Metrohm 870KF User Manual

870 KF Titrino plus
Manual
8.870.8005EN
Metrohm AG CH-9100 Herisau Switzerland Phone +41 71 353 85 85 Fax +41 71 353 89 01 info@metrohm.com www.metrohm.com
870 KF Titrino plus
8.870.8005EN
Manual
04.2013 jb/ebe
Teachware Metrohm AG CH-9100 Herisau teachware@metrohm.com
This documentation is protected by copyright. All rights reserved.
Although all the information given in this documentation has been checked with great care, errors cannot be entirely excluded. Should you notice any mistakes please send us your comments using the address given above.
Documentation in additional languages can be found on
http://documents.metrohm.com.
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Table of contents

1 Introduction 1
1.1 Instrument description ......................................................... 1
1.1.1 Titration and measuring modes ................................................ 1
1.1.2 Connectors .............................................................................. 1
1.1.3 Intended use ........................................................................... 1
1.2 About the documentation ................................................... 2
1.2.1 Symbols and conventions ........................................................ 2
1.3 Safety instructions ................................................................ 3
1.3.1 General notes on safety ........................................................... 3
1.3.2 Electrical safety ........................................................................ 3
1.3.3 Tubing and capillary connections ............................................. 4
1.3.4 Flammable solvents and chemicals ........................................... 4
1.3.5 Recycling and disposal ............................................................. 4
2 Overview of the instrument 6
Table of contents
3 Water determination according to Karl Fischer (KFT) 8
4 Installation 9
4.1 Setting up the instrument .................................................... 9
4.1.1 Packaging ................................................................................ 9
4.1.2 Checks .................................................................................... 9
4.1.3 Location .................................................................................. 9
4.2 Connecting a sensor ............................................................. 9
4.3 Connecting a stirrer ............................................................ 10
4.4 Connecting a balance ......................................................... 11
4.5 Connecting a keyboard, printer and other USB devi-
ces ........................................................................................ 11
4.6 Connecting instruments to the remote connector .......... 14
4.7 Attaching the exchange unit ............................................. 15
5 Operation 16
5.1 Switching the instrument on and off ............................... 16
5.2 Fundamentals of operation ............................................... 17
5.2.1 The keypad ............................................................................ 17
5.2.2 Structure of the dialog windows ............................................ 18
5.2.3 Navigating in the dialog ......................................................... 18
5.2.4 Entering text and numbers ..................................................... 19
5.2.5 Selecting from a selection list ................................................. 20
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III
Table of contents
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5.3 Methods .............................................................................. 20
5.3.1 Method templates ................................................................. 20
5.3.2 Loading a method ................................................................. 21
5.3.3 Saving a method ................................................................... 21
5.3.4 Exporting a method ............................................................... 21
5.4 Sample data ........................................................................ 22
5.4.1 Entering sample data in the main dialog ................................ 22
5.4.2 Requesting sample data at the start of the determination ...... 23
5.5 Carrying out a determination ............................................ 24
5.6 Live modifications .............................................................. 27
5.6.1 Editing the sample data of the running determination ............ 27
5.6.2 Editing the live parameters ..................................................... 28
5.7 Results ................................................................................. 29
5.8 Statistics .............................................................................. 30
5.9 Printing a report manually ................................................. 31
5.10 Manual control ................................................................... 33
5.10.1 Dosing ................................................................................... 33
5.10.2 Stirring .................................................................................. 37
6 System settings 39
6.1 Basic settings ...................................................................... 39
6.2 Managing solutions ............................................................ 42
6.2.1 General ................................................................................. 42
6.2.2 Editing the solution data ........................................................ 43
6.3 File management ................................................................ 44
6.4 Configuring external devices ............................................. 46
6.5 Instrument diagnosis .......................................................... 49
6.5.1 Loading program versions and language files ......................... 49
6.5.2 Diagnosis functions ............................................................... 50
7 Parameters 51
7.1 Karl Fischer Titrations (KFT) .............................................. 51
7.1.1 Conditioning ......................................................................... 51
7.1.2 Start conditions ..................................................................... 52
7.1.3 Control parameters ................................................................ 53
7.1.4 Titration parameters .............................................................. 56
7.1.5 Stop conditions ..................................................................... 58
7.1.6 Calculations - Methods "Blank Ipol/Upol" ............................... 59
7.1.7 Calculations - Methods "Titer Ipol/Upol" ................................ 60
7.1.8 Calculations - Methods "KFT Ipol/Upol", "KFT Ipol/Upol–
Blank" ................................................................................... 61
7.1.9 Statistics ................................................................................ 63
7.1.10 Reports .................................................................................. 63
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IV
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8 Operation and maintenance 66
9 Troubleshooting 67
10 Appendix 70
Table of contents
8.1 Quality Management and qualification with Metrohm .. 66
9.1 Karl Fischer titration .......................................................... 67
9.2 Miscellaneous ..................................................................... 68
10.1 Exchange unit ..................................................................... 70
10.1.1 Maximum dosing and filling rate ............................................ 70
10.1.2 Parameters for the preparing (PREP) ....................................... 70
10.2 Stirring rate ......................................................................... 71
10.3 Balance ................................................................................ 71
10.4 USB devices ......................................................................... 72
10.4.1 6.2147.000 numerical USB keypad ........................................ 72
10.4.2 Key assignment of a USB keyboard ........................................ 73
10.4.3 PC mouse .............................................................................. 73
10.4.4 Printer ................................................................................... 74
10.5 System initialization ........................................................... 74
10.6 Remote interface ................................................................ 76
10.6.1 Pin assignment of the remote interface .................................. 76
10.6.2 Status diagram of the remote interface .................................. 77
10.7 Remote control via an RS-232 connection ....................... 77
10.7.1 Commands and variables ....................................................... 78
10.8 Arithmetic algorithms in the 870 KF Titrino plus ............ 80
11 Technical specifications 83
11.1 Measuring inputs ................................................................ 83
11.1.1 Polarizer ................................................................................ 83
11.2 Dosing drive ........................................................................ 84
11.3 Interfaces ............................................................................. 84
11.4 Mains connection ............................................................... 84
11.5 Safety specifications ........................................................... 84
11.6 Electromagnetic compatibility (EMC) ................................ 85
11.7 Ambient temperature ......................................................... 85
11.8 Reference conditions .......................................................... 86
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11.9 Dimensions .......................................................................... 86
12 Warranty (guarantee) 87
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Table of contents
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13 Accessories 89
13.1 Scope of delivery ................................................................ 89
13.2 Optional accessories ........................................................... 94
Index 97
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VI
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Table of figures

Figure 1 Front 870 KF Titrino plus ................................................................... 6
Figure 2 Rear 870 KF Titrino plus .................................................................... 7
Figure 3 Reagent dosing for KFT ..................................................................... 8
Figure 4 Connecting a polarizable electrode .................................................... 9
Figure 5 Connecting a stirrer ......................................................................... 10
Figure 6 Connecting a balance ...................................................................... 11
Figure 7 Connecting USB devices .................................................................. 12
Figure 8 Connecting the USB stick ................................................................ 13
Figure 9 Connecting the 6.2147.000 USB keyboard with USB stick and
printer ............................................................................................. 13
Figure 10 Connecting the USB hub with USB stick, printer and the 6.2148.030
RS-232/USB Box (for connecting balances). ...................................... 14
Figure 11 Connecting a remote cable ............................................................. 14
Figure 12 Attaching the exchange unit ........................................................... 15
Figure 13 Keypad 870 KF Titrino plus .............................................................. 17
Figure 14 Directory structure on the USB flash drive ........................................ 45
Figure 15 Rotational speed depending on stirring rate .................................... 71
Figure 16 Pin assignment of remote socket and remote plug .......................... 76
Figure 17 Remote status diagram .................................................................... 77
Figure 18 Connecting the RS-232/USB Box to the PC ...................................... 78
Table of figures
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VII
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1 Introduction

1.1 Instrument description

The 870 KF Titrino plus is an instrument used for volumetric water content determination according to Karl Fischer. There are method templates available which are already configured except for a few parameters. If parameters are changed, then these will be saved automatically. The methods can be exported to a connected USB flash drive. This function makes it possible for you to copy methods quickly and easily from one instrument to another.

1.1.1 Titration and measuring modes

The following titration and measuring modes are supported:
KFT
Volumetric water content determination according to Karl Fischer.
Measuring modes:
Ipol (voltametric measurement with selectable polarization cur-
rent)
Upol (amperometric measurement with selectable polarization
voltage)

1 Introduction

1.1.2 Connectors

The instrument is equipped with the following connectors:
MSB connector (Metrohm Serial Bus)
USB (OTG) connector
Electrode connector
Remote connector

1.1.3 Intended use

The 870 KF Titrino plus is designed for usage as a titrator in analytical lab­oratories. Its main application field is volumetric titration.
This instrument is suitable for processing chemicals and flammable sam­ples. The usage of the 870 KF Titrino plus therefore requires that the user have basic knowledge and experience in the handling of toxic and caustic substances. Knowledge with respect to the application of the fire preven­tion measures prescribed for laboratories is also mandatory.
For connecting a stirrer.
The 6.2151.100 adapter can be used to connect, for example, a
printer, a USB flash drive or a USB keyboard.
For connecting polarizable electrodes.
For connecting instruments with a remote interface.
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1.2 About the documentation

1.2 About the documentation
CAUTION
Please read through this documentation carefully before putting the instrument into operation. The documentation contains information and warnings which the user must follow in order to ensure safe opera­tion of the instrument.

1.2.1 Symbols and conventions

The following symbols and formatting may appear in this documentation:
Cross-reference to figure legend
The first number refers to the figure number, the sec­ond to the instrument part in the figure.
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Instruction step
Carry out these steps in the sequence shown.
Method Dialog text, parameter in the software
File New Menu or menu item
[Next] Button or key
WARNING
This symbol draws attention to a possible life-threat­ening hazard or risk of injury.
WARNING
This symbol draws attention to a possible hazard due to electrical current.
WARNING
This symbol draws attention to a possible hazard due to heat or hot instrument parts.
WARNING
This symbol draws attention to a possible biological hazard.
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CAUTION
This symbol draws attention to possible damage to instruments or instrument parts.
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1.3 Safety instructions

1.3.1 General notes on safety

WARNING
This instrument may only be operated in accordance with the specifica­tions in this documentation.
This instrument has left the factory in a flawless state in terms of technical safety. To maintain this state and ensure non-hazardous operation of the instrument, the following instructions must be observed carefully.

1.3.2 Electrical safety

The electrical safety when working with the instrument is ensured as part of the international standard IEC 61010.
1 Introduction
NOTE
This symbol highlights additional information and tips.
WARNING
Only personnel qualified by Metrohm are authorized to carry out service work on electronic components.
WARNING
Never open the housing of the instrument. The instrument could be damaged by this. There is also a risk of serious injury if live components are touched.
There are no parts inside the housing which can be serviced or replaced by the user.
Mains voltage
WARNING
An incorrect mains voltage can damage the instrument.
870 KF Titrino plus
Only operate this instrument with a mains voltage specified for it (see rear panel of the instrument).
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1.3 Safety instructions
Protection against electrostatic charges
WARNING
Electronic components are sensitive to electrostatic charges and can be destroyed by discharges.
Do not fail to pull the mains cable out of the mains connection socket before you set up or disconnect electrical plug connections at the rear of the instrument.

1.3.3 Tubing and capillary connections

CAUTION
Leaks in tubing and capillary connections are a safety risk. Tighten all connections well by hand. Avoid applying excessive force to tubing connections. Damaged tubing ends lead to leakage. Appropriate tools can be used to loosen connections.
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Check the connections regularly for leakage. If the instrument is used mainly in unattended operation, then weekly inspections are manda­tory.

1.3.4 Flammable solvents and chemicals

WARNING
All relevant safety measures are to be observed when working with flammable solvents and chemicals.
Set up the instrument in a well-ventilated location (e.g. fume cup-
board).
Keep all sources of flame far from the workplace. Clean up spilled liquids and solids immediately. Follow the safety instructions of the chemical manufacturer.

1.3.5 Recycling and disposal

This product is covered by European Directive 2002/96/EC, WEEE – Waste from Electrical and Electronic Equipment.
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4
The correct disposal of your old equipment will help to prevent negative effects on the environment and public health.
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1 Introduction
More details about the disposal of your old equipment can be obtained from your local authorities, from waste disposal companies or from your local dealer.
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2 Overview of the instrument

2
5
4
3
1
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Figure 1 Front 870 KF Titrino plus
Piston rod
1
Of the dosing drive.
Coupling
3
For switching the flat stopcock.
Keypad
5
Contact pins
2
For the data chip.
Display
4
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1
2
5
4
3
6
2 Overview of the instrument
Figure 2 Rear 870 KF Titrino plus
Type plate
1
Contains specifications concerning mains voltage and serial number.
USB (OTG) connector
3
For connecting printers, USB sticks, USB hubs, etc.
Remote connector
5
For connecting instruments with a remote interface. D-Sub, 9-pin.
Mains connection socket
2
MSB connector
4
Metrohm Serial Bus.
For connecting a stirrer. Mini DIN, 9-pin.
Electrode connector (Pol.)
6
For connecting polarizable electrodes, e.g. double Pt electrodes. Socket F.
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EP
KFT Ipol
KFT Upol
EP
V/mL
Continuous dosing
Initial dosing
V/mL
V/mL
U/mV
t/s
I/µA
Control range
Control range
3 Water determination according to Karl Fischer
(KFT)
Karl Fischer Titration is a method for volumetric water determination. Con­ditioning is carried out automatically both before and after the actual titra­tion. The reagent dosing is controlled in such a way that a predefined endpoint is reached as quickly and as accurately as possible. The volume steps and the rate of reagent dosing are regulated by the difference between the current measured value and the predefined endpoint. This means that titration is performed more slowly in the control range and that smaller volumes are added. The titration is stopped at the endpoint either drift-controlled or after a waiting time. The volume dosed until the endpoint is used to calculate the water content of the sample.
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Figure 3
Reagent dosing for KFT
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4 Installation

4.1 Setting up the instrument

4.1.1 Packaging

The instrument is supplied in highly protective special packaging together with the separately packed accessories. Keep this packaging, as only this ensures safe transportation of the instrument.

4.1.2 Checks

Immediately after receipt, check whether the shipment has arrived com­plete and without damage by comparing it with the delivery note.

4.1.3 Location

The instrument has been developed for operation indoors and may not be used in explosive environments.

4 Installation

Place the instrument in a location of the laboratory which is suitable for operation, free of vibrations, protected from corrosive atmosphere, and contamination by chemicals.
The instrument should be protected against excessive temperature fluctu­ations and direct sunlight.

4.2 Connecting a sensor

Connecting a polarizable electrode
Figure 4
Connecting a polarizable electrode
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4.3 Connecting a stirrer

NOTE
The electrode cable is protected against accidental disconnection of the cable by means of a pull-out protection feature. If you wish to remove the plug, then you must first retract the outer plug sleeve.
4.3 Connecting a stirrer
You can connect the following stirrers:
801 Stirrer 803 Ti Stand 804 Ti Stand (requires rod stirrer)
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Figure 5
Connecting a stirrer
CAUTION
Make sure that the flat side of the plug matches the marking on the socket.
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4.4 Connecting a balance

Balances are equipped with a serial RS-232 interface as a rule. To connect a balance, you require a 6.2148.030 RS-232/USB Box.
Figure 6 Connecting a balance
When a 6.2151.020 USB cable is used, then the 6.2148.030 RS-232/USB Box can be connected to the 870 KF Titrino plus by means of a USB hub or a 6.2151.100 adapter (see Chapter 4.5, page 11).
4 Installation
Connect the 9-pin plug of the respective balance connecting cable to the RS 232/1 connector. Consult the user manual of the balance in order to select the correct connecting cable.
The parameters for the RS-232 interface on the instrument must match those on the balance (see "Editing the COM1 settings", page 47). Addi­tionally consult the user manual of the balance.
4.5 Connecting a keyboard, printer and other USB devi­ces
The 870 KF Titrino plus has a USB (OTG) connector. Use the provided
6.2151.100 adapter USB MINI (OTG) - USB A for connecting USB devices as e.g. printers, keyboards or USB sticks, see the following figure.
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4.5 Connecting a keyboard, printer and other USB devices
6.2151.100
Figure 7 Connecting USB devices
CAUTION
Switch the instrument off before connecting or disconnecting a USB device or a USB stick.
The 870 KF Titrino plus can only recognize the device immediately after switching on.
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The following devices can be operated directly on the USB connector with the 6.2151.100 adapter:
USB sticks (for the backup or storing of methods) 6.2147.000 numerical USB keypad 6.2148.030 RS-232/USB Box (for connecting balances or for the
RS-232 remote control)
USB hub (with or without an own power supply)
The 6.2147.000 numerical USB keypad serves for comfortable numer­ical input and for navigating in the dialog. In addition, it provides two USB connectors. Connect additional USB devices to the keypad.
NOTE
Most of the USB devices need a so-called hub in order to work cor­rectly.
A USB hub is a distributor to which several USB devices can be connec­ted. USB hubs are available in specialty stores in a number of different models.
The USB (OTG) connector of the 870 KF Titrino plus has no such hub. The 6.2147.000 numerical USB keypad has a USB hub and two USB connectors.
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USB MINI (OTG)-USB
USB stick
6.2151.100
USB MINI (OTG)-USB
USB stick
Keypad
6.2147.000
6.2151.100
Printer
4 Installation
The following devices can only be connected to a 6.2147.000 numerical keypad or to a USB hub:
Printer (with USB connector, use the 6.2151.020 connecting cable) Barcode reader (with USB cable) Mouse (PC mouse with USB cable, for navigating in the dialog)
The following devices can only be connected to a USB hub:
PC keyboard (with USB cable, for the comfortable input of letters and
numbers)
Keypad with numerical keypad (with USB cable)
If you wish to connect several different instruments without own power supply, then you must possibly use a USB hub with own power
supply (self powered). The USB (OTG) connector of the 870 KF Titrino plus is not designed for supplying power to several devices with elevated elec­tricity requirements.
Also observe the instructions in chapter 10.4, page 72.
Examples:
Figure 8
Connecting the USB stick
Figure 9 Connecting the 6.2147.000 USB keyboard with USB stick and
printer
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4.6 Connecting instruments to the remote connector

USB MINI (OTG)-USB
USB stick
USB-Hub
RS-232/USB Box
6.2148.030
6.2151.100
Printer
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Figure 10 Connecting the USB hub with USB stick, printer and the
6.2148.030 RS-232/USB Box (for connecting balances).
4.6 Connecting instruments to the remote connector
The 870 KF Titrino plus can be integrated in an automation system with the aid of a remote cable.
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Figure 11
Connecting a remote cable
A variety of different connecting cables are available for connecting Metrohm instruments (e.g. sample changers) (see Optional Accessories chapter).
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4.7 Attaching the exchange unit

4 Installation
Figure 12 Attaching the exchange unit
To attach the exchange unit, proceed as follows:
Slide the exchange unit from the front onto the 870 KF Titrino plus
1
and push all the way to the rear.
It must snap in audibly.
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5.1 Switching the instrument on and off

5 Operation

5.1 Switching the instrument on and off
Switching on the instrument
Proceed as follows:
Press the red [STOP] key.
1
The instrument is initialized and a system test performed. This process takes some time.
If a buret unit has been attached, then a request appears to carry
out the PREP function:
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All tubings and the cylinder are rinsed with the PREP (Preparing) function. The preparing of the buret unit is described in chapter "Preparing the buret unit (PREP)", page 33.
Confirm the message with [OK].
The display of this message can be deactivated in the system set­tings (see "PREP warning", page 41).
The main dialog is displayed:
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Switching off the instrument
The instrument is switched off with the [STOP] key. The fact that the key needs to be pressed down for an extended time prevents accidental switch off.
Proceed as follows:
Keep the red [STOP] key pressed down for at least 3 s.
1
A progress bar is displayed. If the key is released during this time, then the instrument will not be switched off.

5.2 Fundamentals of operation

5.2.1 The keypad

5 Operation
Figure 13
Keypad 870 KF Titrino plus
BACK Apply the input and exit the dialog.
Move the selection bar either up or down by one
line at a time. Select the character to be entered in the text editor.
Select the character to be entered in the text and
number editor. Select the individual functions in the function bar.
OK Confirm the selection.
STOP Stop an ongoing method run or a manual func-
tion. Switch the instrument on or off.
START Start a method run or a manual function.
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5.2 Fundamentals of operation

5.2.2 Structure of the dialog windows

The current dialog title is displayed on the left-hand side of the title bar. The current status of the system is displayed in the upper right-hand cor­ner:
ready The instrument is in normal status.
cond.busy The working medium is being conditioned.
cond.ok The working medium is conditioned.
busy A method has been started.
Some dialogs have a so-called function bar on the bottom line. The func­tions contained therein can be selected with the arrow keys [] or [] and executed with [OK].
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5.2.3 Navigating in the dialog

The selection bar is displayed in inverted style. Use the arrow keys [] and [] to move the selection bar upward or downward one line at a time. If
a dialog text is marked with "", then additional settings are available in a subordinate dialog. Use [OK] to access this dialog.
Example: System settings
Use the [BACK] key to return to the next higher level.
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5.2.4 Entering text and numbers

In the editing dialog for text input or numerical input, select the individual characters with the arrow keys. Use [OK] to apply the character in the input field. The following functions are available:
5 Operation
Editing function
Description
Accept The modification is applied and the editing dialog
is exited.
Cancel The editing dialog is exited without applying the
modification.
Clear The content of the input field is deleted com-
pletely.
The character left of the cursor is deleted (back­space).
Text editor only
The cursor within the input field is shifted to the left by one character each time that [OK] is pressed.
Text editor only
The cursor within the input field is shifted to the right by one character each time that [OK] is pressed.
870 KF Titrino plus
[BACK] The modification is applied and the editing dialog
is exited.
The [BACK] key has the same function as Accept.
A commercially available USB keyboard can be connected to make it eas­ier to enter text and numbers. The assignment of the keys on the PC key­board is described in chapter 10.4.2, page 73.
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5.3 Methods

5.2.5 Selecting from a selection list

In a selection list, select the individual entries with the arrow keys [] and []. Accept the selection with [OK] or [BACK].
5.3 Methods

5.3.1 Method templates

The 870 KF Titrino plus contains method templates which are already con­figured except for a few parameters.
The following method templates can be selected:
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KFT Ipol Method with adjustable polarization current.
The blank value is not taken into account for the calculation.
Titer Ipol Titer determination with adjustable polarization
current.
Blank Ipol Blank value determination with adjustable polari-
zation current.
KFT Ipol–Blank Method with adjustable polarization current.
The blank value is taken into account for the cal­culation.
KFT Upol Method with adjustable polarization voltage.
The blank value is not taken into account for the calculation.
Titer Upol Titer determination with adjustable polarization
voltage.
Blank Upol Blank value determination with adjustable polari-
zation voltage.
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KFT Upol–Blank Method with adjustable polarization voltage.
The blank value is taken into account for the cal­culation.
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5.3.2 Loading a method

To load a method, proceed as follows:
1
Open the method table
In the main dialog, select Method and press [OK].
The method table with the stored templates opens:
2
Select a method
Select the desired method.
3
Load the method
In the function bar, select Load and press [OK].
5 Operation
The method is now loaded and is displayed in the main dialog under Method.

5.3.3 Saving a method

If the method parameters are changed, then these will be saved automati­cally. It is not possible to save a method under a different name.

5.3.4 Exporting a method

Methods can be exported to a connected USB stick.
This function is possible only if a USB stick is connected as an external storage medium.
To export a method, proceed as follows:
1
Open the method table
In the main dialog, select Method and press [OK].
NOTE
870 KF Titrino plus
The method table with the stored templates opens:
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5.4 Sample data

2
Select a method
Select the desired method.
3
Export the method
In the function bar, select Export and press [OK].
The method is exported. The directory structure on the USB stick is listed in chapter 6.3, page 44.
5.4 Sample data
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You can enter the sample data (identification, sample size, etc.) in a vari­ety of ways:
Directly in the main dialog. Automatic request immediately after the start of the determination (see
Chapter 5.4.2, page 23).
You can also send the sample size and the unit from a connected balance in any case. With some balances, the sample identification and method can be also sent (see Chapter 10.3, page 71).

5.4.1 Entering sample data in the main dialog

For a sample, you can enter the sample data directly in the main dialog, even while the determination is running (see Chapter 5.6, page 27).
ID1
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22
Sample identification.
Entry max. 10 characters Default value empty
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ID2
Sample size
Unit
5 Operation
Sample identification.
Entry max. 10 characters Default value empty
Sample size.
Input range –999999999 - 9999999999 Default value 1.0
Unit of the sample size.
Selection g | mg | µg | mL | µL | pieces | User-defined Default value g
User-defined
A user-defined unit can be created. This will be added to the selection list. The previous entry will be overwritten as soon as the new unit has been defined.

5.4.2 Requesting sample data at the start of the determination

The sample data can be requested immediately after the start of the deter­mination in order to ensure that the sample data entry is not forgotten. This automatic request is indispensable when you reweigh your samples.
The corresponding parameters must be activated under Start conditions for this purpose. If the parameter Hold at request is activated, then the run will be paused and must be continued with [START] after the input of the sample data. If Hold at request is deactivated, then the titration will be started in the background. This dialog will be displayed until the entering of the sample data is confirmed with [START], even if the the titration is already completed. This ensures that the sample data is avail­able for calculations.
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5.5 Carrying out a determination

5.5 Carrying out a determination
The sample size can be entered in the following ways when a determina­tion is carried out:
Enter manually on the instrument. Send automatically from a connected balance. For this purpose, check
the manual for the balance.
Proceed as follows to carry out a determination:
1
Loading the method
See Chapter "Loading a method", Page 21.
2
Starting conditioning
Press [START].
Conditioning starts. Conditioning not OK is displayed until the endpoint is reached. The working medium is titrated to the endpoint. This is indicated by Conditioning OK. The status is kept stable.
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The stirring rate can be modified with the Stirrer function. The fol­lowing dialog is opened by pressing [OK]:
The stirring rate can be reduced with Stir- and increased with Stir+. Off switches the stirrer off. On is now displayed instead. This can be used to switch the stirrer back on. This dialog is exited with [BACK].
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3
Adding sample
NOTE
Calculate the amount of the sample in such a way that a titrant consumption of 10…90% of the cylinder volume will result.
If Conditioning OK is displayed, press [START].
Conditioning is stopped. The request for adding the sample will be displayed for 8 s. The sample must be added during this time.
5 Operation
Add the sample.
Afterward, the request for the sample size appears:
4
Entering the sample size
Press [OK].
The editing dialog opens.
Enter the sample size and apply with Accept or [BACK].
5
Starting the titration
Press [START].
The titration starts and the curve is displayed:
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5.5 Carrying out a determination
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The axes are scaled automatically.
The stirring rate can be modified during titration with the Stirrer function. The following dialog is opened by pressing [OK]:
The stirring rate can be reduced with Stir- and increased with Stir+. Off switches the stirrer off. On is now displayed instead. This can be used to switch the stirrer back on. This dialog is exited with [BACK].
After the completion of the titration, the results dialog is displayed. Conditioning is restarted automatically.
6
Canceling the conditioning
Press [STOP].
Conditioning is canceled and the dosing cylinder is filled.
Canceling a determination manually
A determination can be canceled at any time with the [STOP] key.
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5.6 Live modifications

5.6.1 Editing the sample data of the running determination

The sample data can be entered or modified in the main dialog while a determination is running. In calculations always the sample data entered at the end of the titration in the main dialog is used.
Proceed as follows to edit the sample data:
1
Displaying the main dialog
Press [BACK].
The main dialog is displayed. The determination continues to run in the background.
2
Editing the sample data
Edit the sample data and apply with Accept or [BACK].
3
Displaying the live dialog
Press [BACK].
5 Operation
or
Select Menu and press [OK].
Select the menu item Live dialog and press [OK].
The live dialog is displayed once again.
NOTE
If the determination is finished while an editing dialog is opened (e.g. of the sample size), then this will be closed automatically and the results dialog will be displayed. The value entered must be entered once more and the determination must be recalculated.
Make sure that the editing dialogs are closed before the determination is finished.
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5.6 Live modifications

5.6.2 Editing the live parameters

Certain method parameters can be edited while a determination is being carried out. The only parameters that can be modified are those that can be selected. Nevertheless, all of the parameters are visible. The modified parameters are taken into account at once. If you modify, for instance, the start conditions after the start volume has been dosed, then these modifications will not be taken into account until the next determination.
Proceed as follows to edit the parameters:
1
Displaying the main dialog
Press [BACK].
The main dialog is displayed. The determination continues to run in the background.
2
Opening the main menu
Select Menu and press [OK].
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3
Editing the method parameters
Select the menu item Parameters and press [OK]. Change the desired parameters accordingly.
4
Displaying the live dialog
Select the menu item Live dialog in the main menu and press
[OK].
or
Press [BACK] in the main dialog.
The live dialog is displayed once again.
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5.7 Results

Curve
Recalculate
5 Operation
Menu Results
After the completion of the titration, the results dialog is displayed:
The calculated result and the endpoint volume are shown in the overview.
Display the curve of the current determination.
Recalculate the current determination. The procedure will be executed immediately.
Statistics
Display the statistical overview of a determination series (see Chapter 5.8, page 30).
Displaying the curve
The curve of the current determination can be displayed with the Curve function.
The arrow keys [] and [] can be used to move to the individual measur­ing points. A cross hair is used to show the current position on the curve. The data (volume, measured value, time, etc.) for the respective measur­ing point is indicated on the right-hand side.
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5.8 Statistics

Recalculating
All of the results are recalculated with the Recalculate function. This is necessary if, for example, the calculation, the titer or the sample size has been modified.
5.8 Statistics
Menu Results Statistics
The statistical overview of a determination series can be displayed in the Results dialog with the Statistics function.
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NOTE
Recalculation cannot be undone.
NOTE
Details
Reset
This function is visible only if statistics has been activated.
The mean value (Mean), the absolute and the relative standard deviation (s abs and s rel) are displayed in the overview. For the mean value, the number of individual results from which it has been calculated is displayed in parentheses. In this example, it is 3. The Statistics line shows how many determinations have already been carried out and how many deter­minations are to be carried out in total. All three determinations were car­ried out in this example.
Display additional data.
Delete all statistics data.
Increase
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30
Add a further determination to the determination series.
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On/Off
5 Operation
Displaying statistical details
Additional data from the determination series can be displayed with the Details function.
The result and the sample size of each determination are shown.
Remove the selected determination from the statistics. The line will then be marked with an asterisk (*), the statistics will be recalculated automati­cally.
Deleting statistical data
All statistical data is deleted with the Reset function. The statistics data is deleted automatically in the following cases:
When all of the determinations of the determination series have been
carried out and a new determination has been started afterwards.
When a new method is loaded.
Adding a determination to a determination series
You can use the function Increase to add an additional sample to a determination series, e.g. because a determination was faulty and had to be removed from the statistics. The second number in the Statistics line will be increased automatically by one.

5.9 Printing a report manually

Menu Print reports
Proceed as follows to print a report manually:
1
Opening the main menu
In the main dialog, select Menu and press [OK].
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5.9 Printing a report manually
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2
Opening the print dialog
Select the menu item Print reports and press [OK].
The dialog window with the available reports opens:
3
Selecting the report
Select the desired report and press [OK].
The report is printed out.
The following reports can be printed out manually:
Results Result report with determination properties,
sample data, calculated results, etc.
Curve Curve report. The width of the curve is defined in
the system settings (see "Graphics width", page
46).
Measuring point
Measuring point list report.
list
Parameters Report with all method parameters of the loaded
method.
System System report with system settings, solution list,
external devices, etc.
Calculations/Statis­tics
Calculation report. The statistics are also printed out in the case of multiple determinations. The individual determinations with the respective sample size, the mean value, the absolute and the relative standard deviation are printed out for each result.
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5 Operation
PC/LIMS Machine-readable report with all of the data for
a determination. This report can be saved as a TXT file to a connected USB flash drive or sent to a terminal program or a LIMS via an RS-232 interface. The definition is made in the system settings (see "PC/LIMS report", page 46).
Report as in method

5.10 Manual control

Menu Manual control
The following functions are available in the manual control:
Dosing Stirring
The available subfunctions are listed for each function in the function bar.
The reports that are defined in the method will be printed out.
NOTE

5.10.1 Dosing

870 KF Titrino plus
The Stirrer function can only be selected if a stirrer is connected.
The following dosing functions are available in the manual control:
Prepare the buret unit (PREP)
Continuous dosing
Rinse the cylinder and tubings of the buret unit (see Chapter 10.1.2, page 70).
Dose while the [START] key is pressed.
(DOS)
Dose a fixed vol-
Dose a specified volume.
ume (ADD)
Preparing the buret unit (PREP)
The PREP function is used to rinse the cylinder and tubings of the buret unit and fill them air bubble-free. You should carry out this function before the first determination or once per day.
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33
5.10 Manual control
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Proceed as follows:
1
Open the manual control
In the main dialog, select Menu and press [OK].
The main menu opens.
Select the menu item Manual control and press [OK].
Manual control opens.
2
Select the dosing function
Select the Dosing item.
In the function bar, select PREP and press [OK].
The following message is displayed:
3
Start the preparing
CAUTION
Make sure that the buret tip is directed into a vessel that can accommodate the cylinder volume of your buret unit several times over.
Select Yes and confirm the message with [OK].
Preparing is carried out.
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5 Operation
Continuous dosing (DOS)
Continuous dosing will be carried out with the DOS function for as long as you keep the [START] key pressed down.
Proceed as follows:
1
Open the manual control
In the main dialog, select Menu and press [OK].
The main menu opens.
Select the menu item Manual control and press [OK].
Manual control opens.
2
Select the dosing function
Select the Dosing item.
In the function bar, select DOS and press [OK].
3
Configure the dosing function
NOTE
The dosing and filling rates should be decreased for viscous liq-
uids.
The maximum dosing and filling rates depend on the cylinder
volume (see Chapter 10.1.1, page 70).
Enter the dosing rate. Enter the filling rate.
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5.10 Manual control
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4
Start dosing
Press [START].
The status changes to busy, the dosed volume is displayed. When the volume of one cylinder has been dosed, the dosing cylinder will be refilled automatically.
5
Fill the cylinder
Press [STOP] or [BACK].
The dosing cylinder is filled. If you start the filling with [BACK], then the dialog will also be exited.
Dosing a particular volume (ADD)
You can dose a particular volume with the ADD function.
Proceed as follows:
1
Open the manual control
In the main dialog, select Menu and press [OK].
The main menu opens.
Select the menu item Manual control and press [OK].
Manual control opens.
2
Select the dosing function
Select the Dosing item.
In the function bar, select ADD and press [OK].
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3
Configure the dosing function
NOTE
The dosing and filling rates should be decreased for viscous liq-
uids.
The maximum dosing and filling rates depend on the cylinder
volume (see Chapter 10.1.1, page 70).
Enter the desired volume. Enter the dosing rate. Enter the filling rate.
4
Start dosing
Press [START].
The status changes to busy, the dosed volume is displayed. When the volume of one cylinder has been dosed, the dosing cylinder will be refilled automatically.
5
Fill the cylinder
Press [STOP] or [BACK].
5 Operation

5.10.2 Stirring

The dosing cylinder is filled. If you start the filling with [BACK], then the dialog will also be exited.
You can control a connected stirrer manually.
Proceed as follows:
1
Opening the manual control
In the main dialog, select Menu and press [OK].
The main menu opens.
Select the menu item Manual control and press [OK].
Manual control opens.
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5.10 Manual control
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2
Setting the stirring rate
Select the Stirrer item.
In the function bar, select Stir- or Stir+.
The stirring rate will be increased or decreased by one step each time the [OK] key is pressed. The algebraic sign changes the direction in which the stirring is done. When viewing the stirrer from above, this means:
– "+": counterclockwise rotation – "–": clockwise rotation
3
Switching on the stirrer
In the function bar, select On and press [OK].
The stirrer is started and stirs at the rate which has been set. Off is now displayed in the function bar.
4
Switching off the stirrer
In the function bar, select Off and confirm with [OK].
The stirrer is stopped.
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6 System settings

6.1 Basic settings

Menu System Settings
This chapter contains a description of general instrument settings.
User name
A user name can be entered here for the report. This parameter will only be printed if a user has been defined.
Entry max. 12 characters Default value empty
Instrument name
A instrument name can be entered here for the report. This parameter will only be printed if a designation has been defined.

6 System settings

Serial number
Program version
Time
Date
Language
Entry max. 10 characters Default value empty
Serial number of the instrument. This is printed as a part of the instrument identification in the report header.
Version number of the instrument software. This is printed as a part of the instrument identification in the report header.
Current time. Only valid numbers can be entered.
Format: hh:mm:ss
Current date. Only valid numbers can be entered.
Format: YYYY:MM:DD
Setting the dialog language. An additional language can be selected besides English.
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6.1 Basic settings
Dialog type
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NOTE
In order to ensure that a second language can be selected, it must first be installed. This installation must be carried out by specialist personnel. In chapter Language files, page 49, you will find details regarding the installation of a second language.
The user dialog can be limited for routine operations. One can operate normally with methods in the limited dialog. However, no settings can be made or methods deleted.
The resetting of the dialog will take effect as soon as you exit the main menu.
The limitation of the dialog results in the following:
The menu items System and Parameters are not shown in the main
menu.
Methods can only be loaded, but not deleted, exported or created.
NOTE
If the limited dialog for routine operation is activated, then the expert dialog cannot be activated during ongoing operation. To change the dialog type, the 870 KF Titrino plus must be switched off and then back on again. The expert dialog can be forced as soon as the instrument is started up again. Then it is possible to enter whatever settings one wishes, e.g. the changing of the dialog type. If the instrument is switched off again without changing the dialog type, then the routine dialog will remain activated.
Forcing the expert dialog:
Switch on the instrument. Wait for the display of the instrument logo with the lettering easy,
safe, precise.
Press the [STOP] key once again and hold it down while also briefly
pressing the [BACK] key.
Release both keys once again.
Selection
Expert | Routine
Default value Expert
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40
Expert
Complete dialog.
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Contrast
6 System settings
Routine
Limited dialog for routine operations.
The contrast of the display can be adjusted with the arrow keys [] and
[].
[⇦]: the contrast will be decreased by one step each time the key is
pressed.
[]: the contrast will be increased by one step each time the key is
pressed.
Input range 150 - 240 Default value 212
NOTE
Alternatively, the contrast can also be modified in the following man­ner:
Beep
PREP warning
Keep the red [STOP] key pressed down. As soon as the progress bar appears, also press the arrow key [] or [] repeatedly.
This method will, however, cause the contrast to be modified by several steps.
If this parameter is activated, then a short beep will sound in the following cases:
When a key is pressed. At the end of the determination. When the system remains conditioned without interruption for 10 sec-
onds.
Selection on | off Default value on
If this parameter is activated, then the recommendation will be made to carry out the function PREP (Preparing):
After the instrument is switched on. Each time a buret unit is attached.
870 KF Titrino plus
All tubing and the cylinder are rinsed with this function (see Chapter
10.1.2, page 70).
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6.2 Managing solutions

Selection on | off Default value on
6.2 Managing solutions

6.2.1 General

Menu System Solutions
Solutions can be used in intelligent buret units or in non-intelligent buret units. Intelligent buret units have a built-in data chip on which the data for the reagent is stored. This data is automatically read out during attach­ment and entered in the solution list.
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Edit
New
The name and the type are specified for each solution in the solution list. The asterisk (*) on the right-hand side indicates that this buret unit is attached (only for intelligent buret units). An unlimited number of solu­tions in buret units with data chip can be added to the solution list. The number of solutions in buret units without data chip is limited to 10 items.
Meaning of the type:
EU: exchange unit without data chip IEU: exchange unit with integrated data chip
not defined is the standard solution. It can be used to carry out determi­nations without having configured a solution. If you carry out a titer deter­mination with the titration parameter Solution = not defined, then the result will be saved as titer of this solution. If you carry out a titration with the titration parameter Solution = not defined, then the data of this solution will be used for the calculation. The titer and the concentration can be edited, but this standard solution can neither be renamed nor deleted.
Edit the data of the selected solution, see following chapter.
Add a new solution to the list, see following chapter.
Delete
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Delete the selected solution from the list.
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6.2.2 Editing the solution data

Name
The designation of the solution is used for unambiguous identification.
Entry max. 24 characters Default value empty
Type
The model of the buret unit is displayed.
Cylinder volume
Cylinder volume of the buret unit in mL. The cylinder volume is automati­cally read out with intelligent buret units.
Selection 1 | 5 | 10 | 20 | 50 Default value 20
Concentration
Concentration of the solution.
6 System settings
Concentration unit
Titer
Titer unit
Input range –999999999 - 9999999999 Default value 1.000
Unit of the concentration.
Selection µmol/mL | mmol/L | mol/L | g/L | mg/L | mg/mL |
µg/L | ppm | % | mEq/L | User-defined
Default value mol/L
User-defined
A user-defined unit can be created. This will be added to the selection list. The previous entry will be overwritten as soon as the new unit has been defined. A blank entry can be generated this way as well.
Titer of the solution.
Input range –999999999 - 9999999999 Default value 1.000
Unit of the titer.
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Selection µmol/mL | mmol/L | mol/L | g/L | mg/L | mg/mL |
µg/L | ppm | % | mEq/L | empty | User-defined
Default value empty
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43

6.3 File management

Date titer det.
Monitoring
Time interval
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User-defined
A user-defined unit can be created. This will be added to the selection list. The previous entry will be overwritten as soon as the new unit has been defined. A blank entry can be generated this way as well.
Date of the last titer determination.
Activating and deactivating the titer monitoring.
Selection on | off Default value off
This parameter is visible only when Monitoring = on.
You will be notified that this time interval (in days) has elapsed when start­ing a method. You can then select whether or not you would still like to start the method.
Input range 1 - 999 d Default value 999 d
6.3 File management
Menu System File management
NOTE
This menu item is visible only if a USB flash drive has been connected as an external storage medium.
Methods can be imported and deleted from a USB flash drive in this dia­log. Only methods located in the Files directory are displayed in the list (see "Directory structure on the USB flash drive", page 45).
A backup of the system can be created (all data and settings). Similarly, an existing backup can be reloaded.
Import
Import the selected method.
Delete
Backup
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44
Delete the selected method.
Create a backup of all data and settings on the USB flash drive.
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Restore
6 System settings
NOTE
Only one backup can be created on the same USB flash drive.
If a backup is already stored on the flash drive, then this will be over­written as soon as the function is performed once again.
Load the backup from a connected USB flash drive.
Directory structure on the USB flash drive
A directory with the instrument number will be created on the USB flash drive. The structure within this directory appears as follows:
Figure 14
Directory structure on the USB flash drive
Backup All of the files of the backup are stored in this
directory. The directory is created as soon as a backup is created for the first time.
Files Exported methods are stored in this directory.
The directory is created as soon as a backup is exported for the first time.
Only methods located in this directory can be imported.
pc_lims_report PC/LIMS reports are stored in this directory as
TXT files. The directory is created as soon as a PC/LIMS report is printed for the first time.
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6.4 Configuring external devices

6.4 Configuring external devices
Menu System External devices
PC/LIMS report
Specification of the storage location for the PC/LIMS report. The PC/LIMS report is a machine-readable report with all of the important data for a determination. It can be saved as follows:
as a TXT file on a USB flash drive. to a LIMS via an RS-232 interface. The 6.2148.030 RS-232/USB Box is
required for this purpose.
Selection COM2 | USB Stick Default value USB Stick
COM2
The report is sent via the serial COM2 interface. The interface parame­ters set in the dialog COM2 settings are used (see "Editing the COM2 settings", page 48).
USB Stick
The report will be saved as a TXT file on the USB flash drive in the folder pc_lims_report.
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Printer
Graphics width
Keyboard layout
If a printer is connected, then the printer type needs to be defined here in order for the reports to be printed out correctly.
The printers that have the designation ESC-POS are so-called POS printers (point-of-sale printers), i.e. they print on continuous paper.
Selection Citizen (ESC-POS) | Custom (ESC-POS) | Epson |
Epson (ESC-POS) | HP DeskJet | HP LaserJet | Seiko (ESC-POS)
Default value HP DeskJet
Adjust the width of the curve to be printed out to the paper width of the printer to be used. The default value depends on the selected printer. The height of the curve is 2/3 of the width.
Input range 100 - 3000 Pixels
A commercially available USB keyboard can be connected to make it eas­ier to enter text and numbers. Specify the country-specific keyboard lay­out.
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Balance
6 System settings
Selection English US | French FR | German CH | German
DE | Spanish ES
Default value English US
If you have connected a balance, then you must define the balance type here.
Selection AND | Mettler | Mettler AT | Mettler AX |
Ohaus | Precisa | Sartorius | Shimadzu
Default value Sartorius
The following table indicates the balance type that needs to be selected for the balance model:
Balance
Balance type
AND AND
Mettler AB, AE, AG, AM,
Mettler
AJ, PE, PM, PJ, PR, XP, XS
Mettler AT Mettler AT
Mettler AX, MX, UMX, PG,
Mettler AX
AB-S, PB-S
Ohaus Voyager, Explorer,
Ohaus
Analytical Plus
Precisa Precisa
Sartorius Sartorius
Shimadzu BX, BW Shimadzu
Editing the COM1 settings
Menu System External devices COM1 settings
The interface parameters for the connected balance are set under COM1 settings.
Baud rate
Data bits
870 KF Titrino plus
Transfer rate in characters per second.
Selection 1200 | 2400 | 4800 | 9600 | 19200 | 38400 |
57600 | 115200
Default value 9600
Number of data bits.
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47
6.4 Configuring external devices
Stop bits
Parity
Handshake
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Selection 7 | 8 Default value 8
Number of stop bits.
Selection 1 | 2 Default value 1
Type of parity testing.
Selection even | none | odd Default value none
Type of the data transfer protocol.
Selection hardware | software | none Default value hardware
NOTE
If communications problems occur, set the parameter Handshake to software, and make another attempt.
Editing the COM2 settings
Menu System External devices COM2 settings
The interface parameters for instruments connected to the RS-232/2 con­nector of the RS-232/USB Box (e.g. PC) are set under COM2 settings. The parameters and input ranges are identical to those for the COM1 interface.
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6.5 Instrument diagnosis

6.5.1 Loading program versions and language files

Menu System Diagnosis
New program versions or language files can be loaded from a USB flash drive. The corresponding file must be saved on the USB flash drive in a directory with the instrument number (e.g. 848 or 863).
You can distinguish between language files and program files by noting how the file name is constructed.
Program files
They are instrument-specific. The file name has the following structure:
5XXXyyyy.bin where
6 System settings
XXX =
yyyy =
Instrument type (e.g. 848 for the 848 Titrino plus)
Program version
Language files
They can be recognized by means of the two-digit language code in the file name. A language file contains the dialog texts for various instrument types. It is not instrument-specific. The file name has the following struc­ture:
5848xxxxYY.bin where
xxxx =
YY =
Version number
Language, e.g. DE (German), FR (French), ES (Spanish)
Loading a file
Proceed as follows:
1
Connecting the USB flash drive
Plug in the USB flash drive with the 6.2151.100 adapter (USB
MINI (OTG) - USB A) at the instrument's USB port.
Switch on the instrument.
2
Opening the update dialog
Under Menu System Diagnosis, select the menu item
Software update.
Press [OK].
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3
Opening the file selection
Press [OK].
The selection list with the program and language files present on the USB flash drive opens.
4
Selecting the file
Use the arrow keys to select the required file. Press [OK].
5
Starting the update
Press [START].
The update process is started, it runs automatically. At the end of the process, the instrument will be switched off automatically and switched back on again. No user intervention is required.

6.5.2 Diagnosis functions

Electronic and mechanical functional groups in Metrohm instruments can and should be checked as part of regular maintenance by specialist per­sonnel from Metrohm. Please ask your local Metrohm representative regarding the precise terms and conditions involved in concluding a corre­sponding maintenance agreement.
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7 Parameters

7.1 Karl Fischer Titrations (KFT)

7.1.1 Conditioning

Menu Parameters Conditioning
Under Conditioning, the conditions required for conditioning are defined.
Conditioning
If this parameter is switched on, then the first time the titration is started the working medium will be titrated to the endpoint with the specified control parameters. The status is kept stable. The actual method run does not begin until [START] has been pressed once more. Conditioning will be carried out again automatically after the titration.

7 Parameters

Start drift
Drift correction
Selection on | off Default value on
Conditioning OK will be displayed as soon as this volume drift has been reached and the titration can be started.
Input range 1 - 999 µL/min Default value 20 µL/min
The endpoint volume can be corrected by taking the drift value into account. For this, the volume drift is multiplied with the drift correction time and this value is then subtracted from the endpoint volume. The drift correction time is the time interval between the end of conditioning and the end of the determination.
Selection auto | manual | off Default value off
auto
The value of the current volume drift is applied automatically at the start of the titration.
manual
If the volume drift is known throughout a prolonged period of time, then this can be entered manually.
off
No drift correction takes place.
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Drift value
Cond. stop volume
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This parameter is visible only when Drift correction = manual.
Volume drift for manual drift correction.
Input range 0.0 - 99.9 µL/min Default value 0.0 µL/min
Maximum permissible volume that can be dosed during conditioning. Conditioning is stopped when the specified volume is dosed. If condition­ing is continued by pressing [START] once again, then the titrant volume that has already been dosed will not be taken into account; i.e. the dosing starts again at zero. The stop volume should be adjusted to the size of the titration cell in order to prevent any overflow.
Input range 0.00000 - 9999.99 mL Default value 20.0000 mL Selection off
Cond. stop time
Maximum permissible time over which conditioning may take place. Con­ditioning is stopped when the specified time has elapsed.
Input range 0 - 999999 s Selection off Default value off

7.1.2 Start conditions

Menu Parameters Start conditions
The parameters that are carried out before the start of titration are defined under Start conditions.
Start volume
Volume that is dosed prior to the start of the titration.
Input range 0.00000 - 9999.99 mL Default value 0.00000 mL
Dosing rate
Rate at which the start volume is dosed. The maximum dosing rate depends on the cylinder volume (see Chapter 10.1.1, page 70).
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Input range 0.01 - 166.00 mL/min Selection max. Default value max.
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Pause
Request sample ID
Request sample size
7 Parameters
Waiting time, e.g. in case of a slow response of the electrode after the start or reaction time after the dosing of a start volume.
Input range 0 - 999999 s Default value 0 s
Selection of the sample identification that is queried in the method run.
Selection off | ID1 | ID2 | ID1&ID2 Default value off
If this parameter is switched on, then the value for the sample size will be queried.
Selection on | off Default value on
For the methods "Blank Ipol" and "Blank Upol" the default value is off.
Request sample unit
If this parameter is switched on, then the unit for the sample size will be queried.
Selection on | off Default value off
Hold at request
If this parameter is switched on, then the method run will be paused dur­ing the query. If the parameter is switched off, the titration will be started in the background.
Selection on | off Default value on

7.1.3 Control parameters

Menu Parameters Control parameters
Under Control parameters, the control parameters for the endpoint are defined.
Endpoint at
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Measured value for the endpoint.
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7.1 Karl Fischer Titrations (KFT)
Titration rate
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Measuring mode Ipol:
Input range –1250.0 - 1250.0 mV Default value 250.0 mV Selection off
Measuring mode Upol:
Input range –125.00 - 125.00 µA Default value 25.00 µA Selection off
Three predefined sets of parameters can be selected for the titration rate.
Selection slow | optimal | fast | user Default value optimal
slow
For samples with a low water content or samples which release their moisture only slowly.
optimal
For all standard titrations. The parameters have been optimized for the most frequent applications.
fast
For uncritical samples with high water content.
user
The individual titration parameters can be modified.
The settings of the individual titration rates are listed in table 1, page
55.
Dynamics
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This parameter is visible only when Titration rate = user.
This parameter defines the control range before the specified endpoint. Individual volume steps are dosed in the control range, the dosing is finely controlled. The closer the endpoint, the slower the dosing until the vol­ume increment defined under Min. increment has been reached. The larger the control range, the slower the titration. Outside the control range, dosing is carried out continuously, and the dosing rate is defined under Max. rate.
Measuring mode Ipol:
Input range
0.1 - 1250.0 mV
Default value 100.0 mV Selection off
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Max. rate
Min. increment
7 Parameters
Measuring mode Upol:
Input range 0.01 - 125.00 µA Default value 10.00 µA Selection off
This parameter is visible only when Titration rate = user.
Rate at which dosing is carried out outside of the control range. The maxi­mum dosing rate depends on the cylinder volume (see Chapter 10.1.1, page 70) .
Input range 0.01 - 166.00 mL/min Selection max. Default value max.
This parameter is visible only when Titration rate = user.
Minimum volume increment that is dosed at the beginning of the titration and in the control range at the end of the titration. This parameter has a decisive influence on the titration rate and thus also on the accuracy. The smaller the selected minimum increment, the slower the titration.
Input range 0.1 - 99.90 µL Selection min. Default value min.
Table 1 Default values of the predefined titration rates for KFT
Titration rate
slow optimal fast
Dynamics
– Ipol
– Upol
300.0 mV
40.00 µA
100.0 mV
10.00 µA
30.0 mV
5.00 µA
Max. rate 1.00 mL/min maximum maximum
Min. increment minimum (= cylinder
volume/10000)
minimum (= cylinder volume/10000)
5.00 µL
Stop criterion
The titration is stopped when the endpoint has been reached and this stop criterion has been fulfilled. If no stop criterion has been selected then the titration will not be stopped. The stop conditions (see Chapter 7.1.5, page 58) always lead to a stop, even if the stop criterion has not been reached.
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Stop drift
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Selection drift | time | rel. drift | off Default value drift
drift
The titration is stopped when the stop drift has been reached.
time
The titration is stopped when the endpoint has been exceeded during a certain period of time (Delay time).
rel. drift
The titration is stopped when the sum of the drift at the start of the titration and the relative stop drift has been reached.
off
The titration will not be stopped until the stop conditions have been fulfilled.
This parameter is visible only when Stop criterion = drift.
Titration is stopped when the endpoint and the stop drift have been reached.
Input range 1 - 999 µL/min Default value 20 µL/min
Delay time
This parameter is visible only when Stop criterion = time.
When the endpoint is reached, the specified time is allowed to elapse after the last dosing and the titration is then stopped.
Input range 0 - 999 s Default value 10 s
Relative stop drift
This parameter is visible only when Stop criterion = rel. drift.
The titration is stopped when the endpoint and the sum of the drift at the start of the titration and the relative stop drift have been reached.
Input range 1 - 999 µL/min Default value 10 µL/min

7.1.4 Titration parameters

Menu Parameters Titration parameters
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Under Titration parameters, the parameters influencing the sequence of the entire titration are defined.
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Solution
7 Parameters
Selection of the solution from the solution list. We recommend always selecting the solution. This ensures that the correct data (titer, concentra­tion, etc.) is always used for the calculation. Solutions are defined under System Solutions.
For buret units with integrated data chip, a check is made in the method run to verify whether the correct solution has been attached and whether the type of dosing drive matches. For buret units without integrated data chip, the cylinder volume and the type of dosing drive are checked. The validity of the titer is checked for the selected solution at the start of the determination.
I(pol)
U(pol)
Electrode test
Selection
Selection of configured solution | not defined
Default value not defined
not defined
No check takes place.
The polarization current is the current that is applied to a polarizable elec­trode during the voltametric measurement. This parameter is available only with I(pol) determinations.
Input range –125 - 125 µA (Increment: 1) Default value 50 µA
The polarization voltage is the voltage applied to the polarizable electrode during an amperometric measurement. This parameter is available only with U(pol) determinations.
Input range –1250 - 1250 mV (Increment: 10) Default value 400 mV
For polarizable electrodes, an electrode test can be carried out. A check is made that the electrode is properly connected and that no short-circuit is present. The electrode test is carried out when the determination is started. This parameter is available only with I(pol) and U(pol) determina­tions.
Stirrer
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Selection on | off Default value off
When this parameter is switched on, then the stirrer is switched on at the start of the determination.
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7.1 Karl Fischer Titrations (KFT)
Stirring rate
Temperature
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Selection on | off Default value on
Setting the stirring rate. It can be set in steps of –15 to +15. The default setting 8 corresponds to 1000 U/min. The formula for calculating the rota­tional speed is specified in chapter 10.2, page 71. The optimum stirring rate can be tested in the manual control.
The algebraic sign of the stirring rate changes the direction in which the stirring is done. When the stirrer is viewed from above, this means:
"+": counterclockwise rotation "–": clockwise rotation
Input range –15 - 15 Default value 8
Manually entered titration temperature.
Input range –20.0 - 150.0 °C Default value 25.0 °C
Extraction time
Minimum duration of the titration. The titration will not be stopped during the extraction time, even if the endpoint has already been reached. The titration is however stopped if a stop condition is fulfilled during this time (see Chapter 7.1.5, page 58). The entering of an extraction time is e.g. recommended with samples that release water slowly or if a Karl Fischer oven is used.
Input range 0 - 999999 s Default value 0 s

7.1.5 Stop conditions

Menu Parameters Stop conditions
Under Stop conditions, the conditions for stopping a titration are defined, if this does not occur automatically. This could be the case when the endpoint set is not reached or if the stop criterion (see "Stop crite- rion", page 55) is not fulfilled.
Stop volume
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The titration is stopped when the specified volume has been dosed since the start of the titration. This volume should be adjusted to the size of the titration vessel in order to prevent the contents from running over.
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Stop time
Filling rate
7 Parameters
Input range 0.00000 - 9999.99 mL Default value 100.000 mL Selection off
The titration is stopped when the specified time has elapsed following the termination of the start conditions.
Input range 0 - 999999 s Selection off Default value off
Rate at which the dosing cylinder is filled after the titration. The maximum filling rate depends on the cylinder volume (see Chapter 10.1.1, page
70).
Input range 0.01 - 166.00 mL/min Selection max. Default value max.

7.1.6 Calculations - Methods "Blank Ipol/Upol"

Menu Parameters Calculation
Calculation formula
EP1*FCT
The calculation formula is predefined and cannot be edited.
The calculated result is saved as a variable Blank CV01 or Blank CV02 for each measuring mode separately (see page 62).
Factor (FCT)
If a larger amount of solvent is used for determining the blank value than is later used for the sample, then this factor must be used to convert the endpoint volume accordingly.
Input range –999999999 - 9999999999 Default value 1.0
Decimal places
Number of decimal places used to display the result.
Input range 0 - 5 Default value 2
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7.1 Karl Fischer Titrations (KFT)
Result unit
The result unit is displayed and saved together with the result. It cannot be modified.
Selection mL

7.1.7 Calculations - Methods "Titer Ipol/Upol"

Menu Parameters Calculation
Calculation formula
(C00*FCT)/EP1
The calculation formula is predefined and cannot be edited.
The calculated result (value and unit) is saved as the titer of the solution used.
The Factor (FCT) parameter must be adjusted according to what is used to determine the titer of the reagent and which unit the sample size has. If the calculation formula is selected and the [OK] key is pressed, then a table with the conversion factors will be displayed:
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Factor (FCT)
Decimal places
Table 2
Standard used Sample size
Conversion table
Factor (FCT)
in …
Water Standard 10 mg/g g Water content in mg/g
(see certificate)
Water g 1000
Water µL Density of water in
g/mL
Sodium tartrate dihydrate g 156.6
Sodium tartrate dihydrate mg 0.1566
Conversion factor, see table above.
Input range –999999999 - 9999999999 Default value 1.0
Number of decimal places used to display the result.
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Input range 0 - 5 Default value 4
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7 Parameters
Result unit
The result unit is displayed and saved together with the result.
Selection % | ppm | mg/mL | g | mg | mL | mg/piece |
User-defined
Default value mg/mL
User-defined
A user-defined unit can be created. This will be added to the selection list. The previous entry will be overwritten as soon as the new unit has been defined. A blank entry can be generated this way as well.

7.1.8 Calculations - Methods "KFT Ipol/Upol", "KFT Ipol/Upol–Blank"

Menu Parameters Calculation
Calculation formula for KFT Ipol/Upol
EP1*TITER*FCT/(C00*DIV)
Calculation formula for KFT Ipol–Blank
(EP1–CV01)*TITER*FCT/(C00*DIV)
Calculation formula for KFT Upol–Blank
(EP1–CV02)*TITER*FCT/(C00*DIV)
The calculation formulas are predefined and cannot be modified.
The Factor (FCT) and Divisor (DIV) parameters need to be adjusted, depending on the unit used for the sample size and the result. If the calcu­lation formula is selected and the [OK] key is pressed, then a table with the conversion factors will be displayed:
Table 3
Result unit Sample size
Conversion table
Factor (FCT) Divisor (DIV)
in …
% g 0.1 1
% mg 100 1
% mL 0.1 Density of the
sample in g/mL
ppm g 1000 1
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ppm mL 1000 Density of the
sample in g/mL
mg/mL g Density of the
1
sample in g/mL
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Factor (FCT)
Divisor (DIV)
Titer
Result unit Sample size
Factor (FCT) Divisor (DIV)
in …
mg/mL mL 1 1
mg/piece pieces 1 1
Conversion factor, see table above.
Input range –999999999 - 9999999999 Default value 0.1
Conversion factor, see table above.
Input range –999999999 - 9999999999 Default value 1.0
Titer of the solution used. As soon as a solution has been selected under Titration parameters, the value and the unit will be read out from the solution data under System Solutions and displayed here. If the titer is changed here manually, then the solution data will be updated.
Blank (CV01/2)
Decimal places
NOTE
Only the numerical value is taken into account in the calculation for­mula. The calculation will then provide a correct result only if the unit of the titer is mg/mL.
Input range
0.00000001 - 9999999999
Default value 1.000
This parameter is visible only with the methods KFT Ipol–Blank and KFT Upol–Blank.
This value is calculated with the blank value determination (methods Blank Ipol and Blank Upol) and entered here. The value can also be modified manually.
Input range –999999999 - 9999999999 mL Default value 0.0 mL
Number of decimal places used to display the result.
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Result unit

7.1.9 Statistics

7 Parameters
Input range 0 - 5 Default value 2
The result unit is displayed and saved together with the result.
Selection % | ppm | mg/mL | g | mg | mL | mg/piece |
User-defined
Default value %
User-defined
A user-defined unit can be created. This will be added to the selection list. The previous entry will be overwritten as soon as the new unit has been defined. A blank entry can be generated this way as well.
Menu Parameters Statistics
The statistics calculation of a multiple determination is switched on under
Statistics and it is defined how many determinations the series contains.
Statistics
Number of samples

7.1.10 Reports

If this funtion is switched on, then statistics calculations will be carried out for all of the defined results.
Selection on | off Default value off
For the methods "Titer Ipol" and "Titer Upol" the default value is on.
The number of determinations that are carried out for the statistics calcu­lations.
If an additional determination must be added to the determination series, because one determination was incorrect, for example, then this can be accomplished in the statistical overview (see Chapter 5.8, page 30).
Input range 2 - 20 Default value 3
Menu Parameters Reports
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The reports that will be printed out automatically in connection with a determination are defined under Reports.
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Results
Curve
Calculations/Statistics
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The result report contains the calculated results, equivalence points and endpoints, sample data, etc.
Selection on | off Default value off
Curve report. The width of the curve is defined in the system settings (see "Graphics width", page 46).
Selection on | off Default value off
Output of the calculation formulas for the individual results. The results are printed with the maximum resolution. This makes recalculation with an external program possible. The following data is printed out in addition when statistics is switched on:
Measuring point list
Parameters
PC/LIMS
Result and sample size of the individual determinations Mean value as well as absolute and relative standard deviation
Selection on | off Default value off
Output of the measuring point list.
Selection on | off Default value off
All of the parameters of the current method are printed out with the para­meter report.
Selection on | off Default value off
The PC/LIMS report is a machine-readable report with all of the data important for a determination. The PC/LIMS report can be saved as a TXT file on a USB storage medium or sent via an RS-232 interface to a LIMS. The output location is defined in the system settings (see "PC/LIMS report", page 46).
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The file name of the TXT file is constructed as follows: PC_LIMS_Report­ID1-YYYYMMDD-hhmmss.txt.
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7 Parameters
Selection on | off Default value off
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8.1 Quality Management and qualification with Metrohm

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8 Operation and maintenance

8.1 Quality Management and qualification with Metrohm
Quality management
Metrohm offers you comprehensive support in implementing quality man­agement measures for instruments and software. Further information on this can be found in the brochure "Metrohm Quality Management" available from your local Metrohm representative.
Qualification
Please contact your local Metrohm representative for support in qualifica­tion of instruments and software. The Installation Qualification (IQ) and Operational Qualification (OQ) are offered by Metrohm represen­tatives as a service. They are carried out by trained employees using stan­dardized qualification documents and in accordance with the currently applicable requirements of the regulated industry. Further information on this can be found in the brochure "Analytical Instrument Qualifica- tion – Confidence in quality with IQ/OQ".
Maintenance
The electronic and mechanical functional groups of Metrohm instruments can and should be checked by specialist personnel from Metrohm as part of a regular preventive maintenance schedule. Please ask your local Metrohm representative regarding the precise terms and conditions involved in concluding a corresponding maintenance agreement. Further information on this can be found in the brochure "Metrohm Care Con- tracts – Protect your investment the smart way" available from your local Metrohm representative.
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9 Troubleshooting

9.1 Karl Fischer titration

Problem Cause Remedy

9 Troubleshooting

The drift is very high during conditioning.
The drift becomes greater after each titration.
The titration will not be finished.
The titration cell is leaking. Check seals and septum. If necessary,
replace.
Replace molecular sieve.
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
Add buffer, see technical literature.
optimum range anymore.
The titration cell is leaking. Check seals and septum. If necessary,
replace.
Replace molecular sieve.
The minimum increment is too low.
The stop criterion is unsuit­able.
See also: The drift increases after each titration.
Define Titration rate = user and increase the minimum volume increment (Min. incre- ment) (see Chapter 7.1.3, page 53).
Adjust the control parameters (see Chapter
7.1.3, page 53):
Increase the stop drift. Select a short delay time.
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9.2 Miscellaneous

Problem Cause Remedy
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The sample is over­titrated.
The solution becomes darker after each titration.
The increments at the end of the titration are too high.
The amount of methanol in the working medium is too low.
The electrode may be cov­ered.
The electrode may be cov­ered.
Define Titration rate = user and reduce
dosing rate (Max. rate) (see Chapter
7.1.3, page 53).
The following experiment provides a clue for the optimum dosing rate: During condi­tioning, display the drift and add sample without starting the titration. Select a value below the highest drift as dosing rate.
Stir faster.
Replace the working medium. Reduce the amount of solubilizer, if work-
ing with solvent mixtures, see technical lit­erature.
Wipe off the electrode with ethanol or a suita­ble solvent.
Replace the working medium.
Wipe off the electrode with ethanol or a suita­ble solvent.
The electrode has a short circuit.
The endpoint is reached too quickly.
The titration times with volumetric titration are con­stantly longer.
The dosing rate outside the control range is too high.
With two-component reagents the buffer capacity of the solvent can be exhausted.
9.2 Miscellaneous
Problem
No report is printed. The printer is not recog-
Cause Remedy
nized by the instrument.
1. Check the Pt wires.
2. Switch on the electrode test.
Define Titration rate = user and reduce the dosing rate (Max. rate) (see Chapter 7.1.3, page 53).
Replace the working medium.
Switch the 870 KF Titrino plus off and on
again.
Use a hub on the USB connector and con-
nect the printer to the hub.
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Problem Cause Remedy
9 Troubleshooting
The USB keyboard or the PC mouse does not function.
The display is no longer readable.
Mettler XP balances send "R" or "O ----" as ID1.
Message 020-511 "Action not possi­ble" is displayed.
The printer model is not compatible.
The keyboard or mouse is not recognized by the instrument.
Use a printer which fulfills the required specifi­cations (see Chapter 10.4.4, page 74).
Switch the 870 KF Titrino plus off and on
again.
Use a hub on the USB connector and con-
nect the keyboard or mouse to the hub.
The keyboard or the mouse is not compatible.
The contrast is set incor­rectly.
The automatic calibration
Use a model which fulfills the required specifi­cations (see Chapter 10.4, page 72).
Adjust the contrast correctly (see Chapter 6.1, page 39).
Switch off the automatic calibration.
of the balance is switched on.
The USB stick is no longer connected.
1. Connect the USB stick.
2. Switch the instrument off and on again.
The USB stick is full. Use a different USB stick.
Delete files with the aid of a PC.
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10.1 Exchange unit

10 Appendix

10.1 Exchange unit

10.1.1 Maximum dosing and filling rate

The maximum dosing rate and maximum filling rate for the exchange unit depend on the cylinder volume:
Cylinder volume Maximum rate
1 mL 3.00 mL/min
5 mL 15.00 mL/min
10 mL 30.00 mL/min
20 mL 60.00 mL/min
50 mL 150.00 mL/min
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Independent of the cylinder volume, values ranging from 0.01 to 166.00 mL/min can always be entered. When the function is carried out the rate will be, if necessary, decreased automatically to the highest possible value.

10.1.2 Parameters for the preparing (PREP)

The PREP function (Preparing) is used to rinse the cylinder and tubings of the exchange unit and fill them air bubble-free. You should carry out this function before the first determination or once per day.
Preparing is carried out with the following, non-alterable settings:
The entire cylinder volume is dosed twice with the maximum dosing
rate.
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2000
1500
1000
500
-15 -10 -5 0 5 10 15
r/min

10.2 Stirring rate

The stirring rate can be adjusted in steps of –15 to +15.
The approximate rotational speed can be calculated with the following formula:
Example:
Stirring rate set: 8
Rotational speed in rpm = 125 · 8 = 1000
10 Appendix
Rotational speed/min (r/min) = 125 · stirring rate

10.3 Balance

Figure 15
Rotational speed depending on stirring rate
The sample size and the associated unit can be sent from a connected bal­ance. The sample size is transmitted as a number with up to ten charac­ters (including algebraic sign and decimal point).
Sample size and unit are sent as a single character string. They are separa­ted by a space character. The string is terminated with the ASCII charac­ters CR and LF.
If the balance sends a negative sample size (e.g. when you are reweighing a sample), then the algebraic sign is adopted. The algebraic sign is, how­ever, ignored for the calculations.
NOTE
With some balances, the sample identification and the method can be sent in addition to the sample size.
Make sure that the balance does not send the sample size until the end.
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10.4 USB devices

Mettler AX
For the Mettler AX balance, the fields that contain the sample identifica­tion or the method must be designated as follows:
Designation for the field with the method name: METHOD Designation for the field with sample identification 1: ID1 Designation for the field with sample identification 2: ID2
10.4 USB devices
USB peripheral devices that are to be connected must support either the USB 1.0/1.1 (Full Speed) or the USB 2.0 (High Speed) standard. The maximum data transfer rate is however in any case 12 MBit/s.
Keyboards, PC mice and barcode readers are so-called HID devices (Human Interface Device) and can be connected via a USB hub only.
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NOTE
Printers should also be connected via a USB hub. Depending on the manufacturer or printer type a direct connection is however possible.

10.4.1 6.2147.000 numerical USB keypad

The [Num Lock] key must be pressed for navigating in the dialog. The arrow keys are effective in conjunction with it.
The respective editing dialog must be opened for the numerical input.
Table 4
Key of the 870 KF Titrino plus or function in the editing dia­log
[BACK] [Home]
[] [] [] []
[] [] [] []
[OK] [Enter]
Key assignment
Key on the numerical USB keypad
[BS] (backspace)
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Clear [Del]
Accept [Home]
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10.4.2 Key assignment of a USB keyboard

A commercially available USB keyboard can be connected to make it eas­ier to enter text and numbers.
The respective editing dialog must be opened for the text input and numerical input.
Table 5 Key assignment
10 Appendix
Key of the 870 KF Titrino plus
Key on the USB keyboard or function in the editing dia­log
[BACK] [Esc]
[] [] [] []
[] [] [] []
[OK] [] (enter key)
or
[Enter] on the numerical keypad
[STOP] [Ctrl] + [S]
[START] [Ctrl] + [G]
[] (backspace)
Clear [Delete]
Cancel [Ctrl] + [Q]
Accept [Esc]

10.4.3 PC mouse

870 KF Titrino plus
NOTE
The lettering of the USB keyboard may differ from above lettering, depending on the country-specific keyboard used.
In order to make navigating in the dialog of the 870 KF Titrino plus easier, a PC mouse can be connected.
Table 6
Mouse functions
Key of the 870 KF Titrino plus Mouse function
[OK] Left mouse button
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10.5 System initialization

10.4.4 Printer

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Key of the 870 KF Titrino plus Mouse function
[BACK] Right mouse button
[] [] [] [] Mouse movement vertical/hori-
zontal
[] [] Scroll wheel vertical
The range of USB printers available is extremely varied and constantly changing. The following points must be taken into account when select­ing a printer:
USB interface necessary Printer language: HP-PCL, Canon BJL Commands, Epson ESC P/2 or
ESC/POS
NOTE
Inexpensive printers are often designed solely for use with a PC and may not be equipped with one of the printer languages listed above. Such models are not suitable for this reason.
10.5 System initialization
In very rare instances, a faulty file system (e.g. because of a program crash) may lead to an impairment of program functioning. The internal file system must be initialized in such cases.
CAUTION
All user data (methods, solutions, etc.) are deleted if a system initializa­tion is carried out. Afterwards, the instrument will have the factory set­tings again.
We recommend creating a backup of the system at regular intervals in order to avoid data losses.
After a system initialization the program versions and language files do not have to be reloaded. Only the selection of the dialog language may have to be reset in the system settings.
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Proceed as follows for the system initialization:
1
Switching off the instrument
Keep the red [STOP] key pressed down for at least 3 s.
A progress bar is displayed. If the key is released during this time, then the instrument will not be switched off.
2
Switching on the instrument
Keep the red [STOP] key pressed down for approx. 10 s.
The dialog for confirmation of the initialization is displayed for 8 s. The initialization must be confirmed during this time.
10 Appendix
3
Confirming the initialization
NOTE
If the request is not confirmed within 8 s, then the procedure will be canceled.
Press [BACK] twice.
Initialization is started. The process takes approximately 80 s. The instrument will be automatically restarted after successful initializa­tion.
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10.6 Remote interface

1
5
6
9
5
1
9
6
+5 V
t
p
10.6 Remote interface

10.6.1 Pin assignment of the remote interface

Figure 16 Pin assignment of remote socket and remote plug
The above figure of the pin assignment applies for all Metrohm instru­ments with 9-pin D-Sub remote connector.
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Table 7
Inputs and outputs of the remote interface
Pin No. Assignment Function
1 Output 0 Ready/EOD
2 Output 1 -
3 Output 2 Titration
4 Output 3 Cond OK
5 Output 4 Error
6 0 volt (GND)
7 +5 volts
8 Input 0 Start
9 Input 1 Stop
Inputs
approx. 5 kΩ Pull-up
tp > 100 ms
active = low, inactive = high
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t
p
[START]
Output 0
Output 1
Output 3
Output 2
Output 4
ready/EOD
condOK
Error
Start
Stop
Input 0
Input 1
EOD
[START]
[STOP]
Titr/Determ
10 Appendix
Outputs
Open Collector
tp > 200 ms
active = low, inactive = high
IC = 20 mA, V
CEO
+5 V: maximum load = 20 mA

10.6.2 Status diagram of the remote interface

Figure 17
EOD = End of Determination
Remote status diagram
= 40 V

10.7 Remote control via an RS-232 connection

The 870 KF Titrino plus can be remote controlled via an RS-232 connec­tion. For this, a 6.2148.030 RS-232/USB Box is necessary. Connect the RS-232/USB Box to the USB interface of the instrument.
The RS-232/USB Box has two connectors for RS-232 instruments. The RS-232 remote control functions only through the connector RS-232/2. The connector RS-232/1 is designed for connection with a balance. Con­nect the RS-232/2 connector of the RS-232/USB Box to a serial interface (COM interface marked with the symbol IOIOI) of a PC. Use a
6.2134.040 connection cable.
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10.7 Remote control via an RS-232 connection
6.2134.040
Figure 18 Connecting the RS-232/USB Box to the PC
Interface parameters
We recommend the following parameters for the RS-232 interface COM2:
Baud rate: 19200 Data bits: 8 Stop bits: 1 Parity: none Handshake: software
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On the 870 KF Titrino plus, adjust the interface parameters under Menu System External devices COM2 settings.
Transfer protocol
The data communication is synchronous. On each command there is an acknowledgement by the instrument.
A command must be sent to the instrument with the control characters CR LF as terminator. The acknowledgements of the instrument will also be transferred with CR LF as terminator.
The instrument does not send spontaneous messages.

10.7.1 Commands and variables

Command
$G Start/Continue Corresponds to the key [START] or [Con-
$S Stop Corresponds to the key [STOP]
$H Hold Hold the method run
Function Comment
tinue]
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Command Function Comment
10 Appendix
$D Scan instrument sta-
tus
Acknowledgements: Ready;0, Busy;0, Hold;0 or Cond;0 (0 = no message)
If a message on the instrument requires the interaction of the user, the acknowl­edgement of the status scan displays the corresponding message number. Exam­ple:
Busy;010-119
= "Check buret unit"
The message can be confirmed with [OK] or [Cancel], see below.
$A
Confirm message Confirm the message on the instrument
with [OK]
A mandatory status scan providing the message number must take place immedi­ately before confirming the message, see above.
$A(OK), $A(CANCEL) Confirm message Confirm the message with [OK] or [Can-
cel]
$A(YES), $A(NO) Confirm message Confirm the message with [Yes] or [No]
$L(method name) Load method The method name has to be known and
unique.
$Q(variable) Request variable value Examples for variables: EP1, R1, C00.
List of variables, see below.
Variable Comment
C00 Sample size
EP1 Volume of the endpoint EP1
CI# Sample identification (# = 1…2)
R1 Result
CV01 Common variable (blank value at KFT Ipol)
CV02 Common variable (blank value at KFT Upol)
SMN1 Mean value of result R#
TITER Titer of selected solution
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10.8 Arithmetic algorithms in the 870 KF Titrino plus

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Variable Comment
CONC Concentration of selected solution
FCT Factor
DIV Divisor
MCV End volume, i.e. total dosed volume at the end of the titration
EM1 Measured value of the endpoint EP1
ED1 Time at the endpoint EP1
MSV Start volume
DD Duration of the entire determination
The values of the variables are only available after the end of a determina­tion (in the status 'ready').
Acknowledgement of
Comment
the instrument
OK Command executed
E1 Method not found
E2 Invalid variable
E3 Invalid command
10.8 Arithmetic algorithms in the 870 KF Titrino plus
Numerical format
The software of the 870 KF Titrino plus calculates in accordance with the widespread standard IEEE 754 (IEEE Standard for Binary Floating-Point Arithmetic for Microprocessor Systems). This means that the numbers are used in calculations in "double precision" (64 bit). Decimal numbers are converted into binary numbers in the computer and used in this form for calculations. The output on the display and in reports once again contains decimal numbers; the binary numbers are thus converted back into deci­mal numbers. In order to be able to check the internal calculations per­formed by the computer yourself in accordance with IEEE 754, the num­bers are reproduced in the calculation report in complete accuracy. A min­imal difference may arise between an originally entered decimal number and the internal computer representation in complete accuracy in the range of the rear decimal places. This difference results from the fact that an exact binary equivalent does not exist for every decimal number. If, for example, you enter the sample size 50.3 mg, this will be depicted in the calculation report in "double precision" with 5.02999999999999E+01.
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10 Appendix
Rounding-off process
Measured values and results are rounded to the defined number of deci­mal places (commercial rounding, in accordance with the US Pharmaco­peia USP). If the digit at the first dropped decimal place is 1, 2, 3 or 4, then it will be rounded off; if this digit is 5, 6, 7, 8 or 9, then it will be rounded up. Negative digits will be rounded in accordance with their amount, i.e. away from zero.
Examples:
2.33 yields 2.3
2.35 yields 2.4
2.47 yields 2.5
–2.38 yields –2.4
–2.45 yields –2.5
Statistics
The arithmetic mean value and the absolute and relative standard devia­tions of results are calculated:
You can statistically evaluate a maximum of five results (1 k 5) calcu­lated in a determination. A statistical series can contain a maximum of 20 determinations (1 n 20).
The following convention applies to the subsequent formulas:
1 n 20 and 1 k 5.
Mean value:
Absolute standard deviation:
Relative standard deviation (in %):
Explanations
The individual values are incorporated in the statistics with full accuracy.
15 significant places are yielded when the 64 bit numerical format is applied for the floating-point number in decimal presentation.
870 KF Titrino plus
The accuracy can be controlled by the selection of the prefix of the unit (milli, micro) and the number of decimal places.
Example:
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10.8 Arithmetic algorithms in the 870 KF Titrino plus
The result displayed, 1234.56789158763 mg/L, has 15 significant pla­ces. It should be rounded off to three decimal places according to the above rounding-off process:
1234.568 mg/L.
If the same result is expressed in "g/L" (1.23456789158763 g/L), and is also rounded off to three decimal place, this yields
1.235 g/L.
I.e. you obtain the lowest losses in accuracy with rounding when you select the application and the numerical format in such a way that the numbers displayed have as many places before the decimal point as possi­ble.
A complete recalculation of the statistics using a pocket calculator or PC calculation programs may exhibit deviations. This can be explained by the different binary numerical formats used by these computers.
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NOTE
The above losses of accuracy by rounding off in the range of significant places are only relevant theoretically. They are generally several orders of magnitude less than measurement technique uncertainties (balance errors, dosing errors, measuring errors).
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11 Technical specifications

11.1 Measuring inputs

The measuring cycle is 100 ms for all measuring modes.

11.1.1 Polarizer

A measuring input (Pol.) for polarizable electrodes.
11 Technical specifications
Measuring mode Ipol
Polarization current
Measuring range
Resolution 0.1 mV
Measuring accuracy
Measuring mode Upol
Polarization voltage
Measuring range
Resolution 0.01 µA
Measuring accuracy
Determination with adjustable polarization current.
–120 - +120 µA (increment: 1 µA) –125 - –121 µA / +121 - +125 µA: non-guaranteed values, dependent on reference voltage +2.5 V
–1,200 - +1,200 mV
±0.2 mV (±1 digit, without sensor error, under reference conditions)
Determination with adjustable polarization voltage.
–1,200 - +1,200 mV (increment: 10 mV) –1,250 - –1,210 mV / +1,210 - +1,250 mV: non-guaranteed values, dependent on reference voltage +2.5 V
–120 - +120 µA
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11.2 Dosing drive

11.2 Dosing drive
Resolution 10,000 steps per cylinder volume
Exchange unit
Cylinder volume 1 mL
5 mL 10 mL 20 mL 50 mL
Accuracy Fulfills ISO/DIN standard 8655-3

11.3 Interfaces

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USB (OTG) connec-
For connecting USB devices.
tor
MSB connector For connecting a stirrer.
Remote connector For connecting instruments with a remote interface.

11.4 Mains connection

Voltage
Frequency 50 - 60 Hz
Power consump­tion
Fuse 2 × 2.0 ATH, electronic overload protection
100 - 240 V (± 10%)
45 W

11.5 Safety specifications

This instrument fulfills the following electrical safety requirements:
CE designation in accordance with the EU directives:
2006/95/EC (Low Voltage Directive, LVD) 2004/108/EC (EMC Directive, EMC)
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Federal Inspectorate for Heavy Current Installations ESTI (Accreditation Number SCESp 033)
Safety mark for certification type 2 in accordance with NEV (type
testing with market monitoring, EMC conformity)
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11 Technical specifications
ETL Listed Mark:
Control number 3144965 UL 61010-1 CSA-C22.2 No. 61010-1
Design and testing According to EN/IEC/UL 61010-1, CSA-C22.2 No. 61010-1, protection
class I, EN/IEC 60529, degree of protection IP40.
Safety instructions This document contains safety instructions which have to be followed
by the user in order to ensure safe operation of the instrument.

11.6 Electromagnetic compatibility (EMC)

Emission
Standards fulfil­led
Immunity
Standards fulfil­led
EN/IEC 61326-1 EN/IEC 61000-6-3 EN 55022 / CISPR 22
EN/IEC 61326-1 EN/IEC 61000-6-2 EN/IEC 61000-4-2 EN/IEC 61000-4-3 EN/IEC 61000-4-4 EN/IEC 61000-4-5 EN/IEC 61000-4-6 EN/IEC 61000-4-11 EN/IEC 61000-4-14

11.7 Ambient temperature

Nominal function range
Storage –20 - +60 °C
Transport –40 - +60 °C
870 KF Titrino plus
+5 - +45 °C (at a maximum of 85% humidity)
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11.8 Reference conditions

11.8 Reference conditions
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Ambient tempera­ture
Relative humidity 60%
Operating temper­ature status
Validity of the data
+25 °C (±3 °C)
Instrument in operation at least 30 min
After adjustment

11.9 Dimensions

Material of hous­ing
Material of display cover
Width 142 mm
Height 164 mm
Depth 310 mm
Polybutylene terephthalate (PBT)
Glass
Weight 2,950 g
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12 Warranty (guarantee)

Metrohm guarantees that the deliveries and services it provides are free of defects in materials, design or manufacturing.
The general warranty period is 36 months (exclusions below) from the date of delivery or 18 months in the event of continuous operation. The warranty remains valid on the condition that the servicing is provided by a service organization authorized by Metrohm at defined intervals and with a defined scope.
The warranty period for anion suppressors of the type "MSM" is 120 months from the date of delivery or 60 months in the case of continuous operation.
The warranty period for IC separation columns is 90 days after start-up.
For third-party components that are recognizable as such, the manufac­turer's warranty regulations apply.
12 Warranty (guarantee)
Consumables and materials with limited storage life and glass breakage in the case of electrodes or other glass parts are excluded from the warranty.
Warranty claims cannot be asserted if the ordering party has failed to meet its payment obligations according to schedule.
During the warranty period, Metrohm undertakes either to replace free of charge or to credit the purchaser for any modules or components that can be shown to be faulty. Any transport or customs fees that may apply are the ordering party’s responsibility.
The precondition for this is that the ordering party has to specify the arti­cle number, the article designation, an adequate error description, the delivery date and (if applicable) the serial number or chip data in the Sup­port Tracker. Metrohm then decides whether a replacement or a credit note is to be issued or whether the faulty part has to be returned using the Return Material Authorization (RMA). If a replacement or credit note is issued, the ordering party undertakes to store the faulty part for at least 24 months in accordance with the current storage directives (in compli­ance with ESD guidelines) and to hold it in readiness for onsite inspection or for return shipment to Metrohm. Metrohm reserves the right to invoice the ordering party for these articles, including retroactively, in the event of noncompliance with these preconditions.
870 KF Titrino plus
The same warranty periods that are specified for a corresponding new part apply to parts that are replaced or repaired within the above-men­tioned warranty periods. However, replacement or repair of a part does not extend the warranty period of the entire system.
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Deficiencies arising from circumstances that are not the responsibility of Metrohm, such as improper storage or improper use, etc., are expressly excluded from the warranty.
Metrohm also offers a 120 month spare parts availability guarantee and a 60 month PC software support warranty, calculated from the date on which the product is withdrawn from the market. The content of this war­ranty is the ability of the customer to obtain functioning spare parts or appropriate software support at market prices during the time of the war­ranty period.
If Metrohm AG is unable to meet this obligation due to circumstances beyond the control of Metrohm AG, then the ordering party shall be offered alternative solutions at preferential conditions.
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13 Accessories

NOTE
Subject to change without notice.

13.1 Scope of delivery

2.870.0010 870 KF Titrino plus
13 Accessories
Qty.
Order no. Description
1 1.870.0010 870 KF Titrino plus
1 6.0338.100 Double Pt-wire electrode for volumetry
Double Pt-wire electrode, Metrohm plug-in head G, for volumetric Karl Fischer titration and 684/737 Coulometer (cell with diaphragm).
Shaft material: Glass Measuring range: –2000 ... 2000 Measuring unit: mV Temperature range, long-
term (°C): Temperature range, short­term (°C): SGJ sleeve: No
Shaft diameter top (mm): 8 Shaft diameter bottom (mm): 8 Min. immersion depth (mm): 5 Electrode plug-in head: Metrohm plug-in head G Indicator electrode type: Pt Indicator electrode shape: Wire
1 6.1244.040 Set of seals
–20 ... 70
–20 ... 70
870 KF Titrino plus
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13.1 Scope of delivery
Qty. Order no. Description
1 6.1403.040 KF Adsorber tube
Used with KF equipment. Including cover and O-ring.
Height (mm): 113 Outer diameter (mm): 8
1 6.1414.030 KF titration vessel lid
For volumetric KF titrations.
Material: PTFE Material remark: Insert
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1 6.1415.220 Titration vessel / 20-90 mL
Material: Clear glass Height (mm): 80 Outer diameter (mm): 78 Volume (mL): 20 ... 90
1 6.1415.250 Titration vessel / 50-150 mL
Material: Clear glass Height (mm): 80 Outer diameter (mm): 78 Volume (mL): 50 ... 150
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