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870 KF Titrino plus
Manual
8.870.8003EN
Page 2
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Metrohm AG
CH-9101 Herisau
Switzerland
Phone +41 71 353 85 85
Fax +41 71 353 89 01
info@metrohm.com
www.metrohm.com
870 KF Titrino plus
Manual
8.870.8003EN 10.2009 jb
Page 4
Teachware
Metrohm AG
CH-9101 Herisau
teachware@metrohm.com
This documentation is protected by copyright. All rights reserved.
Although all the information given in this documentation has been checked
with great care, errors cannot be entirely excluded. Should you notice any
mistakes please send us your comments using the address given above.
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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 ......................................................... 10
4.5 Connecting keyboard, printer and other USB devi-
ces ........................................................................................ 11
4.6 Connecting instruments to the remote connector .......... 14
4.7 Attaching the exchange unit ............................................. 14
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 ............................................ 17
5.2.3 Navigating in the dialog ......................................................... 18
5.2.4 Entering text and numbers ..................................................... 18
5.2.5 Selecting from a selection list ................................................. 19
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III
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Table of contents
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5.3 Methods .............................................................................. 20
5.3.1 Method templates ................................................................. 20
5.3.2 Loading a method ................................................................. 20
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 time of determination
start ...................................................................................... 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 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 .......................................................... 48
6.5.1 Loading program versions and language files ......................... 48
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 Handling and maintenance 65
9 Troubleshooting 66
10 Appendix 69
Table of contents
8.1 Quality Management and validation with Metrohm ....... 65
9.1 Karl Fischer titration .......................................................... 66
9.2 Miscellaneous ..................................................................... 67
10.1 Exchange unit ..................................................................... 69
10.1.1 Maximum dosing and filling rate ............................................ 69
10.1.2 Parameters for the preparing (PREP) ....................................... 69
10.2 Stirring rate ......................................................................... 69
10.3 Balance ................................................................................ 70
10.4 USB devices ......................................................................... 71
10.4.1 Numerical USB keypad 6.2147.000 ........................................ 71
10.4.2 Key assignment of a USB keyboard ........................................ 71
10.4.3 PC mouse .............................................................................. 72
10.4.4 Printer ................................................................................... 73
10.5 System initialization ........................................................... 73
10.6 Remote interface ................................................................ 74
10.6.1 Pin assignment of the remote interface .................................. 74
10.6.2 Status diagram of the remote interface .................................. 75
10.7 Remote control via an RS-232 connection ....................... 76
10.7.1 Commands and variables ....................................................... 77
11 Technical specifications 79
11.1 Measuring inputs ................................................................ 79
11.1.1 Polarizer ................................................................................ 79
11.2 Dosing drive ........................................................................ 80
11.3 Interfaces ............................................................................. 80
11.4 Mains connection ............................................................... 80
11.5 Safety specification ............................................................ 80
11.6 Electromagnetic compatibility (EMC) ................................ 81
11.7 Ambient temperature ......................................................... 81
11.8 Reference conditions .......................................................... 81
11.9 Dimensions .......................................................................... 82
870 KF Titrino plus
12 Conformity and warranty 83
12.1 Declaration of Conformity ................................................. 83
12.2 Quality Management Principles ........................................ 84
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V
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Table of contents
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12.3 Warranty (guarantee) ......................................................... 85
13 Accessories 86
13.1 Scope of delivery ................................................................ 86
13.2 Optional accessories ........................................................... 91
Index 93
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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 ................................................................. 11
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). ..................................... 13
Figure 11 Connecting a remote cable ............................................................. 14
Figure 12 Attaching the exchange unit ........................................................... 14
Figure 13 Keypad 870 KF Titrino plus .............................................................. 17
Figure 14 Directory structure on the USB stick ................................................. 45
Figure 15 Rotational speed depending on stirring rate .................................... 70
Figure 16 Pin assignment of remote socket and plug ...................................... 74
Figure 17 Remote status diagram .................................................................... 75
Figure 18 Connecting the RS-232/USB Box to the PC ...................................... 76
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 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 on a connected USB stick. 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 determination according to Karl Fischer.
Measuring modes:
– Ipol (voltametric measurement with adjustable polarization cur-
rent)
– Upol (amperometric measurement with adjustable 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.
The present instrument is suitable for processing chemicals and flammable
samples. The usage of the 870 KF Titrino plus therefore requires that the
user has 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 Stick 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 have to be followed by the user in order to ensure safe
operation of the instrument.
1.2.1 Symbols and conventions
The following symbols and styles are used in this documentation:
Cross-reference to figure legend
The first number refers to the figure number, the second to the instrument part in the figure.
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Instruction step
Carry out these steps in the sequence shown.
Method Dialog text, parameter in the software
File ▶ New
[Next] Button or key
Menu or menu item
Warning
This symbol draws attention to a possible life hazard
or risk of injury.
Warning
This symbol draws attention to a possible hazard due
to electrical current.
Warning
This symbol draws attention to a possible hazard due
to heat or hot instrument parts.
Warning
This symbol draws attention to a possible biological
hazard.
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2
Caution
This symbol draws attention to a possible damage of
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 marks 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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3
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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.
Always pull the mains cable out of the mains connection socket before
connecting or disconnecting electrical appliances on the rear panel of the
instrument.
1.3.3 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. laboratory
flue).
￭ Keep all sources of flame far from the workplace.
￭ Clean up spilled fluids and solids immediately.
￭ Follow the safety instructions of the chemical manufacturer.
1.3.5 Recycling and disposal
This product is covered by European Directive 2002/96/EC, WEEE – Waste
from Electrical and Electronic Equipment.
The correct disposal of your old equipment will help to prevent negative
effects on the environment and public health.
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4
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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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6
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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 driftcontrolled 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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8
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 suitable for operation
and free of vibrations, if possible protected from corrosive atmospheres 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.
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.
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6.2151.100
4 Installation
Figure 6 Connecting a balance
When a 6.2151.020 USB cable is used, then the 6.2148.030 RS-232/USB
Box can be connected to the 870 KF Titrino plus by means of a USB hub or
a 6.2151.100 adapter (see Chapter 4.5, page 11).
Connect the 9-pin plug of the respective balance connecting cable to the
RS 232/1 connector. Consult the user manual of the balance in order to
select the correct connecting cable.
The parameters for the RS-232 interface on the instrument must match those
on the balance (see "Editing the COM1 settings", page 47). Additionally
consult the user manual of the balance.
4.5 Connecting 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.
Figure 7 Connecting USB devices
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4.5 Connecting keyboard, printer and other USB devices
Caution
Switch the instrument off before connecting or disconnecting a USB
device or a USB stick.
The 870 KF Titrino plus can recognize the device immediately after switching on.
The following devices can directly be operated 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.
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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.
The following devices can only be connected to a 6.2147.000 numer-
ical 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)
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12
If you wish to connect a variety of 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
870 KF Titrino plus
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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
USB MINI (OTG)-USB
USB stick
USB-Hub
RS-232/USB Box
6.2148.030
6.2151.100
Printer
4 Installation
designed for supplying power to several devices with elevated electricity
requirements.
Also observe the instructions in chapter 10.4, page 71.
Examples:
Figure 8 Connecting the USB stick
Figure 9 Connecting the 6.2147.000 USB keyboard with USB stick and
printer
Figure 10 Connecting the USB hub with USB stick, printer and the
6.2148.030 RS-232/USB Box (for connecting balances).
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4.6 Connecting instruments to the remote connector
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4.6 Connecting instruments to the remote connector
The 870 KF Titrino plus can be integrated in an automation system with the
aid of a remote cable.
Figure 11 Connecting a remote cable
A variety of different connecting cables are available for connecting
Metrohm instruments (e.g. sample changers) (see Optional Accessories
chapter).
4.7 Attaching the exchange unit
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 and
1
push all the way to the rear.
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14
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4 Installation
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 34.
￭ Confirm the message with [OK].
The display of this message can be switched off in the system settings (see "PREP warning", page 41).
The main dialog is displayed:
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.
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16
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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
Figure 13 Keypad 870 KF Titrino plus
5 Operation
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/off.
START Start a method run or a manual function.
5.2.2 Structure of the dialog windows
870 KF Titrino plus
The current dialog title is displayed on the left-hand side of the title line. The
current status of the system is displayed in the upper right-hand corner.
ready The instrument is in normal state.
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5.2 Fundamentals of operation
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].
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.
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Example: System settings
Use the [BACK] key to return to the next higher level.
5.2.4 Entering text and numbers
In the editing dialog for text or numerical input you can select the individual
characters with the arrow keys. Use [OK] to apply the character in the input
field. The following functions are available:
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5 Operation
Editing function Description
Accept
Cancel
Delete
[BACK]
The modification is applied and the editing dialog
is exited.
The editing dialog is exited without applying the
modification.
The contents of the input field is deleted completely.
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.
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 71.
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].
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5.3 Methods
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:
KFT Ipol Method with adjustable polarization current.
Titer Ipol Titer determination with adjustable polarization
Blank Ipol Blank value determination with adjustable polari-
KFT Ipol–Blank Method with adjustable polarization current.
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The blank value is not taken into account for the
calculation.
current.
zation current.
KFT Upol Method with adjustable polarization voltage.
Titer Upol Titer determination with adjustable polarization
Blank Upol Blank value determination with adjustable polari-
KFT Upol–Blank Method with adjustable polarization voltage.
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 blank value is taken into account for the calculation.
The blank value is not taken into account for the
calculation.
voltage.
zation voltage.
The blank value is taken into account for the calculation.
￭￭￭￭￭￭￭￭
20
The method table with the stored templates opens:
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2
Select a method
￭ Select the desired method.
3
Load the method
￭ In the function bar, select Load and press [OK].
The method is now loaded and is displayed in the main dialog under
Method.
5.3.3 Saving a method
If the method parameters are changed, then these will be saved automatically. It is not possible to save a method under a different name.
5 Operation
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].
The method table with the stored templates opens:
Note
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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
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).
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You can also send the sample size and the unit from a connected balance
in any case. The sample identification and the method can be additionally
sent with some balances (see Chapter 10.3, page 70).
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
Sample identification.
Input
Default value
max. 10 characters
empty
ID2
￭￭￭￭￭￭￭￭
22
Sample identification.
Input
Default value
max. 10 characters
empty
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Sample size
5 Operation
Sample size.
Range
Default value
–999999999 ... 9999999999
1.0
Unit
Unit of sample size.
Selection
Default value
g | mg | µg | mL | µL | pieces | User-defined
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 time of determination start
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 inquiry is requisite for reweighing.
The corresponding parameters must be switched on under Start condi-
tions for this purpose. If the Hold at request parameter is switched on,
then the run will be paused and must be continued with [START] after the
sample data has been entered. If the parameter Hold at request is switched
off, 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. Consult the user manual
for the balance for this purpose.
The following instructions describe how to enter the sample size on the 870
KF Titrino plus.
1
Load the method
￭ See Chapter Loading a method, Page 20.
2
Start conditioning
￭ Press [START].
Conditioning begins. Conditioning not OK is displayed until the end-
point 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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￭￭￭￭￭￭￭￭
24
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
Add the 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.
￭ When Conditioning OK is displayed, press [START].
Conditioning is stopped. The request for adding the sample will be
displayed for 8 s.
The sample should be added during this time.
5 Operation
￭ Add the sample.
Afterward, the request for the sample size appears:
4
Enter the sample size
￭ Press [OK].
The editing dialog opens.
￭ Enter the sample size and apply with Accept or [BACK].
5
Start 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
Cancel 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
Display the main dialog
￭ Press [BACK].
The main dialog is displayed. The determination continues to run in the
background.
2
Edit the sample data
￭ Edit the sample data and accept with Accept or [BACK].
3
Display 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 the editing dialog is opened (e.g. of
the sample size), then this will be closed automatically and the result 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 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 e.g. 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
Display the main dialog
￭ Press [BACK].
The main dialog is displayed. The determination continues to run in the
background.
2
Open the main menu
￭ Select Menu and press [OK].
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
3
Edit the method parameters
￭ Select the menu item Parameters and press [OK].
￭ Change the desired parameters accordingly.
4
Display 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
Recalc
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 Recalc 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.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
Note
Recalculation cannot be undone.
Note
Details
Reset
This function is visible only if statistics has been switched on.
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 was calculated is displayed in
parentheses. There are three of these in this example. The Statistics line
shows how many determinations have already been carried out and how
many determinations are to carried out in total. All three determinations
were carried out in this example.
Display additional data.
Delete all statistical data.
Increase
￭￭￭￭￭￭￭￭
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 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
In case that, for example, a determination was faulty and had to be removed
from the statistics, an additional sample can be added to a determination
series with the Increase function. The second number in the Statistics line
will be increased automatically by one.
5.9 Printing a report manually
Menu ▶ Print reports
To print a report manually, proceed as follows:
1
Open 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
Open the print dialog
￭ Select the menu item Print reports and press [OK].
The dialog window with the available reports opens:
3
Select a 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, sam-
ple 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 when there are multiple determinations. The
individual determinations with the respective sample size will be printed out for each result, along
with the mean value and the absolute and the relative standard deviation.
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5 Operation
Report as in
method
PC/LIMS Machine-readable report with all of the data for a
5.10 Manual Control
Menu ▶ Manual control
The following functions are available in the manual control:
￭ Dosing
￭ Stirring
The reports that are defined in the method will be
printed out.
determination. This report can be saved as a TXT
file on a connected USB stick or sent to a terminal
program or to a LIMS via an RS-232 interface. The
definition is made in the system settings (see "PC/
LIMS report", page 46).
5.10.1 Dosing
The available subfunctions are listed for each function in the function bar.
Note
The Stirrer function can only be selected if a stirrer is connected.
The following dosing functions are available in the manual control:
Prepare buret unit
(PREP)
Continuous dosing
Rinse the cylinder and tubings of the buret unit
(see Chapter 10.1.2, page 69).
Dose while the [START] key is pressed.
(DOS)
Dose fixed volume
Dose a specified volume.
(ADD)
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5.10 Manual Control
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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.
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 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 rate should be decreased for viscous liquids.
￭ The maximum dosing and filling rate depends on the cylinder
volume (see Chapter 10.1.1, page 69) .
￭ Enter the dosing rate.
￭ Enter the filling rate.
4
Start dosing
￭ Press [START].
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5.10 Manual Control
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The status changes to busy, the dosed volume is displayed. When a
cylinder volume has been added, 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 rate should be decreased for viscous liquids.
￭ The maximum dosing and filling rate depends on the cylinder
volume (see Chapter 10.1.1, page 69) .
￭ 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 a
cylinder volume has been added, 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
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.
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5.10 Manual Control
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2
Set 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 the stirrer is viewed from above, this means:
– "+": counterclockwise rotation
– "–": clockwise rotation
3
Switch 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
Switch off the stirrer
￭ In the function bar, select Off and press [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.
6 System settings
Instrument name
Serial number
Program version
Time
Input
Default value
An instrument name for the report can be entered here. This parameter will
only be printed if a designation has been defined.
Input
Default value
Serial number of the instrument. This is printed as a component of the
instrument identification in the report header.
Version number of the instrument software. This is printed as a component
of the instrument identification in the report header.
Current time. Only valid numbers can be entered.
Format: hh:mm:ss
max. 12 characters
empty
max. 10 characters
empty
Date
Language
870 KF Titrino plus
Current date. Only valid numbers can be entered.
Format: YYYY:MM:DD
Setting the dialog language. In addition to English a further language can
be selected.
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6.1 Basic settings
Dialog type
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Note
A second language must be installed in advance in order to be able to
select it here. The installation may only be carried out by competent personnel.
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 does not take effect until the main menu is exited.
The limitation of the dialog has the following effects:
￭ 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 is activated for routine operations, then the expert
dialog cannot be switched on during running operations. 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 at the time the instrument is
started. 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
Default value
Expert | Routine
Expert
￭￭￭￭￭￭￭￭
40
Expert
Complete dialog.
Routine
Limited dialog for routine operations.
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Contrast
6 System settings
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.
Beep
Range
Default value
150 ... 240
212
Note
Alternatively, the contrast can also be modified in the following manner:
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 switched on, then a short beep will be heard in the following cases:
￭ When a key is pressed.
￭ At the end of the determination.
￭ If the system has been conditioned uninterruptedly for 10 s.
Selection
Default value
on | off
on
PREP warning
870 KF Titrino plus
If this parameter is switched on, then the recommendation to carry out the
PREP (preparing) function will be displayed in the following cases:
￭ After the instrument has been switched on.
￭ Each time a buret unit has been attached.
This function causes all tubings and the cylinder to be rinsed (see Chapter
10.1.2, page 69).
Selection
Default value
on | off
on
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6.2 Managing solutions
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.
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.
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Edit
New
Delete
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 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.
6 System settings
Type
Cylinder volume
Concentration
Concentration unit
Input
Default value
max. 24 characters
empty
The model of the buret unit is displayed.
Cylinder volume of the buret unit in mL. The cylinder volume is automatically
read out with intelligent buret units.
Selection
Default value
1 | 5 | 10 | 20 | 50
20
Concentration of the solution.
Range
Default value
–999999999 ... 9999999999
1.000
Units used to specify the concentration.
Titer
Titer unit
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.
Range
Default value
–999999999 ... 9999999999
1.000
Unit of the titer.
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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6.3 File management
Date titer det.
Monitoring
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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.
Switching the titer monitoring on and off.
Selection
Default value
Time interval
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.
Range
Default value
6.3 File management
Menu ▶ System ▶ File management
Note
This menu item is visible only when a USB stick has been connected as an
external storage medium.
on | off
off
1 ... 999 d
999 d
Import
Delete
Backup
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44
Methods can be imported and deleted from a USB stick in this dialog. Only
methods located in the Files directory are displayed in the list (see "Directory
structure on the USB stick", page 45).
A backup copy can be made of the system (all data and settings). Similarly,
an existing backup copy can be stored.
Import the selected method.
Delete the selected method.
Create a backup copy of all data and settings on the USB stick.
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Restore
6 System settings
Note
Only one backup copy can be created on the same USB stick.
If a backup copy has already been stored on the stick, then it will be
overwritten when this function is carried out again.
Load the backup copy from a connected USB stick.
Directory structure on the USB stick
A directory with the instrument number is generated on the USB stick. The
structure within the directory appears as follows:
Figure 14 Directory structure on the USB stick
Backup All of the files of the backup copy are stored in this
directory. The directory will be created the first
time a backup copy is saved.
Files Exported methods will be stored in this directory.
The directory will be created the first time a
method is exported.
Only methods being located in this directory can
be imported.
pc_lims_report PC/LIMS reports are stored in this directory as a
TXT file. The directory will be created the first time
a PC/LIMS report is printed out.
870 KF Titrino plus
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6.4 Configuring external devices
6.4 Configuring external devices
Menu ▶ System ▶ External devices
PC/LIMS report
Specification of the memory location for the PC/LIMS report. The PC/LIMS
report is a machine-readable report with all of the data important for a
determination. It can be saved as follows:
￭ as a TXT file on a USB stick.
￭ to a LIMS via an RS-232 interface. The 6.2148.030 RS-232/USB Box is
required for this purpose.
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Printer
Selection
Default value
COM2 | USB Stick
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 set-
tings", page 48).
USB Stick
The report will be saved as a TXT file on the USB stick in the folder
pc_lims_report.
If a printer is connected, then the printer type needs to be defined here in
order for the reports to be printed out correctly.
The printers that have the designation ESC-POS are so-called POS printers
(point-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
Graphics width
Keyboard layout
￭￭￭￭￭￭￭￭
46
Adjust the width of the curve to be printed out to the paper width of the
printer to be used. The standard value depends on the selected printer. The
height of the curve is 2/3 of the width.
Range
100 ... 3000 Pixels
A commercially available USB keyboard can be connected to make it easier
to enter text and numbers. Define the country-specific keyboard layout here.
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6 System settings
Balance
Selection
English US | French FR | German CH | German
DE | Spanish ES
Default value
English US
If a balance has been connected, then the balance type needs to be defined
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 Type of balance
AND AND
Mettler AB, AG, AM, PM,
Mettler
XP, XS
Mettler AT Mettler AT
Mettler AX, MX, UMX, PG,
Mettler AX
AB-S
Baud rate
Data bits
Ohaus Voyager, Explorer,
Ohaus
Analytical Plus
Precisa Precisa
Sartorius Sartorius
Shimadzu BX, BW Shimadzu
Editing the COM1 settings
Under COM1 settings the interface parameters for the connected balance
are set.
Transfer rate in characters per second.
Selection
1200 | 2400 | 4800 | 9600 | 19200 | 38400 |
57600 | 115200
Default value
9600
Number of data bits.
Selection
Default value
7 | 8
8
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6.5 Instrument diagnosis
Stop bits
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Number of stop bits.
Parity
Handshake
Selection
Default value
Type of parity testing.
Selection
Default value
Type of data transfer protocol.
Selection
Default value
Note
In case of communication problems, try the software handshake (software).
Editing the COM2 settings
Under COM2 settings the interface parameters for devices connected to
the RS-232/2 connector of the RS-232 USB Box are set (e.g. PC). The
parameters and input ranges are the same as for the COM1 interface.
1 | 2
1
even | none | odd
none
hardware | software | none
hardware
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 stick. The
corresponding file must be saved on the USB stick 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 whereas
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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 whereas
xxxx =
YY =
Version number
Language, e.g. DE (German), FR (French), ES (Spanish)
Loading a file
Proceed as follows:
1
Connect the USB stick
￭ Plug in the USB stick with the 6.2151.100 adapter (USB MINI (OTG)
- USB A) at the USB port on the instrument.
￭ Switch on the instrument.
2
Open the update dialog
￭ Under Menu ▶ System ▶ Diagnosis, select the menu item Soft-
ware update.
￭ Press [OK].
3
Open the file selection
￭ Press [OK].
The selection list with the program and language files available on the
USB stick is opened.
4
Select the file
￭ Select the required file with the arrow keys.
￭ Press [OK].
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6.5 Instrument diagnosis
5
Start the update
￭ Press [START].
The update process is started, it runs automatically. At the end of the
process, the instrument is automatically switched off and then 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 agent 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
Default value
Conditioning OK will be displayed as soon as this volume drift has been
reached and the titration can be started.
Range
Default value
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
Default value
auto
The value of the current volume drift is applied automatically at the start
of the titration.
on | off
on
1 ... 999 µL/min
20 µL/min
auto | manual | off
off
870 KF Titrino plus
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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7.1 Karl Fischer Titrations (KFT)
Drift value
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This parameter is visible only when Drift correction = manual.
Volume drift for manual drift correction.
Cond. stop volume
Cond. stop time
Range
Default value
0.0 ... 99.9 µL/min
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.
Range
Default value
Selection
0.00000 ... 9999.99 mL
20.0000 mL
off
Maximum permissible time over which conditioning may take place. Conditioning is stopped when the specified time has elapsed.
Range
Selection
Default value
0 ... 999999 s
off
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.
Range
Default value
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 69).
Range
Selection
Default value
0.00000 ... 9999.99 mL
0.00000 mL
0.01 ... 166.00 mL/min
max.
max.
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Pause
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.
Request sample ID
Request sample size
Request sample unit
Range
Default value
0 ... 999999 s
0 s
Selection of the sample identification that is queried in the method run.
Selection
Default value
off | ID1 | ID2 | ID1&ID2
off
If this parameter is switched on, then the value for the sample size will be
queried.
Selection
Default value
on | off
on
For the methods "Blank Ipol" and "Blank Upol" the
default value is off.
If this parameter is switched on, then the unit for the sample size will be
queried.
Selection
Default value
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
Default value
7.1.3 Control parameters
Menu ▶ Parameters ▶ Control parameters
Under Control parameters, the control parameters for the endpoint are
defined.
Endpoint at
Measured value for the endpoint.
on | off
off
on | off
on
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7.1 Karl Fischer Titrations (KFT)
Titration rate
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Measuring mode Ipol:
Range
Default value
Selection
–1250.0 ... 1250.0 mV
250.0 mV
off
Measuring mode Upol:
Range
Default value
Selection
–125.00 ... 125.00 µA
25.00 µA
off
Three predefined sets of parameters can be selected for the titration rate.
Dynamics
Selection
Default value
slow | optimal | fast | user
optimal
slow
For samples with a low water content or samples which release their
moisture only slowly.
optimal
For all standard titrations. The parameters have been optimized for the
most frequent applications.
fast
For uncritical samples with high water content.
user
The individual titration parameters can be modified.
The settings of the individual titration rates are listed in table 1, page 55.
This parameter is visible only when Titration rate = user.
This parameter defines the control range before the specified endpoint.
Individual volume steps are dosed in the control range, the dosing is finely
controlled. The closer the endpoint, the slower the dosing until the 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.
￭￭￭￭￭￭￭￭
54
Measuring mode Ipol:
Range
Default value
Selection
Measuring mode Upol:
Range
Default value
0.1 ... 1250.0 mV
100.0 mV
off
0.01 ... 125.00 µA
10.00 µA
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7 Parameters
Max. rate
Min. increment
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
69) .
Range
Selection
Default value
0.01 ... 166.00 mL/min
max.
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.
Range
Selection
Default value
0.1 ... 99.90 µL
min.
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.
Selection
Default value
drift | time | rel. drift | off
drift
870 KF Titrino plus
drift
The titration is stopped when the stop drift has been reached.
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7.1 Karl Fischer Titrations (KFT)
Stop drift
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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.
Range
Default value
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.
Range
Default value
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.
Range
Default value
7.1.4 Titration parameters
Menu ▶ Parameters ▶ Titration parameters
1 ... 999 µL/min
20 µL/min
0 ... 999 s
10 s
1 ... 999 µL/min
10 µL/min
Solution
￭￭￭￭￭￭￭￭
56
Under Titration parameters, the parameters influencing the sequence of
the entire titration are defined.
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 Sys-
tem ▶ Solutions.
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7 Parameters
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
Default value
Selection of configured solution | not defined
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.
Range
Default value
–125 ... 125 µA (Increment: 1)
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.
Range
Default value
–1250 ... 1250 mV (Increment: 10)
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
Stirring rate
870 KF Titrino plus
Selection
Default value
on | off
off
When this parameter is switched on, then the stirrer is switched on at the
start of the determination.
Selection
Default value
on | off
on
Setting the stirring rate. It can be set in steps of –15 to +15. The default
setting 8 corresponds to 1000 U/min. The formula for calculating the rota-
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7.1 Karl Fischer Titrations (KFT)
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tional speed is specified in chapter 10.2, page 69. 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
Range
Default value
Temperature
Manually entered titration temperature.
Range
Default value
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.
Range
Default value
7.1.5 Stop conditions
–15 ... 15
8
–20.0 ... 150.0 °C
25.0 °C
0 ... 999999 s
0 s
Stop volume
Stop time
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 criterion", page
55) is not fulfilled.
The titration is stopped when the specified volume has been dosed since the
start of the titration. This volume should be adjusted to the size of the titration vessel in order to prevent the contents from running over.
Range
Default value
Selection
0.00000 ... 9999.99 mL
100.000 mL
off
The titration is stopped when the specified time has elapsed following the
termination of the start conditions.
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7 Parameters
Range
Selection
Default value
0 ... 999999 s
off
off
Filling rate
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
69).
Range
Selection
Default value
0.01 ... 166.00 mL/min
max.
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)
Decimal places
Result unit
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.
Range
Default value
–999999999 ... 9999999999
1.0
Number of decimal places used to display the result.
Range
Default value
0 ... 5
2
The result unit is displayed and saved together with the result. It cannot be
modified.
Selection
mL
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7.1 Karl Fischer Titrations (KFT)
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:
Table 2 Conversion table
Standard used Sample size in…Factor (FCT)
Water Standard 10 mg/g g Water content in mg/g
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(see certificate)
Factor (FCT)
Decimal places
Result unit
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.
Range
Default value
–999999999 ... 9999999999
1.0
Number of decimal places used to display the result.
Range
Default value
0 ... 5
4
The result unit is displayed and saved together with the result.
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60
Selection
Default value
% | ppm | mg/mL | g | mg | mL | mg/piece | User-
defined
mg/mL
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7 Parameters
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 Conversion table
Result unit Sample size in…Factor (FCT) Divisor (DIV)
% g 0.1 1
% mg 100 1
% mL 0.1 Density of the
sample in g/mL
ppm g 1000 1
ppm mL 1000 Density of the
sample in g/mL
mg/mL g Density of the
1
sample in g/mL
mg/mL mL 1 1
Factor (FCT)
870 KF Titrino plus
mg/piece pieces 1 1
Conversion factor, see table above.
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Divisor (DIV)
Titer
Range
Default value
–999999999 ... 9999999999
0.1
Conversion factor, see table above.
Range
Default value
–999999999 ... 9999999999
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.
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.
Blank (CV01/2)
Decimal places
Result unit
Range
Default value
0.00000001 ... 9999999999
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.
Range
Default value
–999999999 ... 9999999999 mL
0.0 mL
Number of decimal places used to display the result.
Range
Default value
0 ... 5
2
The result unit is displayed and saved together with the result.
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62
Selection
Default value
% | ppm | mg/mL | g | mg | mL | mg/piece | User-
defined
%
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7.1.9 Statistics
Statistics
7 Parameters
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.
If this funtion is switched on, then statistics calculations will be carried out
for all of the defined results.
Number of samples
7.1.10 Reports
Selection
Default value
on | off
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).
Range
Default value
2 ... 20
3
Menu ▶ Parameters ▶ Reports
The reports that will be printed out automatically in connection with a
determination are defined under Reports.
Results
Curve
870 KF Titrino plus
The result report contains the calculated results, equivalence points and
endpoints, sample data, etc.
Selection
Default value
on | off
off
Curve report. The width of the curve is defined in the system settings (see
"Graphics width", page 46).
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7.1 Karl Fischer Titrations (KFT)
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Calculations/Statistics
Measuring point list
Parameters
Selection
Default value
on | off
off
Output of the calculation formulas for the individual results. The results are
printed with the maximum resolution. This makes recalculation with an
external program possible. The following data is printed out in addition
when statistics is switched on:
￭ Result and sample size of the individual determinations
￭ Mean value as well as absolute and relative standard deviation
Selection
Default value
on | off
off
Output of the measuring point list.
Selection
Default value
on | off
off
All of the parameters of the current method are printed out with the parameter report.
PC/LIMS
Selection
Default value
on | off
off
The PC/LIMS report is a machine-readable report with all of the data important for a determination. The PC/LIMS report can be saved as a TXT file on
a USB storage medium or sent via an RS-232 interface to a LIMS. The output
location is defined in the system settings (see "PC/LIMS report", page 46).
The file name of the TXT file is constructed as follows: PC_LIMS_Report-ID1-
YYYYMMDD-hhmmss.txt.
Selection
Default value
on | off
off
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8 Handling and maintenance
8 Handling and maintenance
8.1 Quality Management and validation with Metrohm
Quality Management
Metrohm offers you comprehensive support in implementing quality management measures for instruments and software. Further information on
this can be found in the brochure «Quality Management with
Metrohm» available from your local Metrohm agent.
Validation
Please contact your local Metrohm agent for support in validating instruments and software. Here you can also obtain validation documentation to
provide help for carrying out the Installation Qualification (IQ) and the
Operational Qualification (OQ). IQ and OQ are also offered as a service
by the Metrohm agents. In addition, various application bulletins are also
available on the subject, which also contain Standard Operating Proce-
dures (SOP) for testing analytical measuring instruments for reproducibility
and correctness.
Maintenance
Electronic and mechanical functional groups in Metrohm instruments can
and should be checked as part of regular maintenance by specialist personnel from Metrohm. Please ask your local Metrohm agent regarding the
precise terms and conditions involved in concluding a corresponding maintenance agreement.
Note
You can find information on the subjects of quality management, validation and maintenance as well as an overview of the documents currently
available at www.metrohm.com/com/ under Support.
870 KF Titrino plus
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9.1 Karl Fischer titration
9 Troubleshooting
9.1 Karl Fischer titration
Problem Cause Remedy
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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.
The sample releases water very
slowly.
A side reaction is taking place.
The pH value is not in the optimum range anymore.
The titration cell is leaking.
￭ Check seals and septum. If necessary,
replace.
￭ Replace molecular sieve.
￭ Adjust the method.
￭ Add solubilizer.
￭ Increase the temperature (possibly
using a KF oven).
￭ See technical literature.
￭ Use special reagents.
￭ Adjust the method (increase/decrease
the temperature, external extraction).
￭ See technical literature.
Add buffer, see technical literature.
￭ 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. increment) (see Chapter 7.1.3,
page 53).
Adjust the control parameters (see Chap-
ter 7.1.3, page 53):
￭ Increase the stop drift.
￭ Select a short delay time.
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Problem Cause Remedy
9 Troubleshooting
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
working 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 endpoint is
reached too quickly.
The electrode has a short cir-
cuit.
The dosing rate outside the
control range is too high.
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).
The titration times with
volumetric titration are
constantly longer.
With two-component
reagents the buffer capacity of
the solvent can be exhausted.
Replace the working medium.
9.2 Miscellaneous
Problem Cause Remedy
No report is printed.
The printer is not recognized by
the instrument.
￭ Switch the 870 KF Titrino plus off and
on again.
￭ Use a hub on the USB connector and
connect the printer to the hub.
870 KF Titrino plus
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9.2 Miscellaneous
Problem Cause Remedy
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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.
The keyboard or the mouse is
not compatible.
The contrast is set incorrectly.
The automatic calibration of
the balance is switched on.
The USB stick is no longer connected.
Use a printer which fulfills the required
specifications (see Chapter 10.4.4, page
73).
￭ Switch the 870 KF Titrino plus off and
on again.
￭ Use a hub on the USB connector and
connect the keyboard or mouse to the
hub.
Use a model which fulfills the required
specifications (see Chapter 10.4, page
71).
Adjust the contrast correctly (see Chapter
6.1, page 39).
Switch off the automatic calibration.
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 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
10 Appendix
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.
10.2 Stirring rate
The stirring rate can be adjusted in steps of –15 to +15.
The approximate rotational speed can be calculated with the following formula:
Rotational speed/min (r/min) = 125 · stirring rate
Example:
870 KF Titrino plus
Stirring rate set: 8
Rotational speed in rpm = 125 · 8 = 1000
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10.3 Balance
2000
1500
1000
500
-15 -10 -5 0 5 10 15
r/min
10.3 Balance
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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 reweighing), 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.
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
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10.4 USB devices
Note
USB peripheral devices that are to be connected directly must support the
USB 1.0/1.1 (Full Speed) or USB 2.0 (High Speed) standard. The maximum
data transfer rate is however in any case 12 MBit/s.
Keyboards, PC mice and barcode readers are so-called HID devices
(Human Interface Device) and can be connected via a USB hub only.
Printers should also be connected via a USB hub. Depending on the manufacturer or printer type a direct connection is however possible.
10.4.1 Numerical USB keypad 6.2147.000
The key [Num Lock] must be pressed for navigating in the dialog. Then the
arrow keys are effective.
10 Appendix
The respective editing dialog must be opened for the number input.
Table 4 Keyboard assignment
Key of the 870 KF Titrino plus
or function in the editing dialog
[BACK] [Home]
[⇧] [⇩] [↑] [↓]
[⇦] [⇨] [←] [→]
[OK] [Enter]
Delete [Del]
Accept [Home]
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.
Key on the numerical USB keypad
[BS] (backspace)
870 KF Titrino plus
The respective editing dialog must be opened for text and number inputs.
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10.4 USB devices
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Table 5 Keyboard assignment
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)
Delete [Delete]
Cancel [Strg] + [Q]
Accept [Esc]
10.4.3 PC mouse
Note
The lettering of the USB keyboard can 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]
[BACK]
[⇧] [⇩] [⇦] [⇨]
Left mouse button
Right mouse button
Mouse movement vertical/horizon-
tal
[⇧] [⇩]
Scroll wheel vertical
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10.4.4 Printer
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
10 Appendix
In very rare instances, it could happen that a faulty file system (e.g. because
of a program crash) will lead to an impairment of program functioning. The
internal file system needs to 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 copy 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.
Proceed as follows for system initialization:
1
Switch off the instrument
￭ Keep the red [STOP] key pressed down for at least 3 s.
870 KF Titrino plus
A progress bar is displayed. If the key is released during this time, then
the instrument will not be switched off.
2
Switch on the instrument
￭ Keep the red [STOP] key pressed down for approx. 10 s.
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10.6 Remote interface
1
5
6
9
5
1
9
6
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The dialog for confirmation of the initialization is displayed for 8 s. The
initialization must be confirmed during this time.
3
Confirm the initialization
Note
If the query is not confirmed within 8 s, then the procedure will be
interrupted.
￭ Press [BACK] twice.
Initialization is started. The process takes approximately 80 s. The
instrument will be automatically restarted after successful initialization.
10.6 Remote interface
10.6.1 Pin assignment of the remote interface
Figure 16 Pin assignment of remote socket and plug
The above figure of the pin assignment applies for all Metrohm instruments
with 9-pin D-Sub remote connectors.
Table 7 Inputs and outputs of the remote interface
Pin No. Assigment Function
1 Output 0 Ready/EOD
2 Output 1 -
3 Output 2 Titration
4 Output 3 Cond OK
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+5 V
t
p
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
Pin No. Assigment Function
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
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
= 40 V
870 KF Titrino plus
Figure 17 Remote status diagram
EOD = End of Determination
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10.7 Remote control via an RS-232 connection
6.2134.040
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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 devices. The RS-232
remote control only works via the RS-232/2 connector. The RS-232/1 connector is provided for a connection to a balance. Connect the RS-232/2
connector of the RS-232/USB Box to a serial interface (COM1 or COM2,
designated with the symbol IOIO) of a PC. Use a 6.2134.040 connection
cable.
Figure 18 Connecting the RS-232/USB Box to the PC
Interface parameters
We recommend the following parameters for the RS-232 interface COM2:
￭ Baud rate: 19200
￭ Data bits: 8
￭ Stop bits: 1
￭ Parity: none
￭ Handshake: software
On the 870 KF Titrino plus the interface parameters are set under
Menu ▶ System ▶ External devices ▶ COM2 settings.
Transfer protocol
The data communication is synchronous. On each command there is an
answer by the instrument.
A command must be sent to the instrument with the control character CR
LF as terminator. The answers of the instrument will also be transferred with
CR LF as terminator.
The instrument does not send spontaneous messages.
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10.7.1 Commands and variables
Command Function Comment
10 Appendix
$G
$S
$H
$D
$A
Start/Continue
Corresponds to the key [START] or [Con-
tinue]
Stop
Corresponds to the key [STOP]
Hold Hold the method run
Scan instrument status Answers: 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 answer of the
status scan displays the corresponding
message number. Example:
Busy;010-119
= "Check buret unit"
The message can be quit with [OK] or
[Cancel], see below.
Quit message Confirm the message on the instrument
with [OK]
A mandatory status scan providing the
message number must take place immediately before quitting the message, see
above.
$A(OK), $A(CANCEL)
$A(YES), $A(NO)
$L(
method name
$Q(
variable
)
)
Quit message
Quit message
Load method The method name has to be known and
Request variable value Examples for variables: EP1, R1, C00.
Variable Comment
C00
EP1
CI#
R1
Sample size
Volume of the endpoint EP1
Sample identification (# = 1…2)
Result
Confirm the message with [OK] or [Can-
cel]
Confirm the message with [Yes] or [No]
unique.
List of variables, see below
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10.7 Remote control via an RS-232 connection
Variable Comment
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CV01
CV02
SMN1
TITER
CONC
FCT
DIV
MCV
EM1
ED1
MSV
DD
Answer of the instrument
Common variable (blank value at KFT Ipol)
Common variable (blank value at KFT Upol)
Mean value of result R#
Titer of selected solution
Concentration of selected solution
Factor
Divisor
End volume, i.e. total dosed volume at the end of the titration
Measured value of the endpoint EP1
Time at the endpoint EP1
Start volume
Duration of the entire determination
The values of the variables are only available after the end of a determination
(in the status 'ready').
Comment
OK
E1
E2
E3
Command executed
Method not found
Invalid variable
Invalid command
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11 Technical specifications
11.1 Measuring inputs
11.1.1 Polarizer
A measuring input (Pol.) for polarizable electrodes.
11 Technical specifications
Measuring mode
Ipol
Polarization current
Measuring
range
Resolution
Measuring
accuracy
Measuring mode
Upol
Polarization
voltage
Measuring
range
Resolution
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
–1200…1200 mV
0.1 mV
±0.2 mV
(±1 digit, without sensor error, under reference conditions)
Determination with adjustable polarization voltage.
–1200…1200 mV (increment: 10 mV)
–1250…–1210 mV / +1210…+1250 mV: non-guaranteed values,
dependent on reference voltage +2.5 V
–120…120 µA
0.01 µA
–
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11.2 Dosing drive
11.2 Dosing drive
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Resolution
10000 steps per cylinder volume
Exchange unit
Cylinder volume
Accuracy
￭ 1 mL
￭ 5 mL
￭ 10 mL
￭ 20 mL
￭ 50 mL
Fulfills ISO/DIN standard 8655-3
11.3 Interfaces
USB (OTG) connector
MSB connector
Remote connector
For connecting USB devices.
For connecting a stirrer.
For connecting instruments with a remote interface.
11.4 Mains connection
Voltage
Frequency
Power consump-
100…240 V
50…60 Hz
45 W
tion
Fuse
2 × 2.0 ATH, electronic overload protection
11.5 Safety specification
Design and testing
Safety instructions
According to EN/IEC/UL 61010-1, CSA-C22.2 No. 61010-1
Protection class I, degree of protection IP40
The documentation contains safety instructions which have to be followed by the user in order to ensure safe operation of the instrument.
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11.6 Electromagnetic compatibility (EMC)
11 Technical specifications
Emission
Immunity
Standards fulfilled:
￭ EN/IEC 61326-1
￭ EN/IEC 61000-6-3
￭ EN 55022 / CISPR 22
Standards fulfilled:
￭ 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
￭ NAMUR
11.7 Ambient temperature
Nominal function
range
+5…+45 °C
(at a maximum of 85 % humidity)
Storage
Transport
–20…+60 °C
–40…+60 °C
11.8 Reference conditions
Ambient temperature
Rel. humidity
Operating temperature status
Validity of the data
+25 °C ± 3 °C
≤ 60 %
Instrument in operation at least 30 minutes
After adjustment
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11.9 Dimensions
11.9 Dimensions
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Material of housing
Material of display
cover
Width
Height
Depth
Weight
Polybutylene terephthalate (PBT)
Glass
142 mm
164 mm
310 mm
2950 g
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12 Conformity and warranty
12.1 Declaration of Conformity
This is to certify the conformity to the standard specifications for electrical
appliances and accessories, as well as to the standard specifications for
security and to system validation issued by the manufacturing company.
12 Conformity and warranty
Name of commodity
Electromagnetic compatibility
Safety specifications
870 KF Titrino plus
Titrator for volumetric water determination according to Karl Fischer.
This instrument has been built and has undergone final type testing according to the standards:
Emission: EN/IEC 61326-1: 2006, EN/IEC 61000-6-3: 2004,
EN 55022 / CISPR 22: 2006
Immunity: EN/IEC 61326-1: 2006, EN/IEC 61000-6-2: 2005,
EN/IEC 61000-4-2: 2001,
EN/IEC 61000-4-3: 2002,
EN/IEC 61000-4-4: 2004,
EN/IEC 61000-4-5: 2001,
EN/IEC 61000-4-6: 2001,
EN/IEC 61000-4-11: 2004,
EN/IEC 61000-4-14: 2004, NAMUR: 2004
EN/IEC 61010-1: 2001, UL 61010-1: 2004,
CSA-C22.2 No. 61010-1: 2004, protection class I
Manufacturer
870 KF Titrino plus
This instrument meets the requirements of the CE mark as contained in the
EU directives 2006/95/EC (LVD), 2004/108/EC (EMC). It fulfils the following
specifications:
EN 61326-1 Electrical equipment for measurement, control and
laboratory use – EMC requirements
EN 61010-1 Safety requirements for electrical equipment for
measurement, control and laboratory use
This instrument meets the requirements of the ETL Listed Mark for the North
American market. It conforms to the electrical safety standards UL 61010-1
and CSA-C22.2 No. 61010-1. This product is listed in Intertek’s Directory of
Listed Products.
Metrohm Ltd., CH-9101 Herisau/Switzerland
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12.2 Quality Management Principles
Metrohm Ltd. is holder of the SQS certificate ISO 9001:2000 Quality management system for development, production and sales of instruments and
accessories for ion analysis.
Herisau, 16 January, 2009
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D. Strohm
Vice President, Head of R&D
12.2 Quality Management Principles
Metrohm Ltd. holds the ISO 9001:2000 Certificate, registration number
10872-02, issued by SQS (Swiss Association for Quality and Management
Systems). Internal and external audits are carried out periodically to assure
that the standards defined by Metrohm’s QM Manual are maintained.
The steps involved in the design, manufacture and servicing of instruments
are fully documented and the resulting reports are archived for ten years.
The development of software for PCs and instruments is also duly documented and the documents and source codes are archived. Both remain the
possession of Metrohm. A non-disclosure agreement may be asked to be
provided by those requiring access to them.
The implementation of the ISO 9001:2000 quality management system is
described in Metrohm’s QM Manual, which comprises detailed instructions
on the following fields of activity:
Instrument development
The organization of the instrument design, its planning and the intermediate
controls are fully documented and traceable. Laboratory testing accompanies all phases of instrument development.
A. Dellenbach
Head of Quality Management
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84
Software development
Software development occurs in terms of the software life cycle. Tests are
performed to detect programming errors and to assess the program’s functionality in a laboratory environment.
Components
All components used in the Metrohm instruments have to satisfy the quality
standards that are defined and implemented for our products. Suppliers of
components are audited by Metrohm as the need arises.
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Manufacture
The measures put into practice in the production of our instruments guarantee a constant quality standard. Production planning and manufacturing
procedures, maintenance of production means and testing of components,
intermediate and finished products are prescribed.
Customer support and service
Customer support involves all phases of instrument acquisition and use by
the customer, i.e. consulting to define the adequate equipment for the analytical problem at hand, delivery of the equipment, user manuals, training,
after-sales service and processing of customer complaints. The Metrohm
service organization is equipped to support customers in implementing
standards such as GLP, GMP, ISO 900X, in performing Operational Qualification and Performance Verification of the system components or in carrying
out the System Validation for the quantitative determination of a substance
in a given matrix.
12.3 Warranty (guarantee)
12 Conformity and warranty
Metrohm guarantees that the deliveries and services it provides are free from
material, design or manufacturing errors. The warranty period is 36 months
from the day of delivery; for day and night operation it is 18 months. The
warranty remains valid on condition that the service is provided by an
authorized Metrohm service organization.
Glass breakage is excluded from the warranty for electrodes and other
glassware. The warranty for the accuracy corresponds to the technical specifications given in this manual. For components from third parties that make
up a considerable part of our instrument, the manufacturer's warranty provisions apply. Warranty claims cannot be pursued if the Customer has not
complied with the obligations to make payment on time.
During the warranty period Metrohm undertakes, at its own choice, to either
repair at its own premises, free of charge, any instruments that can be shown
to be faulty or to replace them. Transport costs are to the Customer's
account.
Faults arising from circumstances that are not the responsibility of Metrohm,
such as improper storage or improper use, etc. are expressly excluded from
the warranty.
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13.1 Scope of delivery
13 Accessories
Note
Subject to change without notice.
13.1 Scope of delivery
2.870.0010 870 KF Titrino plus
Qty. Order no. Description
1 1.870.0010 870 KF Titrino plus
1 6.0338.100 Double Pt-wire electrode
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):
–20 ... 70
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1 6.1244.040 Set of seals
870 KF Titrino plus
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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
13 Accessories
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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13.1 Scope of delivery
Qty. Order no. Description
2 6.1448.010 Septum 12 mm, 5 pieces
Set of 5 items.
Material: Silicone rubber
Height (mm): 2
Outer diameter (mm): 12
2 6.1903.020 Stirring bar / 16 mm
Stirring Bar with magnetic core, PTFE coated, length 16 mm
Material: PTFE
Outer diameter (mm): 4
Length (mm): 16
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2 6.1903.030 Stirring bar / 25 mm
Stirring Bar with magnetic core, PTFE coated, length 25 mm
Material: PTFE
Outer diameter (mm): 5
Length (mm): 25
1 6.2104.020 Electrode cable / 1 m / F
For connecting electrodes with Metrohm plug-in head G to Metrohm
instruments (socket F).
Length (m): 1
1 6.2147.000 Numerical USB keypad
Numerical USB keypad for Titrino plus, Dosimat plus, 862 Compact
Titrosampler and 869 Compact Sample Changer. Incl. USB Hub with
two connectors.
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Qty. Order no. Description
1 6.2151.100 Adapter USB MINI (OTG) - USB A
For connecting USB instruments.
1 6.2412.000 Glass weighing spoon
Used with 6.1414.030 Titration vessel lid or 6.1455.31X, 6.1464.32X,
6.1465.320 Titration vessels. For Karl Fischer water determinations.
Including protective tube.
Material: Glass
Length (mm): 120
13 Accessories
2 6.2730.010 Screw nipple
Made of PP. For 6.1448.010 Septum or for mounting 6.1403.040 Drying tube or 6.0338.100 Electrode in 6.1414.030 and 6.1414.040 KF
Titration vessel lids. Used for KF titrations.
Material: PP
Inner diameter (mm): 11.5
Length (mm): 23.5
1 6.2730.020 Septum stopper
With E.301.0041 O-ring. For 6.1448.010 Septum and 6.1414.030
Titration vessel lid. Used for KF applications.
Outer diameter (mm): 18
Length (mm): 30
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13.1 Scope of delivery
Qty. Order no. Description
3 6.2730.030 Stopper
Nipple and E.301.0043 O-ring included. For 6.1414.030 Titration vessel lid. Used with KF Titrators, VA Stands, VA Computrace and IC
Dilution technique.
Length (mm): 38
1 6.2739.010 Wrench
For exchange units.
Length (mm): 190
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1 6.2811.000 Molecular sieve
Molecular sieve. Bottle containing 250 g. Pore size: 0.3 nm. Without
moisture indicator. For Rancimats and Karl Fischer instruments.
1 6.2122.0x0 Mains cable with C13 line socket IEC-60320-
C13
Cable plug according to customer requirements.
Switzerland: Type SEV 12
6.2122.020
Germany, …: Type CEE(7), VII
6.2122.040
USA, …: Type NEMA/ASA
6.2122.070
1 8.870.8003EN Manual 870 KF Titrino plus
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870 KF Titrino plus
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