622555_88518002EN_Manual_851_Titrando_

851 Titrando

Manual8.851.8002EN

Metrohm AGCH-9101 HerisauSwitzerlandPhone +41 71 353 85 85Fax +41 71 353 89 [email protected]

851 Titrando

Manual

8.851.8002EN 09.2010 ek

TeachwareMetrohm AGCH-9101 [email protected]

This documentation is protected by copyright. All rights reserved.

Although all the information given in this documentation has beenchecked with great care, errors cannot be entirely excluded. Should younotice any mistakes please send us your comments using the addressgiven above.

Documentation in additional languages can be found onhttp://products.metrohm.com under Literature/Technical documenta-tion.

http://products.metrohm.com

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents

851 Titrando ￭￭￭￭￭￭￭￭ III

Table of contents

1 Introduction 1

1.1 The Titrando system ............................................................. 1

1.2 Instrument description ......................................................... 2

1.3 Titration modes — Measuring modes — Dosing com-mands .................................................................................... 3

1.4 About the documentation ................................................... 31.4.1 Symbols and conventions ........................................................ 3

1.5 Safety instructions ................................................................ 41.5.1 General notes on safety ........................................................... 41.5.2 Electrical safety ........................................................................ 41.5.3 Working with liquids ................................................................ 51.5.4 Flammable solvents and chemicals ........................................... 61.5.5 Recycling and disposal ............................................................. 6

2 Overview of the instrument 7

3 Installation 9

3.1 Setting up the instrument .................................................... 93.1.1 Packaging ................................................................................ 93.1.2 Checks .................................................................................... 93.1.3 Location .................................................................................. 9

3.2 Connecting controller ........................................................... 93.2.1 Operation ................................................................................ 9

3.3 Connecting MSB devices ................................................... 133.3.1 Connecting dosing devices .................................................... 143.3.2 Connecting a stirrer or titration stand .................................... 153.3.3 Connecting a remote box ...................................................... 16

3.4 Connecting USB devices ..................................................... 173.4.1 General ................................................................................. 173.4.2 Connecting a printer .............................................................. 173.4.3 Connecting a balance ............................................................ 183.4.4 Connecting a PC keyboard (only Titrando with Touch Con-

trol) ....................................................................................... 203.4.5 Connecting a barcode reader ................................................. 203.4.6 Connecting a USB hub ........................................................... 223.4.7 Connecting a Bluetooth® adapter .......................................... 22

3.5 Titration vessel for coulometric KF titration .................... 253.5.1 Mounting the coulometer cell ................................................ 253.5.2 Coulometer cell - Default setup ............................................. 263.5.3 Coulometer cell with addition and aspiration tube (use with

Ti Stand) ................................................................................ 30

Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

IV ￭￭￭￭￭￭￭￭ 851 Titrando

3.5.4 Coulometer cell with aspiration equipment (use with Dos-ino) ....................................................................................... 31

3.5.5 Coulometer cell with KF oven ................................................ 323.5.6 Coulometer cell with Oven Sampler ....................................... 32

3.6 Connecting sensors ............................................................ 333.6.1 General ................................................................................. 333.6.2 Connecting generator electrode ............................................ 333.6.3 Connecting indicator electrode .............................................. 333.6.4 Connecting a temperature sensor .......................................... 34

4 Coulometric titration 36

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

4.2 Working with water standards ......................................... 374.2.1 Certified water standards ....................................................... 374.2.2 Practical recommendations .................................................... 37

4.3 Sample addition .................................................................. 394.3.1 Sample size ........................................................................... 394.3.2 Working with liquid samples .................................................. 394.3.3 Working with solid samples ................................................... 40

4.4 Optimum working conditions ........................................... 414.4.1 General ................................................................................. 414.4.2 Drift ...................................................................................... 414.4.3 Reagent exchange ................................................................. 414.4.4 Indicator electrode ................................................................ 42

5 Handling and maintenance 43

5.1 General information ........................................................... 435.1.1 Care ...................................................................................... 435.1.2 Maintenance by Metrohm Service .......................................... 43

5.2 Generator electrode ........................................................... 445.2.1 Generator electrode without diaphragm ................................ 445.2.2 Generator electrode with diaphragm ..................................... 44

5.3 Quality Management and validation with Metrohm ....... 45

6 Troubleshooting 47

6.1 General ................................................................................ 47

6.2 Karl Fischer Titration .......................................................... 47

7 Appendix 49

7.1 Remote interface ................................................................ 497.1.1 Pin assignment of the remote interface .................................. 49

8 Technical specifications 53

8.1 Measuring interface ........................................................... 538.1.1 Generator electrode .............................................................. 53

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851 Titrando ￭￭￭￭￭￭￭￭ V

8.1.2 Indicator electrode ................................................................ 538.1.3 Temperature .......................................................................... 53

8.2 Mains connection ............................................................... 54

8.3 Safety specifications ........................................................... 54

8.4 Electromagnetic compatibility (EMC) ................................ 54

8.5 Ambient temperature ......................................................... 55

8.6 Interfaces ............................................................................. 55

9 Conformity and warranty 56

9.1 Declaration of Conformity ................................................. 56

9.2 Quality Management Principles ........................................ 57

9.3 Warranty (guarantee) ......................................................... 58

10 Accessories 59

10.1 Scope of delivery ................................................................ 5910.1.1 851 Titrando 2.851.0110 ...................................................... 5910.1.2 851 Titrando 2.851.0010 ...................................................... 6510.1.3 851 Titrando 2.851.0020 ...................................................... 72

10.2 Optionales Zubehör ............................................................ 7910.2.1 851 Titrando 2.851.0010, 2.851.0020, 2.851.0110 .............. 79

Index 83

Table of figures ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

VI ￭￭￭￭￭￭￭￭ 851 Titrando

Table of figures

Figure 1 The Titrando system .......................................................................... 1Figure 2 Front 851 Titrando ............................................................................ 7Figure 3 Rear 851 Titrando ............................................................................. 8Figure 4 Connecting a Touch Control ............................................................ 10Figure 5 Connecting a computer ................................................................... 12Figure 6 MSB connections ............................................................................ 13Figure 7 Connecting a dosing device ............................................................. 15Figure 8 Connecting MSB stirrer .................................................................... 15Figure 9 Rod stirrer and titration stand .......................................................... 16Figure 10 Connecting a remote box ................................................................ 17Figure 11 Connecting a balance ...................................................................... 19Figure 12 Connecting a generator electrode ................................................... 33Figure 13 Connecting an indicator electrode ................................................... 34Figure 14 Connecting a temperature sensor .................................................... 34Figure 15 Connectors of the remote box ......................................................... 49Figure 16 Pin assignment of remote socket and plug ...................................... 49

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction

851 Titrando ￭￭￭￭￭￭￭￭ 1

1 Introduction

1.1 The Titrando system

The Titrando is the core of the modular Titrando system. Operation is car-ried 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. Thefollowing figure provides an overview of the peripheral devices you canconnect to the 851 Titrando.

MSBUSB

Controller

Input 1 / 2

Sensors

PC Keyboard

BarcodeReader

USB Hub

USB

/RS-

232

Con

vert

er

Balance

Touch Control

USB Sample ProcessorRobotic Titrosampler

Printer

Relay Box

Remote Box

Dosing Interface

Stirrer / Ti Stand Dosino Dosimat

On

Status

805Dosima

Metroh

On

Titrando

Tower-PC

Figure 1 The Titrando system

1.2 Instrument description ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

2 ￭￭￭￭￭￭￭￭ 851 Titrando

Up to three control devices (Titrandos, Dosing Interfaces, USB Sample Pro-cessors etc.) can be controlled via USB connection by PC Control/TouchControl.

You can request information on special applications in the "ApplicationBulletins" and "Application Notes"; available free of charge via theMetrohm agent responsible. Various monographs on the subjects of titra-tion techniques and electrodes are also available.

Updating the device software is described in the manual or the help of thecorresponding PC software respectively.

1.2 Instrument description

The 851 Titrando has the following characteristics:

￭ OperationOperation is carried out by means of a touch-sensitive Touch Controlor with a high-performance PC software.

￭ DosingAn external dosing drive.

￭ MSB connectorsFour MSB connectors (Metrohm Serial Bus) to control dosing devices(Dosimat with exchange unit or Dosino with dosing unit), stirrer ortitration stand and remote boxes.

￭ USB connectorsTwo USB connectors, through which devices such as printers, PC key-boards, barcode readers or additional control devices (Titrando, USBSample Processor, Dosing Interface, etc.) can be connected.

￭ Measuring interfaceThe measuring interface includes one measuring input (Gen.) for agenerator electrode, one measuring input (Temp.) for a temperaturesensor, e.g. Pt 1000 or NTC and one high-ohm measuring input (Ind.)for a double Pt electrode.

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851 Titrando ￭￭￭￭￭￭￭￭ 3

1.3 Titration modes — Measuring modes — Dosing com-mands

The following titration modes, measuring modes and dosing commandsare supported:

￭ MEAS For measurements the following measuring modes can be selected:

– T (temperature measurement),￭ KFC

Coulometric Karl Fischer titration for water determination with volta-metric measurement.

￭ BRCCoulometric 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 theinstrument into operation. The documentation contains informationand warnings which have to be followed by the user in order to ensuresafe operation of the instrument.

1.4.1 Symbols and conventionsThe following symbols and styles are used in this documentation:

Cross-reference to figure legend

The first number refers to the figure number, thesecond to the instrument part in the figure.

Instruction step

Carry out these steps in the sequence shown.

1.5 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

4 ￭￭￭￭￭￭￭￭ 851 Titrando

Warning

This symbol draws attention to a possible life hazardor risk of injury.

Warning

This symbol draws attention to a possible hazard dueto electrical current.

Warning

This symbol draws attention to a possible hazard dueto heat or hot instrument parts.

Warning

This symbol draws attention to a possible biologicalhazard.

Caution

This symbol draws attention to a possible damage ofinstruments or instrument parts.

Note

This symbol marks additional information and tips.

1.5 Safety instructions

1.5.1 General notes on safety

Warning

This instrument may only be operated in accordance with the specifica-tions in this documentation.

This instrument has left the factory in a flawless state in terms of technicalsafety. To maintain this state and ensure non-hazardous operation of theinstrument, the following instructions must be observed carefully.

1.5.2 Electrical safetyThe electrical safety when working with the instrument is ensured as partof the international standard IEC 61010.

Warning

Only personnel qualified by Metrohm are authorized to carry out servicework on electronic components.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction

851 Titrando ￭￭￭￭￭￭￭￭ 5

Warning

Never open the housing of the instrument. The instrument could bedamaged by this. There is also a risk of serious injury if live componentsare touched.

There are no parts inside the housing which can be serviced or replacedby the user.

Mains voltage

Warning

An incorrect mains voltage can damage the instrument.

Only operate this instrument with a mains voltage specified for it (seerear panel of the instrument).

Protection against electrostatic charges

Warning

Electronic components are sensitive to electrostatic charges and can bedestroyed by discharges.

Always pull the mains cable out of the mains connection socket beforeconnecting or disconnecting electrical appliances on the rear panel ofthe instrument.

1.5.3 Working with liquids

Caution

Periodically check all system connections for leaks. Observe the relevantregulations in respect to working with flammable and/or toxic fluidsand their disposal.

1.5 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

6 ￭￭￭￭￭￭￭￭ 851 Titrando

1.5.4 Flammable solvents and chemicals

Warning

All relevant safety measures are to be observed when working withflammable solvents and chemicals.

￭ Set up the instrument in a well-ventilated location (e.g. laboratoryflue).

￭ 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 disposalThis product is covered by European Directive 2002/96/EC, WEEE – Wastefrom Electrical and Electronic Equipment.

The correct disposal of your old equipment will help to prevent negativeeffects on the environment and public health.

More details about the disposal of your old equipment can be obtainedfrom your local authorities, from waste disposal companies or from yourlocal dealer.

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851 Titrando ￭￭￭￭￭￭￭￭ 7

2 Overview of the instrument

1

On

Gen.

23

851 Titrando

Figure 2 Front 851 Titrando

1 Bottle holderWith holding clamps, for two reagent bot-tles

2 LED "On"Lights up when the Titrando and a controller(Touch Control or computer) are connectedto the mains and switched on.

3 LED "Gen."Lights up when the Titrando and the gener-ator electrode are connected and switchedon.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

8 ￭￭￭￭￭￭￭￭ 851 Titrando

Figure 3 Rear 851 Titrando

1 Type plateContains specifications concerning mainsvoltage, instrument type and serial number.

2 USB connector (USB 1 and USB 2)USB ports (type A) for connecting printer,keyboard, barcode reader, additional Titran-dos, USB Sample Processor, etc.

3 Controller connectorConnection of a Touch Control or PC withinstalled PC software. Mini DIN, 9-pin.

4 MSB connector (MSB 1 bis MSB 4)Metrohm Serial Bus. For connecting externaldosing devices, stirrers to remote boxes.Mini DIN, 9-pin.

5 Mains connection socket 6 Measuring interface 1 (Input 1)

7 Electrode connector (Gen.)For connecting a generator electrode

8 Temperature sensor connector (Temp.)For connecting a temperature sensor, e.g.Pt1000 or NTC sensor. Two B sockets, 2mm.

9 Electrode connector (Ind.)For connecting a double Pt electrode. SocketF.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

851 Titrando ￭￭￭￭￭￭￭￭ 9

3 Installation

3.1 Setting up the instrument

3.1.1 PackagingThe instrument is supplied in highly protective special packaging togetherwith the separately packed accessories. Keep this packaging, as only thisensures safe transportation of the instrument.

3.1.2 ChecksImmediately after receipt, check whether the shipment has arrived com-plete and without damage by comparing it with the delivery note.

3.1.3 LocationThe instrument has been developed for operation indoors and may not beused in explosive environments.

Place the instrument in a location of the laboratory which is suitable foroperation, free of vibrations, protected from corrosive atmosphere, andcontamination by chemicals.

The instrument should be protected against excessive temperature fluctu-ations and direct sunlight.

3.2 Connecting controller

3.2.1 OperationTwo different versions are available for operating the 851 Titrando:

Caution

Take care to ensure that the mains cable is pulled out of the mains con-nection socket before either setting up or disconnecting connectionsbetween the instruments.

3.2.1.1 Connecting a Touch Control

Connect the Touch Control as follows:

3.2 Connecting controller ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

10 ￭￭￭￭￭￭￭￭ 851 Titrando

1 Note

The plug is protected against accidental disconnection of the cableby means of a "pull-out protection" feature. If you wish to pull outthe plug, you will first need to pull back the outer plug sleevemarked with arrows.

Insert the plug of the Touch Control connection cable into the con-troller 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. Atthe time of switch on system tests are run automatically on both theTitrando and the Touch Control. The LED On on the front of theTitrando lights up when the system test has been completed and theinstrument is ready for operation.

Caution

The Touch Control must be shut down properly by switching off withthe ON/OFF switch on the rear of the instrument before the currentsupply is interrupted. If this is not done, then there is a danger of dataloss. Because of the fact that the power supply for the Touch Control isprovided through the Titrando, you must never separate the Titrandofrom the mains (e.g. by switching off with a connector strip) before youhave switched off the Touch Control.

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851 Titrando ￭￭￭￭￭￭￭￭ 11

If you would prefer not to position the Touch Control directly next to theTitrando, then you can lengthen the connection between Titrando andTouch Control using the 6.2151.010 cable. The maximum connectionlength permitted is 5 m.

3.2.1.2 Connecting a computer

The 851 Titrando requires a USB connection to a computer in order to beable to be controlled by a PC software. When a controller cable6.2151.000 is used, the instrument can be connected directly, either to aUSB socket on a computer, to a connected USB hub or to a differentMetrohm control instrument.

Cable connection and driver installation

A driver installation is required in order to ensure that the 851 Titrando isrecognized by the PC software. To accomplish this, you must comply withthe procedures specified. The following steps are necessary:

1 Install software

￭ Insert the PC software installation CD and carry out the installa-tion 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 notalready done this.The LED On on the 851 Titrando is not yet illuminated!

￭ Connect the instrument to a USB connector (Type A) of your com-puter (see manual of your computer). The 6.2151.000 cable isused for this purpose.

3.2 Connecting controller ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

12 ￭￭￭￭￭￭￭￭ 851 Titrando

6.2151.000

Figure 5 Connecting a computer

For Windows 2000: the instrument is recognized and the driver isinstalled automatically.

For Windows XP: the instrument is recognized and the installationassistant for the driver is started automatically. Select the option"Install software automatically" and click on [Next >]. Exit the assis-tant with [Finish].

For Windows Vista: the instrument is recognized and the installa-tion assistant for the driver is started automatically. Select the option"Find and install driver software". Agree to all of the requests thatfollow. The installation assistant will be exited automatically.

The On LED on the 851 Titrando lights up when the driver installa-tion has been exited and the device is ready for operation.

Note

The plug on the instrument end of the 6.2151.000 controller cable isprotected against accidental disconnection by means of a pull-out pro-tection feature. If you wish to pull out the plug, you will first need topull back the outer plug sleeve marked with arrows.

Registering and configuring the instrument in the PC soft-ware

The instrument must be registered in the configuration of your PC soft-ware. Once that has been done, you can then configure it according toyour requirements. Proceed as follows:

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

851 Titrando ￭￭￭￭￭￭￭￭ 13

1 Set up the instrument

￭ Start up PC software.The instrument is recognized automatically. The configuration dia-log for the instrument is displayed.

￭ Make configuration settings for the instrument and its connec-tors.

More detailed information concerning the configuration of theinstrument can be found in the documentation for the respective PCsoftware.

3.3 Connecting MSB devices

In order to connect MSB devices, e.g.stirrers or dosing devices, Metrohminstruments are equipped with up a maximum of four connectors at whatis referred to as the Metrohm Serial Bus (MSB). Various kinds of peripheraldevices can be connected in sequence (in series, as a "daisy chain") at asingle MSB connector (8-pin Mini DIN socket) and controlled simultane-ously by the respective control instrument. In addition to the connectioncable, stirrers and the remote box are each equipped with their own MSBsocket for this purpose.

The following illustration provides an overview of the devices that can beconnected to an MSB socket, along with a number of different cablingvariations.

MSB

Stirrer / Ti Stand

Dosimat / Dosino

Dosimat

Remote Box

Dosino / DosimatDosino

Relay Box

Ti Stand / Stirrer

Figure 6 MSB connections

The question of which peripheral devices are supported depends on thecontrol instrument.

3.3 Connecting MSB devices ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

14 ￭￭￭￭￭￭￭￭ 851 Titrando

Note

When connecting MSB devices together, the following must beobserved:

￭ Only one device of the same type can be used at a single MSB con-nector at one time.

￭ Type 700 Dosino and 685 Dosimat dosing devices cannot be con-nected 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 con-trol instrument recognizes when it is switched on which instrument isconnected at which MSB connector. The operating unit or the controlsoftware enters the connected MSB devices into the system configura-tion (Device manager).

MSB connections can be extended with the 6.2151.010 cable. The lengthof the connection must not exceed a maximum of 15 m.

3.3.1 Connecting dosing devicesFour dosing devices can be connected to the instrument (MSB 1 toMSB 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.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

851 Titrando ￭￭￭￭￭￭￭￭ 15

Figure 7 Connecting a dosing device

3.3.2 Connecting a stirrer or titration standYou can use a magnetic stirrer 801 Stirrer or 803 Ti Stand (stirring "frombelow") or the 804 Ti Stand with a rod stirrer 802 Stirrer (stirring "fromabove").

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 therear of the control instrument.

￭ If desired, connect the rod stirrer to the stirrer socket (with stirrersymbol) of the titration stand.

￭ Start the control software.

Figure 8 Connecting MSB stirrer

3.3 Connecting MSB devices ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

16 ￭￭￭￭￭￭￭￭ 851 Titrando

Figure 9 Rod stirrer and titration stand

3.3.3 Connecting a remote boxInstruments that are controlled via remote lines and/or which send controlsignals via remote lines can be connected using the 6.2148.010 remotebox. In addition to Metrohm, other instrument manufacturers also usesimilar connectors that make it possible to connect different instrumentstogether. These interfaces are also frequently given the designations "TTLLogic", "I/O Control" or "Relay Control" and generally have a signal levelof 5 volts.

Control signals are understood to be electrical line statuses or brief(＞ 200 ms) electrical pulses which display the operational state of aninstrument or which trigger or report an event. Sequences on a variety ofinstruments can thus be coordinated in a single complex automation sys-tem. 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.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

851 Titrando ￭￭￭￭￭￭￭￭ 17

Figure 10 Connecting a remote box

You can, for example, connect an 849 Level Control Box (fill level monitorin a waste canister) or a 731 Relay Box (switch box for 230/110 volt alter-nating current sockets and low-voltage direct current outlets). The remotebox also has an MSB socket at which a further MSB instrument, e.g. adosing device or a stirrer, can be connected.

You will find precise information concerning the pin assignment of theinterface on the remote box in the appendix (see Chapter 7.1, page 49).

3.4 Connecting USB devices

3.4.1 GeneralThe 851 Titrando has two USB connectors (type A sockets) for peripheraldevices with USB interfaces. The Titrando functions as a USB hub (distribu-tor) no matter how it is operated. If you wish to connect more than twodevices to the USB, you can also use an additional commercially availableUSB hub .

Caution

If you operate the Titrando with the aid of the Touch Control, take careto ensure that the Touch Control is switched off when you set up ordisconnect connections between the various instruments. If you use aPC software to control the Titrando, you should exit the programbefore you set up or disconnect the USB connections.

3.4.2 Connecting a printerPrinters that are connected to the 851 Titrando with Touch Control mustmeet 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.

3.4 Connecting USB devices ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

18 ￭￭￭￭￭￭￭￭ 851 Titrando

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 ofthe 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 balanceIf you control the 851 Titrando with a PC software, connect the balancedirectly to the serial port (COM) on the computer. This is usually 9-pin andmarked with the symbol IOIOI. If you operate the Titrando with the helpof the Touch Control, you will need the 6.2148.020 RS-232/USB Box forconnecting a balance.

The following table offers an overview of the balances that you can usetogether with the Titrando system and of which cable you will need forconnection to the RS-232 interface:

Balance Cable

AND ER-60, 120, 180,182FR-200, 300FX 200, 300, 320with RS-232 interface (OP-03)

6.2125.020 + 6.2125.010

Mettler AB, AG, PR (LC-RS9) In the scope of delivery for thebalance

Mettler AM, PM, PE with interfaceoption 016

or

Mettler AJ, PJ with interfaceoption 018

6.2146.020 + 6.2125.010

also from Mettler: ME 47473adapter and either ME 42500hand switch or ME 46278 footswitch

Mettler AT 6.2146.020 + 6.2125.010

also from Mettler: ME 42500hand switch or ME 46278 footswitch

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

6.2134.120

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

851 Titrando ￭￭￭￭￭￭￭￭ 19

Balance Cable

Mettler AE with interface option011 or 012

6.2125.020 + 6.2125.010

also from Mettler: ME 42500hand switch or ME 46278 footswitch

Ohaus Voyager, Explorer, Analyti-cal Plus

Cable AS017-09 from Ohaus

Precisa balances with RS-232-Cinterface

6.2125.080 + 6.2125.010

Sartorius MP8, MC1 6.2134.060

Shimadzu BX, BW 6.2125.080 + 6.2125.010

Operation with Touch Control

Connect the balance as follows:

1 With the aid of the 6.2151.030 cable, connect the USB connector ofthe 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 theRS-232 interface of the balance (see table for cable).

Figure 11 Connecting a balance


4 Switch on the balance.

5 Switch on the RS-232 interface of the balance.


20 ￭￭￭￭￭￭￭￭ 851 Titrando

6 Configure the RS-232 interface of the RS-232/USB Box in the devicemanager of the Touch Control as described in the manual for the PCControl / Touch Control.

Operation with PC software

Connect the balance as follows:

1 Connect the RS-232 interface of the computer with the RS-232 inter-face 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 man-ager of the PC Control software as described in the manual for thePC 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 youoperate the 851 Titrando with the aid of the Touch Control, then you canconnect 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 USBsockets of the Titrando.


The keyboard will be recognized automatically and entered in thedevice manager.

3 Configure the keyboard in the device manager of the Touch Controlas described in the manual for the PC Control / Touch Control.

3.4.5 Connecting a barcode readerThe barcode reader is used as an aid for text and numerical input. You canconnect a barcode reader with USB interface.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

851 Titrando ￭￭￭￭￭￭￭￭ 21

Operation with Touch Control

Connect the barcode reader as follows:

1 Insert the USB plug of the barcode reader (type A) into one of theUSB sockets of the Titrando.


The barcode reader will be recognized automatically and entered inthe device manager of the Touch Control.

3 Configure the barcode reader in the device manager as described inthe 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 theUSB sockets of the Titrando or the computer.

2 Start the PC software.

3 Configure the barcode reader in the device manager as described inthe manual for the PC Control / Touch Control.

Settings on the barcode reader:

Program the barcode reader as follows (also see manual for the barcodereader).

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 man-ual for PC Control / Touch Control).

3 Make sure that the barcode reader is set in such a way that Ctrl char-acters (ASCII 00 to 31) can be sent.


22 ￭￭￭￭￭￭￭￭ 851 Titrando

4 Program the barcode reader in such a way that the ASCII character02 (STX or Ctrl B) is sent as the first character. This first character isnormally referred to as the "Preamble" or "Prefix Code".

5 Program the barcode reader in such a way that the ASCII character04 (EOT or Ctrl D) is sent as the last character. This last character isnormally referred to as the "Postamble", "Record Suffix" or "PostfixCode".

6 Exit the programming mode.

3.4.6 Connecting a USB hubIf you wish to connect more than two devices to the USB connector of theTitrando, 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 ofthe Titrando (type A) with the USB connector of the hub (type B, seemanual 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® adapterPrinters and balances (or other devices with RS-232 connection) can beoptionally connected using a wireless Bluetooth® connection. Printers andbalance models with integrated Bluetooth® functionality are to be recom-mended for this purpose. Bluetooth® printer adapters for the USB inter-face can be obtained commercially, as can also Bluetooth® serial adaptersfor RS-232 connections (e.g. for balances).

Note

Bluetooth® is a registered and copyrighted name of the Bluetooth®

Special Interest Group (Bluetooth® SIG, Inc.).

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

851 Titrando ￭￭￭￭￭￭￭￭ 23

PC Control

If the Titrando system is operated with the PC Control software, then aBluetooth USB adapter can be connected to one of the USB sockets onthe computer (or of the Titrando / USB Sample Processor). The driver soft-ware (for MS Windows 2000/XP) included in the scope of delivery by themanufacturer of the Bluetooth adapter must be installed in accordancewith the directions contained in the associated manual. A Bluetooth USBadapter must support the Bluetooth specifications HCRP (HardcopyCable Replacement Profile) for printers and/or SPP (Serial Port Pro-file) for balances or RS-232 connections. Printer drivers must be set upprior to the installation of the Bluetooth adapter.

840 Touch Control

If the Titrando system is operated as a stand-alone system with a 840Touch Control, then the Metrohm Bluetooth USB adapter for the840 (6.2162.000, Bluetooth® V1.1 qualified Class 2 device) is required fora Bluetooth connection.

Note

The Metrohm Bluetooth USB adapter cannot be operated on acomputer. The adapter is intended exclusively for use in a Titrando sys-tem in stand-alone operation, i.e. with a 840 Touch Control operatingunit as controller. The prerequisite is the Touch Control Software ver-sion 5.840.0130 or higher.

The Metrohm Bluetooth USB adapter permits wireless data transfer fordistances 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 ofthe Titrando.


The Bluetooth USB adapter is recognized automatically.

3 Configure the adapter in the device manager of the Touch Control asdescribed in the manual for the PC Control / Touch Control.

Printer and Bluetooth

A Bluetooth-compatible printer or a Bluetooth printer adapter must sup-port the HCRP (Hardcopy Cable Replacement Profile).


24 ￭￭￭￭￭￭￭￭ 851 Titrando

The necessary settings for a Bluetooth-compatible printer can be found inthe user manual for it. Bluetooth printer adapters can usually be connec-ted without configuration to the USB connector of the respective printer.Comply with the instructions contained in the documentation for theprinter adapter. Enter the definition of the printer type in the device man-ager of the Touch Control.

Balances and Bluetooth

A Bluetooth-compatible balance or a Bluetooth serial adapter must com-ply with the SPP (Serial Port Profile) in accordance to Bluetooth specifi-cations. If the balance manufacturer offers a specific Bluetooth serialadapter, then this is to be preferred to a commercially available adapter.

Bluetooth serial adapters must be configured on the PC with the help ofan auxiliary program supplied by the manufacturer. The data transferparameters of the instrument and the adapter must match one another.The Bluetooth serial adapter must be defined as the acceptor and not asthe initiator of a serial connection. Authentication with a PIN code is notsupported.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

851 Titrando ￭￭￭￭￭￭￭￭ 25

3.5 Titration vessel for coulometric KF titration

3.5.1 Mounting the coulometer cell

Mounting the coulometer cell

6.2047.020

6.1464.320

6.2016.050

1

2

Mount the coulometer cell as follows on a titration stand:

1 Fix the 6.2047.020 titration vessel holder to the 6.2016.050 supportrod.

2 Slide the 6.1464.320 titration vessel from above into the titrationvessel holder.

3.5 Titration vessel for coulometric KF titration ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

26 ￭￭￭￭￭￭￭￭ 851 Titrando

3.5.2 Coulometer cell - Default setup

Filling the adsorber tube

Before setting up the coulometer cell the 6.1403.030 adsorber tube hasto be filled with 6.2811.000 molecular sieve. Proceed as follows:

1

2

3

4

6.1403.030

6.2811.000

1 Insert a small cotton plug into the adsorber tube below. Do not packthe cotton too tightly.

2 Fill up the molecular sieve up to the ¾ level.

3 Place a small cotton plug on the molecular sieve. Do not pack thecotton too tightly.

4 Seal the adsorber tube with the appropriate cover.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

851 Titrando ￭￭￭￭￭￭￭￭ 27

Setting up the coulometer cell

6.1903.030

6.1464.320

6.2713.010

6.1437.000

6.0345.100

6.2713.020

6.1403.030

6.1448.020

6.2701.040

6.2713.000

6.0341.100

2

1

2

3

2

4

5

6

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 putthem 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 thelower ground joint edge.

3 Insert the 6.0341.100 indicator electrode into the left ground jointopening.


28 ￭￭￭￭￭￭￭￭ 851 Titrando

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 theadsorber tube into the ground joint opening in the middle.

6 Put the 6.1448.020 septum onto the front opening of the titrationvessel 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 dia-phragm)

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 ofthe anolyte should roughly be 1-2 mm above the level of the catho-lyte.

The level of the anolyte and the catholyte must roughly be even, sothat no anolyte flows into the generator electrode or catholyte intothe titration vessel, respectively.

3 Close the last opening with the 6.1437.000 ground joint stopper.

Filling the titration vessel (generator electrode withoutdiaphragm)

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.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

851 Titrando ￭￭￭￭￭￭￭￭ 29

1

2 Unscrew the cover of the generator electrode.

2

3 Screw the 6.2104.020 electrode cable tightly onto the indicator elec-trode.

4 Screw the 6.2104.120 electrode cable tightly onto the generatorelectrode.

3

4

6.2104.020

6.2104.120


30 ￭￭￭￭￭￭￭￭ 851 Titrando

Mark the screw head of the electrode cable. This prevents you frommixing-up the indicator and generator electrode.

3.5.3 Coulometer cell with addition and aspiration tube (use with TiStand)

Mounting the addition and aspiration tube

6.1437.000

6.2713.010

6.1439.010

1

2

3

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 addi-tion and aspiration tube.

2 Place the 6.1437.000 stopper onto the ground joint sleeve on theaddition and aspiration tube.

3 Insert altogether into the ground joint opening.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

851 Titrando ￭￭￭￭￭￭￭￭ 31

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 acomplete dosing unit and a 50 mL glass cylinder. For aspirating greasysamples with which only the sample and not the whole reagent is aspira-ted, we recommend using a dosing unit with a 20 mL cylinder. For highlyviscous samples a dosing unit with a 10 mL cylinder is suitable.

Mounting the aspiration tip

2

6.1543.070

31

6.1446.060

6.2730.030

Insert the aspiration tip as follows into the coulometer cell:

1 Screw the 6.2730.030 nipple, with stopper and O-ring, onto the6.1446.060 stopper.

2 Pull out the stopper.

3 Slide the 6.1534.070 aspiration tip through the stopper.


32 ￭￭￭￭￭￭￭￭ 851 Titrando

4

4 Insert the stopper together with the aspiration tip into the groundjoint opening with the ground joint sleeve.

Slide the aspiration tip into the coulometer cell as far as it touchesthe vessel base.

3.5.5 Coulometer cell with KF ovenWith samples that release their water only slowly or only at higher tem-peratures, the heating method is used. The sample is being heated in a KFoven and the water released is forwarded together with a carrier gas intothe titration vessel. A detailed description of setting up the coulometer cellwith the KF oven can be found in the manual of the oven.

3.5.6 Coulometer cell with Oven SamplerWith a large amount of samples the determination of the water contentcan be automated with the aid of an Oven Sample Processor. A detaileddescription of setting up the coulometer cell with the Oven Sampler canbe found in the manual of the Oven Sampler.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

851 Titrando ￭￭￭￭￭￭￭￭ 33

3.6 Connecting sensors

3.6.1 GeneralThe measuring interface includes one measuring input (Gen.) for a gener-ator electrode, one measuring input (Temp.) for a temperature sensor,e.g. Pt 1000 or NTC and one high-ohm measuring input (Ind.) for a dou-ble Pt electrode.

3.6.2 Connecting generator electrodeConnect the generator electrode as follows:

1 Plug the electrode plug into the Gen. socket of the Titrando.

Temp.

Gen.

Figure 12 Connecting a generator electrode

Note

The electrode cable is protected against accidental disconnectionof the cable by means of a pull-out protection feature. If you wishto remove the plug, you will first need to pull back the outer plugsleeve.

3.6.3 Connecting indicator electrodeConnect the indicator electrode as follows:

1 Plug the electrode plug into the Ind. socket of the Titrando.

3.6 Connecting sensors ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

34 ￭￭￭￭￭￭￭￭ 851 Titrando

Figure 13 Connecting an indicator electrode

Note

The electrode cable is protected against accidental disconnectionof the cable by means of a pull-out protection feature. If you wishto remove the plug, you will first need to pull back the outer plugsleeve.

3.6.4 Connecting a temperature sensorA temperature sensor of the Pt 1000 or NTC type can be connected to theTemp. connector.

Connect the temperature sensor as follows:

1 Plug the temperature sensor plugs into the Temp. sockets of theTitrando.

Temp.

Ind.

Figure 14 Connecting a temperature sensor

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

851 Titrando ￭￭￭￭￭￭￭￭ 35

Note

The red plug must always be plugged into the red socket at thetemperature sensor for the purpose of shielding against disrup-tions.

4.1 Principle of the KF coulometry ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

36 ￭￭￭￭￭￭￭￭ 851 Titrando

4 Coulometric titration

4.1 Principle of the KF coulometry

The coulometric Karl Fischer titration is a variation of the classicwater determination method according to Karl Fischer. The conventionalmethod works with a methanolic solution of iodine, sulfur dioxide and abase as buffer substance. When titrating a sample containing water, sev-eral reactions take place, which can be summarized by the followingequation:

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 gener-ated electrochemically directly in the electrolyte containing iodine ("elec-tronic buret"). Between the amount of electric charge and the amount ofgenerated iodine, there is a strictly quantitative relationship, which is usedfor high-precision dosing of the iodine. No titer needs to be determined,as the coulometric Karl Fischer method is an absolute determination. Itmust only be ensured that the reaction generating the iodine runs with a100 % of current efficiency. This is the case with all the reagents availableat present.

The endpoint indication is effected voltametrically by modulating an alter-nating current of constant strength to a double Pt electrode. This produ-ces a voltage difference between the Pt wires, which significantly declineswhen lowest amounts of free iodine are present. This circumstance is usedfor detecting the endpoint of the titration.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Coulometric titration

851 Titrando ￭￭￭￭￭￭￭￭ 37

4.2 Working with water standards

4.2.1 Certified water standardsFor validating the instrument as a whole, integrated system, commerciallyavailable, certified water standards with water contents of 1.00 ± 0.003mg/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 prefer-red.

Table 1 Recommended sample sizes

Water standard solution 1.0 mg/g 0.2…2.0 g

Water standard solution 0.1 mg/g 0.5…5.0 g

4.2.2 Practical recommendationsFor validation, it is essential to work very accurately. In order to reducepossible measuring inaccuracies, sample preparation and processingshould 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 fora few seconds.

The inside of the syringe is being rinsed by standard and freed fromwater 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 anair bubble to ensure that no solution remains in the needle.

4.2 Working with water standards ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

38 ￭￭￭￭￭￭￭￭ 851 Titrando

9 Wipe off the needle with a Kleenex cloth and cover it with theappropriate 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 byhand, press [START] and inject approx. 1 mL of the standardthrough the septum.

There are two possibilities:

12 Inject the standard without immersing the needle into the reagentliquid. If a little drop remains on the end of the needle, it should beaspirated back before pulling the needle out of the septum.

The standard must not be expelled onto the electrode nor onto thesides 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 bal-ance.

15 Read off the value displayed by the balance and enter it as samplesize on the Touch Control or in PC Control.

16 As soon as the determination has been finished and the titration cellhas been conditioned (drift stable), the next determination can bestarted.


851 Titrando ￭￭￭￭￭￭￭￭ 39

4.3 Sample addition

This chapter contains a few notes concerning sample addition. A com-plete description of this topic is not possible here. Further notes can befound in the literature by the reagent manufacturers and in the followingMetrohm Application Bulletins:

Bulletin No. Title

No. 142 Karl Fischer water determinations in gaseous samples

No. 145 The determination of small water contents in plastics

No. 209 Water determinations in insulating oils, hydrocarbons and their products

No. 273 Validation of KF coulometers according to GLP / ISO 9001

4.3.1 Sample sizeThe sample size should be small in order to be able to titrate as manysamples as possible in the same electrolyte solution and in order to keepthe titration time short. However, ensure that the sample contains at least50 µg of H2O. The following table provides clues for the sample size.

Table 2 Recommended sample sizes

Content of the sample Sample size H2O, to be determined

(Water content)

10000 ppm = 1 % 10 mg…100 mg 100 µg…1000 µg

1000 ppm = 0.1 % 100 mg…1 g 100 µg…1000 µg

100 ppm = 0.01 % 1 g 100 µg

10 ppm = 0.001 % 5 g 50 µg

4.3.2 Working with liquid samplesLiquid samples are added with a syringe. Either use a syringe with along needle, and immerse it into the reagent when injecting, or inject witha short needle and aspirate the last drop back into the needle. The sampleamount injected is best determined by reweighing.

For the determination of traces and validations glass syringes shouldbe used. We recommend obtaining them from a specialized syringe man-ufacturer.

Highly volatile samples and samples of low viscosity should becooled before sampling. This reduces losses during processing. The

4.3 Sample addition ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

40 ￭￭￭￭￭￭￭￭ 851 Titrando

syringe, however, must not be cooled directly, as condensates could beformed. For the same reason, avoid aspirating air through a syringe thathas been cooled by filling it with a cooled sample.

Samples of high viscosity can be thinned by heating. The syringe mustbe heated as well. The same target can be reached by diluting with suita-ble solvents. In this case the water content of the solvent has to be deter-mined and subtracted as blank value.

Paste and fats can be added to the measuring cell with a syringe with-out needle. You can use the ground joint opening for this. If you alsowant to aspirate, you can use the opening with the septum stopper. Thesample amount is best determined by reweighing.

With samples containing only traces of water the syringe has to be pre-dried well. If possible, the syringe should be rinsed with the sample solu-tion by filling in and rejecting solution several times.

4.3.3 Working with solid samplesIf possible, solid samples are to be extracted or dissolved in a suitable sol-vent. The resulting solution is being injected, in doing so, a blank valuecorrection for the solvent has to be carried out.

If there is no suitable solvent for a solid sample, or if the sample is reactingwith the Karl Fischer solution, then the drying oven should be used.

If solid samples have to be added directly to the measuring cell, the cellwithout diaphragm should be used. The samples can be added throughthe 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


851 Titrando ￭￭￭￭￭￭￭￭ 41

4.4 Optimum working conditions

4.4.1 GeneralIf a well-pre-dried titration vessel with a generator electrode without dia-phragm is being set up, the base drift is reached within 30 minutesapproximately. We recommend carefully shaking the titration vessel sev-eral times during this time.

With a generator electrode with diaphragm you should expect a prepara-tion time of approx. 2 hours.

To obtain precise determinations of amounts of water smaller than 100µg, it may be of advantage to condition the instrument over night beforeusing it.

If the Titrando is switched off for a longer period with a filled titration ves-sel, 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 µg/min is all right. Lower values, how-ever, are quite possible. Higher but stable values still produce good results,because the drift can be compensated. More detailed information can befound in the corresponding software manual.

A constantly high drift can be caused by water-containing deposits ininaccessible parts of the cell. In these cases, shaking the titration vesselcan reduce the value. Ensure that there are no drops above the liquid levelin the titration vessel.

Generator electrodes with diaphragm should only be shaken to an extentthat the catholyte and anolyte are not being mixed up. If the drift remainshigh for a longer time after shaking the cell, then the electrolyte solutionshould be exchanged.

When working with the oven, a drift of ≤ 10 µg/min is all right. The driftdepends on the gas flow (the smaller the gas flow, the lower the drift).

4.4.3 Reagent exchangeThe 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.

4.4 Optimum working conditions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

42 ￭￭￭￭￭￭￭￭ 851 Titrando

The simplest way to remove the used electrolyte solution out of the cell isby aspirating. To do this, you can use e.g. an 803 TiStand with built-inmembrane pump. An advantage is, that the cell does not have to be dis-assembled.

In the case of severe contamination, the cell can be rinsed with a suitablesolvent which is aspirated as well.

When using the generator electrode with diaphragm, the catholyte shouldbe exchanged approx. once a week. Longer use can cause blackening andyellow precipitates in the cathode chamber. A discernable stench is also asign for having used the catholyte for too long.

4.4.4 Indicator electrodeA new indicator electrode can take a certain warm-up time for formingthe surface. During this time, unexpectedly long titration times and highmeasurement results can occur. This phenomenon will, however, disap-pear after a short time of use. In order to accelerate the setting of a newindicator electrode, the 851 Titrando can be conditioned e.g. over night.

A contaminated indicator electrode can be carefully cleaned with an abra-sive agent (Alox (6.2802.000 polishing set) or toothpaste). After the clean-ing, rinse with ethanol.

The two Pt wires of the indicator electrode should run as parallel as possi-ble to one another. Check when inserting.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Handling and maintenance

851 Titrando ￭￭￭￭￭￭￭￭ 43

5 Handling and maintenance

5.1 General information

5.1.1 CareThe 851 Titrando requires appropriate care. Excess contamination of theinstrument may result in functional disruptions and a reduction in the serv-ice 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 mainsconnection socket) should be protected from contamination.

Caution

Although this is extensively prevented by design measures, the mainsplug should be unplugged immediately if aggressive media has penetra-ted the inside of the instrument, so as to avoid serious damage to theinstrument electronics. In such cases, the Metrohm Service must beinformed.

5.1.2 Maintenance by Metrohm ServiceMaintenance of the 851 Titrando is best carried out as part of an annualservice, which is performed by specialist personnel of the Metrohm com-pany. If working frequently with caustic and corrosive chemicals, a shortermaintenance interval could be necessary.

The Metrohm service department offers every form of technical advice formaintenance and service of all Metrohm instruments.

5.2 Generator electrode ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

44 ￭￭￭￭￭￭￭￭ 851 Titrando

5.2 Generator electrode

5.2.1 Generator electrode without diaphragmThe 6.0345.100 generator electrode without diaphragm is easy to handleand to clean. It only needs one reagent and is quickly ready to be used (nomoisture deposits in the diaphragm !). The generator electrode withoutdiaphragm is suitable for most applications. It especially should be usedfor severely contaminated samples.

5.2.1.1 Reagents

Only use reagents which are especially determined for generator electro-des without diaphragms. Details can be found in the documentation ofthe reagent manufacturers.

5.2.1.2 Cleaning

As a rule, the electrolyte solution can be exchanged without special clean-ing of the parts. If cleaning is necessary anyway, ensure that the Pt net ofthe 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 theparts are being dried in the drying oven the temperature must not exceed70°C (plastic parts!).

5.2.2 Generator electrode with diaphragmThe 6.0344.100 generator electrode with diaphragm should be used if thesamples contain ketones because special reagents for ketones are onlyavailable for generator electrodes with diaphragm. If your reagent has alow conductivity, e.g. because you have to add chloroform to the samplebecause of its solubility, you should prefer the generator electrode withdiaphragm. It is also recommended when you have to rely on a high accu-racy in the lowest trace range.

5.2.2.1 Reagents

Reagents for the coulometric water determination with generator electro-des with diaphragm consist of the anode solution (anolyte), which is filledin the titration vessel, and the cathode solution (catholyte), which is filledin the generator electrode.

For the water determinations in ketones, special reagents have to be used(see the documentation of the reagent manufacturers).

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Handling and maintenance

851 Titrando ￭￭￭￭￭￭￭￭ 45

5.2.2.2 Cleaning

As a rule, the electrolyte solution can be exchanged without special clean-ing of the parts. If cleaning is necessary anyway, ensure that the Pt net ofthe 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 letthe filling flow out. Repeat 2-3 times. This procedure should also be car-ried out after the cleaning described above.

Dry well all parts after cleaning. A hairdryer can be used for this. If theparts are being dried in the drying oven the temperature must not exceed70°C (plastic parts!).

5.3 Quality Management and validation with Metrohm

Quality Management

Metrohm offers you comprehensive support in implementing quality man-agement measures for instruments and software. Further information onthis can be found in the brochure «Quality Management withMetrohm» available from your local Metrohm agent.

Validation

Please contact your local Metrohm agent for support in validating instru-ments and software. Here you can also obtain validation documentationto provide help for carrying out the Installation Qualification (IQ) andthe Operational Qualification (OQ). IQ and OQ are also offered as aservice by the Metrohm agents. In addition, various application bulletinsare also available on the subject, which also contain Standard Operat-ing Procedures (SOP) for testing analytical measuring instruments forreproducibility and correctness.

Maintenance

Electronic and mechanical functional groups in Metrohm instruments canand should be checked as part of regular maintenance by specialist per-sonnel from Metrohm. Please ask your local Metrohm agent regarding the

5.3 Quality Management and validation with Metrohm ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

46 ￭￭￭￭￭￭￭￭ 851 Titrando

precise terms and conditions involved in concluding a correspondingmaintenance agreement.

Note

You can find information on the subjects of quality management, vali-dation and maintenance as well as an overview of the documents cur-rently available at www.metrohm.com/com/ under Support.

http://www.metrohm.com/com/

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6 Troubleshooting

851 Titrando ￭￭￭￭￭￭￭￭ 47

6 Troubleshooting

6.1 General

Problem Cause Remedy

LED "On" is not illu-

minated although

the Titrando is con-

nected to the mains.

The Touch Control or the

computer has not been

switched on yet or the

plugs are not correctly

connected.

Check the plug connections and switch on the

Touch Control or the computer.

6.2 Karl Fischer Titration


The drift is very high

during conditioning.

The titration cell is leaking. ￭ Check seals and septum. If necessary,

replace.

￭ Replace molecular sieve.

The drift becomes

greater after each

titration.

The sample releases water

very slowly.

￭ Adjust the method.

￭ Add solubilizer.

￭ Increase the temperature (possibly using a

KF oven).

￭ See technical literature.

A side reaction is taking

place.

￭ Use special reagents.

￭ Adjust the method (increase/decrease the

temperature, external extraction).

￭ See technical literature.

The pH value is not in the

optimum range anymore.

Add buffer, see technical literature.

The titration will not

be finished.

The titration cell is leaking. ￭ 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).

The stop criterion is unsuit-

able.

Change the control parameters (see manual/

help of the software used)

￭ Increase the stop drift.

6.2 Karl Fischer Titration ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

48 ￭￭￭￭￭￭￭￭ 851 Titrando


￭ Select a short delay time.

See also: The drift increases

after each titration.

The sample is over-

titrated.

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 condi-

tioning, display the drift and add sample

without starting the titration. Select a value

below the highest drift as dosing rate.

￭ Stir faster.

The amount of methanol in

the working medium is too

low.

￭ Replace the working medium.

￭ Reduce the amount of solubilizer, if work-

ing with solvent mixtures, see technical lit-

erature.

The indicator electrode

could be covered.

Clean the electrode with ethanol or a suitable

solvent.

The solution

becomes darker

after each titration.

Replace the working medium.

The indicator electrode

could be covered.

Clean the electrode with ethanol or a suitable

solvent.

The indicator electrode has

a short circuit.

1. Check the Pt wires.

2. Switch on the electrode test.

The endpoint is

reached too quickly.

The dosing rate outside the

control range is too high.

1. Select user defined titration rate

2. Reduce the dosing rate (see manual/help of

the software used).

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7 Appendix

851 Titrando ￭￭￭￭￭￭￭￭ 49

7 Appendix

7.1 Remote interface

The 6.2148.010 remote box allows devices to be controlled which cannotbe connected directly to the MSB interface of the Titrando.

1

2

3

Figure 15 Connectors of the remote box

1 CableFor connecting the Titrando.

2 MSB connectorMetrohm Serial Bus. For connecting externaldosing devices or stirrers.

3 Remote connectorFor connecting devices with a remote inter-face.

7.1.1 Pin assignment of the remote interface13

1

1425

113

1425

Figure 16 Pin assignment of remote socket and plug

The above presentation of the pin assignment of a Metrohm remote inter-face applies not only for the remote box, but also for all Metrohm deviceswith 25-pin D-Sub remote connection.

7.1 Remote interface ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

50 ￭￭￭￭￭￭￭￭ 851 Titrando

Inputs

+5 V approx. 50 kΩ Pull-up

tptp >20 ms

active = low, inactive = high

Outputs

Open Collector

tptp >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 theindividual pins and their function.

Table 3 Inputs and outputs of the remote interface

Assignment Pin No. Function

Input 0 21 Start

Input 1 9 Stop

Input 2 22 Quit

Input 3 10

Input 4 23 -

Input 5 11

Input 6 24

Input 7 12

Output 0 5 Ready

Output 1 18 Conditioning OK

Output 2 4 Determination

Output 3 17 EOD

Output 4 3

Output 5 16 Error

Output 6 1

Output 7 2 Warning

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7 Appendix

851 Titrando ￭￭￭￭￭￭￭￭ 51

Assignment Pin No. Function

Output 8 6

Output 9 7

Output 10 8

Output 11 13

Output 12 19

Output 13 20

0 volts / GND 14

+5 volts 15

0 volts / GND 25

Table 4 Explanation of the individual functions

Function Explanation

Start The current method is started at the time ofactivation.

tpulse > 100 ms

Stop The current method is canceled (Stop) at thetime of activation.

tpulse > 100 ms

Quit The current command in the determinationrun will be canceled at the time of activation.

tpulse > 100 ms

Ready The instrument is ready to receive a start sig-nal.

Conditioning OK The line is set when Conditioning with SETand KFT titration is at OK. The line remainsset until the determination is started with[START].

Determination The instrument performs a data-generatingdetermination.

EOD End of Determination.

Pulse (tpulse = 200 ms) after a determinationor after a buffer/standard during calibrationusing a Sample Processor.

Error The line is set for error message display.

7.1 Remote interface ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

52 ￭￭￭￭￭￭￭￭ 851 Titrando

Function Explanation

Warning The line is set for warning message display.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 8 Technical specifications

851 Titrando ￭￭￭￭￭￭￭￭ 53

8 Technical specifications

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 Generator electrodeOne measuring input (Gen.) for a generator electrode.

Imax 400 mAContinuous current and pulsed

8.1.2 Indicator electrodeOne measuring input (Ind.) for an indicator electrode.

Measuring modeIpol

Determination with adjustable polarization current.

AC 5, 10, 20 und 30 µA

DC –125…+125 µA

8.1.3 TemperatureOne measuring input (Temp.) for temperature sensors, Pt 1000 or NTC.Automatic temperature compensation for NTC sensors R (25 °C) and Bvalue can be configured.

Measuring range

Pt 1000 –150…+250 °C

NTC –5…+250 °C(R (25 °C) = 30'000Ω and B (25/50) = 4100 K)

Resolution

PT 1000 0.1 °C

NTC 0.1 °C

Measuring accu-racy

PT 1000 ± 0.2 °C(Applies for measuring range 20…+150°C; ±1 digit; without sensorerror, under reference conditions)

NTC ±0.6 °C(Applies for measuring range +10…+40°C; ±1 digit; without sensorerror, under reference conditions)

8.2 Mains connection ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

54 ￭￭￭￭￭￭￭￭ 851 Titrando

8.2 Mains connection

Voltage 100…240 V

Frequency 50…60 Hz

Power consump-tion

maximum 45 W

Fuse Electronic overload protection

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 fol-lowed by the user in order to ensure safe operation of the instrument.

8.4 Electromagnetic compatibility (EMC)

Emission 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

Immunity 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

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 8 Technical specifications

851 Titrando ￭￭￭￭￭￭￭￭ 55

8.5 Ambient temperature

Nominal functionrange

+5…+45 °C

Storage –20…+60 °C

Transport –40…+60 °C

8.6 Interfaces

USB connectors

USB ports 2 USB downstream ports (model A sockets), each 500 mA, for con-necting peripheral devices such as printers, keyboards, barcode readersor RS-232/USB boxes (Metrohm order no. 6.2148.020).

Controller connection

Controller port USB upstream port with auxiliary power supply (Mini DIN socket) forconnecting Touch Control or computer for controlling the 851Titrando.

Touch Control With integrated Touch Control cable

Computer With cable 6.2151.000

MSB connectors (Metrohm Serial Bus)

Dosing device

Stirrer Connection for a maximum of 4 stirrers.Stirrer control: manual On/Off switching or coordination with the titra-tion sequence.Rate in 15 stages and shift direction can be selected

Remote Box Connection for a maximum of four remote boxes. Remote boxes canbe used to actuate and monitor external devices.

9.1 Declaration of Conformity ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

56 ￭￭￭￭￭￭￭￭ 851 Titrando

9 Conformity and warranty

9.1 Declaration of Conformity

This is to certify the conformity to the standard specifications for electricalappliances and accessories, as well as to the standard specifications forsecurity 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 PC-Software

This instrument has been built and has undergone final type testingaccording to the standards:

Electromagneticcompatibility

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

Immunity: 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

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 inthe EU directives 2006/95/EC (LVD), 2004/108/EC (EMC). It fulfils the fol-lowing specifications:

EN 61326-1 Electrical equipment for measurement, controland laboratory use – EMC requirements

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 9 Conformity and warranty

851 Titrando ￭￭￭￭￭￭￭￭ 57

EN 61010-1 Safety requirements for electrical equipment formeasurement, control and laboratory use

Manufacturer Metrohm Ltd., CH-9101 Herisau/Switzerland

Metrohm Ltd. is holder of the SQS certificate ISO 9001:2000 Quality man-agement system for development, production and sales of instrumentsand 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 number10872-02, issued by SQS (Swiss Association for Quality and ManagementSystems). Internal and external audits are carried out periodically to assurethat the standards defined by Metrohm’s QM Manual are maintained.

The steps involved in the design, manufacture and servicing of instrumentsare fully documented and the resulting reports are archived for ten years.The development of software for PCs and instruments is also duly docu-mented and the documents and source codes are archived. Both remainthe possession of Metrohm. A non-disclosure agreement may be asked tobe provided by those requiring access to them.

The implementation of the ISO 9001:2000 quality management system isdescribed in Metrohm’s QM Manual, which comprises detailed instruc-tions on the following fields of activity:

Instrument development

The organization of the instrument design, its planning and the intermedi-ate controls are fully documented and traceable. Laboratory testingaccompanies all phases of instrument development.

Software development

Software development occurs in terms of the software life cycle. Tests areperformed to detect programming errors and to assess the program’sfunctionality in a laboratory environment.

9.3 Warranty (guarantee) ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

58 ￭￭￭￭￭￭￭￭ 851 Titrando

Components

All components used in the Metrohm instruments have to satisfy the qual-ity standards that are defined and implemented for our products. Suppli-ers of components are audited by Metrohm as the need arises.

Manufacture

The measures put into practice in the production of our instruments guar-antee a constant quality standard. Production planning and manufacturingprocedures, maintenance of production means and testing of compo-nents, intermediate and finished products are prescribed.

Customer support and service

Customer support involves all phases of instrument acquisition and use bythe customer, i.e. consulting to define the adequate equipment for theanalytical problem at hand, delivery of the equipment, user manuals, train-ing, after-sales service and processing of customer complaints. TheMetrohm service organization is equipped to support customers in imple-menting standards such as GLP, GMP, ISO 900X, in performing Opera-tional Qualification and Performance Verification of the system compo-nents or in carrying out the System Validation for the quantitative determi-nation of a substance in a given matrix.

9.3 Warranty (guarantee)

Metrohm guarantees that the deliveries and services it provides are freefrom material, design or manufacturing errors. The warranty period is 36months from the day of delivery; for day and night operation it is 18months. The warranty remains valid on condition that the service is provi-ded by an authorized Metrohm service organization.

Glass breakage is excluded from the warranty for electrodes and otherglassware. The warranty for the accuracy corresponds to the technicalspecifications given in this manual. For components from third parties thatmake up a considerable part of our instrument, the manufacturer's war-ranty provisions apply. Warranty claims cannot be pursued if the Customerhas not complied with the obligations to make payment on time.

During the warranty period Metrohm undertakes, at its own choice, toeither repair at its own premises, free of charge, any instruments that canbe shown to be faulty or to replace them. Transport costs are to the Cus-tomer's account.

Faults arising from circumstances that are not the responsibility ofMetrohm, such as improper storage or improper use, etc. are expresslyexcluded from the warranty.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 10 Accessories

851 Titrando ￭￭￭￭￭￭￭￭ 59

10 Accessories

10.1 Scope of delivery

Note

Subject to change without notice.

10.1.1 851 Titrando 2.851.0110

Qty. Order no. Description

1 1.851.0010 851 Titrando

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(mm):

10

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


Shaft diameter top (mm): 24

Shaft diameter bottom (mm): 24

Length from standard groundjoint (mm):

85


15

Electrode plug-in head: Metrohm plug-in head G

Indicator electrode type: Cathode = Pt sheet

Indicator electrode type (ref-erence):

Anode = Pt net

10.1 Scope of delivery ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

60 ￭￭￭￭￭￭￭￭ 851 Titrando


Ground joint sleeve: Standard ground joint 29/22

1 6.1403.030 KF adsorber tube for coulometer cell

Height (mm): 93

SGJ size: B-17/19

1 6.1437.000 Ground joint stopper SGJ 14

Material: Glass

Height (mm): 34

SGJ size: B-14/15

1 6.1446.060 Stopper / B-14/15 / M10

Material: PP

Height (mm): 22

SGJ size: B-14/15

2 6.1448.020 Septum / 16 mm / 5 pieces

Set of 5 pieces.

Material: Silicone rubber

Height (mm): 2

Outer diameter (mm): 16

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 10 Accessories

851 Titrando ￭￭￭￭￭￭￭￭ 61


1 6.1464.320 KF titration vessel / 80 - 250 mL / coulomet-ric

Material: Clear glass

Height (mm): 114

Opening ground joint: A-29/22, 2 x A-14/15

Volume (mL): 80 ... 250

1 6.1903.030 Stirring bar / 25 mm

Stirring bar with magnetic core, PTFE covering, length 25 mm

Material: PTFE


Length (mm): 25

1 6.2047.020 Titration vessel holder

Titration vessel holder for coulometric cells.

1 6.2103.130 Adapter red plug 2 mm / 4 mm socket

For connecting plug B (4 mm) to socket 2 mm.


62 ￭￭￭￭￭￭￭￭ 851 Titrando


1 6.2103.140 Adapter black plug 2 mm / socket B 4 mm


1 6.2104.020 Electrode cable / 1 m / F

For connecting electrodes with Metrohm plug-in head G to Metrohminstruments (socket F).

Length (m): 1

1 6.2104.120 Electrode cable / 1 m / H

With plug H. For the connection generator electrode - KF coulome-ter.

Length (m): 1

1 6.2701.040 Screw cap

Of PBTP. With a hole for the 6.1448.020 septum. For the6.5405.000 cell without diaphragm and the 6.1464.32X and6.1465.320 titration vessels.

Material: PBTP

Height (mm): 20


Inner diameter (mm): 18

3 6.2713.000 Sleeve

For the fat-free ground joint connection with the standard groundjoint SGJ 14

Material: PTFE film

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 10 Accessories

851 Titrando ￭￭￭￭￭￭￭￭ 63


1 6.2713.010 Sleeve

Sleeve for the fat-free ground joint connection with the standardground joint SGJ 29

Material: PTFE film

1 6.2713.020 Sleeve


Material: PTFE film

1 6.2730.030 Stopper

Including nipple and E.301.0043 O-ring. For 6.1414.030 titrationvessel lids. For KF instruments, VA stands, VA Computrace and ICDilution.

Length (mm): 38

1 6.2738.000 Funnel

For the KF coulometer

Material: PP




64 ￭￭￭￭￭￭￭￭ 851 Titrando


1 6.2811.000 Molecular sieve

Molecular sieve. Bottle of 250 g. Pore size: 0.3 nm. Without moistureindicator. For Rancimats and Karl Fischer instruments.

2 6.2816.010 Needle

For the 6.2816.000 syringe

Outer diameter (mm): 0.8

Length (mm): 80

2 6.2816.090 Syringe 5 mL

Syringe 5 mL of PP, with Luer connector

Material: PP

1 6.2122.0x0 Mains cable with C13 line socketIEC-60320-C13

Cable plug according to customer requirements.

Switzerland: Type SEV 126.2122.020

Germany, …: Type CEE(7), VII6.2122.040

USA, …: Type NEMA/ASA6.2122.070

1 8.851.8002EN 851 Titrando Manual

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 10 Accessories

851 Titrando ￭￭￭￭￭￭￭￭ 65

10.1.2 851 Titrando 2.851.0010


1 1.851.0010 851 Titrando

1 1.801.0010 801 Stirrer

Magnetic Stirrer without stand. With permanently attached cable forMSB (Metrohm Serial Bus).



Measuring range: –2000 ...2000

Measuring unit: mV




10




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




85


15


Indicator electrode type: Cathode = Pt net


Anode = Pt net

Ground joint sleeve: Standard ground joint 29/22


66 ￭￭￭￭￭￭￭￭ 851 Titrando



For KF coulometers

Height (mm): 93

SGJ size: B-17/19


Material: Glass

Height (mm): 34

SGJ size: B-14/15

1 6.1446.060 Stopper / B-14/15 / M10

Material: PP

Height (mm): 22

SGJ size: B-14/15

2 6.1448.020 Septum / 16 mm / 5 pieces

Set of 5 pieces.


Height (mm): 2


￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 10 Accessories

851 Titrando ￭￭￭￭￭￭￭￭ 67




Height (mm): 114


Volume (mL): 80 ... 250

1 6.1903.030 Stirring bar / 25 mm


Material: PTFE


Length (mm): 25

1 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.

1 6.2013.010 Clamping ring

For support rods with a diameter of 10 mm

Material: Metal

Width (mm): 20

Height (mm): 16


68 ￭￭￭￭￭￭￭￭ 851 Titrando


1 6.2016.030 Support rod / 250 mm

Material: Steel, stainless 18/8


Length (mm): 250





￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 10 Accessories

851 Titrando ￭￭￭￭￭￭￭￭ 69






Length (m): 1



Length (m): 1

1 6.2701.040 Screw cap

Of PBTP. With a hole for the 6.1448.020 septum. For the6.5405.000 cell without diaphragm and the 6.1464.32X and6.1465.320 titration vessels. For 684, 737, 756 KF coulometers

Material: PBTP

Height (mm): 20



3 6.2713.000 Sleeve


Material: PTFE film


70 ￭￭￭￭￭￭￭￭ 851 Titrando


1 6.2713.010 Sleeve


Material: PTFE film

1 6.2713.020 Sleeve


Material: PTFE film

1 6.2730.030 Stopper


Length (mm): 38

1 6.2738.000 Funnel


Material: PP



￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 10 Accessories

851 Titrando ￭￭￭￭￭￭￭￭ 71



Molecular sieve. Bottle of 250 g. Pore size: 0.3 nm. Without moistureindicator. For Rancimats and Karl Fischer instruments

2 6.2816.010 Needle



Length (mm): 80

2 6.2816.090 Syringe 5 mL


Material: PP



Switzerland: Type SEV 126.2122.020





72 ￭￭￭￭￭￭￭￭ 851 Titrando

10.1.3 851 Titrando 2.851.0020


1 1.851.0010 851 Titrando

1 1.801.0010 801 Stirrer

Magnetic Stirrer without stand. With permanently attached cable forMSB (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 canbe added later.



Measuring range: –2000 ... 2000

Measuring unit: mV




10




Pressure load: > 0

1 6.0344.100 Generator electrode with diaphragm

Generator electrode for Karl Fischer titrations, with diaphragm,standard ground joint 29/22





85


15


Indicator electrode type: Cathode = Pt net


Anode = Pt net

SGJ sleeve: Standard ground joint 29/22

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 10 Accessories

851 Titrando ￭￭￭￭￭￭￭￭ 73



For KF coulometers

Height (mm): 93

SGJ size: B-17/19


Material: Glass

Height (mm): 34

SGJ size: B-14/15

1 6.1446.060 Stopper / B-14/15 / M10

Material: PP

Height (mm): 22

SGJ size: B-14/15

2 6.1448.020 Septum / 16 mm / 5 pieces

Set of 5 pieces.


Height (mm): 2



74 ￭￭￭￭￭￭￭￭ 851 Titrando




Height (mm): 114


Volume (mL): 80 ... 250

1 6.1903.030 Stirring bar / 25 mm


Material: PTFE


Length (mm): 25

1 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.

1 6.2013.010 Clamping ring

For support rods with a diameter of 10 mm

Material: Metal

Width (mm): 20

Height (mm): 16

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 10 Accessories

851 Titrando ￭￭￭￭￭￭￭￭ 75


1 6.2016.030 Support rod / 250 mm

Material: Steel, stainless 18/8


Length (mm): 250






76 ￭￭￭￭￭￭￭￭ 851 Titrando






Length (m): 1



Length (m): 1

1 6.2701.040 Screw cap

Of PBTP. With a hole for the 6.1448.020 septum. For the6.5405.000 cell without diaphragm and the 6.1464.32X and6.1465.320 titration vessels.

Material: PBTP

Height (mm): 20



3 6.2713.000 Sleeve


Material: PTFE film

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 10 Accessories

851 Titrando ￭￭￭￭￭￭￭￭ 77


1 6.2713.010 Sleeve


Material: PTFE film

1 6.2713.020 Sleeve


Material: PTFE film

1 6.2730.030 Stopper


Length (mm): 38

1 6.2738.000 Funnel


Material: PP




78 ￭￭￭￭￭￭￭￭ 851 Titrando



Molecular sieve. Bottle of 250 g. Pore size: 0.3 nm. Without moistureindicator. For Rancimats and Karl Fischer instruments

2 6.2816.010 Needle



Length (mm): 80

2 6.2816.090 Syringe 5 mL


Material: PP

1 6.6051.000 Titrando method CF card

Memory card with application methods



Switzerland: Type SEV 12

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 10 Accessories

851 Titrando ￭￭￭￭￭￭￭￭ 79


6.2122.020




10.2 Optionales Zubehör

10.2.1 851 Titrando 2.851.0010, 2.851.0020, 2.851.0110

Order no. Description

2.800.0010 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 Inter-face. Touch-sensitive color display. Simple and intuitive user guidance. Compli-ant with 21 CFR Part 11. Two PCMCIA card slots. Standard dialog languageEnglish; one further language can be retrofitted. Including CompactFlash cardwith adapter, demo version of the PC Control Software.

2.801.0010 801 Stirrer

Magnetic stirrer without stand for use with Titrino plus, Titrandos, Sample Pro-cessors, 805 Dosimats and 780/781 pH Meters. With permanently attachedcable for MSB (Metrohm Serial Bus).

10.2 Optionales Zubehör ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

80 ￭￭￭￭￭￭￭￭ 851 Titrando


2.803.0010 803 Ti Stand

Compact titration stand with magnetic stirrer and built-in pump for solvent addi-tion and aspiration of the titration vessel contents. Suitable for Karl Fischer titra-tions with Titrandos. MSB connection. Including comprehensive accessories, sol-vent bottle and waste bottle.

Dimensions in mm (W/H/D): 106/ 101/ 220

Dimensions remark: Height with support rod: 412 mm

2.860.0010 860 KF Thermoprep

The 860 KF Thermoprep is designed for the thermal sample preparation in KarlFischer titration. A lot of substances cannot be analyzed by direct Karl Fischertitration as they are not soluble, react with the Karl Fischer reagent or releasethe water only very slowly or not until heated to high temperatures. Usingtightly sealed sample vials the sample is inserted in the oven. Subsequently thesamples 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 KarlFischer titration. The oven method is suitable for samples that only release theirmoisture at higher temperature, for hardly soluble samples or samples thatundergo 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 controlledvia remote lines. With permanently attached cable.

6.2148.020 RS 232/USB Box

Extends the Titrandos, USB Sample Processors, Dosing Interface, Titrosampler bytwo RS 232 interfaces for the connection of e.g. balance, PC, LIMS. Requires6.2151.030 cable.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 10 Accessories

851 Titrando ￭￭￭￭￭￭￭￭ 81


6.3032.120 Dosing Unit 2 mL

Dosing unit with integrated data chip with 2 mL glass cylinder and light protec-tion, mountable on reagent bottle with ISO/DIN GL45 glass thread. FEP tubingconnection, antidiffusion buret tip.

Volume (mL): 2


Dosing unit with integrated data chip with 5 mL glass cylinder and light protec-tion, mountable on reagent bottle with ISO/DIN GL45 thread. FEP tubing con-nection, antidiffusion buret tip.

Volume (mL): 5



Volume (mL): 10



Volume (mL): 20



Volume (mL): 50

10.2 Optionales Zubehör ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

82 ￭￭￭￭￭￭￭￭ 851 Titrando


6.6050.500 Titrando PC Control-SW 6.0

PC software for controlling Titrandos, USB Sample Processors, 846 Dosing Inter-face, 847 USB Lab Link. Simple and intuitive user guidance. Method and datacompatible with Touch Control. With freely progammable favorites for fastmethod access. Compliant with 21 CFR Part 11. Standard dialog languagesEnglish and German; one further language can be retrofitted. Including hard-ware dongle. The 6.2151.000 Cable is required for connecting the Titrando to aPC.

6.6056.211 Tiamo 2.x Light CD: 1 Lizenz

6.6056.212 Tiamo 2.x Full CD: 1 Lizenz

6.6056.213 Tiamo 2.x Multi CD:3 Lizenzen

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Index

851 Titrando ￭￭￭￭￭￭￭￭ 83

Index

Numbers/Symbols685 Dosimat ............................ 14700 Dosino .............................. 14800 Dosino .............................. 14801 Stirrer ................................ 15803 Ti Stand ............................. 15804 Ti Stand ............................. 15805 Dosimat ............................ 14

BBalance .................................... 18Bluetooth adapter

Connecting ........................ 22

CComputer

Connecting ........................ 11Connecting

Balance .............................. 18Barcode reader ................... 20Bluetooth adapter .............. 22Computer ........................... 11Dosing devices ................... 14MSB devices ....................... 13PC keyboard ....................... 20Printer ................................ 17Remote box ........................ 16Stirrer or titration stand ...... 15Touch Control ...................... 9USB hub ............................. 22

Connecting a barcode reader . . . 20Connector

Double Pt electrode .............. 8Generator electrode ............. 8MSB ..................................... 2Temperature sensor .............. 8USB ...................................... 2

ControllerConnector ............................ 8

Controller cable 6.2151.000 .... 11Coulometric KF titration

Certified water standards .... 37Liquid samples .................... 39Practical recommendations . 37Principle ............................. 36Sample size ........................ 39Solid samples ..................... 40Working conditions ............ 41

DDevice software

Update ................................. 2Dosing command ....................... 3

ADD ..................................... 3EMPTY ................................. 3LQH ..................................... 3PREP ..................................... 3

Dosing devicesConnecting ........................ 14

DriverInstall ................................. 11

EElectrostatic charge .................... 5

GGLP .......................................... 45Guarantee ................................ 58

IInstallation

Driver ................................. 11Instrument description ................ 2Instrument type .......................... 8

KKeyboard ................................. 20

LLED

On ..................................... 47

MMagnetic stirrer

Connecting ........................ 15Mains connection ....................... 8Mains voltage ............................. 5Maintenance ............................ 43Measuring interface ................ 2, 8Measuring mode ........................ 3

MEAS ................................... 3MEAS T ................................ 3

Metrohm Serial Bus MSB, see also"MSB" ...................................... 13MSB

Connecting devices ............ 13Connector ............................ 8

MSB.Connector .......................... 2

OOverview of the instrument ........ 7

PPC keyboard ............................. 20Pins .......................................... 49Printer ...................................... 17

QQuality Management ................ 45

RRemote

Input .................................. 50Interface ............................. 49Output ............................... 50

Remote boxConnecting ........................ 16Pin assignment ................... 49

SSafety instructions ...................... 4Serial number ............................. 8Service ....................................... 4Service Agreement ................... 45Stirrer

Connecting ........................ 15System test ............................... 10

TTitrando system .......................... 1Titration mode ........................... 3

BRC ...................................... 3KFC ...................................... 3

Titration stand .......................... 15Connecting ........................ 15

Touch ControlConnecting .......................... 9

UUpdate

Device software .................... 2USB

Connector ............................ 8USB connector ........................... 2USB hub

Connecting ........................ 22

VValidation ................................. 45

Index ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

84 ￭￭￭￭￭￭￭￭ 851 Titrando

WWarranty .................................. 58

Windows .................................. 12

622555_88518002EN_Manual_851_Titrando_

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