88518002EN Manual 851 Titrando

851 Titrando
Manual
8.851.8002EN
Metrohm AG CH-9101 Herisau Switzerland Phone +41 71 353 85 85 Fax +41 71 353 89 01 info@metrohm.com www.metrohm.com
851 Titrando
Manual
8.851.8002EN
09.2010 ek
Teachware Metrohm AG CH-9101 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://products.metrohm.com under Literature/Technical documentation.
Table of contents
Table of contents
1 Introduction
1.1 1.2 1.3
The Titrando system ............................................................. 1 Instrument description ......................................................... 2 Titration modes Measuring modes Dosing commands .................................................................................... 3
1.4 About the documentation ................................................... 3 1.4.1 Symbols and conventions ........................................................ 3 1.5 Safety instructions ................................................................ 4 1.5.1 General notes on safety ........................................................... 4 1.5.2 Electrical safety ........................................................................ 4 1.5.3 Working with liquids ................................................................ 5 1.5.4 Flammable solvents and chemicals ........................................... 6 1.5.5 Recycling and disposal ............................................................. 6
2 Overview of the instrument 3 Installation
7 9
3.1 Setting up the instrument .................................................... 9 3.1.1 Packaging ................................................................................ 9 3.1.2 Checks .................................................................................... 9 3.1.3 Location .................................................................................. 9 3.2 Connecting controller ........................................................... 9 3.2.1 Operation ................................................................................ 9 3.3 Connecting MSB devices ................................................... 13 3.3.1 Connecting dosing devices .................................................... 14 3.3.2 Connecting a stirrer or titration stand .................................... 15 3.3.3 Connecting a remote box ...................................................... 16 3.4 Connecting USB devices ..................................................... 17 3.4.1 General ................................................................................. 17 3.4.2 Connecting a printer .............................................................. 17 3.4.3 Connecting a balance ............................................................ 18 3.4.4 Connecting a PC keyboard (only Titrando with Touch Control) ....................................................................................... 20 3.4.5 Connecting a barcode reader ................................................. 20 3.4.6 Connecting a USB hub ........................................................... 22 3.4.7 Connecting a Bluetooth adapter .......................................... 22 3.5 Titration vessel for coulometric KF titration .................... 25 3.5.1 Mounting the coulometer cell ................................................ 25 3.5.2 Coulometer cell - Default setup ............................................. 26 3.5.3 Coulometer cell with addition and aspiration tube (use with Ti Stand) ................................................................................ 30
851 Titrando
III
Table of contents
3.5.4 3.5.5 3.5.6
Coulometer cell with aspiration equipment (use with Dosino) ....................................................................................... 31 Coulometer cell with KF oven ................................................ 32 Coulometer cell with Oven Sampler ....................................... 32
3.6 Connecting sensors ............................................................ 33 3.6.1 General ................................................................................. 33 3.6.2 Connecting generator electrode ............................................ 33 3.6.3 Connecting indicator electrode .............................................. 33 3.6.4 Connecting a temperature sensor .......................................... 34
4 Coulometric titration
4.1
36
Principle of the KF coulometry .......................................... 36
4.2 Working with water standards ......................................... 37 4.2.1 Certified water standards ....................................................... 37 4.2.2 Practical recommendations .................................................... 37 4.3 Sample addition .................................................................. 39 4.3.1 Sample size ........................................................................... 39 4.3.2 Working with liquid samples .................................................. 39 4.3.3 Working with solid samples ................................................... 40 4.4 Optimum working conditions ........................................... 41 4.4.1 General ................................................................................. 41 4.4.2 Drift ...................................................................................... 41 4.4.3 Reagent exchange ................................................................. 41 4.4.4 Indicator electrode ................................................................ 42
5 Handling and maintenance
43
5.1 General information ........................................................... 43 5.1.1 Care ...................................................................................... 43 5.1.2 Maintenance by Metrohm Service .......................................... 43 5.2 Generator electrode ........................................................... 44 5.2.1 Generator electrode without diaphragm ................................ 44 5.2.2 Generator electrode with diaphragm ..................................... 44 5.3 Quality Management and validation with Metrohm ....... 45
6 Troubleshooting
6.1 6.2
47
General ................................................................................ 47 Karl Fischer Titration .......................................................... 47
7 Appendix
49
7.1 Remote interface ................................................................ 49 7.1.1 Pin assignment of the remote interface .................................. 49
8 Technical specifications
53
8.1 Measuring interface ........................................................... 53 8.1.1 Generator electrode .............................................................. 53
IV
851 Titrando
Table of contents
8.1.2 8.1.3 8.2 8.3 8.4 8.5 8.6
Indicator electrode ................................................................ 53 Temperature .......................................................................... 53 Mains connection ............................................................... 54 Safety specifications ........................................................... 54 Electromagnetic compatibility (EMC) ................................ 54 Ambient temperature ......................................................... 55 Interfaces ............................................................................. 55
9 Conformity and warranty

9.1 9.2 9.3
56
Declaration of Conformity ................................................. 56 Quality Management Principles ........................................ 57 Warranty (guarantee) ......................................................... 58
10 Accessories
59
10.1 Scope of delivery ................................................................ 59 10.1.1 851 Titrando 2.851.0110 ...................................................... 59 10.1.2 851 Titrando 2.851.0010 ...................................................... 65 10.1.3 851 Titrando 2.851.0020 ...................................................... 72 10.2 Optionales Zubehr ............................................................ 79 10.2.1 851 Titrando 2.851.0010, 2.851.0020, 2.851.0110 .............. 79
Index
83
851 Titrando
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 The Titrando system .......................................................................... 1 Front 851 Titrando ............................................................................ 7 Rear 851 Titrando ............................................................................. 8 Connecting a Touch Control ............................................................ 10 Connecting a computer ................................................................... 12 MSB connections ............................................................................ 13 Connecting a dosing device ............................................................. 15 Connecting MSB stirrer .................................................................... 15 Rod stirrer and titration stand .......................................................... 16 Connecting a remote box ................................................................ 17 Connecting a balance ...................................................................... 19 Connecting a generator electrode ................................................... 33 Connecting an indicator electrode ................................................... 34 Connecting a temperature sensor .................................................... 34 Connectors of the remote box ......................................................... 49 Pin assignment of remote socket and plug ...................................... 49
VI
851 Titrando
1 Introduction
1 Introduction
1.1 The Titrando system
The Titrando is the core of the modular Titrando system. Operation is carried out by a Touch Control with touch-sensitive screen ("Stand alone" titrator) or by a computer with a corresponding software. A Titrando system can contain numerous, various kinds of devices. The following figure provides an overview of the peripheral devices you can connect to the 851 Titrando.
Tower-PC Sensors Dosing Interface USB Sample Processor Robotic Titrosampler
Input 1 / 2
Touch Control
Controller
Relay Box Printer
USB
On
MSB
Remote Box
PC Keyboard
USB Hub
On Status
USB
Barcode Reader
/RS2
32 C
onve r
ter
Titrando
80 m D i 5 s o a
Me r o t h
Balance
Stirrer / Ti Stand
Dosino
Dosimat
Figure 1
The Titrando system
851 Titrando
1.2 Instrument description
Up to three control devices (Titrandos, Dosing Interfaces, USB Sample Processors etc.) can be controlled via USB connection by PC Control/Touch Control. You can request information on special applications in the "Application Bulletins" and "Application Notes"; available free of charge via the Metrohm agent responsible. Various monographs on the subjects of titration techniques and electrodes are also available. Updating the device software is described in the manual or the help of the corresponding PC software respectively.
1.2
Instrument description
The 851 Titrando has the following characteristics:
Operation Operation is carried out by means of a touch-sensitive Touch Control or with a high-performance PC software. Dosing An external dosing drive. MSB connectors Four MSB connectors (Metrohm Serial Bus) to control dosing devices (Dosimat with exchange unit or Dosino with dosing unit), stirrer or titration stand and remote boxes. USB connectors Two USB connectors, through which devices such as printers, PC keyboards, barcode readers or additional control devices (Titrando, USB Sample Processor, Dosing Interface, etc.) can be connected. Measuring interface The measuring interface includes one measuring input (Gen.) for a generator electrode, one measuring input (Temp.) for a temperature sensor, e.g. Pt 1000 or NTC and one high-ohm measuring input (Ind.) for a double Pt electrode.
851 Titrando
1 Introduction
1.3
Titration modes Measuring modes Dosing commands

The following titration modes, measuring modes and dosing commands are supported:
MEAS For measurements the following measuring modes can be selected: T (temperature measurement), KFC Coulometric Karl Fischer titration for water determination with voltametric measurement. BRC Coulometric bromine index determination. Dosing commands The following commands for dosing can be selected: ADD (adding a predefined volume) LQH (for executing complex dosing tasks) PREP (rinsing the cylinder and tubings of an exchange or dosing unit) EMPTY (for emptying cylinder and tubings)
1.4
About the documentation

Caution Please read through this documentation carefully before putting the instrument into operation. The documentation contains information and warnings which have to be followed by the user in order to ensure safe operation of the instrument.
1.4.1
Symbols and conventions

The following symbols and styles are used in this documentation: Cross-reference to figure legend The first number refers to the figure number, the second to the instrument part in the figure. Instruction step Carry out these steps in the sequence shown.
851 Titrando
1.5 Safety instructions
Warning This symbol draws attention to a possible life 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. Warning This symbol draws attention to a possible biological hazard. Caution This symbol draws attention to a possible damage of instruments or instrument parts. Note This symbol marks additional information and tips.
1.5
1.5.1
Safety instructions
General notes on safety
Warning This instrument may only be operated in accordance with the specifications 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.
1.5.2
Electrical safety
The electrical safety when working with the instrument is ensured as part of the international standard IEC 61010. Warning Only personnel qualified by Metrohm are authorized to carry out service work on electronic components.
851 Titrando
1 Introduction
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 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). Protection against electrostatic charges Warning Electronic components are sensitive to electrostatic charges and can be destroyed by discharges. Always pull the mains cable out of the mains connection socket before connecting or disconnecting electrical appliances on the rear panel of the instrument.
1.5.3
Working with liquids

Caution Periodically check all system connections for leaks. Observe the relevant regulations in respect to working with flammable and/or toxic fluids and their disposal.
851 Titrando
1.5 Safety instructions
1.5.4
Flammable solvents and chemicals

Warning 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. laboratory flue). Keep all sources of flame far from the workplace. Clean up spilled fluids and solids immediately. Follow the safety instructions of the chemical manufacturer.
1.5.5
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. 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.
851 Titrando
2 Overview of the instrument
2 Overview of the instrument
On Gen. 851 Titran
2 3
do
Figure 2
1
Front 851 Titrando

2 LED "On" Lights up when the Titrando and a controller (Touch Control or computer) are connected to the mains and switched on.
Bottle holder With holding clamps, for two reagent bottles LED "Gen." Lights up when the Titrando and the generator electrode are connected and switched on.
851 Titrando
Figure 3
1
Rear 851 Titrando

2 USB connector (USB 1 and USB 2) USB ports (type A) for connecting printer, keyboard, barcode reader, additional Titrandos, USB Sample Processor, etc. MSB connector (MSB 1 bis MSB 4) Metrohm Serial Bus. For connecting external dosing devices, stirrers to remote boxes. Mini DIN, 9-pin. Measuring interface 1 (Input 1) Temperature sensor connector (Temp.) For connecting a temperature sensor, e.g. Pt1000 or NTC sensor. Two B sockets, 2 mm.
Type plate Contains specifications concerning mains voltage, instrument type and serial number. Controller connector Connection of a Touch Control or PC with installed PC software. Mini DIN, 9-pin. Mains connection socket Electrode connector (Gen.) For connecting a generator electrode
5 7
6 8
Electrode connector (Ind.) For connecting a double Pt electrode. Socket F.
851 Titrando
3 Installation
3 Installation
3.1
3.1.1
Setting up the instrument

Packaging
The instrument is supplied in highly protective special packaging together with the separately packed accessories. Keep this packaging, as only this ensures safe transportation of the instrument.
3.1.2
Checks
Immediately after receipt, check whether the shipment has arrived complete and without damage by comparing it with the delivery note.
3.1.3
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 fluctuations and direct sunlight.
3.2
3.2.1
Connecting controller
Operation
Two different versions are available for operating the 851 Titrando: Caution Take care to ensure that the mains cable is pulled out of the mains connection socket before either setting up or disconnecting connections between the instruments.
3.2.1.1
Connecting a Touch Control Connect the Touch Control as follows:
851 Titrando
3.2 Connecting controller
Note The plug is protected against accidental disconnection of the cable by means of a "pull-out protection" feature. If you wish to pull out the plug, you will first need to pull back the outer plug sleeve marked with arrows. Insert the plug of the Touch Control connection cable into the controller socket.
Figure 4
Connecting a Touch Control
2 Connect all peripheral devices.

Connect MSB devices (see Chapter 3.3, page 13) Connect USB devices (see Chapter 3.4, page 17)
3 Connect the Titrando to the mains. 4 Switch on the Touch Control. The Touch Control power supply is supplied through the Titrando. At the time of switch on system tests are run automatically on both the Titrando and the Touch Control. The LED On on the front of the Titrando lights up when the system test has been completed and the instrument is ready for operation. Caution The Touch Control must be shut down properly by switching off with the ON/OFF switch on the rear of the instrument before the current supply is interrupted. If this is not done, then there is a danger of data loss. Because of the fact that the power supply for the Touch Control is provided through the Titrando, you must never separate the Titrando from the mains (e.g. by switching off with a connector strip) before you have switched off the Touch Control.
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851 Titrando
3 Installation
If you would prefer not to position the Touch Control directly next to the Titrando, then you can lengthen the connection between Titrando and Touch Control using the 6.2151.010 cable. The maximum connection length permitted is 5 m. 3.2.1.2 Connecting a computer The 851 Titrando requires a USB connection to a computer in order to be able to be controlled by a PC software. When a controller cable 6.2151.000 is used, the instrument can be connected directly, either to a USB socket on a computer, to a connected USB hub or to a different Metrohm control instrument. Cable connection and driver installation A driver installation is required in order to ensure that the 851 Titrando is recognized by the PC software. To accomplish this, you must comply with the procedures specified. The following steps are necessary: 1 Install software

Insert the PC software installation CD and carry out the installation program directions. Exit the program if you have started it after the installation.
2 Establish cable connections
Connect all peripheral devices to the instrument. Connect MSB devices (see Chapter 3.3, page 13) Connect USB devices (see Chapter 3.4, page 17) Connect the instrument to the mains supply if you have not already done this. The LED On on the 851 Titrando is not yet illuminated! Connect the instrument to a USB connector (Type A) of your computer (see manual of your computer). The 6.2151.000 cable is used for this purpose.
851 Titrando
11
3.2 Connecting controller
6.2151.000
Figure 5
Connecting a computer
For Windows 2000: the instrument is recognized and the driver is installed automatically. For Windows XP: the instrument is recognized and the installation assistant for the driver is started automatically. Select the option "Install software automatically" and click on [Next >]. Exit the assistant with [Finish]. For Windows Vista: the instrument is recognized and the installation assistant for the driver is started automatically. Select the option "Find and install driver software". Agree to all of the requests that follow. The installation assistant will be exited automatically. The On LED on the 851 Titrando lights up when the driver installation has been exited and the device is ready for operation. Note The plug on the instrument end of the 6.2151.000 controller cable is protected against accidental disconnection by means of a pull-out protection feature. If you wish to pull out the plug, you will first need to pull back the outer plug sleeve marked with arrows. Registering and configuring the instrument in the PC software The instrument must be registered in the configuration of your PC software. Once that has been done, you can then configure it according to your requirements. Proceed as follows:
12
851 Titrando
3 Installation
1 Set up the instrument
Start up PC software. The instrument is recognized automatically. The configuration dialog for the instrument is displayed. Make configuration settings for the instrument and its connectors.
More detailed information concerning the configuration of the instrument can be found in the documentation for the respective PC software.
3.3
Connecting MSB devices

In order to connect MSB devices, e.g.stirrers or dosing devices, Metrohm instruments are equipped with up a maximum of four connectors at what is referred to as the Metrohm Serial Bus (MSB). Various kinds of peripheral devices can be connected in sequence (in series, as a "daisy chain") at a single MSB connector (8-pin Mini DIN socket) and controlled simultaneously by the respective control instrument. In addition to the connection cable, stirrers and the remote box are each equipped with their own MSB socket for this purpose. The following illustration provides an overview of the devices that can be connected to an MSB socket, along with a number of different cabling variations.
Stirrer / Ti Stand MSB Remote Box Ti Stand / Stirrer Relay Box
Dosino / Dosimat Dosino Dosimat
Dosimat / Dosino
Figure 6
MSB connections
The question of which peripheral devices are supported depends on the control instrument.
851 Titrando
13
3.3 Connecting MSB devices
Note When connecting MSB devices together, the following must be observed:

Only one device of the same type can be used at a single MSB connector at one time. Type 700 Dosino and 685 Dosimat dosing devices cannot be connected together with other MSB instruments on a shared connector. These dosing devices must be connected separately. Caution
Exit the control software before you plug MSB instruments in. The control instrument recognizes when it is switched on which instrument is connected at which MSB connector. The operating unit or the control software enters the connected MSB devices into the system configuration (Device manager). MSB connections can be extended with the 6.2151.010 cable. The length of the connection must not exceed a maximum of 15 m.
3.3.1
Connecting dosing devices

Four dosing devices can be connected to the instrument (MSB 1 to MSB 4). The types of dosing devices that are supported are:

800 Dosino 700 Dosino 805 Dosimat 685 Dosimat
Proceed as follows: 1 Connect a dosing device

Exit the control software. Connect the connection cable to one of the sockets marked with MSB on the rear of the control instrument. Start the control software.
14
851 Titrando
3 Installation
Figure 7
Connecting a dosing device
3.3.2
Connecting a stirrer or titration stand

You can use a magnetic stirrer 801 Stirrer or 803 Ti Stand (stirring "from below") or the 804 Ti Stand with a rod stirrer 802 Stirrer (stirring "from above"). Connect a stirrer or a titration stand as follows: 1 Connect a stirrer or titration stand

Exit the control software. Connect the connection cable of the magnetic stirrer or of the titration stand to one of the sockets marked with MSB on the rear of the control instrument. If desired, connect the rod stirrer to the stirrer socket (with stirrer symbol) of the titration stand. Start the control software.
Figure 8
Connecting MSB stirrer
851 Titrando
15
3.3 Connecting MSB devices
Figure 9
Rod stirrer and titration stand
3.3.3
Connecting a remote box

Instruments that are controlled via remote lines and/or which send control signals via remote lines can be connected using the 6.2148.010 remote box. In addition to Metrohm, other instrument manufacturers also use similar connectors that make it possible to connect different instruments together. These interfaces are also frequently given the designations "TTL Logic", "I/O Control" or "Relay Control" and generally have a signal level of 5 volts. Control signals are understood to be electrical line statuses or brief ( 200 ms) electrical pulses which display the operational state of an instrument or which trigger or report an event. Sequences on a variety of instruments can thus be coordinated in a single complex automation system. No exchange of data is possible, however. Proceed as follows: 1 Connect a remote box

Exit the control software. Connect the remote box connection cable to one of the sockets marked with MSB on the rear of the control instrument. Start the control software.
16
851 Titrando
3 Installation
Figure 10
Connecting a remote box
You can, for example, connect an 849 Level Control Box (fill level monitor in a waste canister) or a 731 Relay Box (switch box for 230/110 volt alternating current sockets and low-voltage direct current outlets). The remote box also has an MSB socket at which a further MSB instrument, e.g. a dosing device or a stirrer, can be connected. You will find precise information concerning the pin assignment of the interface on the remote box in the appendix (see Chapter 7.1, page 49).
3.4
3.4.1
Connecting USB devices

General
The 851 Titrando has two USB connectors (type A sockets) for peripheral devices with USB interfaces. The Titrando functions as a USB hub (distributor) no matter how it is operated. If you wish to connect more than two devices to the USB, you can also use an additional commercially available USB hub . Caution If you operate the Titrando with the aid of the Touch Control, take care to ensure that the Touch Control is switched off when you set up or disconnect connections between the various instruments. If you use a PC software to control the Titrando, you should exit the program before you set up or disconnect the USB connections.
3.4.2
Connecting a printer
Printers that are connected to the 851 Titrando with Touch Control must meet the following requirements:

Printer languages: HP-PCL, Canon BJL Commands or Epson ESC P/2 Printer resolution: 300 dots/inch or 360 dots/inch (Epson) Paper format: A4 or Letter, single-sheet feed.
851 Titrando
17
3.4 Connecting USB devices
Connect the printer as follows: 1 Switch off the Touch Control. 2 With the aid of the 6.2151.020 cable, connect the USB connector of the Titrando (type A) with the USB connector of the printer (type B, see manual for the printer). 3 Switch on the printer first, then the Touch Control. 4 Configure the printer in the device manager of the Touch Control (see manual for PC Control/Touch Control).
3.4.3
Connecting a balance
If you control the 851 Titrando with a PC software, connect the balance directly to the serial port (COM) on the computer. This is usually 9-pin and marked with the symbol IOIOI. If you operate the Titrando with the help of the Touch Control, you will need the 6.2148.020 RS-232/USB Box for connecting a balance. The following table offers an overview of the balances that you can use together with the Titrando system and of which cable you will need for connection to the RS-232 interface: Balance AND ER-60, 120, 180, 182FR-200, 300FX 200, 300, 320 with RS-232 interface (OP-03) Mettler AB, AG, PR (LC-RS9) Mettler AM, PM, PE with interface option 016 or Mettler AJ, PJ with interface option 018 Mettler AT Cable 6.2125.020 + 6.2125.010
In the scope of delivery for the balance 6.2146.020 + 6.2125.010 also from Mettler: ME 47473 adapter and either ME 42500 hand switch or ME 46278 foot switch 6.2146.020 + 6.2125.010 also from Mettler: ME 42500 hand switch or ME 46278 foot switch
Mettler AX, MX, UMX, PG, AB-S, PB-S
6.2134.120
18
851 Titrando
3 Installation
Balance Mettler AE with interface option 011 or 012
Cable 6.2125.020 + 6.2125.010 also from Mettler: ME 42500 hand switch or ME 46278 foot switch Cable AS017-09 from Ohaus 6.2125.080 + 6.2125.010 6.2134.060 6.2125.080 + 6.2125.010
Ohaus Voyager, Explorer, Analytical Plus Precisa balances with RS-232-C interface Sartorius MP8, MC1 Shimadzu BX, BW Operation with Touch Control Connect the balance as follows:
1 With the aid of the 6.2151.030 cable, connect the USB connector of the Titrando (type A) with the USB connector of the RS-232/USB Box (type B). 2 Connect one of the RS-interfaces of the RS-232/USB box with the RS-232 interface of the balance (see table for cable).
Figure 11
Connecting a balance
3 Switch on the Touch Control. 4 Switch on the balance. 5 Switch on the RS-232 interface of the balance.
851 Titrando
19
6 Configure the RS-232 interface of the RS-232/USB Box in the device manager of the Touch Control as described in the manual for the PC Control / Touch Control. Operation with PC software Connect the balance as follows: 1 Connect the RS-232 interface of the computer with the RS-232 interface of the balance (see table for cable). 2 Switch on the balance. 3 Configure the RS-232 interface of the balance. 4 Configure the RS-232 interface of the computer in the device manager of the PC Control software as described in the manual for the PC Control / Touch Control.
3.4.4
Connecting a PC keyboard (only Titrando with Touch Control)

The PC keyboard is used as an aid for text and numerical input. If you operate the 851 Titrando with the aid of the Touch Control, then you can connect a PC keyboard with USB interface to the Titrando. Connect the PC keyboard as follows: 1 Insert the USB plug of the keyboard (type A) into one of the USB sockets of the Titrando. 2 Switch on the Touch Control. The keyboard will be recognized automatically and entered in the device manager. 3 Configure the keyboard in the device manager of the Touch Control as described in the manual for the PC Control / Touch Control.
3.4.5
Connecting a barcode reader

The barcode reader is used as an aid for text and numerical input. You can connect a barcode reader with USB interface.
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851 Titrando
3 Installation
Operation with Touch Control Connect the barcode reader as follows: 1 Insert the USB plug of the barcode reader (type A) into one of the USB sockets of the Titrando. 2 Switch on the Touch Control. The barcode reader will be recognized automatically and entered in the device manager of the Touch Control. 3 Configure the barcode reader in the device manager as described in the manual for the PC Control / Touch Control. Operation with a PC software Connect the barcode reader as follows: 1 Insert the USB plug of the barcode reader (type A) into one of the USB sockets of the Titrando or the computer. 2 Start the PC software. 3 Configure the barcode reader in the device manager as described in the manual for the PC Control / Touch Control. Settings on the barcode reader: Program the barcode reader as follows (also see manual for the barcode reader). 1 Switch the barcode reader to programming mode. 2 Specify the desired layout for the keyboard (USA, Germany, France, Spain, German-speaking Switzerland). This setting must match the setting in the device manager (see manual for PC Control / Touch Control). 3 Make sure that the barcode reader is set in such a way that Ctrl characters (ASCII 00 to 31) can be sent.
851 Titrando
21
4 Program the barcode reader in such a way that the ASCII character 02 (STX or Ctrl B) is sent as the first character. This first character is normally referred to as the "Preamble" or "Prefix Code". 5 Program the barcode reader in such a way that the ASCII character 04 (EOT or Ctrl D) is sent as the last character. This last character is normally referred to as the "Postamble", "Record Suffix" or "Postfix Code". 6 Exit the programming mode.
3.4.6
Connecting a USB hub

If you wish to connect more than two devices to the USB connector of the Titrando, you can also use an additional commercially available USB hub (distributor). If you operate the Titrando with the aid of the Touch Control, then you should use a USB hub with its own power supply. Connect the USB hub as follows: 1 Switch off the Touch Control and/or close the PC software. 2 With the aid of the 6.2151.020 cable, connect the USB connector of the Titrando (type A) with the USB connector of the hub (type B, see manual for the hub). 3 Switch on the Touch Control, or start PC software respectively. The USB hub is recognized automatically.
3.4.7
Connecting a Bluetooth adapter

Printers and balances (or other devices with RS-232 connection) can be optionally connected using a wireless Bluetooth connection. Printers and balance models with integrated Bluetooth functionality are to be recommended for this purpose. Bluetooth printer adapters for the USB interface can be obtained commercially, as can also Bluetooth serial adapters for RS-232 connections (e.g. for balances). Note Bluetooth is a registered and copyrighted name of the Bluetooth Special Interest Group (Bluetooth SIG, Inc.).
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851 Titrando
3 Installation
PC Control If the Titrando system is operated with the PC Control software, then a Bluetooth USB adapter can be connected to one of the USB sockets on the computer (or of the Titrando / USB Sample Processor). The driver software (for MS Windows 2000/XP) included in the scope of delivery by the manufacturer of the Bluetooth adapter must be installed in accordance with the directions contained in the associated manual. A Bluetooth USB adapter must support the Bluetooth specifications HCRP (Hardcopy Cable Replacement Profile) for printers and/or SPP (Serial Port Profile) for balances or RS-232 connections. Printer drivers must be set up prior to the installation of the Bluetooth adapter. 840 Touch Control If the Titrando system is operated as a stand-alone system with a 840 Touch Control, then the Metrohm Bluetooth USB adapter for the 840 (6.2162.000, Bluetooth V1.1 qualified Class 2 device) is required for a Bluetooth connection. Note The Metrohm Bluetooth USB adapter cannot be operated on a computer. The adapter is intended exclusively for use in a Titrando system in stand-alone operation, i.e. with a 840 Touch Control operating unit as controller. The prerequisite is the Touch Control Software version 5.840.0130 or higher. The Metrohm Bluetooth USB adapter permits wireless data transfer for distances up to 10 m. Install the Metrohm Bluetooth USB adapter as follows: 1 Plug the Bluetooth adapter into an open USB interface on the rear of the Titrando. 2 Switch on the Touch Control. The Bluetooth USB adapter is recognized automatically. 3 Configure the adapter in the device manager of the Touch Control as described in the manual for the PC Control / Touch Control. Printer and Bluetooth A Bluetooth-compatible printer or a Bluetooth printer adapter must support the HCRP (Hardcopy Cable Replacement Profile).
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23
The necessary settings for a Bluetooth-compatible printer can be found in the user manual for it. Bluetooth printer adapters can usually be connected without configuration to the USB connector of the respective printer. Comply with the instructions contained in the documentation for the printer adapter. Enter the definition of the printer type in the device manager of the Touch Control. Balances and Bluetooth A Bluetooth-compatible balance or a Bluetooth serial adapter must comply with the SPP (Serial Port Profile) in accordance to Bluetooth specifications. If the balance manufacturer offers a specific Bluetooth serial adapter, then this is to be preferred to a commercially available adapter. Bluetooth serial adapters must be configured on the PC with the help of an auxiliary program supplied by the manufacturer. The data transfer parameters of the instrument and the adapter must match one another. The Bluetooth serial adapter must be defined as the acceptor and not as the initiator of a serial connection. Authentication with a PIN code is not supported.
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851 Titrando
3 Installation
3.5
3.5.1
Titration vessel for coulometric KF titration

Mounting the coulometer cell
Mounting the coulometer cell
2
6.2016.050
1
6.1464.320
6.2047.020
Mount the coulometer cell as follows on a titration stand: 1 Fix the 6.2047.020 titration vessel holder to the 6.2016.050 support rod. 2 Slide the 6.1464.320 titration vessel from above into the titration vessel holder.
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25
3.5 Titration vessel for coulometric KF titration
3.5.2
Coulometer cell - Default setup

Filling the adsorber tube Before setting up the coulometer cell the 6.1403.030 adsorber tube has to be filled with 6.2811.000 molecular sieve. Proceed as follows:
6.1403.030
3
6.2811.000
2 1
1 Insert a small cotton plug into the adsorber tube below. Do not pack the cotton too tightly. 2 Fill up the molecular sieve up to the level. 3 Place a small cotton plug on the molecular sieve. Do not pack the cotton too tightly. 4 Seal the adsorber tube with the appropriate cover.
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851 Titrando
3 Installation
Setting up the coulometer cell
6.1403.030
4
6.2713.020
6.0341.100
6.0345.100
3
6.2713.000 6.2701.040 6.1448.020
5
6.1437.000 6.2713.010
2 6
6.1464.320 6.1903.030
Set up the coulometer cell as follows: 1 Place the 6.1903.030 stirring bar in the titration vessel. 2 Cut the 6.2713.xxx ground joint sleeves to the right length and put them on all the ground joints of the inserts. When cutting the ground joint sleeves, ensure that there are no "frayed" edges. The ground joint sleeves must not jut out of the lower ground joint edge. 3 Insert the 6.0341.100 indicator electrode into the left ground joint opening.
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27
4 Insert the adsorber tube into the generator electrode. 5 Insert the 6.0345.100 generator electrode without diaphgram (6.0344.100 generator electrode with diaphragm) together with the adsorber tube into the ground joint opening in the middle. 6 Put the 6.1448.020 septum onto the front opening of the titration vessel and screw on the 6.2701.040 screw cap. Only tighten until it seals. The septum must not bend. Filling the titration vessel (generator electrode with diaphragm) When using a generator electrode with diaphragm proceed as follows: 1 Fill in approx. 5 mL of catholyte into the generator electrode. 2 Fill in approx. 100 mL of anolyte into the titration vessel. The level of the anolyte should roughly be 1-2 mm above the level of the catholyte. The level of the anolyte and the catholyte must roughly be even, so that no anolyte flows into the generator electrode or catholyte into the titration vessel, respectively. 3 Close the last opening with the 6.1437.000 ground joint stopper. Filling the titration vessel (generator electrode without diaphragm) When using a generator electrode without diaphragm proceed as follows: 1 Fill the titration vessel with approx. 100 mL of reagent. 2 Close the last opening with the 6.1437.000 ground joint stopper. Screwing on the electrode cable Screw on the electrode cable as follows: 1 Unscrew the cover of the indicator electrode.
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851 Titrando
3 Installation
2 Unscrew the cover of the generator electrode.
3 Screw the 6.2104.020 electrode cable tightly onto the indicator electrode. 4 Screw the 6.2104.120 electrode cable tightly onto the generator electrode.
6.2104.020
3
6.2104.120
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29
Mark the screw head of the electrode cable. This prevents you from mixing-up the indicator and generator electrode.
3.5.3
Coulometer cell with addition and aspiration tube (use with Ti Stand)
Mounting the addition and aspiration tube
6.1437.000
2
6.2713.010
6.1439.010
Insert the addition and aspiration tube as follows into the coulometer cell: 1 Insert the 6.2713.010 ground joint sleeve into the 6.1439.010 addition and aspiration tube. 2 Place the 6.1437.000 stopper onto the ground joint sleeve on the addition and aspiration tube. 3 Insert altogether into the ground joint opening.
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851 Titrando
3 Installation
3.5.4
Coulometer cell with aspiration equipment (use with Dosino)

A Dosino allows the automatic changing of reagents. For aspiration, the 6.5617.000 aspiration equipment is used, including a complete dosing unit and a 50 mL glass cylinder. For aspirating greasy samples with which only the sample and not the whole reagent is aspirated, we recommend using a dosing unit with a 20 mL cylinder. For highly viscous samples a dosing unit with a 10 mL cylinder is suitable. Mounting the aspiration tip
6.1543.070 6.2730.030
2 1
6.1446.060
Insert the aspiration tip as follows into the coulometer cell: 1 Screw the 6.2730.030 nipple, with stopper and O-ring, onto the 6.1446.060 stopper. 2 Pull out the stopper. 3 Slide the 6.1534.070 aspiration tip through the stopper.
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31
4 Insert the stopper together with the aspiration tip into the ground joint opening with the ground joint sleeve. Slide the aspiration tip into the coulometer cell as far as it touches the vessel base.
3.5.5
Coulometer cell with KF oven

With samples that release their water only slowly or only at higher temperatures, the heating method is used. The sample is being heated in a KF oven and the water released is forwarded together with a carrier gas into the titration vessel. A detailed description of setting up the coulometer cell with the KF oven can be found in the manual of the oven.
3.5.6
Coulometer cell with Oven Sampler

With a large amount of samples the determination of the water content can be automated with the aid of an Oven Sample Processor. A detailed description of setting up the coulometer cell with the Oven Sampler can be found in the manual of the Oven Sampler.
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851 Titrando
3 Installation
3.6
3.6.1
Connecting sensors
General
The measuring interface includes one measuring input (Gen.) for a generator electrode, one measuring input (Temp.) for a temperature sensor, e.g. Pt 1000 or NTC and one high-ohm measuring input (Ind.) for a double Pt electrode.
3.6.2
Connecting generator electrode

Connect the generator electrode as follows: 1 Plug the electrode plug into the Gen. socket of the Titrando.
Gen.
Temp.
Figure 12
Connecting a generator electrode 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, you will first need to pull back the outer plug sleeve.
3.6.3
Connecting indicator electrode

Connect the indicator electrode as follows: 1 Plug the electrode plug into the Ind. socket of the Titrando.
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33
3.6 Connecting sensors
Figure 13
Connecting an indicator electrode 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, you will first need to pull back the outer plug sleeve.
3.6.4
Connecting a temperature sensor

A temperature sensor of the Pt 1000 or NTC type can be connected to the Temp. connector. Connect the temperature sensor as follows: 1 Plug the temperature sensor plugs into the Temp. sockets of the Titrando.
Temp.
Ind.
Figure 14
Connecting a temperature sensor
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851 Titrando
3 Installation
Note The red plug must always be plugged into the red socket at the temperature sensor for the purpose of shielding against disruptions.
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35
4.1 Principle of the KF coulometry
4.1 Principle of the KF coulometry
The coulometric Karl Fischer titration is a variation of the classic water determination method according to Karl Fischer. The conventional method works with a methanolic solution of iodine, sulfur dioxide and a base as buffer substance. When titrating a sample containing water, several reactions take place, which can be summarized by the following equation: H2O + I2 + [RNH]SO3CH3 + 2 RN [RNH]SO4CH3 + 2 [RNH]I According to the equation above the I2 reacts quantitatively with H2O. This chemical equation serves as a basis for the water determination. With coulometric Karl Fischer titration, the necessary iodine is generated electrochemically directly in the electrolyte containing iodine ("electronic buret"). Between the amount of electric charge and the amount of generated iodine, there is a strictly quantitative relationship, which is used for high-precision dosing of the iodine. No titer needs to be determined, as the coulometric Karl Fischer method is an absolute determination. It must only be ensured that the reaction generating the iodine runs with a 100 % of current efficiency. This is the case with all the reagents available at present. The endpoint indication is effected voltametrically by modulating an alternating current of constant strength to a double Pt electrode. This produces a voltage difference between the Pt wires, which significantly declines when lowest amounts of free iodine are present. This circumstance is used for detecting the endpoint of the titration.
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851 Titrando
4.2
4.2.1
Working with water standards

Certified water standards
For validating the instrument as a whole, integrated system, commercially available, certified water standards with water contents of 1.00 0.003 mg/g and/or 0.10 0.005 mg/g should be used. Note The 1.0 mg/g standard is easier to handle and therefore to be preferred. Table 1 Recommended sample sizes 0.22.0 g 0.55.0 g
Water standard solution 1.0 mg/g Water standard solution 0.1 mg/g
4.2.2
Practical recommendations
For validation, it is essential to work very accurately. In order to reduce possible measuring inaccuracies, sample preparation and processing should follow a defined scheme . 1 Put on gloves (always with KF titration). 2 Take a new plastic syringe and open it. 3 Take a new ampoule of KF standard and shake it shortly. 4 Open the ampoule and fill the syringe with 1 mL of the standard. 5 Pull out the piston of the syringe to its end and shake the syringe for a few seconds. The inside of the syringe is being rinsed by standard and freed from water contamination. 6 Expel the used standard into a waste bottle. 7 Repeat the same procedure with 1 mL of the standard. 8 Fill the syringe with the rest of the standard. At the end, aspirate an air bubble to ensure that no solution remains in the needle.
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4.2 Working with water standards
9 Wipe off the needle with a Kleenex cloth and cover it with the appropriate cap. 10 Place the syringe on the balance and press [TARA]. 11 As soon as the drift on the 851 Titrando is stable, take the syringe by hand, press [START] and inject approx. 1 mL of the standard through the septum. There are two possibilities: 12 Inject the standard without immersing the needle into the reagent liquid. If a little drop remains on the end of the needle, it should be aspirated back before pulling the needle out of the septum. The standard must not be expelled onto the electrode nor onto the sides of the titration vessel. Or 13 Inject directly underneath the surface of the KF solution. 14 Close the syringe with the same cap and place it back on the balance. 15 Read off the value displayed by the balance and enter it as sample size on the Touch Control or in PC Control. 16 As soon as the determination has been finished and the titration cell has been conditioned (drift stable), the next determination can be started.
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851 Titrando
4.3
Sample addition
This chapter contains a few notes concerning sample addition. A complete description of this topic is not possible here. Further notes can be found in the literature by the reagent manufacturers and in the following Metrohm Application Bulletins:
Bulletin No. No. 142 No. 145 No. 209 No. 273
Title Karl Fischer water determinations in gaseous samples The determination of small water contents in plastics Water determinations in insulating oils, hydrocarbons and their products Validation of KF coulometers according to GLP / ISO 9001
4.3.1
Sample size
The sample size should be small in order to be able to titrate as many samples as possible in the same electrolyte solution and in order to keep the titration time short. However, ensure that the sample contains at least 50 g of H2O. The following table provides clues for the sample size.
Table 2
Recommended sample sizes Sample size H2O, to be determined (Water content) 10000 ppm = 1 % 1000 ppm = 0.1 % 100 ppm = 0.01 % 10 ppm = 0.001 % 10 mg100 mg 100 mg1 g 1g 5g 100 g1000 g 100 g1000 g 100 g 50 g
Content of the sample
4.3.2
Working with liquid samples

Liquid samples are added with a syringe. Either use a syringe with a long needle, and immerse it into the reagent when injecting, or inject with a short needle and aspirate the last drop back into the needle. The sample amount injected is best determined by reweighing. For the determination of traces and validations glass syringes should be used. We recommend obtaining them from a specialized syringe manufacturer. Highly volatile samples and samples of low viscosity should be cooled before sampling. This reduces losses during processing. The
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4.3 Sample addition
syringe, however, must not be cooled directly, as condensates could be formed. For the same reason, avoid aspirating air through a syringe that has been cooled by filling it with a cooled sample. Samples of high viscosity can be thinned by heating. The syringe must be heated as well. The same target can be reached by diluting with suitable solvents. In this case the water content of the solvent has to be determined and subtracted as blank value. Paste and fats can be added to the measuring cell with a syringe without needle. You can use the ground joint opening for this. If you also want to aspirate, you can use the opening with the septum stopper. The sample amount is best determined by reweighing. With samples containing only traces of water the syringe has to be predried well. If possible, the syringe should be rinsed with the sample solution by filling in and rejecting solution several times.
4.3.3
Working with solid samples

If possible, solid samples are to be extracted or dissolved in a suitable solvent. The resulting solution is being injected, in doing so, a blank value correction for the solvent has to be carried out. If there is no suitable solvent for a solid sample, or if the sample is reacting with the Karl Fischer solution, then the drying oven should be used. If solid samples have to be added directly to the measuring cell, the cell without diaphragm should be used. The samples can be added through the ground joint opening or through the side opening. While doing so, take care to ensure that

the sample completely releases its moisture no side reaction with the Karl Fischer solution takes place the surfaces of the electrodes are not covered by the sample substance (incomplete KF reaction!) the Pt net of the generator electrode is not being damaged the Pt wires of the indicator electrode are not being damaged
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851 Titrando
4.4
4.4.1
Optimum working conditions

General
If a well-pre-dried titration vessel with a generator electrode without diaphragm is being set up, the base drift is reached within 30 minutes approximately. We recommend carefully shaking the titration vessel several times during this time. With a generator electrode with diaphragm you should expect a preparation time of approx. 2 hours. To obtain precise determinations of amounts of water smaller than 100 g, it may be of advantage to condition the instrument over night before using it. If the Titrando is switched off for a longer period with a filled titration vessel, re-conditioning can take a few moments after switching it on again. With continuous use, the Titrando should not be switched off over night.
4.4.2
Drift
A constant drift in the range of 4 g/min is all right. Lower values, however, are quite possible. Higher but stable values still produce good results, because the drift can be compensated. More detailed information can be found in the corresponding software manual. A constantly high drift can be caused by water-containing deposits in inaccessible parts of the cell. In these cases, shaking the titration vessel can reduce the value. Ensure that there are no drops above the liquid level in the titration vessel. Generator electrodes with diaphragm should only be shaken to an extent that the catholyte and anolyte are not being mixed up. If the drift remains high for a longer time after shaking the cell, then the electrolyte solution should be exchanged. When working with the oven, a drift of 10 g/min is all right. The drift depends on the gas flow (the smaller the gas flow, the lower the drift).
4.4.3
Reagent exchange
The electrolyte solutions must be exchanged in the following cases:

the titration vessel is too full the capacity of the reagent is exhausted the drift is too high, and cannot be reduced by shaking the cell a two-phase-mixture is being formed in the titration vessel; in this case it is also possible to aspirate the sample phase only.
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4.4 Optimum working conditions
The simplest way to remove the used electrolyte solution out of the cell is by aspirating. To do this, you can use e.g. an 803 TiStand with built-in membrane pump. An advantage is, that the cell does not have to be disassembled. In the case of severe contamination, the cell can be rinsed with a suitable solvent which is aspirated as well. When using the generator electrode with diaphragm, the catholyte should be exchanged approx. once a week. Longer use can cause blackening and yellow precipitates in the cathode chamber. A discernable stench is also a sign for having used the catholyte for too long.
4.4.4
Indicator electrode
A new indicator electrode can take a certain warm-up time for forming the surface. During this time, unexpectedly long titration times and high measurement results can occur. This phenomenon will, however, disappear after a short time of use. In order to accelerate the setting of a new indicator electrode, the 851 Titrando can be conditioned e.g. over night. A contaminated indicator electrode can be carefully cleaned with an abrasive agent (Alox (6.2802.000 polishing set) or toothpaste). After the cleaning, rinse with ethanol. The two Pt wires of the indicator electrode should run as parallel as possible to one another. Check when inserting.
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851 Titrando

5.1
5.1.1
General information
Care
The 851 Titrando requires appropriate care. Excess contamination of the instrument may result in functional disruptions and a reduction in the service life of the sturdy mechanics and electronics. Spilled chemicals and solvents must be removed immediately. Above all, the plug connections on the rear of the instrument (in particular the mains connection socket) should be protected from contamination. Caution Although this is extensively prevented by design measures, the mains plug should be unplugged immediately if aggressive media has penetrated the inside of the instrument, so as to avoid serious damage to the instrument electronics. In such cases, the Metrohm Service must be informed.
5.1.2
Maintenance by Metrohm Service

Maintenance of the 851 Titrando is best carried out as part of an annual service, which is performed by specialist personnel of the Metrohm company. If working frequently with caustic and corrosive chemicals, a shorter maintenance interval could be necessary. The Metrohm service department offers every form of technical advice for maintenance and service of all Metrohm instruments.
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5.2 Generator electrode
5.2
5.2.1
Generator electrode
Generator electrode without diaphragm
The 6.0345.100 generator electrode without diaphragm is easy to handle and to clean. It only needs one reagent and is quickly ready to be used (no moisture deposits in the diaphragm !). The generator electrode without diaphragm is suitable for most applications. It especially should be used for severely contaminated samples.
5.2.1.1
Reagents Only use reagents which are especially determined for generator electrodes without diaphragms. Details can be found in the documentation of the reagent manufacturers.
5.2.1.2
Cleaning As a rule, the electrolyte solution can be exchanged without special cleaning of the parts. If cleaning is necessary anyway, ensure that the Pt net of the generator electrode is not being damaged. Contaminations containing oil First clean with a solvent (e.g. hexane), then rinse with ethanol. Saline depositions First clean with water, then rinse with ethanol. Dry well all parts after cleaning. A hairdryer can be used for this. If the parts are being dried in the drying oven the temperature must not exceed 70C (plastic parts!).
5.2.2
Generator electrode with diaphragm

The 6.0344.100 generator electrode with diaphragm should be used if the samples contain ketones because special reagents for ketones are only available for generator electrodes with diaphragm. If your reagent has a low conductivity, e.g. because you have to add chloroform to the sample because of its solubility, you should prefer the generator electrode with diaphragm. It is also recommended when you have to rely on a high accuracy in the lowest trace range.
5.2.2.1
Reagents Reagents for the coulometric water determination with generator electrodes with diaphragm consist of the anode solution (anolyte), which is filled in the titration vessel, and the cathode solution (catholyte), which is filled in the generator electrode. For the water determinations in ketones, special reagents have to be used (see the documentation of the reagent manufacturers).
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851 Titrando
5.2.2.2
Cleaning As a rule, the electrolyte solution can be exchanged without special cleaning of the parts. If cleaning is necessary anyway, ensure that the Pt net of the generator electrode is not being damaged. Resinous residues on the diaphragm Hang the generator electrode vertically onto a support rod, fill with conc. HNO3 and leave over night. First rinse with water, then with ethanol. Contaminations containing oil First clean with a solvent (e.g. hexane), then rinse with ethanol. Saline depositions First clean with water, then rinse with ethanol. Cleaning (rinsing) the diaphragm Fill the cathode chamber of the generator electrode with methanol and let the filling flow out. Repeat 2-3 times. This procedure should also be carried out after the cleaning described above. Dry well all parts after cleaning. A hairdryer can be used for this. If the parts are being dried in the drying oven the temperature must not exceed 70C (plastic parts!).
5.3
Quality Management and validation with Metrohm

Quality Management Metrohm offers you comprehensive support in implementing quality management measures for instruments and software. Further information on this can be found in the brochure Quality Management with Metrohm available from your local Metrohm agent. Validation Please contact your local Metrohm agent for support in validating instruments and software. Here you can also obtain validation documentation to provide help for carrying out the Installation Qualification (IQ) and the Operational Qualification (OQ). IQ and OQ are also offered as a service by the Metrohm agents. In addition, various application bulletins are also available on the subject, which also contain Standard Operating Procedures (SOP) for testing analytical measuring instruments for reproducibility and correctness. Maintenance Electronic and mechanical functional groups in Metrohm instruments can and should be checked as part of regular maintenance by specialist personnel from Metrohm. Please ask your local Metrohm agent regarding the
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45
5.3 Quality Management and validation with Metrohm
precise terms and conditions involved in concluding a corresponding maintenance agreement. Note You can find information on the subjects of quality management, validation and maintenance as well as an overview of the documents currently available at www.metrohm.com/com/ under Support.
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851 Titrando
6 Troubleshooting
6 Troubleshooting
6.1
Problem LED "On" is not illuminated although the Titrando is connected to the mains.
General
Cause The Touch Control or the computer has not been switched on yet or the plugs are not correctly connected. Remedy Check the plug connections and switch on the Touch Control or the computer.
6.2
Problem
Karl Fischer Titration

Cause The titration cell is leaking. Remedy
The drift is very high during conditioning.
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. Use special reagents. Adjust the method (increase/decrease the temperature, external extraction). See technical literature.
The drift becomes greater after each titration.
The sample releases water very slowly.
A side reaction is taking place.
The pH value is not in the optimum range anymore. The titration will not be finished. The titration cell is leaking.
Add buffer, see technical literature.
Check seals and septum. If necessary, replace. Replace molecular sieve.
The minimum increment is too low.
1. Select the user defined titration rate 2. Increase the minimum volume increment. (see manual/help of the software used). Change the control parameters (see manual/ help of the software used)
The stop criterion is unsuitable.
Increase the stop drift.
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6.2 Karl Fischer Titration
Cause Remedy Select a short delay time.
Problem
See also: The drift increases after each titration. The sample is overtitrated. The increments at the end of the titration are too high.
Select the user defined titration rate and then change the control parameters (see manual/help of the software used) The following experiment provides a clue for the optimum dosing rate: During conditioning, display the drift and add sample without starting the titration. Select a value below the highest drift as dosing rate. Stir faster. Replace the working medium. Reduce the amount of solubilizer, if working with solvent mixtures, see technical literature.
The amount of methanol in the working medium is too low.
The indicator electrode could be covered. The solution becomes darker after each titration.
Clean the electrode with ethanol or a suitable solvent. Replace the working medium.
The indicator electrode could be covered. The indicator electrode has a short circuit.
Clean the electrode with ethanol or a suitable solvent. 1. Check the Pt wires. 2. Switch on the electrode test. 1. Select user defined titration rate 2. Reduce the dosing rate (see manual/help of the software used).
The endpoint is reached too quickly.
The dosing rate outside the control range is too high.
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851 Titrando
7 Appendix
7 Appendix
7.1 Remote interface
The 6.2148.010 remote box allows devices to be controlled which cannot be connected directly to the MSB interface of the Titrando.
1
2 3
Figure 15
1 Cable For connecting the Titrando.
Connectors of the remote box

2 MSB connector Metrohm Serial Bus. For connecting external dosing devices or stirrers.
Remote connector For connecting devices with a remote interface.
7.1.1
Pin assignment of the remote interface

13 1 1 13
25 14 14 25
Figure 16
Pin assignment of remote socket and plug
The above presentation of the pin assignment of a Metrohm remote interface applies not only for the remote box, but also for all Metrohm devices with 25-pin D-Sub remote connection.
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49
Inputs
+5 V
approx. 50 k Pull-up
tp
tp >20 ms
active = low, inactive = high Outputs Open Collector

tp
tp >200 ms
active = low, inactive = high IC = 20 mA, VCEO = 40 V +5 V: maximum load = 20 mA The following tables offer information concerning the allocation of the individual pins and their function. Table 3 Inputs and outputs of the remote interface Pin No. 21 9 22 10 23 11 24 12 5 18 4 17 3 16 1 2 Warning Error Ready Conditioning OK Determination EOD Function Start Stop Quit
Assignment Input 0 Input 1 Input 2 Input 3 Input 4 Input 5 Input 6 Input 7 Output 0 Output 1 Output 2 Output 3 Output 4 Output 5 Output 6 Output 7
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851 Titrando
7 Appendix
Assignment Output 8 Output 9 Output 10 Output 11 Output 12 Output 13 0 volts / GND +5 volts 0 volts / GND Table 4
Pin No. 6 7 8 13 19 20 14 15 25
Function
Explanation of the individual functions Explanation The current method is started at the time of activation. tpulse > 100 ms
Function Start
Stop
The current method is canceled (Stop) at the time of activation. tpulse > 100 ms
Quit
The current command in the determination run will be canceled at the time of activation. tpulse > 100 ms
Ready Conditioning OK
The instrument is ready to receive a start signal. The line is set when Conditioning with SET and KFT titration is at OK. The line remains set until the determination is started with [START]. The instrument performs a data-generating determination. End of Determination. Pulse (tpulse = 200 ms) after a determination or after a buffer/standard during calibration using a Sample Processor.
Determination EOD
Error
The line is set for error message display.
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51
Function Warning
Explanation The line is set for warning message display.
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851 Titrando
8.1 Measuring interface
The 851 Titrando has one galvanically isolated measuring interface. The measuring cycle is 100 ms for all measuring modes.
8.1.1
Imax
Generator electrode
One measuring input (Gen.) for a generator electrode. 400 mA Continuous current and pulsed
8.1.2
Indicator electrode
One measuring input (Ind.) for an indicator electrode. Determination with adjustable polarization current. 5, 10, 20 und 30 A 125+125 A
Measuring mode Ipol AC DC
8.1.3
Temperature
One measuring input (Temp.) for temperature sensors, Pt 1000 or NTC. Automatic temperature compensation for NTC sensors R (25 C) and B value can be configured.
Measuring range Pt 1000 NTC Resolution PT 1000 NTC Measuring accuracy PT 1000 0.2 C (Applies for measuring range 20+150C; 1 digit; without sensor error, under reference conditions) 0.6 C (Applies for measuring range +10+40C; 1 digit; without sensor error, under reference conditions) 0.1 C 0.1 C 150+250 C 5+250 C (R (25 C) = 30'000 and B (25/50) = 4100 K)
NTC
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53
8.2 Mains connection
8.2
Voltage Frequency
Mains connection
100240 V 5060 Hz maximum 45 W Electronic overload protection
Power consumption Fuse
8.3
Safety specifications

Design and testing
EN/IEC 61010-1: 2001 UL 61010-1: 2004 CSA-C22.2 No. 61010-1: 2004 Protection class I
Safety instructions
The documentation contains safety instructions which have to be followed by the user in order to ensure safe operation of the instrument.
8.4
Emission
Electromagnetic compatibility (EMC)

Standards fulfilled: EN 61326-1: 2006 EN 61000-6-3: 2006 EN 61000-6-4: 2006 EN 55011 / CISPR 11: 2007 EN 61000-3-2:2006 EN 61000-3-3:2005 Standards fulfilled: EN 61326-1:2006 EN 61000-6-1: 2007 EN 61000-6-2: 2005 EN 61000-4-2: 2001 EN 61000-4-3: 2006 EN 61000-4-4: 2004 EN 61000-4-5: 2006 EN 61000-4-6: 2007 EN 61000-4-8: 2001 EN 61000-4-11: 2004 EN 61000-4-14: 2004 EN 61000-4-28:2000 + A1:2004 NE 21: 2004
Immunity
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851 Titrando
8.5
Ambient temperature
+5+45 C 20+60 C 40+60 C
Nominal function range Storage Transport
8.6
USB ports
Interfaces
USB connectors 2 USB downstream ports (model A sockets), each 500 mA, for connecting peripheral devices such as printers, keyboards, barcode readers or RS-232/USB boxes (Metrohm order no. 6.2148.020). Controller connection
Controller port
USB upstream port with auxiliary power supply (Mini DIN socket) for connecting Touch Control or computer for controlling the 851 Titrando. With integrated Touch Control cable With cable 6.2151.000 MSB connectors (Metrohm Serial Bus)
Touch Control Computer
Dosing device Stirrer Connection for a maximum of 4 stirrers. Stirrer control: manual On/Off switching or coordination with the titration sequence. Rate in 15 stages and shift direction can be selected Connection for a maximum of four remote boxes. Remote boxes can be used to actuate and monitor external devices.
Remote Box
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9.1 Declaration of Conformity

9.1 Declaration of Conformity
This is to certify the conformity to the standard specifications for electrical appliances and accessories, as well as to the standard specifications for security and to system validation issued by the manufacturing company. Name of commodity 851 Titrando Universal titrator, controlled by a Touch Control or a computer with PCSoftware This instrument has been built and has undergone final type testing according to the standards: Electromagnetic compatibility Emission: EN/IEC 61326-1: 2006, EN/IEC 61000-6-3: 2006, EN/IEC 61000-6-4: 2006, EN 55011 / CISPR 11: 2007, EN/IEC 61000-3-2: 2006, EN/IEC 61000-3-3: 2005 EN/IEC 61326-1: 2006, EN/IEC 61000-6-1: 2007, EN/IEC 61000-6-2: 2005, EN/IEC 61000-4-2: 2001, EN/IEC 61000-4-3: 2006, EN/IEC 61000-4-4: 2004, EN/IEC 61000-4-5: 2006, EN/IEC 61000-4-6: 2007, EN/IEC 61000-4-8: 2001, EN/IEC 61000-4-11: 2004, EN/IEC 61000-4-14: 2004, EN/IEC 61000-4-28: 2000 + A1:2004, NE 21: 2004
Immunity:
Safety specifications
EN/IEC 61010-1: 2001, UL 61010-1: 2004, CSA-C22.2 No. 61010-1: 2004, protection class I This instrument meets the requirements of the CE mark as contained in the EU directives 2006/95/EC (LVD), 2004/108/EC (EMC). It fulfils the following specifications: EN 61326-1 Electrical equipment for measurement, control and laboratory use EMC requirements
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851 Titrando
EN 61010-1
Safety requirements for electrical equipment for measurement, control and laboratory use
Manufacturer
Metrohm Ltd., CH-9101 Herisau/Switzerland Metrohm Ltd. is holder of the SQS certificate ISO 9001:2000 Quality management system for development, production and sales of instruments and accessories for ion analysis. Herisau, 22 May, 2008
D. Strohm Vice President, Head of R&D
A. Dellenbach Head of Quality Management
9.2
Quality Management Principles

Metrohm Ltd. holds the ISO 9001:2000 Certificate, registration number 10872-02, issued by SQS (Swiss Association for Quality and Management Systems). Internal and external audits are carried out periodically to assure that the standards defined by Metrohms QM Manual are maintained. The steps involved in the design, manufacture and servicing of instruments are fully documented and the resulting reports are archived for ten years. The development of software for PCs and instruments is also duly documented and the documents and source codes are archived. Both remain the possession of Metrohm. A non-disclosure agreement may be asked to be provided by those requiring access to them. The implementation of the ISO 9001:2000 quality management system is described in Metrohms QM Manual, which comprises detailed instructions on the following fields of activity: Instrument development The organization of the instrument design, its planning and the intermediate controls are fully documented and traceable. Laboratory testing accompanies all phases of instrument development. Software development Software development occurs in terms of the software life cycle. Tests are performed to detect programming errors and to assess the programs functionality in a laboratory environment.
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9.3 Warranty (guarantee)
Components All components used in the Metrohm instruments have to satisfy the quality standards that are defined and implemented for our products. Suppliers of components are audited by Metrohm as the need arises. Manufacture The measures put into practice in the production of our instruments guarantee a constant quality standard. Production planning and manufacturing procedures, maintenance of production means and testing of components, intermediate and finished products are prescribed. Customer support and service Customer support involves all phases of instrument acquisition and use by the customer, i.e. consulting to define the adequate equipment for the analytical problem at hand, delivery of the equipment, user manuals, training, after-sales service and processing of customer complaints. The Metrohm service organization is equipped to support customers in implementing standards such as GLP, GMP, ISO 900X, in performing Operational Qualification and Performance Verification of the system components or in carrying out the System Validation for the quantitative determination of a substance in a given matrix.
9.3
Warranty (guarantee)
Metrohm guarantees that the deliveries and services it provides are free from material, design or manufacturing errors. The warranty period is 36 months from the day of delivery; for day and night operation it is 18 months. The warranty remains valid on condition that the service is provided by an authorized Metrohm service organization. Glass breakage is excluded from the warranty for electrodes and other glassware. The warranty for the accuracy corresponds to the technical specifications given in this manual. For components from third parties that make up a considerable part of our instrument, the manufacturer's warranty provisions apply. Warranty claims cannot be pursued if the Customer has not complied with the obligations to make payment on time. During the warranty period Metrohm undertakes, at its own choice, to either repair at its own premises, free of charge, any instruments that can be shown to be faulty or to replace them. Transport costs are to the Customer's account. Faults arising from circumstances that are not the responsibility of Metrohm, such as improper storage or improper use, etc. are expressly excluded from the warranty.
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10 Accessories
10 Accessories
10.1 Scope of delivery
Note Subject to change without notice.
10.1.1
Qty. 1 1
851 Titrando 2.851.0110

Order no. 1.851.0010 6.0341.100 Description 851 Titrando Double Pt wire electrode
Double Pt wire electrode (0.8 x 4 mm), standard ground joint, Metrohm plug-in head G, for Karl Fischer titrations Measuring range: 2000 ...2000 Measuring unit: mV Temp. continuous (C): 20 ...70 Shaft length to head (mm): 125 Minimum immersion depth 10 (mm): Indicator electrode type: Pt Indicator electrode form: Wire Filling-in lock: None Pressure load: >0 1 6.0345.100 Generator electrode without diaphragm
Generator electrode for Karl Fischer titrations, without diaphragm, standard ground joint 29/22 Temp. continuous (C): 20 ...70 Shaft diameter top (mm): 24 Shaft diameter bottom (mm): 24 Length from standard ground 85 joint (mm): Minimum immersion depth 15 (mm): Electrode plug-in head: Metrohm plug-in head G Indicator electrode type: Cathode = Pt sheet Indicator electrode type (ref- Anode = Pt net erence):
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Description Standard ground joint 29/22 KF adsorber tube for coulometer cell 93 B-17/19
Qty. 1
Order no. 6.1403.030 Height (mm): SGJ size:
Ground joint sleeve:
6.1437.000 Material: Height (mm): SGJ size:
Ground joint stopper SGJ 14 Glass 34 B-14/15
Stopper / B-14/15 / M10 PP 22 B-14/15
6.1448.020
Septum / 16 mm / 5 pieces Silicone rubber 2 16
Set of 5 pieces. Material: Height (mm): Outer diameter (mm):
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851 Titrando
Qty. 1 Order no. 6.1464.320 Description KF titration vessel / 80 - 250 mL / coulometric Clear glass 114 A-29/22, 2 x A-14/15 80 ... 250
10 Accessories
Material: Height (mm): Opening ground joint: Volume (mL):
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
6.2047.020
Titration vessel holder
Titration vessel holder for coulometric cells.
6.2103.130
Adapter red plug 2 mm / 4 mm socket
For connecting plug B (4 mm) to socket 2 mm.
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Description Adapter black plug 2 mm / socket B 4 mm
Qty. 1
Order no. 6.2103.140
6.2104.020
Electrode cable / 1 m / F
For connecting electrodes with Metrohm plug-in head G to Metrohm instruments (socket F). Length (m): 1
6.2104.120
Electrode cable / 1 m / H
With plug H. For the connection generator electrode - KF coulometer. Length (m): 1
6.2701.040
Screw cap
Of PBTP. With a hole for the 6.1448.020 septum. For the 6.5405.000 cell without diaphragm and the 6.1464.32X and 6.1465.320 titration vessels. Material: PBTP Height (mm): 20 Outer diameter (mm): 24 Inner diameter (mm): 18
6.2713.000
Sleeve
For the fat-free ground joint connection with the standard ground joint SGJ 14 Material: PTFE film
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851 Titrando
Qty. 1 Order no. 6.2713.010 Description Sleeve
10 Accessories
Sleeve for the fat-free ground joint connection with the standard ground joint SGJ 29 Material: PTFE film
6.2713.020
Sleeve
6.2730.030
Stopper
Including nipple and E.301.0043 O-ring. For 6.1414.030 titration vessel lids. For KF instruments, VA stands, VA Computrace and IC Dilution. Length (mm): 38
6.2738.000
Funnel PP 50 6
For the KF coulometer Material: Outer diameter (mm): Inner diameter (mm):
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Description Molecular sieve
Qty. 1
Order no. 6.2811.000
Molecular sieve. Bottle of 250 g. Pore size: 0.3 nm. Without moisture indicator. For Rancimats and Karl Fischer instruments.
6.2816.010
Needle 0.8 80
For the 6.2816.000 syringe Outer diameter (mm): Length (mm):
6.2816.090
Syringe 5 mL
Syringe 5 mL of PP, with Luer connector Material: PP
6.2122.0x0
Mains cable with C13 line socket IEC-60320-C13
Cable plug according to customer requirements. Switzerland: Type SEV 12 6.2122.020 Germany, : Type CEE(7), VII 6.2122.040 USA, : Type NEMA/ASA 6.2122.070 1 8.851.8002EN 851 Titrando Manual
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851 Titrando
10 Accessories
10.1.2
Qty. 1 1
851 Titrando 2.851.0010

Order no. 1.851.0010 1.801.0010 Description 851 Titrando 801 Stirrer
Magnetic Stirrer without stand. With permanently attached cable for MSB (Metrohm Serial Bus). 1 6.0341.100 Double Pt wire electrode
Double Pt wire electrode (0.8 x 4 mm), standard ground joint, Metrohm plug-in head G, for Karl Fischer titrations Measuring range: 2000 ...2000 Measuring unit: mV Temp. continuous (C): 20 ...70 Shaft length to head (mm): 125 Minimum immersion depth 10 (mm): Indicator electrode type: Pt Indicator electrode form: Wire Filling-in lock: None Pressure load: >0 1 6.0344.100 Generator electrode with diaphragm
Generator electrode for Karl Fischer titrations, with diaphragm, standard ground joint 29/22 Temp. continuous (C): 20 ... 70 Shaft diameter top (mm): 24 Shaft diameter bottom (mm): 24 Length from standard ground 85 joint (mm): Minimum immersion depth 15 (mm): Electrode plug-in head: Metrohm plug-in head G Indicator electrode type: Cathode = Pt net Indicator electrode type (ref- Anode = Pt net erence): Ground joint sleeve: Standard ground joint 29/22
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Description KF adsorber tube for coulometer cell 93 B-17/19
Qty. 1
Order no. 6.1403.030
For KF coulometers Height (mm): SGJ size:
Stopper / B-14/15 / M10 PP 22 B-14/15
6.1448.020
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851 Titrando
Qty. 1 Order no. 6.1464.320 Description KF titration vessel / 80 - 250 mL / coulometric Clear glass 114 A-29/22, 2 x A-14/15 80 ... 250
10 Accessories
6.1903.030
6.2001.060
Base plate without support rod
For mounting the 801, 804, 803 stirrers on a Titrando, Titrino plus, Dosimat plus and on the 856 and 867 measuring modules.
6.2013.010
Clamping ring
For support rods with a diameter of 10 mm Material: Metal Width (mm): 20 Height (mm): 16
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Description Support rod / 250 mm Steel, stainless 18/8 10 250
Qty. 1
Order no. 6.2016.030
Material: Outer diameter (mm): Length (mm):
6.2047.020
6.2103.130
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851 Titrando
Qty. 1 Order no. 6.2103.140 Description Adapter black plug 2 mm / socket B 4 mm
10 Accessories
6.2104.020
6.2104.120
6.2701.040
Screw cap
Of PBTP. With a hole for the 6.1448.020 septum. For the 6.5405.000 cell without diaphragm and the 6.1464.32X and 6.1465.320 titration vessels. For 684, 737, 756 KF coulometers Material: PBTP Height (mm): 20 Outer diameter (mm): 24 Inner diameter (mm): 18
6.2713.000
Sleeve
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Description Sleeve
Qty. 1
Order no. 6.2713.010
6.2713.020
Sleeve
6.2730.030
Stopper
6.2738.000
Funnel PP 50 6
70
851 Titrando
Qty. 1 Order no. 6.2811.000 Description Molecular sieve
10 Accessories
Molecular sieve. Bottle of 250 g. Pore size: 0.3 nm. Without moisture indicator. For Rancimats and Karl Fischer instruments
6.2816.010
Needle 0.8 80
6.2816.090
Syringe 5 mL
6.2122.0x0
Cable plug according to customer requirements. Switzerland: Type SEV 12 6.2122.020 Germany, : Type CEE(7), VII 6.2122.040 USA, : Type NEMA/ASA 6.2122.070 1 8.851.8002EN 851 Titrando Manual
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10.1.3
Qty. 1 1
851 Titrando 2.851.0020

Order no. 1.851.0010 1.801.0010 Description 851 Titrando 801 Stirrer
Magnetic Stirrer without stand. With permanently attached cable for MSB (Metrohm Serial Bus). 1 1.840.0100 840 Touch Control
Operating element with touch-sensitive color display for Titrandos. Default languages German and English. One additional language can be added later. 1 6.0341.100 Double Pt wire electrode
Double Pt wire electrode (0.8 x 4 mm), standard ground joint, Metrohm plug-in head G, for Karl Fischer titrations Measuring range: 2000 ... 2000 Measuring unit: mV Temp. continuous (C): 20 ... 70 Shaft length to head (mm): 125 Minimum immersion depth 10 (mm): Indicator electrode type: Pt Indicator electrode form: Wire Filling-in lock: None Pressure load: >0 1 6.0344.100 Generator electrode with diaphragm
Generator electrode for Karl Fischer titrations, with diaphragm, standard ground joint 29/22 Temp. continuous (C): 20 ... 70 Shaft diameter top (mm): 24 Shaft diameter bottom (mm): 24 Length from standard ground 85 joint (mm): Minimum immersion depth 15 (mm): Electrode plug-in head: Metrohm plug-in head G Indicator electrode type: Cathode = Pt net Indicator electrode type (ref- Anode = Pt net erence): SGJ sleeve: Standard ground joint 29/22
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851 Titrando
Qty. 1 Order no. 6.1403.030 Description KF adsorber tube for coulometer cell 93 B-17/19
10 Accessories
For KF coulometers Height (mm): SGJ size:
Stopper / B-14/15 / M10 PP 22 B-14/15
6.1448.020
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Description KF titration vessel / 80 - 250 mL / coulometric Clear glass 114 A-29/22, 2 x A-14/15 80 ... 250
Qty. 1
Order no. 6.1464.320
6.1903.030
6.2001.060
Base plate without support rod
For mounting the 801, 804, 803 stirrers on a Titrando, Titrino plus, Dosimat plus and on the 856 and 867 measuring modules.
6.2013.010
Clamping ring
For support rods with a diameter of 10 mm Material: Metal Width (mm): 20 Height (mm): 16
74
851 Titrando
Qty. 1 Order no. 6.2016.030 Description Support rod / 250 mm Steel, stainless 18/8 10 250
10 Accessories
Material: Outer diameter (mm): Length (mm):
6.2047.020
6.2103.130
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Description Adapter black plug 2 mm / socket B 4 mm
Qty. 1
Order no. 6.2103.140
6.2104.020
6.2104.120
6.2701.040
Screw cap
Of PBTP. With a hole for the 6.1448.020 septum. For the 6.5405.000 cell without diaphragm and the 6.1464.32X and 6.1465.320 titration vessels. Material: PBTP Height (mm): 20 Outer diameter (mm): 24 Inner diameter (mm): 18
6.2713.000
Sleeve
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851 Titrando
Qty. 1 Order no. 6.2713.010 Description Sleeve
10 Accessories
6.2713.020
Sleeve
6.2730.030
Stopper
6.2738.000
Funnel PP 50 6
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77
Description Molecular sieve
Qty. 1
Order no. 6.2811.000
Molecular sieve. Bottle of 250 g. Pore size: 0.3 nm. Without moisture indicator. For Rancimats and Karl Fischer instruments
6.2816.010
Needle 0.8 80
6.2816.090
Syringe 5 mL
6.6051.000
Titrando method CF card
Memory card with application methods
6.2122.0x0
Cable plug according to customer requirements. Switzerland: Type SEV 12
78
851 Titrando
Qty. Order no. Germany, : USA, : 1 8.851.8002EN Description 6.2122.020 Type CEE(7), VII 6.2122.040 Type NEMA/ASA 6.2122.070 851 Titrando Manual
10 Accessories
10.2
10.2.1
Order no. 2.800.0010
Optionales Zubehr
851 Titrando 2.851.0010, 2.851.0020, 2.851.0110
Description 800 Dosino
Drive with write/read hardware for intelligent dosing units. With fixed cable.
2.840.0100
840 Touch Control
Operating element for Titrandos, USB Sample Processors and 846 Dosing Interface. Touch-sensitive color display. Simple and intuitive user guidance. Compliant with 21 CFR Part 11. Two PCMCIA card slots. Standard dialog language English; one further language can be retrofitted. Including CompactFlash card with adapter, demo version of the PC Control Software.
2.801.0010
801 Stirrer
Magnetic stirrer without stand for use with Titrino plus, Titrandos, Sample Processors, 805 Dosimats and 780/781 pH Meters. With permanently attached cable for MSB (Metrohm Serial Bus).
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10.2 Optionales Zubehr
Order no. 2.803.0010
Description 803 Ti Stand
Compact titration stand with magnetic stirrer and built-in pump for solvent addition and aspiration of the titration vessel contents. Suitable for Karl Fischer titrations with Titrandos. MSB connection. Including comprehensive accessories, solvent 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 the thermal sample preparation in Karl Fischer titration. A lot of substances cannot be analyzed by direct Karl Fischer titration as they are not soluble, react with the Karl Fischer reagent or release the water only very slowly or not until heated to high temperatures. Using tightly sealed sample vials the sample is inserted in the oven. Subsequently the samples can be analyzed by any volumetric or coulometric KF titrator. Dimensions in mm (W/H/D): 440/500/230 2.874.0010 874 USB Oven Sample Processor
The 874 Oven Sample Processor is used for thermal sample preparation in Karl Fischer titration. The oven method is suitable for samples that only release their moisture at higher temperature, for hardly soluble samples or samples that undergo side-reactions with the KF reagent. Dimensions in mm (W/H/D): 280/550/490 6.2148.010 Remote Box MSB
Additional remote interface for the connection of devices that can be controlled via remote lines. With permanently attached cable.
6.2148.020
RS 232/USB Box
Extends the Titrandos, USB Sample Processors, Dosing Interface, Titrosampler by two RS 232 interfaces for the connection of e.g. balance, PC, LIMS. Requires 6.2151.030 cable.
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851 Titrando
Order no. 6.3032.120 Description Dosing Unit 2 mL
10 Accessories
Dosing unit with integrated data chip with 2 mL glass cylinder and light protection, mountable on reagent bottle with ISO/DIN GL45 glass thread. FEP tubing connection, antidiffusion buret tip. Volume (mL): 2
6.3032.150
Dosing Unit 5 mL
Dosing unit with integrated data chip with 5 mL glass cylinder and light protection, mountable on reagent bottle with ISO/DIN GL45 thread. FEP tubing connection, antidiffusion buret tip. Volume (mL): 5
6.3032.210
Dosing Unit 10 mL
6.3032.220
Dosing Unit 20 mL
6.3032.250
Dosing Unit 50 mL
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10.2 Optionales Zubehr
Order no. 6.6050.500
Description Titrando PC Control-SW 6.0
PC software for controlling Titrandos, USB Sample Processors, 846 Dosing Interface, 847 USB Lab Link. Simple and intuitive user guidance. Method and data compatible with Touch Control. With freely progammable favorites for fast method access. Compliant with 21 CFR Part 11. Standard dialog languages English and German; one further language can be retrofitted. Including hardware dongle. The 6.2151.000 Cable is required for connecting the Titrando to a PC. 6.6056.211 6.6056.212 6.6056.213 Tiamo 2.x Light CD: 1 Lizenz Tiamo 2.x Full CD: 1 Lizenz Tiamo 2.x Multi CD:3 Lizenzen
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Index
Index
Numbers/Symbols 685 Dosimat ............................ 14 700 Dosino .............................. 14 800 Dosino .............................. 14 801 Stirrer ................................ 15 803 Ti Stand ............................. 15 804 Ti Stand ............................. 15 805 Dosimat ............................ 14 B Balance .................................... 18 Bluetooth adapter Connecting ........................ 22 C Computer Connecting ........................ 11 Connecting Balance .............................. 18 Barcode reader ................... 20 Bluetooth adapter .............. 22 Computer ........................... 11 Dosing devices ................... 14 MSB devices ....................... 13 PC keyboard ....................... 20 Printer ................................ 17 Remote box ........................ 16 Stirrer or titration stand ...... 15 Touch Control ...................... 9 USB hub ............................. 22 Connecting a barcode reader . . . 20 Connector Double Pt electrode .............. 8 Generator electrode ............. 8 MSB ..................................... 2 Temperature sensor .............. 8 USB ...................................... 2 Controller Connector ............................ 8 Controller cable 6.2151.000 .... 11 Coulometric KF titration Certified water standards .... 37 Liquid samples .................... 39 Practical recommendations . 37 Principle ............................. 36 Sample size ........................ 39 Solid samples ..................... 40 Working conditions ............ 41 D Device software Update ................................. 2 Dosing command ....................... 3 ADD ..................................... 3 EMPTY ................................. 3 LQH ..................................... 3 PREP ..................................... 3 Dosing devices Connecting ........................ 14 Driver Install ................................. 11 E Electrostatic charge .................... 5 G GLP .......................................... 45 Guarantee ................................ 58 I Installation Driver ................................. 11 Instrument description ................ 2 Instrument type .......................... 8 K Keyboard ................................. 20 L LED On ..................................... 47 M Magnetic stirrer Connecting ........................ 15 Mains connection ....................... 8 Mains voltage ............................. 5 Maintenance ............................ 43 Measuring interface ................ 2, 8 Measuring mode ........................ 3 MEAS ................................... 3 MEAS T ................................ 3 Metrohm Serial Bus MSB, see also "MSB" ...................................... 13 MSB Connecting devices ............ 13 Connector ............................ 8 MSB.Connector .......................... 2 O Overview of the instrument ........ 7 P PC keyboard ............................. 20 Pins .......................................... 49 Printer ...................................... 17 Q Quality Management ................ 45 R Remote Input .................................. 50 Interface ............................. 49 Output ............................... 50 Remote box Connecting ........................ 16 Pin assignment ................... 49 S Safety instructions ...................... 4 Serial number ............................. 8 Service ....................................... 4 Service Agreement ................... 45 Stirrer Connecting ........................ 15 System test ............................... 10 T Titrando system .......................... 1 Titration mode ........................... 3 BRC ...................................... 3 KFC ...................................... 3 Titration stand .......................... 15 Connecting ........................ 15 Touch Control Connecting .......................... 9 U Update Device software .................... 2 USB Connector ............................ 8 USB connector ........................... 2 USB hub Connecting ........................ 22 V Validation ................................. 45
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83
Index W Warranty .................................. 58 Windows .................................. 12
84
851 Titrando

88518002EN Manual 851 Titrando

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851 Titrando

Teachware Metrohm AG CH-9101 Herisau teachware@metrohm.com

2 Overview of the instrument 3 Installation

3.5.4 3.5.5 3.5.6

Principle of the KF coulometry .......................................... 36

5 Handling and maintenance

General ................................................................................ 47 Karl Fischer Titration .......................................................... 47

8.1 Measuring interface ........................................................... 53 8.1.1 Generator electrode .............................................................. 53

8.1.2 8.1.3 8.2 8.3 8.4 8.5 8.6

9 Conformity and warranty

Tower-PC Sensors Dosing Interface USB Sample Processor Robotic Titrosampler

Relay Box Printer

The Titrando system

1.2 Instrument description

Titration modes Measuring modes Dosing commands

About the documentation

Symbols and conventions

1.5 Safety instructions

Working with liquids

1.5 Safety instructions

Flammable solvents and chemicals

Recycling and disposal

2 Overview of the instrument

2 Overview of the instrument

On Gen. 851 Titran

Front 851 Titrando

Rear 851 Titrando

Electrode connector (Ind.) For connecting a double Pt electrode. Socket F.

Setting up the instrument

Connecting a Touch Control Connect the Touch Control as follows:

3.2 Connecting controller

Connecting a Touch Control

2 Connect all peripheral devices.

2 Establish cable connections

3.2 Connecting controller

1 Set up the instrument

Connecting MSB devices

Dosino / Dosimat Dosino Dosimat

3.3 Connecting MSB devices

Connecting dosing devices

800 Dosino 700 Dosino 805 Dosimat 685 Dosimat

Proceed as follows: 1 Connect a dosing device

Connecting a dosing device

Connecting a stirrer or titration stand

Connecting MSB stirrer

3.3 Connecting MSB devices

Rod stirrer and titration stand

Connecting a remote box

Connecting a remote box

Connecting USB devices

3.4 Connecting USB devices

Mettler AX, MX, UMX, PG, AB-S, PB-S

Balance Mettler AE with interface option 011 or 012

3.4 Connecting USB devices

Connecting a PC keyboard (only Titrando with Touch Control)

Connecting a barcode reader

3.4 Connecting USB devices

Connecting a USB hub

Connecting a Bluetooth adapter

3.4 Connecting USB devices

Titration vessel for coulometric KF titration

3.5 Titration vessel for coulometric KF titration