Operating Instructions Titration Unit TitroLine easy
Contents
1. Time Time Name Name Result 337 mV Result 257 mV Total consumpt Doe Total consumpt 4 30 ml Result 2 084 ml 4 305 Fig 15 Fig 16 8 2 Connecting a computer The titrator can be connected to a PC using a cable of the TZ 3098 type The functions of the titrator can be remote controlled using the set of commands below The commands can be sent to the titrator using so called terminal programs and the responses of the titrator can also be followed on the screen 49 8 3 Commands set The commands of the titrator are to be interpreted as ASCII characters The commands use only capital let ters All commands have to end on lt CR gt lt LF gt The lt CR gt lt LF gt characters correspond to the ASCII char acters 13 and 10 of the ASCII character table Command Response Action VE Version 99 01 Output of the version number RH Ident TitroLine easy Hardware identification RC Last command Repeat last command RA UNIT 20 ml Inquire size of unit SH Y Stop titration SM Y Start selected method SR Y Stop burette SS7 0 Send desired pH value prior to EP titration to TL easy FP Y Measurement function in pH range FV Y Measurement function in mV range FT Y Measurement function in temperature range M Measurement value Inquire measurement value within set range LC Output calibration parameter LR Output of results printout LD Output data EX Y EXIT function return to execution level BF Y B2. intervals of 10 seconds Used in difficult titrations 6 mV fast strong Fast titration with steep jumps Example lodometry with thiosulphate as titration agent 7 mV fast flat Fast titration with flat jumps Example Chloride under favourable conditions with large quantities of silver nitrate 8 mV exact strong Accurate titration with steep jumps Example Titrations with KMnO or Cerium 9 mvV exact flat Accurate titration with flat jumps Example Chloride under normal or difficult conditions 10 mV0 1 ml 10 sec Linear titration in equal increments of 0 1 ml at repeated regular in tervals of 10 seconds Used in difficult titrations or titrations in which other parameters fail From a basic menu EP EQ Man an extended depression of the lt F3 gt key gt 3 sec will take you to the lt setting gt menu Another short depression of the lt F3 gt key the screen will change to lt select parameter re cord gt This menu can be used to invoke the individual methods using the arrow keys To select the desired method press the lt F1 gt key Pressing the lt F2 gt key will take you to the Standard pH titration method whereas the lt F3 gt key leads to the Standard mV titration method 42 4 8 Manual titration Manual titration can be used to carry out any titration to a change of colour without using an electrode To do so press the lt F3 gt key to switch the titrator to the manual titrat
3. The reagent bottle is empty Replace or refill the reagent bottle The hose is not immersed deeply Immerse the hose deeper in the bottle or fill up reagents enough in the reagent bottle Hoses of the dosing unit are mixed up Exchange hose connections The dosing unit is not properly locked Lock the dosing unit by a quarter rotation at the lower position Air bubbles in the titration system The valve is defective Exchange 3 2 way valve The hose connections Check Has the hose been pulled out of threaded connection are not tight Screw hose manually on Replace hoses including threaded connections When setting on a new dosing unit the piston rod is not properly pulled in the device rattles Inclined piston rod Set on piston rod vertically again Titration solution is not titrated dosed The dosing unit is not properly filled Perform initial filling Lock dosing unit in the lower position by a quarter rotation properly locked to the right Fig 20 The hose or the titration tip are Check clear passage through hose and titration tip The system contains air bubbles Please refer to Air bubbles in the dosing system Undissolved parts in the titration Filter or replace titration solution solution The data transfer to the printer computer does not work Set transfer parameters properly ettings 4800 baud 7 data bits no parity no handshake Are you using a suitable cable sea TZ 3095 for the pri
4. EQ lt START gt neutral red lt F1 gt rince calibrate The Rinsing function can be started in this status only If a key other than lt F1 gt is pressed the display will switch to lt FILL gt A receptacle with a volume of at least 100 ml has to be placed under the burette tip since titration solution will escape The Titration Unit TitroLine easy will perform two take in and dosing operations It will display lt lt device rinsing gt gt The rinsing operation can be stopped by pressing the lt STOP gt key the Titration Unit TitroLine easy will remain in this position Using the lt FILL gt key a normal filling process can subsequently be started If it is intended to rinse the unit between individual titrations it has to be switched off an then on again The display will show lt lt rinsing lt F1 gt gt again Changing different titration solutions is impossible in this way GJ chapter 11 1 Changing the titration solution 4 4 Filling For normal filling or refilling press the lt FILL gt key e g after an interruption of a filling or rinsing process The filling process will be performed automatically with the display showing lt lt device fills gt gt 40 4 5 End point In this mode you can titrate to a set pH end point Using the lt f gt and lt gt keys you can set the end point by scrolling from pH 0 0 and pH 14 0 As soon as the end point of a colour indicator is reached the name of
5. Part 3 has to be verified Use interruptions gt If the titration unit is not being used over a longer period of time the liquids contained in the system have to be removed and the titration unit has to be flushed out with distilled water If this is omitted the piston may be destroyed and the Titration Unit TitroLine easy will become untight If the liquid is left in the system one has to reckon with corrosion and an alteration of solutions used over the time Since the state of the art does not provide plastic hoses which are absolutely free of diffusion occurrences these precaution measures apply in particular to the hose line section Cleaning gt The titration unit can be cleaned using a moist piece of cloth with normal household cleaning agents gt The bottom and rear side have to be treated dry In no case must liquid penetrate into the interior of the titration unit 52 11 Replacing the dosing unit disassembly and installation As a rule the need for replacing the dosing unit occurs only rarely The dosing unit has to be replaced if such a replacement becomes necessary as a result of a defect or of an inspection of the titration unit The dosing unit is equipped with lateral ribs around its circumference with one of these ribs being in double design This double rib serves as a mark for the correct placement of the dosing unit GQ Fig 17 Pos 2 resp Fig 19 Pos 2 Important note The disassembly of the dosing
6. according DIN 19 266 Part 3 Display Calibration Connections Electrode Reference electrode Temp Meas Sensor Stirrer Interface RS 232 C RS 232 C interface Power supply Casing material Front foil Casing dimensions Weight Climate 33 SCHOTT Matrix LCD with 64 x 128 pixel and background illumination contrast adjustable using knurled know J 3 8 keyboard display automatically using 2 out of 8 possible buffer solutions Standard buffer solutions according to DIN 19 266 and NBS or with integral pH values pH 2 00 4 00 4 01 6 87 7 00 9 18 10 00 12 45 DIN socket according to DIN 19 262 or BNC 1 x 4mm socket Resistance Thermometer Pt 1000 2 x 4mm sockets and 1 x 2 mm socket Plug connection in the casing bottom for Stirrer TM 96 low voltage for the TM 96 put in by the Titration Unit TitroLine easy for connection of a printer or a computer PC with serial interface RS 232 C fixed settings 4800 baud word length 7 bits 2 stop bits no parity corresponds to Protection Class Il according to DIN EN 61 010 Part 1 not suitable for use in hazardous environments Mains 230 V 50 60 Hz or 115 V 50 60 Hz modification inside the device Power draw 24 VA Polypropylen with flame shield Polyester 135 x 310 x 205 mm w xh x d including dosing unit without stirrer approx 2 2 kg Environmental temperature 10 40 C for operation and storage Humidity according to E
7. cases and cannot be predicted without knowledge of the specific case Therefore the replacement of titration solutions must always be performed under the supervision of experts who ensure the correctness of the future analyses If the decision to change the titration solution has been made the first thing to do is to remove the dosing unit as it is described in chapters 11 1 or 11 2 respectively If possible the residue of the titration solution should be removed by hand by carefully pushing the projecting piston rod towards the hoses When doing so more liquid will leak out of the titration tip and the residual volume is furthermore reduced Removing the old titration solution can be accelerated by moving the piston rod of the dosing unit positioned top down The suction hose is then immersed in the new solution or in water as intermediate liquid By moving the pis ton several times in both directions pumping the previous liquid is gradually replaced by new liquid Sub sequently the dosing unit is set on again according to the description in chapter 11 1 and 11 2 12 Storage transportation and environment If the titration units are to be stored temporarily or transported the best solution to protect the devices is to use the original packing In many cases the original packing will no longer be available so that an alterna tive packing has to be put together Welding the titration units in a foil is an advantageous solution Prior to this i
8. design the Pt 1000 banana plug connects to the Pt 1000 sockets directly next to the Ref socket or beneath it e Indicator electrodes glass electrodes without reference electrode connect to the Electrode socket and the separate reference electrode connects to the Ref socket 3 7 Switching on off connections pH electrode Temp meas sensor with 2 mm plug Reference electrode with 4 mm plug Temp meas sensor with 4 mm plug Manual key button Printer computer PC Mains switch on off Fig 10 Connections on the back panel 3 8 Keyboard display contrast Fig 11 Keyboard with manual key button accessory All functions of the Titration Unit TitroLine easy are triggered using the keyboard The display indicates in dialogue mode which active keys can be pressed to proceed with the work If a manual key button is con nected the Start Stop and FILL functions can also be started using the manual key button The contrast of the display can be adjusted using the knurled knob which is accessible at the right bottom front of the Titration Unit TitroLine easy 39 4 What is to be noted before starting 4 1 Setting the language of the country The titration units are set ex works to the desired language If a different language is to be set the lt SET gt key on the start menu has to be kept depressed for more than 3 seconds On the lt lt s
9. immersed into the sample with the diaphragm of the electrode be ing fully immersed A standard value of 30 mm will suffice for this immersion e The stopper at the filling hole of the electrode has to be removed not applicable for electrodes without fill ing hole e All plugs have to be plugged in properly e No hoses must be wrinkled or contain air bubbles 43 5 Titration with the Titration Unit TitroLine easy device ready device ready pH endpoint lt START gt auto find EQ lt START gt pH 7 0 lt v gt lt l gt gt neutral red rinse lt F1 gt rince lt F1 gt calibrate lt CAL gt ee calibrate lt CAL gt Mode EQ EP Man lt SET gt KKK device ready Manual titration mode 0 00 m Display example showing a method start a termination and a regular end of the titration START STOP 4 analysis EQ runs 1 23 pH 4 56 ml lt STOP gt a Manual termination of the Regular end of titration using lt STOP gt the titration analysis EQ ready STOP bebe analysis interrupted bai kk total mi 5 67 lt lt Start menu gt gt 44 6 Calibration with the Titration Unit TitroLine easy Rinse electrode without protection cap with water and start calibration Dip electrode into the first buffer until the junction is covered The display shows lt lt please wait gt gt during buffer identification In the next step which is
10. interrupt Press longer Lo IL Lr 45 FILL SET F3 CAL F2 FILL SET F3 Set cal parameters to default kk kk Setting Lanquage kkkkkk F1 gt F2 gt F3 gt F4 gt Ko lt STOP gt FILL 1 Setting the German language 9 REKK Setting Initialize calib Buffer 1 7 00 lt gt el lt SET gt lt STOP gt kkkk Setting Initialize calib Buffer 2 4 00 lt gt lt T gt lt SET gt lt STOP gt lt t gt lt gt other buffer lt SET gt memorize lt STOP gt interrupt 7 1 kk kk Setting Status page 1 2 Analysis EEEE Method none End of analysis EP pH 7 0 Manual temp 25 0 C Status page 2 2 lt F5 gt Status page 2 2 Calibration pH 7 00 pH 4 00 100 1 pH 7 0 Status page 1 2 lt F5 gt lt STOP gt Formula 2 Input value Vol B F1 F2 F3 Q F1 0001 000 F2 kkk lt F1 gt lt F2 gt lt F3 gt lt F4 gt lt F5 gt lt STOP gt 0001 000 F3 0001 000 Q 0001 000 B 0000 000 J ia Calculation formula Vol B F1 F2 F3 Q F1 0001 000 lt gt lt gt lt F1 gt lt SET gt lt STOP gt increase value D reduce value F1 selection place SET memorize STOP interrupt 46 Setting calculation formula and input v
11. unit as such is only possible using a special tool TZ 3630 and should only be done by experienced persons The sealing lip of the PTFE piston and the sealings of the liquid system may be damaged or incorrectly positioned in the course of such a disassembly As a re sult titration liquid would leak in unwanted places Caution Wear protective glasses Runoff gt Press the lt FILL F1 gt key for five seconds and keep it depressed until the display shows lt lt change of the dosing unit gt gt Caution place a receptable under the titration tip A When the piston moves upwards titration solution will be dosed out of the burette tip gt If lt lt unlock unit gt gt is displayed the dosing unit has to be unlocked by rotating it by rotating it by 90 to the left counter clockwise Fig 17 gt Press lt START gt The motor of the Titration Unit TitroLine easy will now automatically move the dosing unit upwards After the display shows lt lt remove unit set on new unit gt gt remove the dosing unit CQ Fig 18 The process is completed Detaching the dosing unit Placement of the dosing unit Fig 17 Unlocking Fig 18 Removal Fig 19 Placement Fig 20 Locking gt Set on new inspected if necessary repaired dosing unit vertically When doing so the M double rib C4 Fig 3 must point at the position 2 of the casing marking Subsequently switch the Titration Unit TitroLine easy on The running motor will now pu
12. 2004 Bottle set for titration agent with brown glass bottle TZ 2007 Bottle set for titration agent with square Duran bottle TZ 2008 Bottle set on with S 40 thread for reagent bottle e g Merck make TZ 2005 Bottle set on with GL 45 thread for reagent bottle e g Riedel de Ha n Schott make TZ 3025 Stirrer TM 96 with PTFE stirring rod TZ 3460 Printer with RS 232 C interface incl printer cable TZ 3095 1 5 m data cable RS 232 C with plug for printer connection 1 side 4 channel mini DIN plug 2 side 25 channel sub miniature D socket TZ 3098 Data cable set 1 5 m data cable RS 232 C 1 side 4 channel mini DIN plug 2 side 9 channel sub miniature D socket Adapter 9 channel plug gt 25 channel socket TZ 3680 Manual key button Spare parts TZ 3000 valve TZ 3280 hose set TZ 3630 mounting wrench TZ 3660 electrode titration tip holder TZ 3665 stand rod TZ 3680 manual key button TZ 3130 dosing unit 20 ml complete assembled 55 14 Elimination of disturbances The display does not respond to keys being pressed the display is dark The internal program is disturbed Switch the device off and switch it on again after 10 seconds e g by electrostatic loading or a mains overvoltage The display contrast is misadjusted Use the knurled knob at the right sid of the bottom to adjust the contrast The stirrer does not work The connection contacts are dirty Clean contacts The dosing unit is not properly filled
13. 29 Operating Instructions Titration Unit TitroLine easy CONTENTS PAGE 1 Properties of the Titration Unit TitroLine C sy ccccseseeeesseneeeeseeneeeeeeeneeeeseceeeeeeseeneeenseeeeenseneeeenes 30 Tt taton SOMMONS 3 2 2 cescks e E caceud bene teen teparevaed ch ceva EAA EE A EEE EN 30 2 Warning and Safety information cccceseeeeeseseeeeeeeeeeeseeeseeeeeseseeeseeseeeeeseseeneeseseseeeseseseeusesesseeesenseenens 34 A Setting and COMMISSIONING ccceseseeeeeeeeeeeeeeeeee ee eeeeeeeeeeeeeeeenaceeeeenseeeeeeesseeeeseseseeeeeseseeeeeesesenseesenees 35 3 1 Unpacking and setting up of the Titration Unit TitroLine easy 35 3 2 Installation of the stprer 2000 ENEE tiririka nana dh REENEN ee AEN ENEE edu 35 3 3 Installing a Eu EEN 35 3 4 Installing the burette tips is s cdi ceca AEN EEN AEN AEN Nee EE KAREN 36 3 5 Installation of the manual key button and the printer computer PC accessories 100sneeeesne 37 Ap Connecting the electrode EENEG neddhennedeedhtend dedi ENEE 38 3 7 Switching on off connections cece ce ceeeeee cece cee e ee teeeeeaeee cnet ee saeaanaeceeeeeeedeceaaeaeeeeeeeeeeeeieeeeeeess 38 3 8 Keyboard display contrast 38 4 What is to be noted before Starting ccccccesseeeeseseeeeeeeeseeeeeseeeeeseseseeesesesneeesesesneeseseeneesesesnensnnesenens 39 4 1 Setting the language of the country eceee centr ee ette ee erent ee ee tates ee eaeeeeetaeeeeesaaeeeseenaeeeeeenaeeeeeaes 39 4 2 Titratio
14. Dosing accuracy DIN EN ISO 8655 Part 3 or better typical systematic error lt 0 1 random error lt 0 05 according to table 1 DIN EN ISO 8655 Part 3 Volume display 00 00 50 00 ml with a resolution of 0 01 ml Measuring input The built in measuring inputs enable the following sensors to be connected pH single rod measurement chain pH single rod measurement chain with integrated temperature sensor and or temperature measuring sensor Resistance Thermometer Pt 1000 electrode with an mV signal between 1400 and 1400 mV with built in reference electrode or separate reference electrode Measuring input pH mV input with 12 bit transducer for accurate resolution during the titration Connection electrode socket according to DIN 19 262 or BNC socket and reference electrode 1 x 4 mm socket Measuring l Display Accuracy l Input resistance range resolution without sensor Q SEI 0 01 0 05 t1digt gt 5e10 1400 1400 1 l 1 digit gt 5 10 Measuring input Connection of temperature measuring sensor for Resistance Thermometer Pt 1000 connection 2 x 4 mm sockets and 1 x 2 mm socket Measuring Display resolution Accuracy range without sensor 20 115 0 1 0 5K 1 digit Accuracy indicated in terms of measuring incertainty with a confidence of 95 In addition the measuring incertainty of the sensor has to be taken in account as well For instance it is for pH electrodes A pH 0 012 0 03
15. N 61 010 Part 1 maximal relative humidity 80 for temperatures up to 31 C linear decrease down to 50 relative humidity at a temperature of 40 C S registered trademark for SCHOTT GLAS Mainz 34 2 Warning and safety information The Titration Unit TitroLine easy corresponds to protection class II It was manufactured and tested accord ing to DIN EN 61 010 Part 1 Protective Measures for Electronic Measurement Devices and has left the factory in an impeccable condition as concerns safety technology In order to maintain this condition and to ensure safe operation the user should observe the notes and warning information contained in the present operating instructions Development and production is done within a system which meets the requirements laid down in the DIN EN ISO 9001 standard For reasons of safety the Titration Unit TitroLine easy must be opened by authorised persons only this means for instance that work on electrical equipment must only be performed by qualified specialists A In the case of nonobservance of these provisions the Titration Unit TitroLine easy may constitute a danger electrical accidents of persons or fire hazard Moreover in the case of unauthorised in tervention in the Titration Unit TitroLine easy as well as in the case of negligently or deliberately caused damage the warranty will become void Prior to switching the device on it has to be ensured that the operating voltage of the Titration Un
16. alue Calculation Set formula Input value Set unit kk kk kkk k Units _ according to the calculation formula lt F2 gt or lt F1 gt kkk Input value Weight F1 Vol F2 0001 000 lt F1 gt 0001 000 lt F2 gt 001 0000 lt F4 gt lt STOP gt Calculation formula Weight F1 Vol F2 Fi 0001 000 lt t gt lt gt lt F1 gt lt SET gt lt STOP gt T increase value D reduce value F1 selection place SET memorize STOP interrupt Calculation formula Formula 1 lt F1 gt Weight F1 Vol F2 Formula 2 lt F2 gt Vol B F1 F2 F3 Q No formula lt F3 gt lt STOP gt CAL F2 47 7 2 Setting mV titrations In addition to pH titrations the Titration Unit TitroLine easy is capable of performing mV titrations EQ and EP titration methods can be performed in analogy to the pH titrations The upper line of the display shows the current measurement value pH or mV until the value does not change any more over a period of two minutes Subsequently the display will change to READY EQ and EP titrations are possible You can perform a equivalence point titration with automatic detection EQ or an end point titration to a defined end point EP In contrast to pH titration the calibration menu item is no longer necessary If the lt SET gt key is held depressed for
17. as to be carried out gt Once per quarter the electrical contacts plugs stirrer manual key button have to be inspected for cor rosion if the titration unit is used in premises with an occasional occurrence of corrosive matters in their atmosphere gt If there is suspicion that a solution is attacking the glass excessively the maintenance intervals are to be reduced accordingly In case of disturbances gt If a disturbance a malfunction or another defect becomes obvious the maintenance work has to be car ried out immediately gt Ifit has to be assumed that A safe operation is no longer possible AA please refer to chapter 1 Warn ing and safety information Maintenance work to be carried out Check whether humidity has penetrated below the dosing unit To do so remove the dosing unit chapter 3 Fig 1 to 4 resp Fig 7 to 10 If humidity can actually be found there one can conclude that the piston in the cylinder is no longer tight Check the hoses the threaded connections and the seals for visible damage contamination and leak age Installation of the screw connections Fig 11 Check the electrical plug in contacts for corrosion and mechanical damage Defective parts have to be repaired or replaced by new parts Defective glass parts have to be replaced in any case gt gt After each maintenance process the measurement technical reliability according to DIN 12 650 Part 6 or Part 7 or ISO DIS 8 655
18. ectrode defective or too old gt electrode not enough immersed ERROR 1 lt STOP gt gt wrong titration reagent gt electrode has not overtaken the pH value of the sample gt electrode defective gt already titrated sample titration quit error message kkk START STOP device ready pH end point lt START gt wd TS pH 7 0 neutral red fill lt FILL gt 51 10 Maintenance and care of the Titration Unit TitroLine easy To retain the function of the Titration Unit TitroLine easy the following inspection and maintenance work are to be carried out Note on wear and tear In a larger sense the valve and the glass cylinder are parts being subject to wear and tear this means that their glass surfaces may wear down in use This wear and tear may lead to an adulteration of the dosed volumes For this reason the dosing accuracy of the device should be checked Maintenance intervals Normal operation gt As a rule the max intervals for carrying out all maintenance work are 3 months In the case of special load Special load is present if for instance solutions are used which are suitable to attack glass e g solutions containing alkali fluoride or phosphate or if the average use exceeds 40 titrations per day Once per month the dosing unit has to be inspected visually in order to check damages and in addition a test according to DIN 12 650 Part 6 or Part 7 or ISO DIS 8655 Part 3 h
19. eight of chlorine F2 100 conversion F3 1000 conversion weighed in quantity g to mg Q 1 no conversion required B 0 no blank value in the case of concentrations of this kind The units are selected using the arrow keys Available options ml mmol l mol l ppm g l mg l n To store the setting press lt SET gt lt STOP gt will take you back to the formula selection window 7 3 Working with internal methods The memory of the titration contains 10 different methods which can be selected if necessary please refer to chapter 4 7 These methods include various practice based parameter settings for titration To start titration as usual simply press the lt Start gt key 48 8 RS 232 interface The serial interface connects a printer equipped with a serial interface or a computer to the titrator The in terface is bi directional and is used for result printout or communication with computer programs For de tails please refer to the following chapters 8 1 Connecting a printer The results are automatically output via the RS 232 interface To record the results a printer with a serial interface can be used We recommend the use of a TZ 3460 printer Upon the end of titration the following information is transferred to the printer Printout mV titration EQ Printout mV end point titration KKK KK KKK KKK KKK KK KK kk kk kk kkkkkkkkkkkkkkkkkkkkkk kk Sample number 1 Sample number 1 Date Date
20. etting gt gt Set ting menu press the lt F1 gt key to select a different language lt F1 gt German lt F2 gt French lt F3 gt English lt F4 gt Spanish If you do not wish to change the set language exit the menu by pressing the lt STOP gt key 4 2 Titration solutions standard solutions It has to be ensured in context with all titrations that the suction hose immerses in the titration solution in the storage bottle and that the titration solution is drawn off free of gas bubbles If the Titration Unit TitroLine easy has to be filled first the Rinsing Initial filling working sequence has to be started by pressing the corresponding key A receptacle with a volume of at least 100 ml has to be placed under the burette tip since titration solution will escape It should be noted that the titration solution contained in the hoses may vary by diffusion of the components of the air in the case of long standing times In case of doubt rinsing of the system should also be started in the Rinsing initial filling sequence 4 3 Rinsing and initial filling After switching the unit on press the lt F1 gt key to start the Rinsing initial filling working sequence Start menu Start menu Start menu End point titration Equivalence point titration Manual titration device ready device ready device ready manual titration mode PH end point lt START gt pH 7 0 lt l gt lt ts auto find
21. igh precision glass cylinder and the spindle for the piston feed The controlled three two way valve the easy to read consumption display with ist additional status messages the stand stirrer system and the practical manual key button make the Titration Unit Titro Line easy a device with a comfortable use properties 1 1 Titration solutions To save titration solution and to render the disposal of the chemicals after the analysis as simple as possi ble we recommend to select any titration solutions consumption between 5 ml and 15 ml for titration Solutions to be used In practice any solutions and liquids with the viscosity of lt 10 mm s can be used such as e g non aqueous titration for example perchloric acid in glacial acetic acid However chemicals attacking glass PTFE or FEP or which are explosive such as e g hydrofluoric acid sodium acid or bromine must not be used Suspensions with a high solid contents may block or damage the dosing system General rules The respectively applicable safety guidelines on handling chemicals are to be observed under all circum stances This applies in particular to inflammable and or etching liquids 31 SCHOTT KONFORMITATSERKLARUNG DECLARATION OF CONFORMITY DECLARATION DE CONFORMITE Nous d clarons sous notre seule responsabilit que le We declare under our sole responsibility that the Wir erkl ren in alleiniger Verantwortung dak das Produkt products produit Tit
22. ion mode The addition of the titration agent is done using the keys of the manual keying unit The left i e violet key controls the addition of the titration agent Normal titration OU Fig 12 J e Immerse the titration tip in the sample solution This 1 will increase the accuracy Press the violet key to the first stage The titration so lution will be dosed slowly as long as the key is held depressed 0 01 ml titration stepwise titration QQ Fig 13 Press shortly violet key max 0 3 s 0 0 ml will be ejected each time the key is depressed again The display shows the volume Fast titration Fig 14 Press violet key fully to second stage and keep de pressed The titration solution will be dosed as long as the key is being depressed Fig 14 4 9 Calibration When calibrating the electrode using the Titration Unit TitroLine easy a classic 2 point calibration is per formed with one buffer solution being close to the zero point of the electrode and a second being in the acid or basic range e g pH 7 00 and pH 4 00 This calibration is described in chapter 6 Calibration 4 10 What should not be forgotten e The intake hose has to be immersed in the titration solution e An appropriate stirring speed has to be selected in order to ensure proper mixing of the sample e The burette tip and the electrodes are
23. it TitroLine easy matches the mains voltage The operating voltage is indicated on the specification plate Nonobservance of this provision may result in damage to the Titration Unit TitroLine easy or in personal in jury or damage to property If it has to be assumed that safe operation is impossible the Titration Unit TitroLine easy has to be put out of operation and secured against inadvertent putting to operation In this case please switch the Titration Unit TitroLine easy off pull plug of the mains cable out of the mains socket and remove the Titration Unit TitroLine easy from the place of work Examples for the assumption that a safe operation is no longer possible gt the package is damaged the Titration Unit TitroLine easy shows visible damages gt the Titration Unit TitroLine easy does not function properly gt liquid has penetrated into the casing The Titration Unit TitroLine easy must not be stored or operated in humid rooms For reasons of safety the Titration Unit Titroline easy must only be used for the range of application described in the present operating instructions In the case of deviations from the intended proper use of the device it is up to the user to evaluate the occurring risks A The relevant regulations regarding the handling of the substances used have to be observed The Decree on Hazardous Matters the Chemicals Act and the rules and information of the chemicals trade It has to be ensured on
24. ll the dosing unit downwards If any noise should be come audible at this point please stop the process immediately by pressing the lt START STOP gt key The cause of this rattling noise will be eliminated by setting the dosing unit vertically on again Si As soon as the dosing unit moving downwards has reached the edge of the casing the display requests you to lock the dosing unit manually by rotating it by 90 to the right clockwise Fig 20 gt After locking it start the rinsing and initial filling process using the lt FILL F1 gt Rinsing F1 key 11 1 Replacing the titration solution If titration solutions are to be changed since differing analysis methods are used one should first consider whether the time required for frequent changes is not more expensive than the acquisition of another dos ing unit As a principle and in the case of all piston burette systems a substitution of the titration solution by another one involves mixing and carry over processes The reason for this is the dead volume above the piston in the cylinder and in the hoses The disturbances to be anticipated are the greater the more the new solution differs from the previous type and concentration In the case of highly different solutions the first substitution liquid rinsing should be distilled water and the new titration solution should be filled in only subsequently 53 The possible disturbances are very much different in the individual
25. more than five seconds the Setup menu will appear Use lt F3 gt to change between mV and pH mode Pressing the lt STOP gt key will take you back to the main and start menu The calculation formulae and the unit of the result can be selected using the lt F4 gt key To switch over to the calibration menu use the lt F4 gt key Here you can set the temperature manually To change from the Setup menu to select calculation press the lt F4 gt key This item can be used to se lect two formulae enter the values and select a unit for representation on the display lt F1 gt is used to display the formulae for making a selection The first formula lt F1 gt serves for titer deter mination and hence contains the weighed in quantity in the numerator The lt F1 gt factor can be used for molarity conversion F2 can be used for the molecular weight The lt F2 gt formula 2 serves for contents de termination and takes into account a blank value of B as subtractive member Using lt F3 gt you can switch calculation off After selecting the formula you can enter the individual numeric values To enter the factor of F1 you have to select this factor using lt F1 gt then use the lt FILL gt key to determine the place to be set Using the arrow up and arrow down keys adjust the digits until the proper value is being displayed Example chloride percentage with 1 mol l solution F1 35 45 mol w
26. n solutions Standard soluttons ee ceeceeeeeteee ee eeee ee erent ee ee eaaeeeeetaeeeeesaeeeeetieeeeeenaeeeeeeaes 39 4 3 Rinsing ang imitial MING BEE 39 KE OTT KEE 39 AND HEET DER genee ed Eege dee sede eeh 40 AG EquivalenCeDOmnt sie e leie Eege eege DEE dee ee eege A0 e 8 Ge Ee EIB Lee EE 41 AO Manoa Trator AAT E E A TET A A IRRI OE 42 Bees CATO EE 42 4 10 What should not be forgotten essiri eorna R A TR RE O RA TE N 42 5 Titration with the Titration Unit TitroLine easy ssssuusseenunnnnnnnnnnnnnnnnnnnnnunnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnn na 43 6 Calibration with the Titration Unit TitroLine eaSy ssessusseununeennnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnn na 44 7 Settings nra a a aAA E NANNAN AENEA rA AEA Ka E AA ENa AEAN 45 7 1 Setting calculation formula and input value eee cece ee eeeeeeeeeeeeeeeeeeeeeaeeeseeeaeeeseeeaeeeseeaeeeeteeaaees 46 Ta Settings KLEES 47 Ta Working with internal Methods AAA 47 D RS 232 interface EENEG EENEG aaa A aAa AAN AKEn Eaa ANE a a 48 8 1 Connecting a printer ee KNNEdE riiet i aa a eb bended a ieie aei ai aaa 48 8 2 Connecting a computer 48 83 Commands set ENEE ieia eiiie ia Ea ea ei niti E eieaa er TEE a iaai EA EtA 49 8 4 Properties of the RS 232 interface cccccececeecnececeeeeeeeceneaeeeeeeeeeeeecacaeceeeeeeeseccacaeeeeeeesesessaaeeeeeess 49 9 Eror messagi E 50 10 Maintenance and care of the Titration Unit TitroLine eaSy sssssusssenunseennnnnnnnnnnnnnnnn
27. nalysis It con trols the titration and the used recorded measurement values to calculate the completion of the titration Unless the analysis specification contains a statement on the end point we recommend to titrate in the Auto Find EQ mode As soon as the unit has completed the titration automatically the ml result will be calculated and shown on the display In the case of automatic end point search the displayed consumption will always be slightly above the result since automatic calculation requires some overtitration In this automatic mode a calibra tion of the electrode is not necessarily required and rather serves for checking the condition of the elec trode 41 4 7 Internal methods The titrator features 10 internally stored methods A list and description of the individual methods if given below No Name Description 1 pH fast strong Fast pH titration for strong acids and bases Example Hydrochloric acid with caustic soda 2 pH fast weak Fast pH titration for weak acids and lyes Example Citric acid acetic acid or tartaric acid with diluted caustic soda 3 pH exact strong Accurate pH totration for strong acids and bases Example Hydrochloric acid with caustic soda 4 pH exact weak Accurate pH titration for weak acids and lyes Example Citric acid acetic acid or tartaric acid with diluted caustic soda 5 pH 0 1 ml 10 sec Linear titration in equal increments of 0 1 ml at repeated regular
28. nnnnnnnnnnnnnnn 51 11 Replacing the dosing unit disassembly and installation cccssseeeeeeeseeeeeeeeeneeeeeseneeeneeseeeees 52 11 1 Replacing the titration solution 52 12 Storage transportation and environment ceeeeeeee eee ee ee ee eee seen ee ee ee seneeeaeeeeeeeeeeseseesseaneeeeeeeneees 53 13 Scope of delivery accessories and Spare Parts ccccceceeeeeseeeeeeeeeeeeeeeeseeeeeeeeeseneeeseeeeeeeeeeeneees 54 14 Elimination of disturbances ccccceeeeneeeeeeee ee eeeecen seen eeeneeeeeeeeeeeeseaeeeeeseaeeeeeseeeeeseaseeneeeaseeeeeenseeeeenees 55 Version 040107 E 30 1 Properties of the Titration Unit TitroLine easy Note on disclaimer of liability The measurement or analysis results depend on a multitude of factors So please verify the plausibility of the measurement or analysis results on a regular basis accompanied by appropriate reliability tests In this regard please adhere to the usual methods With the Titration Unit TitroLine easy it is possible to perform all common titrations The most important prerequisite for accurate titration is the accurately functioning dosing technology In ad dition to the high precision glass cylinder made of DURAN borosilicate glass the virtually play free spindle ensure correct titration results All parts coming into contact with the titration and dosing solutions are made of chemically resistant materi als Analysis accuracy is guaranteed by the h
29. not illustrated here wait until the buffer value is stable After this procedure rinse the elec trode with water and dip into the second solution If calibration is done slope and zero point are shown If a wrong buffer is recognised calibration can be repeated lt lt Start menu gt gt Calibration buffer 2 Calibration CAL buffer 1 F2 calibration buffer 2 calibration buffer 1 4 00 pH 7 00 pH rinse electrode and electrode in buffer 2 buffer 2 4 00 lt START gt put electrode in buffer 1 lt gt Display lt l gt lt START gt actual buffer values calibration buffer 2 4 00 pH please wait lt STOP gt calibration buffer 1 7 00 pH calibration please wait lt STOP gt electrode parameters slope 100 0 zero point pH 7 0 calibration lt lt Start menu gt gt calibration end 7 Settings lt lt Start menu gt gt F3 than 3s REKK Setting Lanquage Calibration Titration mV Calculation Status Selection param set lt F1 gt lt F2 gt lt F3 gt pH fast strong Standard pH Standard mV lt t gt lt gt lt STOP gt REKK KREKK Setting Calibration Set buffer 1 lt F1 gt Set buffer 2 lt F2 gt Reset calparam lt F3 gt Temp manual lt gt el lt SET gt lt STOP gt lt l gt 25 1 25 2 25 3 lt gt 24 9 24 8 24 7 lt SET gt memorize lt STOP gt
30. nter ora TZ 3096 3097 for the PC Are the cables properly connected he lower socket is the RS 232 C interface Check cable connection are the screws on the PC side tightened C COM 1 and COM 2 possibly were mixed up Defective cable Replace cable Are the cables properly connected Switch the devices off switch them on again after 10 seconds
31. rator Titration Unit Titrateur TitroLine TitroLine TitroLine easy easy easy auf das sich diese Erkla rung bezieht bereinstimmt mit den Normen und mit dem normativen Dokument to which this declaration re lates is in conformity with the standards DIN EN ISO 8655 Teil 3 and the normative document Technische Daten Titrator TitroLine easy 13 Dezember 2000 SCHOTT Instruments GmbH Hattenbergstrasse 10 55122 Mainz auquel se r f re cette d claration est conforme aux normes et au document normatif Deutschland Germany Allemagne 07 Januar January 07 07 Janivier 2004 AGQSF 0000 A068 01 040107 32 SCHOTT Translation of the legally binding German version Technical data of the Titration Unit TitroLine easy State December 13 2000 Conformity DIN EN ISO 8655 Part 5 Conformity mark Al CE mark C according to the Council Directive 89 336 EMC electromagnetic compatibility generic emission according to standard EN 50 081 Part 1 generic immunity according to standard EN 50 082 Part 2 according to the Council Directive 73 23 EMC low voltage directive Country of origin Made in Germany Propriety rights Patents for the valve system and the titration regulation are applied for Burette parts Cylinder 20 ml DURAN borosilicate glass cylinder UV protection Protective coating material Ultem 1000 amber Valve Motor driven 3 2 way valve made of PTFE ETFE Hoses FEP with UV protection
32. ssembly Cut of hose end evenly Guide hose through shaft Pak wo N gt Push burette tip with pressed in hose onto the shaft Fig 7 Assembled burette tip bn Kg stop hose Slip parts of the threaded clamping joint on to the hose Press burette tip onto the free hose end until it reaches the stop Hold tip firmly and screw threaded clamping joint to the shaft 37 3 5 Installation of the manual key button and the printer computer PC accessories violet key grey key E el Care e RS V The manual key button is only required for manual titration It can also be used for a remote control for the lt START STOP gt violet key and lt FILL gt grey key with automatic titrations Caution The two 4 channel sockets on the side of the unit are identical If the sockets are mixed up the electronics of the Titration Unit TitroLine easy may be damaged Fig 9 Upper socket manual key button lower socket printer computer PC 38 3 6 Connecting the electrode e Single rod measurement chains connect to the Electrode DIN socket If the unit is equipped with a BNC socket according to the user s specification the electrode with the BNC plug connects to the same loca tion e Electrodes with integrated Temperature Measuring Sensor Resistance Thermometer Pt 1000 the elec trode plug DIN or BNC plug connects to the electrode socket and depending on the electrode
33. t has to be made sure that no liquid is left in the dosing unit If the titration unit is to be sent to a service shop it is necessary to indicate the titration solution last used on the accompanying documents or on the piston burette Otherwise the service shop will dispose of the parts damaged or to be replaced as special waste at the charge of the customer The room selected for storage should provide the following conditions gt temperature between 10 and 40 C for operation and storage gt humidity according to EN 61 010 Part 1 maximal relative humidity 80 for temperatures up to 31 C linear decrease down to 50 relative humidity at a temperature of 40 C Although you will use your titration device for a very long time so that the following information comes far too early But if your system has reached the end of its life please observe the regulations applicable for your land and town as to its disposal 54 13 Scope of delivery accessories and spare parts Delivery scope gt Basic device TitroLine easy gt Dosing unit 20 ml TZ 3130 including hoses and screw connectors fitted ready for use on the titration device gt Stand Rod TZ 3665 including 2 pieces M 3 x 10 mm fastening screws DIN 964 gt Electrode titration tip holder TZ 3660 gt Titration tip TZ 3620 All parts included in the scope of delivery are available as spare parts under the stated TZ number Accessories BlueLine12 pH electrode TZ
34. t of the packing Set up the Titration Unit TitroLine easy on any flat surface and connect the mains plug to the mains socket Prior to plugging in the mains plug it has to be ensured that the operating voltage of the device corre sponds to the mains voltage The operating voltage is indicated on the rating plate on the bottom of the Titration Unit TitroLine easy 3 2 Installation of the stirrer Insert the stirrer at the lower right side and fasten it by pushing backwards GJ Fig 1 This automatically connects the power supply to the Stirrer TM 96 Fig 1 Fig 2 Fig 3 Installing the stirrer Titration Unit TitroLine easy Remove the stirrer viewed from below Lift latch slightly push the stirrer Insert the stirrer from below forwards and remove it from into the contact openings downwards of the titration unit then push the stirrer TM 96 backwards until it latches 3 3 Installing the stand Insert the TZ 3665 Strand Rod at the right side J Fig 4 and fasten it on the back panel of the Titration Unit TitroLine easy using the two included screws M3x10mm slot screw driver Install the elec trode burette tip holder as shown in Fig 5 Fig 4 Fig 5 3 4 Installing the burette tip The burette tip consists of the elements shaft with threaded clamping joint hose and slip on tip Fig 6 Disassembled burette tip sip hose e tip lt shaft threaded clamping Burette tip Sequence of a
35. the indicator will be displayed as well pH end point lt START gt pH 7 0 lt gt lt t gt neutral red The table shows the available indicators of a pH end point titration res 1 coour change aset For pH end point titration the pH electrode has to be calibrated in each case since the result is strongly de pending on the condition of the electrode Subsequently titration for a pH or mV end point can be started As soon as the unit has completed the titration automatically the ml result will be shown on the display In the case of pH titration the consump tion will always be at the location where the titration stopped The smallest step of resolution here is 0 01 ml In this place owing to the shape of the titration curve the change of the pH or mV value is ten to one hundred times greater than at any other times of the titration This means that a step which is only just being dosed will exceed the set pH or mV value without the result being corrupted thereby Analogous you may effect an mV end point titration 1400 mV 1400 mV mV end point lt START mV 840 lt l gt lt t gt 4 6 Equivalence point In the Auto Find EQ mode the Titration Unit TitroLine easy can recognize when the correct quantity of titration agent has been added By way of a combined evaluation of electrode signal time added quantity and by using an intelligent control the device is capable of recognising the behaviour of the a
36. the side of the user that the persons entrusted with the use of the Titration Unit TitroLine easy are experts in the handling of substances used in the environment and in the Titration Unit TitroLine easy or that they are supervised by specialised persons respectively Liquids with a high vapour pressure and or matters or mixed matters not qualified for use in the technical data of the titration unit must not be used During all work with titration solutions A Please wear protective glasses A When the piston moves upwards within the cylinder owing to the design of the system a microfilm of dos ing liquid or titration solution will always remain adhered to the inner wall of the cylinder but this has no influence on the dosing accuracy This small residue of liquid however may evaporate and thus penetrate into the zone underneath the piston and if inadmitted liquids are being used the materials of the Titration Unit TitroLine easy may be dissolved or corroded please refer also to Maintenance and Care The Titration Unit TitroLine easy is equipped with integrated circuits EPROMs X rays or other high energy radiation may penetrate through the device s casing and delete the program Please note also the corresponding operating instructions for the devices to be connected 35 3 Setting and commissioning 3 1 Unpacking and setting up of the Titration Unit TitroLine easy Please note that also all the small accessories are taken ou
37. urette is filling KR Y Extend piston DA2 5 Y Dose e g 2 5 ml 8 4 Properties of the RS 232 interface The data transmission properties of the RS 232 interface are firmly set The parameters include 4800 baud 7 bits word length 2 stop bits and NO parity No further settings are required Please make sure that the connected device is set to the same transmission parameters In the case of an incorrect set ting no data transfer can occur or else no readable results will be obtained The data transmission uses the TxD RxD and GROUND lines No handshake lines are present Software handshake XON XOFF is not supported The RS 232 socket must not be confused with the socket for the manual keying unit in order to avoid dam age to the device PIN configuration of the RS 232 socket 4 channel mini DIN PIN 1 TxD PIN 2 RxD PIN 3 Gnd PIN 4 not used 9 Error messages 50 Which are the causes leading to the error messages lt STOP gt returns you to the start menu Error message after calibration O OO OOOOO Error message after titration started ERROR lt STOP gt old buffer solution electrode defective electrode plug defective ERROR wrong buffer lt STOP gt electrode not connected wrong buffer solution old buffer solution electrode defective electrode plug defective or humid ERROR zero point lt STOP gt gt electrode defect ERROR setting time lt STOP gt gt el
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