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870 KF Titrino plus

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1. 36 Dosing rate AXU Ys sacs Seva reenedecces 70 E Electrode COMECE estia en 9 Electrode connector Polarizable electrode 7 Electrostatic charge s 4 End of Determination EOD 77 Exchange unit Attac e aaea a erini 15 870 KF Titrino plus Index Expert dialog 0 0 ceeeeeeeeeees 40 Numerical input 0 0 ce 19 F o Filling rate Operation Maximum elsenda 70 General nissene 17 G P GbR cestode ote ne a a 66 Parameter Graphics width 00 0 eeeee 46 Kee Sesd ee ee ted 51 Guarantees i arnasea 87 Parameters Modify live o a 28 l PC LIMS report 0 0 eee 46 InitialiZation wees 74 Pin assiIQNMent a a 76 Instrument PREP Switch O i sigi 17 Parameters cceeecseeceeeees 70 Switch ON ooaaaiiiiieeoiinnnnnnnnn 16 Preparing Instrument diagnosis 0 49 ParaMe ters cccccccceececeeeeeee 70 Prie a had bleibt oA 31 K PNTE gree eee een eee ee 46 74 Keyboard CONNECT Fe Puan sl 11 CONNEC uilan 11 Program CAS ei atne ac Giakc 74 Key assignment 72 73 Program version Keyboard layout 0 46 Taa EN cere dren E ste 49 Keats thick otek eter rete one 1 8 Parameter yingine 51 Q Quality Management 66 L langage aA 39 R Language file Recalculate cceeeeeeeteee 29 LO aC Aare ee eee 49 Remote Live modifications wo 27 GONMECON e i se reeere 7 Live parameters s s s 28 terface eyecare 76 Pin assign
2. Stop criterion 870 KF Titrino plus The titration is stopped when the endpoint has been reached and this stop criterion has been fulfilled If no stop criterion has been selected then the titration will not be stopped The stop conditions see Chapter 7 1 5 page 58 always lead to a stop even if the stop criterion has not been reached 55 56 7 1 Karl Fischer Titrations KFT 7 1 4 Stop drift Delay time Selection drift time rel drift off Default value drift drift The titration is stopped when the stop drift has been reached time The titration is stopped when the endpoint has been exceeded during a certain period of time Delay time rel drift The titration is stopped when the sum of the drift at the start of the titration and the relative stop drift has been reached off The titration will not be stopped until the stop conditions have been fulfilled This parameter is visible only when Stop criterion drift Titration is stopped when the endpoint and the stop drift have been reached Input range 1 999 pL min Default value 20 pL min This parameter is visible only when Stop criterion time When the endpoint is reached the specified time is allowed to elapse after the last dosing and the titration is then stopped Input range 0 999s Default value 10s Relative stop drift This parameter is visible only when Stop criterion rel drift The titration is stopped
3. n Relative standard deviation in Srel 100 S abs po ee Xg Explanations The individual values are incorporated in the statistics with full accuracy 15 significant places are yielded when the 64 bit numerical format is applied for the floating point number in decimal presentation The accuracy can be controlled by the selection of the prefix of the unit milli micro and the number of decimal places Example 81 82 10 8 Arithmetic algorithms in the 870 KF Titrino plus The result displayed 1234 56789158763 mg L has 15 significant pla ces It should be rounded off to three decimal places according to the above rounding off process 1234 568 mg L If the same result is expressed in g L 1 23456789158763 g L and is also rounded off to three decimal place this yields 1 235 g L l e you obtain the lowest losses in accuracy with rounding when you select the application and the numerical format in such a way that the numbers displayed have as many places before the decimal point as possi ble A complete recalculation of the statistics using a pocket calculator or PC calculation programs may exhibit deviations This can be explained by the different binary numerical formats used by these computers i NOTE The above losses of accuracy by rounding off in the range of significant places are only relevant theoretically They are generally several orders of magnitude less than measurement technique unc
4. Press START The status changes to busy the dosed volume is displayed When the volume of one cylinder has been dosed the dosing cylinder will be refilled automatically 5 Fill the cylinder Press STOP or BACK The dosing cylinder is filled If you start the filling with BACK then the dialog will also be exited Dosing a particular volume ADD You can dose a particular volume with the ADD function Proceed as follows 1 Open the manual control a In the main dialog select Menu and press OK The main menu opens a Select the menu item Manual control and press OK Manual control opens 2 Select the dosing function a Select the Dosing item Manual control Dosing Stirrer aff Dosing rate Filling rate mL mirn Press START key 36 870 KF Titrino plus 5 Operation 3 Configure the dosing function i NOTE a The dosing and filling rates should be decreased for viscous liq uids The maximum dosing and filling rates depend on the cylinder volume see Chapter 10 1 1 page 70 Enter the desired volume Enter the dosing rate a Enter the filling rate 4 Start dosing Press START The status changes to busy the dosed volume is displayed When the volume of one cylinder has been dosed the dosing cylinder will be refilled automatically 5 Fill the cylinder Press STOP or BACK The dosing cylinder is filled If you start the filling with BACK then the dialog
5. 13 Accessories Order no Description 2 803 0010 803 TI Stand with stirrer and pump Compact titration stand with magnetic stirrer and built in pump for solvent addi tion and aspiration of the titration vessel contents Suitable for Karl Fischer titra tions with Titrandos MSB connection Including comprehensive accessories sol vent bottle and waste bottle Dimensions in mm W H D 106 101 220 Dimensions remark Height with support rod 412 mm 2 860 0010 860 KF Thermoprep The 860 KF Thermoprep is designed for thermal sample preparation in Karl Fischer titration Numerous substances cannot be analysed by direct Karl Fischer titration as they are not soluble react with the Karl Fischer reagent or release their water only very slowly or not until heated to high temperatures Using tightly sealed sample vials the sample is inserted in the oven The samples can be subsequently analysed by any volumetric or coulometric KF titrator Dimensions in mm W H D 440 500 230 6 2148 030 RS 232 USB Box Extends the Titrino plus by two RS 232 interfaces for the connection of e g bal ance PC LIMS Requires 6 2151 030 Cable Se N Bs aS a 5 7 245 ad ka Co as Sp O 2 e Mo ue R 6 3026 150 Exchange Unit 5 mL Exchange Unit with integrated data chip with 5 mL glass cylinder and light pro tection PCTFE PTFE flat stopcock FEP tubing connection anti diffusion buret tip and standard amb
6. All relevant safety measures are to be observed when working with flammable solvents and chemicals Set up the instrument in a well ventilated location e g fume cup board Keep all sources of flame far from the workplace Clean up spilled liquids and solids immediately a Follow the safety instructions of the chemical manufacturer 1 3 5 Recycling and disposal This product is covered by European Directive 2002 96 EC WEEE Waste from Electrical and Electronic Equipment The correct disposal of your old equipment will help to prevent negative effects on the environment and public health 870 KF Titrino plus 1 Introduction More details about the disposal of your old equipment can be obtained from your local authorities from waste disposal companies or from your local dealer 870 KF Titrino plus 2 Overview of the instrument Figure 1 Front 870 KF Titrino plus 1 Piston rod 2 Contact pins Of the dosing drive For the data chip 3 Coupling 4 Display For switching the flat stopcock 5 Keypad 870 KF Titrino plus 2 Overview of the instrument Figure 2 Rear 870 KF Titrino plus 1 Type plate Contains specifications concerning mains voltage and serial number 3 USB OTG connector For connecting printers USB sticks USB hubs etc 5 Remote connector For connecting instruments with a remote interface D Sub 9 pin 870 KF Ti
7. Selection on off Default value on 7 1 3 Control parameters Menu gt Parameters gt Control parameters Under Control parameters the control parameters for the endpoint are defined Endpoint at Measured value for the endpoint 870 KF Titrino plus 53 54 7 1 Karl Fischer Titrations KFT Titration rate Dynamics Measuring mode Ipol Input range 1250 0 1250 0 mV Default value 250 0 mV Selection off Measuring mode Upol Input range 125 00 125 00 pA Default value 25 00 pA Selection off Three predefined sets of parameters can be selected for the titration rate Selection slow optimal fast user Default value optimal slow For samples with a low water content or samples which release their moisture only slowly optimal For all standard titrations The parameters have been optimized for the most frequent applications fast For uncritical samples with high water content user The individual titration parameters can be modified The settings of the individual titration rates are listed in table 1 page 55 This parameter is visible only when Titration rate user This parameter defines the control range before the specified endpoint Individual volume steps are dosed in the control range the dosing is finely controlled The closer the endpoint the slower the dosing until the vol ume increment defined under Min increment has been reached The larger the control range th
8. The contrast is set incor rectly The automatic calibration of the balance is switched on Adjust the contrast correctly see Chapter 6 1 page 39 Switch off the automatic calibration Message 020 511 Action not possi ble is displayed The USB Stick is no longer connected 1 Connect the USB stick 2 Switch the instrument off and on again The USB Stick is full Use a different USB stick Delete files with the aid of a PC 870 KF Titrino plus 69 10 1 Exchange unit 10 Appendix 10 1 Exchange unit 10 1 1 Maximum dosing and filling rate The maximum dosing rate and maximum filling rate for the exchange unit depend on the cylinder volume Cylinder volume Maximum rate 1 mL 3 00 mL min 5 mL 15 00 mL min 10 mL 30 00 mL min 20 mL 60 00 mL min 50 mL 150 00 mL min Independent of the cylinder volume values ranging from 0 01 to 166 00 mL min can always be entered When the function is carried out the rate will be if necessary decreased automatically to the highest possible value 10 1 2 Parameters for the preparing PREP The PREP function Preparing is used to rinse the cylinder and tubings of the exchange unit and fill them air bubble free You should carry out this function before the first determination or once per day Preparing is carried out with the following non alterable settings The entire cylinder volume is dosed twice with the ma
9. 3 Methods 5 2 5 Selecting from a selection list Pieces rUser de fined In a selection list select the individual entries with the arrow keys ft and 2 Accept the selection with OK or BACK 5 3 Methods 5 3 1 Method templates The 870 KF Titrino plus contains method templates which are already con figured except for a few parameters The following method templates can be selected KFT Ipol Titer Ipol Blank Ipol KFT Ipol Blank KFT Upol Titer Upol Blank Upol KFT Upol Blank Method with adjustable polarization current The blank value is not taken into account for the calculation Titer determination with adjustable polarization current Blank value determination with adjustable polari zation current Method with adjustable polarization current The blank value is taken into account for the cal culation Method with adjustable polarization voltage The blank value is not taken into account for the calculation Titer determination with adjustable polarization voltage Blank value determination with adjustable polari zation voltage Method with adjustable polarization voltage The blank value is taken into account for the cal culation 870 KF Titrino plus 5 Operation 5 3 2 Loading a method To load a method proceed as follows 1 Open the method table n the main dialog select Method and press OK The method table with the stored templates opens Meth
10. Input range 1 999d Default value 999d 6 3 File management Import Delete Backup Menu gt System gt File management i NOTE This menu item is visible only if a USB flash drive has been connected as an external storage medium Methods can be imported and deleted from a USB flash drive in this dia log Only methods located in the Files directory are displayed in the list see Directory structure on the USB flash drive page 45 A backup of the system can be created all data and settings Similarly an existing backup can be reloaded Import the selected method Delete the selected method Create a backup of all data and settings on the USB flash drive 870 KF Titrino plus Restore 870 KF Titrino plus 6 System settings il NOTE Only one backup can be created on the same USB flash drive If a backup is already stored on the flash drive then this will be over written as soon as the function is performed once again Load the backup from a connected USB flash drive Directory structure on the USB flash drive A directory with the instrument number will be created on the USB flash drive The structure within this directory appears as follows J Backup E 0 Files a Method mmth E pc_lims_report 2 PC_LIMS_Report 20070813 161029 txt Figure 14 Directory structure on the USB flash drive Backup All of the files of the backup are stored in this directory The directory is crea
11. Length mm 23 5 1 6 2730 020 Septum stopper With E 301 0041 O ring For 6 1448 010 Septum and 6 1414 030 Titration vessel lid Used for KF applications a Outer diameter mm 18 Y Length mm 30 s 3 6 2730 030 Stopper i Complete with nipple and E 301 0043 O ring For 6 1414 030 titra tion vessel lid For KF instruments VA measurement stands VA Com putrace and IC Dilution Length mm 38 1 6 2739 010 Wrench For exchange units Length mm 190 870 KF Titrino plus 93 94 13 2 Optional accessories Qty Order no Description 1 6 2811 000 Molecular sieve Molecular sieve Bottle containing 250 g Pore size 0 3 nm Without moisture indicator For Rancimats and Karl Fischer instruments 1 6 6063 901 Demo CD for tiBase 1 1 Demo CD for tiBase Test version for 30 days 1 6 2122 0x0 Power supply cable with IEC 60320 line socket type C13 Cable plug according to customer requirements Switzerland SEV 1011 Type 12 6 2122 020 Germany CEE 7 Type VII 6 2122 040 USA NEMA 5 15 Type 498 6 2122 070 Length 1 5m 1 8 870 8005EN 870 KF Titrino plus Manual 1 8 870 8004EN 870 KF Titrino plus Tutorial 13 2 Optional accessories Order no Description 2 141 0100 USB Thermal printer Neo s Compact printer with USB interface for the Titrino plus and Dosimat plus Paper width 60 mm 40 characters Including 6 2151 120 USB cable 870 KF Titrino plus
12. be edited while a determination is being carried out The only parameters that can be modified are those that can be selected Nevertheless all of the parameters are visible The modified parameters are taken into account at once If you modify for instance the start conditions after the start volume has been dosed then these modifications will not be taken into account until the next determination Proceed as follows to edit the parameters 1 Displaying the main dialog Press BACK The main dialog is displayed The determination continues to run in the background 2 Opening the main menu a Select Menu and press OK Menu rResults eLive dialog Parameters 3 Editing the method parameters a Select the menu item Parameters and press OK a Change the desired parameters accordingly 4 Displaying the live dialog Select the menu item Live dialog in the main menu and press OK or Press BACK in the main dialog The live dialog is displayed once again 28 870 KF Titrino plus 5 7 Curve Recalculate Statistics 870 KF Titrino plus 5 Operation Menu gt Results After the completion of the titration the results dialog is displayed cond ok Corrs X 2 5975 mL Regular stop BASS Recalc Statistics The calculated result and the endpoint volume are shown in the overview Display the curve of the current determination Recalculate the current determination The procedure will
13. be found in the brochure Analytical Instrument Qualifica tion Confidence in quality with 1Q 0Q Maintenance The electronic and mechanical functional groups of Metrohm instruments can and should be checked by specialist personnel from Metrohm as part of a regular preventive maintenance schedule Please ask your local Metrohm representative regarding the precise terms and conditions involved in concluding a corresponding maintenance agreement Further information on this can be found in the brochure Metrohm Care Con tracts Protect your investment the smart way available from your local Metrohm representative 870 KF Titrino plus 9 Troubleshooting 9 1 Karl Fischer titration 9 Troubleshooting Problem Cause Remedy The drift is very high during conditioning The titration cell is leaking The drift becomes greater after each titration The sample releases water very slowly Check seals and septum If necessary replace Replace molecular sieve Adjust the method Add solubilizer Increase the temperature possibly using a KF oven See technical literature A side reaction is taking place Use special reagents Adjust the method increase decrease the temperature external extraction See technical literature The pH value is not in the optimum range anymore Add buffer see technical literature The titration will not be finished The titration
14. be switched off automatically and switched back on again No user intervention is required 6 5 2 Diagnosis functions Electronic and mechanical functional groups in Metrohm instruments can and should be checked as part of regular maintenance by specialist per sonnel from Metrohm Please ask your local Metrohm representative regarding the precise terms and conditions involved in concluding a corre sponding maintenance agreement 870 KF Titrino plus 7 Parameters 7 Parameters 7 1 Karl Fischer Titrations KFT 7 1 1 Conditioning Conditioning Start drift Drift correction 870 KF Titrino plus Menu gt Parameters gt Conditioning Under Conditioning the conditions required for conditioning are defined If this parameter is switched on then the first time the titration is started the working medium will be titrated to the endpoint with the specified control parameters The status is kept stable The actual method run does not begin until START has been pressed once more Conditioning will be carried out again automatically after the titration Selection on off Default value on Conditioning OK will be displayed as soon as this volume drift has been reached and the titration can be started Input range 1 999 pL min Default value 20 pL min The endpoint volume can be corrected by taking the drift value into account For this the volume drift is multiplied with the drift correction time and this v
15. will also be exited 5 10 2 Stirring You can control a connected stirrer manually Proceed as follows 1 Opening the manual control n the main dialog select Menu and press OK The main menu opens Select the menu item Manual control and press OK Manual control opens 870 KF Titrino plus 37 38 5 10 Manual control 2 Setting the stirring rate a Select the Stirrer item Manual control Dosing i ctir Stirt a Inthe function bar select Stir or Stir The stirring rate will be increased or decreased by one step each time the OK key is pressed The algebraic sign changes the direction in which the stirring is done When viewing the stirrer from above this means counterclockwise rotation clockwise rotation 3 Switching on the stirrer a In the function bar select On and press OK The stirrer is started and stirs at the rate which has been set Off is now displayed in the function bar 4 Switching off the stirrer a Inthe function bar select Off and confirm with OK The stirrer is stopped 870 KF Titrino plus 6 System settings 6 System settings 6 1 Basic settings User name Instrument name Serial number Program version Time Date Language 870 KF Titrino plus Menu gt System gt Settings This chapter contains a description of general instrument settings A user name can be entered here for the report This parameter will only be printed if a
16. 232 USB Box for connecting balances cccccceeceeeesseeeeteeenes 14 Connecting a remote cable caress ecdivncetyetishcdeucesiani tipi vnetae manganites 14 Attaching the exchange unit eaters tea ditetntenee thle teares ceeas svi coedea ttn ceases 15 K pad 870 KF Titfino plUS ssnin curie a i 17 Directory structure on the USB flash drive ss ssnissisnsiiseeeseirren 45 Rotational speed depending on stirring rate ee eeeeeeeeeettteeeetees 71 Pin assignment of remote socket and remote plug 0 eeeee 76 Remote status diagram csiscck cia iinnhihcis veudyandulinc a uabeadts seiaeiesigatnag toast 77 Connecting the RS 232 USB Box to the PC cceeeeeceeeeeesteeeeeeeeeees 78 Vil 1 Introduction 1 Introduction 1 1 Instrument description The 870 KF Titrino plus is an instrument used for volumetric water content determination according to Karl Fischer There are method templates available which are already configured except for a few parameters If parameters are changed then these will be saved automatically The methods can be exported to a connected USB flash drive This function makes it possible for you to copy methods quickly and easily from one instrument to another 1 1 1 Titration and measuring modes The following titration and measuring modes are supported KFT Volumetric water content determination according to Karl Fischer Measuring modes Ipol voltametric measurement with selectable po
17. 870 KF Titrino plus Manual 8 870 8005EN 2 Metrohm 2 Metrohm Metrohm AG CH 9100 Herisau Switzerland Phone 41 71 353 85 85 Fax 41 71 353 8901 info metrohm com www metrohm com 870 KF Titrino plus 8 870 8005EN 04 2013 jb ebe Teachware Metrohm AG CH 9100 Herisau teachware metrohm com This documentation is protected by copyright All rights reserved Although all the information given in this documentation has been checked with great care errors cannot be entirely excluded Should you notice any mistakes please send us your comments using the address given above Documentation in additional languages can be found on http documents metrohm com Table of contents Table of contents 1 Introduction 1 1 1 Instrument description 0 00 00 ccc ecereeeeeeeeeeeeeentneeeees 1 1121 Titration and measuring Modes z2cvessorsacesrurnarisivedeieeainsnentoraniet 1 1 1 2 CORNECTOMS seris r aE e E E E E a aaa 1 1 1 3 Intended ISG re a ana tevagdndnactortcuilswin E 1 1 2 About the documentation 0000ieeee eere 2 1 2 1 Symbols and CONVENTIONS cciysientasyiunayteiuidtanivendedekyaisreddeehatne 2 1 3 Safety MStructiOns 5 6 hleu o Gini anth altel dangle 3 1 3 1 General notes on Safety ccecceesceesceeeeeeeeceeseteeeeeeeeseeeteteees 3 13 2 Electrical safety sista aes el da ied AN SS eee a oO 3 1 3 3 Tubing and capillary CONNECTIONS s isei isseire eereereee 4 1 3 4 Flammable solvents and
18. 9999999999 Default value 1 000 Blank CV01 2 This parameter is visible only with the methods KFT Ipol Blank and KFT Upol Blank This value is calculated with the blank value determination methods Blank Ipol and Blank Upol and entered here The value can also be modified manually 999999999 9999999999 mL 0 0 mL Input range Default value Decimal places Number of decimal places used to display the result 870 KF Titrino plus Result unit 7 1 9 Statistics Statistics 7 Parameters Input range 0 5 Default value 2 The result unit is displayed and saved together with the result Selection ppm mg mL g mg mL mg piece User defined Default value User defined A user defined unit can be created This will be added to the selection list The previous entry will be overwritten as soon as the new unit has been defined A blank entry can be generated this way as well Menu gt Parameters gt Statistics The statistics calculation of a multiple determination is switched on under Statistics and it is defined how many determinations the series contains If this funtion is switched on then statistics calculations will be carried out for all of the defined results Selection on off Default value off For the methods Titer Ipol and Titer Upol the default value is on Number of samples 7 1 10 Reports 870 KF Titrino plus The number of determinations that are car
19. Box for connecting balances or for the RS 232 remote control USB hub with or without an own power supply The 6 2147 000 numerical USB keypad serves for comfortable numer ical input and for navigating in the dialog In addition it provides two USB connectors Connect additional USB devices to the keypad NOTE Most of the USB devices need a so called hub in order to work cor rectly A USB hub is a distributor to which several USB devices can be connec ted USB hubs are available in specialty stores in a number of different models The USB OTG connector of the 870 KF Titrino plus has no such hub The 6 2147 000 numerical USB keypad has a USB hub and two USB connectors 870 KF Titrino plus 4 Installation The following devices can only be connected to a 6 2147 000 numerical keypad or to a USB hub a Printer with USB connector use the 6 2151 020 connecting cable Barcode reader with USB cable Mouse PC mouse with USB cable for navigating in the dialog The following devices can only be connected to a USB hub PC keyboard with USB cable for the comfortable input of letters and numbers a Keypad with numerical keypad with USB cable If you wish to connect several different instruments without own power supply then you must possibly use a USB hub with own power supply self powered The USB OTG connector of the 870 KF Titrino plus is not designed for supplying power to several devices with elevate
20. Default value 50 pA The polarization voltage is the voltage applied to the polarizable electrode during an amperometric measurement This parameter is available only with U pol determinations Input range 1250 1250 mV Increment 10 Default value 400 mV For polarizable electrodes an electrode test can be carried out A check is made that the electrode is properly connected and that no short circuit is present The electrode test is carried out when the determination is started This parameter is available only with I pol and U pol determina tions Selection on off Default value off When this parameter is switched on then the stirrer is switched on at the start of the determination 57 58 7 1 Karl Fischer Titrations KFT Stirring rate Temperature Extraction time Selection on off Default value on Setting the stirring rate It can be set in steps of 15 to 15 The default setting 8 corresponds to 1000 U min The formula for calculating the rota tional speed is specified in chapter 10 2 page 71 The optimum stirring rate can be tested in the manual control The algebraic sign of the stirring rate changes the direction in which the stirring is done When the stirrer is viewed from above this means a counterclockwise rotation a clockwise rotation Input range 15 15 Default value 8 Manually entered titration temperature Input range 20 0 150 0 C D
21. IEC 61000 4 14 Ambient temperature 5 45 C at a maximum of 85 humidity 20 60 C 40 60 C 85 86 11 8 Reference conditions 11 8 Reference conditions Ambient tempera 25 C 43 C ture Relative humidity lt 60 Operating temper Instrument in operation at least 30 min ature status Validity of the After adjustment data 11 9 Dimensions Material of hous Polybutylene terephthalate PBT ing Material of display Glass cover Width 142 mm Height 164mm Depth 310 mm Weight 2 950 g 870 KF Titrino plus 12 Warranty guarantee 12 Warranty guarantee 870 KF Titrino plus Metrohm guarantees that the deliveries and services it provides are free of defects in materials design or manufacturing The general warranty period is 36 months exclusions below from the date of delivery or 18 months in the event of continuous operation The warranty remains valid on the condition that the servicing is provided by a service organization authorized by Metrohm at defined intervals and with a defined scope The warranty period for anion suppressors of the type MSM is 120 months from the date of delivery or 60 months in the case of continuous operation The warranty period for IC separation columns is 90 days after start up For third party components that are recognizable as such the manufac turer s warranty regulations apply Consumables and materials with limited storage life and g
22. START after the input of the sample data If Hold at request is deactivated then the titration will be started in the background This dialog will be displayed until the entering of the sample data is confirmed with START even if the the titration is already completed This ensures that the sample data is avail able for calculations 870 KF Titrino plus 23 5 5 Carrying out a determination 5 5 Carrying out a determination The sample size can be entered in the following ways when a determina tion is carried out Enter manually on the instrument Send automatically from a connected balance For this purpose check the manual for the balance Proceed as follows to carry out a determination 1 Loading the method See Chapter Loading a method Page 21 2 Starting conditioning Press START Conditioning starts Conditioning not OK is displayed until the endpoint is reached The working medium is titrated to the endpoint This is indicated by Conditioning OK The status is kept stable KFT Ipol cond ok Conditioning OK 40ri ft 1 7 pl min The stirring rate can be modified with the Stirrer function The fol lowing dialog is opened by pressing OK cond ak MESI Stir Stirt The stirring rate can be reduced with Stir and increased with Stir Off switches the stirrer off On is now displayed instead This can be used to switch the stirrer back on This dialog is exited with BACK 24 870 KF T
23. Switching the instrument on and off Switching on the instrument Proceed as follows 1 Press the red STOP key The instrument is initialized and a system test performed This process takes some time a Ifa buret unit has been attached then a request appears to carry out the PREP function Buret unit Hib 126 The buret unit should be prepared Execute a PREP function All tubings and the cylinder are rinsed with the PREP Preparing function The preparing of the buret unit is described in chapter Preparing the buret unit PREP page 33 a Confirm the message with OK The display of this message can be deactivated in the system set tings see PREP warning page 41 The main dialog is displayed Met hod KFT Ipol Blank IDi IDz2 Sample size Unit 870 KF Titrino plus 5 Operation Switching off the instrument The instrument is switched off with the STOP key The fact that the key needs to be pressed down for an extended time prevents accidental switch off Proceed as follows 1 u Keep the red STOP key pressed down for at least 3 s A progress bar is displayed If the key is released during this time then the instrument will not be switched off 5 2 Fundamentals of operation 5 2 1 The keypad Figure 13 Keypad 870 KF Titrino plus BACK tg OK STOP START 870 KF Titrino plus Apply the input and exit the dialog Move the selection bar either up or down b
24. a an RS 232 connec tion For this a 6 2148 030 RS 232 USB Box is necessary Connect the RS 232 USB Box to the USB interface of the instrument The RS 232 USB Box has two connectors for RS 232 instruments The RS 232 remote control functions only through the connector RS 232 2 The connector RS 232 1 is designed for connection with a balance Con nect the RS 232 2 connector of the RS 232 USB Box to a serial interface COM interface marked with the symbol IOIOI of a PC Use a 6 2134 040 connection cable 870 KF Titrino plus 77 10 7 Remote control via an RS 232 connection 6 2134 040 Figure 18 Connecting the RS 232 USB Box to the PC Interface parameters We recommend the following parameters for the RS 232 interface COM2 Baud rate 19200 Data bits 8 Stop bits 1 Parity none Handshake software On the 870 KF Titrino plus adjust the interface parameters under Menu gt System gt External devices gt COM2 settings Transfer protocol The data communication is synchronous On each command there is an acknowledgement by the instrument A command must be sent to the instrument with the control characters CR LF as terminator The acknowledgements of the instrument will also be transferred with CR LF as terminator The instrument does not send spontaneous messages 10 7 1 Commands and variables Command Function Comment SG Start Continue Corresponds to the key START or Con
25. alue is then subtracted from the endpoint volume The drift correction time is the time interval between the end of conditioning and the end of the determination Selection auto manual off Default value off auto The value of the current volume drift is applied automatically at the start of the titration manual If the volume drift is known throughout a prolonged period of time then this can be entered manually off No drift correction takes place 51 52 7 1 Karl Fischer Titrations KFT Drift value Cond stop volume Cond stop time This parameter is visible only when Drift correction manual Volume drift for manual drift correction Input range 0 0 99 9 pL min Default value 0 0 pL min Maximum permissible volume that can be dosed during conditioning Conditioning is stopped when the specified volume is dosed If condition ing is continued by pressing START once again then the titrant volume that has already been dosed will not be taken into account i e the dosing starts again at zero The stop volume should be adjusted to the size of the titration cell in order to prevent any overflow Input range 0 00000 9999 99 mL Default value 20 0000 mL Selection off Maximum permissible time over which conditioning may take place Con ditioning is stopped when the specified time has elapsed Input range 0 999999 s Selection off Default value off 7 1 2 Start conditions Start
26. ance you require a 6 2148 030 RS 232 USB Box Figure 6 Connecting a balance When a 6 2151 020 USB cable is used then the 6 2148 030 RS 232 USB Box can be connected to the 870 KF Titrino plus by means of a USB hub or a 6 2151 100 adapter see Chapter 4 5 page 11 Connect the 9 pin plug of the respective balance connecting cable to the RS 232 1 connector Consult the user manual of the balance in order to select the correct connecting cable The parameters for the RS 232 interface on the instrument must match those on the balance see Editing the COM1 settings page 47 Addi tionally consult the user manual of the balance 4 5 Connecting a keyboard printer and other USB devi ces The 870 KF Titrino plus has a USB OTG connector Use the provided 6 2151 100 adapter USB MINI OTG USB A for connecting USB devices as e g printers keyboards or USB sticks see the following figure 870 KF Titrino plus 11 12 4 5 Connecting a keyboard printer and other USB devices 6 2151 100 Figure 7 Connecting USB devices Q CAUTION x Switch the instrument off before connecting or disconnecting a USB device or a USB stick The 870 KF Titrino plus can only recognize the device immediately after switching on The following devices can be operated directly on the USB connector with the 6 2151 100 adapter USB sticks for the backup or storing of methods 6 2147 000 numerical USB keypad 6 2148 030 RS 232 USB
27. ange short 20 70 term C SGJ sleeve No Shaft diameter top mm 8 Shaft diameter bottom mm 8 Min immersion depth mm 5 Electrode plug in head Metrohm plug in head G Indicator electrode type Pt Indicator electrode shape Wire 1 6 1244 040 Set of seals OO 870 KF Titrino plus 89 13 1 Scope of delivery Qty Order no Description 1 6 1403 040 KF Adsorber tube Used with KF equipment Including cover and O ring Height mm 113 Outer diameter mm 8 1 6 1414 030 KF titration vessel lid For volumetric KF titrations Material PTFE Material remark Insert 1 6 1415 220 Titration vessel 20 90 mL Material Clear glass Height mm 80 Outer diameter mm 78 Volume mL 20 90 1 6 1415 250 Titration vessel 50 150 mL Material Clear glass Height mm 80 Outer diameter mm 78 Volume mL 50 150 90 870 KF Titrino plus 13 Accessories Qty Order no Description 2 6 1448 010 Septum 12 mm 5 pieces Set of 5 items Material Silicone rubber Na D Height mm 2 YN Outer diameter mm 12 SS yO WSJ 2 6 1903 020 Stirring bar 16 mm Stirring Bar with magnetic core PTFE coated length 16 mm Material PTFE Outer diameter mm 4 Length mm 16 2 6 1903 030 Stirring bar 25 mm Stirring bar with magnetic core PTFE covering length 25 mm Material PTFE Outer diameter mm 5 Length mm 25 1 6 2104 020 Electro
28. be executed immediately Display the statistical overview of a determination series see Chapter 5 8 page 30 Displaying the curve The curve of the current determination can be displayed with the Curve function cond ok i4 1 7378 mL 643 2 miJ 26 s B746 plemin Wt The arrow keys e and can be used to move to the individual measur ing points A cross hair is used to show the current position on the curve The data volume measured value time etc for the respective measur ing point is indicated on the right hand side 29 30 5 8 Statistics 5 8 Details Reset Increase Recalculating i NOTE Recalculation cannot be undone All of the results are recalculated with the Recalculate function This is necessary if for example the calculation the titer or the sample size has been modified Statistics Menu gt Results gt Statistics The statistical overview of a determination series can be displayed in the Results dialog with the Statistics function i NOTE This function is visible only if statistics has been activated Meants gt S 78 abs 8 631 rel 6 54 Statistics 373 MAENG Reset Increase The mean value Mean the absolute and the relative standard deviation s abs and s rel are displayed in the overview For the mean value the number of individual results from which it has been calculated is displayed in parentheses In this example it is 3 Th
29. cal keypad 0 72 PG keyboard neca 73 PC mouse PHILS serno tenas 74 USB OTG CONECTO osi eisein 7 USB device Adapter eise eee eal 11 CONNECT neoa inea 11 USB flash drive Directory structure 45 USERNAME tsr rir kieres 39 v Validation o n 66 Ww Waranty seai elie 87 Water determination according to Karl Fischer nennen aia 8 870 KF Titrino plus
30. calculation formula is selected and the OK key is pressed then a table with the conversion factors will be displayed Table 2 Conversion table Conversion factor see table above Standard used Sample size Factor FCT in Water Standard 10 mg g g Water content in mg g see certificate Water g 1000 Water uL Density of water in g mL Sodium tartrate dihydrate g 156 6 Sodium tartrate dihydrate mg 0 1566 Input range Default value 1 0 999999999 9999999999 Number of decimal places used to display the result Input range 0 5 Default value 4 870 KF Titrino plus 7 Parameters The result unit is displayed and saved together with the result ppm mg mL g mg mL mg piece User defined mg mL A user defined unit can be created This will be added to the selection list The previous entry will be overwritten as soon as the new unit has been defined A blank entry can be generated this way as well Result unit Selection Default value User defined 7 1 8 Calculation formula for KFT Ipol Upol EP1 TITER FCT COO DIV Calculation formula for KFT Ipol Blank EP1 CV01 TITER FCT COO DIV Calculation formula for KFT Upol Blank EP1 CV02 TITER FCT COO DIV Calculations Methods KFT Ipol Upol KFT Ipol Upol Blank Menu gt Parameters gt Calculation The calculation formulas are predefined and cannot be modified Th
31. ccessories Keep this packaging as only this ensures safe transportation of the instrument 4 1 2 Checks Immediately after receipt check whether the shipment has arrived com plete and without damage by comparing it with the delivery note 4 1 3 Location The instrument has been developed for operation indoors and may not be used in explosive environments Place the instrument in a location of the laboratory which is suitable for operation free of vibrations protected from corrosive atmosphere and contamination by chemicals The instrument should be protected against excessive temperature fluctu ations and direct sunlight 4 2 Connecting a sensor Connecting a polarizable electrode Temp Figure 4 Connecting a polarizable electrode 870 KF Titrino plus 10 4 3 Connecting a stirrer i NOTE The electrode cable is protected against accidental disconnection of the cable by means of a pull out protection feature If you wish to remove the plug then you must first retract the outer plug sleeve 4 3 Connecting a stirrer You can connect the following stirrers 801 Stirrer 803 Ti Stand 804 Ti Stand requires rod stirrer Figure 5 Connecting a stirrer CAUTION Make sure that the flat side of the plug matches the marking on the socket 870 KF Titrino plus 4 Installation 4 4 Connecting a balance Balances are equipped with a serial RS 232 interface as a rule To connect a bal
32. cell is leaking Check seals and septum If necessary replace Replace molecular sieve The minimum increment is too low Define Titration rate user and increase the minimum volume increment Min incre ment see Chapter 7 1 3 page 53 The stop criterion is unsuit able Adjust the control parameters see Chapter 7 1 3 page 53 Increase the stop drift Select a short delay time See also The drift increases after each titration 870 KF Titrino plus 67 68 9 2 Miscellaneous Problem Cause Remedy The sample is over titrated The increments at the end of the titration are too high Define Titration rate user and reduce dosing rate Max rate see Chapter 7 1 3 page 53 The following experiment provides a clue for the optimum dosing rate During condi tioning display the drift and add sample without starting the titration Select a value below the highest drift as dosing rate Stir faster The amount of methanol in the working medium is too low a Replace the working medium Reduce the amount of solubilizer if work ing with solvent mixtures see technical lit erature The electrode may be cov ered Wipe off the electrode with ethanol or a suita ble solvent The solution becomes darker after each titration Replace the working medium The electrode may be cov ered Wipe off the electrode with ethanol or a s
33. chemicals c ccccseceeeeeeeeeeeeeeteee 4 1 3 5 Recycling and ISOS 608 i va xtvacstcten sys ateteuge cca pearacta mete ne dea 4 2 Overview of the instrument 6 3 Water determination according to Karl Fischer KFT 8 4 Installation 9 4 1 Setting up the instrument 0 ee eeeeeeetreeeeenees 9 4 1 1 Packaging csan an a a a a a te Mile aa 9 BMD E 1 8 E EE E A E EA 9 4 1 3 LOCATION e er Ae Peet ae Ree Gi Oa 9 4 2 Connecting a sensor eeren 9 4 3 Connecting a stirrer cece ee eeecteeeeeeeeteenteeeees 10 4 4 Connecting a balance ccc cee ceeeeeeeeeeteeeeeentees 11 4 5 Connecting a keyboard printer and other USB devi COS rerelissn EAE A E E E A AA 11 4 6 Connecting instruments to the remote connector 14 4 7 Attaching the exchange unit 00 cc eee 15 5 Operation 16 5 1 Switching the instrument on and off 16 5 2 Fundamentals of operation 0 ccccceeeeereeeeeeeees 17 5 2 1 TOY DIC cia nacre tecsapedy Sorta E tas Remi eae at 17 5 2 2 Structure of the dialog windows sac ea ete 18 5 2 3 Navigating in the dialog os readetecaccerpcunsit a vadiawived th vdveuttardmcedars 18 5 2 4 Entering text and numbers cteenesnter etn d eevee tarde 19 5 2 5 Selecting from a selection list crews cesuteceamusnatea nena sinnetdenanianvians 20 870 KF Titrino plus Table of contents 5 3 Methods ienaa oiie ohn fai eed seed 20 5 3 1 Method templates sssini a
34. d elec tricity requirements Also observe the instructions in chapter 10 4 page 72 Examples USB MINI OTG USB wil lt USE stick 6 2151 100 Figure 8 Connecting the USB stick USB MINI OTG USB 6 2151 100 Keypad 6 2147 000 lt Figure 9 Connecting the 6 2147 000 USB keyboard with USB stick and printer 870 KF Titrino plus 13 4 6 Connecting instruments to the remote connector USB MINI OTG USB RS 232 USB Box ofl aa USB Hub 6 2151 100 6 2148 030 USB stick Figure 10 Connecting the USB hub with USB stick printer and the 6 2148 030 RS 232 USB Box for connecting balances 4 6 Connecting instruments to the remote connector The 870 KF Titrino plus can be integrated in an automation system with the aid of a remote cable Figure 11 Connecting a remote cable A variety of different connecting cables are available for connecting Metrohm instruments e g sample changers see Optional Accessories chapter 14 870 KF Titrino plus 4 Installation 4 7 Attaching the exchange unit To attach the exchange unit proceed as follows 1 Slide the exchange unit from the front onto the 870 KF Titrino plus and push all the way to the rear It must snap in audibly 870 KF Titrino plus 15 5 1 Switching the instrument on and off 5 Operation 5 1
35. de cable 1 m F For connecting electrodes with Metrohm plug in head G to Metrohm instruments socket F Length m 1 870 KF Titrino plus 91 13 1 Scope of delivery Qty Order no Description 1 6 2147 000 Numerical USB keypad Numerical USB keypad for Titrino plus Dosimat plus 862 Compact Titrosampler 869 Compact Sample Changer 863 Compact Auto sampler and 899 Coulometer Including USB hub with two connec tors 1 6 2151 100 Adapter USB MINI OTG USB A For connecting USB instruments 1 6 2412 000 Weighing boats Weighing boat made of glass for the 6 1414 030 titration vessel lid or the 6 1455 31X 6 1464 32X 6 1465 320 titration vessel For KF water determinations Including protective tube Material Glass Length mm 120 1 6 2723 310 Protective cover for Titrino plus Protective cover for display and keypad for all instruments of the Titrino plus family Suitable for 848 Titrino plus 862 Compact Titro sampler 863 Compact Autosampler 865 Dosimat plus 869 Com pact Sample Changer 870 KF Titrino plus 876 Dosimat plus 877 Titrino plus 899 Coulometer Material PVC 870 KF Titrino plus 13 Accessories Qty Order no Description 2 6 2730 010 Screw nipple Made of PP For 6 1448 010 Septum or for mounting 6 1403 040 Drying tube or 6 0338 100 Electrode in 6 1414 030 and 6 1414 040 KF Titration vessel lids Used for KF titrations Material PP Inner diameter mm 11 5
36. e erent ached een ahaa re eae 71 10 3 Balance vend tanta eee ae ORR ee 71 10 4 USB devices tpt tinictescick teed tired ltcel Mead ata aies 72 10 4 1 6 2147 000 numerical USB keypad ec cceeeeeeetteeeeteeeees 72 10 4 2 Key assignment of a USB keyboard s 73 TOA 37 PG MOUSE irie i er eaa agente EE AN ads 73 1044 PRINTEN see ereceista vie n ees hs ee Mace E 74 10 5 System initialization cece eee eeeeeeeeeeeeeteeeeeees 74 10 6 Remote interface cccc eee etter ee teeeeeeenteeeetteeens 76 10 6 1 Pin assignment of the remote interface c cccceeeeeeeeeees 76 10 6 2 Status diagram of the remote interface cece 77 10 7 Remote control via an RS 232 connection 77 10 7 1 Commands and variables ss isseire rererere 78 10 8 Arithmetic algorithms in the 870 KF Titrino plus 80 11 Technical specifications 83 11 1 Measuring inputs ce ceecerreeeeeeeeeettteeeeeteeeeenenees 83 WL casi 1 9 ROVE Sate oe eek E eR aa ID ec had Oe te Nt Sarl cot 83 11 2 Dosing d eni a a EA EEE EA ainsi 84 11 3 _Interfac s citer ie Shasta aA 84 11 4 Mains connection ce ceeeeeceeeeeeeeeeeeeeeeetnennaaes 84 11 5 Safety specifications 0 0senonneone eee teeer ere rere rererere reene 84 11 6 Electromagnetic compatibility EMCO 0 ee 85 11 7 Ambient temperature aeeeeeeee ieee ee erens neree eene 85 11 8 Reference cond
37. e Chapter 10 1 1 page 70 Input range 0 01 166 00 mL min Selection max Default value max 7 1 6 Calculations Methods Blank Ipol Upol Factor FCT Decimal places 870 KF Titrino plus Menu gt Parameters gt Calculation Calculation formula EP1 FCT The calculation formula is predefined and cannot be edited The calculated result is saved as a variable Blank CV0O1 or Blank CV02 for each measuring mode separately see page 62 If a larger amount of solvent is used for determining the blank value than is later used for the sample then this factor must be used to convert the endpoint volume accordingly Input range 999999999 9999999999 Default value 1 0 Number of decimal places used to display the result Input range 0 5 Default value 2 59 60 7 1 Karl Fischer Titrations KFT Result unit 7 1 7 Factor FCT Decimal places The result unit is displayed and saved together with the result It cannot be modified Selection mL Calculations Methods Titer Ipol Upol Menu gt Parameters gt Calculation Calculation formula COO FCT EP1 The calculation formula is predefined and cannot be edited The calculated result value and unit is saved as the titer of the solution used The Factor FCT parameter must be adjusted according to what is used to determine the titer of the reagent and which unit the sample size has If the
38. e Factor FCT and Divisor DIV parameters need to be adjusted depending on the unit used for the sample size and the result If the calcu lation formula is selected and the OK key is pressed then a table with the conversion factors will be displayed Table 3 Conversion table Result unit Sample size Factor FCT Divisor DIV in g 0 1 1 mg 100 1 mL 0 1 Density of the sample in g mL ppm g 1000 1 ppm mL 1000 Density of the sample in g mL mg mL g Density of the 1 sample in g mL 870 KF Titrino plus 61 7 1 Karl Fischer Titrations KFT Result unit Sample size Factor FCT Divisor DIV in mg mL mL 1 1 mg piece pieces 1 1 Factor FCT Conversion factor see table above Input range 999999999 9999999999 Default value 0 1 Divisor DIV Conversion factor see table above Input range 999999999 9999999999 Default value 1 0 Titer Titer of the solution used As soon as a solution has been selected under Titration parameters the value and the unit will be read out from the solution data under System gt Solutions and displayed here If the titer is changed here manually then the solution data will be updated i NOTE Only the numerical value is taken into account in the calculation for mula The calculation will then provide a correct result only if the unit of the titer is mg mL Input range 0 00000001
39. e Statistics line shows how many determinations have already been carried out and how many deter minations are to be carried out in total All three determinations were car ried out in this example Display additional data Delete all statistics data Add a further determination to the determination series 870 KF Titrino plus On Off 5 9 870 KF Titrino plus 5 Operation Displaying statistical details Additional data from the determination series can be displayed with the Details function Sample size 8 4456 g 8 4589 g On Off The result and the sample size of each determination are shown Remove the selected determination from the statistics The line will then be marked with an asterisk the statistics will be recalculated automati cally Deleting statistical data All statistical data is deleted with the Reset function The statistics data is deleted automatically in the following cases a When all of the determinations of the determination series have been carried out and a new determination has been started afterwards a When anew method is loaded Adding a determination to a determination series You can use the function Increase to add an additional sample to a determination series e g because a determination was faulty and had to be removed from the statistics The second number in the Statistics line will be increased automatically by one Printing a report manually Menu gt Prin
40. e slower the titration Outside the control range dosing is carried out continuously and the dosing rate is defined under Max rate Measuring mode Ipol Input range 0 1 1250 0 mV Default value 100 0 mV Selection off 870 KF Titrino plus Max rate Min increment 7 Parameters Measuring mode Upol Input range 0 01 125 00 pA Default value 10 00 pA Selection off This parameter is visible only when Titration rate user Rate at which dosing is carried out outside of the control range The maxi mum dosing rate depends on the cylinder volume see Chapter 10 1 1 page 70 Input range 0 01 166 00 mL min Selection max Default value max This parameter is visible only when Titration rate user Minimum volume increment that is dosed at the beginning of the titration and in the control range at the end of the titration This parameter has a decisive influence on the titration rate and thus also on the accuracy The smaller the selected minimum increment the slower the titration Input range 0 1 99 90 UL Selection min Default value min Table 1 Default values of the predefined titration rates for KFT Titration rate Max rate slow optimal fast Dynamics pol 300 0 mV 100 0 mV 30 0 mV Upol 40 00 pA 10 00 pA 5 00 pA 1 00 mL min maximum maximum Min increment minimum cylinder volume 10000 minimum cylinder 5 00 uL volume 10000
41. ed but not deleted exported or created i NOTE If the limited dialog for routine operation is activated then the expert dialog cannot be activated during ongoing operation To change the dialog type the 870 KF Titrino plus must be switched off and then back on again The expert dialog can be forced as soon as the instrument is started up again Then it is possible to enter whatever settings one wishes e g the changing of the dialog type If the instrument is switched off again without changing the dialog type then the routine dialog will remain activated Forcing the expert dialog m Switch on the instrument Wait for the display of the instrument logo with the lettering easy safe precise Press the STOP key once again and hold it down while also briefly pressing the BACK key Release both keys once again Selection Expert Routine Default value Expert Expert Complete dialog 870 KF Titrino plus Contrast Beep PREP warning 870 KF Titrino plus 6 System settings Routine Limited dialog for routine operations The contrast of the display can be adjusted with the arrow keys e and gt e the contrast will be decreased by one step each time the key is pressed the contrast will be increased by one step each time the key is pressed Input range 150 240 Default value 212 il NOTE Alternatively the contrast can also be modified in the following ma
42. efault value 25 0 C Minimum duration of the titration The titration will not be stopped during the extraction time even if the endpoint has already been reached The titration is however stopped if a stop condition is fulfilled during this time see Chapter 7 1 5 page 58 The entering of an extraction time is e g recommended with samples that release water slowly or if a Karl Fischer oven is used Input range 0 999999 s Default value Os 7 1 5 Stop conditions Stop volume Menu gt Parameters gt Stop conditions Under Stop conditions the conditions for stopping a titration are defined if this does not occur automatically This could be the case when the endpoint set is not reached or if the stop criterion see Stop crite rion page 55 is not fulfilled The titration is stopped when the specified volume has been dosed since the start of the titration This volume should be adjusted to the size of the titration vessel in order to prevent the contents from running over 870 KF Titrino plus Stop time Filling rate 7 Parameters Input range 0 00000 9999 99 mL Default value 100 000 mL Selection off The titration is stopped when the specified time has elapsed following the termination of the start conditions Input range 0 999999 s Selection off Default value off Rate at which the dosing cylinder is filled after the titration The maximum filling rate depends on the cylinder volume se
43. eport with all of the data for a determination This report can be saved as a TXT file to a connected USB flash drive or sent to a terminal program or a LIMS via an RS 232 interface The definition is made in the system settings see PC LIMS report page 46 The reports that are defined in the method will be printed out Menu gt Manual control The following functions are available in the manual control Dosing Stirring Manual control Dosing Stirrer aff awe OS ADI The available subfunctions are listed for each function in the function bar il NOTE The Stirrer function can only be selected if a stirrer is connected 5 10 1 Dosing The following dosing functions are available in the manual control Prepare the buret unit PREP Continuous dosing DOS Dose a fixed vol ume ADD Rinse the cylinder and tubings of the buret unit see Chapter 10 1 2 page 70 Dose while the START key is pressed Dose a specified volume Preparing the buret unit PREP The PREP function is used to rinse the cylinder and tubings of the buret unit and fill them air bubble free You should carry out this function before the first determination or once per day 870 KF Titrino plus 33 5 10 Manual control Proceed as follows 1 Open the manual control a Inthe main dialog select Menu and press OK The main menu opens a Select the menu item Manual control and press OK Manual contr
44. er glass reagent bottle Volume mL 5 870 KF Titrino plus 95 96 13 2 Optional accessories Order no Description 6 3026 210 Exchange Unit 10 mL Exchange unit with integrated data chip with 10 mL glass cylinder and light pro tection PCTFE PTFE flat stopcock FEP tubing connection anti diffusion buret tip and standard amber glass reagent bottle Volume mL 10 6 3026 220 Exchange Unit 20 mL Exchange unit with integrated data chip with 20 mL glass cylinder and light pro tection PCTFE PTFE flat stopcock FEP tubing connection anti diffusion buret tip and standard amber glass reagent bottle Volume mL 20 870 KF Titrino plus Index A Adapter COMMOCE s weiss costes iad tak dete deve 11 B BACKUP saneti eatp deed 44 Balance phit eaii 71 Connect eip 11 Interface parameters 47 Balance type aaas 47 Buret unit Prepare PREP 0 08 33 Cc Calculation Fly eich iel celts al 59 60 61 umerical format 0 80 Rounding off process 81 Conditioning FEil Sade led anh it 51 CONAS Generi ea tas 41 Control parameters EE E EAE E E 53 CUNE dae tela igh e eala 29 D Determination Ciee a a 26 Gary oito ei i n 24 RESU tis Acetic emai ce testee tents 29 DANOS S nip a 50 Dialog language s is 39 oddt iiai air N 49 Dialog type il aee nieta 40 Directory structure 0 45 Dosing Continuous DOS wo 35 Fixed volume ADD
45. ered decimal number and the internal computer representation in complete accuracy in the range of the rear decimal places This difference results from the fact that an exact binary equivalent does not exist for every decimal number If for example you enter the sample size 50 3 mg this will be depicted in the calculation report in double precision with 5 02999999999999E 01 870 KF Titrino plus 870 KF Titrino plus 10 Appendix Rounding off process Measured values and results are rounded to the defined number of deci mal places commercial rounding in accordance with the US Pharmaco peia USP If the digit at the first dropped decimal place is 1 2 3 or 4 then it will be rounded off if this digit is 5 6 7 8 or 9 then it will be rounded up Negative digits will be rounded in accordance with their amount i e away from zero Examples 2 33 yields 2 3 2 35 yields 2 4 2 47 yields 2 5 2 38 yields 2 4 2 45 yields 2 5 Statistics The arithmetic mean value and the absolute and relative standard devia tions of results are calculated You can statistically evaluate a maximum of five results 1 lt k lt 5 calcu lated in a determination A statistical series can contain a maximum of 20 determinations 1 lt n lt 20 The following convention applies to the subsequent formulas 1 lt n lt 20and1 lt k lt 5 M lue 1 lt ean value 1 YR Absolute standard deviation gt R Xy y S abs
46. ertainties balance errors dosing errors measuring errors 870 KF Titrino plus 11 Technical specifications 11 Technical specifications 11 1 Measuring inputs 11 1 1 Polarizer Measuring mode Ipol Polarization current Measuring range Resolution Measuring accuracy Measuring mode Upol Polarization voltage Measuring range Resolution Measuring accuracy 870 KF Titrino plus The measuring cycle is 100 ms for all measuring modes A measuring input Pol for polarizable electrodes Determination with adjustable polarization current 120 120 pA increment 1 UA 125 121 pA 121 125 uA non guaranteed values dependent on reference voltage 2 5 V 1 200 1 200 mV 0 1 mV 0 2 mV 1 digit without sensor error under reference conditions Determination with adjustable polarization voltage 1 200 1 200 mV increment 10 mV 1 250 1 210 mV 1 210 1 250 mV non guaranteed values dependent on reference voltage 2 5 V 120 120 pA 0 01 pA 83 84 11 2 Dosing drive 11 2 Dosing drive Resolution 10 000 steps per cylinder volume Exchange unit Cylinder volume 1mL 5mL 10mL 20mL 50mL Accuracy Fulfills ISO DIN standard 8655 3 11 3 Interfaces USB OTG connec For connecting USB devices tor MSB connector For connecting a stirrer Remote connector For connecting instruments with a remote interface 11 4 Mai
47. f sale printers i e they print on continuous paper Selection Citizen ESC POS Custom ESC POS Epson Epson ESC POS HP DeskJet HP LaserJet Seiko ESC POS Default value HP DeskJet Adjust the width of the curve to be printed out to the paper width of the printer to be used The default value depends on the selected printer The height of the curve is 2 3 of the width Input range 100 3000 Pixels A commercially available USB keyboard can be connected to make it eas ier to enter text and numbers Specify the country specific keyboard lay out 870 KF Titrino plus Balance Baud rate Data bits 870 KF Titrino plus 6 System settings Selection English US French FR German CH German DE Spanish ES Default value English US If you have connected a balance then you must define the balance type here Selection AND Mettler Mettler AT Mettler AX Ohaus Precisa Sartorius Shimadzu Default value Sartorius The following table indicates the balance type that needs to be selected for the balance model Balance Balance type AND AND Mettler AB AE AG AM Mettler AJ PE PM PJ PR XP XS Mettler AT Mettler AT Mettler AX MX UMX PG Mettler AX AB S PB S Ohaus Voyager Explorer Ohaus Analytical Plus Precisa Precisa Sartorius Sartorius Shimadzu BX BW Shimadzu Editing the COM1 settings Menu gt System gt Externa
48. gane thaine 20 5 3 2 toading a MENO a atr e art re en AE A er ee 21 BeBe Saving Metod eraat e A a 21 SIA Exporting a method i ecen esirin N e Soe 21 5 4 Sample Gata enno a a ea a aiaia beana 22 5 4 1 Entering sample data in the main dialog eeeeeseeeeeeees 22 5 4 2 Requesting sample data at the start of the determination 23 5 5 Carrying out a determination 00 eects 24 5 6 Live modifications 0 00ccccccecccc eects eeeeeeenteeeeeees 27 5 6 1 Editing the sample data of the running determination 27 5 6 2 Editing the live parameters ccccceceeeceeesceeeeeeeeeseseeeetenees 28 Bed 4 ROSUIES A 0 hea Se aces ca teak atta ee eau cape ae eas 29 5 8 Statistics ats E AEE E ET eaten nas 30 5 9 Printing a report manually 0 0 coe eee 31 5 10 Manual control 0 00 00 cece ceeceeeteeeeeeeeeeeeeeeeeneaes 33 ERAL O SREE PIOI D EEE A AOA ye T amvaren E EAE ET 33 SAOZ VSN G e a a nthe Latah MS 37 6 System settings 39 6 1 Basic settings eia a tee ete 39 6 2 Managing solutions 00aaea eere ereen 42 6 2 1 EE E E E E S ES 42 6 2 2 Editing the solution data cccceceecceeceeseseeenteseeeetsteeeeeens 43 6 3 File management ee cceeceeeeeeeeeeeeeeeeeeeeeeenteaeeees 44 6 4 Configuring external devices 0ccceeeetteteeeees 46 6 5 Instrument diagnosis cece eeeeeee centr eerren 49 6 5 1 Loading program versio
49. guage files and program files by noting how the file name is constructed Program files They are instrument specific The file name has the following structure 5XXXyyyy bin where XXX Instrument type e g 848 for the 848 Titrino plus yyyy Program version Language files They can be recognized by means of the two digit language code in the file name A language file contains the dialog texts for various instrument types It is not instrument specific The file name has the following struc ture 5848xxxxYY bin where XXxx Version number YY Language e g DE German FR French ES Spanish Loading a file Proceed as follows 1 Connecting the USB flash drive Plugin the USB flash drive with the 6 2151 100 adapter USB MINI OTG USB A at the instrument s USB port Switch on the instrument 2 Opening the update dialog Under Menu gt System gt Diagnosis select the menu item Software update Press OK 870 KF Titrino plus 49 50 6 5 Instrument diagnosis Software update Program version Press START key to continue Opening the file selection Press OK The selection list with the program and language files present on the USB flash drive opens Selecting the file a Use the arrow keys to select the required file Press OK Starting the update Press START The update process is started it runs automatically At the end of the process the instrument will
50. ic algorithms in the 870 KF Titrino plus Variable Comment CONC Concentration of selected solution FCT Factor DIV Divisor MCV End volume i e total dosed volume at the end of the titration EM1 Measured value of the endpoint EP1 ED1 Time at the endpoint EP1 MSV Start volume DD Duration of the entire determination The values of the variables are only available after the end of a determina tion in the status ready Acknowledgement of the instrument Comment OK Command executed E1 Method not found E2 Invalid variable E3 Invalid command 10 8 Arithmetic algorithms in the 870 KF Titrino plus Numerical format The software of the 870 KF Titrino plus calculates in accordance with the widespread standard IEEE 754 IEEE Standard for Binary Floating Point Arithmetic for Microprocessor Systems This means that the numbers are used in calculations in double precision 64 bit Decimal numbers are converted into binary numbers in the computer and used in this form for calculations The output on the display and in reports once again contains decimal numbers the binary numbers are thus converted back into deci mal numbers In order to be able to check the internal calculations per formed by the computer yourself in accordance with IEEE 754 the num bers are reproduced in the calculation report in complete accuracy A min imal difference may arise between an originally ent
51. intelligent buret units An unlimited number of solu tions in buret units with data chip can be added to the solution list The number of solutions in buret units without data chip is limited to 10 items Meaning of the type EU exchange unit without data chip JEU exchange unit with integrated data chip not defined is the standard solution It can be used to carry out determi nations without having configured a solution If you carry out a titer deter mination with the titration parameter Solution not defined then the result will be saved as titer of this solution If you carry out a titration with the titration parameter Solution not defined then the data of this solution will be used for the calculation The titer and the concentration can be edited but this standard solution can neither be renamed nor deleted Edit the data of the selected solution see following chapter Add a new solution to the list see following chapter Delete the selected solution from the list 870 KF Titrino plus 6 System settings 6 2 2 Editing the solution data Name Type Cylinder volume Concentration Concentration unit Titer Titer unit 870 KF Titrino plus The designation of the solution is used for unambiguous identification Entry max 24 characters Default value empty The model of the buret unit is displayed Cylinder volume of the buret unit in mL The cylinder volume is automati cally read out w
52. ith intelligent buret units Selection 1 5 10 20 50 Default value 20 Concentration of the solution Input range 999999999 9999999999 Default value 1 000 Unit of the concentration Selection pmol mL mmol L mol L g L mg L mg mL ug L ppm mEq L User defined Default value mol L User defined A user defined unit can be created This will be added to the selection list The previous entry will be overwritten as soon as the new unit has been defined A blank entry can be generated this way as well Titer of the solution Input range 999999999 9999999999 Default value 1 000 Unit of the titer Selection pmol mL mmol L mol L g L mg L mg mL ug L ppm mEq L empty User defined Default value empty 43 44 6 3 File management Date titer det Monitoring Time interval User defined A user defined unit can be created This will be added to the selection list The previous entry will be overwritten as soon as the new unit has been defined A blank entry can be generated this way as well Date of the last titer determination Activating and deactivating the titer monitoring Selection on off Default value off This parameter is visible only when Monitoring on You will be notified that this time interval in days has elapsed when start ing a method You can then select whether or not you would still like to start the method
53. itions 0 cece eee cece cette eetteetttetees 86 11 9 Dimensions 50 fosssioseestateessesensscebanaghatehactitaanenctheenteatatasereccr ets 86 12 Warranty guarantee 87 870 KF Titrino plus Vi Table of contents 13 Accessories 89 13 1 Scope of delivery sa hseesitin aoerneiiee eine deter cones 89 13 2 Optional accessories 0 0 0 0 cccccceceeceeeeeeeeeeeeeeeetteeeenaees 94 Index 97 870 KF Titrino plus Table of figures Table of figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 Figure 11 Figure 12 Figure 13 Figure 14 Figure 15 Figure 16 Figure 17 Figure 18 870 KF Titrino plus Front 8 FORE TINO plUS asta de eta E gat tyke E E Geran tend 6 Rear 870 KF Titino PluS ienen a es Lastadads Siu tyea ads 7 Reagent dosing for KFT ove Recs ceak onde cde AONE a oa PAN tens Apes 8 Connecting a polarizable electrode ecceeccceeeteeeeeeeeeeeeteeeetteetens 9 Connecting a stirrer ee ee etee cece ceceeeeeeeceeeeeeeeeeaeeeestaeecestaeeecteneeteteats 10 C r ecting a Dal ania sn e bala sha tent ae 11 Connecting USB devices 23 rcisecdeddr sau sanaysoditess Mueashadvaete senencinuecducetaras 12 COMMEGIING lt The SB SUCK srna cates accsuietinntinudan mldaattea tel EOE 13 Connecting the 6 2147 000 USB keyboard with USB stick and printer sails coy ecient a EE Sasa varie A eacimiane 13 Connecting the USB hub with USB stick printer and the 6 2148 030 RS
54. itrino plus 5 Operation 3 Adding sample i NOTE Calculate the amount of the sample in such a way that a titrant consumption of 10 90 of the cylinder volume will result f Conditioning OK is displayed press START Conditioning is stopped The request for adding the sample will be displayed for 8 s The sample must be added during this time EFT Ipol Add sample Add the sample Afterward the request for the sample size appears hold 1 8 Press START key to continue 4 Entering the sample size Press OK The editing dialog opens Enter the sample size and apply with Accept or BACK 5 Starting the titration Press START The titration starts and the curve is displayed 870 KF Titrino plus 25 26 5 5 Carrying out a determination 27 5895 mL 45 plemin 38 s Wt The axes are scaled automatically The stirring rate can be modified during titration with the Stirrer function The following dialog is opened by pressing OK Wiad Stir Stirt The stirring rate can be reduced with Stir and increased with Stir Off switches the stirrer off On is now displayed instead This can be used to switch the stirrer back on This dialog is exited with BACK After the completion of the titration the results dialog is displayed Conditioning is restarted automatically cond ak Regular stop BASS Recalc Statistics 6 Canceling the conditioning Press STOP C
55. l devices Diagnosis Use the BACK key to return to the next higher level 870 KF Titrino plus 5 Operation 5 2 4 Entering text and numbers Hame BHECDIDEFGHIJKLMNOFQRSTUNHSYZ abcdefghijklmnopyrstuyuxuz BHi23S4S56789 p EE Cet le AAA TH6h600Ss445ce i i hbsh00 oa Cancel Clear In the editing dialog for text input or numerical input select the individual characters with the arrow keys Use OK to apply the character in the input field The following functions are available Editing function Description Accept The modification is applied and the editing dialog is exited Cancel The editing dialog is exited without applying the modification Clear The content of the input field is deleted com pletely The character left of the cursor is deleted back Space Text editor only The cursor within the input field is shifted to the left by one character each time that OK is pressed Text editor only The cursor within the input field is shifted to the right by one character each time that OK is pressed BACK The modification is applied and the editing dialog is exited The BACK key has the same function as Accept A commercially available USB keyboard can be connected to make it eas ier to enter text and numbers The assignment of the keys on the PC key board is described in chapter 10 4 2 page 73 870 KF Titrino plus 20 5
56. l devices gt COM1 settings The interface parameters for the connected balance are set under COM1 settings Transfer rate in characters per second Selection 1200 2400 4800 9600 19200 38400 57600 115200 Default value 9600 Number of data bits 47 48 6 4 Configuring external devices Stop bits Parity Handshake Selection 7 8 Default value 8 Number of stop bits Selection 1 2 Default value 1 Type of parity testing Selection even none odd Default value none Type of the data transfer protocol Selection hardware software none Default value hardware i NOTE If communications problems occur set the parameter Handshake to software and make another attempt Editing the COM2 settings Menu gt System gt External devices gt COM2 settings The interface parameters for instruments connected to the RS 232 2 con nector of the RS 232 USB Box e g PC are set under COM2 settings The parameters and input ranges are identical to those for the COM1 interface 870 KF Titrino plus 6 System settings 6 5 Instrument diagnosis 6 5 1 Loading program versions and language files Menu gt System gt Diagnosis New program versions or language files can be loaded from a USB flash drive The corresponding file must be saved on the USB flash drive in a directory with the instrument number e g 848 or 863 You can distinguish between lan
57. larization cur rent Upol amperometric measurement with selectable polarization voltage 1 1 2 Connectors The instrument is equipped with the following connectors MSB connector Metrohm Serial Bus For connecting a stirrer USB OTG connector The 6 2151 100 adapter can be used to connect for example a printer a USB flash drive or a USB keyboard Electrode connector For connecting polarizable electrodes Remote connector For connecting instruments with a remote interface 1 1 3 Intended use The 870 KF Titrino plus is designed for usage as a titrator in analytical lab oratories Its main application field is volumetric titration This instrument is suitable for processing chemicals and flammable sam ples The usage of the 870 KF Titrino plus therefore requires that the user have basic knowledge and experience in the handling of toxic and caustic substances Knowledge with respect to the application of the fire preven tion measures prescribed for laboratories is also mandatory 870 KF Titrino plus 1 2 About the documentation 1 2 About the documentation CAUTION Please read through this documentation carefully before putting the instrument into operation The documentation contains information and warnings which the user must follow in order to ensure safe opera tion of the instrument 1 2 1 Symbols and conventions The following symbols and formatting may appear in this documentation 5 12 Cros
58. lass breakage in the case of electrodes or other glass parts are excluded from the warranty Warranty claims cannot be asserted if the ordering party has failed to meet its payment obligations according to schedule During the warranty period Metrohm undertakes either to replace free of charge or to credit the purchaser for any modules or components that can be shown to be faulty Any transport or customs fees that may apply are the ordering party s responsibility The precondition for this is that the ordering party has to specify the arti cle number the article designation an adequate error description the delivery date and if applicable the serial number or chip data in the Sup port Tracker Metrohm then decides whether a replacement or a credit note is to be issued or whether the faulty part has to be returned using the Return Material Authorization RMA If a replacement or credit note is issued the ordering party undertakes to store the faulty part for at least 24 months in accordance with the current storage directives in compli ance with ESD guidelines and to hold it in readiness for onsite inspection or for return shipment to Metrohm Metrohm reserves the right to invoice the ordering party for these articles including retroactively in the event of noncompliance with these preconditions The same warranty periods that are specified for a corresponding new part apply to parts that are replaced or repaired within the above
59. llows Designation for the field with the method name METHOD Designation for the field with sample identification 1 ID1 Designation for the field with sample identification 2 ID2 10 4 USB devices i NOTE USB peripheral devices that are to be connected must support either the USB 1 0 1 1 Full Speed or the USB 2 0 High Speed standard The maximum data transfer rate is however in any case 12 MBit s Keyboards PC mice and barcode readers are so called HID devices Human Interface Device and can be connected via a USB hub only Printers should also be connected via a USB hub Depending on the manufacturer or printer type a direct connection is however possible 10 4 1 6 2147 000 numerical USB keypad The Num Lock key must be pressed for navigating in the dialog The arrow keys are effective in conjunction with it The respective editing dialog must be opened for the numerical input Table4 Key assignment Key of the 870 KF Titrino plus Key on the numerical USB or function in the editing dia keypad log BACK Home 2 8 t e gt gt OK Enter BS backspace Clear Del Accept Home 870 KF Titrino plus 10 Appendix 10 4 2 Key assignment of a USB keyboard A commercially available USB keyboard can be connected to make it eas ier to enter text and numbers The respective editing dialog must be opened for the text input and nu
60. men tioned warranty periods However replacement or repair of a part does not extend the warranty period of the entire system 87 88 Deficiencies arising from circumstances that are not the responsibility of Metrohm such as improper storage or improper use etc are expressly excluded from the warranty Metrohm also offers a 120 month spare parts availability guarantee and a 60 month PC software support warranty calculated from the date on which the product is withdrawn from the market The content of this war ranty is the ability of the customer to obtain functioning spare parts or appropriate software support at market prices during the time of the war ranty period If Metrohm AG is unable to meet this obligation due to circumstances beyond the control of Metrohm AG then the ordering party shall be offered alternative solutions at preferential conditions 870 KF Titrino plus 13 Accessories 13 1 NOTE 13 Accessories Subject to change without notice Scope of delivery 2 870 0010 870 KF Titrino plus Qty Order no Description 1 1 870 0010 870 KF Titrino plus 1 6 0338 100 Double Pt wire electrode for volumetry Double Pt wire electrode Metrohm plug in head G for volumetric Karl Fischer titration and 684 737 Coulometer cell with diaphragm Shaft material Glass Measuring range 2000 2000 Measuring unit mV Temperature range long 20 70 term C Temperature r
61. ment o 76 M Status diagram oo 77 Mains Voltage o 3 Remote cable Maintenance Agreement 66 Connectas auanei nei 14 Manual control Remote control n 77 DOSING zt saci dctad Auttse te oe 33 Report SUMING weetiesis ealaden stolons Gites 37 Print manually 2 0 0 0 31 Method occ 20 REPOMtS oaiae 63 Result sesegencseheduednedaets 29 Recalculate o 30 Rounding off process 81 Routine dialog 41 RS 232 MSB nterface parameters 48 COMNECHOF ee eee 7 RS 232 CONNECTION s is 77 N Ss Navigate 0 eseeseseeeeeeessen 18 Safety instructions 0cccee 3 98 Index Sample data Modify live Sample size Send from a balance 71 Sensor COMME CE ed a ae es 9 Sensor connector Polarizable electrode 7 SOIWICE eee Stet iat hhices cea 3 SOUTO ieee acts bah iia 42 Add ireen 42 Delete ceceetis chiens 42 Edit solution u 42 Start conditions KET iena Je th a 52 Statistics Anh ae 30 63 Stirrer TOINE E E 10 SUMING TIE epei e 71 Stop conditions KET crese iaa eaa 58 SWITCHIOM cee aie geai 17 SWITCHION 2 n6 tethers 16 System initialization ee 74 System Settings a se 39 T Temperature sensor CONNECTER Siera riea ina 9 TEXCINPUT meierier inap 19 Titration mode KET E Baie E E he EEE 1 Titration parameters KET eee eteo a ee 56 U Update Dialog language u s 49 Program version n 49 SB ee reene a E 72 Numeri
62. merical input Table5 Key assignment Key of the 870 KF Titrino plus Key on the USB keyboard or function in the editing dia log BACK Esc 0 2 tI e gt OK enter key or Enter on the numerical keypad STOP Ctrl S START Ctrl G lt backspace Clear Delete Cancel Ctrl Q Accept Esc il NOTE The lettering of the USB keyboard may differ from above lettering depending on the country specific keyboard used 10 4 3 PC mouse In order to make navigating in the dialog of the 870 KF Titrino plus easier a PC mouse can be connected Table 6 Mouse functions Key of the 870 KF Titrino plus Mouse function OK Left mouse button 870 KF Titrino plus 10 5 System initialization 10 4 4 10 5 Printer Key of the 870 KF Titrino plus Mouse function BACK Right mouse button 1 2 gt Mouse movement vertical hori zontal t 2 Scroll wheel vertical The range of USB printers available is extremely varied and constantly changing The following points must be taken into account when select ing a printer USB interface necessary Printer language HP PCL Canon BJL Commands Epson ESC P 2 or ESC POS i NOTE Inexpensive printers are often designed solely for use with a PC and may not be equipped with one of the printer languages listed above Such
63. models are not suitable for this reason System initialization In very rare instances a faulty file system e g because of a program crash may lead to an impairment of program functioning The internal file system must be initialized in such cases CAUTION x All user data methods solutions etc are deleted if a system initializa tion is carried out Afterwards the instrument will have the factory set tings again We recommend creating a backup of the system at regular intervals in order to avoid data losses After a system initialization the program versions and language files do not have to be reloaded Only the selection of the dialog language may have to be reset in the system settings 870 KF Titrino plus 870 KF Titrino plus 10 Appendix Proceed as follows for the system initialization 1 Switching off the instrument Keep the red STOP key pressed down for at least 3 s A progress bar is displayed If the key is released during this time then the instrument will not be switched off Switching on the instrument Keep the red STOP key pressed down for approx 10 s The dialog for confirmation of the initialization is displayed for 8 s The initialization must be confirmed during this time System reset request detected 27 Press BACK key twice to confirm gt gt Time remaining 8 sec Confirming the initialization i NOTE If the request is not confirmed withi
64. n ner Keep the red STOP key pressed down As soon as the progress bar appears also press the arrow key X or ft repeatedly This method will however cause the contrast to be modified by several steps If this parameter is activated then a short beep will sound in the following cases a When a key is pressed At the end of the determination m When the system remains conditioned without interruption for 10 sec onds Selection on off Default value on If this parameter is activated then the recommendation will be made to carry out the function PREP Preparing a After the instrument is switched on a Each time a buret unit is attached All tubing and the cylinder are rinsed with this function see Chapter 10 1 2 page 70 41 42 6 2 Managing solutions 6 2 6 2 1 Edit New Delete Selection on off Default value on Managing solutions General Menu gt System gt Solutions Solutions can be used in intelligent buret units or in non intelligent buret units Intelligent buret units have a built in data chip on which the data for the reagent is stored This data is automatically read out during attach ment and entered in the solution list Reagent 1 Reagent 2 Sees Hew Delete The name and the type are specified for each solution in the solution list The asterisk on the right hand side indicates that this buret unit is attached only for
65. n 8 s then the procedure will be canceled Press BACK twice Initialization is started The process takes approximately 80 s The instrument will be automatically restarted after successful initializa tion 75 76 10 6 Remote interface 10 6 Remote interface 10 6 1 Pin assignment of the remote interface Figure 16 Pin assignment of remote socket and remote plug The above figure of the pin assignment applies for all Metrohm instru ments with 9 pin D Sub remote connector Table 7 Inputs and outputs of the remote interface Pin No Assignment Function 1 Output 0 Ready EOD 2 Output 1 3 Output 2 Titration 4 Output 3 Cond OK 5 Output 4 Error 6 O volt GND 7 5 volts 8 Input O Start 9 Input 1 Stop Inputs 5V approx 5 kQ Pull up t LI t gt 100 ms active low inactive high 870 KF Titrino plus 10 Appendix Outputs lt t I LT t gt 200 ms active low inactive high le 20 mA VE 40 V Open Collector 5 V maximum load 20 mA 10 6 2 Status diagram of the remote interface START START EOD ready EOD yl Output 0 Output 1 Titr Determ Output 2 condOK Output 3 Error Output 4 Start Input 0 Stop eet Input 1 Figure 17 Remote status diagram EOD End of Determination 10 7 Remote control via an RS 232 connection The 870 KF Titrino plus can be remote controlled vi
66. ns and language files 0 ceee 49 6 5 2 Diagnosis TunEtionS ses Sets tatoo alee Oh othe a a 50 7 Parameters 51 7 1 Karl Fischer Titrations KFT 0 0 000 eee 51 7 1 1 eroine RACINAS ct cece tab EE EE AEA E S EE EEE E EE AE 51 Pilea zotat COMGIMONS saena tik cies sateen a decade a a cota eon 52 7 1 3 Control paraiieteYS acen niei N y oeeie e ToS AA E Ei 53 7 1 4 Titration parameters 200 00 ccc cceceecececeeeeeeaeeeeeeeeceeeeenneeeeeteas 56 Pelee AROS OU OMS sec cee th and ators diontaet ua E E TEREA 58 7 1 6 Calculations Methods Blank Ipol Upol ooo eects 59 7 1 7 Calculations Methods Titer Ipol Upol cca saacvcasrsnasvassaraavens 60 7 1 8 Calculations Methods KFT Ipol Upol KFT lpol Upol Blank sns hatte ast ooh aus ned site ha Naas 61 7 1 9 STQUSUCS utc A cer er set eet he ae A eee AE 63 PNET ARE ORS 2 ait tee at laden sath E E ante hed 63 870 KF Titrino plus Table of contents 8 Operation and maintenance 66 8 1 Quality Management and qualification with Metrohm 66 9 Troubleshooting 67 9 1 Karl Fischer titration cc eeren 67 9 2 Miscellaneous ccccccceccceeeeeeeeeeeeeeeseneeeeeeeeeeneeeeeees 68 10 Appendix 70 10 1 Exchange unit cciih en See Biss rca ieates Se sa ates 70 10 1 1 Maximum dosing and filling rate ee eeeeeeeeeeteeeteeeeteeeeees 70 10 1 2 Parameters for the preparing PREP cccsecceeeeeteeeteeeees 70 10 2 Stirring rat
67. ns connection Voltage 100 240 V 10 Frequency 50 60 Hz Power consump 45 W tion Fuse 2 x 2 0 ATH electronic overload protection 11 5 Safety specifications This instrument fulfills the following electrical safety requirements CE designation in accordance with the EU directives 2006 95 EC Low Voltage Directive LVD 2004 108 EC EMC Directive EMC Federal Inspectorate for Heavy Current Installations ESTI Accreditation Number SCESp 033 Safety mark for certification type 2 in accordance with NEV type testing with market monitoring EMC conformity 870 KF Titrino plus wt ER TEx W Design and testing Safety instructions 11 6 Emission Standards fulfil led Immunity Standards fulfil led 11 7 Nominal function range Storage Transport 870 KF Titrino plus 11 Technical specifications ETL Listed Mark Control number 3144965 UL61010 1 a CSA C22 2 No 61010 1 According to EN IEC UL 61010 1 CSA C22 2 No 61010 1 protection class EN IEC 60529 degree of protection IP40 This document contains safety instructions which have to be followed by the user in order to ensure safe operation of the instrument Electromagnetic compatibility EMC EN IEC 61326 1 EN IEC 61000 6 3 a EN 55022 CISPR 22 EN IEC 61326 1 EN IEC 61000 6 2 EN IEC 61000 4 2 EN IEC 61000 4 3 EN IEC 61000 4 4 EN IEC 61000 4 5 EN IEC 61000 4 6 EN IEC 61000 4 11 EN
68. od table Titer Ipol Blank Ipol KFT Ipol Elank EFT Upol Titer Upol 2 Select a method Select the desired method 3 Load the method Inthe function bar select Load and press OK The method is now loaded and is displayed in the main dialog under Method 5 3 3 Saving a method If the method parameters are changed then these will be saved automati cally It is not possible to save a method under a different name 5 3 4 Exporting a method Methods can be exported to a connected USB stick il NOTE This function is possible only if a USB stick is connected as an external storage medium To export a method proceed as follows 1 Open the method table a n the main dialog select Method and press OK The method table with the stored templates opens 870 KF Titrino plus 21 5 4 Sample data Method table Titer Ipol Blank Ipol EFT Ipol EBlank EFT Upol Titer Upol 2 Select a method Select the desired method 3 Export the method a n the function bar select Export and press OK The method is exported The directory structure on the USB stick is listed in chapter 6 3 page 44 5 4 Sample data You can enter the sample data identification sample size etc in a vari ety of ways Directly in the main dialog Automatic request immediately after the start of the determination see Chapter 5 4 2 page 23 You can also send the sample size and the unit from a connec
69. ol opens 2 Select the dosing function a Select the Dosing item Manual control Dosing Stirrer aff Gwe DOS ADD a Inthe function bar select PREP and press OK The following message is displayed Splash warning H1if 132 Check the buret tip It should point into a vessel Do you want to continue 3 Start the preparing CAUTION Make sure that the buret tip is directed into a vessel that can accommodate the cylinder volume of your buret unit several times over a Select Yes and confirm the message with OK Preparing is carried out 34 870 KF Titrino plus 5 Operation Continuous dosing DOS Continuous dosing will be carried out with the DOS function for as long as you keep the START key pressed down Proceed as follows 1 Open the manual control n the main dialog select Menu and press OK The main menu opens Select the menu item Manual control and press OK Manual control opens 2 Select the dosing function Select the Dosing item Manual control Dosing Stirrer Filling rate max mL min Press START key 3 Configure the dosing function i NOTE a The dosing and filling rates should be decreased for viscous liq uids The maximum dosing and filling rates depend on the cylinder volume see Chapter 10 1 1 page 70 Enter the dosing rate Enter the filling rate 870 KF Titrino plus 35 5 10 Manual control 4 Start dosing
70. onditioning is canceled and the dosing cylinder is filled Canceling a determination manually A determination can be canceled at any time with the STOP key 870 KF Titrino plus 5 Operation 5 6 Live modifications 5 6 1 Editing the sample data of the running determination The sample data can be entered or modified in the main dialog while a determination is running In calculations always the sample data entered at the end of the titration in the main dialog is used Proceed as follows to edit the sample data 1 Displaying the main dialog Press BACK The main dialog is displayed The determination continues to run in the background 2 Editing the sample data Edit the sample data and apply with Accept or BACK 3 Displaying the live dialog Press BACK or Select Menu and press OK Menu Results Live dislog pParameters Select the menu item Live dialog and press OK The live dialog is displayed once again Fa NOTE If the determination is finished while an editing dialog is opened e g of the sample size then this will be closed automatically and the results dialog will be displayed The value entered must be entered once more and the determination must be recalculated Make sure that the editing dialogs are closed before the determination is finished 870 KF Titrino plus 27 5 6 Live modifications 5 6 2 Editing the live parameters Certain method parameters can
71. ried out for the statistics calcu lations If an additional determination must be added to the determination series because one determination was incorrect for example then this can be accomplished in the statistical overview see Chapter 5 8 page 30 Input range 2 20 Default value 3 Menu gt Parameters gt Reports The reports that will be printed out automatically in connection with a determination are defined under Reports 63 64 7 1 Karl Fischer Titrations KFT Results Curve Calculations Statistics Measuring point list Parameters PC LIMS The result report contains the calculated results equivalence points and endpoints sample data etc Selection on off Default value off Curve report The width of the curve is defined in the system settings see Graphics width page 46 Selection on off Default value off Output of the calculation formulas for the individual results The results are printed with the maximum resolution This makes recalculation with an external program possible The following data is printed out in addition when statistics is switched on Result and sample size of the individual determinations Mean value as well as absolute and relative standard deviation Selection on off Default value off Output of the measuring point list Selection on off Default value off All of the parameters of the current method are printed out
72. s reference to figure legend The first number refers to the figure number the sec ond to the instrument part in the figure Instruction step Carry out these steps in the sequence shown Method Dialog text parameter in the software File gt New Menu or menu item Next Button or key gt WARNING This symbol draws attention to a possible life threat ening hazard or risk of injury WARNING This symbol draws attention to a possible hazard due to electrical current WARNING This symbol draws attention to a possible hazard due to heat or hot instrument parts gt gt gt h A WARNING This symbol draws attention to a possible biological hazard CAUTION This symbol draws attention to possible damage to instruments or instrument parts 870 KF Titrino plus 1 Introduction ri NOTE This symbol highlights additional information and tips 1 3 Safety instructions 1 3 1 General notes on safety A WARNING This instrument may only be operated in accordance with the specifica tions in this documentation This instrument has left the factory in a flawless state in terms of technical safety To maintain this state and ensure non hazardous operation of the instrument the following instructions must be observed carefully 1 3 2 Electrical safety The electrical safety when working with the instrument is ensured as part of the international
73. standard IEC 61010 A WARNING Only personnel qualified by Metrohm are authorized to carry out service work on electronic components A WARNING Never open the housing of the instrument The instrument could be damaged by this There is also a risk of serious injury if live components are touched There are no parts inside the housing which can be serviced or replaced by the user Mains voltage A WARNING An incorrect mains voltage can damage the instrument Only operate this instrument with a mains voltage specified for it see rear panel of the instrument 870 KF Titrino plus 1 3 Safety instructions Protection against electrostatic charges A WARNING Electronic components are sensitive to electrostatic charges and can be destroyed by discharges Do not fail to pull the mains cable out of the mains connection socket before you set up or disconnect electrical plug connections at the rear of the instrument 1 3 3 Tubing and capillary connections CAUTION lt x Leaks in tubing and capillary connections are a safety risk Tighten all connections well by hand Avoid applying excessive force to tubing connections Damaged tubing ends lead to leakage Appropriate tools can be used to loosen connections Check the connections regularly for leakage If the instrument is used mainly in unattended operation then weekly inspections are manda tory 1 3 4 Flammable solvents and chemicals A WARNING
74. t reports Proceed as follows to print a report manually 1 Opening the main menu n the main dialog select Menu and press OK 31 5 9 Printing a report manually Menu Manual control rResults Parameters pSustem Print reports 2 Opening the print dialog a Select the menu item Print reports and press OK The dialog window with the available reports opens Measuring point list Parameters System Calculations Statistics Report as in method 3 Selecting the report Select the desired report and press OK The report is printed out The following reports can be printed out manually Results Curve Measuring point list Parameters System Calculations Statis tics 32 Result report with determination properties sample data calculated results etc Curve report The width of the curve is defined in the system settings see Graphics width page 46 Measuring point list report Report with all method parameters of the loaded method System report with system settings solution list external devices etc Calculation report The statistics are also printed out in the case of multiple determinations The individual determinations with the respective sample size the mean value the absolute and the relative standard deviation are printed out for each result 870 KF Titrino plus PC LIMS Report as in method 5 10 Manual control 5 Operation Machine readable r
75. ted as soon as a backup is created for the first time Files Exported methods are stored in this directory The directory is created as soon as a backup is exported for the first time Only methods located in this directory can be imported pc_lims_report PC LIMS reports are stored in this directory as TXT files The directory is created as soon as a PC LIMS report is printed for the first time 45 46 6 4 Configuring external devices 6 4 Configuring external devices PC LIMS report Printer Graphics width Keyboard layout Menu gt System gt External devices Specification of the storage location for the PC LIMS report The PC LIMS report is a machine readable report with all of the important data for a determination It can be saved as follows asa TXT file on a USB flash drive a toa LIMS via an RS 232 interface The 6 2148 030 RS 232 USB Box is required for this purpose Selection COM2 USB Stick Default value USB Stick COM2 The report is sent via the serial COM2 interface The interface parame ters set in the dialog COM2 settings are used see Editing the COM2 settings page 48 USB Stick The report will be saved as a TXT file on the USB flash drive in the folder pc_lims_report If a printer is connected then the printer type needs to be defined here in order for the reports to be printed out correctly The printers that have the designation ESC POS are so called POS printers point o
76. ted balance in any case With some balances the sample identification and method can be also sent see Chapter 10 3 page 71 5 4 1 Entering sample data in the main dialog For a sample you can enter the sample data directly in the main dialog even while the determination is running see Chapter 5 6 page 27 Menu Met hod KFT Ipol Blank Iti Iz Sample size Unit ID1 Sample identification Entry max 10 characters Default value empty 22 870 KF Titrino plus 5 Operation ID2 Sample identification Entry max 10 characters Default value empty Sample size Sample size Input range 999999999 9999999999 Default value 1 0 Unit Unit of the sample size Selection g mg pg mL pL pieces User defined Default value g User defined A user defined unit can be created This will be added to the selection list The previous entry will be overwritten as soon as the new unit has been defined 5 4 2 Requesting sample data at the start of the determination The sample data can be requested immediately after the start of the deter mination in order to ensure that the sample data entry is not forgotten This automatic request is indispensable when you reweigh your samples hold i Press START key to continue The corresponding parameters must be activated under Start conditions for this purpose If the parameter Hold at request is activated then the run will be paused and must be continued with
77. tinue S Stop Corresponds to the key STOP H Hold Hold the method run 78 870 KF Titrino plus 10 Appendix Command Function Comment D Scan instrument sta tus Acknowledgements Ready 0 Busy 0 Hold 0 or Cond 0 0 no message If a message on the instrument requires the interaction of the user the acknowl edgement of the status scan displays the corresponding message number Exam ple Busy 010 119 Check buret unit The message can be confirmed with OK or Cancel see below SA SA OK SA CANCEL Confirm message Confirm message Confirm the message on the instrument with OK A mandatory status scan providing the message number must take place immedi ately before confirming the message see above Confirm the message with OK or Can cel SA YES A NO Confirm message Confirm the message with Yes or No L method name Load method The method name has to be known and unique Q variable Request variable value Examples for variables EP7 R1 COO List of variables see below Variable Comment coo Sample size EP1 Volume of the endpoint EP1 Cl Sample identification 1 2 R1 Result cvo1 Common variable blank value at KFT Ipol cvo2 Common variable blank value at KFT Upol SMN1 Mean value of result R TITER Titer of selected solution 870 KF Titrino plus 79 80 10 8 Arithmet
78. trino plus 2 Mains connection socket MSB connector Metrohm Serial Bus For connecting a stirrer Mini DIN 9 pin Electrode connector Pol For connecting polarizable electrodes e g double Pt electrodes Socket F 3 Water determination according to Karl Fischer KFT Karl Fischer Titration is a method for volumetric water determination Con ditioning is carried out automatically both before and after the actual titra tion The reagent dosing is controlled in such a way that a predefined endpoint is reached as quickly and as accurately as possible The volume steps and the rate of reagent dosing are regulated by the difference between the current measured value and the predefined endpoint This means that titration is performed more slowly in the control range and that smaller volumes are added The titration is stopped at the endpoint either drift controlled or after a waiting time The volume dosed until the endpoint is used to calculate the water content of the sample 4U mV KFT Ipol I I I I I 4 I 1 I I I I r l oi i oi Initial Continuous dosing dosing 1 I fi j I I I I I 1 l KFT Upol ee e I I I I I gt V mL Figure 3 Reagent dosing for KFT 870 KF Titrino plus 4 Installation 4 Installation 4 1 Setting up the instrument 4 1 1 Packaging The instrument is supplied in highly protective special packaging together with the separately packed a
79. uita ble solvent The electrode has a short circuit 1 Check the Pt wires 2 Switch on the electrode test The endpoint is reached too quickly The dosing rate outside the control range is too high Define Titration rate user and reduce the dosing rate Max rate see Chapter 7 1 3 page 53 The titration times with volumetric titration are con stantly longer With two component reagents the buffer capacity of the solvent can be exhausted Replace the working medium 9 2 Miscellaneous Problem Cause Remedy No report is printed The printer is not recog a Switch the 870 KF Titrino plus off and on nized by the instrument again Use a hub on the USB connector and con nect the printer to the hub 870 KF Titrino plus 9 Troubleshooting Problem Cause Remedy The printer model is not compatible Use a printer which fulfills the required specifi cations see Chapter 10 4 4 page 74 The USB keyboard or the PC mouse does not function The keyboard or mouse is not recognized by the instrument a Switch the 870 KF Titrino plus off and on again Use a hub on the USB connector and con nect the keyboard or mouse to the hub The keyboard or the mouse is not compatible Use a model which fulfills the required specifi cations see Chapter 10 4 page 72 The display is no longer readable Mettler XP balances send RS or QO Soom as ID1
80. user has been defined Entry max 12 characters Default value empty A instrument name can be entered here for the report This parameter will only be printed if a designation has been defined Entry max 10 characters Default value empty Serial number of the instrument This is printed as a part of the instrument identification in the report header Version number of the instrument software This is printed as a part of the instrument identification in the report header Current time Only valid numbers can be entered Format hh mm ss Current date Only valid numbers can be entered Format YYYY MM DD Setting the dialog language An additional language can be selected besides English 39 40 6 1 Basic settings Dialog type i NOTE In order to ensure that a second language can be selected it must first be installed This installation must be carried out by specialist personnel In chapter Language files page 49 you will find details regarding the installation of a second language The user dialog can be limited for routine operations One can operate normally with methods in the limited dialog However no settings can be made or methods deleted The resetting of the dialog will take effect as soon as you exit the main menu The limitation of the dialog results in the following The menu items System and Parameters are not shown in the main menu Methods can only be load
81. volume Dosing rate Menu gt Parameters gt Start conditions The parameters that are carried out before the start of titration are defined under Start conditions Volume that is dosed prior to the start of the titration Input range 0 00000 9999 99 mL Default value 0 00000 mL Rate at which the start volume is dosed The maximum dosing rate depends on the cylinder volume see Chapter 10 1 1 page 70 Input range 0 01 166 00 mL min Selection max Default value max 870 KF Titrino plus 7 Parameters Pause Waiting time e g in case of a slow response of the electrode after the start or reaction time after the dosing of a start volume Input range 0 999999 s Default value Os Request sample ID Selection of the sample identification that is queried in the method run Selection off ID1 ID2 ID1 amp ID2 Default value off Request sample size If this parameter is switched on then the value for the sample size will be queried Selection on off Default value on For the methods Blank Ipol and Blank Upol the default value is off Request sample unit If this parameter is switched on then the unit for the sample size will be queried Selection on off Default value off Hold at request If this parameter is switched on then the method run will be paused dur ing the query If the parameter is switched off the titration will be started in the background
82. when the endpoint and the sum of the drift at the start of the titration and the relative stop drift have been reached Input range 1 999 pL min Default value 10 pL min Titration parameters Menu gt Parameters gt Titration parameters Under Titration parameters the parameters influencing the sequence of the entire titration are defined 870 KF Titrino plus Solution pol U pol Electrode test Stirrer 870 KF Titrino plus 7 Parameters Selection of the solution from the solution list We recommend always selecting the solution This ensures that the correct data titer concentra tion etc is always used for the calculation Solutions are defined under System gt Solutions For buret units with integrated data chip a check is made in the method run to verify whether the correct solution has been attached and whether the type of dosing drive matches For buret units without integrated data chip the cylinder volume and the type of dosing drive are checked The validity of the titer is checked for the selected solution at the start of the determination Selection Selection of configured solution not defined Default value not defined not defined No check takes place The polarization current is the current that is applied to a polarizable elec trode during the voltametric measurement This parameter is available only with I pol determinations Input range 125 125 pA Increment 1
83. with the para meter report Selection on off Default value off The PC LIMS report is a machine readable report with all of the data important for a determination The PC LIMS report can be saved as a TXT file on a USB storage medium or sent via an RS 232 interface to a LIMS The output location is defined in the system settings see PC LIMS report page 46 The file name of the TXT file is constructed as follows PC_LIMS_Report ID1 YYYYMMDD hhmmss txt 870 KF Titrino plus 870 KF Titrino plus 7 Parameters Selection Default value on off off 65 8 1 Quality Management and qualification with Metrohm 8 Operation and maintenance 8 1 Quality Management and qualification with Metrohm Quality management Metrohm offers you comprehensive support in implementing quality man agement measures for instruments and software Further information on this can be found in the brochure Metrohm Quality Management available from your local Metrohm representative Qualification Please contact your local Metrohm representative for support in qualifica tion of instruments and software The Installation Qualification IQ and Operational Qualification OQ are offered by Metrohm represen tatives as a service They are carried out by trained employees using stan dardized qualification documents and in accordance with the currently applicable requirements of the regulated industry Further information on this can
84. ximum dosing rate 70 870 KF Titrino plus 10 Appendix 10 2 Stirring rate The stirring rate can be adjusted in steps of 15 to 15 The approximate rotational speed can be calculated with the following formula Rotational speed min r min 125 stirring rate Example Stirring rate set 8 Rotational speed in rom 125 8 1000 r min amp 2000 15 10 5 0 5 10 15 Figure 15 Rotational speed depending on stirring rate 10 3 Balance The sample size and the associated unit can be sent from a connected bal ance The sample size is transmitted as a number with up to ten charac ters including algebraic sign and decimal point Sample size and unit are sent as a single character string They are separa ted by a space character The string is terminated with the ASCII charac ters CR and LF If the balance sends a negative sample size e g when you are reweighing a sample then the algebraic sign is adopted The algebraic sign is how ever ignored for the calculations il NOTE With some balances the sample identification and the method can be sent in addition to the sample size Make sure that the balance does not send the sample size until the end 870 KF Titrino plus 71 10 4 USB devices Mettler AX For the Mettler AX balance the fields that contain the sample identifica tion or the method must be designated as fo
85. y one line at a time Select the character to be entered in the text editor Select the character to be entered in the text and number editor Select the individual functions in the function bar Confirm the selection Stop an ongoing method run or a manual func tion Switch the instrument on or off Start a method run or a manual function 17 5 2 Fundamentals of operation 5 2 2 Structure of the dialog windows gt Settings Solutions File management hExternal devices Diagnosis The current dialog title is displayed on the left hand side of the title bar The current status of the system is displayed in the upper right hand cor ner ready The instrument is in normal status cond busy The working medium is being conditioned cond ok The working medium is conditioned busy A method has been started Some dialogs have a so called function bar on the bottom line The func tions contained therein can be selected with the arrow keys e or gt and executed with OK not defined Reagent 1 Reagent 2 Sees Hew Delete 5 2 3 Navigating in the dialog The selection bar is displayed in inverted style Use the arrow keys ft and 2 to move the selection bar upward or downward one line at a time If a dialog text is marked with gt then additional settings are available in a subordinate dialog Use OK to access this dialog Example System settings Sett ings Solutions File management hExterna

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