LEVEL menu the user no longer has access to the menus blocked here see Section 6 1 38 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Miscellaneous 1 9 7 Audio signal An audio signal either confirms each keystroke or draws your attention to instructions direc tions or error messages In the factory setting of the titrator all these parameters are signalled When you select this menu you are shown the following parameter mask Keystroke Yes You hear a brief signal after every keystroke If you do not wish to hear this press SEL gt No Results Yes You hear a brief signal after every result that appears on the display If you do not wish to hear this press SEL gt No Messages Yes Your attenti
42. Select a condition No Yes Enter the condition 2 70 METTLER DL77 DL70ES DL67 02 93 EDITOR Titer 2 3 16 Titer Titer is an assignment function The result R or Ri or its calculated mean value x or x i of the titration of a titrant is assigned to the titer by the formula t R1 or t d and entered automatically with the date in the appropriate location of the titrant memory see Section 1 1 2 and Use of indexes Section 8 2 1 Select the titrant to which you wish to assign the titer from the recommendation menu or enter one you have installed 2 Enter its concentration mol L 3 Enter the formula t Enter the formula t 4 Select a condition No X X i if you determine the titer with more than one sample n gt 1 and in this case the calculated mean value is assigned to the titer R Ri only when you determine the titer with one sample n 1 Yes Enter the condition y TITRATION y CALCULATION Y STATISTICS y TITER Y RECORD Example of a method for the titer determination of a titrant with a primary standard n 3 Calculation You define the following result R or Ri m VEQ cC C M 1000 z Statistics The mean value of the result R or Ri is calculated for the 3 samples see Statistics function Section 2 3 18 Titer The calculated mean value is assigned to the tit
43. V curve Measured values AE AV V curve Table of values log AE AV V Results APE AV V E t curve V t curve AV At t curve Note The key combination lt index T gt returns the titration sequence to the display during a titration if you have faded it out beforehand If you select Display you are shown the parameter mask default representation Display Representation Titration curve Curve type E V curve 3 28 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Display 3 9 1 Representation With this menu you can specify whether the measured values the table of measured values or a titration curve should appear during the titration Titration curve is stored as the default parameter Since the display has room for only one type of representation you can select the one you wish to follow or view before during or after the titration see selection menu Method in Sections 3 1 3 3 3 and 3 4 You can change these three representations on the display during and after a titration with the aid of the Cursor keys gt Note If you have attached a terminal see Peripherals Section 1 8 3 measured values table of measured values andthe titration curve appear on the screen simultaneously Select from the selection menu between Titration curve Measured values Table of values Results 1 Titration curve The curve selected in the Curve type menu is displayed see next section
44. aid of a polarization current source you can determine water contents by the Karl Fischer method gt 2 mg H20 sample You can perform conductivity measurements and conductometric titrations with an appropriate non Mettler unit equipped with an analog output All titrators have a maximum of four inputs for electrodes two for temperature sensors and three 24 V outputs for stirrer pump or valve attachments They have a maximum of four RS232C CL interfaces enabling you to connect a series of peripheral instuments anattached METTLER balance transfers the sample weight automatically aprinter records the desired results acolorterminal serves as a second display and can be used for remote control ora PC robot can interchange data with the titrator and with an attached METTLER Sample Changer each titrator is turned into a titration system for the automatic analysis of whole series of samples How the three titrators differ from each other DL77 Two titrations can be executed simultaneously and two sample changers can be connected Neither the DL70ES nor the DL67 allow this DL77 These titrators can control a maximum of four burette drives the DL67 two DL7OES l These instruments know the most important titrants and all METTLER sensors whereas the DL67 knows one titrant and one sensor With both titrators a maximum of 10 titration methods can be entered in a list and processed in succession With the DL67 one method ca
45. appears Confirm Titrants with RUN The message Data transmission active appears e Titrants stored in the titrator will be overwritten if their names and concentrations are iden tical to those transferred All other titrants remain stored e Sensors auxiliary reagents and auxiliary instruments stored in the titrator will be overwritten if their names are identical to those transferred e All other resources temperature sensors auxiliary values titration stands peripherals miscellaneous will be overwritten Error message If the installation data are not stored in the computer the message Computer Sequence error appears see above Error message 1 5 6 METTLER DL77 DL70ES DL67 02 93 DOCUMENTATION Memory copy 5 3 Memory copy You can use this menu e to allow the computer to request a copy of all user methods and installation data stored in the titrator or e to request a copy of all methods and installation data stored in the computer by the titrator or e to request a copy of all methods and installation data stored in the first titrator by a second titrator You do not require an RS option for this You must have e attached the computer to the printer interface of the titrator and e loaded the DLWin software or your own program Note No data for the peripherals will be copied 5 3 1 Request by computer for a copy of data stored in the titrator Computer Plug computer connection cab
46. auxiliary output Aux 1 is the second sample changer titration stand The associated stirrer is in stalled at auxiliary output Aux 1 is a titration stand that you have set up independently of the titration stands mentioned e g if you attach a stirrer to a stand The associated stirrer is installed at auxiliary output Aux 1 is the name of the titration stand at which you can run a sample series with out ever being asked to insert the next sample see Section 3 1 3 The associated stirrer is installed at auxiliary output Aux 1 With this stand you can for example use a robot to change the samples DL70ES DL67 ST20 2 is not listed as you can not connect a second sample changer DL77 When two sample changers are connected one must be a ST20A see Sec tion 1 8 4 02 93 METTLER DL77 DL70ES DL67 1 25 Titration stands INSTALLATION You can neither delete a titration stand nor add a new one to the list If you select Stand 1 for instance you are shown the following parameter mask Name Stand 1 Stirrer connection Aux l Default speed 50 Conditioning mode Fix You can not change the name of the titration stand The line is skipped when the selector bar is moved From the selection menu select the stirrer connection to which you wish to attach the stirrer for titration stand 1 If you stir with a stirrer that is not attached to the titrator select here Not to DL The waiting times specified under th
47. auxiliary value 1 23 2 70 8 8 Half neutralization value 2 36 HELP key 2 39 2 53 2 67 3 34 ID1 identification 1 entering 2 16 modifying 3 6 ID2 identification 2 3 7 INC titrant addition EQP 2 41 Indexes 8 10 Indexing forms compilation 8 14 examples 8 10 8 11 8 12 Index key 7 Inflection point 8 20 Information enter key see Tutorial ikey see Tutorial operating instructions 4 system 9 5 Initial potential 2 34 INSTALLATION 1 3 Installation data printing 5 4 Installation instructions 11 3 Instruction function 2 23 Interchangeable burettes see burette Interrupting method 3 17 Interval conditioning fct 2 27 Karl Fischer methods burette 10 5 drift compensation 10 12 drift determination 10 7 standby titration 10 8 titer with Na tartrate 10 8 titration 10 7 Karl Fischer reagents 10 6 Karl Fischer titrations performing 10 9 limits of detection 10 9 reproducibility 10 9 results examples 10 14 safety measures 10 5 12 4 METTLER DL77 DL70ES DL67 02 93 Index Key combinations compilation 7 Language 1 37 Learn titration LEARN EP 2 60 LEARN EQP 2 58 results 3 13 Lift sample changer 4 16 Limits AV 2 40 LIMS 7 5 Line feed 1 29 List continuous 3 40 List once 3 37 Logical operators 8 17 Loop 2 17 M molar mass 2 16 2 68 3 7 8 3 m weight 2 15 3 7 8 3 Malfunctions general comments 9 5 Karl Fischer titrations 10 13 Manual auxiliary instrument 4 22 temperature entry 2 16
48. b The titrator cannot for example save data if the user data memory is full This is possible e for auxiliary reagents you want to add in INSTALLATION e for a method you create in EDITOR e for sample data you want to enter in the method list for methods in ANALYSIS e for permanently saving a modification of a currently running method e for permanently saving the evaluation criteria of the Titration function of a currently running method parameter Stop for reevaluation Measure Confirm the message with RUN Delete method or installation data or inserta second user data memory c The titrator is controlled by a computer and is performing a learn method The EQP or EP parameters of the Titration function are not saved by the titrator Measure Confirm the message with RUN Always perform a learn method with a method stored in the titrator If you are frequently shown the error message you should contact METTLER service 4 Memory faulty Parts of the user data memory are faulty Measure Call METTLER service to have the memory changed In the meantime you can continue working with the titrator 9 4 METTLER DL77 DL70ES DL67 02 93 Error messages and malfunctions 9 2 Other errors and malfunctions The following is a listing of faults and malfunctions which are not reported by the titrator and should help you rectify many of the possible malfunctions yourself thereby reducing your depend
49. be reentered forthe subsequent samples DL67 Thetitrator reloads a previously executed method if you confirm this method with Load Modified method data and previously entered sample data are all deleted 3 14 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Terminate method 3 2 Terminate current method RESET Ifyou wish to terminate the method press RESET The titrator interrupts itimmediately The following mask appears RESET was pressed during the second sample s Titration function Terminate ANALYSIS A Method CALC appears only with the DL77 Sample No 1 2 Titration 1 If you simply wish to terminate the first Titration function confirm Titration 1 with RUN and quit the mask with EXIT The titrator terminates the Titration function definitively the subsequent functions of this sample determination are however processed If you simply wish to terminate the determination of the current sample confirm Sample No 1 2 with RUN and quit the mask with EXIT The titrator terminates the determination of this sample definitively and Results of this sample appears on the display You are asked for the third sample with RUN If you wish to terminate the method confirm ANALYSIS A Method CALC with RUN and quit the mask with EXIT The titrator terminates the method definitively and you are shown the results calculated up to this point on the display Notes a Ifdatahave been transferred
50. can be on any line of the menu Key combinations for commands y U Rinse burette see Section 4 1 1 Y Rinse tip see Section 4 1 2 alt Trigger line feed on the printer see Section 1 8 1 Pp Trigger form feed on the printer see Section 1 8 1 Ate The current display is printed copied Key combinations for menu change MAIN MENU INSTALLATION EDITOR ANALYSIS A Aral cn ANALYSIS B only DL77 AUXILIARY FUNCTIONS DOCUMENTATION USER LEVEL REMOTE CONTROL only if computer is installed Installation Titrants Sensors Temperature sensors Auxiliary reagents Auxiliary instruments Auxiliary values Titration stands Peripherals Miscellaneous 02 93 METTLER DL77 DL70ES DL67 7 Key combinations Editor Method ID METTLER methods User methods New method Method Method Add A Method Method Add BI Auxiliary functions 1 Burette 2 Stirrer 3 Sensor 4 Temperature 5 Sample changer 6 Auxiliary instrument 7 Calibration temperature sensors 8 Offset adjustment sensor inputs Documentation Print Data transfer Memory copy No ID2 Wt vol 1 1 0 0000 g 1 2 0 0000 g 1 3 0 0000 g mV E V curve mL DL67 Load
51. connection and wipe off any drops KF titrants evolve gas SO especially at elevated temperatures causing bubbles to form in the tubing as well as in the burette stopcock For this reason burettes should be rinsed prior to titration 03 03 METTLER TOLEDO DL77 DL70ES DL67 11 9 Installation instructions 11 10 METTLER TOLEDO DL77 DL7OES DL67 03 03 Installation instructions 11 1 3 Equipping the titration stand Screw on titration arm 1 with knurled screw 2 Insert stirring rod 3 and attach propeller stirrer 4 from below to rod Press spacing ring 5 into titration head place clamping ring 6 in threaded ring 7 and screw in place To install a titration vessel turn the threaded ring half a turn to the left attach the vessel and tighten threaded ring 2 Always make sure that the titration vessel is firmly seated in the titration head When working with toxic solvents strong acids or bases you could suffer injury if the titration ms vessel drops out Risk of corrosion Insert burette tip 8 and electrode 9 diagonally opposed this ensures better control in the titration and close the remaining openings with stoppers 11 amp 12 10 This opening is intended for the rinsing bottle connection 13 is the electrode holder 03 03 METTLER TOLEDO DL77 DL70ES DL67 11 11 Installation instructions 11 1 4 Rear view of the titrator
52. corrected for the temperature in the pH value calculation see Section 4 7 Calibration of the temperature sensors Parameters of the mask Titrant Concentration mol L Continuous addition Sensor Unit of meas urement Pretitration End point pH stat Control range mV Tendency Termination criteria Maximum volume mL EE t min s iaa NEEN t max s E Minimum consumption ml Bee Dee ee Time span s Evaluation criteria Time limit t1 s E Time limit t2 s Data storage Time interval s Condition 2 62 METTLER DL77 DL70ES DL67 02 93 EDITOR pH mV stat 1 Select the titrant from the recommendation menu or enter one you have installed see Section 1 1 2 Enter its concentration mol L 3 Select continuous addition This parameter allows a pH stating in which more titrant than will fitin one burette volume is consumed to be performed without interruption For this purpose you use the same titrant You must however rename it and install it on another drive see Section 1 1 3 As soon as the contents of the first burette have been dispensed the second begins dispensing Thus the time required to refill the first burette can be bridged over No Yes Enter the titrant 2 you have installed Enter its concentration mol L 4 Select the sensor from the recommendation menu or enter one you have installed see Section 1 2 5 Select the unit of measureme
53. disconnected from all voltage sources before you remove the baseplate Risk of electric shock In case you have inserted the RS option already place the temperature option next to it and plug connection of ribbon cable 5 into the connector 7 see page 11 15 of the RS option Notes e When you install this option you should adjust the sensor input see Section 4 8 Offset adjustment of the sensor inputs e To connect temperature sensors from other manufacturers you can obtain a Lemo cable plug 4 pin and solder on the corresponding cable see Accessories Section 11 3 2 Soldering scheme e Shielding Pt100 Pt1000 sensor 03 03 METTLER TOLEDO DL77 DL70ES DL67 11 17 Installation instructions 11 1 8 Inserting a user data memory IC The titrator must be disconnected from all voltage sources before you remove the baseplate Risk of electric shock Slide burettes off titrator and unscrew the baseplate ES ing H INS SAM a 4a LER e ie SS SS Y y Y ia 4 lif 1 3 Carefully place user data memory 1 on IC socket 2 of processor board 3 with the IC notch 4 facing the same direction as that of the adjacent IC 4a IC is the abbreviation for Integrated Circuit 11 18 METTLER TOLEDO DL77 DL70ES DL67 03 03 Technical data 11 2 Technical data 11 2 1 Measurement system End point indication Potentiometrically
54. dryness the second Titration function to determine the drift which is then stored under auxiliary value H20 Note a The drift value depends on the tightness of the titration stand and the atmospheric moisture and can be between 10 and 100 ug min 02 93 METTLER DL77 DL70ES DL67 10 7 Karl Fischer methods Note b We have selected a drift determination time of 10 minutes as a compromise between speed and accuracy With 10 minutes the relative standard deviation of the drift is 5 with 5 minutes 12 Caution Do not select this method to titrate water in fresh solvent 10 2 3 3 MKF3 KF Standby Titration For the continuous titration of ingressing moisture The method contains an mV stat function that maintains the potential at 20 mV This potential is an empirical value which irrespective of titrants solvents and samples keeps the titration vessel dry The stating is limited 55 h To perform a titration or drift determination you must always ter minate the standby titration with RESET Caution Do not select this method to titrate water in fresh solvent 10 2 3 4 MKF4 KF Titer with Na Tartrate Titer determination of the KF titrant with sodium tartrate 2 H20 The method contains the same two Titration functions as method MKF1 and also the Titer function which is used to store the determined value in the parameter mask of the titrant Notes a Dispensing of the solvent is not defined in the MKF1 and MKF2 methods If
55. following parameter mask appears 1 Short form method Sample data Raw results last sample Results last sample All results Table of measured values E V curve AE AV V curve log AE AV V curve Would you like a record of the method in short form Select Yes with SEL Would you like a record of all sample data ID1 ID2 molar mass equivalent number weight volume correction factor of the last sample Select Yes with SEL Would you like a record of all raw results such as VEQ or VDISP of the last sample Select Yes with SEL Would you like a record of all results of the last sample Select Yes with SEL Would you like a record of all previously generated results Select Yes with SEL Would you like a record of the table of measured values of the last sample Select Yes with SEL Would you like a record of the titration curve poten tial vs volume of the last sample Select Yes with SEL Would you like a record of the 1st derivative of the titration curve potential vs volume of the last sample The ordinate scale is linear Select Yes with SEL Would you like a record of the 1st derivative of the titration curve potential vs volume of the last sample The ordinate scale is logarithmic Select Yes with SEL 3 32 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Records 10 A B AV V curve 11 E tcurve 12 V t curve 13 AV At t curve Would y
56. function Temperature 02 93 METTLER DL77 DL70ES DL67 4 23 Offset adjustment sensor inputs AUXILIARY FUNCTIONS 4 8 Offset adjustment of the sensor inputs With the aid of this function and the short circuit plug included in the standard equipment you can adjust the sensor inputs yourself This is necessary when e the error message Sensor inputs not adjusted is shown see Note or e you insert a RS or temperature option yourself If you press function number 8 in one of the other menus lt index F gt then 8 you are shown the following menu 1 Modify 2 Start Modify press 1 You are shown the parameter mask 1 Select the sensor input from the selection menu If you confirm the selection with RUN you can adjust the sensor input Start press 2 or RUN You are shown the following Insert short circuit plug Continue Terminate Insert short circuit plug in the selected sensor input and confirm Continue with RUN In the selection menu 3 Stop appears The sensor input is adjusted as soon as 2 Start reappears Note The error message Sensor inputs not adjusted will appear for adjusted sensor inputs when system data have been deleted from the user data memory Measure Switch titrator off and on again the system data will be restored Adjust sensor inputs 4 24 METTLER DL77 DL70ES DL67 02 93 DOCUMENTATION Contents Page 5 DOCUMENTATION 5 3 5 1 ai gu 5 3 5 1 1 E E 5
57. in mmol L measured by means of an ion selective electrode 8 26 METTLER DL77 DL70ES DL67 02 93 Examples of formulae 8 6 2 Constants Weight of sample known C M z C M 10 z C M 1000 z C 1 z C 56 1 C M 1000 z Volume of sample known C M z 10 d where d density C M 1000 z C M 1000 z d C 1000 C 1 C M z C M 10 z C 1 Hj z Volume and weight of sample unknown C Miz C 1 z Unit mg g ppm mol kg mmol g TAN or TBN mg KOH g titer Unit g mL mg L ppm mmol L mol L g L g 100 mL titer the concentration of the volumetric solution is stored as auxiliary value Hj Unit mg mmol 02 93 METTLER DL77 DL70ES DL67 8 27 Examples of formulae 8 6 3 Nominal content a Dispensing Predispensing If you select the parameter nominal content under the Titration function with titration modes DOS EQP and EP to predispense or dispense you must specify three values the amount to be dispensed in of the absolute nominal consumption metered amount the nominal content the conversion constant The conversion constant C converts mmol to the unit of the nominal content The volume that is predispensed or dispensed depending on the nominal content of a substance is calculated from the following formula of absolute nominal consumption nominal content of sample weight or volume x x
58. main menu you are shown this mask immediately 1 Select the sample changer ST20 1 or ST20 2 2 Enter the time s during which the pump attached to the sample changer should perform rinsing The specified time is an empirical value If you confirm the entry with RUN you can start rinsing Start press 2 or RUN e The pump rinses for the specified time To obtain the Auxiliary functions menu again press lt index F gt 4 5 5 Rinsing pump manual If you wish to interrupt a rinsing process manually press function number 5 If you press 5 5 in the Auxiliary functions menu you are immediately shown the selection menu 1 Modify 2 Start 4 18 METTLER DL77 DL70ES DL67 02 93 AUXILIARY FUNCTIONS Sample changer Modify press 1 You are shown the parameter mask 1 Select the sample changer ST20 1 or ST20 2 If you confirm the entry with RUN you can start rinsing Start press 2 or RUN If you press lt index F gt 5 5 2 when e g in the main menu you can start the rinsing process immediately e The pump rinses until you stop the process with RUN or 3 To obtain the Auxiliary functions menu again press lt index F gt 4 5 6 Dosing pump If you wish to dispense for a certain time press function number 6 If you press 5 6 in the Auxiliary functions menu you are immediately shown the selection menu 1 Modify 2 Start Modify press 1 You are shown the parameter mask If you press lt i
59. methods and installation data will be copied The display shows Data trans mission active Caution All methods with the same ID will be overwritten The stored titrants will be overwritten if their names and concentrations are iden tical to those copied The stored sensors auxiliary reagents and auxiliary instruments will be overwritten if their names are identical to those copied All other resources temperature sensors auxiliary values titration stands miscellaneous will be overwritten As soon as the copying operation is at an end the main menu appears in the display indicating that data transmission will now once again be routed across the computer interface Setup original cabling configuration 5 8 METTLER DL77 DL70ES DL67 05 96 DOCUMENTATION Memory copy Error messages 1 If you select Memory copy while methods and or auxiliary functions are active and or methods are stored in the method list under ANALYSIS the following appears Command not possible Terminate all actions Delete all methods in method list ANALYSIS Confirm the error message with RUN terminate all activities with RESET and or press lt Index A gt lt Index B gt and delete the methods from the appropriate list Return to the documentation menu with lt Index D gt 2 When the user data memory is full the computer displays an appropriate error message 5 3 3 Request by Titrator 1 for a
60. minimum 2 46 evaluation procedure segmented 2 48 evaluation procedure standard asymme tric 2 47 TIME 3 13 8 8 10 12 Time controlled auxiliary instrument 4 21 Time acquisition method 3 13 Time auxiliary instrument function 2 31 conditioning function 2 27 entering 1 36 selecting format 1 36 stir function 2 18 Time interval 2 64 Time limits 2 64 Time span 2 64 Time specification auxiliary values 1 23 methods 2 14 sensors 1 12 temperature sensors 1 15 titrants 1 6 Titer determination method excerpt 2 71 entering 1 5 entry through titer determination 1 5 function 2 71 Title function 2 14 Title line parameter mask 1 6 2 10 Titrants adding 1 8 deleting 1 4 installing 1 8 menu tree 1 7 modifying 1 4 Titrant addition end point titration 2 54 equivalence point titration 2 40 Titration function 2 32 menu tree 2 33 Titration curves 1 derivative 2 47 2 48 8 22 2 derivative 2 48 8 22 displaying 3 29 recording 2 78 3 32 Titration mode 2 32 Titration sequences comparison stand 1 ST20 1 3 38 excerpt of a standard method 3 12 on the sample changer 3 39 pH stating 3 24 Titration stand s equipping 11 11 importance 2 16 installation data 1 25 menu tree 1 27 modifying 3 7 selecting 2 15 Titration time 3 13 8 8 10 12 Titrator ID 1 37 Transmission 1 11 Transmission mode bidirectional 1 30 unidirectional 1 30 Turntable sample changer backward 4 17 forward 4 17 U volume 2 15 8 3 Unidirectional trans
61. o JO a SS GO Nc O wW N O On off switch Connector for power cable Fuse holder and voltage selector Sheet with designations of inputs and outputs Interface for attachment of a printer RS232C Interface for attachment of a balance CL Sensor electrode input 1 Reference electrode input for sensor input 1 Sensor electrode input 2 Ground socket Auxiliary output 1 for attachment of stirrer pump valve or relay Auxiliary output 2 for attachment of stirrer pump valve or relay Auxiliary output 3 for attachment of stirrer pump valve or relay 11 12 METTLER TOLEDO DL77 DL7OES DL67 03 03 Installation instructions RS option see Section 11 1 6 14 Sensor electrode input 3 15 Interface for attachment of a Sample Changer RS232C 16 Interface for attachment of a terminal or computer RS232C Temperature option see Section 11 1 7 17 Sensor electrode input 4 18 Temperature sensor input Temp 1 Pt1000 or Pt100 19 Temperature sensor input Temp 2 Pt1000 or Pt100 Note Insertion of the two options can also be reversed the sensor inputs will then be counted from left to right Sensor 1 Sensor 4 It is important for you to know that e the sensor input for the RS option is low resistance e the sensor input for the temperature option is high resistance see Technical data Section 11 2 1 and Sensors Section 1 2 2 page 1 11 03 03 METTLER TOLEDO DL77 DL7OES DL67 11 13
62. of the sensor Select the sensor from the recommendation menu or enter the one you have installed see Section 1 2 2 Select the buffer type from the selection menu For DIN NIST MERCK Titrisol and INGOLD buffers the titrator has 8 values stored in each case and you can select these to calibrate pH electrodes You can enter the values of buffer solutions you have chosen yourself under pH pM pX free selection to calibrate pH or ion selective electrodes DIN NIST buffer pH The buffer values apply to a temperature of 25 C Select the buffer value for the 1st buffer from the selection menu e g pH 1 679 Select the buffer value for the 2nd buffer from the selection menu e g pH 6 865 etc 2 72 METTLER DL77 DL70ES DL67 02 93 EDITOR Calibration b MERCK Titrisol buffer pH The buffer values apply to a temperature of 20 C Select the buffer value for the 1st buffer from the selection menu e g pH 4 Select buffer value 2 for the 2nd buffer from the selection menu e g pH 7 etc c INGOLD buffer pH The buffer values apply to a temperature of 25 C Select the buffer value for the 1st buffer from the selection menu e g pH 4 6 Select the buffer value for the 2nd buffer from the selection menu e g pH 9 21 etc d pH pM pX buffers You have a free choice of maximum eight buffer values Enter the value for the 1st buffer Enter the value for the 2nd buffer
63. only via the Sample function of a method see Section 2 3 2 Example for one method with 40 samples Only the functions in which parameters must be modified are shown Parameters in the Stir and Rinse functions these are not shown in the scheme should not be modified The first 20 samples are titrated using SAMPLE Number samples 20 sae Titration stand ST20 1 titration stand ST20 1 etc TITRATION Titrant HCI HCI and DG11 1 SC are stored as stan Concentration mol L 0 1 dard resources Sensor DG111 SC etc CALCULATION Results Beie The content in g L is calculated Formula R Q C U Constant C M z etc etc STATISTICS Ri i index R1 After 20 sample determinations their etc mean value is calculated SAMPLE Number samples 20 The titrator is told by the 2nd Sample Titration stand ST20 2 function to titrate the next 20 samples etc using titration stand ST20 2 TITRATION Titrant HCI 2 HCI 2 must be added to the list of titrants Concentration mol L 0 1 and DG111 2 to the list of sensors see Sensor DG111 2 Section 1 1 3 and 1 2 3 etc CALCULATION Results Base The result of the 2nd Calculation func tion must receive 2 as the index for Q Formula R2 Q 2 C U A Gr Constant C M z mmol consumption in the 2nd Titration etc etc function see Section 8 2 STATISTICS Ri i index R2 The mean value of the 2nd Titration etc function is calculated CALCULATION Results B
64. second result should equal auxiliary value 4 R1 H5 gt E 2 the expression first result plus auxiliary value 5 should be greater than the potential of the second Measure function Note You will find additional examples in Section 8 6 4 b Logical operators a b AND a b OR Example R1 lt 0 0 R1 gt 10 the first result should lie outside the range from 0 0 to 10 02 93 METTLER DL77 DL70ES DL67 8 17 Functions with a condition Example 1 Determination of the neutralization value of wastewater The pH value of the samples differs greatly so that we have to titrate on the one hand with NaOH and on the other with HCI To execute the determinations with one method we set the conditions for functions excerpt from a method Sample Number sample 10 Titration stand Stand 1 Enty PO usada Fixed volume Volume ML leen 10 0 A a Waste water Molar mass M A 0 0 Equivalent number Z eeeeeeeeeeeeeeneeeeeees 1 Temperature Sensor eseese Manual d Measure SENSON O DG111 SC A nanasan As installed AE La VE 0 5 Alli 2 0 MIN mode Fix L MIN DOE 20 Ma Sica il 300 Y Titration Md taa NaOH Concentration Tomat 0 1 EISE Auge eessen Deeg a DG111 SC ii e gl As installed Titration MOE cccoonocccccccnnoncnnninanancnnnnnnnns EP Titrant additiON 2 02 eeeeeeeeeeeeeeteeeeeee Dynamic AE Set MV TN 8 0 AV MIN meiosis 0 02 AV maxX Im 0 1 AE MV aaas 0 5 ANA EE EEE teeter igen testes 0
65. select TEMP A forinstance you are shown the parameter mask of the Pt sensor in which you can change the parameter values or names Name TEMP A Sensor type Pt100 Sensor input Temp 1 Zero point C 0 0 Date Time 00 00 0000 00 00 1 You can not change the sensor name The line will be skipped when the selector bar is moved 2 Select the sensor type with SEL Pt100 or Pt1000 see Section 11 1 7 3 Select the sensor input with SEL Temp 1 or Temp 2 see Section 11 1 4 4 Enter the zero point of the Pt sensor The zero point of a Pt sensor is the deviation of a measured value from a reference value such as 0 C for an ice bath 5 You can neither delete nor overwrite the date lt refers to the calibration of the Pt sensor using the auxiliary function Calibration temperature sensors and is entered here together with the time automatically see Section 4 7 Notes a The installed zero point is the theoretical value for a new Pt sensor You have to perform a calibration of your sensor if you wish to determine an accurate value When calibrating the zero point is automatically entered here together with the date see auxiliary functionCalibration temperature sensors Section 4 7 b As soon as you change a parameter of the temperature sensor the date and time are deleted 02 93 METTLER DL77 DL70ES DL67 1 15 Temperature sensors INSTALLATION The Ptsensor with the modified parameters is installed when
66. station instrument switched on Burette drive faulty Call METTLER service Wrong potential or Electrode defective Check electrode see pH values electrode sheet Check installation data Use new electrode No dispensing titrant Burette tip blocked Clean burette tip discharged from stopcock or piston Follower cam at burette Insert follower cam cor stopcock installed wrongly rectly see Section 11 1 2 3 9 6 METTLER DL77 DL70ES DL67 02 93 Applications Contents Page 10 Applications iii iba 10 3 10 1 List of the METTLER methods AA 10 4 10 2 Water determination according to Karl Fischer 10 5 10 2 1 safety plore c sts si iS 10 5 10 2 2 PP 10 5 10 2 3 Description of the four Karl Fischer methods ooooooooccnccoooooooccccncncccnonononnnnnns 10 7 10 239 MER KF TARO rra A ae 10 7 10 2 3 2 MFK2 KF Drift Determination kee 10 7 1 20 83 MESS IRF Standby Wate OY spas 10 8 102 34 MFK4 KF Titer with Nae Tanttalo osmosis 10 8 10 2 4 Limits of detection and reproducibility ooooooonccccccnnnnncccccccccnnnnncnanccnnnnn 10 9 10 2 5 Performing Karl Fischer titrations cin 10 9 10 2 5 1 Procedure A Pretitration standby titration and drift determination 10 9 10 2 5 2 Procedure B Pretitration drift and titer determinaton 10 10 10 2 5 3 Procedure C Pretitration drift determination and titration ora Sale Sample aeea E Ee EEE EEEE 10 10 10 2 5 4 Titration Of SG NGS siciliano 10 11
67. the interval but have erroneously placed a conditioning beaker after the third sample beaker The ST20A omits the conditioning beaker 3 You have selected Flexible as conditioning mode a The method has no Conditioning function The ST20A recognizes a conditioning beaker and conditions the sensor for 10 seconds b The method has a Conditioning function with parameters such as Interval 4 Time 30 s Rinse volume 5 mL e The ST20A finds a conditioning beaker after the second sample beaker It then conditions and rinses according to the defined parameters e After the fourth sample beaker the ST20A must condition If it finds no conditioning beaker it searches for one by turning backwards see Note 2b It conditions for 30s and rinses 5 mL 02 93 METTLER DL77 DL70ES DL67 2 29 Conditioning EDITOR c Ifyou would like to condition atliberty during the run but for a certain time and with a defined rinse volume add a Conditioning function to the method and set the interval to 60 for example and set the time and rinse volume The ST20A must not condition during the sample series if this is done Note you can not designate more than 60 samples to a method 2 30 METTLER DL77 DL70ES DL67 02 93 EDITOR Auxiliary instrument 2 3 11 Auxiliary instrument You can use this function to control an auxiliary instrument dispenser relay electromagnetic valve etc that is attached to a 24 V auxiliary o
68. the letter A or B indicates the selected Analysis menu 02 93 METTLER DL77 DL70ES DL67 3 5 Executing a method ANALYSIS When you select ANALYSIS the method list appears together with the selection menu see diagram of the sequence on the previous pages The list is either e blank indicating that you must add a method or e it contains one or several methods already indicating that you can start one of them see Section 3 13 DL67 Since you can store only one method in the method list you load this method see page 3 8 Caution DL67 Confirm Add Load with RUN The method entry mask appears Method ID Enter the identification ID of the desired method If no method with the specified identification is stored in the titrator and you have installed a computer the method will be requested from the computer and added to the method list see Operating Instructions provided with the RS option User Enter your name and press RUN Data entry appears only if you have installed a computer For further details about the communication between the titrator and computer see Section 7 1 and the Operating Instructions provided with the RS option You are shown the method data mask with the following parameters example determination of CaClo see Sections 3 1 2 and 3 1 3 Method data Sample function No 1 ID1 Ca457 Number samples 3 Titration stand Stand 1 Temperature C 25 0 Temperature sens
69. the list by pressing the lt gt plus key You are always shown the following mask Name NaOH Concentration mol L Onli Titer 1 0 Burette volume 10 mL Burette drive Drive 3 Date time 00 00 0000 00 00 1 Select the titrant from the recommendation menu or enter the one you wish to install Note If you install for example several NaOH solutions of the same concentration you must provide each name with a different flag to allow the titrator to distinguish between them e g NaQH 1 2 Enter the concentration mol L 3 Enter the titer only if you know its value If you determine the titer with the titrator its value together with the date is entered here automatically see Titer function Section 2 3 16 4 Select the burette volume from the selection menu 5 Select the burette drive from the selection menu 6 The date together with the time for the newly installed titrant is entered here automatically only after the titer has been determined see Titer function Section 2 3 16 The titrant with the appropriate parameters is installed when you quit the parameter mask with EXIT see the appropriate description at the end of Section 1 1 2 1 8 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Sensors 1 2 Sensors When you select this menu you are shown the installed sensors with the specified parameters unit of measurement and the sensor input You will find the menu tree depicted atthe end of Section 1
70. then calls up the methods in succession and performs the titrations with your help An attached sample changer automates this operation After every sample determination you can perform additional calculations and print out measured values or curves that you have not specified under the corresponding method function This menu demonstrates the differing capabilities of the three titrators DL67 Only one method can be processed ata time DL7OES Up to 10 methods can be entered in a list and run automatically in succession DL77 10 methods can be entered in each of two lists and run in parallel 02 93 METTLER DL77 DL70ES DL67 3 3 Executing a method ANALYSIS 3 1 Executing a method DL67 Menu sequence until the start of a method with RUN and or EXIT Method Method Load e RUN Method entry a Method ID M001 User MM Data entry Method data Sample function No 1 Sample data Sample data Sample data 1D1 HCl Sample No 1 1 Sample No 1 2 Sample No 1 3 Number samples 3 ID2 etc etc Titration stand Stand1 gt Volume U mL 5 0 gt Temperature C 25 0 Minimum mL 4 0 Temperature sensor Manual Maximum mL 6 0 Molar mass M 36 46 Correction factor f 1 0 Equivalent number z 1 EXIT Y Method Method M001 MM Load Start Sample data Method data Cut Record data Y
71. value potential at VEQ 2 referring to the equivalen ce point VEQ in mV or in the installed unit of the sensor used neq Number of equivalence points found applies to one Titration function E EPOT3 EHNV3 EPOT2 EHNV2 EPOT1 EHNV1 V 02 93 METTLER DL77 DL70ES DL67 8 5 List of designations Titration function VP1 Titrant consumption in mL up to buffer potential P1 VP2 or P2 QP1 Titrant consumption in mmol up to the buffer potential P 1 QP2 or P2 P1 Buffer potentials in mV or in the installed unit of the sensor used P2 E 200 P1 100 0 100 P2 200 V VP1 QP1 VP2 QP2 8 6 METTLER DL77 DL70ES DL67 02 93 List of designations pH mV stat function VTOT Total dispensed volume in mL QTOT Total amount of substance dispensed in mmol VI Titrant consumption in mL up to time limit t1 or t2 VT2 VT Titrant consumption in mL up to a different time limit QT1 Titrant consumption in mmol up to time limit t1 or t2 QT2 QT Titrant consumption in mmol up to a different time limit CSTAT Correlation coefficient of the regression lines between t1 and t2 of the V t curve V VTOT QTOT VT2 QT2 VI OT t t1 t2 12 93 METTLER DL77 DL70ES DL67 8 7 List of designations pH mV stat function VSTAT Mean titrant consumption in mL min within the time limits t1 and t2 QSTAT Mean titrant consumption in mmol min within the time limits t1 and t2 xI srel TIME AV At VSTAT QSTAT t1 t2 Calculation func
72. with solvents or deionized H O only Then dry it with oil free com pressed air Never place O rings in organic solvents Never attempt to remove any crystals in the cylinder by scratching with a hard object Pipe cleaners or Q tips are more suitable Never put the parts in a drying oven whose temperature is above 40 C Replace the piston if it leaks or is badly scored at the edge Pay special attention to crystal formation between the lip seals of the piston if you work with NAOH KOH and KF solutions 11 8 METTLER TOLEDO DL77 DL70ES DL67 03 03 Installation instructions 11 1 2 4 General notes You can remove air bubbles at the piston surface by taking the burette out of the guide and lightly tapping its base This causes the air bubbles to rise to the top Then flush the burette You can remove air bubbles in the tubes by tapping the tubes with your fingers while titrant is being siphoned off or dispensed If this does not help undo the suction tube so that the titrant flows back into the bottle screw it on again and rinse the burette air purging In obstinate cases undo both tubes rinse with deionized H O and ethanol and dry using oil free compressed air or vacuum Titrants such as KMnO or KOH in MeOH can easily crystallize in the tip of the burette and block it If you have no immediate use for a titrant it is best to empty and clean the dispensing tube Unscrew connec tion to let the titrant flow out Check the threaded
73. you have to intervene Method Start M001 roro Single method M002 roro List once CALC roro List continuous H Installed are Aux 1 ST20 1 Sensor 1 DG111 SC Sensor 2 DG141 SC Drive 3 0 1 mol L NaOH Drive 3 0 1 mol L AgNO3 Current sample No 1 1 Method ID1 M001 HCI ID2 The titrator titrates all samples of method M001 After completion it waits until all data have been transferred to the printer and starts titrating the samples of method M002 the installation data are the same as for the first method When the titrator has trans ferred all data to the printer the following request appears Change resources Drive 3 0 1 mol L AgNO3 The titrator starts to titrate the samples of method CALC When all data have been transferred to the printer the results of all samples of this method will be displayed The installation data of all methods are dis played This mask appears for all samples but is con firmed by the titrator Change the titrant Attach the DM141 SC sensor and insert it This is not requested as the sensor is in stalled at sensor input 2 02 93 METTLER DL77 DL70ES DL67 3 39 Method list ANALYSIS 3 13 3 3 List continuous Select List continuous if you wish to repeat the listed methods once or several times e When the titrator has completed the first method it moves it to the end of the method l
74. you select an improper sequence when pasting or adding the functions the titrator sends you an error message e g you can not place the Statistics function before the Calculation function However the error message is not outputted until the method is saved 02 93 METTLER DL77 DL70ES DL67 2 9 Modify functions EDITOR 2 2 5 Modify This command shows you a mask with the parameters needed for the function You can modify the values or names of these parameters Notes a The parameters of all functions except those of the Title function are defined by default values or names These are overwritten as soon as you enter a new value or name If you wish to correct a parameter indicate the appropriate letter number with the cursor with gt or then enter the new one With SEL other parameters may be selected from the recommendation or selection menus see Section 1 1 2 The method identification formulae and conditions are checked immediatly after their entry If they are incorrect an error message appears such as Error No 3 Wrong formula Modify Terminate If you confirm Modify with RUN you can change the entry If you confirm Terminate with RUN the most recently saved prior entry appears As soon as you quit a parameter mask with EXIT the values or names are stored The selector bar must be located on a parameter here If you confirm the title line of a parameter mask with EXIT the foll
75. your titrator has two several burette drives we advise installing the KF solvent for a 20 10 mL burette adding the Dispense function to MKF1 or MKF2 and storing this as a user method You thus above all avoid ingress of moisture into the titration vessel through solvent addition b As a calibration substance you can also use deionized H20 or a standard water solution of 5 mg H20 mL modify parameters of the Sample function and the fifth Calculation function accordingly H20 by means of a microliter syringe approx 10 uL accurate to at least 0 5 Standard water solution approx 2 mL accurate to at least 0 5 10 8 METTLER DL77 DL70ES DL67 02 93 Karl Fischer methods 10 2 4 Limits of detection and reproducibility Limit of detection 0 6 mg water for titrant 5 mg H20 mL Reproducibility lt 1 relative standard deviation RSD for samples with a water con tent of 15 25 mg sample To achieve this reproducibility the sample must contain at least 15 mg water 10 2 5 Performing Karl Fischer titrations 10 2 5 1 Procedure A Pretitration standby titration and drift determination Add 40 mL methanol or KF solvent to the titrant vessel see Note a in Section 10 2 3 4 Start method MKF1 to titrate the solvent to dryness so called pretitration Enter 1 for sample weight and number of samples On completion of the pretitration start KF standby titration MKF3 to condition the
76. 0 1 Select the sensor name from the recommendation menu or enter the name of the sensor you wish to install Note If you install for example several DG111 SC sensors you must provide each name with a different flag to allow the titrator to distinguish between them e g DG111 2 2 Select the unit of measurement suitable for the sensor from the selection menu 3 Select the sensor input from the selection menu 4 Enter the zero point of the sensor 5 Enter the slope of the sensor 6 Enter the temperature see explanation of the parameters and note under Modify 7 The date together with the time for the newly installed sensor is entered here automatically only after the sensor has been calibrated see Calibration function Section 2 3 17 The sensor with the appropriate parameters is installed when you quit the parameter mask with EXIT see the appropriate description at the end of Section 1 1 2 1 14 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Temperature sensors 1 3 Temperature sensors When you selectthis menu you are shown the installed temperature sensors with the specified parameters sensor type and sensor unit TEMP A Pt100 Temp 1 TEMP B Pt100 Temp 2 TEMP C Pt1000 Temp 1 TEMP D Pt1000 Temp 2 You can neither delete a temperature sensor nor add a new one to the list You can however install several Pt100 or Pt1000 at the same temperature sensor input Temp 1 or Temp 2 for example If you
77. 1 DG101 SC pH Sensor 1 deleted DG113 SC mV Sensor 1 p L p DG114 SC mV Sensor 1 DG115 SC mV Sensor 1 DM140 SC mV Sensor 2 DM141 SC mV Sensor 2 t DM142 mV Sensor 1 H DP550 T Sensor 2 p 4 DP660 T Sensor 2 M Sensor parameters Name DG111 SC Unit of measurement pH Sensor input Sensor 1 Zero point unit 7 0 Slope mV unit 59 16 Temperature C 25 0 Date time 02 06 1992 10 15 Sensor names DG111 SC amp Enter new name or select entry from DG101 SC i recommendation menu with SEL ore Units of meas lL Select another unit of measurement with SEL ES starts te hen a ee eee Sensor inputs L Select another input with SEL Sensor 1 O Sensor 2 EEN Sensor 3 Enter new zero point or let it be Sensor 4 entered through calibration i Enter new slope or let it be entered gt S through calibration i Enter new temperature The sensor is 02 93 METTLER DL77 DL70ES DL67 Sensors INSTALLATION 1 2 3 Add Select this command if you wish to add a sensor to the sensor list for instance a DG111 SC sensor with different calibration parameters or a sensor not yet installed You can also add a sensor directly to the list by pressing the lt gt plus key You are always shown the following mask Name DG111 SC Unit of measurement mV Sensor input Sensor 1 Zero point Unit 7 0 Slope mV Unit 59 16 Temperature C 250 Date time 00 00 0000 00 0
78. 1 KM58 Ger ID2 aE r Jane The titrator starts the pH stating you have specified the V t curve for its representation in the method S A Press this key combination Y No ID Wt vol The sample data list appears 1 1 0 0000 g Confirm this line with RUN 1 2 0 0000 g 1 3 0 0000 g r The sample data mask appears Sample data Sample No 1 1 Enter ID2 and weight ID2 G 324 Weight m g 0 1456 Minimum g 0 0 Maximum g 0 2 Correction factor f 1 0 Aaf Press this key combination y mL V t curve If the stating is still running the V t curve of the pH mV stat function is displayed again Otherwise the function the titrator is processing appears gt Ss 3 24 METTLER DL77 DL70ES DL67 02 93 Sample data ANALYSIS Notes a b C d If for instance the titration beaker containing sample No 1 has fallen over reselect the first line of the sample data list and overwrite weight or volume with the new value in the sample data mask During the titration you can modify only the data of the samples that have not yet been titrated You can not modify sample data of a method already executed With lt index S gt the sample data list for the current method is always shown If no method is running the sample data list of the method list s first method is shown 02 93 METTLER DL77 DL70ES DL67 3 25 Method data ANALYSIS 3 8 Method data You can change the method data before starti
79. 10 2 6 Adapting function parameters oooccooococcccncncnononannnnncnnnnnoncnnnnnnnnnnnnnnnnncnnnnnnnes 10 12 10 2 7 Drift compensation eer 10 12 10 2 8 Possible problems their cause and rectification oooooooccccccnnncnnnnnnnnnns 10 13 10 2 9 A few examples of results asirio 10 14 Application sbheets nn cnn nc nnne nennen M001 M016 MKF1 MKF4 02 93 METTLER DL77 DL70ES DL67 10 1 Applications 10 Applications In this section you will find application sheets for all methods that we have developed and stored in the titrator as METTLER methods The four methods you need to determine moisture by the Karl Fischer method are described in greater detail Methods M002 M016 include the calibration of pH electrodes and titer determinations which you should always perform before you analyze your samples with the appropriate titrant At the same time these methods serve as a model for the development of your own methods e You can examine the parameters of the individual functions e You can adopt control parameters of the Titration function such as titrant addition and measure mode for the same titration reaction by either modifying the METTLER method and storing it as a user method or developing a new method with the aid of the standard method see Sections 2 1 and 2 1 3 02 93 METTLER DL77 DL70ES DL67 10 3 Applications 10 1 M001 M002 M003 M004 M005 MO06 M007 MOO M009 M010 M011 M012 M013
80. 2 8 8 Scheme for method design 8 36 02 93 METTLER DL77 DL70ES DL67 8 1 List of designations 8 Designations Explanations Examples In this section you will find additional information explanations and examples that supplement the EDITOR section 8 1 List of designations This list shows you the abbreviations of all designations of the parameters and of the raw results determined by the titrator and their definition You must adhere to the upper case or lower case notation of the designations during entries otherwise the titrator outputs an error message Titrant c Nominal concentration of the titrant in mol L Dispense Titration pH mV stat Calculation functions The actual equivalent concentration ACTUAL value of the titrant the product of the nominal concentration c and titer t in mol L is calculated automatically by the titrator Sample function U Sample volume in mL for the Calculation function Sample weight in g for the Calculation function M Molar mass in g mol for the Calculation function z Equivalent number number of reaction entities of the sample compared to the titrant for the Calculation function Note The notation z of DIN standard 32 625 has not been used for the titrator for technical reasons f Correction factor for the Calculation function Measure function E Measured value in mV or in the installed unit of the sensor used Temperature function T Measured temperature in
81. 2 Measured values The measured value pair V mL and E the specified unit of measure ment is displayed 3 Table of measured values The measured value pair V mL and E the specified unit of measurement is displayed with the last five pairs of values 4 The list of the results generated up to this point appears on the display only if you did interrupt the method To follow the selected representation press RUN 02 93 METTLER DL77 DL70ES DL67 3 29 Display ANALYSIS 3 9 2 Curve type With this menu you can specify the curve that can be generated by the Titration or pH mV stat function The E V curve is stored as the default curve Select from the selection menu between E V curve Potentialvsvolume AE AV V curve 1st derivative potential vs volume log AE AV V curve 1st derivative potential vs volume logarithmic A E AV v curve 2nd derivative potential vs volume E t curve Potential vs time V t curve Volume vs time AV At t curve 1st derivative volume vs time To follow the selected curve type on the display press RUN Notes a If you wish to change the curve type during a determination fade out the titration with EXIT select the Display menu select the desired curve type and confirm with RUN The selected curve appears b If you wish to view for instance the table of measured vaiues orthe titration curve once again at the end of a sample determination
82. 2 e lodine ISE DX327 51107680 e Barium ISE DX337 51107674 e Surfactant sensitive electrode DS500 51107670 Reference electrode for e ion selective electrodes DX200 51089935 e surfactant sensitive electrode Inlab 301 52000128 Triaxial cabldelectrode cable with LEMO connector Cable SC LEMO 60 length 60 cm 89601 Cable SC LEMO 100 length 100 cm 89602 Cable SC LEMO 160 length 160 cm 51108034 Adapter cabf DIN LEMO to attach ox electrodes with a DIN connector to the titrator 89600 1 If sensors with DIN connectors are attached to the titrator via the adapter cable the advantages offered by the triaxial cable high level of protection against electrostatic interference are lost in part When using sensors with a very high resistance e g DG113 in nonaqueous solutions we advise against use of the adapter cable 09 2002 METTLER TOLEDO DL77 DL70ES DL67 11 35 Accessories Temperature sensors EE Pt1000 sensor LEMO cable connector 4 pin Elo for temperature sensors non METTLER Accessories for Karl Fischer titrations Double pin platinum electrode Electrode cable SC Banana Length 1 m Polarization current source External titration stand Order No DT1000 88321 DM143 SC 51108061 DK102A DV705 11 36 METTLER TOLEDO DL77 DL70ES DL67 03 2003 Accessories
83. 2 15 Sample EDITOR 4 Enteran initial identification ID1 number or name for all samples of this Sample function 5 Enter the molar mass M The auxiliary value Hj can be entered instead of the number provided that the molar mass has been stored here see Section 1 6 You can change the molar mass M before the start of the method see Section 3 1 6 Enter the equivalent number z For one Sample function you can enter only one molar mass M and one equivalent num ber z for your calculation If your sample contains several substances that have to be determined in the titration through equivalence points you must enter their molar mass and equivalent number in constant C under the Calculation function see Section 2 3 14 7 Select the temperature sensor from the selection menu if you have attached one see Section 1 3 if not select Manual The temperature entered before starting the method will then be used during the run see Section 3 1 With the aid of this parameter the temperature of the sample solution is automatically determined or acquired respectively before the start of the functions Measure Titration and pH mV stat The slope of the pH electrode is then corrected for the temperature in the pH value calculation see Section 1 3 Temperature sensors and Section 4 7 Calibration of the temperature sensors Important The Sample function fulfills two additional tasks within the method sequence 1 Itprovide
84. 3 5 1 3 installati n data rr aien inaia 5 4 5 2 D ta transfer E 5 5 5 2 1 We EE 5 5 5 2 2 ae O A 5 6 5 3 Memory COPY E 5 7 5 3 1 Request by computer for a copy of data stored in titrator 5 7 5 3 2 Request by titrator for a copy of data stored in computer 5 8 5 3 3 Request by Titrator 1 for a copy of data stored in Titrator 2 eee 5 9 02 93 METTLER DL77 DL70ES DL67 5 1 DOCUMENTATION Print 5 DOCUMENTATION In this menu you have the possibility to e print out the methods and installation data stored in the titrator e loadthe methods or installation data stored in a computer or a second titrator into the titrator and e copy all stored user methods and installation data either from the titrator to the computer or the converse or from one titrator to another titrator Menu Print Data transfer Memory copy 5 1 Print If you select Print the following menu appears METTLER methods User methods Installation data You can print out the stored methods and installation data 5 1 1 Methods If you select User methods for example you are shown a list with the method identification and the title of the methods you have stored Notes a Under the command Print in the Editor menu you receive a printout of each method with its functions and parameters see Section 2 1 1 b Ifyou wish to terminate the documentation press RESET Since the printer loads data into it
85. 32 Peripherals menu 1 28 pH stating example 2 65 pH mV stat function 2 62 pH measurement 4 12 12 6 METTLER DL77 DL70ES DL67 02 93 Index Piston assembling 11 5 inserting 11 5 Potential measurement 4 12 Power fuse 11 14 Power supply voltage 11 14 Predispensing 1 2 39 Predispensing 2 2 39 Predispensing end point titration 2 53 equivalence point titration 2 39 Pretitration 2 63 Printer connection 11 23 connection cable 11 27 Diabolo 1 28 DICONIX 180si 1 28 HP Deskjet 1 28 IBM 1 28 installing 1 28 LX800 1 28 Pt100 sensor 1 15 Pt1000 sensor 1 15 Pump function 2 25 Q 2 36 8 5 QDISP 2 24 8 3 QEX 8 5 QP1 QP2 8 6 8 9 QSTAT 2 62 8 8 QT 8 7 8 9 QT1 QT2 2 62 8 7 8 9 QTOT 2 62 8 7 Question mark 2 5 2 14 R result 2 66 8 8 Raw results compilation 8 9 explanation 2 21 recording 2 78 3 32 8 9 storage 8 25 Rear view of the titrator 11 12 Recalculation 3 34 Recommendation menu 1 5 Record function 2 77 Records analysis menu 3 32 Record header 1 37 Reevaluation 2 52 3 19 Reference electrode 1 9 Relative standard deviation 2 75 REMOTE CONTROL 7 3 Remote control 7 7 Representation display 3 29 RESET auxiliary functions 4 5 current method 3 15 documentation 5 3 list continuous 3 40 Resources deleting 1 3 explanation 1 3 list 1 3 Result s displaying 3 29 examples 2 67 2 68 8 26 Karl Fischer titrations 10 14 learn titration 3 13 maximum number method 8 25 R 2 66 2 69
86. 5 ul ld 2 0 MAX DOE 20 0 Delay Slim 15 End point mode EPA Potential MV pH iiss 7 0 TONCONCy cconccccccnnnnnccncnnnnnncnnrnnnnncrnn Positive Maximum volume Tom 40 0 CONMditiON oooocconnccciniciconanacnnncccnnnrnnnnnccinnnos Yes Condition ada ici 1 lt E lt 7 Through this function the titrator acquires the measured value E pH The titrator executes this Titration function only if the measured value E determined previously is in the pH range 1 7 8 18 METTLER DL77 DL70ES DL67 02 93 Functions with a condition Calculation Result Name oooiocccccnnnnccnncnnnnncnnnnnnncnn Acidity Form la enina at R Q C U CONS Tu TN C 1000 Result UI mmol L Decimal places sersa 2 A A Yes CONO EE 1 lt E lt 7 d Titration A A T HCI Concentration Immo 0 1 SONS usada ana DG111 SC UNICO MCAS ccoo As installed Titration mode EP Titrant additiON c ooooconccnnnccnnnonannnncccnnns Dynamic AE Set Im 8 0 AV min ML vecinita 0 02 AV Max Im 0 1 AE MVision 0 5 ER 0 5 MIN DOE 2 0 t IMAX Sl siiin 20 0 Delay Sii 15 End point mode cocococcoccccncccconancncancccnn EPA Potential mV pH siisii 7 0 Tendency 2sccececceceeeeeceteteeeteeccttteees Negative Maximum volume mL 40 0 A A adaa Yes CONGO Merni 7 lt E lt 14 d Calculation AA Basicity ll E R2 Q 2 C2 U CONSTE vercion a C2 1000 SU e mmol L Decimal places ooooonooccccnnicccccnnnccccnn
87. 7 DL70ES DL67 02 93 EDITOR Pump 2 3 8 Pump With the aid of this function you select a time controlled pump at an auxiliary output in order to pump a specified volume of an auxiliary reagent into the titration vessel 1 Select the auxiliary reagent from the recommendation menu or enter one you have installed see Section 1 3 2 Enter the volume mL 3 Select a condition No Yes Enter the condition Notes a You have defined the pump speed mL min which you need to determine experimentally for each auxiliary reagent in the Installation menu by means of the dispensing rate see Section 1 4 2 b If you attach the pump tubing to the wrong connectors you will evacuate instead of dispensing 02 93 METTLER DL77 DL70ES DL67 2 25 Rinse EDITOR 2 3 9 Rinse You use this function only in connection with the sample changer ST20A or ST20 This has a built in rinsing unit that controls the attached pump for rinsing output RINSE or DOSE The tips of the sensors and burettes are rinsed in the middle beaker position see S720 or ST20A Operating Instructions 1 Select the auxiliary reagent from the recommendation menu or enter one you have installed see Section 1 4 2 Enterthe volume mL 3 Select a condition No Yes Enter the condition Notes a You have defined the rate of the rinsing process mL min which you need to determine experimentally in the Installation menu by
88. As soon as it has executed this function it begins to stir at the default speed y Measure MEASURE The titrator acquires the measured value E in each case y Calculation CALCULATION You define a result R E This stores the 3 mea sured values of the 3 buffer solutions y No Ki Series size y Yes Calibration Thetitrator assigns the acquired measured values of the Measure function to the values of the 3 buffer solutions and in this manner calculates the zero point y and the slope of the electrode The entry Ri i index must be the same as in the RECORD Calculation function in this case it is R CALIBRATION 2 74 METTLER DL77 DL70ES DL67 02 93 EDITOR Statistics 2 3 18 Statistics With the aid of this function you obtain a statistical evaluation of the results of a series titration The titrator calculates the mean value x automatically when you have the Statistics function in your method If you nevertheless titrate only one sample with this method the titrator ignores the function 1 Enter Ri i index see Use of Indexes Section 8 2 and the following chart 2 Select the standard deviation s Yes or No 3 Select the relative standard deviation srel Yes or No 4 Select outlier test No Yes The titrator checks the results in accordance with an outlier test following Grubbs It removes outliers and repeats the statist
89. Calculation s designations 8 3 8 8 formulae 8 26 function 2 66 indexes 8 10 recalculation 3 34 Calculation operations 2 66 Calibration data determination 2 72 entry through calibration 1 12 for sensor inputs 1 12 theoretical values 1 12 Calibration function 2 72 sensors 2 72 temperature sensors 4 23 Calibration method 2 74 Character set 1 33 Code sync fct 2 81 Comment sync fct 2 81 Communication protocol 1 33 Communication titrator lt gt computer introduction 7 5 overview 7 5 Comparison operators 8 17 Computer connection 11 23 connection cable 11 38 installing 1 33 Concentration mol L 1 5 8 3 Conditioning function 2 27 Condition for functions 8 16 Conditioning mode fix explanation 2 27 flexible explanation 2 27 selecting 1 26 Conductivity measurement 1 11 Conductometer 1 11 Constants calculation function 2 66 calculations menu 3 34 examples 8 27 Continuous titrant addition 2 54 Continuous addition pH mV stat fct 2 63 Control band 2 54 Control range 2 63 Conversion constant 8 28 Correction factor 3 7 Correlation coefficient 2 62 2 64 CSTAT correlation coefficient 2 62 8 7 8 9 Cursor keys during entry 1 4 2 10 during titration 3 29 Curve type display 3 30 Data administration 7 6 Data backup 7 7 Data bits printer 1 29 system 1 32 Data entry LIMS 3 6 Data storage pH mV stat fct 2 64 Data transfer installation data 5 6 method 5 5 Date entering 1 36 selec
90. DL67 8 15 Functions with a condition 8 3 Functions with a condition In titration praxis there are several applications that require a departure from the sequence defined in the series listing of the functions For this purpose you can set a condition for most of the functions If this condition is not satisfied the function is skipped if itis met the function is executed If no condition has been set again the function is executed You can not set a condition for Title Sample Calibration and Statistics Con FUNCTION y No Conditon satisfied y Yes Function is executed y e FUNCTION Examples of conditions are comparisons of raw results results and numeric values that have been obtained before the conditional function You can define a condition comparison of argument arg with a value a or b by means of operators a and b can be e numeric values e designations e expressions Example of an expression R1 H5 8 16 METTLER DL77 DL70ES DL67 02 93 Functions with a condition a Comparison operators arg gt a greater than arg gt a greater than or equal to gt arg a equal to arg lt a less than or equal to lt arg lt a less than a lt arg lt b in the range arg lt gt a not equal to Examples Ri gt 4 2 the first result should be greater than 4 2 ESTO the potential should be smaller than pH 7 0 R2 H4 the
91. ES DL67 8 23 Restrictions 8 5 8 5 1 Restrictions in method development and execution Maximum number of functions per method The maximum possible number for a particular function that you can add to a method is listed in the following Table The number depends on the method size in each case for example you can not assemble the total of these functions to form a method as the main memory of the titrator is too small 8 5 2 Function Maximum number method A O II A 1 A 4 O eege 6 O II ne se Oe eee a 10 E ler 10 et EE 10 O e 6 PUMA ncsutitccsiejere ebe Edi a R Aa le 6 RINSE ege 6 Re el le e EE 6 Auxiliary instrument oooooonnncccccccnnccccononononononnnnnannnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnes 6 EE geet 6 o EE 2 CS ACUI AMO NT sostenida rs adios 12 Auxiliary value eta 20 Eeer ee 2 A 2 A A E 6 o A A A ON 8 SYNG putada 20 Maximum number of samples DL77 The sample data for a maximum of 600 samples can be entered in the method list of Analysis menu A as well as in that of Analysis menu B You can enter 60 sample data per method DL70ES The sample data for a maximum of 600 samples can be entered in the method list of the Analysis menu You can enter 60 sample data per method DL67 This titrator can store the sample data of maximum 60 samples 8 24 METTLER DL77 DL70ES DL67 02 93 Restrictions 8 5 3 Maximum number of methods in the method list of the Analysis menu DL77 A maximum of 10 met
92. G ito e ooh ee Re a e mL Volume Mb eege bbe wie ce oe ee L 0 Titrant a dition swiss wie ie EN d RL Dynamic ABMS MV sitas isa oe 8 0 AV min ME os seine EEN cee eee hee eee ee 0 05 AY max Tel Zeg Bicone weaved Ooh ed 0 LS AE MV siem e ida e a 0 5 A Tech ries ds ake aa 0 5 mIn Tel rr e a a 2 0 Ema Tel iran sa as ad 20 50 Detay ST wearers e e e wile ere a 0 End pOint mode esas eens doe e eege EPA Potential mV pH A 6 568 TENGENCY desa a eee a eee dede Positive axim m VOLUME sis ia EEN EEN EN ee 20 2 60 METTLER DL77 DL70ES DL67 02 93 EDITOR Titration LEARN EP The titrator always titrates the entire volume of the burette used Thus you must select the weight volume of your sample in accordance with the burette volume The titrator calculates the parameters from the response behavior of the sensor the shape of the titration curve and with due consideration of the burette volume used You thus always obtain e the parameters of the titrant addition Dynamic and e the parameter of the endpoint mode EPA If the titrator finds more than one endpoint it calculates the parameters for the one with the greatest slope The titrator always specifies its tendency at a detected endpoint Ifthe titrator finds no endpoint itinterrupts the method You are shown an error message see Section 3 4 Notes a Since the titrator immediately stores the parameters of the titration mode EP you can titrate a s
93. IONS coooooooccccoooocccccoocccccnooncccconnnnncnonnnnnnnnnnnncnnnonnncnnnnnnes 4 3 4 1 A 4 6 4 1 1 Rinse HKH 4 6 4 1 2 RINSS UN su ci dida 4 7 4 1 3 DISPENSE cecon e 4 7 4 1 4 Dispense continuously sicario 4 8 4 1 5 Manual titration fo 4 9 4 2 A o 4 11 4 3 ER 4 12 4 4 Temperature tee 4 14 4 5 REI e E 4 16 4 5 1 Misa A A 4 16 4 5 2 TUES TO e soii 4 17 4 5 3 T rmtable Dacia a 4 17 4 5 4 Rinsing PUMP E 4 18 4 5 5 Rinsing p mp MATAS lt a 4 18 4 5 6 Dosing PUMP ercer ta 4 19 4 5 7 Dosing pump Hu 4 20 4 5 8 DISPO sr EE carats 4 20 4 6 Auxiliary instrument EE 4 21 4 6 1 Time contro led EE 4 21 4 6 2 Manual geet 4 22 4 7 Calibration of the temperature sensors oooococccoococcccccccccccnaanccnnnccnnannnnno 4 23 4 8 Offset adjustment of the sensor inputs ooooocoononocccccccccccccnancnincccnannnnnno 4 24 02 93 METTLER DL77 DL70ES DL67 4 1 AUXILIARY FUNCTIONS 4 AUXILIARY FUNCTIONS With the aid of this menu you can rinse burettes perform manual titrations start the stirrer measure the pH or temperature of solutions operate the sample changer manually and pump solvents These auxiliary functions are independent of a titration method butthey can support or expand it The menu Auxiliary functions Burette Stirrer Sensor Temperature Sample changer Auxiliary instrument Calibration temperature sensors 0 JO oO FPF W NY R Offset adjustment sensor inputs As with all menus of the titrator you can se
94. IS 3 14 2 Changing the Analysis menus mV E V curve Myla Method Method gt M001 MM Add Interrupt Sample data A Display Stirrer Method data Record data RT mV E V curve mL B Y Method list gt CALC MM AIC3 MM Brom MM Y mV E V curve mL In ANALYSIS B the Titration function of the CALC method is processed To switch to ANALYSIS A press this key combi nation The method list with the selection menu method faded out appears You can select or execute all menus or commands In order to follow the running method M001 on the display press this key combination To switch back to ANALYSIS B press this key combination The method list appears if more than one method is stored You can select one of the methods in order to modify method or sample data using the selec tion menu To follow the still running method CALC on the display immediately press lt index T gt 3 44 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Sample series with 2 sample changers 3 15 Sample series with 2 sample changers If you have connected two sample changers you can sequentially titrate maximally 40 samples from one or several methods unattended The titrator is told to change the titration stand from ST20 1 to ST20 2 or vice versa
95. Installation instructions 11 1 5 Power supply voltage power fuse The titrator operates within a voltage range of 100 120 or 220 240 V The fuse holder serves as range selector Changing the voltage range The instrument is set to the voltage range shown by the opposing arrows 3 If you have to change this lever out the fuse holder 1 with a screwdriver 2 rotate the fuse holder by 180 4 and reinsert This activates the fuse 5 Replacing defective fuses Lever out the fuse holder 1 with a screwdriver 2 Replace the active fuse 6 by one with the same rating 100 120 V T1 6 L250 V 220 240 V T800L250 V Reinsert fuse holder Note The standard equipment includes a set of spare fuses for the voltage you specified when ordering the titrator Caution The titrator should not be used in a power distribution system without a direct ground connection IT power system 11 14 METTLER TOLEDO DL77 DL70ES DL67 03 03 Installation instructions 11 1 6 Inserting an RS option sensor input 2 RS232C interfaces Slide the burette off the titrator and unscrew the baseplate The titrator must be disconnected from all voltage sources before you remove the baseplate 4a 4b 4c Risk of electric shock This description applies in case you insert the RS option first see next section Push in protrusions 1 of three plugs 2 with a screwdriver and push out the plugs
96. L 11 A2E Av2 V curve Would you like a record of the 2nd derivative of the titration curve potential vs volume of the last sample The ordinate scale is linear Select Yes with SEL 12 E t curve Would you like a record ofthetitration curve potential vs time of the last sample Select Yes with SEL 13 V t curve Would you like a record of the titration curve volume vs time of the last sample Select Yes with SEL 14 Av At t curve Would you like a record of the titration curve ofthe 1st derivative volume vs time of the last sample Select Yes with SEL 2 78 METTLER DL77 DL70ES DL67 02 93 EDITOR Record 15 Select a condition No Yes you are shown the following mask Condition Termination after record If you select Condition you must enter a condition If you select Termination after record you have two possibilities No or Yes With this termination parameter you can abort a method when the defined condition is satisfied Example In your method the number of samples is n 3 You wish to abort the method when the titrator finds no equivalence point in one of the samples but would like to use a recorded table of measured values or titration curve for possible determination of the reason for this The condition in this case is neq 0 see Section 8 1 List of designations and Section 8 3 Functions with a condition Your method should comprise the following functions for
97. L smallest volume increment e g 0 05 Enter AV max mL largest volume increment e g 0 3 If no predispensing is performed the titrator dispenses the first two volume increments with AV min The measured value acquisition is equilibrium controlled see Section 2 3 12 2 Titration mode EQP Measure mode EQU You must therefore enter the following parameters AE mV e g 1 At s e g 2 t min s e g 3 t max s e g 30 De equilibrium condition applies only in the end point range defined by the following ormula EP range EP 1 5 AE set Example Ifthe end point is 30 mV the condition thus applies for above values of 15 to 45 mV Outside this range the following applies AE outside 4 AE If the endpoint is reached the following applies AE AE 2 Enter delay s e g 15 This is the time from attainment of the end point up to the definitive termination of the titration If the potential falls below that of the end point during this time the titrator adds additional increments 02 93 METTLER DL77 DL70ES DL67 2 55 Titration EP End point mode EDITOR Selection menu End point mode You have a choice between three end point titrations 1 Select EPA absolute end point The absolute end point is the end point value relative to zero on the electrode signal scale Enter EPA mV pH 2 Select EPR relative end point The relative end point is the difference be
98. L70ES DL67 2 53 Titration EP Continuous EDITOR Selection menu Titrant addition You select the continuous or dynamic titrant addition Continuous The titrator dispenses the titrant slowly at first then at maximum rate up to a specified control band mV pH Within the control range the rate diminishes exponentially In the vicinity of the end point it adds the increment that you define the smallest increment that the titrator can dispense is 1 5 000 of the burette volume It measures the initial potential ET1 after 1 3 s and acquires a measured value every 5 seconds for the table of measured values 1 Enter control band mV pH e g 250 2 Enter delay s e g 15 This is the time from attainment of the end point up to the definitive termination of the titration If the potential falls below that of the end point during this time the titrator adds additional increments 3 Enter AV min mL e g 0 01 This is the smallest increment to be added near the titration end point E mV pH Start of the control range 200 100 Control band 250 mV 4 3 pH 100 End point 200 V mL 2 54 METTLER DL77 DL70ES DL67 02 93 EDITOR Titration EP Dynamic Dynamic The conditions that apply to the dynamic titrant addition are the same as those for DYN of the equivalence point titration EQP see Section 2 3 12 2 1 2 a e D Enter AE set mV e g 10 Enter AV min m
99. M001 are stored in the DL67 02 93 METTLER DL77 DL70ES DL67 1 3 Titrants INSTALLATION 1 1 Titrants When you select this menu you receive the installed titrants with the specified parameters concentration and burette drive You will find the menu tree depicted at the end of Section 1 1 2 NaOH 0 1 mol L Drive 3 HC1 0 1 mol L Drive 3 HC104 0 1 mol L Drive 3 EECa DL67 The DL67 only has stored the titrant NaOH You can however add titrants to the list see Section 1 1 3 If you select for instance NaOH the list will be masked on the right by a selection menu containing the following commands Delete Modify Add 1 1 1 Delete Position the selector bar on this command and confirm with RUN The mask of the selection menu disappears the titrant NaOH is deleted Note You can also delete a titrant directly from the list by pressing the lt gt minus key You can reinstall NaOH with the command Add see Section 1 1 3 1 1 2 Modify If you select this command you are shown the parameter mask of the titrant see next page If you move the selector bar to one of these parameters you can modify its name or value Note a Default values are stored in the titrator for all parameters e g for the concentration of the titrant 0 1 mol L for the titer 1 0 e These values will be overwritten once you have entered new ones e If you want to modify only one digit of a value you must first in
100. Modelo del ciclo de vida de un producto y y Fose Cococimientos b sicos Comenzio del proyecto Imagen del producto Especificaciones Plan de calidad Documentaci n del proyecto Plan del proyecto Protocolo de revisi n Fase Vidbilidad Especificaciones del software Plan de ensayos Protocolo de revisi n Fase Verificaci n Protocolo de revisi n Fase Fin del proyecto Preparaci n Protocolo de revision Utilizaci n Servicio t cnico CRIS Deseos del cliente y 03 99 METTLER DL77 DL70ES DL67 12 17 Dichiarazione di validazione del sistema Con la presente Vi informiamo che prodotti sistemi DL67 DL70ES DL77 inclusi software e accessori sono stati sviluppati controllati e validati secondo le regole tecniche relative al ciclo vita dei prodotti della Mettler Toledo GmbH Analytical Queste regole si basano sulle norme ISO 9001 1994 dettagli di controllo del progetto sono stati verificati ed approvati dall organo di supervisione del progetto PSG Project Supervisory Board prodotti sistemi sono stati controllati e verificati prima della fornitura Per soddisfare le richieste di validazione e GLP i seguenti documenti sono messi a disposizione per la visione da parte di personale autorizzato e Specifiche del prodotto e Linee direttive e Documentazione del progetto e Specifiche del software e Sistema di qualit e Disposizioni per la gestione del progetto e Piano de
101. Not installed Baud rate 4800 Parity Even Number data bits 8 bits Number stop bits 1 stop bit Baud rate system 1200 SG Y 2400 Select instrument Instrument type Select another baud 4800 type with SEL Color terminal rate with SEL 9600 Monochrome term Computer Not installed A PA Select another parity with SEL System parameters Instrument type Computer y Baud rate 4800 O Parity Even Select 7 bits with SEL Number data bits 8 bits Number stop bits 1 stop bit EE AnS l _ Select 2 stop bits with SEL y Computer Character set ASCII Send mode Spontaneous Communication protocol Normal Start end characters lt STX gt lt ETX gt 1 34 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Peripherals 1 8 4 Sample changer Ifyou wish to attach the sample changer ST20A or ST20 you have to install it Select Sample changer and you are shown the following parameter status Select the relevant parameter with SEL Not installed or Installed DL77 This titrator can control two sample changers see Section 1 7 Titration stands ST20 1 and ST20 2 The condition for this is that you must use at least one new sample changer the ST20A ST20 is the name of the older model The second sample changer is connected to the first with the dublex cable ST20A You can designate the two sample changers ST20 1 und ST20 2 using t
102. Operating Instructions METTLER TOLEDO DL77 DL70ES DL67 Titrators INSTALLATION EDITOR ANALYSIS AUXILIARY FUNCTIONS DOCUMENTATION USER LEVEL REMOTE CONTROL Designations Explanations Examples Error messages and malfunctions 10 Applications 11 Installation instructions Technical data Accessories 12 Index Certificates amp Declarations Safety measures The titrators have been tested for the experiments and intended purposes documented in the Tutorial and these Operating Instructions However this does not absolve you from the responsibility of performing your own tests of the products supplied by us regarding their suitability for the methods and purposes you intend to use them for You should therefore observe the following safety measures Measures for your protection Ensure that you plug the power cable supplied into a receptacle outlet that is grounded In the absence of grounding a technical fault could be lethal Switch the instrument off and disconnect the power cable before you open the housin or change blown fuses An electric shock could be lethal Risk of electric shock Never work in an environment subject to explosion hazards The housing of the instrument is not gas tight explosion hazard due to spark formation corrosion caused by the ingress of gases Risk of explosion Always test the titration v
103. Photometrically with DP550 DP660 Conductometrically non Mettler unit with analog output Temperatur e compensation Temperatur e input via keypad or by means of a temperatur e sensor for pH pM pX measurement Amplifier range 2000 mV Resolution 0 1 mV 0 002 pH pM pX Maximum permissible error 0 1 Zero point drift 10 gt 35 C lt 40uV C Sensor input 1 and sensor inputof the temperature option Triaxial socket LEMO e Offset current lt 1 pA 20 C e Input impedance gt 5 10 Q protected up to 1000 V capacitively Reference electrode input ref Banana socket 4 mm e Input impedance gt 3 10 Q protected up to 1000 V capacitively Sensor input 2 and sensor inputof the RS option Triaxial socket LEMO e Offset current lt 30 pA 20 C e Input impedance gt 5 10 Q protected up to 1000 V capacitively Temperatue sensor inputs Emp 1 Temp 2 of the temperatur option e Range 20 C 120 C e Resolution 0 1 C e Maximum permissible error 0 2 C e Measurement principle Four terminal resistance measurement Pt 000 standard or Di 00 The sensor number of the option depends upon its installation see Sections 11 1 4 11 1 6 and 11 1 7 03 03 METTLER TOLEDO DL77 DL70ES DL67 11 19 Technical data 11 2 2 Auxiliary outputs Aux 1 Aux 2 Aux 3 Operating modes Mode 1 For stirrer Mode 2 Other auxiliary instruments Voltage range Mode 1 0 18V 150 mA Mode 2 24V 500 mA Each output is
104. S DL67 2 43 Titration EQP TFIX EDITOR TFIX After each increment addition the titrator waits for the time you have defined before it accepts the measured value 1 Enter At s E mV Measured value Measured value Measured value Measured value Increment addition Increment addition Increment addition At 3s At AS Ata 35S t s 2 44 METTLER DL77 DL70ES DL67 02 93 EDITOR Titration EQP Threshold Equivalence point recognition The equivalence point recognition with a titration curve depends on the reaction type of the components and hence on the evaluation procedure see below this section 1 Inthe evaluation procedures Maximum and Minimum an equivalence pointis recognized when the highest lowest potential value of the titration curve is greater smaller than two preceding and two subsequent values 2 Intheevaluation procedures Standard and Asymmetric an equivalence pointis recognized when the maximum of the absolute values of the 1st derivative of the titration curve is greater than two preceding and two subsequent values 3 In the evaluation procedure Segmented an equivalence point is recognized when the maximum of the absolute values of the 2nd derivative of the titration curve is greater than two preceding and two subsequent values Note For the earliest possible recognition of an equivalence point the titrator requires a certain number of measurement points e The n
105. TTLER burette The titrator acquires the dispensed volume as the raw result VDISP mL or QDISP mmol see List of designations Section 8 1 and the Measure function Section 2 3 4 1 Selectthe titrant from the recommendation menu or enter one that you have installed see Section 1 1 2 Enter its concentration mol L 3 Enter the volume mL A formula such as R1 0 5 can be entered instead of a number R1 is the result of a Calculation function preceding this function 4 Select a condition No Yes Enter the condition Example For a simple back titration you can add e g the Dispense function to the standard method lt Sample SAMPLE You have added your sample to the titration vessel and started the titration The titrator immediately starts to stir e Dispense DISPENSE The titrator dispenses the amount of the selected titrant and acquires the raw result QDISP e Stir STIR You have set a long stirring time to allow the sample to react with the titrant before the titrator starts the back titration ER Titration TITRATION The titrator starts the back titration with a second titrant and acquires the raw result Q consumption of the titrant in mmol up to the equiva y lence point or endpoint Calculation N The formula for the content of the sample y R QDISP Q C m see Section 8 6 Examples of formulae 2 24 METTLER DL7
106. Titration time gt 4 min gt Step by step set EPA of the first Titration function higher 10 2 7 Drift compensation The titrator acquires the running time for each processed method as the raw result TIME see Section 3 1 3 Note a TIME is saved as auxiliary value H19 before starting see method and as H18 at the end of each sample determination The difference between these values gives the titration time see 3rd Calculation function and is used in the drift compensation see 4th Calculation function 10 12 METTLER DL77 DL70ES DL67 02 93 Karl Fischer methods 10 2 8 Problems The titration does not start Possible cause DK102A not switched on Possible problems their cause and rectification Measures Switch on DK102A Initial potential too high above 170 mV Battery voltage of the DK102A current source too low Contaminated electrode Bent platinum tips Check voltage if need be change battery Clean with chromic acid and dry thoroughly Drift value too high Titration vessel not closed Titration vessel not completely dry Check Allow standby titration to continue for a further 1 2 h if need be overnight Overtitrated Contaminated electrode Poor mixing End point of the first Titrati on function too high Clean with chromic acid and dry thoroughly Increase stirring speed Set end point 2 5 mV lower see Section 10 2 6 Long titration time slug
107. Y STATISTICS Y RECORD Sample n 3 lower weight limit 1 0 g upper weight limit 3 0g M 60 01 z 1 Always enter the molar mass and the equivalent number of the substance that is determined first Stir Speed 80 time 60 s The titrator stirs for 60 s to ensure proper suspension of the ketchup before starting the Titration function Titration Titrant 0 1 mol L NaOH sensor DG111 SC unit of measurement mV titration mode EQP Record If you wish to have a record of the titration curve and the table of measured values of this titration you must add the Record function here The titrator will not store these data if a second Titration function follows Instruction The inputted request Add H2SO appears The pH of the solution must be lowered for the chloride determination Confirm the instruction with RUN Titration Titrant 0 1 mol L AgNOsz sensor DM141 SC unit of measurement mV titration mode EQP Calculation R Q C m C M 10 z unit Calculation R2 Q 2 C2 m C2 3 55 M 10 z unit The constant for the determination of chloride must now be entered as numerical value Statistics Ri i index R The mean value of the first result first Calculation function of the three determina tions of the acetic acid content is calculated Statistics Ri i index R2 The mean value of the second result second Calculation function of the thr
108. a parameter with RUN you can start stirring Start press 2 or RUN e The titrator begins to stir at the specified speed You can stop stirring with RUN or 3 To obtain the Auxiliary functions menu again press lt index F gt Note If you wish to execute another auxiliary function e g Dispense or a method which utilizes Stirrer start this auxiliary function first quit the selection menu with the appropriate key combination lt index F gt or lt index A gt and then select the other auxiliary function or start the method 02 93 METTLER DL77 DL70ES DL67 4 11 Sensor AUXILIARY FUNCTIONS 4 3 Sensor With the aid of this function you can measure potential values of solutions mV pH T etc The measured values can be printed out Caution You can measure simultaneously with only two sensors Sensors reserved for a certain method cannot be selected This applies to e the sensors being used in a current method and e all sensors that will be used in the methods that have been activated with the commands List once or List continuous see Sections 3 13 3 2 and 3 13 3 3 If you press function number 3 in one of the other menus lt index F gt then 3 you are shown the selection menu 1 Modify 2 Start Modify press 1 You are shown the parameters whose value or name you can modify If you press lt index F gt 3 1 when e g in the main menu you are shown the parameter mask imm
109. abX light titration software set of Operating Instructions LabX light in accordance with your order 709165 in accordance with your order in accordance with your order 200495 73072 71300 89601 25868 201508 51106330 in accordance with your order D As of June 1999 METTLER TOLEDO will no longer manufacture the DL67 09 2002 METTLER TOLEDO DL77 DL70ES DL67 11 27 Accessories 11 3 2 Optional accessories The numbers enclosed in parentheses refer to the purchase order e g of an interchangeable burette In case of additional orders some parts are available only in multipack form or in minimum quantities Order No 1 Burette drive DV90 2 Interchangeable burettes Interchangeable burette complete 1 mL DV1001 5 mL DV1005 10 mL DV1010 20 mL DV1020 comprising 1 L brown glass bottle 1 71296 e Burette holder 23645 Piston 1 DV1001 51107535 DV1005 51107115 DV1010 51107116 DV1020 51107117 11 28 METTLER TOLEDO DL77 DL70ES DL67 09 2002 Accessories Order No Stopcock 1 with valve di8kmade of PTFE light gray 51107537 ceramic dark brown 51107525 Y Both valve disks are chemically resistant For 24 hour use with titrants that have a tendency to cristallize out we recommend the ceramic disk q Light protection tube 1 23644 Se Dispensing tube 1 with siphon t
110. aces 4 Calculation Result name ssscoisinnecnrnrennn NH 4Cl POM UA rra R3 Q2 2 Conlara ios Result unt mmol Decimal places isc 4 Thetitrator executes the second Titration function lt determines among other things the mmol consumption Q1 2 up to the first equivalence point CH3COOH then the mmol consumption Q2 2 up to the second equivalence point NH4Cl In the second Calculation func tion you define the mmol con sumption for acetic acid You take into account here the titrated excess of the first Titra tion function In the third Calculation function you define the mmol consumption for NH4Cl 02 93 METTLER DL77 DL70ES DL67 8 13 Use of indexes 8 2 1 Compilation of designations according to indexing forms Method Resource Designation Unit Examples Function Current method s Titrant mol L SAMPLE g mL g mol CALCULATION AUXILIARY VALUE TITRATION Oz EPOT1 2 8 14 METTLER DL77 DL70ES DL67 02 93 Use of indexes Function MEASURE Designation Unit mV pH TEMPERATURE PE F K DISPENSE mL mmol TITRATION mV pH mV pH mV pH mL mmol mL mmol mL mmol pH mV STAT mL mmol mL mmol mL mmol mL min mmol min STATISTICS Examples QDISP 2 QT1 2 02 93 METTLER DL77 DL70ES
111. all titrants stored in the titrator on delivery Check what list has been changed If the user data memory is too small the titrator stores only the titrants for which it has space If the memory is full the titrator does not store any titrant In this case you must delete other installation data or one of your methods to create memory space Then switch the titrator off and on again Check that all resources are again present If you are frequently shown the error message you should contact METTLER service 02 93 METTLER DL77 DL70ES DL67 9 3 Error messages and malfunctions 3 Storage not possible a Thetitrator can not assign the titer auxiliary value or the calibration parameters to the appropriate resources as their list is missing titrant sensors or auxiliary values Measure Confirm the message with RUN Check whether the list of the resource has been deleted Switch the titrator off then on again The titrator reloads the standard list of the corresponding resource e g all the titrants stored in the titrator on delivery If the user data memory is too small the titrator stores only the titrants for which it has space If the memory is full the titrator does not store any titrant In this case you must delete other installation data or one of your methods to create memory space Then switch the titrator off and on again Check that all resources are again present
112. aluation criteria 2 51 explanation 8 21 Audio signal 1 39 Automation 7 7 Auto stand 1 25 3 13 Aux 1 2 3 auxiliary outputs 1 18 1 20 1 26 AUXILIARY FUNCTIONS menu 4 3 menu tree 4 4 Auxiliary instrument s adding 1 21 auxiliary function 4 21 deleting 1 20 function 2 31 installing 1 22 menu tree 1 21 modifying 1 20 Auxiliary outputs auxiliary instrument 1 20 auxiliary reagents 1 18 stirrer 1 26 Auxiliary reagents adding 1 18 deleting 1 17 installing 1 19 menu tree 1 19 modifying 1 17 Auxiliary value s entering 1 23 entry through determination 1 23 function 2 70 menu tree 1 24 Auxiliary value memory 1 23 2 70 Back titration example 2 24 Balance s configuration METTLER 1 30 configuration SARTORIUS 1 31 connection 11 23 connection cable 11 37 installing 1 30 Baud rate balances 1 30 1 31 printer 1 29 system 1 32 Bidirectional transmission mode 1 30 3 9 Buffer potential 1 2 51 8 6 8 9 Buffer potential 2 2 51 8 6 8 9 Buffer solutions DIN NIST buffer 2 72 Ingold buffer 2 73 Merck Titrisol buffer 2 73 02 93 METTLER DL77 DL70ES DL67 12 1 Index Burette air bubbles 11 9 equipping 11 7 inserting 11 8 installation instructions 11 5 Karl Fischer titrations 10 5 maintaining 11 5 11 8 menu 4 6 rinsing 4 6 Burette drive inserting 11 3 selecting 1 5 Burette volume selecting 1 5 smallest increment 2 40 C constant 2 67 8 8 c nominal concentration 8 3 c t actual concentration 8 3
113. alue and the drift condition is satisfied but at the latest after t max 7 Select a condition No Yes Enter condition Notes a The Measure Temperature Dispense Titration and pH stat functions generate raw results see List of designations Section 8 1 You can print these out as such on an attached printer see Section 2 3 19 and Section 8 1 1 for exceptions incorporate them in the calculation see Examples of formulae Section 8 6 1 save asaresult if you have assigned them to the result R e g R E see Section 2 3 14 b Atthe end of a titration only the final results are shown on the display of the titrator the raw results can only be printed out c Thetitrator stores raw results up to the titration of the next sample within a loop see Section 8 5 7 02 93 METTLER DL77 DL70ES DL67 2 21 Temperature EDITOR 2 3 5 Temperature You can use this function to measure the temperature of a solution under defined conditions The titrator acquires the measured value as raw result T see Note a in Section 2 3 4 Parameters of the mask Sensor Unit of meas urement AT C Py K At s t min mode t max s Condition 1 Select the temperature sensor from the selection menu see Section 1 3 2 Select the unit of measurement from the selection menu C F or K 3 Enter AT C F K e g 0 02 4 Enter At s e g 2 Note The temperature drift must be l
114. and Use of indexes Section 8 2 The titrator checks your entries when you quit the parameter mask with EXIT If you have entered a wrong formula or constant you will immediatly be sent an error message see Section 2 2 5 Modify functions Note b If you have defined raw results such as R QDISP which the titrator can not know as a Dispense function did not precede this Calculation function you will not be sent an error message until you try to save the method Example A If you require for instance from an NaOH solution that you titrate with HCI not only the wt NaOH as the result but also the mmol consumption of HCI and the potential value of the equivalence point you must specify three calculation functions for this method see Section 8 1 Listofdesignations Section 8 2 Use of indexes and method M001 in the Tutorial Formula Constant Unit 1st Calculation function Al et Delete C with CE mmol it is not needed 2nd Calculation function R2 EPOT Delete C with CE mV it is not needed 3rd Calculation function R3 Q C m for C M 10 z K 02 93 METTLER DL77 DL70ES DL67 2 67 Calculation EDITOR Example B For the calculation of a titration curve with 3 equivalence points acidic mixture of 3 substances you also have to define the parameters of three Calculation functions The respective constants C1 C2 and C3 are then also needed see Use of indexes Section 8 2 R3 R2 R1
115. are in the Method ID M001 method entry mask You can simply change the User roro method ID Data entry Y A Press this key combination Method list The method list appears again etc M001 roro M002 roro 02 93 METTLER DL77 DL70ES DL67 3 35 Method list ANALYSIS Notes a If no method with the specified identification is stored in the titrator and you have installed a computer the method will be requested from the computer and added to the method list see Operating Instructions provided with the RS option b You can modify or enter method and sample data e immediately see Section 3 1 e before starting the method see Section 3 1 e during a current method see Sections 3 7 and 3 8 3 13 2 Modifying the method list You can cut delete an added method and paste it in at another location 3 13 2 1 Cut Example Method list MOO1 roro M002 roro CALC roro KM58 roro Select the method e g KM58 and press the lt gt key minus sign The 4th method together with its sample data is cut deleted however it is stored in a buffer memory so that you can paste it elsewhere 3 13 2 1 Paste You would now like to position the cut method KM58 with its sample data on the top of the method list Select method M001 and press the lt gt key equals sign The former 4th method is now the 1st method Method list KM58 roro MOO1 roro M002 roro CALC roro Caution Bear in mind the sequ
116. ase The mean value of all titrated samples is Formula R3 X X 2 2 calculated with the 3rd Calculation func Constant tion etc 02 93 METTLER DL77 DL70ES DL67 3 45 Sample series with 2 sample changers ANALYSIS If you wish to run several methods on both sample changers with List once one of the methods must be used to initiate the change from one stand to the other in each case An example Method list The first two methods are acid content determina HAC1 dabru tions thus neither titrant nor sensor must be HSO4 dabru changed CALC dabru Method data Ten samples from method HAC1 are titrated Sample function No 4 using titration stand ST20 1 1D1 AA23 Number samples 10 Titration stand ST20 1 Temperature C 25 0 Temperature sensor Manual Molar mass M 60 05 Equivalent number z 1 Method data Seven samples from method HSO4 are titrated Sample function No 1 1D1 SA 666 Number samples 7 Titration stand ST20 1 Temperature C 25 0 Temperature sensor Manual Molar mass M 98 07 Equivalent number z 2 Titration stand ST20 2 is activated by the Sample Sample SS 1 function of method CALC The 15 samples are 1D1 Ca k34 titrated Number samples 15 Titration stand ST20 2 Temperature C 25 0 Temperature sensor Manual Molar mass M 110 99 Equivalent number z 2 3 46 METTLER DL77 DL70ES DL67 02 93 AUXILIARY FUNCTIONS Contents Page 4 AUXILIARY FUNCT
117. ate sensor Parameters of the mask Predispensing Titrant addition End point mode Tendency Maximum volume mL Selection menu Predispensing Predispensing shortens the time of titration Under this selection menu you can predispense a defined volume You either enter the number of mL directly or you let the titrator calculate this if you know the nominal content of the sample to be titrated 1 Select mL and enter the volume A formula such as VDISP x 1 2 can be entered instead of a number VDISP is the volume dispensed in a preceding Dispense function 2 Select nominal content see Section 8 6 3 here you must enter the following values e the metered amount in of the nominal consumption e the nominal content e the conversion constant You can select this constant from the recommendation menu If you press the HELP key selector bar is positioned on Conversion constant the titrator lists the constants with the corresponding units 3 No You need no predispensing Notes a With subsequent continuous titrant addition the titrator dispenses the volume in one step It acquires the potential values ET1 and ET2 see Section 2 3 12 1 Titra tion mode DOS b With subsequent dynamic titrant addition the titrator dispenses the volume in three steps 4 7 2 7 1 7 of the specified volume which allows optimal calculation of the increment to be added It acquires the potential values ET1 and ET2 02 93 METTLER DL77 D
118. ation of the equivalence point The evaluation of segmented curves is performed with the Standard pro cedure but the calculated data of the first derivative are used rather than the data points of the titration curve The equivalence point is thus recog nized not with the aid of the calculated first derivative but by using the calcu lated second derivative The thresh old for the equivalence point recog nition also refers to data of the second derivative The individual sections do not need to be exactly linear Decisive for an ex act determination of the equivalence point is the presence of a distinct break between the individual sections of the titration curve 8 22 METTLER DL77 DL70ES DL67 02 93 Evaluation procedures 8 4 4 Minimum maximum The result of this evaluation is the calculated minimum maximum from the measurement points of the titration The classic example of a titration curve with a minimum is the determination of surfactants using photometric indication The minimum maximum is calculated by a polynomial approximation of the titration curve in the region of the minimum maximum The equivalence point is determined directly from the data of the titration curve 1 K Waldmeier und W Rellstab Fres Z Anal Chem 264 337 1973 2 C F Tubbs Anal Chem 26 1670 1954 3 S Ebel E Glaser R Kantelberg und B Reyer Fres Z Anal Chem 312 604 1982 02 93 METTLER DL77 DL70
119. ber e g samples 9 interval 3 If e g you have entered interval 3 with 5 samples the sensor and burette tips remain in the fifth sample solution To prevent this you must add an additional Conditioning function after the loop and insert a conditioning beaker after the last sample beaker see Section 2 3 2 Example of a sample series performed with the standard method y gt gt gt gt gt 0 b Youcaninsert and mark only one beaker with conditioning solution If this does not directly follow the third sample the ST20A searches for this conditioning beaker by rotating backward It then conditions the sensor for 60 s Afterwards the sample turntable again rotates forwards to the fourth sample Caution There must be no empty positions between the titration vessel of the last titrated sample and the conditioning beaker lt lt O EE 2 28 METTLER DL77 DL70ES DL67 02 93 EDITOR Conditioning If you wish to condition the sensor on completion of a sample series always place a conditioning beaker after the last sample beaker number of samples must be divisible by the interval number The ST20A sees the following conditioning beaker 6000060606 If e g you have entered interval 3 with 5 samples you must add an additional Con ditioning function after the loop and place a conditioning beaker after the last sample beaker 660066 6 c Youhave entered 4 for
120. copy of data stored in Titrator 2 A memory copy from one titrator to the other is possible only if you interconnect the two printer cables using a null modem see Note on page 5 5 Switch on both titrators Titrator 2 Press lt Index D gt and select Memory copy In the menu Memory copy Prepare Request confirm Prepare with RUN This command causes data to be transmitted via the printer interface Titrator 1 press lt Index D gt and select Memory copy In the menu Memory copy Prepare Request confirm Request with RUN 02 93 METTLER DL77 DL70ES DL67 5 9 Memory copy DOCUMENTATION The following menu appears Overwrite memory No Yes No The procedure will be terminated Yes The user methods and installation data will be copied The display shows Data transmission active Caution All methods with the same ID will be overwritten The stored titrants will be overwritten if their names and concentrations are iden tical to those copied The stored sensors auxiliary reagents and auxiliary instruments will be overwritten if their names are identical to those copied All other resources temperature sensors auxiliary values titration stands miscellaneous will be overwritten As soon as the copying operation is at an end the main menu appears in the display indicating that data transmission will now once again be routed across the computer interface
121. cs Ri i index R3 The mean value of the third result third Calculation function for the mmol consump tion is calculated Calculation R4 x 3 C2 U C2 100 09 1000 1 Mcaco3 1000 z for the American degree of hardness ppm CaCO3 Calculation R5 x 3 C3 U C3 100 09 100 1 Mcaco3 100 z for the French degree of hardness 10 mg CaCO3 L Calculation R6 x 3 C4 U C4 56 08 100 1 Mcao 100 z for the German degree of hardness 10 mg CaO L Calculation R7 x 3 X2 C5 U gives the Mg content C5 24 31 1000 z X 3 is the mean value of the 3rd Statistics function x 2 is the mean value of the 2nd Statistics function Note You must enter numerical values for the constants of these 4 calculation functions 02 93 METTLER DL77 DL70ES DL67 8 35 Scheme for method design 8 8 Scheme for method design You can copy this scheme to set up functions with their parameters for a new method before you enter it in the Editor menu Method ID TITLE Title Number samples Molar mass M Titration stand Equivalent number z SAMPLE Entry type Temperature sensor ID1 8 36 METTLER DL77 DL70ES DL67 02 93 Scheme for method design JUULUELULLL 02 93 METTLER DL77 DL70ES DL67 Error messages and malfunctions Contents Page 9 Error messages and malfunctions oooooonnccccccnonnccccccccccconananancncnnnonan
122. ct Measurement with lon Selective Electrodes 51724646 DL7x Application Brochure 7 Incremental Techniques with lon Selective Electrodes 51724648 DL7x Application Brochure 8 Standardization of Titrants l 51724650 DL7x Application Brochure 9 Standardization of Titrants Il 51724652 DL7x Application Brochure 13 Nitrogen Determination by Kjeldahl Digestion 51724769 DL7x Application Brochure 14 Good Labatory Practice in the Titration Lab 51724908 DL7x Application Brochure 15 Guidelines for Result Check Method Validation and Instrument Certification 51724910 DL7x Application Brochure 16 Validation of Titration Methods 51724912 11 40 METTLER TOLEDO DL77 DL70ES DL67 03 2003 Index Index AE end point titration 2 55 equivalence point titration 2 42 measure function 2 20 AE set end point titration 2 55 equivalence point titration 2 40 At end point titration 2 55 equivalence point titration 2 42 measure function 2 20 temperature function 2 22 Absorption 1 11 Accessories optional accessories 11 28 standard equipment 11 27 ANALYSIS 3 3 ANALYSIS A changing to ANALYSIS B 3 44 parallel titrations 3 42 ANALYSIS B changing to ANALYSIS A 3 44 parallel titrations 3 42 Analysis parameters Installed are 1 40 3 8 Results of this sample 1 40 3 12 Applications sheets 10 15 Asterisk method identification 2 5 2 14 previously executed method 3 14 Asymmetric evaluation procedure equivalence point recognition 2 45 ev
123. cted or modified Quit the parameter mask in which you have modified a value with EXIT To continue the titration press lt index A gt The following selection menu appears Save Permanent Temporary No Permanent The modified values are saved permanently in this method Temporary The modified values are saved until the start of the next titration method No You save none of the changes After confirmation of a parameter the selection menu Method reappears Confirm Continue with RUN The representation shown before the interruption reappears on the display and at the same time the printer automatically prints out the entire method with the modified values Note In the sample determination that is interrupted the changes apply only to the functions that the titrator has not yet begun to process Exceptions are the Titration and pH mV stat functions 1st example Dispense function If you interrupt the method during this function and change the volume then continue the method the titrator dispenses the difference of the volume defined in the original method Example defined volume gt 5 mE dispensed at interruption gt 2 mL modified volume gt 7 mL Continue method the titrator dispenses gt 3mL 02 93 METTLER DL77 DL70ES DL67 3 21 Modify method ANALYSIS 2nd example Titration function If you interrupt the method during this function with an EQP titration you can modify for example
124. ction 1 1 2 Enter its concentration mol L 3 Select the sensor from the recommendation menu or enter one you have installed see Section 1 2 4 Select the unit of measurement mV or As installed As installed refers to the unit of measurement you have specified for the sensor see Section 1 2 2 5 Select the titration mode from the selection menu DOS Dispensing EQP Equivalence point titration EP End point titration LEARN EQP Learn titration equivalence point determination LEARN EP Learn titration end point determination 6 Select a condition No Yes Enter the condition 2 32 METTLER DL77 DL70ES DL67 02 93 EDITOR Titration Titration Menu tree Titrant Concentration Sensor Unit of measurement Titration mode Condition Enter c mv Condition Eeer As installed No Enter name or select from recom mendation menu Enter name or select from recom mendation menu DOS Dispensing 1 Dispensing 2 EQP Predispensing 1 Predispensing 2 Titrant addition Measure mode Threshold EQP range Maximum volume mL Termination at potential Termination after n EQPs Termination at slope Termn after nom consumption Combined termn criteria Evaluation procedure Steepest jump only Buffer potential 1 Buffer potential 2 Stop for reevaluation Yes LEARN EQP LEARN EP EP Pr
125. ction 2 64 temperature function 2 22 t min end point titration 2 55 equivalence point titration 2 42 measure function 2 21 pH mV stat function 2 64 temperature function 2 22 Table of measured values displaying 3 29 recording 2 78 3 32 Technical data auxiliary outputs 11 20 burettes 11 20 burette drive module 11 20 display 11 21 general data 11 24 keypad 11 21 measurement system 11 19 memory 11 22 propeller stirrer 11 20 Temperature auxiliary function 4 14 entering 1 12 3 7 entry through calibration 1 12 function 2 22 measuring 1 12 2 16 2 20 2 22 2 32 2 62 2 72 3 7 4 14 Temperature compensation 2 16 2 72 Temperature option accessories 11 38 inserting 11 17 setting 11 16 Temperature sensor s calibrating 4 23 Lemo cable plug 11 17 menu tree 1 16 modifying 3 7 selecting 2 16 Pt100 1 15 Pt1000 1 15 Tendency end point titration 2 57 EQP range 2 49 LEARN EP 2 61 pH mV stat function 2 63 Terminal configuration 7 9 connection 11 23 installing 1 32 key assignment 7 10 Terminate see RESET Termination after n EQP s 2 50 after nominal consumption example 8 30 after record 2 79 at combined criteria 2 51 at maximum volume 2 50 at potential 2 50 at slope 2 50 Termination criteria pH mV stat function 2 64 titration function 2 50 TFIX time increment measure mode 2 44 Threshold 2 45 02 93 METTLER DL77 DL70ES DL67 12 9 Index Threshold value evaluation procedure
126. d contain 15 25 mg water see Section 10 2 4 10 10 METTLER DL77 DL70ES DL67 02 93 Karl Fischer methods Notes c The stirring time and speed of the Stir function in method MKF1 are 10 s and 50 respectively If a longer stirring time or a higher speed are necessary you must change both parameters and save the method as a user method If methods MKF1 MKF2 and MKF3 e are entered in the method list e Auto stand is defined as the titration stand see Section 1 7 and e List once is started the titrator executes the pretitration followed by the drift determination Afterwards it will start the standby titration To titrate a sample after this terminate the standby titration with RESET For the DL67 this is not possible 10 2 5 4 Titration of series The MKF1 method also allows a sample series to be run After the start of the MKF1 method enter the number of samples Perform the individual titrations of the series in succession Notes a The time interval between the individual titrations must be as small as possible since some moisture can always diffuse into the titration vessel during this time and the drift can be compensated only by calculation Youcan notchange the solvent within a series The number of samples of a series depends on the capacity of the solvent With unproblematic samples no interference by the matrix it is approx 100 mg H20 20 mL solvent depending on the solvent us
127. d out and then expelled To stop the operation press RUN or 3 To obtain the Auxiliary functions menu again press lt index F gt 4 6 METTLER DL77 DL70ES DL67 02 93 AUXILIARY FUNCTIONS Burette 4 1 2 Rinse tip To execute this function from within any menu press the key combination lt index U gt and enter the burette drive 1 2 3 or 4 5 of the burette volume is dispensed to avoid possible diffusion effects with the solvent or crystallization in or at the tip of the dispensing tube You can repeat the operation with RUN To obtain the Auxiliary functions menu again press lt index F gt 4 1 3 Dispense With the aid of this function you can dispense a fixed volume To execute it press function number 3 If you press 1 3 in the Auxiliary functions menu you are immediately shown the selection menu 1 Modify 2 Start Modify press 1 You are shown the parameters whose value or name you can change If you press lt index F gt 1 3 1 when e g in the main menu you are shown the parameter mask immediately 1 Select the burette drive from the selection menu 2 Select the burette volume from the selection menu 3 Enter the volume mL If you confirm one of the parameters with RUN you can start dispensing Start press 2 or RUN e The titrator dispenses the specified volume You can stop dispensing with RUN or 3 To obtain the Auxiliary functions menu again press
128. dd the Stir function after the Sample function Speed e g 60 Time e g 30 The titrator stirs for 30 s at 60 maximum speed before it processes the next function It continues to stir at this speed until the next Sample or Stir function 2 18 METTLER DL77 DL70ES DL67 02 93 EDITOR Stir Example B If you would like to wait after the sample addition before starting stirring and before the titrator starts the next function set Speed 0 Time e g 30 The titrator will not stir for 30 s before processing the next function This must be a second Stir function to ensure that the titrator starts to stir Speed e g 70 Time 0 The titrator stirs at 70 maximum speed and immediately begins to process the next function see example in Section 8 7 1 02 93 METTLER DL77 DL70ES DL67 2 19 Measure EDITOR 2 3 4 Measure You can use this function to measure the potential of a solution under defined conditions The titrator acquires the measured value as raw result E see notes at the end of this section If you have selected a temperature sensor in the Sample function the temperature of the sample solution is measured automatically before the titrator executes this function If no sensor is attached parameter Manual the titrator adopts the temperature entered at the start of the method The slope of the pH electrode is then corrected for the temperature in the pH value calculation see Section 4 7 Calibrati
129. dicate the digit with the cursor with or lt prior to entering the new one 1 4 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Titrants Note b With many parameters the titrator has selection or recommendation menus in which you need only select the values or names If a parameter has one of these menus each time it is selected an arrow symbol appears at the extreme right in the middle of the display You can either accept the value or name following the parameter or in the case of Recommendation overwrite directly with a new entry or press SEL to select a new value or name from the recommendation menu that appears in the case of Selection press SEL to select a new value or name from the selection menu that appears You cannot enter the value or name yourself If only two names or values are possible for a parameter these are toggled automatically with SEL Name NaOH Concentration mol L 0 1 Titer 1 0 Burette volume 10 mL Burette drive Drive 3 Date time e g 07 06 1992 12 20 1 You can overwrite the name or press SEL to call up the recommendation menu Recommendation menu You can select a new titrant from the recommendation menu Position the selector bar on for instance HCI and confirm with RUN The recommendation menu disappears and HCI follows Name Enter the concentration mol L Enter the titer only if you know its value If you determine the titer of the ti
130. e lt gt minus key You can reinstall Pump with the command Add see Section 1 5 3 1 5 2 Modify If you select this command you are shown the parameter mask of the auxiliary instrument in which you can change the parameter values Name Pump Auxiliary output Aux 3 1 Select the name from the recommendation menu or enter the name of the device you wish to install in place of the pump 2 Select the auxiliary output from the selection menu Note If you have attached the sample changer ST20A or ST20 this unit offers you an addi tional auxiliary output called DISPENSER a relay make contact see note in Section 1 4 2 1 20 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Auxiliary instruments The auxiliary instrument with the modified parameters is installed when you quit the parameter mask with EXIT see the appropriate description at the end of Section 1 1 2 Menu tree Auxiliary instruments Pump Aux 3 gt Dispenser Aux 3 e Valve Aus 2 teo Auxiliary instrument parameters Name Pump Auxiliary output Aux 3 Enter new name or select entry from recommendation menu with SEL Select another auxiliary output with SEL 1 5 3 Add The auxiliary instrument i is deleted Selection Delete Modify Add Instrument names Pump Dispenser Valve Aux instrument Aux 1 Aux 2 Aux 3 ST20 DOSE ST20 RINSE ST20
131. e interference at his own expense 11 24 METTLER TOLEDO DL77 DL70ES DL67 03 03 Accessories 113 Accessories All the instrument s components and working aids for the titrator that form part of the standard equipment and the optional accessories are listed here Each part that is listed with an order number can be ordered from METTLER TOLEDO 09 2002 METTLER TOLEDO DL77 DL70OES DL67 11 25 Accessories Propeller stirrer Interchangeable burette incl 1 L brown glass bottle Optional accessories Burette drive Manual titration stand Optional accessories 11 26 METTLER TOLEDO DL77 DL70ES DL67 09 2002 Accessories 11 3 1 Standard equipment 1 2 3 4 5 6 7 One One One One One One One One One One One One One DL7OES one burette drive DL77 two burette driv s interchangeable burettes see Optional accessories One electrode holder manual titration stand see Optional accessories One propeller stirrer incl 2 stirring rods One built in RS option One built in temperature option One serial parallel converter Order No set of Operating Instructions DL77 DL70ES DL67in accordance with your order Tutorial RS232C Interface Description power cable set of microfuses connection cable for a printer Phillips screwdriver No 2 tube of silicone grease electrode cable SC LEMO 60 short circuit plug connection cable for a computer CD L
132. e Stir function are always adhered to within the method However you yourself are responsible for the stirring see Stir function Section 2 3 3 Enter the default speed 0 100 of the stirrer e 0 gt the stirrer is inactive e 100 gt the stirrer operates at maximum speed Select the type of conditioning for the Conditioning function Fix or Flexible pertains only to stand ST20 1 or ST20 2 Fix The ST20A ST20 conditions with the parameters designated in the Conditioning function see Section 2 3 10 Flexible The ST20A ST20 conditions every time it finds a conditioning beaker on the turntable Note The titration stand in use is always recorded 1 26 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Titration stands Menu tree Titration stands Stand 1 Aux 1 50 Stand 2 Aux 1 BQ fevers ST20 1 Aux 1 D I rn ST20 2 Aux 1 e Free stand Aux 1 B kan Auto stand Aux 1 D I EE Y Titration stand parameters Name Stand 1 Stirrer connection Aux 1 Default speed 50 Conditioning mode Fix The name cannot be changed Aux titrn stand Aux 1 Aux 2 Aux 3 Notto DL Select other conditoning mode with SEL Flexible 02 93 METTLER DL77 DL70ES DL67 1 27 Peripherals INSTALLATION 1 8 Peripherals When you select this menu you are shown the names of the units you can attach to the titrator via the RS232C or CL interface When yo
133. e that the correct sample data are transferred in each case see also next section A record or certificate must be generated by the computer The appropriate data are needed for this The titrator transfers record data to the computer results measured values etc 7 1 2 2 Administration of instrument specific data In order for you to enter sample data on the computer you must be familiar with the given basic conditions from the method method data The titrator sends the method data of a particular method to the computer on request The method data contain the parameters ofthe Sample function see Section 2 3 2 With the method data the same parameters as in the method data mask can be changed see Section 3 1 With the sample data you can enter the sample identification 2 the weight volume and the correction factor f To undertake these changes you must have loaded an appropriate program on your computer You must manage the methods stored in the titrator from the computer The titrator sends a list of its stored methods on request from the computer The titrator sends a record of the desired method with its functions and parameters on request from the computer You must manage the installation data stored in the titrator using the computer The titrator sends a record of the desired installation data on request from the computer 7 6 METTLER DL77 DL70ES DL67 02 93 Communication Titrator lt g
134. e titrator processes the Titration function The first sample has been titrated You are shown the result of this sample e Ifyou have excluded Results of this sample from appearing using Analysis parameters the titra tor will skip this information see Section 1 9 8 With RUN the sample data mask for the second sample appears Enter ID2 Weigh in the sample enter the weight or have it transferred by a balance Press RUN You are requested to insert the second sample etc No 1 2 Method ID1 CALC Ca457 ID2 B1013 3 12 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Executing a method Notes a The titrator acquires the running time for each processed method as the raw result TIME see List of designations Section 8 1 and Karl Fischer Titrations Section 10 2 7 Start of time acquisition see diagram page 3 11 The method is processed End of time acquisition The result list appears on the display single method provided that Results of this sample has been con firmed If you have specified Auto stand as the titration stand in your method the mask Current sample will not appear in the titration run This means that the next sample determination will be started without a RUN confirmation It is either not necessary to change the sample or it will be changed by a robot driven by the Sync function At the end of a titration method you are shown the results for all samples on the display o
135. econd Titration function Delete the constant with CE No Series size reached S A Statistics Ri i index R The mean value of the first result first Calculation function of the three Ca2 deter y Yes minations is calculated Se AUSTICS Statistics Ri i index R2 The mean value of the y second result second Calculation function for the mmol STATISTICS consumption is calculated Y Record If you wish to have a record of the titration curve RECORD and the table of measured values for this titration you must add the function here 8 34 METTLER DL77 DL70ES DL67 02 93 Examples of methods gt y No SAMPLE Y PUMP Y INSTRUCTION Y CALCULATION TITRATION Y Series size reached Y Yes STATISTICS Y CALCULATION Y CALCULATION CALCULATION Y CALCULATION Y RECORD Sample n 3 fixed volume 50 mL The titrator starts to stir at the default speed as soon as it has executed the function Pump Auxiliary reagent NH3 buffer pH 10 volume 5 mL Instruction The inputted request Add indicator solution appears Confirm the instruction with RUN Titration Titrant 0 1 mol L EDTA sensor DP660 550 unit of measurement mV titration mode EQP Calculation R3 Q 3 titrant consumption in mmol of the third Titration function Delete the constant with CE Statisti
136. ect this formula from the recommendation menu 90 5 g L 5 mL 100 56 11g mol 0 0981 mol L V 4 088 mL HCI are predispensed with these entries You determine the active substance of a tablet with 1 mol L NaOH titer 1 026 The amount of active substance is specified with 20 mmol tablet The sample weight is thus 1 The predispensing should be 70 of the absolute mL consumption Enter the number 70 You expect a nominal content of 20 mmol Enter the number 20 The conversion constant for this content determination is 1 70 20 mmol 1 V 400 1 1 026 mol L 13 65 mL NaOH are predispensed with these entries 02 93 METTLER DL77 DL70ES DL67 8 29 Examples of formulae Termination after nominal consumption Ifyou selectthis parameter under the Titration function with titration mode EQP you must define three values the termination volume in of the absolute nominal consumption the added volume must be e g 10 greater than the nominal consumption to the equivalence point the nominal content the conversion constant The volume that is used as a termination criterion depends on the nominal content of a substance and is calculated using the same formula as above Example You titrate the weight percent of Cl M 35 45 g mol of a salt solution 0 924 g that contains various chlorides with 0 1 mol L AgNQx titer 0 992 You would like to abort the titration when you have t
137. ed Attainment of the capacity limit is shown by a slowdown in the reaction rate 02 93 METTLER DL77 DL70ES DL67 10 11 Karl Fischer methods 10 2 6 Adapting function parameters MKF2 and MKF3 In the MKF2 drift determination and MKF3 standby titration you do not need to modify any parameter values These methods are optimum for all pyridine free titrants and solvents MKF1 and MKF4 If the titrator overtitrates in your determinations or the complete titration takes too long all you have to do is adapt the absolute end point of the first Titration function Karl Fischer reagent EPA range of the Recommended first Titration function EPA value low reaction rate 5 to 2 mV 3 mV moderate reaction rate 10 to 5 mV 5 mV e g one component reagent high reaction rate 25 to 15 mV _20 mV e g two component reagent In the optimum case approx 0 08 mL titrant are consumed in the second Titration function fine titration An acceptable range is 0 04 0 2 mL If the value lies outside this range you can set the EPA of the first Titration function higher or lower step by step The step size for the one component reagent is 2 mV for the two component reagent 5 mV e Reagent consumption of the second Titration function below 0 04 mL Danger of overtitration gt Step by step set EPA of the first Titration function lower e Reagent consumption of the second Titration function above 0 2 mL
138. ed see Section 1 2 4 Select the unit of measurement mV or As installed As installed refers to the unit of measurement you have defined for this sensor see Section 1 2 2 5 Select the titration stand from the selection menu 6 Enter the speed of the stirrer 0 100 e 0 gt stirrer is inactive e 100 gt stirrer operates at maximum speed 7 Enter the temperature C of the solution to be measured if you have not attached a temperature sensor 8 Select the temperature sensor from the selection menu If you confirm one of the parameters with RUN you can start manual titration 02 93 METTLER DL77 DL70ES DL67 4 9 Burette AUXILIARY FUNCTIONS Start press 2 or RUN e The titrator begins to dispense and increases the dispensing rate continuously The left part of the display shows the measured values mL and mV pH in the right part the following selection menu appears Interrupt Terminate Interrupt Dispensing is interrupted by pressing RUN e The potential value will still be measured e Interrupt will be replaced in the display by Continue With RUN the titrator proceeds with the lowest dispensing rate thus addition near the end point can be controlled with the RUN key Terminate The titration is terminated by pressing RUN e The left part of the display shows the results volumes in mL and mmol and the potential value in the selected unit of measurement e Pressi
139. ediately 1 Selectthe sensor from the recommendation menu or enter the one you have installed see Section 1 2 2 Select the unit of measurement mV or As installed As installed refers to the unit of measurement you have defined for this sensor see Section 1 2 2 3 Select the titration stand from the selection menu The titrator now knows which stirrer it has to control see Titration stands Section 1 7 4 Enter the speed of the stirrer 0 100 e 0 gt stirrer is inactive e 100 gt stirrer operates at maximum speed 5 Enter the temperature C of the solution to be measured if you have not attached a temperature sensor 6 Select the temperature sensor from the selection menu 7 Select record Yes or No gt Yes the measured values are recorded 8 Enter At s e g 10 A measured value will be recorded every 10 seconds If you confirm one of the parameters with RUN you can measure the potential of the solution 4 12 METTLER DL77 DL70ES DL67 02 93 AUXILIARY FUNCTIONS Sensor Start press 2 or RUN e The titrator starts to measure the potential of the solution The measured values appear on the display and are recorded To stop the measurement confirm the mask with RUN and press 3 To obtain the Auxiliary functions menu again press lt index F gt Note Ifyou continue the measurement butinthe meantime wish to process other menus quit the display with the approp
140. edispensing Titrant addition End point mode Tendency Maximum volume mL Dispensing 1 mL nom content No Dispensing 2 Potential Predispensing mL nom content No d Enter mL Positive Negative Addition mode EP Continuous Dynamic End point mode EPA EPR EPS 02 93 METTLER DL77 DL70ES DL67 2 33 Titration DOS EDITOR 2 3 12 1 DOS Dispensing In this titration mode the titrator acquires not only the raw results mL VEQ or mmol Q but also the potential values ET1 and ET2 or ET3 before and after dispensing The titrator recog nizes four different dispensing modes Selection menu Dose 1 You can dispense a specified volume You either enter the number of mL directly or you let the titrator calculate this if you know the nominal content of the sample to be titrated 1 Select mL and enter the volume Aformula suchas VDISP 1 2 canbe entered instead of anumber VDISP is the volume dispensed in a preceding Dispense function 2 Select nominal content see Section 8 6 3 you must enter the following values here e the metered amount in of the nominal consumption e the nominal content e the conversion constant You can select this constant from the recommendation menu e the maximum volume mL It is intended as a safeguard If for instance the wrong constant has been selected excess titrant is not dis pensed needlessly If you p
141. edlessly as the titration is always aborted Select Termination at potential The titrator terminates the titration at the specified potential No Yes Enter the potential mV pH A potential stored as an auxiliary value Hj or a formula can be entered instead of a number see Auxiliary values Section 1 6 and Auxiliary value function Section 2 3 15 Select Termination after n EQPs The titrator terminates the titration after a certain number of equivalence points n have been found No Yes Enter n Select Termination at slope The titrator terminates the titration when the slope of the titration curve falls below a specified value The slope of the curve must exceed this absolute value once then fall below it twice to lead to termination No Yes Enter the slope mV pH mL Select Termination after nominal consumption The titrator terminates the titration when the added volume is e g 10 above the nominal consumption up to the equivalence point see Section 8 6 3 No Yes Enter the termination volume in of the nominal consumption Enter the nominal content Enter the conversion constant or select it from the recommendation menu Ifyou pressthe HELP key selector baris positioned on Conversion constant the titra tor lists the constants with the corresponding units 2 50 METTLER DL77 DL70ES DL67 02 93 EDITOR Titration EQP Evaluation criteria Select Combined
142. ee determinations of the chloride content is calculated 02 93 METTLER DL77 DL70ES DL67 8 33 Examples of methods 8 7 3 If your sample contains substances whose determination requires a new sample each time compile a method that comprises submethods in other words a method with two or more Sample functions Single determination of Ca2 content the sum of Ca2 and Mg in drinking water with the calculation ofthe American French and German degree of hardness and the calculation ofthe Mg2 content TITLE AY y SAMPLE Y TITRATION Y STIR Y INSTRUCTION Y TITRATION Y CALCULATION Y CALCULATION Sample n 3 fixed volume 50 mL M 40 08 z 1 The titrator begins to stir as soon as it has executed this func tion Titration Titrant 1 0 mol L NaOH sensor DG111 SC unit of measurement pH titration mode DOS Titration to pH 12 Stir Speed 80 time 120 s The titrator should stir for 2 min to ensure complete preci pitation of the Mg OH o Instruction The inputted request Add indicator solution appears Confirm the instruction with RUN Titration Titrant 0 1 mol L EDTA sensor DP660 550 unit of measurement mV titration mode EQP Calculation R Q 2 C U C M 1000 z unit mg L Calculation R2 Q 2 titrant consumption in mmol of the s
143. ee Auxiliary values Section 1 6 and Auxiliary value function Section 2 3 15 Select Buffer potential 2 No Yes Enter buffer potential 2 mV pH see buffer potential 1 Caution If you have selected P1 and or P2 the titrator checks all termination criteria except maximum volume only when the appropriate buffer potentials P1 and or P2 have been reached With the selection of both buffer potentials you also define the tendency from P1 to P2 and the order If the titrator first finds P2 it will no longer search for P1 02 93 METTLER DL77 DL70ES DL67 2 51 Titration EQP Evaluation criteria EDITOR Select Stop for reevaluation The Titration function is interrupted during the run as soon as termination criteria and the specified condition are fulfilled This enables you to modify parameters for the equivalence point recognition threshold value EQP range and for the evaluation buffer potentials P1 and P2 All data will be reevaluated with the modified parameters see Section 3 5 No Yes Enter a condition for example neq 0 no equivalence point found see Functions with a condition Section 8 3 2 52 METTLER DL77 DL70ES DL67 02 93 EDITOR Titration EP Predispensing 2 3 12 3 EP End point titration With this titration mode you titrate to a specified value of the selected unit of measurement Caution Before an end point titration you should calibrate the appropri
144. ee Section 3 1 1 Select the first line of this mask sample 1 of the first Sample function The sample data mask appears in which you enter these parameters Sample data Sample No 1 1 ID2 G 324 Weight m g 0 1456 Minimum g 0 Maximum g 0 2 Correction factor f 1 0 If you confirm a parameter with RUN the mask for the second sample No 1 2 appears then that of the third sample If no method is running either press RUN The selection menu Method appears or press lt index A gt The method list appears For arunning method press lt index T gt The function the titrator is currently processing appears The procedure for entering sample data from other methods during a titration is described in Section 3 13 3 3 02 93 METTLER DL77 DL70ES DL67 3 23 Sample data ANALYSIS The following example shows the sequence of a pH stating in which the titrator should start the stating immediately after sample addition meaning thatthe sample data are entered later y The titrator processes the Sample function Sample data Sample No 1 1 Confirm the sampie data mask with RUN without ID2 entering the weight Weight m g 0 0 Minimum g 0 0 Maximum g 0 2 Correction factor f 1 0 c Add the sample and confirm immediately with urrent sample RUN No 1 1 Method ID
145. electronically protected against overload 11 2 3 Burette drive module With DC motor Number burettes Maximum 4 Resolution 1 5000 of burette volume 0 2 1 2 and 4 uL Maximum permissible error lt 0 3 relative to the respective burette volume of 5 10 and 20 mL Filling time 20s Delivery time Minimum 20 s 11 2 4 Interchangeable burettes Number burettes Maximum 4 Volumes 1 5 10 and 20 mL Materials in contact with titrant Fluoroplastic borosilicate glass ceramics 11 2 5 Propeller stirrer Maximum speed No load operation around 4000 min In water around 3500 min Power consumption ere lt 4 W 1 2Watl2V typical 11 2 6 Keypad Material Polyester splashpr oof 11 2 7 Display Liquid cristal display with graphics 6 lines 36 characters per line capability 64 x 256 pixels backlit Languages English German French Spanish Italian 11 20 METTLER TOLEDO DL77 DL70ES DL67 03 03 Technical data 11 2 8 Titration modes Equivalence point titration End point titration Learn titration pH stating Karl Fischer titration 11 2 9 Method concept Dynamic or incremental titrant addition Equilibrium controlled or time controlled measured value acquisition Evaluation models for symmetric asymmetric and segmented titra tion curves determination of the minimum or maximum of a titration curve determination of the half neutralization value Continuous or incremental titrant addition to absolute or relative
146. em titrator lt gt computer The functions available for the communication and the prerequisites for data interchange between the titrator and computer are described in the Operating Instructions enclosed with the RS option 7 1 2 Introduction Computers are finding increasing use in labs in the chemical industry In association with an analytical instrument they undertake the following tasks e LIMS tasks Laboratory Information Management System e Administration of instrument specific data e Backup of instrument specific data e Control of sequences automation 7 1 2 1 LIMS tasks At present there exist neither standards directions nor rules that define the tasks of a LIMS It has become apparent however that the following tasks can be handled by most LIMSs e Generation and administration of work sheets e Sample observation from sampling up to archiving of the data obtained e Sample preparation e g weighing e Data acquisition online or via a keyboard e Archiving and administration of results and measured values e Record generation 03 99 METTLER DL77 DL70ES DL67 7 5 Communication Titrator lt gt Computer Important for the titrator are sample preparation and data acquisition Sample data such as weight and identification must be prepared in the computer and stored in a file in a particular format The titrator accepts the sample data at a suitable time automatically The computer must ensur
147. ence of the sample beakers if you execute these commands 3 36 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Method list 3 13 3 Processing the method list If you confirm one of the methods with RUN you can start e g activate it with the selection menu below Start Single method List once List continuous 3 13 3 1 Single method Select Single method if you e have stored only one method or e wish to perform only that method selected among several stored methods The executed method is marked with an asterisk As soon as you start another method all data from the executed method will be deleted If you select the executed method and confirm Start the titrator will reload this method see Restarting a previously executed method Section 3 1 4 3 13 3 2 List once Select List once if you wish to perform several stored methods in succession Here it is immaterial which method you have selected The titrator begins with the method at the start of the method list e The method currently running is marked in the method list with gt e Atthe end ofa processed list only the final method marked with an asterisk will be saved It will be deleted once you start a newly entered list Notes a If you are working at titration stand 1 2 or a free stand the sample data mask appears only if you have not yet entered the weight volume of the samples You must confirm the mask Current sample for every sample b If
148. ency on the METTLER service Note Before you call METTLER service please print out the system information which provides details of the equipment configuration of the titrator and inform the service of these press _T Fault Possible cause The information will be printed out Corrective measure No display on titrator Instrument not connected to power Fuse defective Plug in instrument Check fuse and replace if necessary A few dots of the display are missing Call METTLER service The display does not match the key pressed Call METTLER service Stirrer will not stir Sensors can block stirrer at the titration stand Check placement of sensors Units attached to the outputs are inoperative Auxiliary instrument defective Check instrument at another auxiliary output Call METTLER service Transfer error to attached peripheral Peripheral faulty Check attached units for proper functioning Unit printer balance terminal at serial inter face does not respond Unit not switched on Wrong installation data Wrong configuration switch settings Switch on unit Installation data and configuration must match see Section 1 8 02 93 METTLER DL77 DL70ES DL67 9 5 Error messages and malfunctions Fault Possible cause Corrective measure Burette does not move Check burette drive to zero position when at another
149. end point Water deter mination gt 2 mg H O sample Flexible sequence through a combination of discrete substages function to a method A particular substage can occur more than once and each is processed in succession Functions Conditional functions Result calculation Statistical evaluation Additional functions Title Sample Stir Measure Temperatur e Instr uction Dispense Pump Rinse Conditioning Auxiliar y instrument Titration pH mV stat Calculation Auxiliar y value Titer Calibration Statistics Recor d Sync Execution of the functions only if condition is met Comprehensive calculation of results in the desired unit from all avail able experimental results intermediate results and calculated results Determination of mean value standard deviation and relative stan dard deviation outlier test following Grubbs Burette rinse bur ette dispense fixed volume or continuously manual titration Stirrer stirring and dissolution Sensor mV pH measurement with r ecord of measur ed values Temperature C F K measurement with record of measured values Sample Changer Auxiliary instrument operation of an auxiliary device fixed time or manual Calculations additional calculations of results at the end of every sample determination Records additional record at the end of every sample determination Calibration of the temperature sensors Offset adjustment of the sensor inputs
150. epeated Example In the Stir function the solution is stirred for the specified time regard less of the time stirred before the interruption 02 93 METTLER DL77 DL70ES DL67 3 17 Interrupt method ANALYSIS In most cases you interrupt the determination to modify parameter values of the current method see Section 3 6 The titrator itself interrupts a titration immediately in the following situations 1 After the Titration mode LEARN EQP or LEARN EP if it has not found an equivalence or end point see also Sections 2 3 12 4 5 Confirm the error message with RUN The selection menu reappears see previous page If you wish the titrator to perform the remaining functions of the method select Continue The titration resumes and the representation shown before the interruption reappears on the display If you wish to terminate the method press RESET see Section 3 2 2 During a Titration function if the condition for the specified parameter Stop for reevalu ation is satisfied see next section 3 18 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Reevaluation 3 5 Reevaluation You can reevaluate the titration curve in an equivalence point determination EQP by modifying the titration parameters This is possible only while the Titration function is active Either e you interrupt the current Titration function after a possible predispensing has been completed the selection menu Method appears i
151. er by the formula t X or Xi 02 93 METTLER DL77 DL70ES DL67 2 71 Calibration EDITOR 2 3 17 Calibration You use this function to calibrate an electrode its zero point and its slope are calculated You determine the buffers to be used for the calibration of the sensor The potential of the buffer solutions is determined with the aid of the Measure function see example at the end of the section Notes a Since the slope of an electrode is temperature dependent it is important to specify the temperature at which the calibration is performed e Before the start of the Measure function the temperature of the buffer solution is determined automatically if a temperature sensor is attached Otherwise the temperature entered at the start of the calibration method will be adopted see Sample function Section 2 3 2 If you measure the pH value of a solution at a different temperature at a later date the slope of the sensor is temperature compensated by the titrator Thecalibration data zero point slope and calibration temperature are transferred automatically with the date to the installation data of the sensor see Section 1 2 2 Depending on the number of buffers measured the titrator performs the following calibration e With one buffer sample n 1 it calculates the zero point of the sensor The slope remains unchanged e With several samples n gt 1 it calculates the zero point and the slope
152. eries of samples with the same content n gt 1 in the Sample function The statistics calculation then discards the result of the first sample b If your method has several Titration functions you can select LEARN EQP or LEARN EP for each titration mode 02 93 METTLER DL77 DL70ES DL67 2 61 pH mV stat EDITOR 2 3 13 pH mV stat You use this function to perform a pH stating You determine the parameters which assure the constancy of a potential value which lead to the termination of the pH stating and which are used in the evaluation The titrator acquires the following raw results see Measure function Section 2 3 4 a The titrant consumption in mL VTOT or mmol QTOT up to termination of the pH stating b The titrant consumption in mL VT1 VT2 or mmol QT1 QT2 up to the attainment of the specified time limits t1 and t2 c The mean consumption in mL min VSTAT or mmol min QSTAT within the time limits t1 and t2 see Section 8 1 d Thecorrelation coefficient CSTAT this results from the calculation of the mean consumption through linear regression see Section 8 1 List of designations If you have selected a temperature sensor in the Sample function the temperature of the sample solution is measured automatically before the titrator executes this function If no sensor is attached parameter Manual the titrator adopts the temperature entered at the start of the method The slope of the pH electrode is then
153. ers you should enter for the titration mode EQP select LEARN EQP Titration function selection of the parameters example Titrant AgNO3 Concentration mol L 0 01 Sensor DM140 SC Unit of meas urement As installed Titration mode LEARN EQP Condition No When you start the method the titrator executes one function after the other As soon as it has completed the Titration function it calculates the parameters for the titration mode EQP stores them and sends the data to the printer While the parameters of the Titration function are being printed the titrator executes the remaining functions Printout of a learned EQP titration LEARN TITRATION Method le2 Version 30 Sep 1992 10 14 Titration 1 NET ch ef creses A A e EE E AgNO3 Concentration mol L ooooooooo o ooo 0 05 SENSO msi a Ses SE SE A ee ee eo DM141 SC Unit Of MEAS mis EE ENE ow Wile heh war As installed Titration Mode wine ida bale wow aie Game de EQP PYECISPENSANG L mice wipe e wee ewe io eels ee mL Volum ME ta dale Se ete nuti EES Od PYECISPENSANG ENN ewe elo we EM wee To potential Potential MV PH ssal ais se e gg 16 5 Titrant addition emi NN i wees DYN ABMSSU Tock eis as bee Seba 8 0 Limits AV eseu ENER ar Relative AV min SdosVol ooooo 05 AV max buVol 4 0 Meas re Mode es EE EE as e Gow ee e EQU AE MV mesero ic Re cae eee ee E 3 At Sted eke tees aioe bg eked tied s 2
154. ess than AT At 0 01 C s during the period At 2 s if the temperature is to be acquired as a measured value This occurs within a defined time interval t min and t max 5 Select t min from the following menu a Fix Enter t min s e g 3 Instead of a fixed time you can select a condition The measured value must be greater or less than a specified set value b T gt greater than set value Enter set value C F K c T lt less than set value Enter set value C F K 6 Enter t max s e g 30 Note If you select 5b 5c the titrator will start the next function only when the measured temperature is greater less than the set value and the drift condition is satisfied but at the latest after t max 7 Select a condition No Yes Enter condition 2 22 METTLER DL77 DL70ES DL67 02 93 EDITOR Instruction 2 3 6 Instruction This function allows you to intervene manually in the sequence of the titration method in other words the method is interrupted The entered text appears at the desired position during the current method in the display and is supported audibly The method does not continue until you confirm the instruction with RUN 1 Enter the instruction 2 Select a condition No Yes Enter the condition 02 93 METTLER DL77 DL70ES DL67 2 23 Dispense EDITOR 2 3 7 Dispense With the aid of this function you dispense a specified volume of titrant with a ME
155. essel for firm seating in the titration head If it falls off you could injure yourself if working with toxic titrants and solvents or ES 2 strong acids or bases Risk of corrosion When using chemicals and solvents comply with the instructions of the producer and the general lab safety rules Additional safety precautions for Karl Fischer titrations are described in Section 10 2 Measures for operational safety Check the set operating voltage before you switch on the titrator see Section 11 1 5 The instrument will be damaged if the operating voltage does not match the line voltage Use only fuses of the specified type if you need to change them Have the instrument serviced only by METTLER TOLEDO Service Always wipe off splashed liquids immediately The instrument is not water proof Exclude the following environmental influences e powerful vibrations e direct sunlight e atmospheric humidity greater than 80 e temperatures below 5 C and above 40 C e powerful electric or magnetic fields Caution 11 97 METTLER DL77 DL70ES DL67 1 Introduction The DL77 DL70 ES and DL67 METTLER titrators are microprocessor controlled analytical instruments that provide accurate and reproducible results thanks to their built in intelligence With these titrators you can perform end point equivalence point and pH stat titrations measure pH mV and temperature and determine TAN TBN and p m values With the
156. essories supplied with the instruments Mettler Toledo GmbH 1993 1995 1996 1997 1998 1999 2002 2003 2004 ME 705094E Printed in Switzerland 0404 2 12 Mettler Toledo GmbH Analytical Sonnenbergstrasse 74 CH 8603 Schwerzenbach Tel 41 1 806 77 11 Fax 41 1 806 73 50 Internet http www mt com
157. ethod once more see above you are shown the next incorrect function etc b Ifyou have entered a method identification under the Title function that already exists the selection menu ID exists appears Overwrite ID Confirm with RUN The new or modified method is saved that with the same identification is deleted Modify ID Confirm with RUN You are shown alist of the method functions and can modify the method ID using the Title function Then you can save the method see above If you are not shown any error message when you confirm Save with Yes the list of user methods with the stored method appears in the display Note If you press a key combination lt index letter gt in the function list to quit the Editor menu the selection menu Save always appears first 02 93 METTLER DL77 DL70ES DL67 2 11 Menu tree EDITOR EDITOR Menu tree Method ID METTLER methods User methods New method Method ID METTLER methods User methods Method ID GR41 M001 Acid content KM59 ol stat of Gerusil M002 Titer of NaOH 0 1 mol L UB33 H3PO in Cola drinks etc etc l yy Method Method Method Print Print Print Delete Modify Delete Modify Modify y Modify method Modify method Modify method New method Title GR41 Title M001 Title KM59 Title Sample Sam
158. ex P gt causes a form feed Select the paper format from the selection menu e DIN A4 width 21 cm length 29 7 cm e 81 2 11 width 81 2 inches length 11 inches e 81 2 12 width 81 2 inches length 12 inches Select the automatic form feed with SEL Yes or No e Yes The printer inserts a form feed at the end of each document e No Each document is separated from the next by a space of 2 lines Select the frame lines for the record from the selection menu e Straight The printout will be framed with continuous lines e Dotted The printout will be framed with dashed lines the printing proceeds at twice the previous rate e None no frame Printing proceeds fastest with this parameter Select the baud rate from the selection menu e 1200 e 2400 e 4800 e 9600 Select the parity from the selection menu e Even e Odd e None Select the data bits with SEL 8 bits or 7 bits 10 Select the stop bits with SEL 1 stop bit or 2 stop bits Attach the printer to the data output with the designation Printer The connection cable is part of the standard equipment of the titrator see Section 11 3 Accessories 02 93 METTLER DL77 DL70ES DL67 1 29 Peripherals INSTALLATION 1 8 2 Balance If you wish to attach a balance you have to install it Select Balance and you are shown the following parameter Transmission mode Select from the selection menu e Unidirectional e Bidirect
159. f you merely wish to copy the Measure function in order to paste it in elsewhere position the selector bar on this command and confirm with RUN The Measure function remains at this location and is also stored in a buffer memory so that it can be pasted in elsewhere The function remains stored until you either cut or modify another function 2 2 3 Paste You now wish to paste in the cut or copied Measure function before the Stir function Position the selector bar on the Stir function and press the lt gt equals key 2 8 METTLER DL77 DL70ES DL67 02 93 EDITOR Select functions The Measure function now follows the Dispense function Title Sample Dispense Measure Stir Titration Calculation Record You can paste a function only if you have first cut or copied it Since the Measure function is still stored you can also paste it in ahead of the Titration function for instance 2 2 4 Add You would like to add the Auxiliary value function to the method in this case before the Record function Position the selector bar on the Record function and press the lt gt plus key You arenow shown a list of all functions except Title function Position the selector bar on the Auxiliary value function and confirm with RUN The Auxiliary value function now follows the Calculation function Title Sample Dispense Measure Star Titration Calculation Auxiliary value Record Note If
160. g time is displayed 3 Rinse Should electrodes and burette tips be rinsed after conditioning No Yes Select the auxiliary reagent from the recommendation menu or enter one you have installed see Section 1 3 Enter the volume mL Caution If you select this parameter the beaker can overflow after some time if you have inserted only one conditioning beaker in the turntable but condition the sensor after every sample 4 Select a condition No Yes Enter the condition Notes When installing the sample changer titration stand you can select Fix or Flexible as condition ing mode see Section 1 7 Fix The ST20A ST20 conditions with the parameters specified in this function see below Note 2 Flexible The ST20A ST20 conditions whenever it finds a conditioning beaker see below Note 3 When titrating in non aqueous media for example this mode allows you to place additional conditioning beakers where ever necessary during the method run 1 Conditioning samples are marked on the sample turntable by red plugs 02 93 METTLER DL77 DL70ES DL67 2 27 Conditioning EDITOR 2 You have selected Fix as conditioning mode a You can follow the above example and insert and mark a beaker with the conditioning solution after every third sample 0000000 6 If you wish to condition the sensor on completion of asample series you must ensure that the number of samples can be divided by the interval num
161. gish approach to end point End point of the first Titrati on function too low Slow water loss from the sample Reaction of the sample with KF reagent side reaction Set end point 2 5 mV higher see Section 10 2 6 Pulverize sample or perform external extraction Direct titration not possible Infinite pretitration Method MKF2 or MKF3 selected for the pretitration Select method MKF 1 02 93 METTLER DL77 DL70ES DL67 10 13 Karl Fischer methods Problems Possible cause Measures Initial weight too low Sample should contain at least 15 mg water Drift changes drastically Perform drift determination Poor reproducibility more frequently Long wait times between the titrations without standby titration First value of a series Series after a standby Start a drift determination always too low or too titration before a series high Explanation The MKF1 and MKF3 methods do not have the same Titration functions KF titration dynamic EP standby titration mV stat The end point level is thus not identical As a consequence after a standby titration the first value of a series can differ 10 2 9 A few examples of results Titration with one component reagent EPA of the first Titration function 5 mV Drift 38 ug min Titer determination with sodium tartrate D em X 1 07233 RSD 0 4 Titration 10 uL water n 4 X 9 97 mg RSD 0 4 Titration 0 03 g cognac n 6 X
162. gt The method list appears During a current method press lt index T gt The function the titrator is currently processing appears Note In order to modify the method data from other methods while running a method press lt index A gt The method list appears Confirm the desired method with RUN and select Method data in the selection menu 3 8 1 Record data You can check all entered sample data together with the most important associated method data by requesting a record Confirm Record data with RUN All sample data stored in the memory are printed out 02 93 METTLER DL77 DL70ES DL67 3 27 Display ANALYSIS 3 9 Display This menu is used for the following tasks e to select the parameters titration curve table of measured values or measured values that the titrator can represent on the display if it executes functions or auxiliary functions that generate the necessary experimental data e to again follow the titration progress on the display if you have previously faded it out e to view the titration curve or table of measured values of the last sample once again at the end of its determination e to view the results that the titrator has generated during a titration method up to this time or to fade in the list of all results again at the end of the method Display Representation Titration curve Curve type E V curve Representation Curve type Titration curve E
163. he identi fication switch of the ST20A see the ST20A installation instructions Two sample changers can be used for e parallel titrations of a sample series on each of the sample changers Analysis A and Analysis B see Section 3 14 successive determinations of sample series with a total of 40 samples unattended The conditions for this are described in Section 3 15 Connection scheme for 2 sample changers Duplex cable ST20A to ST20 ST20A Connection cable ST20 ST20A Titrator ST20 or ST20A 02 93 METTLER DL77 DL70ES DL67 1 35 Miscellaneous INSTALLATION 1 9 Miscellaneous When you select this menu you are shown the various submenus and parameters whose values or names you can or must select or specify Date time format Enter date time Language Record header Titrator ID Routine level Audio signal Analysis parameters 1 9 1 Date time format You are offered several ways to write the date and time If you wish to modify the existing formats select this parameter and you are shown the following parameters Date format Select the new format from the selection menu Time format Select the other format with SEL Note If you modify the format after one month for example the new format will be adopted for all previously stored data 1 9 2 Enter date time In the course of time you may possibly need to reset the dates When you select this line you are shown the foll
164. he mask of the selection menu disappears the DG111 SC sensor is deleted Note You can also delete a sensor directly from the list by pressing the lt gt minus key You can reinstall the DG111 SC with the Add command see Section 1 2 3 1 2 2 Modify If you select this command you are shown the parameter mask of the sensor in which you can change the parameter values Name DG111 SC Unit of measurement pH Sensor input Sensor 1 Zero point Unit 7 0 Slope mV Unit 59 16 Temperature C 250 Date time e g 02 06 1992 10 15 1 Selectthe sensor name from the recommendation menu or enter the one you wish to install in place of the DG111 SC sensor 2 Select the unit of measurement suitable for the sensor from the selection menu Within a method you can later again choose between the selected unit of measurement and mV in the functions Measure Titration and pH mV stat see Section 2 3 4 12 13 mV Either there is no other unit of measurement suitable for the sensor or you require only mV If you select the unit mv for a sensor the calibration parameters zero point slope and temperature are ignored by the titrator pH After you select pH you then enterthe calibration parameters for a pH electrode or you let the titrator do it see notes a and b on page 1 12 pM M represents any cation After you select pm you then enter the calibration parameters for a pM electrode or you let the titrator do it see no
165. he sample and informs the titrator of this so that it can continue the analysis Allow titrator to continue To allow several titrators to be attached to alow end computer the titrator can be so configured that it will transmit data to the computer only when this sends the appropriate inquiry polling 7 8 METTLER DL77 DL70ES DL67 02 93 Configuration of the terminal 7 2 Configuration of the terminal DEC VT340 You have attached the terminal to the titrator and have installed it see Section 1 8 3 To configure it Switch off the titrator switch on the terminal and wait until the message VT340 OK is displayed Press the Set Up key the SET UP DIRECTORY is displayed If you have already configured the terminal for other connections first select Recall Factory Default Settings to reactivate the default configuration parameters If you have not used the terminal before you can modify the default parameters imme diatly Select General Set Up and modify the following parameter Terminal mode VT300 8bit Select Display Set Up and modify the following parameters Scrolling jump Status Display host writable Select Communications Set Up and modify the following parameters Transmit Speed 9600 Receive XOFF Point 512 Character Format 8 bits even parity These parameters must correspond to the entered instal lation data Select Keyboard Set Up and modify the following parameter Keypad mode numeric if the key
166. hods can be entered in the method list of Analysis menu A as well as in that of Analysis menu B DL7OES A maximum of 10 methods can be entered in the method list of the Analysis menu DL67 One method can be entered 8 5 4 Maximum number of equivalence points per method The titrator can determine maximum 16 equivalence points per method titration mode EQP distributed among one or several Titration functions If the method has for example several Sample functions a maximum of 16 equivalence points will be determined distributed among these Sample functions Should more than 16 equivalence points be present the rest will not be determined The method however will be continued 8 5 5 Maximum number of measurement points per Titration function The titrator can store 300 measurement points per Titration function it then terminates the function 8 5 6 Maximum number of results per method The titrator can store 180 results per method it then terminates the method Example If you titrate 30 samples with a method the titrator can store 6 results for each individual sample 8 5 7 How long does the titrator store data 1 Measured values of the Titration or pH mV stat function The titrator stores the measured values until the next Titration or pH mV stat function 2 Raw results The titrator stores all raw results up to the titration of the next sample within a loop If the method has several Sample functions the raw result
167. i test e Dati del servizio clientela esigenze dei clienti e Rapporti di revisione e Codice originale La Mettler Toledo GmbH Analytical rimarr in possesso di tutti i documenti e di tutte le loro copie e contrarr un accordo di discrezione con coloro che desiderassero visionare tali documenti alar bo UP fof Schwerzenbach Dr Bernhard Grob Dr Urs Spitz Marzo 1999 General Manager Manager Business Area Business Unit Analytical Titration 12 18 METTLER DL77 DL70ES DL67 03 99 Modello di ciclo vita di un prodotto dee Studio del progetto Redlizzczione del progetto y Inizio del progetto Fase Conoscenze di base Specifiche del prodotto Linee direttive Sistema di qualita Documentazione del progetto Sistema del progetto Rapporto di revisione Fase Fattibilit Specifiche del software Piano del test Rapporto di revisione Fase Conferma Rapporto di revisione Fose Fine del progetto Disponibilit servizio dientela CRIS Esigenze da dienti Utilizzozione y 03 99 METTLER DL77 DL70ES DL67 12 19 To protect your METTLER TOLEDO product s future METTLER TOLEDO Service assures the quality measuring accuracy and preservation of value of all METTLER TOLEDO products for years to come Please send for full details about our attractive terms of service Thank you Printed on 100 chlorine free paper for the sake of our environment P705094 of the acc
168. ical evaluation The outlier test is not performed until the number of samples n is greater than 3 n gt 3 02 93 METTLER DL77 DL70ES DL67 2 75 Statistics EDITOR Example of a titration method for a known acid mixture 2 equivalence points where the percent content of both components with corresponding standard deviation is required as result TITLE gt y SAMPLE y TITRATION y CALCULATION y CALCULATION y No WA Series size reached d Yes STATISTICS Y STATISTICS Y RECORD Sample The number of samples is n 5 Thetitrator begins to stir atthe default speed as soon as it has executed this function Titration The titrator acquires the raw results Q1 and Q2 Calculation You define the result R R1 for the evaluation of the first equivalence point R Q1 C1 m see Calculation function Section 2 3 14 Calculation You define the result R2 for the evaluation of the second equivalence point R2 Q2 C2 m Statistics The entry Ri i index must be the same as in the Calculation function In the first Statistics function R in the second Statistics function R2 The titrator assigns the 5 results R or R2 of the 5 samples to the statistics functions and thus calculates the mean values x and the corresponding standard deviations 2 76 METTLER DL77 DL70ES
169. il you switch on the printer and starts to transfer its data e the computer sends an appropriate error message Short form method Sample data Would you like a record of the method in short form Select Yes with SEL Would you like a record of all sample data ID1 ID2 molar mass equivalent number weight volume correction factor of the completed titration method Select Yes with SEL 02 93 METTLER DL77 DL70ES DL67 2 77 Record EDITOR Raw results last sample Would you like a record of all raw results such as VEQ or VDISP of the last sample Select Yes with SEL 5 Results last sample Would you like a record of all results of the last sample Select Yes with SEL 6 All results Would you like a record of all results ofthe completed titration method Select Yes with SEL 7 Table of measured values Would you like a record of the table of measured values of the last sample Select Yes with SEL 8 E V curve Would you like a record ofthetitration curve potential vs volume of the last sample Select Yes with SEL 9 AE AV V curve Would you like a record of the 1st derivative of the titration curve potential vs volume ofthe last sample The ordinate scale is linear Select Yes with SEL 10 log AE AV V curve Would you like a record of the 1st derivative of the titration curve potential vs volume of the last sample The ordinate scale is logarithmic Select Yes with SE
170. ion 2 36 8 20 formulae for limiting 8 31 maximum number method 8 25 Equivalence point recognition EQP titration 2 45 LEARN EQP 2 59 Equivalence point titration menu tree 2 37 titration mode 2 36 Equivalent number calculation function 2 68 entering 2 16 modifying 3 7 Error messages data transfer 5 5 learn titration 3 18 memory copy 5 9 5 10 remote control 7 3 with reference to Section 9 1 9 3 ET1 2 34 2 35 2 39 2 53 8 4 ET2 2 34 2 39 2 53 8 4 ET3 2 35 2 39 8 4 02 93 METTLER DL77 DL70ES DL67 12 3 Index Evaluation criteria pH mV stat function 2 64 titration function 2 51 Evaluation procedure explanation 8 20 titration function 2 45 2 51 EXIT key 1 6 2 10 2 11 3 8 3 10 3 16 Expert 6 3 f correction factor 3 7 8 3 Fix conditioning mode 2 27 Fixed volume sample data mask 3 10 sample function 2 15 Flexible conditioning mode 2 27 Formulae auxiliary value function 2 70 calculation function 2 66 calculations menu 3 34 constants 8 27 for limiting the equivalence point 8 31 nominal consumption 8 30 nominal content 8 28 results 8 26 titer function 2 71 Form feed 1 29 Frame lines printout 1 29 Free stand 1 25 Function s adding 2 9 copying 2 8 cutting 2 8 deleting 2 8 explanation 2 3 list 2 3 maximum number method 8 24 modifying 2 10 2 14 pasting 2 8 selecting 2 8 Function number 4 3 Functions with a condition examples 2 79 8 18 8 19 explanation 8 16 Fuse replacement 11 14 H
171. ion 3 1 or measured automatically if you have attached and installed a temperature sensor see Sections 1 3 2 3 2 and 2 3 17 7 Youcanneither delete nor overwrite the date It refers to the calibration of the sensor using the method function Calibration and is entered here together with the time automatically see Calibration function Section 2 3 17 Notes a The calibration parameter values of the titrator installed in the factory are theoretical values for a new sensor You have to perform a calibration of your sensor if you wish to determine accurate values see Calibration function Section 2 3 17 b When a pH pM or pX sensor is calibrated the calibration parameters zero point slope temperature are entered here automatically c As soon as you change a sensor parameter the date and time are deleted Caution Donottransfer the calibration data obtained for glass electrodes attached to sensor input 1 or for the temperature option sensor input to the electrodes you attach to sensor input 2 or the sensor input of the RS option Recalibrate these sensors to obtain correct values The sensor with the modified parameters is installed when you quit the parameter mask with EXIT see the appropriate description at the end of Section 1 1 2 1 12 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Sensors Menu tree Sensors Selection rio DG111 SC pH Sensor
172. ional e Not installed Unidirectional In the case of the weight request the balance transfers the current weight value without stability detector continuously and this is displayed by the titrator You must confirm this display with RUN for the value to be accepted Titrator Data to titrator Balance Configuration Send Cont Bidirectional Inthe case of the weight request the balance transfers the current weight value when the titrator requests it and this value is then displayed by the titrator with stability detector On AM PM and AT balances the weight limits are superimposed on the balance display see Section 3 1 1 The titrator accepts the weight value when you press either the RUN or the transfer key of the balance Command from titrator Titrator p a Data to Titrator Balance Configuration Send Stable Send on Transfer Note a You can attach every METTLER balance fitted with a CL interface The data output of the attached balance must be configured as follows e Baud rate e Parity e Operating mode 2400 even Send Cont for unidirectional transmission mode Send Stable Send on Transfer for bidirectional transmission mode 1 30 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Peripherals Notes b With AT balances the following settings are important e Unit Prt on print transfer com
173. ip 70 cm 25687 J Suction tube 1 83 cm 25688 a Gasket 1 min order quantity 5 23981 Cy for 1 L brown glass bottle a Tip holder 1 for burette tip 23960 Stopper ST 14 5 1 min order quantity 5 23646 Set of labels 1 51107506 09 2002 METTLER TOLEDO DL77 DL70ES DL67 11 29 Accessories Order No Z Dispensing tube with siphon tip 100 cm 25961 i Drying tubewith cover 23961 E Drying tube holder 23915 lt gt 2 U EN Molecular sieve 250 g 71478 av Gas inlet 23721 Siphon tip set set of 5 23240 Adapter for bottles by Merck DE 23774 Fisher US 23787 3 Titration stand Manual titration stand complete 51108760 Electrode holder 51108730 11 30 METTLER TOLEDO DL77 DL70ES DL67 09 2002 Accessories Order No A Dual titration stand complete DV92 ot comprising Propeller stirrer incl 2 stirring rods see 4 below and Angle bracket 1 25655 ieee Spacing ring 1 23842 Clamping ring 1 25653 Threaded ring 1 25652 Knurled screw 2 25650 Electrode holder 2 min order quantity 5 25654 Stopper ST 14 5 3 min order quantity 5 23451 Stopper ST 7 5 2 min order quantity 5 23452 09 2002 METTLER TOLEDO DL77 DL70ES DL67 11 31 Accessories Order No Titration vessel 100 mL 7 polypro
174. is predispensing mode follows the selected parameters of the main titration however the increments are greater The titrator also registers the measured values quicker and acquires the potential values ET1 and ET3 see titration mode DOS Section 2 3 12 1 b You can link Predispensing 1 with Predispensing 2 02 93 METTLER DL77 DL70ES DL67 2 39 Titration EQP DYN EDITOR Selection menu Titrant addition You can select the dynamic DYN or incremental INC addition mode You can not decide the optimum addition mode for your titration until you know what type of titration curve you have DYN The volume increment added by the titrator changes within the defined limits AV min and AV max This should lead to a constant potential difference AE per increment E mV AE AE set AE AE3 V mL 1 Enter AE set mV e g 10 2 Select the limits AV and enter AV min smallest increment and AV max largest incre ment as absolute or relative values a Absolute Enter AV min mL e g 0 05 see following page Enter AV max mL e g 0 3 Notes a The smallest increment that the titrator can add is 1 5 000 of the burette volume 1 mL burette gt 0 0002 mL 5 mL burette gt 0 001 mL 10 mL burette gt 0 002 mL 20 mL burette gt 0 004 mL b If no predispensing takes place the titrator adds the first two volume increments with AV min 2 40 METTLER DL77 DL70ES DL67 02 93
175. ist All data of the method data mask remain stored ID1 number samples titration stand temperature temperature sensor molar mass and equivalent number You can modify these see Section 3 8 All data of the sample data mask are deleted ID2 weight volume and correction factor as soon as the titrator starts the second method If you have defined a fixed volume in the Sample function this remains stored Enter all data that you have to modify and or new data you have to save during the titration of the following methods see scheme on the next page e When the titrator has completed the second method it also moves it to the end of the method list etc e The method currently running is marked in the method list with gt You close the List continuous procedure with RESET If the titrator has no sample data for the method to be processed the sample data mask will be shown Press RESET In the menu that appears example Terminate ANALYSIS A Method RM35 appears only with the DL77 confirm Method RM35 with RUN and quit the mask with EXIT List continuous is terminated definitively This most recently started method is marked with an asterisk and remains stored together with all shifted methods without sample data Should you now restart List continuous the titrator would begin with method RM35 3 40 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Method list Example showing ho
176. itrated to 10 above the expected mL consumption that is 110 Enter the number 110 You expect a chloride fraction of 50 mg g Enter the number 50 The conversion constant for this content determination is M z Select this formula from the recommendation menu ya 110 50 mg g 0 924 g 100 35 45 g mol 0 0992 mol L 14 45 mL AgNO are titrated with these entries before the titration is termina ted Ifthe calculated amount falls between two increments the next increment will still be added Depending on the increment size a volume of 14 47 mL for example can thus be titrated 8 30 METTLER DL77 DL70ES DL67 02 93 Examples of formulae 8 6 4 Formulae for limiting the equivalence point To calculate the consumption of titrant for a specific equivalence point in a titration curve with several equivalence points you can have Q identified by a condition such as R1 Q EPOT gt 50 R1 Q EPOT gt 50 2 R1 Q EPOT 100 2 R1 Q EPOT P1 R1 Q EPOT H11 R1 Q P1 lt EPOT lt 300 Titrant consumption up to the 1st equivalence point of the 1st Titration function Equivalence points with a potential under 50 mV e g 51 300 will not be considered Titrant consumption up to the 1st equivalence point of the 2nd Titration function Equivalence points with a potential under 50 mV e g 51 300 will not be considered Titrant consumption up to the 1st equivalence point of the
177. itration for the rapid titration of 80 90 of the water content of a solvent or sample e Titration to absolute end point with dynamic titrant addition see Section 2 3 12 3 The absolute end point EPA is 5 0 mV e The wait time between the increments is 2 4 s the increment size 0 08 0 2 mL Second Titration function Fine titration for titration of the water content of the solvent or sample e Titration to absolute end point with dynamic titrant addition The absolute end point EPA is 5 0 mV e The wait time between the increments is 7 7 5 s the increment size 0 015 0 02 mL We have selected the parameters for both Titration functions so that the use of different solvents has no appreciable influence on the titration progress No titrant consumption in the second Titration function fine titration means overtitration in the first Titration function The display then shows you how to proceed with the message Overtitrated You must set the EPA of the first Titration function lower 10 2 3 2 MKF2 KF Drift Determination With solution titrated to dryness a small titrant consumption can always be detected and this is due to moisture diffusing into the system You must measure and store this drift in order to take it into account in the content calculation of a sample The MKF2 method contains two Titration functions separated by a wait time of ten minutes The first Titration function is used to titrate the solution to
178. l IS09001 1994 based Life cycle rules of Mettler Toledo GmbH Analytical Life cycle checkpoint details were reviewed and approved by the Project Supervisory Group PSG The products systems were tested to meet functional and performance specifications and release criteria at release to shipment In order to support GLP and validation requirements we will make the following documents available to an authorized governmental or regulatory agency for inspection e Product Guidelines e Performance Specifications e Documentation Plan e Software Specifications e Quality Plan e Project Management System e Test Plan e Customer Requirements e Review Reports e Source Code Mettler Toledo GmbH Analytical will maintain possession of all documents and their reproductions and may require a non disclosure agreement to be provided by those requiring access to these documents Yuhaso UP fof Schwerzenbach Dr Bernhard Grob Dr Urs Spitz March 1999 General Manager Manager Business Area Business Unit Analytical Titration 12 14 METTLER DL77 DL70ES DL67 03 99 Product Life Cycle Model Ideas Project Study Project Release Project Start Phose Basic Know how Product Guidelines Performance Specifications Qudiity Plan Documentation Plan Project Plan Review Report Phase Software Specifications Feasibility EE Review Report Phose Confirmation Review Report Phose projactend Readiness Customer Complain
179. le function in order to save them see Section 2 3 1 b Ifyou modify a user method or simply wish to copy it and keep the original you must give it a new method identification under the Title function see Section 2 3 1 c If you select a user method that is entered in the method list of the Analysis menu and not yet executed the message Method is blocked appears To modify this method you have to give ita new method identification under the Title function The method in the method list remains unchanged see Sections 3 1 and 3 13 02 93 METTLER DL77 DL70ES DL67 2 7 Select functions EDITOR 2 2 Select functions When you select the Title function you are shown this selection menu on the right of the display Modify You can only modify the Title function since the storage and call options require thatit is always first in the sequence of functions If you select the Measure function you are shown the following selection menu on the right of the display Cut Copy Paste Add Modify 2 2 1 Cut Position the selector bar on the command and confirm with RUN You can also cut a function directly from the list by pressing the lt gt minus key The Measure function is deleted at this location However it is stored in a buffer memory so that you can paste it in elsewhere if appropriate see Section 2 2 3 The function remains stored until you either cut or modify another function 2 2 2 Copy I
180. le into the printer port of the titrator Switch on the computer and start DLWin Titrator Switch on the titrator press lt Index D gt and select Memory copy The following menu appears Memory copy Prepare Request Confirm Prepare with RUN This command causes data to be transmitted via the printer interface Computer Select Backup in the main menu Select Request memory copy in the backup menu the data are copied Titrator Data transmission active appears in the display As soon as the copying operation is at an end the main menu appears in the display indicating that data transmission will now once again be routed across the computer interface 03 99 METTLER DL77 DL70ES DL67 5 7 Memory copy DOCUMENTATION Setup original cabling configuration Note All errors which can appear during the storage operation are listed in the Operating Instructions enclosed with the RS option 5 3 2 Request by titrator for a copy of data stored in the computer Computer Plug computer connection cable into the printer port of the titrator Switch on the computer and start DLWin Titrator Switch on the titrator press lt Index D gt and select Memory copy The following menu appears Memory copy Prepare Request Confirm Request with RUN The following menu appears Overwrite memory No Yes No The procedure will be terminated Yes The user
181. lect the relevant parameter value with SEL Spontaneous or On request Spontaneous The titrator sends the computer requests and data as soon as they are generated assumes that the computer is ready On request The titrator awaits the appropriate inquiry from the com puter before sending a request or data Communication Selectthe relevant parameter value with SEL Normal or Reduced protocol Normal The data received either by the titrator or the computer will be checked and errors found will be announced with error messages safety mechanism active Reduced Data received will neither be checked nor acknowledged consequently no error messages will be sent Safety mechanism in active Start end Select the relevant parameter value with SEL lt CR gt or lt STX gt characters lt ETX gt These start of text and end of text characters for telegrams to be sent depend on the input possibilities of your computer You will find additional information regarding communication between the titrator and the computer in Section 7 1 and in the Operating Instructions provided with the RS option 02 93 METTLER DL77 DL70ES DL67 1 33 Peripherals INSTALLATION Peripherals Menu tree for system with computer Peripherals Printer Not installed 1 Balance Not installed 1 System Not installed j Sample changer Not installed System parameter Instrument type
182. lect this menu and its submenus by moving the selector bar and confirming with RUN Since you have to select the menu and the auxiliary functions frequently there is a faster way e Use the key combination lt index F gt to obtain the menu e For the auxiliary functions themselves numeric keys take over the function of the selector bar and the RUN key You press only the key with the function number that precedes every auxiliary function If you know the function number you can already press the corresponding keys in any menu see menu representation on the following page Note Thelines 4 Temperature and 7 Calibration temperature sensors appear only if you have inserted a temperature option the line 5 Sample changer appears when you have installed an ST20A ST20 see Sections 11 1 7 and 1 8 4 02 93 METTLER DL77 DL70ES DL67 4 3 2910 830210 4410 YAILLAW vv 6 c0 Menu tree with function numbers To obtain the selection menu immediately from any other menu press the lt index F gt key then the following function numbers Auxiliary functions 1 Burette 2 Stirrer 3 Sensor 4 Temperature 5 Sample changer 6 Auxiliary instrument 7 Calibration temperature sensors 8 Offset adjustment sensor inputs Burette 4 1 Rinse burette 2 Rinse burette 11 S SCH 3 Rinse tip 12 4 Dispense cont S Dispense 13 1 5 Man titra
183. led on burette drive 3 for the Karl Fischer titrant To protect the titrant against moisture mount the drying tube holder in the opening of the burette holder fill the drying tube with molecular sieves or some other drying agent and position on the drying tube holder see Accessories page 11 30 Caution KF titrants evolve gas SO especially at elevated temperatures causing bubbles to form in the tubing as well as in the burette stopcock For this reason you should rinse burettes prior to titration Titration head Always insert the electrode and burette tip diagonal to each other so that the solution is thoroughly mixed before its potential is measured by the electrode To dispense the KF solvent take the appropriate measures see Section 10 2 3 4 Note a 02 93 METTLER DL77 DL70ES DL67 10 5 Karl Fischer methods Insert the gas inlet if you wish to titrate under a dry inert gas Insert the septum stopper if you wish to add liquids using a syringe Close the remaining openings with stoppers The weighing spoon is used to add solids The drain cock serves to empty the titration vessel Double pin platinum electrode Attach the electrode to the polarization current source DK102A Attach a triaxial cable to the current source and plug it into sensor input 1 Sensor input 2 is less suitable Polarization current source Switch on the current source only when the platinum ti
184. lt index F gt 02 93 METTLER DL77 DL70ES DL67 4 7 Burette AUXILIARY FUNCTIONS 4 1 4 Dispense continuously With the aid of this function you can dispense continuously and follow the change in potential with the dispensing on the display To execute the function press function number 4 If you press 1 4 in the Auxiliary functions menu you are immediately shown the selection menu 1 Modify 2 Start Modify press 1 You are shown the parameters whose value or name you can change If you press lt index F gt 1 41 when e g in the main menu you are shown the parameter mask immediately 1 Select the burette drive from the selection menu 2 Select the burette volume from the selection menu 3 Enter the rate mL min at which dispensing should be performed 4 Select the sensor from the recommendation menu or enter the one you have installed The sensor acquires the measured values in the unit of measurement you have installed see Section 1 2 2 5 Select the titration stand from the selection menu 6 Enter the speed of the stirrer 0 100 e 0 gt stirrer is inactive e 100 gt stirrer operates at maximum speed 7 Enter the temperature C of the solution to be measured if you have not attached a temperature sensor 8 Select the temperature sensor from the selection menu If you confirm one of the parameters with RUN you can start dispensing Start press 2 or RUN e The titrator dispense
185. mV pH pM pX T Minimum Maximum 0 0 0 Standard Asymmetric 10 0 2 1 Segmented 10 0 2 1 With the aid of the appropriate titration curve or table of measured values there is no table for the 2nd derivative you can read off the potential value the values for AE AV or the values for A2E AV2 and then enter the threshold value 1 Example of the threshold value of a titration curve for the evaluation procedure Minimum The minimum of this titration curve is at 150 mV You can enter for instance 30 as thresh old value The sign for the mV value must also be entered E mV 200 100 Threshold value 30 100 Minimum 200 V mL 2 46 METTLER DL77 DL70ES DL67 02 93 EDITOR Titration EQP Threshold 2 Example ofthe threshold value of a titration curve for the evaluation procedures Standard and Asymmetric E mv Titration curve V mL AE AV mV mL 1st derivative Maximum absolute Measured value Threshold V mL 02 93 METTLER DL77 DL70ES DL67 2 47 Titration EQP Threshold EDITOR 3 Example of the threshold value of a titration curve for the evaluation procedure Seg mented Titration curve E mV V mL 1st derivative AE AV mV mL V mL REES A E AV mV mL Maximum absolute lt a Measured value Threshold value V mL 2 48 METTLER DL77 DL70ES DL67 02 93 EDITOR Titration EQP EQP range EQP
186. mand on g balance unit in g e Int FACE SENd S Stb transmission mode standby bd 2400 baud rate 2400 PAr E parity even HS OFF handshake XON XOFF off c With AB PB and PR balances the LC CL cable must be configured as follows SS e Left switch position 7 q woo EM e Middle switch position 3 e Right switch position 4 d You can also attach SARTORIUS balances with the converter cable RS CL CL RS see Accessories Section 11 3 for this you must select Bidirectional as the transmission mode We have tested the following balances e BA 3100 P e E 12000 S e A200S e MC1 LC 220 S e MC1 RC 210 P The data output of the attached balances must be configured as follows e Data output ext print command irrespective of stability e Baud rate 2400 e Parity even e Stop bit 1 e Weight unit g 12 93 METTLER DL77 DL70ES DL67 1 31 Peripherals INSTALLATION 1 8 3 System If you wish to attach a terminal or a computer you must first install these devices Select System and you are shown the following parameters Instrument type Not installed Baud rate 4800 Parity Even Number data bits 8 bits Number stop bits 1 stop bit 1 Select the instrument type from the selection menu e Color terminal e Monochrome term e Computer e Not installed 2 Select the baud rate from the selection menu e 1200 e 2400 e 4800 e 9600 3 Select the parity from the selection menu e Even e Odd e
187. means of the dispensing rate parameter see Section 1 4 2 b Ifyou perform a method series on the sample changer and the titrator has titrated the last sample of the last method sensor and burette tip are rinsed in the middle beaker position The sample beaker is then raised so that the sensor does nat dry out in other words it remains in the sample solution To prevent this you must add a Conditioning function to the last method and position a condi tioning beaker after the final sample beaker Y A TITRATION Y CALCULATION Y RINSE No Series size reached The Conditioning function mustthen be afterthe Y loop of the last method so that the titrator does not STATISTICS perform conditioning after every sample determi Y nation see Section 2 3 2 Example of a sample CONDITIONING series performed with the standard method and y Section 2 3 10 Conditioning 2 26 METTLER DL77 DL70ES DL67 02 93 EDITOR Conditioning 2 3 10 Conditioning You use this function only in connection with the sample changer ST20A or ST20 You determine how often and how long a sensor is kept in a solution with stirring between individual samples or series to clean it or ensure its operational reliability 1 Enter the interval number of samples e g 3 2 Enter the time s e g 60 gt After three titrated samples conditioning is performed for 60 s The running conditionin
188. method data mask the sample data mask nor the request regarding the current sample see Sample function Section 2 3 2 Ifthe method has two Sample functions the method data mask reappears after confirma tion with RUN In this case a 2 follows Sample function No Ifyou have selected Fixed volume in the Sample function and have specified the volume only ID2 and the correction factor can be entered or modified in the sample data mask The entry limits Minimum and Maximum are missing If you do not need these entries you can skip this mask by quitting the previous method data mask with EXIT If you confirm the sample data mask with RUN a mask for each sample of the designated number of samples in this Sample function will be shown in succession for several Sample functions masks for the other function s samples will be shown as well Sample No 2 1 and so on Sample data need not be entered at this point You can circumvent the sample data masks by leaving the previous method data mask with EXIT see menu sequences on pages 3 4 3 5 und 3 11 e The sample data mask will then appear prior to the request Current sample You can enter the weight volume for the first sample only e The mask will not reappear if you have specified results within a method under the Calculation function that do not need the weight volume entry in other words the titrator needs no entries Example R VEQ or R Q If you must enter the weight or v
189. mission mode 1 30 Units 2 67 8 27 Units of measurement potential 1 10 1 11 temperature 2 22 User data memory accessories 11 39 inserting 11 18 technical data 11 22 USER LEVEL 6 3 User methods 2 6 12 10 METTLER DL77 DL70ES DL67 02 93 Index VDISP 2 24 8 3 VEQ 2 36 8 5 VEX 8 5 Voltage range 11 14 Volume entering 3 7 selecting 2 15 Volume limits at volume entry 3 9 entering 2 15 VP1 VP2 8 6 8 9 VSTAT 2 62 8 8 VT 2 64 8 7 8 9 VT1 VT2 2 62 8 7 8 9 VTOT 2 62 8 7 Water determination 10 5 Weight entering 3 7 selecting 2 15 transferred by balance 3 9 Weight limits at weight entry 3 9 entering 2 15 in the sample data mask 3 7 x mean value 2 75 8 8 z equivalent number 2 16 2 68 3 7 8 3 Zero point sensor calculation 2 72 entry through calibration 1 12 explanation 1 11 theoretical value 1 12 Zero point temperature sensor entry through calibration 1 15 explanation 1 15 theoretical value 1 15 02 93 METTLER DL77 DL70ES DL67 12 11 1509001 certificate for METTLER TOLEDO The Mettler Toledo GmbH company Greifensee was examined and evaluated in 1991 by the Swiss Association for Quality and Management Systems SQS and was awarded the ISO 9001 certificate This certifies that Mettler Toledo GmbH Greifensee has a quality management system that conforms with the international standards of the ISO 9000 series Repeat audits are carried out by the SQS at intervals to check
190. mmediately see below or e the titrator interrupts the Titration function right before the end when the condition specified for the parameter Stop for reevaluation is fulfilled see Evaluation criteria Section 2 3 12 2 In this case the following mask is displayed Reevaluation necessary Titration 1 neg 0 specified condition Confirm this message with RUN The following selection menu appears DL77 DL70ES DL67 see Section see Section Method Method Add 3 1 3 13 1 Continue 3 4 Continue 3 4 Sample data 3 7 Sample data 3 7 Display 3 9 Display 3 9 Stirrer 3 10 Stirrer 3 10 Records 3 11 Records 3 11 Calculations 3 12 Calculations 3 12 Method data 3 8 Method data 3 8 Modify method 3 6 Modify method 3 6 Reevaluation 3 5 Reevaluation 3 5 Record data 3 8 1 Record data 3 8 1 a If you interrupt a METTLER method the menus Modify method and Reevaluation are missing This also applies to methods stored only in the computer see Method ID Section 3 1 02 93 METTLER DL77 DL70ES DL67 3 19 Reevaluation ANALYSIS Select Reevaluation The following parameter mask appears Reevaluation Threshold EQP range Steepest Jump only Buffer potential 1 Buffer potential 2 Modify the appropriate parameters and quit the mask with EXIT The following selection menu appears Save Permanent Temporary No Permanent The modified values of this Titration functi
191. n be entered at a time While a titration is running you can develop and save a new method or you can enter sample data for the next titration method This is not possible with the DL67 02 93 METTLER DL77 DL70ES DL67 3 Operating concept What information will you find where 1 The TUTORIAL provided with the standard equipment will help you to overcome any inhibitions you may have with regard to the new instrument You will get to know the function keys the keypad and the display Using a stored method for an acid base titration you will perform your first analysis 2 These Operating Instructions provide a complete description of the concept and oper ating characteristics of the three titrators The operating concept and a compilation of the key combinations follow this introduction 3 TheRS232C Interface Description i e a detailed description of the communication bet ween titrator and computer is provided with the standard equipment since June 1999 Note These Operating Instructions apply to software version 3 0 or 3 1 The organization of the Operating Instructions The organization is based on a modular principle This allows supplementation or the inter change of individual sections or pages new text sections carry the date of issue in the footer on every page The operating concept of the titrator The operation of the titrator is menu driven What does this mean The titrator handles various tasks
192. n mode c The earliest possible equivalence point will be recognized if it lies in the vicinity of the sixth measurement point measurement points from a pretitration are not considered see Equivalence point recognition page 2 45 Ifthe equivalence point lies in the vicinity of the fifth point for instance it will not be recognized 02 93 METTLER DL77 DL70ES DL67 2 59 Titration LEARN EP EDITOR 2 3 12 5 LEARN EP Learn titration end point determination If you are not sure what parameters you should enter for the titration mode EP select LEARN EP Titration function selection of the parameter example Titrant NaOH Concentration mol L 0 Sensor DG111 SC Unit of meas urement As installed Titration mode LEARN EP Condition No When you start the method the titrator executes one function after the other As soon as it has completed the Titration function it calculates the parameters for the titration mode EP stores them and sends the data to the printer While the parameters of the Titration function are being printed the titrator executes the remaining functions Printout of a learned EP titration LEARN TITRATION Method Ber LEARN TITRATION Version 30 Nov 1992 12353 Titration 1 TitrantNa0H Concentration mol L oooooooooo ooo 0 1 SENSOT sens a a eed EE E da DG111 SC Unit OF MEAS ie iia eid Ne RTE teje EE id iia As installed Titration Mode usas a e as ds Er EP PHECISPESNSAN
193. nSO solution with the concentration of 0 1 mol L is stored that is used as volumetric solution for the titer determination of EDTA see METTLER method M007 Section 10 H1 c ZnS04 0 1 H2 LH etc You can neither delete H1 to H20 nor add H21 to the list If you select H1 for instance you are shown the following parameter mask Auxiliary value Hl ID text c znSO0g Value 0 1 Date time 00 00 0000 00 00 1 You can not change the name H1 The line will be skipped when the selector bar is moved 2 Modify eventually the identification text 3 Modify the value do not modify it if you use method M007 4 Youcan not enter the date It refers to the determination of the auxiliary value using the method function Auxiliary value and is entered here together with the time automatically see Section 2 3 15 Notes a You can delete the data of an auxiliary value only by overwriting it or letting the titrator overwrite it through the Auxiliary value function b You receive no warning from the titrator if you overwrite an auxiliary value If you make full use of the auxiliary value memory you should print out a list of its values occasionally see Section 5 1 2 c If you modify an auxiliary value parameter the date time is deleted 02 93 METTLER DL77 DL70ES DL67 1 23 Auxiliary values INSTALLATION The auxiliary value with the modified parameters is installed when you quit the parameter mask with EXIT see the a
194. nate Sensor Sensor 1 Stirrer Aux 1 Dispense Drive 3 All functions are now interrupted To terminate them select Sensor and confirm with RUN confirm Stirrer with RUN confirm Dispense with RUN and quit the mask with EXIT You are shown the display in which you have pressed RESET 02 93 METTLER DL77 DL70ES DL67 4 5 Burette AUXILIARY FUNCTIONS 4 1 Burette If you rinse burettes or burette tips or wish to dispense a certain volume select this auxiliary function You can press 1 in the Auxiliary functions menu when in any other menu lt index F gt then 1 You are shown the following submenu 1 Rinse burette Drive 3 2 Rinse tip Drive 3 3 Dispense Drive 3 4 Dispense cont inuously Drive 3 5 Man ual titration NaOH DG111 SC Caution Only two burette drives can be active simultaneously Burettes reserved for a certain method cannot be selected This applies to e the burettes in use for a current method and e all burettes that will be used in the methods that have been activated with the commands List once or List continuous see Sections 3 13 3 2 and 3 13 3 3 4 1 1 Rinse burette To execute this function from within any menu press the key combination lt index U gt and enter the burette drive 1 2 3 or 4 The titrator delivers 1 burette volume The piston of the burette moves below the zero position so that air bubbles that hide in the stopcock are sucke
195. nce If you have the weight transferred by a balance press SEL You are shown the mask Weight 0 00000 gt 0 13460 Accept weight When the weight value is stable confirm Accept weight If the weight is below the minimum three minus signs appear after Weight if it is above the maximum three plus signs are displayed You can modify the weighing or confirm it see Note a If you have selected the bidirectional transmission mode you can accelerate the entry process Press SEL at the weight entry 0 0000 in the first sample data mask The sample number e g no 1 1 is faded in on AT AM and PM balances Press the TARA key so that the current weight appears on the display of the balance With these balances the weight limits also appear so that you can change the weight if need be Confirm the weight transfer with the Print key of the balance the titrator automatically readies itself for the weight entry of the next sample In this manner you can enter the weight values of all samples of a method without pressing a key of the titrator If you have the Mettler DataPac M connected to AM or PM balances you can enter the ID2 on this Press lt CLEAR gt enter ID2 press lt ENTER gt 02 93 METTLER DL77 DL70ES DL67 3 9 Executing a method ANALYSIS 3 1 2 Notes on method and sample data mask a If there is no Sample function in a method you are shown neither the
196. nction are defined with default values or names You can accept or modify these you can also add additional functions to this standard method see Sections 2 2 3 and 2 2 4 Note To set up a method with more than the standard functions you will find the scheme in Section 8 8 useful You can copy this scheme and use it to design the method which you can then enter in this menu 2 1 1 Print Position the selector bar on this command and confirm with RUN The method together with its functions and the corresponding parameter values will be printed out on an attached printer 2 6 METTLER DL77 DL70ES DL67 02 93 EDITOR Select methods 2 1 2 Delete Position the selector bar on this command and confirm with RUN In the selection menu Delete method you can confirm or cancel the selection Yes The method is deleted No The method remains stored Notes a METTLER methods can not be deleted b If a user method is entered in the method list of the Analysis menu and not yet executed the message Method is blocked appears see also Note c in the next section 2 1 3 Modify When you select this command you receive a list with all functions included in this titration method e g Title Sample Measure Dispense Stir Titration Calculation Record Notes a You can modify METTLER methods to match your requirements but you must then provide them with a new method identification under the Tit
197. nd and confirm with RUN The mask of the selection menu disappears the auxiliary reagent H20 is deleted Note You can also delete an auxiliary reagent directly from the list by pressing the lt gt minus key You can reinstall H20 with the command Add see Section 1 4 3 1 4 2 Modify If you select this command you are shown the parameter mask of the auxiliary reagent in which you can change the parameter values Name H20 Dispensing rate mL min 250 Auxiliary output Aux 2 1 Selectthe name ofthe auxiliary reagent from the recommendation menu or enter the name of the reagent you wish to install in place of H20 02 93 METTLER DL77 DL70ES DL67 1 17 Auxiliary reagents INSTALLATION 2 Enter the dispensing rate mL min of the device Notes a The titrator uses the dispensing rate to calculate the volume to be dispensed for time controlled pumps or electromagnetic valves see functions Pump and Rinse Sections 2 3 8 and 2 3 9 b The dispensing rate of each device must be determined experimentally in advance for each solvent Add the particular solvent using the dispensing device to a measuring cylinder within 1 minute stopwatch and note the volume Repeat this procedure for e g periods of 20 30 and 40 seconds Use the different volumes to calculate the mean value per minute and enter this value 3 Select the auxiliary output from the selection menu Note The titrator has three auxiliary o
198. ndex F gt 5 6 1 when e g in the main menu you are shown it immediately 1 Select the sample changer ST20 1 or ST20 2 2 Enter the time s during which the pump attached to the sample changer should perform dispensing The specified time is an empirical value If you confirm the entry with RUN you can start dispensing Start press 2 or RUN e The pump dispenses for the specified time To obtain the Auxiliary functions menu again press lt index F gt 02 93 METTLER DL77 DL70ES DL67 4 19 Sample changer AUXILIARY FUNCTIONS 4 5 7 Dosing pump manual If you wish to interrupt a dispensing operation manually press function number 7 If you press 5 7 in the Auxiliary functions menu you are immediately shown the selection menu 1 Modify 2 Start Modify press 1 You are shown the parameter mask 1 Select the sample changer ST20 1 or ST20 2 If you confirm the selection with RUN you can start dispensing Start press 2 or RUN If you press lt index F gt 5 7 2 when e g in the main menu you can start the dispensing process immediately e The pump dispenses until you stop the process with RUN or 3 To obtain the Auxiliary functions menu again press lt index F gt 4 5 8 Dispenser If you have attached a dispenser to the DISPENSER output of the sample changer press function number 8 If you press 5 8 in the Auxiliary functions menu you are immediately shown the selection menu
199. ndex i is the number of the parameter within a function Index j is the counter for the number of functions within a method The following designations are associated with this indexing form Q VEQ EHNV EPOT Example Q2 2 mmol consumption up to the second equivalence point of the second Titration function Excerpt from a method determination of HCI CH3COOH und NH4CI with NaOH Two Titration functions were selected because for CH3COOH and NH4Cl different values were defined for the equilibrium controlled measured value acquisition EQU y Titration E mV A The titrator executes the first Ti tration function and titrates up to the equivalence point of HCI It determines among other things the mmol consumption Q1 1 and the mmol excess QEX 1 EQP1 Qq1 1 Q V mL QEX 1 QEX lt gt lt on QEX 1 Eeer HCI In the first Calculation function esult name oocoonoccccconannccnnns you definethe mmol consumption Formula ori R1 Q1 1 for HCI a RUE Since you can omit index 1 the Salt unit occconcccooornoooooos mmo formula can also ben 0 Decimal places 4 8 12 METTLER DL77 DL70ES DL67 02 93 Use of indexes Titration E mV EQP1 EQP2 gt V mV lt gt Q1 2 Q2 2 Calculation Result name ooccccccnncnnnccincc CH3COOH SA R2 Q1 2 QEX 1 CONSIGN veian Result unt mmol Decimal pl
200. ng Print in the right part of the display enables you to print the results To start with the next manual titration press EXIT and confirm Start To obtain the Auxiliary functions menu again press lt index F gt 4 10 METTLER DL77 DL70ES DL67 02 93 AUXILIARY FUNCTIONS Stirrer 4 2 Stirrer If you wish to stir solutions to dissolve substances or to support a titration method without a Sample function select this auxiliary function Caution Stirrer outputs reserved for a certain method using the titration stand specified in the Sample function cannot be selected This applies to e the stirrer output being used in a current method and e all stirrer outputs that will be used in the methods that have been activated with the commands List once or List continuous see Sections 3 13 3 2 and 3 13 3 3 If you press function number 2 in one of the other menus lt index F gt then 2 you are shown the selection menu 1 Modify 2 Start Modify press 1 You are shown the parameters whose value or name you can modify If you press lt index F gt 2 1 when e g in the main menu you are shown the parameter mask immediately 1 Select the titration stand from the selection menu The titrator now knows which stirrer it has to control see Titration stands Section 1 7 2 Enter the speed of the stirrer 0 100 e 0 gt stirrer is inactive e 100 gt stirrer operates at maximum speed If you confirm
201. ng the method You can change the number of samples during a current method before the titrator processes the Statistics function e If you increase the number the corresponding lines are added at the end of the sample data list e If you decrease the number the corresponding lines are deleted at the end of the sample data list You can then enter the data of the added number of samples in the Sample data menu see Section 3 7 Before starting a method Select the method in the method list see Section 3 13 not valid for the DL67 Select Method data from the selection menu The method data list appears During a current method Press EXIT and select Method data The method data list of the current method appears e g No CDI Samp Stand Ll das 3 Stand 1 If one method has two or more Sample functions these will also be listed such as No CDI Samp Stand LT Ca t 3 Stand 1 2 Mg Ca 5 Stand 1 If you confirm the first line No 1 with RUN the method data mask appears Method data Sample function No dl ID1 Ca Number samples 3 Titration stand Stand 1 Temperature pC 23 0 Temperature sensor Manual Molar mass M 110 99 Equivalent number z 2 3 26 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Method data Modify the appropriate parameters When no method is running either press RUN The selection menu Method appears or press lt index A
202. nly when the titrator has transferred all data to the printer only when the method has Record as its last function During this operation the message Output unit writing record appears Note All results of a learn titration are marked on the display with an exclamation mark If you confirm the result list with RUN the selection menu appears DL77 DL70ES DL67 see Section see Section Method Method Add 3 1 3 13 1 Load 3 1 3 1 4 Start 3 1 3 1 4 3 1 3 3 Start 3 1 3 1 4 Sample data 3 Sample data 3 Display 3 9 Display 3 9 Records 3 11 Records 3 11 Calculations 3 12 Calculations 3 12 Method data 3 8 Method data 3 8 Cut 3 13 2 1 C t 3 13 2 1 Record data 3 8 1 Record data 3 8 1 You can select all menus or execute all commands of this selection menu before starting the next method 02 93 METTLER DL77 DL70ES DL67 3 13 Executing a method ANALYSIS Note The executed method is marked by an asterisk Before you start the next method you can reexamine the sample data or have them printed out see Sections 3 7 and 3 8 1 As soon as you start the next method all data of the executed method are deleted 3 1 4 Restarting a previously executed method If you select the previously used method and confirm Start the titrator reloads this method automatically In doing this stored modified method data are retained whereas sample data entered for the previous series are deleted and must
203. nnannn 9 3 9 1 Error messages Of the titrator ooooonnicnccccnnnnnnncccccccncconnnanncnnnnnnnnnnrannnnnrnnnanannn 9 3 9 2 Oth r err rs and Malicia 9 5 02 93 METTLER DL77 DL70ES DL67 9 1 Error messages and malfunctions 9 Error messages and malfunctions 9 1 Error messages of the titrator The titrator sends you messages regarding errors that you can rectify yourself Four such messages draw your attention to this section 1 EEPROM inserted wrongly EEPROM user data memory Forsome reason or other you have inserted the user data memory in which the installation data are stored into the second IC socket see Section 11 1 8 Illustration IC socket 2 Measure Switch off the titrator and disconnect from power supply Insert the user data memory into the first IC socket 2 Faulty data deleted a The titrator has saved only parts of a method if e g during storage of this method the power failed It deletes this method completely Itis also possible that several methods have been deleted Measure Confirm the message with RUN Check whether your methods have been deleted and reenter if necessary b The titrator has saved only parts of parameters of a resource if e g during storage of these parameters the power failed It deletes the entire list of this resource e g all titrants or all sensors Measure Confirm the message with RUN The titrator now loads the standard list of the resource e g
204. nnos 2 CONCItION iiss essione nano Yes CONQILION EE 7 lt E lt 14 The titrator calculates the neutrali zation value through the mmol con sumption of base The titrator executes this Titration function only if the measured value E determined previously is in the pH range 7 14 The titrator calculates the neutrali zation value through the mmol con sumption of acid Example 2 In METTLER method M002 Titer is a conditional function Titer A o vans NaOH Concentration Immo 0 1 Formula A A X CONGO Main gege tere eege ee Yes CONAN soisissa saaan 0 9 lt X lt 1 1 The titrator enters the calculated mean value x of the Statistics func tion in the installation data of the titrant only if it lies in the range 0 9 1 1 02 93 METTLER DL77 DL70ES DL67 8 19 Evaluation procedures 8 4 Evaluation procedures The titrator has various procedures to determine the equivalence points of a titration curve accurately e Standard e Asymmetric e Segmented e Minimum maximum 8 4 1 Standard You use this procedure for all S shaped titration curves The evaluation is effected with the aid of an iterative procedure nonlinear regression 1 The titration of a strong acid with a strong base is used as a mathematical model The determined equivalence point in this model always lies in the vicinity of the inflection point At least five measurement points around the inflection point are used for the evalua
205. nt mV or As installed As installed refers to the unit of measurement you have defined for the sensor see Section 1 2 2 6 Pretitration You select the pretitration if your solution does not yet have the value of the potential you need for the pH stating Yes Enter control band mV pH see Section 2 3 12 3 Titration mode EP No 7 End point pH stat From the selection menu select the absolute or other end point and define the potential value that should be kept constant during the pH stating EPA Enter mV pH value see Section 2 3 12 3 Titration mode EP EPS Enter the end point see Section 2 3 12 3 Titration mode EP 8 Control range As a control range you define a potential value that controls the end point range The smaller this value the faster the titrator reacts to a deviation from the potential value of the defined end point potential Enter control range mV e g 2 9 Select the tendency Positive or Negative see Section 2 3 12 3 Titration mode EP The choice of tendency refers to the added titrant The actual reaction investigated by pH stating always leads to a change in the opposite direction 02 93 METTLER DL77 DL70ES DL67 2 63 pH mV stat EDITOR 10 Enter the termination criteria a Maximum volume mL e g 40 The entry is intended as a safeguard If the titration is faulty excess titrant will not be added needlessly b Minimum time
206. ntent dispensing b dispensing to a potential c dispensing to the slope of the curve 02 93 METTLER DL77 DL70ES DL67 2 35 Titration EQP EDITOR 2 3 12 2 EQP Equivalence point titration The equivalence point is the point at which exactly the same number of equivalents of titrant and analyte have reacted In most cases it is virtually identical to the inflection point of the titration curve This inflection point is recognized EPOT equivalence point potential and the equivalence point calculated VEQ or Q mL or mmol consumption up to the equivalence point With this titration mode the titrator also determines the half neutralization value EHNV as araw result Parameters of the mask Predispensing 1 Predispensing 2 Titrant addition Measure mod Equivalence point recognition Threshold ba EQP range Termination criteria Maximum volume mL a denia Termination at potential RE Termination after n EQP s ON Termination at slope Bee Termn ination after nom inal consumption VE Combined termn ination criteria Evaluation criteria Evaluation procedure aa Steepest jump only eege Buffer potential 1 nie Buffer potential 2 a Stop for reevaluation 2 36 METTLER DL77 DL70ES DL67 02 93 EDITOR 02 93 METTLER DL77 DL70ES DL67 2 37 EDITOR 2 38 METTLER DL77 DL70ES DL67 02 93 EDITOR Titration EQP Predispensing A predispensing shortens the titration time The titrator
207. nu again press lt index F gt 4 22 METTLER DL77 DL70ES DL67 02 93 AUXILIARY FUNCTIONS Calibration temperature sensors 4 7 Calibration of the temperature sensors With the aid of this function you can calibrate your Pt100 or Pt1000 sensors to be certain that the measured temperature values are correct Note Section 11 1 7 describes how to setthe temperature options for use of eitherthe Pt100 or Pt1000 sensors If you press function number 7 in one of the other menus lt index F gt then 7 you are shown the following menu 1 Modify 2 Start Modify press 1 You are shown the parameter mask 1 Select the temperature input from the selection menu If you confirm the selection with RUN you can calibrate the temperature sensor Start press 2 or RUN You are shown the following Immerse sensor in ice water Continue Terminate Immerse the sensor in ice water we recommend to use a Dewar vessel Wait for some time so that the sensor can cool to 0 C Then confirm Continue with RUN In the selection menu 3 Stop appears The temperature sensor is calibrated as soon as 2 Start reappears Should the measured temperature value notlie within the range of 2 C to 2 C the following error message will appear Measured value out of limits Measured value not stored Confirm the message with RUN and first check the temperature value given by the sensor using the auxiliary
208. o the external control unit and then waits until this sends back the same code Only then does the titrator start to process the next method function 2 Enter the code A number between 1 and 32 3 Enter a comment in the space foreseen for it This comment appears on the display when the function is executed 4 Select a condition No Yes Enter the condition Notes a You will find additional information regarding the communication between the titrator and the external control unit in Section 7 b Two titrators can also be synchronized by means of the system interface using the SYNC function see Operating Instructions RS232C Interface Description provi ded with the RS option c With the DL77 it is possible to use the SYNC function to synchronize the two method lists in Analysis menus A and B see Operating Instructions RS232C Interface Description provided with the RS option 02 93 METTLER DL77 DL70ES DL67 2 81 ANALYSIS Contents Page 3 ANALYSIS rails 3 3 3 1 Exe uting a method sesos ico 3 4 3 1 1 Notes On AP 3 9 3 1 2 Notes on method and sample data maek un 3 10 3 1 3 Titration SEQUENCE ENEE 3 12 3 1 4 Restarting a previously executed method AEN 3 14 3 2 Terminate current method RESET 0 0 0 0 ccccccccceccceeeeeeeeeeeeeeeeeeeeeeees 3 15 3 3 Fade out current method AAA 3 16 3 4 Interrupt current Method AA 3 17 3 5 Reevaluation sra 3 19 3 6 Modify current Method AA 3 21 3 7 Sample data
209. olume during the titration for example when no time may be lost by back weighing confirm the sample data mask with RUN without entering the weight Since the titrator does not need the sample data until it performs calculations the sample data mask reappears in the display either e when the titrator reaches the Titration function in which a predispensing to nominal content or a termination criterion after nominal content has been specified or e when it reaches the Calculation function in which the weight m is needed for the result see Examples of methods Section 8 7 1 You also have the possibility to fade out the titration with EXIT and enter the weight in the selection menu Sample data see Sections 3 3 and 3 7 3 10 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Executing a method Example of the menu sequence when weight volume must be entered during the active method Method Method Add DL67 Load y Method entry Method ID CALC User UB Data entry Y Method data Sample function No 1 ID1 Ca457 Method Method Number samples 3 CALC UB Add DL67 Load Titration stand Stand 1 M EXIT Start Temperature C 25 0 Sample data Temperature sensor Manual Method data Molar mass M 110 99 Cut Equivalent number z 2 Record data Method Start DL67 This mask CALC UB Single method does not Li
210. on 2 3 modifying 2 7 printing 2 6 recording 2 77 saving 2 11 selecting 2 5 Method selection menu method completed 3 13 method faded out 3 16 method interrupted 3 17 3 19 starting method 3 8 Method data menu 3 26 modifying before starting method 3 6 3 26 modifying during current method 3 26 printing 3 27 Method data list 3 26 Method data mask notes 3 10 Methods development design scheme 8 36 examples 8 32 maximum number method list 8 25 printing list 5 3 Method ID entering 2 14 3 6 explanation 2 5 modifying 2 11 overwriting 2 11 Method list filling 3 35 modifying 3 36 processing 3 37 Method series 2 26 with 2 sample changers 3 46 titration sequences 3 38 3 39 METTLER methods list 10 4 memory 11 22 selecting 2 5 Minimum evaluation procedure equivalence point recognition 2 45 evaluation criteria 2 51 explanation 8 23 Miscellaneous menu 1 36 Moisture determination 10 5 Molar mass calculation function 2 68 entering 2 16 modifying 3 7 neq number of equivalence points 8 5 New method 2 6 Nominal content dispensing 8 28 predispensing 8 28 Null modem pin assignment 11 24 Number samples entering 2 15 modifying 3 6 Numeric keys 4 3 Offset adjustment 4 24 Operating concept 4 Outlier test 2 75 Output unit 2 77 P1 P2 8 6 8 9 Paper printer fanfold 1 28 single sheet 1 28 Paper format 1 29 Parallel titrations notes 3 43 procedure 3 42 Parity balances 1 30 printer 1 29 system 1
211. on are saved permanently in this method Temporary The modified values of this Titration function are saved only until the end of the current method No You save none of the changes If you confirm Permanent or Temporary with RUN the titrator will reevaluate the titration curve The printer simultaneously prints out this Titration function with the modified param eters The selection menu Method reappears If your modifications still satisfy the specified condition the message Reevaluation necessary reappears Confirm Continue with RUN On the display appears e the representation of the Titration function shown before the interruption if additional dispensing for example is necessary due to the changed parameters or e the next function the titrator must process Note To evaluate the consequences of your modification you can e inspect the curve or table of measured values and print it out Display or Records menu see Sections 3 9 and 3 1 1 e check the new raw results of the Titration function by assigning these to Rx or Cx e g Rx VEQ oder Cx VP1 Calculations menu see Section 3 12 3 20 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Modify method 3 6 Modify current method You have interrupted the current method and selected Modify method You are shown all method functions In these functions you can modify only the numeric parameter values no other parameter values or names can be sele
212. on is drawn to error messages directions and instructions by a signal If you do not wish to hear this press SEL gt No Notes a Error messages You must confirm each error message with RUN and rectify the error Otherwise the titrator will not continue with the desired operation b Instructions Your current method includes the function Instruction under which you have entered a text You must confirm this with RUN before the titrator can continue operation see Section 2 3 6 c Directions During the sequence of a method the titrator will give you directions that you must confirm with RUN before it can continue operation 02 93 METTLER DL77 DL70ES DL67 1 39 Miscellaneous INSTALLATION 1 9 8 Analysis parameters During the course of a titration method certain information which must be confirmed with RUN for the titration to proceed will appear on the display e Initially the mask Installed are see Section 3 1 e After the titration the mask Results of this sample see Section 3 1 3 These two masks can be excluded to accelerate the titration course If you select this menu you are shown the following parameter mask Installation data Yes The mask Installed are appears prior to titration of each sample Should this not happen press SEL gt No Results last sample The mask Results of this sample appears after titration of each sample Should this not happen press SEL gt No
213. on of the temperature sensors Caution Stirringis performed underthis function only ifpreceded bythe Sample function see Sample function page 16 Important Parameters of the mask Sensor Unit of meas urement AE mV At s t min mode t max s Condition 1 Select the sensor from the recommendation menu or enter one you have installed see Section 1 2 2 Select the unit of measurement mV or As installed As installed refers to the unit of measurement you have specified for the sensor see Section 1 2 2 3 Enter AE mV e g 1 4 Enter At s e g 2 Note The drift in the electrode potential must be less than AE At 0 5 mV s during the period At 2 s if the potential is to be acquired as a measured value This occurs within a defined time interval t min and t max See representation in Section 2 3 12 2 Titration mode EQP Measure mode EQU 2 20 METTLER DL77 DL70ES DL67 02 93 EDITOR Measure 5 Select t min from the following menu a Fix Enter t min s e g 3 Instead of a fixed time you can select a condition The measured value must be greater or less than a specified set value b E gt greater than set value Enter set value mV pH c E lt less than set value Enter set value mV pH 6 Enter t max s e g 30 Note If you select 5b 5c the titrator will start the next function only when the measured potential E is greater less than the set v
214. onto the burette holder thus positioning the piston exactly Piston must project 7 mm Position of piston rod 03 03 METTLER TOLEDO DL77 DL70ES DL67 11 7 Installation instructions 11 1 2 3 Maintaining the burette parts Depending on the titrant you should clean the burette cylinder piston stopcock and tubing relatively often Slide the burette off the titrator invert it so that the stopcock points towards you and carefully take out the piston this causes the burette contents to flow out through the suction tubing waste or titrant bottle In the same position turn the stopcock through 90 clockwise and any liquid in the stopcock will flow out through the dispensing tubing waste bottle Unscrew the suction dispensing and connection tubing 1 mL burette 5 10 or 20 mL burette Unscrew the knurled screw of the burette and Unscrew the locking screw of the burette and remove the O ring from the glass cylinder using take out the glass cylinder tweezers Caution Do not misplace the centering ring of Unscrew the holder of the glass cylinder and the burette housing take out the cylinder Caution Do not misplace O ring Press the cam of the stopcock inward and lift the stopcock up and out Cam Depending on the contamination caused by the titrant rinse cylinder and tubing with acids or deion ized H O then with ethanol and finally dry the parts with oil free compressed air or vacuum Rinse the stopcock
215. or Manual Molar mass M 110 99 Equivalent number z 2 1 1 refers to the first Sample function within the method You can not change this specifi cation see also Section 3 1 2 2 You entered identification 1 which applies to all samples of this method under the Sample function Here you can modify or delete this entry see Section 2 3 2 3 You can modify the number of samples entered under the Sample function n 1 to 60 3 6 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Executing a method 4 Youcan modify the titration stand entered under the Sample function see Section 1 7 5 Enter the current temperature of the solutions to be titrated if you have not attached a temperature sensor Temperature sensor Manual 6 You can modify the temperature sensor entered under the Sample function 7 Youcan modify the molar mass M entered under the Sample function for example if you have to determine MgCl instead of CaClo 8 You can modify the equivalent number entered under the Sample function If you confirm one of the parameters of the method data mask with RUN you are shown the sample data mask see also Section 3 1 2 Sample data Sample No 1 1 ID2 Weight m g 0 0 Minimum g 0 1 Maximum g 0 2 Correction factor f 1 0 1 1 1 refers to the first Sample function and the first sample and can not be changed see Section 3 1 2 2 Enter an identification for this sample 3 Enter the weight m
216. ost common constants with the corresponding units 4 Select the result unit from the recommendation menu or enter the one you need for your calculation 5 Enter the number of decimal places that you desire in the result If you confirm one of the parameters with RUN the result will be displayed 3 34 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Method list 3 13 Method list You can add a maximum of 10 methods each with at most 60 samples to the method list These will be stored with the modified method data and entered sample data They remain stored when the titrator is turned off the data from an executed method however will be deleted You can change the order of the methods DL67 The titrator can load only one method see Section 3 1 3 13 1 Filling the method list Method Method If the method list is empty it appears together with Add the selection menu Confirm Add with RUN y SE nicined Sate Enter or modify the method identification your Method ne o name and the data entry if necessary User Data entry V A Press this key combination Method Method The method list with the entries and the selection M001 roro Add menu appears Start Sample data Method data Cut Record data Press this key Y Method entry The names you entered forthe first method
217. ou like a record of the 2nd derivative of the titration curve potential vs volume of the last sample The ordinate scale is linear Select Yes with SEL Would you like a record of the titration curve poten tial vs time of the last sample Select Yes with SEL Would you like a record of the titration curve volume vs time of the last sample Select Yes with SEL Would you like a record of the titration curve of the1st derivative volume vs time of the last sample Select Yes with SEL If you confirm one of the parameters with RUN the data are printed out 02 93 METTLER DL77 DL70ES DL67 3 33 Calculations ANALYSIS 3 10 Calculations With the aid of this function you can perform additional calculations at the end of every sample determination For this you must interrupt the method see Section 3 4 The result appears on the display it can not be printed out If you select this menu the following parameter mask appears Calculations Result name Formula Rx Constant Cx Result unit Decimal places 1 Enter the result name 2 Select the formula from the recommendation menu or enter the one you need for your calculation Caution Always enter Cx as constant 3 Select the constant from the recommendation menu or enter the one you need for your calculation Note If you press HELP you are shown for Formula the most common formulae listed with the possible units and for Constant the m
218. ought after equivalence point Theoretical considerations show that the true equivalence point with asymmetric titration curves is always between the inflection point and that branch of the titration curve with the greater curvature the smaller circle of curvature The result of the Tubbs evaluation approaches the true equivalence point very closely when the course of the titration curve is regular and allows calculation of the two branches lt _ Intersection point EQP V For the evaluation at least 6 measured points on either side of the inflection point in the region of greatest curvature are needed If the shape of titration curve does not allow calculation of the circles of curvature the titrator calculates the equivalence point according to the standard procedure You will be given an appropriate warning in the result record if this is the case 02 93 METTLER DL77 DL70ES DL67 8 21 Evaluation procedures 8 4 3 Segmented Various indication methods e g photometry conductometry and amperometry generate titration curves with linear or approximated linear sections segmented curves The titrator also evaluates such curves for you E Titration curve V AE AV 1st derivative V A E AV 2nd derivative The evaluation procedure used is based on the following consideration The first derivative of a segmented curve displays the typical shape of an S shaped curve whose inflection point represents a good approxim
219. owed 11 2 12 Additional data Housing Titration stand Dimensions Weight Power supply Fuse rating Frequency Power consumption Ambient conditions Ambient temperatare Atmosperic humidity Use Overvoltage category Pollution degree Polyester Polypropylene Width 360 mm depth 400 mm height 260 mm approx 11 5 kg with one burette drive 100 120 V or 220 240 V 10 T1 6L250V T800L250V 50 60 Hz 600 mA 300 mA 5 C 40 C Maximum relative atmospheric humidity of 80 for temperatures up to 31 C decreasing linearly to 50 relative atmospheric humidity at 40 C indoors II 2 04 04 METTLER TOLEDO DL77 DL70ES DL67 11 23 Technical data FCC Rules and Radio Interference Regulations This equipment has been tested and found to comply with the limits for a Class A digital device pursuant to both Part 15 of the FCC Rules and the radio interference regulations ofthe Canadian Department of Communications These limits ar e designed to pr ovide reasonable pr otection against har mful inter fer ence when the equipment is operated in a commercial environment This equipment generates uses and can radiate radio frequency energy and if not installed and used in accordance with the instruction manual may cause harmful interference to radio communications Operation of this equipment in a residential area is like to cause harmful interference in which case the user will be required to correct th
220. owing mask appears Save modifications Yes No If you confirm Yes with RUN the titrator stores the changed values or names If you confirm No with RUN the old remain stored The display then shows either the method functions or the master parameter mask If you press a key combination lt index letter gt to quit the Editor menu the following selection menu appears Save Yes No If you confirm Yes with RUN the titrator stores the changed method If you confirm No with RUN the old values remain stored If you do not wish to modify the parameters of a function after you have checked them quit the mask with Exit The location of the selector bar is immaterial here The values of this function remain stored 2 10 METTLER DL77 DL70ES DL67 02 93 EDITOR Save method 2 2 6 Save method After modification of each function you can save your method Press EXIT regardless of the current position of the selector bar The selection menu Save appears No Confirm with RUN The method with the modified parameters is not saved the old version is retained Yes Confirm with RUN The titrator now checks the method and if several errors are present draws your attention to the first one Confirm these messages with RUN in each case a Youareshown thelist of the method functions with the selector bar on the first incorrect function After you have corrected its parameters and saved the m
221. owing parameters Day Enter the appropriate data Month Year Hour Minute 1 36 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Miscellaneous 1 9 3 Language The titrator understands and outputs English German French Italian and Spanish Select this parameter if you wish to change the current language and you are shown the following parameter Active language Select the new language from the selection menu 1 9 4 Record header Select this parameter if you wish to enter a text that should appear on every record of a titration method You are shown the following parameter mask Text You have these two lines available for entry Text 1 9 5 Titrator ID Select this parameter if you wish to enter an identification for your titrator it will appear in every record header You are shown the following parameter Titrator ID Enter an identification 02 93 METTLER DL77 DL70ES DL67 1 37 Miscellaneous INSTALLATION 1 9 6 Routine level With the aid of this menu you set up a precondition that determines whether all people who work with the titrator should also have access to the main menus in other words be allowed to delete installation data or modify methods If for example you have temporary staff who can perform only routine analyses it is practical to block their access to several menus When the titrator is delivered you have access to all menus they are open To change this situation select
222. p of instrument specific data oooooococccccnnnnncccoccncccnnnnncnncncnnnonnnannncnnnns 7 7 7 1 2 4 Control of sequences automation RE 7 7 7 2 Configuration of the terminal DEC VT340 ooooccccccccconocccccccccnccccncccncnn 7 9 02 93 METTLER DL77 DL70ES DL67 7 1 REMOTE CONTROL 7 Remote control This section describes the REMOTE CONTROL menu provides an overview of the com munication between titrator and computer and explains the configuration of an attached ter minal REMOTE CONTROL menu You can use this menu for exclusive control of the titrator by a computer in other words you can neither enter data in the titrator nor initiate activities For this you must have e installed the computer in the installation menu under Peripherals and e loaded the DLWin software or your own program Note You will find further details in the Operating Instructions RS232C Interface Description enclosed with the RS option Computer Switch on the computer and start DLWin Titrator Confirm REMOTE CONTROL in the main menu with RUN and select On with SEL Quit the mask with EXIT The following MAIN MENU appears MAIN MENU ANALYSIS A ANALYSIS B appears only with the DL77 REMOTE CONTROL Note If e g auxiliary functions are active or methods are entered in the method list of the Analysis menu the following error message will be shown Command not possible Terminate all actions
223. parameter mask immediately 1 Select the auxiliary output from the selection menu 2 Enter the time s This is the time during which the voltage of 24 V should be applied to the auxiliary output With the aid of a pump or dispenser you can dispense exact volumes if you know the dispensing rate for the particular solvent If you confirm one of the parameters with RUN you can activate the instrument Start press 2 or RUN e At the auxiliary output the voltage of 24 V is applied for the specified time You can repeat the operation with RUN To obtain the Auxiliary functions menu again press lt index F gt 02 93 METTLER DL77 DL70ES DL67 4 21 Auxiliary instrument AUXILIARY FUNCTIONS 4 6 2 Manual If you wish to stop the function of the auxiliary unit manually press function number 2 If you press 6 2 in the Auxiliary functions menu you are immediately shown the selection menu 1 Modify 2 Start Modify press 1 You are shown the parameter mask 1 Select the auxiliary output from the selection menu If you confirm the entry with RUN you can activate the instrument Start press 2 or RUN If you know what auxiliary output is stored you can e g when in the main menu immediately start the function of the auxiliary instrument with lt index F gt 6 2 2 e The voltage of 24 V remains applied to the auxiliary output until you stop the operation with RUN or 3 To obtain the Auxiliary functions me
224. pecified conditions STIR Stir The titrator should not stir when you add the sample Y The speed 0 the time 0 so that it immediately starts INSTRUCTION with the next function Y Instruction The entered request Add sample appears STIR supported by an audio signal You confirm the instruction Y with RUN after sample addition TITRATION Stir The titrator must stir and first dissolve the added y sample The speed 70 the time 30 s CALCULATION Titration The titrator starts to execute the Titration func Y tion If you have specified a predispensing to nominal content the titrator first requests entry of the weight N 2 Series size Calculation If you have not yet entered the weight the reached titrator requests the values when it executes this function y Ve Note Ifyou add a Calculation function with R m after the STATISTICS Instruction function the titrator requests the weight y immediately RECORD 8 32 METTLER DL77 DL70ES DL67 02 93 Examples of methods 8 7 2 Method with 2 Titration functions Determination of the acetic acid and chloride contents in ketchup TITLE gt y SAMPLE Y STIR Y TITRATION Y RECORD Y INSTRUCTION Y TITRATION Y CALCULATION Y CALCULATION Y No Series size reached Y Yes STATISTICS
225. pecified equilibrium AE At the titrator will acquire the measured value and add the next increment This can be established at the earliest at t min and should be established at the latest at t max At t max the measured value is acquired at all events even if the equilibrium condition has not yet been met Examples for equilibrium conditions fast titrations slow titrations acid base titrations precipitation titrations in aqueous media in non aqueous media 1 Enter AE mV 1 0 5 2 Enter At s 1 2 3 Enter t min s 3 4 4 Enter t max s 15 30 Notes a When measuring in EQU increment addition is rapid in the flat segment of the titration curve and slow in the steep segment b The titrator acquires the time and the titrant volume together with the potential These measured values can be printed after the sample has been titrated see Section 2 3 19 Record 2 42 METTLER DL77 DL70ES DL67 02 93 EDITOR Titration EQP EQU E mV 164 163 162 161 160 159 158 157 156 155 154 153 152 151 At 2s At 2sS a ae a mv PA C Increment addition E Increment addition t s 0o 1 t min 50 1 t min 5 7 a The defined equilibrium condition has not been satisfied t min The equilibrium condition has not been satisfied after 3 s b The equilibrium condition has been satisfied after 5 4 or 6 9 s for the first time 02 93 METTLER DL77 DL70E
226. ple Sample Sample etc Stir etc Stir Titration Titration Calculation Calculation Calculation Statistics Calculation Record Calculation Record Statistics y Record Function Function Modify Cut Copy Paste Add Modify Title Sample Method ID M001 Number samples 2 Title Acid content Titration stand Stand 1 Date time 31 08 1992 13 40 Entry type Volume U 1D1 HCI Molar mass M 36 46 Equivalent number z 1 Temperature sensor Manual 2 12 METTLER DL77 DL70ES DL67 02 93 EDITOR Menu tree EDITOR Menu tree the way back The method function is saved The method is not saved Method ID METTLER methods User methods New method A A f Method ID METTLER methods User methods Method ID GR41 M001 Acid content KM59 ol stat of Gerusil M002 Titer of NaOH 0 1 mol L UB33 H3PQ in Cola drinks etc AE38 NaOH in regeneration bath etc A A A A RUN RUN RUN RUN Save Save Save No ee No No Yes Yes Yes Modify method Modify method Modify method Title GR41 Title AE38 Title KM59 Sample Sample Sample etc Stir etc Titration Calculation Record Statistics Record A Save modifications No Save modifications No Yes RUN gt lt RUN Title Method ID AE38 Number samples 3 Title NaOH in regeneration bath Titration stand Stand 1 Date time 10 10 1992 12 28 Entry type Weight m
227. ple data are deleted The command allows a new method to be loaded if you modify the identification of the old one Confirm Start with RUN The following selection menu appears not on the DL67 see page 3 4 Menu sequence Start Single method List once List continuous Confirm Single method with RUN You are shown the installed resources to check if your installation matches this information Notes a If you have not installed any resources you are shown the error message Installation data missing for e g 1 mol L AgNO3 b Ifyou have excluded the appearance of Installation data in Analysis parameters the mask Installed are will not appear see Section 1 9 8 c Up to this mask EXIT or a key combination index letter can be used to leave the menu sequence before the start of the actual titration Values entered up to this point are saved If you confirm the installation data with RUN the titrator will process the method 3 8 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Executing a method 3 1 1 Notes on weight entry a Ifyou violate the upper or lower weight limits but nevertheless confirm this entry with RUN you are shown the following message Entry outside limits Modify entry Save entry If you confirm Modify entry with RUN you are again shown the sample data mask to allow you to change the weighing If you confirm Save entry with RUN the titrator follows the menu seque
228. ppropriate description at the end of Section 1 1 2 Menu tree Auxiliary values Auxiliary value parameters H1 c ZnSO 0 1 gt Auxiliary value H1 H2 Wi 0 e ID text c ZnSOs H3 1 0 nl Value 0 1 etc Date time 00 00 0000 00 00 Enter new ID Text or let it be _ entered through titration SEENEN AARE ARAPA SEENEN SEENEN SEENEN EES Se Enter new value or let it be entered through titration Date time is entered only through titration by the titrator by means of the method function Auxiiliary value 1 24 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Titration stands 1 7 Titration stands When you select this menu you are shown the names of six possible titration stands with the specified parameters stirrer connection and default speed The names of the titration stands are permanently installed in other words you can not modify them Stand 1 Stand 2 ST20 1 sT20 2 Free stand Auto stand Stand 1 Stand 2 sT20 1 sT20 2 Free stand Auto stand Aux 50 Aux 50 Aux 50 Aux 50 Aux 50 Aux 50 is the titration stand you receive with the standard equipment of the titrator The associated stirrer is installed at auxiliary output Aux 1 is the second titration stand of a dual titration stand The associated stirrer is installed at auxiliary output Aux 1 is the first sample changer titration stand The associated stirrer is installed at
229. ps of the electrode are completely covered by solvent Never set the current higher than 1 uA Normally 0 2 0 5 uA suffice It is important to have an initial potential of at least 170 mV If not set a higher current Always switch off the current source when not in use Karl Fischer reagents With METTLER methods MKF1 MKF4 we have worked with the pyridine free KF reagents from Riedel de Haen HYDRANAL Merck Fluka and J T Baker ReAquant and used both one and two component reagents Solvents With the one component reagent methanol is used as the solvent To improve the solubility of samples we also used solvent mixtures of methanol with chloroform formamide toluene or 1 decanol In these mixtures the proportion of methanol should be greater than 50 exception with chloroform greater than 20 In the case of the two component reagent the KF solvent is used as solvent Again we have added other solvents such as methanol chloroform formamide toluene and 1 decanol The proportion of KF solvent should be above 50 in these mixtures 10 6 METTLER DL77 DL70ES DL67 02 93 Karl Fischer methods 10 2 3 Description of the four Karl Fischer methods Four methods are stored in the titrator for the KF titration 10 2 3 1 MKF1 KF Titration For the titration of the solvent pretitration or for the titration of a sample This method has two Titration functions First Titration function Rough t
230. pylene 2 set of 1400 101974 Additional glassware and auxiliary components for the titration stand Titration vessel 100 mL 7 polypropylene red set of 1400 25777 D Titration vessel 80 mL glass set of 20 101446 Titration vessel 250 mL glass set of 10 23515 F Titration vessel 5 20 mL glass 23516 Thermostatable titration vessel 80 mL glass 23517 O D Plastic cover for titration vessels set of 20 51108481 Heat exchanger for thermostating 2 9 incl adapter with taper joint 23834 D dEr Rinsing unit complete IG with titration head insert and stoppers a LBS for unused openings in titration head 23821 1 set of stoppers for rinsing unit 101230 11 32 METTLER TOLEDO DL77 DL70ES DL67 09 2002 Accessories Order No 4 Propeller stirrer y incl 2 stirring rods 25736 Ba Propeller stirring rod 101229 Micropropeller stirring rod 655073 de for titration vessel 23516 Caution Propeller stirrers for the DL40 DL21 DL25 titrators cannot be used Microfuse 11 6 L250V for 100 120 V set of 3 18560 T800L250V for 220 240 V set of 3 20182 Operating German 705093 Instructions English 705094 French 705095 Tutorial German 705096 English 705097 French 705098 Spanish 705163 Italian 705164 Memo card German 709160 English 709161 French 709162 Spanish 709163 Italian 709164 09 2002 METTLER TOLEDO DL77 DL70OES DL67 11 33 Accessories Sensors
231. r 300 measured values by leaving every second measured value in the memory At the same time it automatically doubles the time interval 13 Select a condition No Yes Enter the condition 2 64 METTLER DL77 DL70ES DL67 02 93 EDITOR pH mV stat Example of pH stating profile AV At mL s t s t max e 1 Pretitration 2 When the end point is attained the titrator waits for 5 s before outputting an audio signal and sending the message Pretitration complete Please add sample In the meantime the titrator continues to stir and exert control 3 Enter your sample and confirm the message with RUN pH stating begins Note If you have to take away the titration vessel to add the sample you can interrupt the pH stating see Section 3 4 4 The termination condition AV At has been met the pH stating is aborted Notes a The table of measured values of the record contains data of the pretitration and the pH stating If both titration steps call for more than 300 measured values the titrator stores only the measured values of the pH stating b If you require a record of the curves you receive only that of the actual pH stating You can follow the graphical representation of the pretitration only on the display 02 93 METTLER DL77 DL70ES DL67 2 65 Calculation EDITOR 2 3 14 Calculation With the aid of this function you can calculate one result R for each sample Parameters of the mask Re
232. r Pt sensors plus 1 sensor input 25872 Cable connector 8 pin DIN 89144 to be prepared as an RS short circuit plug for the DL77 to synchronize methods User data memory 25817 Se Adapter cable DIN connector banana sockets 25914 11 38 METTLER TOLEDO DL77 DL70ES DL67 09 2002 Accessories Order No Peristaltic pump SP250 with Novoprene tubes and hose clamps 51108016 Adapter cable mini DIN RCA Length 0 5 m 51108350 Novoprene tubes for SP250 1x1 m 10x120 mm 51190969 Fluorosilicone elastomer tubes 5x120 mm 51108149 Dispensing unit DU200 EU version 51370200 US version 51370210 Connection cable DU200 DL7x 51370511 Sampling unit SU24 51108018 Auxiliary output expander AOE06 51108019 Heating system DH100 7 Serial parallel converter 51108024 METTLER TOLEDO DL77 DL70ES DL67 11 39 Accessories Order No METTLER TOLEDO literature and brochures Basics of Titration 51725008 Fundamentals of Titration 704153 Guide to pH Measurement 51300047 Guide to lon Selective Measurement 51300075 Guide to Conductivity and Dissolved Oxygen 51724716 DL7O Application Brochure 1 18 Customer methods 724492 DL7O Application Brochure 2 Various methods 724557 DL7O Application Brochure 3 TAN and TBN 724559 DL7x Application Brochure 4 Gold and Silver 724613 DL7x Application Brochure 5 Determinations in Water 51724634 DL7x Application Brochure 6 Dire
233. rals you obtain a list of all peripheral units with the corresponding parameters If you select Miscellaneous you obtain a list of all submenus with the corresponding parameter values names or text 5 4 METTLER DL77 DL70ES DL67 02 93 DOCUMENTATION Data transfer 5 2 Data transfer You can use this menu to transfer the methods and installation data which you have stored in the computer to the titrator For this you must have e attached the computer to the computer interface e installed it under Peripherals in the Installation menu and e loaded the DLWin software or your own program Computer Switch on the computer and start DLWin Titrator Switch on the titrator press lt Index D gt and select Data transfer The following menu appears Data transfer Method Installation data Itis also possible to transfer the methods and installation data you have stored in Titrator 1 to Titrator 2 For this you must have e installed a computer in the Installation menu for both instruments and connected the instruments via their computer interfaces using the printer cables intercon nected by a null modem Switch on both titrators and select Data transfer in the second titrator see above Note A null modem is not included in the standard equipment The required pin assignment of the connector is thus shown in Section 11 2 11 5 2 1 Method You would like to transfer a method to the tit
234. range To identify the equivalence point you can also define a potential range For this you enter two potential values the order in which you enter them defines the tendency to specify the part of the titration curve falling or rising where the equivalence point should be located Equivalence points that lie outside this EQP range or which exhibit the opposite tendency are not registered No Yes Enter limit A mV pH Enter limit B mV pH A formula such as H2 50 or a potential stored as an auxiliary value can be entered instead of a number see Auxiliary values Section 1 6 and Auxiliary value function Section 2 3 15 E mV Limit B Limit A Tendency from A to B V mL Note The EQP range refers to the titration curve i e it is independent of the evaluation procedure 02 93 METTLER DL77 DL70ES DL67 2 49 Titration EQP Termination criteria EDITOR Termination criteria You can determine when atitration should be terminated by selecting six different parameters The titrator can abort the titration either e after the first of the selected criteria is satisfied or e after all selected criteria are satisfied e An exception is the maximum volume the titration is always terminated immediately once this has been reached Maximum volume You must enter the maximum volume mL It is intended as a safeguard If the titration is faulty excess titrant is not dispensed ne
235. rator Confirm Method with RUN the method identification mask appears Enter the ID of the desired method and confirm with RUN The message Data transmission active appears The method is added as a user method the method identification mask then reappears Caution A method with the same ID will be overwritten 03 99 METTLER DL77 DL70ES DL67 5 5 Data transfer DOCUMENTATION Error messages 1 If the method is not stored in the computer the following message appears Computer Sequence error Order code Error code E033 E037 E054 Confirm the message with RUN Error code E033 User data memory full Error code E037 Working data memory full too many resources in a block Error code E054 RESET has been pressed on the titrator which receives the data 2 If a method with the same ID is active or is stored in the method list ANALYSIS the following error message appears on the computer Command not possible Terminate all actions Delete all methods in method list ANALYSIS Confirm the error message with RUN terminate the method with RESET and or press lt Index A gt lt Index B gt and delete the method from the appropriate list Return to the documentation menu with lt Index D gt 5 2 2 Installation data For example you would like to transfer the list of titrants to the titrator Confirm Installation data with RUN the list of all resources
236. recognizes four predispensing modes Selection menu Predispensing 1 Under this selection menu you can predispense a certain volume You either enter the number of mL directly or you let the titrator calculate this if you know the nominal content of the sample to be titrated 1 Select mL and enter the volume A formula such as VDISP x 1 2 can be entered instead of a number VDISP is the volume dispensed in a preceding Dispense function 2 Select nominal content see Section 8 6 3 you must enter the following values e the metered amount in of nominal consumption e the nominal content e the conversion constant You can select this constant from the recommendation menu If you press the HELP key selector bar is positioned on Conversion constant the titrator lists the constants with the corresponding units 3 No You do not need this kind of predispensing Note The titrator dispenses the titrant in three steps 4 7 2 7 1 7 of the specified volume which allows optimum calculation of the volume increment added when a dynamic titration follows It acquires the potential values ET1 and ET2 see titration mode DOS Section 2 3 12 1 Selection menu Predispensing 2 You can predispense to either a specified potential or a specified slope of the titration curve 1 Enter the potential mV pH 2 Enter the slope mV pH mL 3 No You do not need this kind of predispensing Notes a The titrant addition in th
237. recording 2 78 3 32 Ri 2 75 sample data mask 3 10 storage 8 25 units 2 67 2 68 8 26 Result list 3 13 Result units 2 66 3 34 Rinse conditioning function 2 27 function 2 26 Rinse tip 4 7 Rinsing pump sample changer 4 18 Rinsing pump manual Sample changer 4 18 Routine 6 3 Routine level 1 38 RS232C interface pin assigment 11 23 RS option accessories 11 38 inserting 11 15 02 93 METTLER DL77 DL70ES DL67 12 7 Index s standard deviation 2 75 8 8 Safety measures for your protection 1 10 5 11 3 11 11 for operational reliability 1 Sample function 2 15 responsibility 2 16 Sample changer auxiliary function 4 16 connection 11 23 connection cable 11 38 connection scheme 1 35 installing 1 35 method series 3 46 sample series 3 45 titration sequences 3 38 3 39 Sample data entering before starting method 3 7 3 23 entering during current method 3 10 3 23 entering for List continuous 3 41 menu 3 23 printing 3 27 recording 2 77 3 32 Sample data list 3 23 3 25 Sample data mask notes 3 10 Samples maximum number 8 24 Sample series example 2 17 sample function 2 16 statistics function 2 17 with 2 sample changers 3 45 Save measured values pH mV stat fct 2 64 methods 2 11 modified current method 3 21 parameters 2 10 reevaluation 3 20 resources 1 3 1 6 with key combinations 7 Scheme method design 8 36 Segmented evaluation procedure equivalence point recognition 2 45 evaluation criteria
238. ress the HELP key selector bar is positioned on Conversion constant the titrator lists the constants with the corresponding units 3 No You do not need this dispensing mode Note With these dispensing parameters the titrator waits for establishment of an equilibrium in the solution before it acquires the initial potential ET1 It then dispenses and after reestablishment of equilibrium acquires ET2 Selection menu Dose 2 You can dispense either to a specified potential or a specified slope of the titration curve 1 When you select potential you obtain the following parameters e Potential Enter the potential mV pH e Maximum volume mL Enter the volume Itis intended as a safeguard If for instance the wrong parameters have been selected excess titrant is not dispensed needlessly 2 34 METTLER DL77 DL70ES DL67 02 93 EDITOR Titration DOS 2 When you select the slope you obtain the following parameters e Slope Enter the slope mV pH mL e Maximum volume mL Enter the volume see point 1 3 No You do not need this dispensing mode Notes a Withthese dispensing parameters the titrator dispenses dynamically with equilibrium controlled acquisition of the measured value see representation under Section 2 3 12 2 Titration mode EQP Measure mode EQU lt acquires the potential values EI and ET3 b You can link Dose 1 with Dose 2 E mV E E A nl A ET2 RES i V mL a mL or nominal co
239. riate key combination index letter Printout of the mea sured values continues To follow the measured values later on the display press lt index F gt 3 4 02 93 METTLER DL77 DL70ES DL67 4 13 Temperature AUXILIARY FUNCTIONS 4 4 Temperature With the aid of this function you can measure temperature values of solutions C F or K The measured values can be printed out Caution Temperature sensors reserved for a certain method cannot be selected This applies to e the temperature sensor being used in a current method and e all temperature sensors that will be used in the methods that have been activated with the commands List once or List continuous see Sections 3 13 3 2 and 3 13 3 3 If you press function number 4 in one of the other menus lt index F gt then 4 you are shown the selection menu 1 Modify 2 Start Modify press 1 You are shown the parameters whose value or name you can modify If you press lt index F gt 4 1 when e g in the main menu you are shown the parameter mask immediately 1 Select the temperature sensor from the selection menu 2 Select the unit of measurement from the selection menu 3 Select the titration stand from the selection menu The titrator now knows which stirrer it has to control see Titration stands Section 1 7 4 Enter the speed of the stirrer 0 100 e 0 gt stirrer is inactive e 100 gt stirrer operates at maximum speed 5
240. rocessor board When you install additional burette drives the first connector 2a is allocated to burette drive 1 the second connector 2b to burette drive 2 etc Screw on the baseplate and place the burette guides on the free openings 11 4 METTLER TOLEDO DL77 DL70ES DL67 03 03 Installation instructions 11 1 2 DV1001 DV1005 DV1010 DV1020 burettes The 5 10 and 20 mL burettes differ only in the size of their cylinder centering ring and piston whereas the 1 mL burette has a different construction its piston is longer piston guide and cylinder holder replace the centering ring of the other burettes Instead of the locking screw its glass cylinder is fastened with an O ring and a knurled nut 1 mL burette 5 10 20 mL burette Va Connection tubing DES A 14 Knurled nut 3 O ring fl Stopcock Ae Stopcock Locking screw N Ui Cylinder holder ele A 2 S TAN y Glass cylinder L JY S 4 MI J Piston Piston rod E Piston guide Protection tube Lip seal
241. rs se sescosmcenasecuynnnes cxewenenvescxseessnevenrceencense soueeteccewexnsieueexenveneade 1 40 1 2 METTLER DL77 DL70ES DL67 02 93 INSTALLATION 1 INSTALLATION In order to perform titrations the titrator must be acquainted with the titrants and their concentration the sensors with their possible unit of measurement and the solvents that it can dispense by means of pumps It must know the burette drive on which the burette is located the input to which the sensor is connected and what output carries the stirrer lt needs the names of the attached units such as a balance or printer in order to transfer data In this menu you enter and store the names of all chemical and mechanical resources you install them The most common titrants solvents and all METTLER sensors are already installed in the titrator Not only can you delete these resources or modify their parameters but you also have the possibility to install new ones List of resources Titrants Sensors Temperature sensors Auxiliary reagents Auxiliary instruments Auxiliary values Titration stands Peripherals Miscellaneous Caution All resources needed for the METTLER methods stored in the application data base are installed accordingly If you delete one of these the titrator will wait until start of titration of aMETTLER method before outputting the error message that the resource is not installed DL67 Only the titrant and the sensor for METTLER method
242. rts titrating the samples of method KvE1 the installation data are the same as for the second method When the titrator has transferred all data to the printer the results of all samples of this method are shown Note The mask Current sample is shown for each sample It is however confirmed by the titrator Stand 1 2 Free Installed are Aux 1 Stand 1 Sensor 1 DG111 SC Drive 3 0 1 mol L NaOH Current sample No 1 1 Method ID1 ID2 M001 HCI y The titrator titrates the first sample of method M001 The results of this sample are displayed if desired see Section 1 9 8 Current sample No 1 2 Method ID1 ID2 M001 HCI Y The titrator titrates the second sample of method M001 The results of this sample are displayed etc Y Current sample No 1 1 Method ID1 ID2 M002 KHP The titrator titrates the first sample of method M002 The results of this sample are displayed etc Y Current sample No 1 1 Method ID1 ID2 KvE1 H2S0O4 y The titrator titrates the first sample of method KvE1 You receive the results of this sample etc The results of all samples of this method are displayed at the end 3 38 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Method list If the titrator should process methods that use the same burette drives or sensor inputs on the ST20A ST20 sample changer in succession
243. ry instruments etc e all the associated drives inputs and outputs that are reserved for active methods under ANALYSIS A can not be used for methods under ANALYSIS B Active e is either a running Single method or e are all methods that have been started with the commands List once or List continu ous Parallel titrations can be for example performed with titration stand ST20 1 Sample series and Stand 1 Karl Fischer Using two connected sample changers you can for example determine two sample series in parallel ST20 1 and ST20 2 see Section 1 8 4 The running method s functions Record are executed sequentially e Should the titrator first process a Record function under ANALYSIS B then these data will be printed out first e If the titrator reaches a Record function under ANALYSIS A a short time thereafter it will wait with the method processing until the data under ANALYSIS B have been printed out You can change from one Analysis menu to the other at anytime using the key combination lt index A gt or lt index B gt respectively see example on the next page The Sync function can be used to coordinate methods in the method lists of Analysis menus A and B by their chronological sequence For this you need the RS option as well as an RS short circuit plug see Sync Section 2 3 20 and Operating Instructions provided with the RS option 02 93 METTLER DL77 DL70ES DL67 3 43 Parallel titrations ANALYS
244. s B x Piston E el Y Centering rin We SAN i Burette housing Wr g ring 03 03 METTLER TOLEDO DL77 DL70ES DL67 11 5 Installation instructions 11 1 2 1 Equipping the burette Lay gasket on bottle and screw on burette holder Insert stopper or a drying tube with holder Caution If you use a stopper as protection for the titrant always use the stopper with flat side Otherwise a partial vacuum forms in the bottle order no 23646 Push suction tubing into the bottle slide the red PVC tubing over the fitting as kink protection and fasten other end to left connection of burette head Screw dispensing tubing into connection at right and place burette tip in tip holder Suction tube Dispensing tube Tip holder Burette assembled Stopper Burette holder Gasket 11 6 METTLER TOLEDO DL77 DL70ES DL67 03 03 Installation instructions 11 1 2 2 Inserting the burette Slide the burette onto burette drive 3 1 with the stop of arrestment knob 2 located on left side Check that piston rod is correctly positioned in push rod 3 Fix burette by turning the arrestment knob to the right gu Wi Note Before sliding the burette onto the titrator check the exact position of the stopcock and the piston rod If the piston has been pushed too far into the cylin Position of der carefully take it out a short way Then press ZE the burette
245. s continuously and acquires the potential values of the solution undergoing change You can follow the measured values mL and mV pH on the display in the selection menu Aux function you can select the display with 4 while dispensing To stop the dispensing confirm the display with RUN and press 3 To obtain the Auxiliary functions menu again press lt index F gt 4 8 METTLER DL77 DL70ES DL67 02 93 AUXILIARY FUNCTIONS Burette Note If you carry on with the continuous dispensing but wish to process other menus in the meantime quit the display with the appropriate key combination index letter To follow the measured values later on the display press lt index F gt 1 4 4 4 1 5 Manual titration With the aid of this function you can titrate manually and follow the change in potential with the dispensing on the display To execute the function press function number 5 If you press 1 5 in the Auxiliary functions menu you are immediately shown the selection menu 1 Modify 2 Start Modify press 1 You are shown the parameters whose value or name you can change If you press lt index F gt 1 5 1 when e g in the main menu you are shown the parameter mask immediately 1 Select the titrant from the recommendation menu or enter the one you have installed see Section 1 1 2 Enter its concentration mol L 3 Select the sensor from the recommendation menu or enter the one you have install
246. s memory instantly the documentation is not interrupted immediately If the titrator is not performing any other task the following mask is displayed Terminate Documentation Printer Confirm Documentation Printer with RUN and quit the mask with EXIT The documentation is terminated definitively 02 93 METTLER DL77 DL70ES DL67 5 3 Print DOCUMENTATION 5 1 2 Installation data You can print out the following installed resources see Section 1 Titrants Sensors Temperature sensors Auxiliary reagents Auxiliary instruments Auxiliary values Titration stands Peripherals Miscellaneous If you select Titrants you obtain a list of the installed titrants with the corresponding parameters If you select Sensors you obtain a list of the installed sensors with the corresponding parameters If you select Temperature sensors you obtain a list of the installed Pt sensors with the corresponding parameters If you select Auxiliary reagents you obtain a list of the installed auxiliary reagents with the corresponding parameters If you select Auxiliary instruments you obtain a list of the installed auxiliary instruments with the corresponding parameters If you select Auxiliary values you obtain a list of the stored auxiliary values with the cor responding parameters If you select Titration stands you obtain a list of the titration stands with the corresponding parameters If you select Periphe
247. s of the numeric keypad at extreme right of keypad should be active application if key combinations should replace the num bers of the numeric keypad see following page Select Save Current Settings to save the modified parameters Press the Set Up key to quit the SET UP DIRECTORY Switch on the titrator the terminal display is now activated by the titrator 02 93 METTLER DL77 DL70ES DL67 7 9 Configuration of the terminal If you have switched off both instruments first switch on the terminal then switch on the titrator You can use the keypad of the teminal to operate the titrator The keys are assigned as follows RUN gt Do EXIT gt F17 RESET gt F20 SEL gt Select CE Remove HELP gt Help i gt Find T T gt Prev Screen T 4 Next Screen If you have saved application as a parameter for the numeric keypad the numbers are assigned to the following key combinations of the titrator Y M gt 0 MAIN MENU Y LI gt 1 INSTALLATION menu Y E gt 2 EDITOR menu 4 lA gt 3 ANALYSIS A menu ite gt 4 DOCUMENTATION menu V LF gt 5 AUXILIARY FUNCTIONS menu V S 6 Sample data list Hait gt 7 Display of the current method y B gt 8 ANALYSIS B menu U y Rinse burette V4 Y SS Rinse tip L gt DEI Line feed on the printer P gt PF2 Form feed on
248. s of the sample titrated most recently within the loop will be stored 3 Results The titrator stores all results up to the start of the next method 02 93 METTLER DL77 DL70ES DL67 8 25 Examples of formulae 8 6 Examples of formulae 8 6 1 Results R QxC m standard formula C f M z unit R Q C U standard formula C f M z unit R m VEQ c C R U VEQ c C R Q C R Q R VEQ R VEQ m R QDISP Q C m R Q His C m R Q m Hj C R ET1 2 R E 3 R pw E 1000 Content of a sample with weighing ppm mg g TAN mg KOH g mol kg mmol g Content of a sample solution g L ppm g mL mg L g 100mL mol L mmol L Titer determined using primary standard Titer determined with volumetric solution Content per sample m 1 mmol consumption as result mL consumption as result mL g as result Back titration QDISP dispensed amount of substance in mmol of the Dispense function Q mmol consumption up to the equivalence point or end point of the Titration function titration mode EQP or EP Solvent blank value incorporated in the calcula tion blank value stored as Hj Matrix blank value incorporated in the calculation mmol g matrix blank value stored as Hj Initial potential of the second Titration function as result Measured value of the third Measure function as result Anion concentration
249. s the titrator with information regarding which titration stand is used for titration The titration stand is linked with the stirrer connection and the default speed see Section 1 7 As soon as the titrator has executed the Sample function it starts to stir at the default speed If there is no Sample function in a method the titrator does not stir as it has no information regarding the titration stand A method with the Stir function but without the Sample function can not be saved for this reason In this case you can enter the command to stir via the auxiliary function Stirrer see Section 4 2 2 For the titrator the function is the identifier for the start of a series n gt 1 in other words all functions that lie between the Title function and the Sample function will not be exe cuted after titration of the first sample 2 16 METTLER DL77 DL70ES DL67 02 93 EDITOR Sample The identifier for the end of a series is the Statistics function The titrator repeats all functions within the loop Sample Statistics n times Ifthe Statistics function is missing in your method only the first sample will be titrated i e n is set to 1 Example of a sample series performed with the TLE standard method gt y SAMPLE y STIR y TITRATION y CALCULATION Y Series size reached y Yes STATISTICS y RECORD No
250. s with the DL77 Two Analysis menus A und B exist for the simultaneous execution of methods They are equivalent in terms of their build up and functionality meaning that you can start titration under ANALYSIS A or ANALYSIS B You can store 10 methods with a maximum of 60 samples in both method lists Procedure example Method Method Add A y Method ID Method entry M001 ANALYSIS A is selected Confirm Add with RUN Enter the method identification and your name User MM A etc Data entry c If you use the titration stand 1 or 2 urrent sample A h WRC confirm this mask wi No 1 1 A re Bn M001 HCI If you use titration stand ST20 1 or 2 the titrator confirms this mask Stir function The method M001 is processed You can switch Wait time s 10 A over to ANALYSIS B Speed 50 V B Press this key combination y Method Method ANALYSIS B is selected Add B Confirm Add with RUN y Method entry Method ID CALC p Enter the method identification and your name User MM etc Data entry Current sample No 1 1 B Ifyou confirm this mask with RUN the method CALC Method ID CALC Ca457 is processed ID2 3 42 METTLER DL77 DL70ES DL67 02 93 ANALYSIS Parallel titrations 3 14 1 Notes on parallel titrations a All resources titrants sensors auxilia
251. ss a key combination lt index letter gt to quit the Installation menu the modified parameters are stored automatically if the selector bar is positioned on a parameter line If itis positioned on the title line the selection menu Save modifications appears again see above 1 6 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Titrants Menu tree Titrant Selection O NaOH 0 1 mell Drive Delete da HCI 0 1 mol L Drive3 Modify TS doleisd HClO 0 1 mol L Drive ri mum_nua Add etc Titrant parameters Name NaOH Concentration mol L 0 1 Titer 1 0 Burette volume 10 mL Burette drive Drive 3 Date time 07 06 1992 12 20 Enter new name or select a entry from recommendation ar E menu with SEL ei DEE HCI HCIO SE etc gt Enter new concentration Enter new titer or let it be entered through titration Select another burette EE with SEL urette volume AS 1 mL 5 mL 10 mL 20 mL Select another drive Burette drive with SEL Drive 1 Ee Drive 2 Drive 3 Drive 4 Date time is entered only through titer determination by the titrator 02 93 METTLER DL77 DL70ES DL67 1 7 Titrants INSTALLATION 1 1 3 Add Select this command if you wish to add a titrant to the titrant list for instance NaOH of concentration 1 0 mol L or with a different burette volume or a new titrant You can also add a titrant directly to
252. st once appear List continuous y Installed are Aux 1 Stand 1 Sensor 2 DM141 SC Drive 3 0 1 mol L AgNO3 The method is processed Sample data Sample No 1 1 1D2 B1012 Weight m g 0 1346 Minimum g 0 1 Maximum g 0 2 Correction factor f 1 0 Y Current sample No 1 1 Method Di CALC Ca457 ID2 B1012 02 93 METTLER DL77 DL70ES DL67 3 11 Executing a method ANALYSIS 3 1 3 Titration sequence excerpt of the described method Y Sample data Sample No 1 1 ID2 B1012 Weight m g 0 1346 Minimum g 0 1 Maximum g 0 2 Correction factor f 1 0 Y Current Sample No 1 1 Method ID1 CALC Ca457 ID2 B1012 Stir function Wait time s 30 Speed 80 E V curve mL Results of this sample CALC Ca determination Sample 1 1 R1 1 29 46 CaClo Y Sample data Sample No 1 2 ID2 B1013 Weight m g 0 1405 Minimum g 0 1 Maximum g 0 2 Correction factor f 1 0 Y Current sample The titrator processes the method and has reached the Sample function Enter ID2 Weigh in the sample and enter the weight for the first sample or have it transferred by a balance Press RUN The titration vessel must now be attached to the titration stand The titrator stirs at 80 maximum speed and waits 30 s CaCl is dissolved during this time The run ning time is shown Th
253. sult name Formula Constant Result unit Decimal places Condition Enter the result name e g NaOH Select the formula from the recommendation menu or enter the one you need for your calculation Select the constant from the recommendation menu or enter the one you need for your calculation Select the result unit from the recommendation menu or enter the one you need for your calculation Enter the number of places after the decimal point that you require in the result Select a condition No Yes Enter the condition Notes a You have a completely free selection of parameters 2 4 and you can interlink all available parameters and numeric values see Sections 8 6 1 and 8 6 2 b The following operations are available for calculations e Addition e Subtraction e Multiplication e Division e Logarithm to the base 10 lg x e Logarithm to the base e In x e Exponential to the base 10 pw x e Exponential to the base e ex x e Square sq x e Square root sr x 2 66 METTLER DL77 DL70ES DL67 02 93 EDITOR Calculation Notes c If you press HELP you are shown for Formula the most common formulae listed with the possible units and for Constant the most common constants with the corresponding units You can have the formula as well as the constant stored as an auxiliary value and enter here as Hj e g R Ri H Hj or C Ci H Hj see Auxiliary values Section 1 6
254. t Computer 7 1 2 3 Backup of instrument specific data All instrument specific data decisive for an analysis must be stored in a central unit Such data can pertain to methods or installation and may be changed only in the titrator e g in the EDITOR On the one hand this meets GLP Good Laboratory Practice demands on the other hand problems with different versions of a method date time can be avoided if several titrators are attached to the computer Itis possible to interchange methods and installation data between the computer and the titrator 7 1 2 4 Control of sequences automation A method must be started in the computer remote control The remote control can be switched on and off in the REMOTE CONTROL menu of the titrator status On or Off On The titrator is controlled exclusively by the computer You can use the titrator only to follow the progress of the analysis shortened menu Off The Analysis working area is accessible from the computer and by you from the titrator As long as methods are entered and processed the working area remains reserved for the respective Master With the DL77 you can start a method in working area A from the computer and at the same time one in working area B from the titrator Methods are added in the computer to the method list of the titrator The method is started with List once if a method is not already running The sequence of the methods can then be s
255. t min s e g 600 c Maximum time t max s e g 1800 d Minimum consumption mL e g 0 05 e Time span s e g 120 The titration is terminated when not more than 0 05 mL titrant is consumed within a time interval of 120 s This condition can be effective at the earliest after 600 s After 1800 s the titration is terminated even if the condition has not been met 11 Enter the time limits for the evaluation a Time limit t s e g 300 b Time limit t2 s e g 1200 Note The time limits are not restricted to the values t1 and t2 entered here You can calculate for instance in additional Calculation functions e the titrant consumption between different time limits with R QSTAT 100 200 e the titrant consumption up to a different time limit with R VT 200 e the correlation coefficient between different time limits with R CSTAT 300 600 In this manner after a pH stating you can use Calculations in the Analysis menu to define new time limits for results see Section 3 12 12 Enter the time interval s for the data storage e g 10 The current measured value and the associated volume are stored every 10s The titrator can store and print out maximum 300 measured values If you have entered an interval that is too small the titrator first eliminates the values of the pretitration after 300 measured values If the limit of 300 measured values is exceeded again the titrator shortens the number by half afte
256. te You will find examples of methods in Section 8 7 02 93 METTLER DL77 DL70ES DL67 2 17 Stir EDITOR 2 3 3 Stir With the aid of this function you determine the stirring or waiting times and specify new stirring speeds Caution Iltis essential that the Stir function is preceded by a Sample function within a method see Sample function page 16 Important 1 Enter the speed of the stirrer e 0 gt stirrer is inactive e 100 stirrer operates at maximum speed 2 Enter the time s e 0 means that the titrator will not wait at all e 10 thatitwillwait 10 s before it starts the next function Itthen stirs at the specified speed in each case The running stir time is displayed 3 Select a condition No Yes Enter the condition Notes a You can set a condition for most of the functions If this is met the function is executed if it is not met the function will be skipped see Functions with a condition Section 8 3 and an additional example under the Record function Section 2 3 19 If you have not selected a condition the function is executed b The speed you have specified applies to all following functions up to the next Sample or Stir function c However during a titration you can change the specified speed see Section 3 10 Example A If you would like to continue stirring for some time after sample addition to dissolve a solid before the titrator starts the next function you must a
257. termination criteria The titration is terminated only after all the specified criteria have been fulfilled exception maximum volume see above Evaluation criteria You determine which type of calculation should be used to calculate the equivalence point found and select the jump of a titration curve or potential values that you wish to have evaluated You can combine these parameters Evaluation procedures You can choose the procedure which is suitable for the titration curve from several calculation modes see Section 8 4 Standard Evaluation procedure for all S shaped titration curves Asymmetric Evaluation procedure for S shaped highly asymmetric titration curves Segmented Evaluation procedure for titration curves with individual sections seg mented curve Minimum Determination of the minimum of a titration curve Maximum Determination of the maximum of a titration curve Select Steepest jump only No Yes Only the steepest jump of the titration curve is evaluated by the titrator Select Buffer potential 1 When a buffer potential is selected the titrator not only evaluates any equivalence points present but also the titrant consumption in mmol QP1 QP2 or mL VP1 VP2 up to the attainment of these potential values see List of designations Section 8 1 No Yes Enter buffer potential 1 mV pH A potential stored as an auxiliary value Hj or a formula can be entered instead of a number s
258. ters used without bracketed index have no meaningful connection with the method function The following designations are associated with this indexing form R C H Example R3 third result see example under indexing form 4 Note R R1 applies in other words the index 1 can be omitted This also applies to the indexing forms under points 3 and 4 8 10 METTLER DL77 DL70ES DL67 02 93 Use of indexes 3 Parameters of the form X j Index jis the function counter The following designations are associated with this indexing form E T VDISP QDISP ET1 ET2 ETS VEX QEX neq VP1 VP2 QP1 QP2 P1 P2 VTOT QTOT VTI VT2 QT1 QT2 VSTAT QSTAT CSTAT X S srel Example E 2 Measured value of the second Measure function excerpt from a method SAMPLE The titrator executes this function it starts to stir MEASURE The titrator acquires the raw result E of the first Measure function To obtain the measured value E of the first Measure function as ALCULATION ee a result set R1 E 1 DISPENSE The titrator dispenses the particular volume of a titrant The titrator stirs for a defined time before it has to measure the Sun potential of the solution Thetitrator acquires the raw result E ofthe second Measure func MEASURE f tion CALCULATION To obtain the measured value E of the second Measure function as a result set R2 E 2 02 93 METTLER DL77 DL70ES DL67 8 11 Use of indexes 4 Parameters of the form Xilj I
259. tes a and b on page 1 12 pX X represents any anion After you select pX you then enter the calibration parameters for a pX electrode or you let the titrator do it see notes a and b on page 1 12 1 10 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Sensors o Kj After you select T you then enter the calibration parameters of a phototrode unit of measurement transmission see Operating Instructions Phototrode After you select A you then enter the calibration parameters of a phototrode unit of measurement transmission The absorption A log T is calculated see Operating Instructions Phototrode us cm Afteryouselectus cm you then enter the calibration parameters of the conduc tivity cell mS cm AfteryouselectmS cmyou then enter the calibration parameters of the conduc tivity cell Note Conductivity measurements and conductivity titrations can be performed using a conductometer equipped with an analog output 3 Select the sensor input from the selection menu Notes a Caution In the standard configuration of the titrator you have the sensor 1 and sensor 2 input available You should select the sensor 1 input for all glass electrodes as this has the highest input resistance see Rear view of the titrator Section 11 1 4 and Technical data Section 11 2 1 For technical reasons only the low resistance sensor input 2 may be selected for phototrodes see Rear view of the titrator
260. that the quality management system is operated in the proper manner and is continuously updated in relation to changes brought about Certificado 180 9001 para METTLER TOLEDO La firma Mettler Toledo GmbH Greifensee ha sido inspeccionada por la Asociaci n Suiza para Sistemas de Calidad y Gesti n SQS habiendo obtenido el certificado ISO 9001 Esto acredita que Mettler Toledo GmbH Greifensee dispone de un sistema de gesti n de calidad que cumple las normas internacionales ISO serie 9000 Con motivo de las inspecciones de repetibilidad por parte de la SQS se comprueba peri dicamente si el sistema de gesti n de calidad se manipula correctamente y se ajusta de modo continuo Certificato 1509001 per la METTLER TOLEDO Il sistema di garanzia della qualita della Societ Mettler Toledo GmbH Greifensee certificato ISO 9001 sin dal 1991 dall Associazione Svizzera per Sistemi di Qualita e di Gestione SQS e cosi fornisce la dimostrazione che il suo sistema Garanzia di Qualita soddisfa i massimi requisiti ll sistema della garanzia della qualita Mettler Toledo viene verificato periodicamente SQS dando cos evidenza di un continuo aggiornamento e corretta gestione 03 99 METTLER DL77 DL70ES DL67 12 13 Declaration of System Validation We herewith inform you that the products systems DL67 DL7OES DL77 including software and accessories were developed tested and successfully validated according to the internationa
261. the following parameter mask User level Expert Press SEL gt Routine If you quit this menu with EXIT the menus you blocked under Routine level are now no longer accessible or their access is limited Only the accessible menus appear in the display under MAIN MENU under the Editor menu the METTLER and user methods are accessible for a printout only under the Analysis menu the submenu Modify method is missing The USER LEVEL menu is no longer visible To redisplay it position the selector bar on the title line MAIN MENU and enter E X P All menus reappear on the display If you wish to switch over to Expert select USER LEVEL and press SEL If you wish to make modifications in one of the menus but do not switch from routine level select the menu and modify parameters in the submenu As soonas you confirm the title line of the menu e g Installation or Editor or press lt Index M gt only the accessible menus appear in the main menu The blocked menus are opened only temporarily 02 93 METTLER DL77 DL70ES DL67 6 3 REMOTE CONTROL Contents Page 7 Remote Control 7 3 REMOTE CONTROL menu usaras aaa aaa 7 3 7 1 Communication between titrator and computer oooooccccnnnccccccccccccnnccos 7 5 7 1 1 MT aaa ees a A eee ee 7 5 7 1 2 att dee CMON WE 7 5 7 1 2 1 eener 7 5 7 1 2 2 Administration of instrument specific data cooonniccccnnnnnnnccccccccccnnnnnnanannnnnns 7 6 7 1 2 3 Backu
262. the printer 7 10 METTLER DL77 DL70ES DL67 02 93 Designations Explanations Examples Contents Page 8 Designations Explanations Examples ooooococccccccocccccccccccoconanannccncnono 8 3 8 1 List f d signations EE 8 3 8 1 1 Compilation of the raw results 8 9 8 2 Use f indexes cise ete E E EEE EA 8 10 8 2 1 Compilation of designations according to indexing forms ooooooccccccccnincccccoo 8 14 8 3 Functions with a condition 8 16 8 4 Evaluation procedures A 8 20 8 4 1 A WE 8 20 8 4 2 PS VOTING actoral EE 8 21 8 4 3 SIEI AP 8 22 8 4 4 Minimi maXinU seta liar 8 23 8 5 Restrictions in method development and execution 8 24 8 5 1 Maximum number of functions per method 8 24 8 5 2 Maximum number of samples ene 8 24 8 5 3 Maximum number of methods in the method list of the Analysis menu 8 25 8 5 4 Maximum number of equivalence points per method coooooccccccccnnnccccccccccos 8 25 8 5 5 Maximum number of measurement points per Titration function 8 25 8 5 6 Maximum number of results per method 8 25 8 5 7 How long does the titrator store data 8 25 8 6 Examples Of formulae conocio roca cnc nnnnnnnnnnn nn nnnnnnns 8 26 8 6 1 A 8 26 8 6 2 el CN 8 27 8 6 3 Nominal Coment ios 8 28 8 6 4 Formulae for limiting the equivalence point 8 31 8 7 Examples of methods oooooooooccccccccoccccocccccccccnnnanononcncnnnnn ono nnnnnnnnnnn nn nnnnnnns 8 3
263. this Title Sample Stir Titration Calculation Record function with condition table of measured values and titration curve are selected Statistics Record 02 93 METTLER DL77 DL70ES DL67 2 79 Record EDITOR TITLE gt y SAMPLE STIR TITRATION No Y CALCULATION y Record gt Output Unit eee eee Printer Cond RECORD Table of measured values Yes E V CUVE coonocccnnnccccnnncnnnnancnnns Yes Condition a a Yes y Condition ooococccconocacinicccncnno neq 0 Termination after record Yes N 7 Condition satisfied Series size reached d Yes ae STATISTICS 1 The table of measured values is recorded 2 The titration curve is recorded 3 The method is aborted RECORD 2 80 METTLER DL77 DL70ES DL67 02 93 EDITOR Sync 2 3 20 Sync Under this function you specify the parameters for the synchronization of the titrator with an external control unit The synchronization takes place via the system interface 1 Select the synchronization mode Send or Send Wait a In the synchronization mode Send the titrator transmits the numeric code you have defined to the external control unit and then begins to process the next method function immediately b In the synchronization mode Send Wait the titrator transmits the numeric code you have defined t
264. ting format 1 36 12 2 METTLER DL77 DL70ES DL67 02 93 Index Date specification auxiliary values 1 23 methods 2 14 sensors 1 12 temperature sensors 1 15 titrants 1 6 Decimal places 2 66 3 34 Default speed 1 26 2 16 Default values 1 4 2 10 Delay 2 54 2 55 Designations compilation 8 14 explanation 8 3 Dispense auxiliary function 4 7 function 2 24 Dispenser sample changer 4 20 Dispense continuously 4 8 Dispensing rate 1 18 Display analysis menu 3 28 DK102A polarization current source 10 6 DOCUMENTATION 5 3 DOS dispense 2 34 Dose 1 2 34 Dose 2 2 34 Dosing pump sample changer 4 19 Dosing pump manual sample changer 4 20 Drift compensation 10 12 Drift Karl Fischer titrations 10 7 potential measurement 2 20 temperature measurement 2 22 DYN titrant addition EQP 2 40 Dynamic titrant addition EP 2 55 EHNV half neutralization value 2 36 8 5 Electrodes METTLER 1 9 E potential 2 20 8 3 EDITOR menu 2 3 menu tree 2 12 2 13 End point mode EP EPA 2 56 EPR 2 56 EPS 2 56 End point mode pH stat EPA 2 63 EPS 2 63 End point range 2 55 End point titration 2 53 EP end point titration 2 53 EPA absolute end point 2 56 2 63 EPOT 2 36 8 5 EPR relative end point 2 56 EPS other end point 2 56 2 63 EQP equivalence point titration 2 36 EQP range 2 49 EQU equilibrium controlled measure mode 2 42 Equilibrium controlled measured value acquisition 2 42 2 55 Equivalence point s explanat
265. tion Calculated result Calculation constant Titer function Titer Auxiliary function Auxiliary value Statistics function Mean value Standard deviation Relative standard deviation in Current method Elapsed time of a current method in seconds see Sections 3 1 3 and 10 2 7 8 8 METTLER DL77 DL70ES DL67 List of designations 8 1 1 Compilation of the raw results Method Function Raw results Printed if Raw results last sample is selected in the Record function Current method no MEASURE E TEMPERATURE T DISPENSE VDISP QDISP TITRATION ET1 ET2 ET3 VEQ Q VEX QEX EPOT EHNV neq P1 P2 VP1 QP1 VP2 QP2 pH mV STAT VTOT QTOT VT1 QT1 VT2 QT2 VT QT VSTAT QSTAT CSTAT Note To obtain the raw results which are not printed out by default assign them to the result R e g R QP1 R VTI 12 93 METTLER DL77 DL70ES DL67 8 9 Use of indexes 8 2 Use of indexes Since functions can occur more than once within a method and also parameters can appear repeatedly within a function the parameter designation must be qualified by indexes The titrator recognizes 4 different indexing forms 1 Parameters without index The following designations are associated with these parameters c t m U M E f TIME The parameters always refer to the current titrant the current sample or the current method 2 Parameters of the form Xi All parame
266. tion In addition the slope from measurement pointto measurement point must increase or decrease If this condition is not met this iterative procedure can not be employed In such cases the determination relies on interpolation of the inflection point of the titration curve You will be given an appropriate warning in the result record E Inflection point 8 20 METTLER DL77 DL70ES DL67 02 93 Evaluation procedures 8 4 2 Asymmetric With markedly asymmetric curves the standard procedure can lead to a systematic error The difference between the true equivalence point and the inflection point can then be greater than the precision normally achievable For such cases the titrator is equipped with an evaluation method following Tubbs 2 This empirical approximation method is an old established procedure for the evaluation of asymmetric titration curves recorded in an analog fashion lt can also be used for digital determinations of titration curves 3 The result of the Tubbs evaluation is closer than the inflection point to the true equivalence point The evaluation procedure is based on the following considerations Both branches of the titration curve possess a circle of curvature with minimum radius that can be drawn in The ratio of the two radii is determined by the asymmetry of the curve The intersection point of the straight line connecting the midpoints My and Mo of the circles with the titration curve represents the s
267. tion Dispense continuously 14 Manual titration 15 2 i Stirrer 2 gt Aux function Sensor 3 3 gt Temperature 4 Sample changer Lift 51 4 1 Litt A A Tabie toward 2 1 Modify Turntable forward 52 3 Tunable backward 3 Turntable backward 53 4 Rinsing pump RM Rinsing pump 54 5 iia pump manual gt Rinsing pump manual 55 gt osing pump m 7 Dosing pump manual fe Dosing pump SS 8 Dispenser gt Dosing pump manual 57 6 aSa Dispenser 58 Auxiliary instrument 4 Ki e 2 Time controlled 61 7 a Manual 62 Calibration 7 8 Offset adjustment 8 SNOLLONA3 AYVITIIXNV AUXILIARY FUNCTIONS Notes a With the following key combinations the two auxiliary functions Rinse burette and Rinse tip can be executed even faster lt Index U gt Rinse burette Press 1 2 3 or 4 to select the burette drive The burette is rinsed lt Index Y gt gt Rinse tip Press 1 2 3 or 4 to select the burette drive The burette tip is rinsed b Once one of the auxiliary functions has been executed you can quit the selection menu Aux function 1 Modify 2 Start with EXIT The next higher menu will appear or with a key combination index letter The selected menu will appear c Should several auxiliary functions be active such as Sensor at titration stand 1 and Stirrer and Burette Dispense at titration stand 2 and you would like to stop all three press RESET The following display will appear Termi
268. titration vessel A newly installed titration vessel is still not completely dry after the pretitration Note If the titration vessel is already conditioned you can immediately perform the drift determination MKF2 Allow method MKF3 to run until the drift is stable This normally takes 2 hours We recommend letting the standby titration run overnight Note For the standby titration to follow the pretitration automatically enter methods MFK1 and MFK3 in the method list select titration stand Auto stand instead of Stand 2 see Section 1 7 and start List once With the DL67 this is not possible Terminate the standby titration with RESET Start the drift determination MKF2 Note You should perform drift determinations fairly often to check the value 02 93 METTLER DL77 DL70ES DL67 10 9 Karl Fischer methods 10 2 5 2 Procedure B Pretitration drift and titer determination After the first drift determination empty the titration vessel add 40 mL methanol or KF solvent see Note a in Section 10 2 3 4 and start method MKF 1 to titrate the solvent to dryness Start method MKF2 to check the drift Start method MKF4 to determine the titer of the KF titrant Notes a The concentration of the KF titrant has been set at 5 mol L corresponding to 5 g H20 L The titrator does not recognize the unit g L for titrants b To achieve good reproducibility the initial weight of sodium tar
269. to enter an asterisk or a question mark after the first second or third letters numbers of the method ID replaces all subsequent letters numbers For example x results in the display of all methods with an ID beginning with this letter or number replaces one letter or number within the ID For example xy z will result in the display of all methods with an ID containing these three letters numbers METTLER methods When you select this option you receive a list of all methods stored in the application data base with the identification and the name of the method M001 Acid content M002 Titer of NaOH 0 1 mol L etc If you select M001 for instance the method is masked on the right by the following selection menu Print Modify 02 93 METTLER DL77 DL70ES DL67 2 5 Select methods EDITOR User methods If you select this you are shown alist of methods with the identification and name of the method if you yourself have stored a method in the user data memory e g KM59 pH stat of Gerusil UB33 H3P04 in cola drinks If you then select a method it is masked on the right by the following selection menu Print Delete Modify New Method If you wish to develop a new method select New Method You are shown the standard method with the following functions Title Sample Stir Titration Calculation Statistics Record All parameters of the functions except those of the Title fu
270. to the connected output unit already these are printed out written b If the titrator is executing several activities e g auxiliary functions they are interrupted and displayed too see Section 4 Note c 02 93 METTLER DL77 DL70ES DL67 3 15 Fade out method ANALYSIS 3 3 Fade out current method If you wish to enter sample data during atitration or wish to modify the stirrer speed or the curve type of the representation Titration or pH mV stat function press EXIT The following selection menu appears DL77 DL70ES DL67 see Section see Section Method Method Add 3 1 3 13 1 Interrupt 3 4 Interrupt 3 4 Sample data 3 7 Sample data 3 7 Display 3 9 Display 3 9 Stirrer 3 10 Stirrer 3 10 Method data 3 8 Method data 3 8 Record data 3 8 1 Record data 3 8 1 The titration continues to run in the background Italso continues to run if you use the required key combination index letter to select another menu To fade in the titration again press lt index T gt If the titrator is still processing the Titration function the curve or table of measured values for example appears on the display if not the method function is displayed that the titrator is processing at the time DL67 Jumping to other menus are impossible during a titration You can only select menus i e the commands in the selection menu The following key combinations are possible e lt index
271. trant with the titrator its value is entered here together with the date automatically see Titer function Section 2 3 16 Select the burette volume from the selection menu Selection menu You press SEL position the selector bar on for instance 5 mL in the selection menu and confirm with RUN The selection menu disappears and 5 mL now follows burette volume Select the burette drive from the selection menu 02 93 METTLER DL77 DL70ES DL67 1 5 Titrants INSTALLATION DL67 It is only possible to select one of two burette drives for this titrator If more than two drives have been installed the titrator will recognize each of the first two counting from left to right 6 You can neither delete nor overwrite the date lt refers to the titer determination of the titrant using the method function Titer and is entered here together with the time automatically see Titer function Section 2 3 16 Note As soon as you change a titrant parameter the date and time are deleted The titrant with the modified parameters is installed when you quit the parameter mask with EXIT Here the selector bar can be positioned on any parameter but not on the title line If you confirm the title line with EXIT the following selection menu appears Save modifications Yes No If you confirm Yes with RUN the titrator stores the modified values or names If you confirm No with RUN the old values remain in force Note If you pre
272. trate should be 0 09 0 12 g 0 1 mg see also Section 10 2 4 c Inthe titer determination you must take into account the limited solubility of sodium tartrate in methanol and chloroform In 40 mL methanol you can perform max 4 titer determinations In 1 1 mixtures of chloroform methanol the titer determination with sodium tartrate is not possible since it does not completely dissolve The solubility of sodium tartrate is very goodin the KF solvent of the two component reagent d If methods MKF1 MKF2 and MKF3 e are entered in the method list e Auto stand is defined as the titration stand see Section 1 7 and e List once is started the titrator executes the pretitration followed by the drift determination Afterwards it will start the standby titration To determine the titer after this terminate the standby titration with RESET For the DL67 this is not possible 10 2 5 3 Procedure C Pretitration drift determination and titration of a single sample Add 40 mL methanol or KF solvent see Note a in Section 10 2 3 4 and start method MKF1 to titrate the solvent to dryness Start method MKF2 to check the drift Then immediately start method MKF1 to determine the water content of the sample Notes a If you interrupt the individual determinations you should start the MKF3 standby titration to ensure that the titrant vessel remains free from water b To achieve good reproducibility the sample shoul
273. tration pH mV stat Calculation Auxiliary value Titer Calibration Statistics Record sync 02 93 METTLER DL77 DL70ES DL67 2 3 EDITOR The individual functions comprise parameters whose values or names can be modified When you develop a new method you are always shown the standard method with default parameters which you can then modify to suit your needs see New Method Section 2 1 Method print eing delete modify cut copy paste add modify modify Parameter You modify a method by changing its functions You modify a function by changing its parameters You will find the representation of the Editor menu tree at the end of Section 2 2 2 4 METTLER DL77 DL70ES DL67 02 93 EDITOR Select methods 2 1 Select methods You are shown the following submenu in the Editor menu Method ID METTLER methods User methods New method Under method ID you can call up all stored methods under METTLER methods only those in the application data base and under user methods only those methods available in the user data memory Method ID The method identification is a 4 character alphanumeric identifier of a method If you know it select Method ID see Title function Section 2 3 1 Enterthe method ID and confirm with RUN The entry will be masked by the following selection menu Print Delete appears only after ID entry of a user method Modify Note Itis possible
274. ts CRIS Customer Requirements 03 99 METTLER DL77 DL70ES DL67 12 15 D claraci n de validaci n del sistema Por la presente le informamos que los productos sistemas DL67 DL7OES DL77 incluido el software y los accesorios han sido desarrollados probados y verificados con xito de acuerdo con las reglas sobre ciclo de vida de producto de Mettler Toledo GmbH Analytical Estas reglas se basan en la norma 9001 1994 Los puntos de control de proyecto han sido comprobados y ratificados por el grupo de Control de Proyecto Project Supervisory Group o PSG La comprobaci n de los productos sistemas se ha realizado antes de su entrega Como apoyo a las exigencias GLP y de validaci n ponemos el siguiente material a disposici n de las personas autorizadas para su examen e Imagen del producto e Especificaciones e Documentaci n del proyecto e Especificaciones del software e Plan de calidad e Directiva Gesti n de Proyecto e Plan de ensayos e Datos del servicio postventa y de deseos del cliente e Protocolos de revisi n e C digo fuente Mettler Toledo GmbH Analytical conservar la propiedad de todo el material y sus reproducciones y llegar a un acuerdo de confidencialidad con quienes quieran examinar este material Labr ho MP LA Schwerzenbach Dr Bernhard Grob Dr Urs Spitz Marzo 1999 General Manager Manager Business Area Business Unit Analytical Titration 12 16 METTLER DL77 DL70ES DL67 03 99
275. tween the electrode signal at the start and end of the titration Enter EPR mV pH E mV pH TENDENCY positive mV negative pH TENDENCY negative mV 300 Start potential positive pH 200 EPR 310 mV pH 5 2 100 End potential EPA 30 mV pH 7 5 100 V mL 3 Select EPS other end point Enter the end point e g H2 This end point can be stored as auxiliary value Hj and you can call it up here see Auxiliary value function Section 2 3 15 and Auxiliary values Section 1 6 Example Assuming you have stored the value of EPOT of Hau at 1st equivalence point under H2 and you would now like to titrate to this potential enter H2 You can also enter a formula such as E 200 Eis the measured potential of a preceding Measure function 2 56 METTLER DL77 DL70ES DL67 02 93 EDITOR Titration EP Tendency Tendency A titration exhibits a positive or negative potential or pH change see illustration This has to be specified by you Select Positive or Negative Caution A positive potential change means a negative pH change Maximum volume You must enter the volume mL It is intended as a safeguard If the titration is faulty excess titrant will not be dispensed needlessly 02 93 METTLER DL77 DL70ES DL67 2 57 Titration LEARN EQP EDITOR 2 3 12 4 LEARN EQP Learn titration equivalence point determination If you are not sure what paramet
276. u receive the titrator no unit is installed Printer Not installed Balance Not installed System Not installed Sample changer Not installed 1 8 1 Printer If you wish to attach a printer you have to install it Select Printer and you are shown the follow ing parameter mask Status Not installed Printer type LX800 Paper Fanfold Paper format 81 5 11 Automatic form feed No Frame lines Straight Baud rate 2400 Parity Even Number data bits 8 bits Number stop bits 1 stop bit 1 Select the status with SEL Not installed or Installed 2 Select the printer type from the selection menu e LX800 EPSON ESC P command language e HP Deskjet HP PCL IIl command language e DICONIX 180si extended IBM Proprinter command language e IBM IBM Proprinter command language e Diabolo 630 ASCII characters 3 Select the paper with SEL Fanfold or Single sheet e Single sheet A form feed is forced at the end of a page Ifyou select Yes for Automatic form feed see Parameter 5 a header and a footer will be printed on each page of the record 1 28 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Peripherals 9 Caution Do not activate the printer s line feed or form feed functions if you have selected Automatic form feed for the Single sheet paper mode On the titrator the following key combinations will activate the printer functions lt index L gt causes a line feed lt ind
277. umber depends on the evaluation procedure e Measurement points from a predispensing are not considered Evaluation procedure Earliest possible Measurement EQP at points necessary Minimum Maximum 4th measurement point Standard 4th measurement point Asymmetric 4th measurement point 10 Segmented 5th measurement point 8 An example for the evaluation procedure Minimum If the third measurement point lies in the vicinity of the lowest potential value it will not be recognized as an equivalence point You must or can assist the recognition using two parameters Threshold To prevent small disturbances in the curve being identified as an equivalence point you must specify a threshold value mV pH mV pH mL or mV pH mL2 This must be exceeded Note a Themaximum value of the threshold should not exceed half the expected maximum value of the first or second derivative at the equivalence point 02 93 METTLER DL77 DL70ES DL67 2 45 Titration EQP Threshold EDITOR Note b The maximum or minimum the maximum of the absolute values of the 1st deri vative and the maximum of the absolute values of the 2nd derivative of a titration curve all depend on so many factors solvent concentration sensor type of reaction etc that you can not define the right threshold value until you have performed the first titration You can enter one of the following values for this Evaluation procedure
278. using your thumbs Place option in housing next to analog board 3 First fasten option to housing with two screws 4a amp b then with three screws 4c d e Plug connection 5 of cable of RS option into connector 6 of analog board 7 is the connector for the next option see next section Note When you install this option you should adjust the sensor input see Section 4 8 Offset adjustment of the sensor inputs 03 03 METTLER TOLEDO DL77 DL70ES DL67 11 15 Installation instructions 11 1 7 Temperature option 1 sensor input 2 temperature sensor inputs Setting We have set the temperature option to Pt1000 sensors by default If you perform temperature measurements with Pt100 sensors you must alter the setting prior to installing the option Pt1000 Pt100 Remove all double jumpers on the pin bases 1 2 3 4 and replug one pin to the right of the original position the option is now set for Pt100 sensors 5 is the connection cable 6 the connector for the next option 11 16 METTLER TOLEDO DL77 DL70ES DL67 03 03 Installation instructions Inserting Insertion of the temperature option corresponds to that of the RS option see Section 11 1 6 implying that you can insert either one or the other option Slide burettes off titrator and unscrew the baseplate The titrator must be
279. utput of the titrator 1 Selectthe name of the auxiliary instrument from the recommendation menu or enter one you have installed see Section 1 5 2 Enterthe time s ltindicates how long the voltage should be applied at the auxiliary output A formula may be entered instead of a number for example H5 2 H5 is a time increment which has been saved as an auxiliary value see Section 1 6 3 Select a condition No Yes Enter the condition 02 93 METTLER DL77 DL70ES DL67 2 31 Titration EDITOR 2 9 12 Titration Under this function you determine the mode control and evaluation of a titration Depending onthe titration mode the titrator acquires several measured values and volumes as raw results see List of designations Section 8 1 and Measure function Section 2 3 4 If you have selected a temperature sensor in the Sample function the temperature of the sample solution is measured automatically before the titrator executes this function If no sensor is attached parameter Manual the titrator adopts the temperature entered at the start of the method The slope of the pH electrode is then corrected for the temperature in the pH value calculation see Section 4 7 Calibration of the temperature sensors Parameters of the mask Titrant Concentration mol L sensor Unit of meas urement Titration mode Condition 1 Select the titrant from the recommendation menu or enter one you have installed see Se
280. utputs Aux 1 2 and 3 One auxiliary output of the titrator is normally assigned to the stirrer e g Aux 1 see Section 1 7 You should thus select only Aux 2 and or Aux 3 for this auxiliary reagent see Technical data Section 11 2 2 If you have attached the sample changer ST20A or ST20 this unit offers you two addi tional outputs called RINSE and DOSE The auxiliary reagent with the modified parameters is installed when you quit the parameter mask with EXIT see the appropriate description at the end of Section 1 1 2 1 4 3 Add Select this command when you wish to add an auxiliary reagent to the list You can also add an auxiliary reagent directly to the list by pressing the lt gt plus key You are always shown the following mask Name H20 Dispensing rate mL min 250 Auxiliary output Aux 2 1 Select the name from the recommendation menu or enter the reagent you wish to install Note If you install several auxiliary reagents with the same name you must provide each one with a different flag to allow the titrator to distinguish between them e g H20 2 2 Enter the dispensing rate mL min of the device 1 18 METTLER DL77 DL70ES DL67 02 93 INSTALLATION Auxiliary reagents 3 Select the auxiliary output from the selection menu The auxiliary reagent with the appropriate parameters is installed when you quit the parameter mask with EXIT see the appropriate description at the end of Section
281. w to enter sample data for methods while List continuous is being processed mV E V curve Method M001 is running To enter the sample data for method HPO4 mL SS S A press this key combination Method list gt MO01 roro HSO4 roro HPO4 roro Confirm the last method with RUN y Method Method gt M001 roro Add HSO4 roro Sample data Confirm Sample data with RUN HPO4 roro Method data Cut Record data Y No ID2 Wt vol 1 1 0 0000 g Confirm first line with RUN 1 2 0 0000 g 1 3 0 0000 g Sample data Sample data Sample data Sample No 1 1 Sample No 1 2 Sample No 1 3 ID2 PS 389A ID2 PS 389B ID2 PS 389C Weight m g 2 4871 gt Weight m g 2 543 Weight m g 2 2671 Minimum g 2 0 Minimum g 2 0 Minimum g 2 0 Maximum g 3 0 Maximum g 3 0 Maximum g 3 0 Correction factor f 1 0 Correction factor f 1 0 Correction factor f 1 0 D ser D Y T Enter the second identification the correction y factor if necessary and the weight and confirm mV E V curve with RUN the sample data mask for the second then for the third sample appears z L To follow the titration course of the method again 2 press lt lndex T gt 02 93 METTLER DL77 DL70ES DL67 3 41 Parallel titrations ANALYSIS 3 14 Parallel titration
282. ynchronized only with the computer Entries which need a method during an analysis are requested from the computer by the titrator e g Current sample gt The sequence status e g List processed and the error status e g Short circuit is sent to the computer The most important auxiliary functions must be initiated at the computer These are Rinsing a burette Dispensing Measuring a potential steady state Stirring Auxiliary instrument time controlled Entering a titer Entering an auxiliary value LE LJ This results in a wide range of additional remote control possibilities 02 93 METTLER DL77 DL70ES DL67 7 7 Communication Titrator lt gt Computer External operations should be synchronized with the sequence of an analysis This synchro nization is explained in what follows with the aid of a few examples 1 When you work at the computer your attention must be drawn to any result calculated during the analysis that lies outside the limits Thetitrator sends an appropriate signal to the computer The computer shows you the message corresponding to this signal 2 Inaddition to the titrator the computer controls e g a robot The task of the robotis to insert the samples in the titrator The titrator has to tell the computer when the next sample should be inserted and wait until this has happened Request to continue The computer for its part knows when the robot has inserted t
283. you quit the parameter mask with EXIT see the appropriate description at the end of Section 1 1 2 Menu tree Temperature sensors TEMPA Pt100 TEMP B Pt100 TEMP CG Pt1000 TEMP D Pt1000 Temp 1 Temp 2 Temp 1 Temp 2 Temperature sensors _ gt Name aes Sensor type Sensor input es Zero point C Date time TEMP A Pt100 Temp 1 0 00 00 0000 00 00 through calibration Enter new zero point or let it be entered Date time is entered only through zero point calibration by the titrator METTLER DL77 DL70ES DL67 02 93 INSTALLATION Auxiliary reagents 1 4 Auxiliary reagents When you select this menu you receive the installed auxiliary reagents with the specified parameters dispensing rate and auxiliary output An auxiliary reagent is a solvent that is dispensed using atime controlled device e g adiaphragm pump or an electromagnetic valve You will find the representation of the menu tree at the end of Section 1 4 3 H20 250 mL min Aux 2 CH30H 250 mL min Aux 2 CHC13 250 mL min Aux 2 etc DL67 Only auxiliary reagent H20 is stored in the DL67 You can however add auxiliary rea gents to the the list see Section 1 4 3 If you select H20 for instance the list is masked on the right by a selection menu containing the following commands Delete Modify Add 1 4 1 Delete Position the selector bar on this comma
284. you use the auto stand the mask Current sample will not appear This means that the next sample determination will be started without a RUN confirmation Thus you can assign the sample changes for each method to a robot c If you have attached the sample changer the titrator titrates the samples of all methods without the need for you to intervene A requirement here is that e all sample data have been entered e the methods use the same resources or that their installation data are specified on different drives titrants and inputs sensors see comparison of the titration sequences on the next page 02 93 METTLER DL77 DL70ES DL67 3 37 Method list ANALYSIS Comparison of the titration sequence for several methods at the titration stand ST20 1 ST20 2 or at Stand 1 2 or a free stand Method roro roro KvE1 roro Start Single method List once List continuous M001 M002 ST20 1 Installed are Aux 1 ST20 1 Sensor 1 DG111 SC Drive 3 0 1 mol L NaOH Y Current sample No 1 1 Method ID1 ID2 M001 HCI The titrator titrates all samples in method MOO After completion it waits until all data have been transferred to the printer and starts titrating the samples in Method M002 the installation data are the same as for the first method After completion the titrator waits until all data have been transferred to the printer and sta

Operating Instructions METTLER TOLEDO DL77 / DL70ES / DL67

Contents

Download Pdf Manuals

Related Search

Related Contents