Manual KF

Gebrauchsanleitung
Titrator TitroLine KF trace Titrator TitroLine KF trace Titrateur TitroLine KF trace
Operating Instructions
Mode d'emploi
Gebrauchsanleitung ............................................................................................................. Seite 1 . 47

Wichtige Hinweise: Die Gebrauchsanleitung vor der ersten Inbetriebnahme des Titrators TitroLine KF trace bitte sorgfltig lesen and beachten. Aus Sicherheitsgrnden darf der Titrator TitroLine KF trace ausschlielich nur fr die in dieser Gebrauchsanleitung beschriebenen Zwecke eingesetzt werden. Bitte beachten Sie auch die Gebrauchsanleitungen fr die anzuschlieenden Gerte. Alle in dieser Gebrauchsanleitung enthaltenen Angaben sind zum Zeitpunkt der Drucklegung gltige Daten. Es knnen jedoch von SCHOTT INSTRUMENTS sowohl aus technischen and kaufmnnischen Grnden, als auch aus der Notwendigkeit heraus, gesetzliche Bestimmungen der verschiedenen Lnder zu bercksichtigen, Ergnzungen am Titrator TitroLine KF trace vorgenommen werden, ohne dass die beschriebenen Eigenschaften beeinflusst werden.
Operating Instructions ...................................................................................................... Page 49 . 95

Important notes: Before initial operation of the Titrator TitroLine KF trace please read and observe all operating instructions carefully. For safety reasons the Titrator TitroLine KF trace may only be used for the purposes described in these present operating instructions. Please also observe the operating instructions for the units to be connected. All specifications in this instruction manual are guidance values which are valid at the time of printing. However, for technical or commercial reasons or in the necessity to comply with the statuary stipulations of various countries, SCHOTT INSTRUMENTS may perform additions to the Titrator TitroLine KF trace without changing the described properties.
Mode demploi ................................................................................................................... Page 97 .. 143

Instructions importantes: Prire de lire et dobserver attentivement le mode d'emploi avant la premire mise en marche du Titrateur TitroLine KF. Pour des raisons de scurit, le Titrateur TitroLine KF trace pourra tre utilis exclusivement pour les usages dcrits dans ce prsent mode d'emploi. Nous vous prions de respecter galement les modes d'emploi pour les appareils connecter. Toutes les indications comprises dans ce mode demploi sont donnes titre indicatif au moment de l'impression. Pour des raisons techniques et/ou commerciales ainsi qu'en raison des dispositions lgales existantes dans les diffrents pays, SCHOTT INSTRUMENTS se rserve le droit d'effectuer des supplments concernant le TitrateurTitroLine KF trace qui ninfluencent pas les caractristiques dcrits.
49
TABLE OF CONTENTS
PAGE
Characteristics of the Titrator TitroLine KF trace ............................................50

1.1 1.2 General Information ...............................................................................................................50 Reagents................................................................................................................................50
2 3
Warning and Safety Advises..............................................................................54 Installation and Initial Operation .......................................................................55

3.1 3.2 3.3 3.4 3.5 3.6 Unpacking the Titrator TitroLine KF Trace.............................................................................55 Setting up the TitroLine KF trace ...........................................................................................56 Connecting Power Supply, Electrodes and Accessory..........................................................59 Setting up of the Titration Stand TM KF and the Titration Vessel .........................................60 Filling the Titration Vessels ....................................................................................................64 Switch on Device, First Conditioning .....................................................................................64 Keys and Contrast..................................................................................................................66 Start Picture, Main Menu and Method Selection ...................................................................67 Language Selection ...............................................................................................................67 General Information ...............................................................................................................70 Volume and Weighted sample ...............................................................................................70 Result Formula....................................................................................................................71 Result Unit...........................................................................................................................72 Result Decimal Places ........................................................................................................72 Result Statistics...................................................................................................................72 Documentation .......................................................................................................................73 Titration Parameters ..............................................................................................................75 Result Re-calculation ...........................................................................................................77 General Information ...............................................................................................................78 Device Parameters ................................................................................................................79 System Information ................................................................................................................80 Configuration RS-232 ............................................................................................................80 Reset......................................................................................................................................80 Date and Time........................................................................................................................81 Password ...............................................................................................................................81 Theory ....................................................................................................................................83 Work flow ...............................................................................................................................84 Handling .................................................................................................................................85 Working techniques ...............................................................................................................86 Verification .............................................................................................................................88 Tips and Tricks.......................................................................................................................89 General Information ...............................................................................................................90 Chaining of Several Titrators TitroLine KF trace Daisy Chain Concept .......................90 Instruction Set for RS-Communication ..................................................................................90 Connection of Analytical Balances ........................................................................................92 Connection of Printers ...........................................................................................................92
Working with the Titrator TitroLine KF trace....................................................65

4.1 4.2 4.3
Method Parameter ..............................................................................................70

5.1 5.2 5.3 5.4 5.5 5.6 5.7 5.8 5.9
System Configuration ........................................................................................78

6.1 6.2 6.3 6.4 6.5 6.6 6.7
Basics and Working Information.......................................................................83

7.1 7.2 7.3 7.4 7.5 7.6
Data Communication via RS-232-and USB Interfaces.....................................90

8.1 8.2 8.3
Connection of Analytical Balances and Printer ...............................................92

9.1 9.2
10 11 12 13
Trouble Shooting ................................................................................................93 Maintenance and Servicing of the Titrators TitroLine KF trace......................94 Storage, Transport and Environmental Concerns ...........................................94 Accessory and Spare Parts .............................................................................. 95
Version: 080807-E
50
Characteristics of the Titrator TitroLine KF trace
1.1 General Information

Nonwarranty Clause The measuring or analysis results depend on many factors. Please check the measuring and/or analysis results regularly for plausibility and carry out appropriate reliability tests. Please mind all common validation procedures too.
The titrator TitroLine KF trace is a very complex and completely coulometric titrator used to measure the humidity ratio according to Karl-Fischer. The titrators operability allows you to work in an uncomplicated way. The display asks you to select the respective functions and/or to set the respective parameters. The titrators display shows you the actual status even during the operation sequence. The methods for sample titrations and the collection of blank values are already pre-assigned. Thus, it is possible to start the titration directly after installation. Normally, it is not necessary to change the titration parameters. Almost all parts are already pre-assembled. Thus, the measuring place can easily be installed within minutes. Due to the connection of a PC-keyboard, e.g. TZ 2835, it is easier to weight samples and to enter alphabetical sample designations.
1.2 Reagents
Solutions to be used: All common and modern Karl-Fischer reagents can be used for the coulometry process. There is a general rule: It is strictly necessary to mind all valid safety guidelines for chemical products. This applies particularly to inflammable and/or caustic liquids.
Note:
Signs used in the text and their meanings:
! = Warning sign << ... >> = Display content < ....... > = Button = See e.g. illustration, chapter, instruction manual
KONFORMITTSERKLRUNG DECLARATION OF CONFORMITY DCLARATION DE CONFORMIT
Wir erklren in alleiniger Verantwortung, dass das Produkt
We declare under our sole responsibility that the product
Nous dclarons sous notre seule responsabilit que le produit
Titrator
Titration Unit
Titrateur
TitroLine KF trace
auf das sich diese Erklrung bezieht bereinstimmt mit dem normativen Dokument
TitroLine KF trace
to which this declaration relates is in conformity with the normative document
TitroLine KF trace
auquel se rfre cette dclaration est conforme au document normatif
Technische Daten
Technical data
Caractristiques techniques
Titrator TitroLine KF trace

15.10.2007
und / and / et
Titrierstand TM KF
15.10.2007
SCHOTT Instruments GmbH Hattenbergstrae 10 55122 Mainz Deutschland, Germany, Allemagne

15. Oktober, October 15 , 15 Octobre 2007 AGQSF 0000-A063-01/071015
th
Technical Data
Hardware CE-Mark:
TitroLine KF trace
As at 10/15/2007
Country of origin: Display: Ports: Electrode:
EMV - compatibility according to Council Directive 89/336/EWG; Transient emissions according to norm EN 50 081, part 1 Interference resistance according to norm EN 50 082, part 1 and 2 Low voltage directive according to Council Directive 73/23/EWG, Last amended by Council Directive 93/68/EWG, Test criteria EN 61 010, part 1 Germany / made in Germany Matrix-LCD display 69 x 39 mm, 64 x 128 pixel with backlighting and contrast settings port for double platinum electrode, 2 x 4 mm sockets, colour blue port generator electrode, 2 x 4 mm sockets, colours green and black For PC-keyboard with PS/2-plug such as TZ 2835 Port for low voltage connection phone jack, positive pole at pin contact, inside contact = 2,1 mm, USA/Japan; low voltage output 12 V Two bi-directional RS-232-C- interfaces (RS232-C 1 and RS232-C 2) Plug connections: 4-pole edge connector mini DIN Configuration of RS-232-C- interfaces 1 and 2 separately configurable: Baud rate: 1200, 2400, 4800, 9600 or 19200 baud; Word length: 7 or 8; stop bit 1; parity: no, even or odd; Address: 00 ... 15 Besides the RS232-1 to connect a PC to control the titrator and for data transfer Multiple range power supply 100-240 V; 50/60 Hz, power input: 30 VA Equivalent to protection class II according to DIN EN 61 010, part 1, Not suitable for explosive environments Polypropylene Polyester 200 x 265 x 205 mm (H x W x D) with titration stand TM 135/TM KF 310 x 135 x 205 mm (H x W x D), height including titration vessel Ca. 1,4 kg for module 1 and 3, ca. 2,5 kg for the entire device incl. titration stand TMKF (Module 2 and 4) Ambient temperature: + 10 ... + 40 C for operation and storage Humidity according to EN 61 010, part 1: Maximum relative humidity 0 % for temperatures up to 31 C, Linearly decreasing up to 50 % relative humidity with a temperature of 40 C
Keyboard: TM 135/TM KF: Interfaces: RS-232-C
USB
Power supply:
Materials: Housing: Front foil: Housing dimension:
Weight:
Climate:
th
Technical Data
CE - Mark
Titration Stand TM KF
In connection with the titrator TitroLine KF trace
As at 10/15/2007
Country of origin: Pump:
EMV compatibility according to Council Directive 89/336/EWG; Transient emissions according to norm EN 50 081, part 1 Interference resistance according to norm EN 50 082, part 2 Low voltage directive according to Council Directive 73/23/EWG Last amended by directive 93/68/EWG; test criteria EN 61 010, part 1 Germany / made in Germany Free volume flow - air-: flow rate 2,25 l / min Delivery pressure max. 1,5 bar Flow rate liquid medium ca. 0,8 l / min 50 ... 1000 U/min PVC- hose, outer diameter 6 x 1 mm PTFE- hose, outer diameter 4 x 0,5 mm Low voltage input 12 V / on the backside of titration stand Plug connection: plug for low voltage connection phone jack-, Positive pole at pin contact, inside contact = 2,1 mm, USA/Japan, Power supply via titrator TitroLine KF trace Polypropylene; Ca. 78 x 130 x 180 mm, H x W x D (height without tripod rod) Ca. 0,9 kg
Stirring speed: Hoses:
Connections Power supply (top);:
Housing Material: Dimensions: Weight: Ambient conditions:
Not suitable for explosive environments! Climate: Ambient temperature: Humidity: + 10 C ... + 40 C for storage and transport. According to EN 61 010, part 1: Maximum relative humidity 80 % for temperatures up to 31 C, Linearly decreasing up to 50 % relative humidity With a temperature of 40 C
Software Measuring range 10 g 100 mg / 1 ppm 5 % (recommended) Measuring speed Max. 2 mg/min Number methods: 10 (there of one to determine the blank value) Conditioning Automatically with drift determination End point criteria Drift, stop drift tolerance Auto start after sample allowance Yes Statistics Mean value, standard deviation and relative standard deviation (max. 10) Re-calculation After new weighted sample or sample voume has been entered Curve printout Measuring unit/time Documentation GLP compliant
th
54
Warning and Safety Advises
The titrator TitroLine KF trace complies with protection class II. The titrator TitroLine KF trace has been built and tested according to DIN EN 61 010, part 1, safety measures for electronical measuring instruments, and has left the factory in flawless condition as regards safety. In order to retain this condition and to guarantee riskless operation, the user is to observe all notices and warning advises included in this instruction manual. The product has been developed and produced in a system which complies with the norm DIN EN ISO 9001. For safety reasons the titrator TitroLine KF trace must only be opened by authorised personnel; e.g. works at the electrical facility must only be carried out by trained specialists.
! With non-observance the titrator trace can have hazardous effects: electrical accidents of persons or fire danger. Furthermore, the guaranteeing expires if the titrator trace TitroLine KF is interfered by unauthorised persons or deliberate damage. !
Prior to the switch-on it must be ensured that the operating voltage of the Titrator TitroLine KF trace complies with the mains voltage. With non-observance the titrator TitroLine KF trace can be damaged and could cause personal injury or material damage. If it seems to be likely that safe operation cannot be ensured, the titrator TitroLine KF trace must be put out of action and must be protected against accidental starts. Please switch off the titrator TitroLine KF trace, pull the plug of the mains cable out of the power outlet and remove the titrator TitroLine KF trace from the work station. It seems to be likely that riskless operation cannot be ensured if the packaging is damaged, if the titrator TitroLine KF trace has visible damaging, if the titrator TitroLine KF trace does not work as intended, if liquid has entered the housing, if the titrator has been altered technically or if unauthorised persons have tried to repair the device. If, in such a case, the user puts the device into operation, all resulting risks vest in the user. The Titrator TitroLine KF trace must not be stored or operated in wet rooms. Due to safety reasons, the titrator TitroLine KF trace must only be used for application fields described in the operating instructions. With operating conditions differing from the specified normal operation the user must assess the existing risks on his / her own.
! All relevant regulations referring the handling of used materials must be adhered to: the Ordinance on Hazardous Substances, the Chemicals Act as well as the chemical trading regulations and advises. On the side of the operator it must be ensured that persons who are entrusted with the operation of the titrator TitroLine KF trace are technical experts in using the substances typical for the titrator TitroLine KF trace and/or are supervised by competent persons.
With all works that involve with chemicals: ! Wear protective goggles! ! The titrator TitroLine KF trace is provided with integrated circuits (e.g. flash memory). X-rays or other energetic radiation can permeate the device housing and may delete the operating system.
55
Installation and Initial Operation
3.1 Unpacking the Titrator TitroLine KF Trace

All components of the titrator TitroLine KF trace Module 1 and 3 are located in one single package and, within this package, they are arranged in such a way that it is very easy to take them out. In addition, modules 2 and 4 contain a package for the titration stand TM KF as well as accessory. On the top side of the package there is the instruction manual. Fig. 1
Fig. 1 Underneath you can find the two packages for the generator and indicator electrode Fig. 2
If you have removed the electrode packages and the foam inlet, you will see the magnetic stirrer TM 135 (only with module 1 and 3!), the titration vessel TZ 1751 or TZ 1754, the stand rod TZ 1748 as well as the retaining clip TZ 1749. Fig. 3
56
Thereafter, you find some accessory, such as a small bottle with drying agent, glass wool, syringes with needles etc., and the titrator itself. Fig. 4
Underneath the accessory packaging there is the power supply pack of the TitroLine KF trace.
Fig. 5
3.2 Setting up the TitroLine KF trace

The titrator TitroLine KF trace can be mounted on any desired plain basis. Prior to inserting the mains plug, it must be ensured that the operating voltage of the titrator TitroLine KF trace complies with the mains voltage. Normally, this should not be a problem since the power pack is designed as a multiple voltage level power pack with a range of 100 240 V. Depending on the power socket, the EURO-plug or the US-plug must be connected to the power pack. UK-adaptors are available on demand. The operating voltage is specified on the type plate underside the titrator TitroLine KF trace.
! The titrator TitroLine KF trace may not be used in explosive environments. !

Please ensure that all of the smaller additional parts are taken out of the packaging. The delivery supply is listed in the associated packing list.
57
Put the magnetic stirrer TM 135 next to the basic device.
Fig. 6
Screw the stand rod into the provided nut of the magnetic stirrer.
Fig. 7
Mount the retaining clip onto the tripod rod.
Fig. 8
58
Clamp the titration vessel onto the retaining clip. Fix the titration vessel in such a way that the bottom of the titration vessel stands directly at the upper surface of the magnetic stirrer Fig. 9
Put the indicator electrode KF 1150 and the generator electrode (TZ 1752 or TZ 1753) into the provided openings NS 7,5 and NS 19 ( Fig. 10), and the electrode cables into the colour-coded socket. The indicator electrode has a fixed cable with 2 blue plugs. The cable LB 04 NN has a green and black plug and is connected to the provided port of the generator electrode. (See also next Chapter 3.3).
59
3.3 Connecting Power Supply, Electrodes and Accessory

Fig. 11 Ports on the back side of the titrator TitroLine KF trace
From top to bottom: Top left USB: Top right Gen: Left 12 V Out: Right Ind: PS2: RS1: RS2: Mains switch 12 V In: USB-port (slave) to connect a PC Sockets of generator electrode. Please mind the colour codes! Socket of titration stand magnetic stirrer TM 135 or pump/magnetic stirrer TM KF Sockets (blue) of indicator electrode KF 1150 Port of PC-keyboard with PS/2-plug such as TZ 2835 Printer / PC Balance and connection of additional titrators, Chapter 8.2 Chaining of additional titrators TitroLine KF trace Daisy-Chain On-off switch Connection of external multiple range power supply
Connect the magnetic stirrer or the TMKF with the cable TZ 1577. Please use the upper connection socket at the magnetic stirrer/TMKF. The socket at the titrator can be found directly below the USBsocket. For further information see Fig. 11
60
3.4 Setting up of the Titration Stand TM KF and the Titration Vessel

Modules 2 and 4 are supplied with the titration stand TM KF and the titration vessel TZ 1754. Normally, the titration stand is to be mounted on the right side next to the titrator TitroLine KF trace. Fig. 12 Connections of the back side of the titration stand TM KF and KF Trace
As seen from front side: Connect the right tube clip to the back side of the titration stand and the tube clip on the drying bottle ( Fig. 12) with one of the two short PVC-tubes ( Fig. 12). Connect the other tube clip of the drying bottle with the tube clip of the brown square bottle (->KF reagent bottle) using the other short PVC-tube ( Fig. 12). Connect the left tube clip on the back side of the titration stand and the tube clip on the waste bottle Fig. 12). with the longer PVC-tube (
61
Put the stand rod (
Fig. 13) into the provided receiver of the titration stand and seize it manually.
Fig. 13 Mount the retaining clip to the stand rod. ( Fig. 14)
Fig. 14 Clamp the titration vessel to the retaining clip. Fix the titration vessel in such a way that the bottom stands directly at the upper surface of the titration stand. ( Fig. 15)
Fig. 15
62
Put the threaded pipe with the NS 14/23 core and the GL 14-thread in one of the NS-14.5-openings. Put both PTFE-tubes through both bore holes of the septum. Please put one tube through up to the bottom of the titration vessel. The other tube only approx. 1-2 cm. Fig. 16
Fig. 16 Put the other end of the PTFE-tube, which touches the bottom of the titration vessel, through the opening on the cap of the clear square bottle (-> disposal bottle). Put the other tube through the opening of the cap of the brown reagent bottle. Adjust the dosage and the disposal tubes as depicted in Fig. 17. Then seize the screwing with the tubes on the bottles.
Fig. 17 Fill the drying bottle ( cap and tighten. Fig. 18) up to two thirds with the provided molecular sieve 0,3 nm. Close the
Fig. 18
63
Fill the KF Anolyte into the brown 1 l-reagent bottle. You can also connect the GL 45 adaptor directly to the anolyte bottle if it has a GL-45 thread. It is also possible to use other reagent bottles with a GL 45 thread or a S 40 thread (adaptor TZ 1795) instead of the provided square laboratory bottle. Power Supply of the Titration Stand TM KF The titrator stand is energised via the titrator. Connect the titration stand and the titrator with the provided low voltage cable TZ 1577. Please use the upper connection socket at the magnetic stirrer/TMKF. The socket on the titrator is to be found directly below the USB-port. (See Fig. 16). Working with the titration stand Dosage: Pump the anolyte into the titration vessel by pressing the front part of the rocker switch. As long as you press the button the dosing process proceeds. Siphon off: Siphon off the solution from the titration vessel by pressing the back part of the rocker switch. As long as you press the button it will be siphoned off. Note: Mind the fill level of the waste bottle. Before you siphon off the titrating solution please make sure that the disposal bottle can absorb this amount of solution.
The built-in magnetic stirrer stirs the liquids in the titration vessel. You can adjust the stirring speed at the turning knob at the front side of the titration stand ( Fig. 19).
Fig.19 Troubles Problems might occur if the tubes are not connected properly or the pressure / low pressure system has a leakage. Then, after a few seconds operating time of the pump, no reagents will be conveyed anymore. When checking the tubes please observe that the bottle screwing and all adaptors are leak-proof. The same applies to the tube connections of the drying bottle. Note: Buckled tubes cause incorrect dosages and also the siphon off process does not work properly. Please check the tubes and their connections for leak-tightness on a regular basis. Replace if necessary.
If the reagents continue to run in from the storage bottle after the actual dosage process has ended, position the bottle at lower level than the titration vessel. If the reagents continue to run in from the storage bottle between the dosage process and the siphon off process, please wait a few seconds between the changes. We recommend to remove the glass adaptor with the dosing and exhaust hose after adding the KF-anolyte and to close the ground-in opening with the provided die glass stopper NS 14,5.
64
3.5 Filling the Titration Vessels

Fill the titration vessel approx. up to a half with anolytes that are suitable for the respective application. (Module 1 and 3). You can even use the pump for modules 2 and 4. If you use a generator electrode with diaphragm (included in delivery with module 3 and 4), it is necessary to fill an ampoule with catholyte into the generator electrode. Here, please use also a glass funnel or better a syringe with needle ( Fig. 20).
Fig. 20
3.6 Switch on Device, First Conditioning

Set the stirring speed at the TM 135/TMKF between 3 and 4 (Dont forget magnetic stirring bar!). Now switch on the device. The mains switch is situated on the right at the back side of the TitroLine KF Trace. As soon it is turned on the TitroLine KF trace starts the conditioning process. If the anolyte has freshly been filled in, the conditioning can take up to 10-20 minutes. The drift display is then > 1500 g/min. If the drift has fallen below 10 g/min, the TitroLine KF trace is ready for first measurements.
65
Working with the Titrator TitroLine KF trace

Menu Structure
*
Start Menu
Method 01 * Start <Start> Selection <Mode> Edit Paramater <F2> 0 ppm 0 ppm g/min
Water Mean Drift
<Mode>
Select Methods
<Start>
* *
Test Titration
* *
<Edit Parameter>
*
<F2>
Method 01 *
* M e t h o d s e l e c t io n 1* M e th o d 0 1 M e th o d 0 2 M e th o d 0 3 M e th o d 0 4 M e th o d 0 5 Selection < > Enter<F1> ESC<F4>
Method 01 Conditioning ready Dose sample!
Drift Stop
3 g/min ESC<F4>
V o lu m e /w e ig h t Result Documentation Titration parameters Select < > Enter<F1> ESC<F4>
Select <>
* Method selection 3* System settings
* * Method 01 Sample ID 1 * *
Selection <> Enter<F1>
ESC<F4>
Input < > Enter<F1>
<Del> ESC<F4>
<Enter>
<F1>
<Start>
* * Method 01 W eight [mg] * *
0010.00
Input < > Enter<F1> <Del> ESC<F4>
<Start>/<Enter>
66
4.1 Keys and Contrast

You can change the contrast of the display with the thumb wheel situated on the right at the underside of the titrator. The titrator TitroLine KF trace can be operated with the key field in the front of the device or with a connected PC-keyboard (PS-2 compatible).
Keyboard of the TitroLine KF trace Fig. 21

FILL F1 START STOP
F2
F5
With the keypad at the front of the titrator TitroLine KF trace ( Fig. 21) it is possible to operate the entire device. However, with the input of alphanumerical sample designations it is recommended to use an external PCkeyboard. We recommend the keyboard TZ 2835. ( Fig. 22) The keypad at the device has 6 keys. In every situation the display at the titrator TitroLine KF trace shows the keys to be pressed at the device itself or at the PC-keyboard.
F3 MODE F4
Fig. 22 Keys <F1> <F2> <F3> <F4> - F 9 <F10> Num Lock Prt Sc Sys Rq Scroll Lock <ESC> Function Starts the selected method No function Edit parameters Have no functions Display online graphics / measuring graphics from main menu No function No function No function Selects the selection menu for the methods from the main menu Alternatively: The previous menu level can be reached with <ESC>. Selection of individual menus. Selection of parameters. Input of sample numbers and various parameters. Confirms entered parameters. Both keys always mean <ENTER>. Deletes an entered number / an entered sign above the cursor. Alphanumerical inputs possible. Upper / lower case possible. Have no function.
< > < > Cursor key 0...9, Decimal point <ENTER> or <> < Backspace > Alphabetical characters, ASCII-signs All other keys
TLKF-trace_080807_ENG.doc
67
4.2 Start Picture, Main Menu and Method Selection

Schott Instruments TitroLine KF trace Softwareversion V 07/45a
After the switch on of the titrator TitroLine KF trace the Start Picture ( Fig. 23) shows the device name and the software version. The start picture shows up for approx. 5 s and then changes automatically into the Main Menu ( Fig. 24). Then, the method which has last been used shows up in the display.
Fig. 23
* Method 01 * Start <Start> Selection: <Mode> Edit paramater <F2> 0 ppm 0 ppm g/min
Water Mean Drift
The current method can be started in the main menu with <Start>. With <F2> and/or Edit Parameter you go the parameter settings of the selected method. Via <Mode>/<F4> you go to the Method Selection ( Fig. 25).
Fig. 24
* M e t h o d s e le c t io n * M e th o d 01 M e th o d 0 2 M e th o d 0 3 M e th o d 0 4 M e th o d 0 5 Selection < > Enter<F1> ESC<F4>
By pressing the and - buttons you can select the desired method. This selection is to be confirmed with <F1> and/or <ENTER>. With <F4> or <ESC> you go back to the main menu. By repeatedly pressing the arrow keys you see more possible selection options ( Fig. 26).
Fig. 25
Fig. 26
Method selection * Method 06 Method 07 Method 08 Method 09 Method 10 (blank) Selection <> Enter<F1> ESC<F4>
If the arrow keys are pressed once again, you get into the System settings. ( Fig. 27 ).
Method selection System settings
In the System settings menu are e.g. the language settings ( Chap. 3).
Fig. 27
ESC<F4>
4.3 Language Selection

On delivery the titrator TitroLine KF trace is set to English. In order to select another language (German, French or Spanish), please go from the main menu ( Fig. 24) to the Configuration Menu ( Fig. 28) with <Mode> and/or <F4> via the Method Selection Menu ( Fig. 25/26/27), and then directly into the language selection ( Fig. 29).
68
Systemeinstellungen
Fig. 28
Language Device parameters System information RS232 configuration Selection < > Enter<F1> ESC<F4>
Fig. 29
System settings * Language * English Deutsch Francais Espanol Selection < > Enter<F1> ESC<F4>
* *
The respective language is selected with the arrow keys <> and confirmed with <Enter> and/or <F1>. Now, the display changes into the selected language and automatically jumps back one level to the configuration menu.
4.4 Starting a Titration

Once all preparations have been finished, you can start to titrate samples. Start the selected method with the <Start>-button in the main menu. At first, the titrator starts the conditioning process ( Fig. 30). Here the titration cell is titrated until it is dry. This includes the entire water of the anolyte and even adherent liquids in the titration vessel
* *
Method 01 Conditioning
* *
12.4 g/min
Fig. 30
Stop ESC<F4>
During the conditioning process the titrator TitroLine KF trace shows the current Drift in g/min. If the titration cell is dry, the display changes as illustrated in Fig. 31.
* *
Method 01 Conditioning ready Dose sample!
* *
Now the display asks you to dose the sample. The liquid sample is now dosed through the septum into the titration vessel. Advises on how to handle the samples and some more useful advises can be found in Chap. 6. The request disappears after a few seconds. The input of an alphanumerical sample designation is only possible with a PC-keyboard connected. ( Fig. 22). Up to 14 alphanumerical characters can be entered. With the <Backspace> - key it is possible to delete an entry already made. The input is confirmed with <Enter> or <F1>. Without an external keyboard the sample designation is automatically counted up starting with 1. With the keyboard TZ 2835 or any other PC-keyboard the numerical values are entered directly via the number pad. If no external keyboard is connected, the numerical values are set with the arrow keys <>, <>, or <>. With the arrow key <> the respective number is to be selected. The value is altered with the arrow keys <> and <>. The input is confirmed with <Enter> or <F1>. Please enter the sample quantity in mg or ml and confirm the input with <Enter> or <F1>. ( Fig. 33). The measurement can now be started with the preset parameters.
Drift Stop
3 g/min ESC<F4>
Fig. 31
* * Method 01 Sample ID * *
1 Enter ESC <F1> <F4> DEL
Fig. 32
0010.00
Input Enter < > <F4> ESC<F4>
Fig. 33
69
* * W ater
Method 01 Measuring
* * 60 ppm
Drift Stop
100 g/min ESC<F4>
The titration is carried out as long as the predefined end criteria are reached. Normally, this is a particular drift value and a particular drift-stop tolerance ( Chap. 5.8). During the measurement the current result is shown in the unit desired (ppm, %, etc.). The titration can be cancelled with the <ESC>-key at all times.
Fig. 34
* Method 01 Start Selection: Edit paramater * <Start> <Mode> <F2> 220 ppm 225 ppm 1,5 g/min
W ater Mean Drift
Fig. 35
At the end of the titration the result is shown on the display. The result is the water content of the sample in ppm, %, g or in any other unit selected. The average value of up to 10 measurements and the current drift in g/min are also shown. If a printer is connected, the result is printed on the printer with additional information. The next titration can immediately be started with the <Start>-button.
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Method Parameter

On delivery the methods in the titrator TitroLine KF trace are pre-allocated with common parameters. However, every user can adapt the parameter of the individual methods as desired. With <F2> (and F3 with an external keyboard) you go from the main menu into the method parameters menu ( Fig. 36).
Method 01
Fig. 36
V o lu m e / w e ig h t Result Documentation Titration parameters Selection < > Enter<F1> ESC<F4>
In the field Volume/weight you can choose whether a sample is entered in ml or a weighted sample in mg, and if the weighted samples are to be entered manually or automatically via a connected analytical balance. In the field Result you can edit the factors of the formula, can select the units, set the decimal places and can activate the statistics. In the field Documentation you can select the form of the documentation: brief, standard with curve, GLP, only display.
The actual parameters of the titration can be set in the field Titration Parameter. Adjustable parameters for the titration are: Start drift The stop drift The stop-drift tolerance The stop delay time Min. and max. titration time [g/min]] [g/min] [g/min] [s] [min]
5.2 Volume and Weighted sample

On delivery the sample/weighted sample is set to no. If the result is to be calculated in ppm or %, it is necessary to enter a sample amount. A weighted sample can be entered manually as mg-value and a volume as ml-value. If an analytical balance is connected to the titrator, the weighted sample should be change to Weighted automatic. Now, you can transfer the weighted sample directly to the titrator via a keystroke at the balance. ( Fig. 37)
* *
Fig. 37
Method 01 * V o lu m e / w e ig h t * Weight manual W eight automatic Volume manual None Selection < > Enter<F1> ESC<F4>
With the method blank value the method parameter sample/weighted sample is not activated, since it is worked without weighted sample/sample and the result is always calculated in g.
With the Volume manual it is necessary to add the substance with a calibrated syringe (e.g. Hamilton).
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5.3 Result Formula

Method 01 * Result * Formula Unit Decim als Statistic Selection < > Enter<F1> ESC<F4> * *
Via the method parameter menu ( Fig. 36) you can go to the result-menu ( Fig. 38). With <ENTER> and/or <F1> you can reach the formula editor ( Fig. 39).
Fig. 38
Fig. 39
Method 01 * (g-B)*D*F1*F2/EW * F1 F2 Density (D) Blank (B) Selection < > Enter<F1> ESC<F4>
* *
2 different formulas are used in the titrator TitroLine KF trace. The formula displayed in Fig. 39 is only used for methods 01-09.
* * F1 F2
Method 10 g*F1*F2
* *
The blank value method 10 uses a simple calculation formula for g ( Fig. 40).
Fig. 40
Selection < > Enter<F1>
ESC<F4>
The following items mean in detail: g Absolutely measured water value in g F1 Conversion factor, default value = 1,000 F2 Conversion factor, default value = 1,000 Density D Density of the sample/standard. Default value is 1,00 g/ml Blank value B In g. Default value = 0,000 g EW Weighted sample in mg or volume in ml, default value = 1,000 With the methods 01-09 an internal (not visible!) conversion factor is calculated for the selected units ppm and %. Thus, the result is calculated correctly and additional inputs are not necessary. With method 10 (blank value) the result can only be calculated in g. Input Numerical Values
* * Method 01 Formula: Value F1 * *
001.000
Fig. 41
Input < > Enter<F1> ESC<F4>
Input with keypad at the titrator TitroLine KF trace: By means of the key the desired place can be selected. With and it is possible to edit the numerical value. With <F1> the input is confirmed. Input with a connected PC-keyboard: Simply enter the numerical value by means of the numerical keys. With <Backspace> an individual numerical value can be deleted. With <ENTER> the input is confirmed.
72
5.4 Result Unit

* * Method 01 * Result * Formula Unit Decimals Statistic Selection < > Enter<F1> ESC<F4>
Via the menu method parameter ( Fig. 36) you can go to the result menu ( Fig. 42). With <> and <F1> and/or <ENTER> you can go to the submenu Unit ( Fig. 43).
Fig. 42
* *
Method 01 Unit
* *
Possible units are %, ppm, mg ( Fig. 43)
Fig. 43
% ppm mg Selection < > Enter<F1>
ESC<F4>
* *
Method 01 U nit
mg/l, mg/pc (pc = piece) and g ( Fig. 44).
Fig. 44
mg/l mg/pc g Selection < > Enter<F1>
ESC<F4>
5.5 Result Decimal Places

* * * Method 01 Number of Decimals 1 * * *
Fig. 45
Input < > Enter<F1> ESC<F4>
From the result menu ( Fig. 42) you reach the decimal places menu ( Fig. 45). Here, the decimal place of a result can be edited with <> or <> and/or by directly entering the numerical value. For all methods the default value is 1. Up to 3 decimal places are adjustable. With <F1> or <ENTER> the input can be confirmed.
5.6 Result Statistics

* * * Method 01 Statistic Average of 01 Titrations Selection Enter<F1> < > <ESC><F4> * * *
Fig. 46
From the result menu ( Fig. 42) you reach the statistics menu ( Fig. 46). If you want to calculate a samples average value from multiple analyses, here the number of all single measurements is to be entered. With a double analysis the numerical value to be entered would be 2. The default value is 1 for all methods. Additionally, with a connected printer it is possible to print the standard deviation (SD) and the relative standard deviation (RSD).
73
5.7 Documentation
* Method 01 *
Fig. 47
Volume/weight Result Documentation Titration parameters Auswahl < > Enter<F1> ESC<F4>
With <F2> (and/or <F3 with an external keyboard) you can go from the main menu to the method parameters menu ( Fig. 47). From there you can go to the documentation menu by pressing <> twice and <F1> or <Enter> ( Fig. 48).
* *
Fig. 48
Method 01 * Documentation * Short Standard (with curve) GLP Only display Selection < > Enter<F1> ESC<F4>
* * Method 01 D o c u m e n t a t io n Print Method * *
There, it is possible to choose between four different types of documentation forms. The preset value is Short. The display always shows the water content, the mean value of the water content and the current drift. The same applies to the other documentation forms.
The currently selected method can be printed separately. ( Fig. 49).
ESC<F4>
Fig. 49
Print out short form:
Print out standard with curve:
74
Print out GLP
Print out Method
75
5.8 Titration Parameters
Method 01
Fig. 50
V o lu m e / w e ig h t Result Documentation Titration parameter Selection < > Enter<F1> ESC<F4>
You can go with F2 (and/or F3 with an external keyboard) from the main menu via the method parameters ( Fig. 50) to the titration parameters by pressing 3 times <> and <F1> or <Enter> ( Fig. 51).
Fig. 51
* T i t r a t io n c o n t r o l * * * S t a r t d r if t Stop drift Stop drift tol. Stop delay time Selection < > Enter<F1> ESC<F4>
Titration parameters are those parameters with which it is possible to control the titration process. Thus, they are also called control parameters. Fig. 52 shows the first 4 titration parameters.
* *
T i t r a t io n c o n t r o l
* *
M in t i t r a t i o n t i m e Max titration time Selection < > Enter<F1>
With 1 times <> or 4 times <> the remaining 2 titration parameters can be reached ( Fig. 52).
Fig. 52
ESC<F4>
Start Drift The value of the start drift in g/min must be equal or even lower in order to start a titration. If the value is exceeded, the TitroLine KF trace is in the conditioning mode. The standard value is 10,00 g/min. This value can be entered from 0,01 to 250 g/min. Stop delay time Is the time in seconds in which the drift-stop criteria are being checked. The stop delay time can be set between 0 and 60 seconds. The preset standard value is 5 s. Stop Drift The stop drift in g/min is not an absolute end value. The end value of a titration is always the currently measured drift + stop drift. An example: If the current drift shows a value of 1,5 g/min and the stop drift is set to 2,0 g/min, then the end drift actually to be reached is 3,5 g/min. This means: The lower the entered stop drift, the longer takes the measurement. If a high stop drift (e.g. 20 g/min) is entered, the measurement ends significantly faster. Low value = exact measurement, high value = inexact measurement. As stop drift 2 g/min are preset as standard value. The value can be entered from 0,01 to 25 g/min. Diagram 1 shows on the left the titration curve with the measured variable water per time and the derived variable drift per time.
76
Water and Drift 160 140 120 100

Water
Drift and Drift tolerance

700 600 500
Drift
Drift
700 600 500 400 300 200 100 0 0 20 [s] 40 60
500 400 300 200 100 0

Drift tolerance
400 300 200 100 0 0 20 [s] Water [g] Drift [g/m in] 40 60
80 60 40 20 0
Drift [g/min]
Drift Tolerance [g/min2]
Diagram 1: Water and drift on the left, drift tolerance on the right Stop Drift Tolerance If the drift change is within the stop drift tolerance during the entire follow-up time, the measurement will be ended.
As stop drift tolerance 0,01 g/min is preset as standard value. The value can be entered from 0,01 to 25,00 g/min. In case the drift stop has not been reached as criterion, as new stop criterion is the stop drift tolerance will be used. It is the derivative of the drift with respect to time. Diagram 2 shows the typical progression of the stop drift tolerance. Thus, the automatic stop of titrations with side reactions is possible.
Diagram 2: The criterion stop drift as difference to the start drift, the stop drift tolerance as stability criterion for the drift. Only one of the two end criteria stop drift and stop drift tolerance must be met to end the measurement.
77
Min. Titration Time After the minimum titration time has passed, the adjusted stop criteria are checked. The min. titration time can be adjusted from 0,1 to 30,0 minutes. The standard value is preset to 0,5 minutes for all methods. Particularly when worked with a baking oven the minimum titration time must be higher. Max. Titration Time The maximum titration time is used with samples that generate an increased drift in the end and when it is not possible to achieve stable end values. The max. titration time can be adjusted from 0,0 to 60,0 min. The standard value is preset to 10,0 min. for all methods.
5.9 Result Re-calculation

Method 01 * Result * Formula Unit Decimals Statistic Selection < > Enter<F1> ESC<F4> * *
From the method parameter and the result menu ( Fig. 53) you can go to the menu New caclulation by repeatedly pressing or better 1 x ( Fig. 54)
Fig. 53
* *
Method 01 Result New calculation
* *
In the menu New caclulation you can reset the statistics memory (Reset Statistics), delete one or more values of a multiple analysis (Correction Mean Value) and enter a new weighted or a new volume. ( Fig. 55)
Fig. 54
ESC<F4>
Method 01 * N e w c a l c u la t io n * R e s e t S t a t is t ic Correct mean New weight New volume Selection < > Enter<F1> ESC<F4> Fig. 55
* *
By selecting Yes in the field reset statistics the statistics memory can be reset. With No the display automatically goes back into the New caclulation menu list.
3 * * *
Method 01 N ew c a lc u la tio n C o rrec t m e an Delete sample No.01
* * *
Fig. 56
ESC<F4>
By deleting a value from a measurement series the mean value, the absolute and relative standard deviation are newly calculated. It is recommended to thoroughly think about deleting a result of a multiple analysis. In case of doubt it is better to carry out a new experimental series. After the number of the value to be deleted from the measurement series (1-10) has been entered and confirmed, the values are automatically recalculated.( Fig. 56)
78
* *
Methode 01 New calculation new weight
* *
00160.40
Fig. 57
Input < > Enter<F1> <Del> ESC<F4>
A result correction is necessary if e.g. a weighted sample or a sample has been entered incorrectly. After the input ( Fig. 57) of the new weighted sample in mg or the sample in ml a new result is automatically be calculated and output in a display or a connected printer (Option).
System Configuration
Method 01 Start Selection Edit paramater
* <Start> <Mode> <F2> 0 ppm 0 ppm g/min
From the main menu ( Fig. 58) you can go to the menu method selection with Mode/F4 (or ESC with an external keyboard) ( Fig. 59).
Water Mean Drift
Fig. 58
* M e t h o d s e le c t io n * M e th o d 01 M e th o d 0 2 M e th o d 0 3 M e th o d 0 4 M e th o d 0 5 Selection < > Enter<F1> ESC<F4>
By pressing the arrow key <> 1 x you get to the system settings ( Fig. 60).
Fig. 59
Methoden selection System settings
Please confirm the selection with F1 or <Enter>. Now the first menu of the system settings appears. ( Fig. 61).
Fig. 60
ESC<F4>
S ys t e m s e t t i n g s
Fig. 61
Language Device parameters System information RS232 Configuration Selection < > Enter<F1> ESC<F4>
Language settings are described in Chap. 4.3. Here you can see the device parameter settings, the system information and the configuration of the RS232-interfaces. By repeatedly pressing the arrow key <> you can go to the 2nd configuration menu Fig. 62).
79
S ys t e m s e t t i n g s R eset Time/date Password
Here it possible to carry out a RESET, to adjust Date and Time, and to activate a Password.
Fig. 62
ESC<F4>
6.2 Device Parameters

* S y st e m se t t i n g s * D ev i ce p ara m ete rs Working point Control factor Current cal. factor Selection < > Enter<F1> * *
From the 1st configuration menu you can get to the so-called Device Parameters. ( Fig. 63). Caution! The device parameters should only be changed and/or adjusted in case of servicing.
Fig. 63
ESC<F4>
* *
S y s t e m s e t t in g s W o r k in g p o i n t *
0300 mV
Selection < > Enter<F1> ESC<F4
The working point ( Fig. 64) in mV is the base value for the indicator electrode. It can be set from 1 to 1000 mV. 300 mV is preset as standard value.
Fig. 64
* * S y s t e m s e t t in g s C o n tro l f a c to r* *
004
Input < > Enter<F1> ESC<F4
The control factor ( Fig. 65) is a factor for the indicator control. It can be set from 1 to 128. The preset value is 4.
Fig. 65
* S ys t e m s e t t i n g s * * C u r r e n t c a l ib r a t io n f a c t o r 0.001860 Input < > Enter<F1>
The current calibration factor ( also predefined.
Fig. 66) is
Fig. 66
ESC<F4>
80
6.3 System Information

* S ys t e m s e t t i n g s *
From the 1st configuration menu ( Fig. 67) you can call up the system information. ( Fig. 68).
Fig.67
Language Device parameters System informationen RS232 Configuration Selection< > Enter<F1> ESC<F4>
T i tro L i n e K F trac e S o f t wa re Serial no. Address Meas. No. Back <F4> 0 7 /45 a 00739001 01 125
There you find the version number of the software as well as the serial number and the physic address of the devise. The measurement number indicates the number of titrations carried out so far.
Fig. 68
6.4 Configuration RS-232

* * System settings * Configuration RS232 *
Fig. 69
Address RS232-I (printer/PC) RS232-II (balance) Selection < > Enter<F1> ESC<F4>
From the 1st configuration menu ( Fig. 67) you can go to the configuration menu of both serial interfaces RS232. ( Fig. 69) The two RS-232-interfaces of the titrator TitroLine KF trace can be configured differently if it is necessary to configure a connected balance differently from a connected printer.
The device address is preset to 01. It is configurable from 00 up to address 15. It can be changed if several devices are interlinked (Titrator TitroLine KF trace, piston burettes TITRONIC universal etc.), see also Chap. 8.2 On delivery both RS-232-interfaces are preset to the following parameters: Baud rate: 4800, Parity: No, Data: 8. The baud rate can be set from <1200> to <19200>. Parity can be set from <No> to <Even> or <Odd>. The data bits Data can either be set to <7 Bit> or to <8 Bit>.
6.5 Reset
* * System settings Reset Yes No Selection < > Enter<F1> ESC<F4> * *
From the 2nd configuration menu ( Fig. 62) you can go to the Reset mode ( Fig. 70). By confirming <Yes> the reset will be started. The device is reset to its delivery status.
Fig. 70
81
6.6 Date and Time

* * System settings Time/Date
Time Date 11:11:36 11:11:07
* *
From the 2nd configuration menu ( Fig. 62) you can go to the Time and Date Settings. ( Fig. 71). If the time or date are to be corrected, please select the respective menu item and confirm with <Enter> or <F1>.
Fig. 71
ESC<F4>
* *
System settings Edit time

12:00:36
* *
Fig. 72
Selection < > Enter<F1> ESC<F4>
The date is shown in the form hh:mm:ss. ( Fig. 72) keypad: The value to be changed is to be selected with the - key and can be edited with the keys . The input is completed with <F1>. External keyboard: The entire time is to be entered completely in a row. The date is shown in the form tt:mm:jj. ( Fig. 73) keypad: The value to be changed is to be selected with the - key and edited with the keys . External keyboard: The entire date is to be entered completely in a row. The input is completed with <Enter>.
* *
System settings Edit date

11.11.07
* *
Fig. 73
Selection < > Enter<F1> ESC<F4>
6.7 Password
* * S ys t e m s e t t i n g s P a s sw ord * *
From the 2nd configuration menu ( you can go to the password menu (
Fig. 62) Fig. 74).
P a s s w o rd o f f P as s w ord o n
Fig. 74
ESC<F4>
* *
S y st e m se t t i n g s P a ssw o r d D ef i ni ti on o f u se r
* *
Fig. 75
F ra nk Z ap pa Input < > Enter<F1>
If you have selected <Password on>, you first have to enter a User. The easiest way is to use a connected PC-keyboard, but you can also use the arrow keys and/or . The maximum number to be entered is 20 characters. The input is to be confirmed with <F1> or <Enter>.
ESC<F4>
82
* S y s t e m s e t t in g s * D e f i n it io n o f n e w p a s s w o rd : *************** Input < > Enter<F1>
Fig. 76
ESC<F4>
The next step is to enter a password. The password must have at least 6 characters (alphanumeric!). Maximum length is 20 characters. The input must be repeated for 1 x. The password will be requested every time you request access to the method parameters and the configuration. The password can easily be deactivated with Password off.
83
Basics and Working Information
7.1 Theory
In coulometry, the KF solution contains iodide. This iodide will be oxidised to iodine at the anode of the generator cell. At the cathode, in parallel thereto, mainly hydrogen will be generated which will mount in the form of small bubbles to the surface and hence become withdrawn from the balance. The iodine being generated reacts immediately with the water according to the Karl Fischer reaction. During the entire titration process, only iodide is present in the solution. This will change all at a sudden as soon as no more water is left in the titration cell. As a result of the further addition of iodine, iodine and iodide will be coexisting in parallel and form a reversible redox pair A voltage is applied to the indicator electrode, and this will cause the iodide to release its electron at the positive anode, and iodine will form. At the cathode, the electron will again be passed on to the iodine, and again iodide will form. In this way, it is possible to measure a current which will detect the end of the reaction. However, this occurs only directly at the surface of the two platinum pins which means that no iodine can react with the water of the sample. In volumetric titration, the iodine is dosed using a motor piston burette, but the detection of the end of titration is identical ( Fig. 77)
Fig. 77
84
7.2 Work flow

Immediately after power-up, the coulometer will start to condition the reagent in the titration cell. Therefore, the anolyte has to be filled in the titration vessel always prior to power-up. In the generator electrode, hydrogen will be formed at the cathode, whereas iodine will form at the bottom of the anode of the generator electrode ( Fig. 78)
Fig. 78 The minimum filling height inside the titration vessel should be 3 cm so that the generator electrode is properly immersed ( Fig. 79): The maximum filling height is 1 cm below the vessels top. The stirring speed should be adapted manually to the filling height. However, the minimum setting of the speed should not be less than stage 3-3.5.
Fig. 79. Within a short time, as a function of the amount of humidity contained in the titration vessel, the drift will reach a stable value. Under normal conditions, this value will be between 0.5 g/min and 10 g/min. A drift below 0.5 g/min is indicative of a previous overreaction (e.g. caused by too slow stirring), whereas a too high drift indicates an intrusion of humidity or side reactions of a preceding sample. If an increased drift is stable over a couple of minutes, titration is nevertheless possible since a delta criterion, defined as a function of the initial drift, is input as a break criterion (please refer to titration parameters).
85
Fig. 80
Schematic flow Fill in anolyte/catholyte
Switch the titrator on!
Anolyte is conditioned
Start Titration
Place sample in titration vessel Next titration
Weighing-in and description
Titration is running
Results will be displayed or printed
7.3 Handling
The indicator electrode is placed in the titration vessel in the opening with the NS 7.5 and connected to the device using the two blue plugs. Use a funnel to fill in the reagent up to a minimum filling height of 3 cm. Subsequently, insert the generator electrode. Place a drying tube with a fresh dried molecule sieve (0.3 nm) on top of the generator electrode. Prior to that, the molecule sieve is to be dried at a minimum temperature of 250C for six hours. Use the enclosed cable to connect the generator electrode to the titrator, with the green plug connecting to the green socket and the black plug to the black one. Use a fresh septum to close the sample filling hole. The septum has to be impermeable to atmospheric humidity If you are using a generator electrode with a diaphragm, a funnel or a needle with syringe should be used immediately after the insertion of the generator electrode to fill the cathode reagent in the generator electrode up to the filling height of the anolyte. Apart from that, the working procedure is the same. Handling the sample using a one-way syringe Usually, samples are drawn up using a one-way syringe or a calibrated glass syringe and then injected into the titration vessel. In this context, the absolute water quantity per sample should be within the range of 20 g to 2000 g of water. If the water quantity is less than that, "accuracy" will decrees, if it is larger, the duration of the titration will increase. A water quantity of 2000 g will be titrated in less than two minutes. The following weighed-in quantities are recommended with the corresponding quantities of water in the sample: Water amount Unit Sample amount in the sample 10 ppm 1,0 - 10 100 ppm 0,5 - 5,0 1000 pm 0,1 - 1,0 1 % 50 - 500 10 % 5 - 100 100 % 1 - 10 Weighing-in of a sample, adding and weighing back Unit g g g mg mg mg Water amount [g] 10 - 100 50 - 500 100 1 000 500 - 5 000 500 - 10 000 1 000 - 10 000
86
If a sample is drawn up using a syringe, it has to be ensured that no air will be drawn through the sample. Depending of the atmospheric humidity, air may contain a lot of water, possibly even more than the sample itself. It is possible to rinse the syringe beforehand with the sample. The diameter of the needle is to be adapted to the viscosity of the sample. With low viscous samples, one should use a 0.8 or even a 1.0 mm needle. The larger the diameter of the needle, the more often needs the septum to be replaced. The low drift is a good indicator for a tight septum. Under normal conditions (small needle diameter), it is possible to titrate approximately 20-30 or even more samples using one septum. Place the syringe with a sample on the analytical balance, then tare the balance. The sample is dosed into the titration vessel, the syringe is put back on the analytical balance and weighed back. The weighed-in quantity, now with a negative sign, is input as absolute value in the titrator or automatically transferred, respectively. If a multiple determination is being carried out, it has proven in practice to draw the entire sample quantity into the syringe and then inject partial quantities of it into the titration vessel. As a rule, this will lead to smaller standard deviations compared to drawing up each small partial quantity anew. The main reason for this is found in the risk of taking up atmospheric humidity from the air. Generally, it is also possible to use a calibrated syringe (e.g. from Hamilton) to add samples as a volume. As a matter of course, if the result is to be calculated in terms of ppm or %, the density of the liquid has to be taken into account. It may be input in the calculation formula.
7.4 Working techniques

A distinction is made between the following working techniques: o Direct addition of a sample using a syringe. o External extraction o Working with an oven Solid samples are usually not placed in the titration vessel, since this would involve a high frequency of the change of the reagent. Direct addition of a liquid sample using a syringe A standard is supposed to be used as an example to illustrate the working method. Open the ampoule by breaking off its tip (point away from user ). Subsequently, place the open ampoule back in the pack with the opening pointing up. Now, use a 5 ml one-way syringe and a 80 mm long needle with a diameter of 0.8 mm to draw up approximately 5 ml of standard. Prior to that, one should rinse the syringe one or two times using 1 ml of standard in order to dry it ( Fig. 81).
Fig. 81
87
Place the filled syringe on the balance as illustrated, then tare the balance ( Fig. 82). On the Titroline KF trace, the method is started by pressing the Start key.
Fig. 82 Subsequently, a part of the syringe contents, for instance approx 1 ml, is injected into the titration vessel ( Fig. 83). The syringe containing the residual quantity of standard solution is weighed back, the quantity reading is input as weighed-in quantity on the coulometer ( Fig. 84).
Fig. 83
0010.00
Input Enter < > <F4> ESC<F4>
If the analytical balance is connected to the KF Trace, pressing the Print key will automatically transfer the weighed-in quantity. Subsequently, titration will begin automatically
Fig. 84
88
At the end of titration, the result will automatically be printed out according to the settings made ( Fig. 85)
Fig. 85
External extraction is used in the following cases: o If the water is extracted from the sample only slowly o If one has to reckon with side reactions. o Frequently in the case of solid samples o If a special solvent has to be used The description of external extraction can be found in an additional document. If required, please feel free to contact us.
7.5 Verification
The verification of the coulometer is done using a standard. We recommend the use of liquid standards with percentages of 0.1 mg of water per gram up to 1 mg of water per gram Recovery is determined by a multiple determination of a standard. The mean value and the relative standard deviation are determined. Triple up to tenfold determinations are usual. The mean value reflects the recovered value of the standard. The relative standard deviation indicates the reliability of the determination. Typical values of a standard with 1 mg of water / g of standard with a weighed-in quantity of 0.5000 g up to 2.0000 g are given below: Recovery: 950 - 1050 ppm (97% - 103%) Reproducibility: +/- 30 ppm (SD); +/- 3 % (RSD) Linearity can be performed in the same working step if weighing-in was made using different quantities. Using the 1 mg of water / g standard, the weighing-in operations can start at 0.5 g to be increased, for instance, up to 2.0 g in six steps. The correlation coefficient and the zero passage may be used as check parameters. The example below shows weighing-ins of approximately 500 to 1500 mg of water standard. Recovery and relative standard deviation are within the range of acceptance.
89
Weight-in quantity [mg] Water [mg] 550 552 640 646 765 772 873 878 979 985 1085 1096 1209 1219 1312 1320 1408 1418 1532 1542 Mean value RSD
Water [%] 100,4 100,9 100,9 100,6 100,6 101,0 100,8 100,6 100,7 100,7 100,7 0,2
7.6 Tips and Tricks

It takes a long time until the drift displays small values (< 8l/min) The TitroLine KF trace is switched on, the drift shows value below 100 l/min. Switch the stirrer off. After approx 5 seconds, iodine will be generated at the anode. Considering that no stirring action is present, there is no feedback from the indicator electrode ordering to stop iodine production. After a few seconds, start the stirrer; you may also shake the titration vessel if required. After the distribution and reaction of the iodine with the residual water, the drift ought to have dropped down to 0 l/min. Please note: as a matter of course, this drift is not real, which means one has to wait a little until the real drift between 0.5 and 5 g/min will be displayed.
Speed up the drying process of the titration vessel. In order to speed up the drying process, use a one-way syringe to add so many drops of KF single component reagent 5 mg/millimetre until a slightly yellowish colour becomes visible. The drift will drop to a typical value below 100 l/min. If a drift of 0 l/min is being displayed, overtitration has occurred. By adding some drops of methanol or ethanol, it is now possible to add a small quantity of water again. Drift to high (permanent values > 10 l/min) o o o o Dry or replace molecular sieve Clean all ground faces, use a grease at the top edge. Replace septum Renew anolyte or catholyte
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Data Communication via RS-232-and USB Interfaces

The titrator TitroLine KF trace has two serial RS-232-C- interfaces to communicate data with other devices. By means of these two interfaces it is possible to operate several devices on one computer (PC) interface. In addition to that, the TitroLine KF trace also has a USB-interface, which can only be used to connect a PC. RS-232-C- 1 establishes the connection to a connected computer, a printer with a serial interface or to the previous device of the Daisy Chain. At the RS-232-C- 2 it is even possible to connect additional devices (Daisy Chain Concept). PIN-assignment of the RS-232-C- interfaces: PIN-No. 1 2 3 Meaning / Description T x D Data output R x D Data input Digital mass
8.2 Chaining of Several Titrators TitroLine KF trace Daisy Chain Concept

In order to activate several devices in a chain individually, each device must have an own device address. For this it is at first necessary to establish a connection from the computer to the RS-232-C- interface 1 of the first devise in the chain by means of a RS-232-C- data cable, e.g. Type No. TZ 3098. With the additional RS-232-C- data cable, Type No. TZ 3094, the RS-232-C- interface 2 of the first device is connected with the RS-232-C-interface 1 of the second device. At interface 2 of the second device it is possible to connect an additional device. The address always consists of two characters: e.g. address 1 of the two ASCII- characters <0> and <1>. The addresses can be set from 00 to 15, i.e. 16 possibilities. It must be ensured that the devices in a chain have different addresses. If a device is addressed with its address, this device will process this command without sending it to another device. The reply to the computer has also an own address. The addresses are allocated as described in Chapter 6.4. The titrator TitroLine KF trace receives from a computer the commands (if provided with the titrators address) at interface 1 and then sends its reply via the same interface. If the address of the incoming command does not correspond to the titrators device address, the entire command will we redirected to interface 2. This interface 2 is connected to interface 1 of an additional device. This device checks now the address and responds to this command like the first titrator TitroLine KF trace. All information (data strings) which arrive at interface 2 of the titrator TitroLine KF trace will immediately be send to the computer via interface 1. Thus, the computer receives the data of all devices. In practice it is possible to connect up to 16 devices to one computer- (PC-) interface.
8.3 Instruction Set for RS-Communication

The commands consist of three parts: Address two-digit aa, e.g.: 01 Command e.g.: BP Variable, if necessary e.g.: 14 and end of command <CR> <LF> Every command must be completed with the ASCII - sign <CR> and <LF> (Carriage Return and Line Feed). Only if the respective action has ended the answers will be returned to the computer. Example: The command to dose 12,5 ml, with the previous filling of the cylinder and zero points of the display, shall be sent to a flask burette with the address 5. The command consists of the characters: 05DO12.5<CR LF> In detail: 05 = Device address DO = Dosage command with filling and zero points of the display 12.5 = Volume in ml to be dosed <CR LF> = Control character as command end
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Command
aaKA aaKD aaKE aaMC1...XX aaM aaMT aaLD
Description
What key is pressed? Keyboard disabled Keyboard enabled Selection of a method Measuring value in ug water Condition measuring value Time from start and/or titration For online graphic Output measuring value (indicator, electricity, drift, Electricity raw data value) Output current drift Output content of methods Output documentation Output result (short form) Output device parameter (calibration factor, Operating point, control factor) Send sample quantity Requirements of identification Send last command Report status Possible status answers are: titration, cond, ready, Continue after stop / continue the function after stop Start of selected method Send calibrating factor Adjust working point Adjust control factor Test current generator by giving a control point Disable conditioning Enable conditioning Write string into nth matrix line: the string to be written with TEXT (Limit number of characters to 21) as delimiter attach command: e.g.: 01SD1 Please start titration Delete display entirely Switch on display entirely Reset EEPROM to factory data Stop of function currently running Set display language to German Set display language to Englisch -EnglishSet display language to Franzsisch -FranaisSet display language to Spanisch -EspaolVersion number of software Set serial number Request serial number
Answer
AaKey:Text aaY aaY aaY aaM108.5ug aaMT108.5ug,10s aaLD298.4mV, 0.5mA, 2.7ug/min,272 aa0,5 g/min
aaDV aaLI aaLO aaLR aaLDP
aaSAM10.05mg aaRH aaRC aaRS aaSC aaSM aaSCAL0,00186 aaSWP300.0mV aaSCF4 aaGEN1000 aaCOD aaCOE aaSD1..8
aaLDP0.00186, 300.0mV,4 aaY aaIdent:TL KFC aaletzter Befehl aaStatus:text aaY aaY aaY aaY aaY aaY aaY aaY aaY
aaST0 aaST1 aaSEEPROM aaSR aaSYS5 aaSYS1 aaSYS2 aaSYS3 aaVE aaSS00625521 aaGS
aaY aaY aaY aaY aaY aaY aaY aaY aaVersion:07.01 aaY aaGS00625521
92
Connection of Analytical Balances and Printer
9.1 Connection of Analytical Balances

As it often happens that the sample is weighed in on an analytical balance, it makes sense to connect this balance to the titrator TitroLine KF trace. To connect the balance to the titrator TitroLine KF trace, the balance must have a RS-232-C-interface and the connection cable must be configured accordingly. For the following types of balances there are already assembled connection cables: Balance Sartorius (all types), partially Kern Mettler AT, PR, PM Mettler, AB-S, AG, PG Precisa XT-Series Kern with 9-pole RS232 TZ-Number TZ 3092 TZ 3093 TZ 3099 TZ 3183 TZ 3180
For all other types of balances it is possible to obtain an already assembled connection cable (on demand). For this we need detailed information about the RS-232-C-interface of the balance used. The connection cable is to be connected to the RS-232-C-interface 2 of the titrator TitroLine KF trace. This side of the connection cables always consists of a 4-pole mini-plug. The other side of the cable can, depending on the type of balance, be a 25-pole plug (Sartorius), a 9-pole plug (Mettler AB-S) or a 15-pole specialised plug (Mettler AT) etc. In order to allow the balance data to be sent to the titrator, the data transmission parameters of the titrator and the balance must correspond to each other. Additionally, it is necessary to carry out some more standard settings on the side of the balances: The balance is to send the balance data via RS-232-C only by means of a print command. The balance is to send the balance data only after the display standstill. The balance should never be set to automatic sending and/or send continuously. Handshake on the balance must be set to off, or even Software Handshake or Pause. No special characters such as S or St are allowed to be used as prefix in the balance data of the balance data string. In such a case it might be possible that the TitroLine KF trace cannot process the balance data correctly. After you have connected the balance with the appropriate cable to the titrator TitroLine KF trace and have adjusted all settings in the balance software, and possibly in the titrator TitroLine KF trace, you can now test the data transfer of the balance very easily. Start the one method. Confirm the sample designation. Then, the display asks you: a) To press the print-button at the balance Parameters to weighted sample automatically b) To enter the weighted sample then the parameters are still set to weighted sample manually Put an object onto the balance and press the print button. After the standstill of the balance display there will be beep at the titrator TitroLine KF trace and the transmitted balance data appear: a) After approx. 5 sec. in the display and the display changes automatically into the measuring display. b) The weighted sample must again be confirmed with <Enter> or <F1>.
9.2 Connection of Printers

It is possible to connect a printer with a RS-232-C-interface, such as the Epson LQ 300, to the serial interface 1 of the titrator TitroLine KF trace. Here we need a data cable TZ 3095 (25-pole interface). To send the results and additional data to the printer, the data transmission parameters of the titrator and the printer must correspond to each other. The transmission parameters of the printer TZ 3461/TZ 3466 by SCHOTT Instruments are already correctly configured and the data cable TZ 3090 is included in delivery of the printer.
93
10 Trouble Shooting
The device does not react to keystrokes, the display is dark. Failure Solution The internal program is defective Switch off device and restart after 10 s (e.g. due to electrostatic charge or grid overvoltage) The contrast of the display is misaligned Adjust contrast at milled screw down right
The data transmission to the printer / computer is not working. Failure Solution Adjust transmission parameters properly Setting: 4800 baud, 7 data bits, no parity, Used cable does not fit Use TZ 3090 for printer TZ 3461/TZ 3466 and/or TZ 3097/TZ 3091 for PC Cable not properly connected The upper 4-pole jack is the RS-232-C-interface 1 Check cable connection, screws on PC side tightened On side of PC COM 1 and COM 2 might be interchanged Cable defective Replace cable Printer / PC or TitroLine KF trace Switch off device and restart after 10 s malfunctioning
The titration process is too slow or does not work at all. Failure Solution No or too less Iod produced at the Check if generator electrode is connected properly. Observe generator electrode colour codes of plug Exchange anolyte. If necessary exchange catholyte Clean generator electrode with water and/or suitable solvents (e.g. alcohol). With heavy pollution it is possible to use chrome sulphuric acid. (See also Chapter 7 and 11) Check if indicator electrode is properly connected and if both platinum pins do not touch each other. Iod is produced within the generator Check if generator electrode is connected properly. Observe electrode and not down at the platinum colour codes of plug wire
94
11 Maintenance and Servicing of the Titrators TitroLine KF trace

To maintain the functional capability of the titrator TitroLine KF trace it is necessary to carry out all testing and maintenance works. Wear Notes Generator electrode When the generating electrode is heavily soiled a cleaning with HNO3 (65 %) is recommended. Rinse the electrode with dest. water and alcohol afterwards and let it dry in a cabinet dryer at 80 C. Interruptions of use If the TitroLine KF Titrator is not used for more than one week it is recommended to remove the liquids from the titration vessel and if necessary from the generating electrode. Rinse the titarion vessel and electrodes with dest. water and alcohol afterwards and let it dry in a cabinet dryer at 80 C. When the titration vessel is heavily soiled it can be cleaned with a standard laboratory detergent. Rinse the titarion vessel and electrodes with dest. water and alcohol afterwards and let it dry in a cabinet dryer at 80 C. Cleaning The titrator TitroLine KF trace is to be cleaned with a wet cloth and common household cleaning agents. Both under and back side must be treated dry. The liquid must not enter the housing of the titrator TitroLine KF trace.
12 Storage, Transport and Environmental Concerns

If the titrator TitroLine KF trace is to be put into interim storage or must be transported, the best way to protect the device is to use the original packing. However, in many cases this packing is not at ones fingertips, so it is recommended to use an equivalent packing.
Previously it must be ensured that the KF-reagent has been removed from the titration vessel/generator electrode. Subsequently, it is to be rinsed with alcohol (ethanol, isopropanol) which must then also be removed.
As storage location we recommend rooms which have the following conditions: Temperature between + 10 and + 40 C for operation and storage, Humidity according to EN 61 010, part 1: Maximum relative humidity 80 % for temperatures up to 31 C, Linearly decreasing to 50 % relative humidity with a temperature of 40 C Your titrator TitroLine KF trace will certainly have a long service life. However, it is necessary to mind the following advice: If it is necessary to dispose your device, please observe all official regulations of your country and/or city.
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13 Accessory and Spare Parts

Accessory
TZ 1052 TZ 1060 TZ 1751 TZ 1752 TZ 1753 TZ 1754 TZ 1795 TZ 2835 TZ 3461 TZ 3466 Drying oven to determinate water according to KF Set of accessory for drying oven TZ 1052 Titration vessel with 3 openings Generator electrode without diaphragm Generator electrode with diaphragm Titration vessel with 5 openings for TMKF and/or connection KF oven Adaptor for solvent and disposal bottle with S 40 thread PC-keyboard Printer with RS-232-C- interface, including 1,5 m printer cable TZ 3090, 230 V Printer with RS-232-C- interface, including 1,5 m printer cable TZ 3090, 115 V with plug for printer connection of printer TZ 3461/66: 1st side: 4-pole plug mini DIN 2nd side: western plug for connection to Sartorius balances 1st side: 4-pole plug mini DIN 2nd side: 25-pole plug (balance) for connection of Mettler AT, PR, PM balances 1st side: 4-pole plug mini DIN 2nd side: 15-pole plug (balance) for connection of Mettler PG, AB-S, AG balances 1st side: 4-pole plug mini DIN 2nd side: 9-pole plug (balance) TitroLine KF trace TitroLine KF trace Daisy Chain concept 1st side and 2. Side: 4-pole plug mini DIN with plug for printer connection (e.g. Epson LQ 300): 1st side: 4-pole plug mini DIN 2nd side: 25-pole plug sub-miniature-D 2nd side: 9-pole jack sub miniature 1st side: 4-pole plug mini DIN 2nd side: 9-pole jack sub miniature D 9-pole plug 25-pole jack
TZ 3090 1,5 m data cable RS-232-C
TZ 3094 1,0 m data cable RS-232-C:
TZ 3098 1,5 m data cable RS-232-C: Adaptor:
Spare Parts
KF 1150 Micro-double-platinum-electrode
Notes
Typ / Type / Type / Tipo:
Titrator TitroLine KF trace
Bescheinigung des Herstellers Wir besttigen, dass das oben genannte Gert gem DIN EN ISO 9001, Absatz 8.2.4 berwachung und Messung des Produkts geprft wurde und dass die festgelegten Qualittsanforderungen an das Produkt erfllt werden.
Suppliers Certificate We certify that the equipment was verified according DIN EN ISO 9001, part 8.2.4 Monitoring and measurement of product and that the specified requirements for the product are met.
Certificat du fournisseur Nous certifions que le produit a t vrifi selon DIN EN ISO 9001, partie 8.2.4 Surveillance et mesure du produit et que les exigences spcifies pour le produit sont respectes.
Printed in Germany
SCHOTT Instruments GmbH Postfach 24 43 55014 Mainz Hattenbergstrae 10 55122 Mainz
Tel.: +49 (0)6131/66-5111 Fax: +49 (0)6131/66-5001 E-Mail: titration@schottinstruments.com www.schottinstruments.com
EDV 008272298
Version 080807 M

Manual KF

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Gebrauchsanleitung

Titrator TitroLine KF trace Titrator TitroLine KF trace Titrateur TitroLine KF trace

Gebrauchsanleitung ............................................................................................................. Seite 1 . 47

Operating Instructions ...................................................................................................... Page 49 . 95

Mode demploi ................................................................................................................... Page 97 .. 143

Characteristics of the Titrator TitroLine KF trace ............................................50

Warning and Safety Advises..............................................................................54 Installation and Initial Operation .......................................................................55

Working with the Titrator TitroLine KF trace....................................................65

Method Parameter ..............................................................................................70

System Configuration ........................................................................................78

Basics and Working Information.......................................................................83

Data Communication via RS-232-and USB Interfaces.....................................90

Connection of Analytical Balances and Printer ...............................................92

Characteristics of the Titrator TitroLine KF trace

1.1 General Information

Signs used in the text and their meanings:

KONFORMITTSERKLRUNG DECLARATION OF CONFORMITY DCLARATION DE CONFORMIT

Wir erklren in alleiniger Verantwortung, dass das Produkt

We declare under our sole responsibility that the product

Nous dclarons sous notre seule responsabilit que le produit

Titrator TitroLine KF trace

SCHOTT Instruments GmbH Hattenbergstrae 10 55122 Mainz Deutschland, Germany, Allemagne

Country of origin: Display: Ports: Electrode:

Keyboard: TM 135/TM KF: Interfaces: RS-232-C

Materials: Housing: Front foil: Housing dimension:

15. Oktober, October 15 , 15 Octobre 2007 AGQSF 0000-A063-01/071015

Country of origin: Pump:

Stirring speed: Hoses:

Connections Power supply (top);:

Housing Material: Dimensions: Weight: Ambient conditions:

15. Oktober, October 15 , 15 Octobre 2007 AGQSF 0000-A063-01/071015

Warning and Safety Advises

Installation and Initial Operation

3.1 Unpacking the Titrator TitroLine KF Trace

3.2 Setting up the TitroLine KF trace

! The titrator TitroLine KF trace may not be used in explosive environments. !

Put the magnetic stirrer TM 135 next to the basic device.

Mount the retaining clip onto the tripod rod.

3.3 Connecting Power Supply, Electrodes and Accessory

3.4 Setting up of the Titration Stand TM KF and the Titration Vessel

Put the stand rod (

3.5 Filling the Titration Vessels

3.6 Switch on Device, First Conditioning

Working with the Titrator TitroLine KF trace

Water Mean Drift

* M e t h o d s e l e c t io n 1* M e th o d 0 1 M e th o d 0 2 M e th o d 0 3 M e th o d 0 4 M e th o d 0 5 Selection < > Enter<F1> ESC<F4>

Method 01 Conditioning ready Dose sample!

V o lu m e /w e ig h t Result Documentation Titration parameters Select < > Enter<F1> ESC<F4>

Selection <> Enter<F1>

Input < > Enter<F1>

4.1 Keys and Contrast

Keyboard of the TitroLine KF trace Fig. 21

4.2 Start Picture, Main Menu and Method Selection

Water Mean Drift

Method selection System settings

Selection <> Enter<F1>

4.3 Language Selection

4.4 Starting a Titration

Method 01 Conditioning ready Dose sample!

1 Enter ESC <F1> <F4> DEL

100 g/min ESC<F4>

W ater Mean Drift

5.1 General Information

V o lu m e / w e ig h t Result Documentation Titration parameters Selection < > Enter<F1> ESC<F4>