Metrohm 870KF User Manual
870 KF Titrino plus
Manual
8.870.8005EN
Metrohm AG
CH-9100 Herisau
Switzerland
Phone +41 71 353 85 85
Fax +41 71 353 89 01
info@metrohm.com
www.metrohm.com
870 KF Titrino plus
8.870.8005EN
Manual
04.2013 jb/ebe
Teachware
Metrohm AG
CH-9100 Herisau
teachware@metrohm.com
This documentation is protected by copyright. All rights reserved.
Although all the information given in this documentation has been
checked with great care, errors cannot be entirely excluded. Should you
notice any mistakes please send us your comments using the address
given above.
Documentation in additional languages can be found on
http://documents.metrohm.com.
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Table of contents
1 Introduction 1
1.1 Instrument description ......................................................... 1
1.1.1 Titration and measuring modes ................................................ 1
1.1.2 Connectors .............................................................................. 1
1.1.3 Intended use ........................................................................... 1
1.2 About the documentation ................................................... 2
1.2.1 Symbols and conventions ........................................................ 2
1.3 Safety instructions ................................................................ 3
1.3.1 General notes on safety ........................................................... 3
1.3.2 Electrical safety ........................................................................ 3
1.3.3 Tubing and capillary connections ............................................. 4
1.3.4 Flammable solvents and chemicals ........................................... 4
1.3.5 Recycling and disposal ............................................................. 4
2 Overview of the instrument 6
Table of contents
3 Water determination according to Karl Fischer (KFT) 8
4 Installation 9
4.1 Setting up the instrument .................................................... 9
4.1.1 Packaging ................................................................................ 9
4.1.2 Checks .................................................................................... 9
4.1.3 Location .................................................................................. 9
4.2 Connecting a sensor ............................................................. 9
4.3 Connecting a stirrer ............................................................ 10
4.4 Connecting a balance ......................................................... 11
4.5 Connecting a keyboard, printer and other USB devi-
ces ........................................................................................ 11
4.6 Connecting instruments to the remote connector .......... 14
4.7 Attaching the exchange unit ............................................. 15
5 Operation 16
5.1 Switching the instrument on and off ............................... 16
5.2 Fundamentals of operation ............................................... 17
5.2.1 The keypad ............................................................................ 17
5.2.2 Structure of the dialog windows ............................................ 18
5.2.3 Navigating in the dialog ......................................................... 18
5.2.4 Entering text and numbers ..................................................... 19
5.2.5 Selecting from a selection list ................................................. 20
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Table of contents
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5.3 Methods .............................................................................. 20
5.3.1 Method templates ................................................................. 20
5.3.2 Loading a method ................................................................. 21
5.3.3 Saving a method ................................................................... 21
5.3.4 Exporting a method ............................................................... 21
5.4 Sample data ........................................................................ 22
5.4.1 Entering sample data in the main dialog ................................ 22
5.4.2 Requesting sample data at the start of the determination ...... 23
5.5 Carrying out a determination ............................................ 24
5.6 Live modifications .............................................................. 27
5.6.1 Editing the sample data of the running determination ............ 27
5.6.2 Editing the live parameters ..................................................... 28
5.7 Results ................................................................................. 29
5.8 Statistics .............................................................................. 30
5.9 Printing a report manually ................................................. 31
5.10 Manual control ................................................................... 33
5.10.1 Dosing ................................................................................... 33
5.10.2 Stirring .................................................................................. 37
6 System settings 39
6.1 Basic settings ...................................................................... 39
6.2 Managing solutions ............................................................ 42
6.2.1 General ................................................................................. 42
6.2.2 Editing the solution data ........................................................ 43
6.3 File management ................................................................ 44
6.4 Configuring external devices ............................................. 46
6.5 Instrument diagnosis .......................................................... 49
6.5.1 Loading program versions and language files ......................... 49
6.5.2 Diagnosis functions ............................................................... 50
7 Parameters 51
7.1 Karl Fischer Titrations (KFT) .............................................. 51
7.1.1 Conditioning ......................................................................... 51
7.1.2 Start conditions ..................................................................... 52
7.1.3 Control parameters ................................................................ 53
7.1.4 Titration parameters .............................................................. 56
7.1.5 Stop conditions ..................................................................... 58
7.1.6 Calculations - Methods "Blank Ipol/Upol" ............................... 59
7.1.7 Calculations - Methods "Titer Ipol/Upol" ................................ 60
7.1.8 Calculations - Methods "KFT Ipol/Upol", "KFT Ipol/Upol–
Blank" ................................................................................... 61
7.1.9 Statistics ................................................................................ 63
7.1.10 Reports .................................................................................. 63
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IV
870 KF Titrino plus
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8 Operation and maintenance 66
9 Troubleshooting 67
10 Appendix 70
Table of contents
8.1 Quality Management and qualification with Metrohm .. 66
9.1 Karl Fischer titration .......................................................... 67
9.2 Miscellaneous ..................................................................... 68
10.1 Exchange unit ..................................................................... 70
10.1.1 Maximum dosing and filling rate ............................................ 70
10.1.2 Parameters for the preparing (PREP) ....................................... 70
10.2 Stirring rate ......................................................................... 71
10.3 Balance ................................................................................ 71
10.4 USB devices ......................................................................... 72
10.4.1 6.2147.000 numerical USB keypad ........................................ 72
10.4.2 Key assignment of a USB keyboard ........................................ 73
10.4.3 PC mouse .............................................................................. 73
10.4.4 Printer ................................................................................... 74
10.5 System initialization ........................................................... 74
10.6 Remote interface ................................................................ 76
10.6.1 Pin assignment of the remote interface .................................. 76
10.6.2 Status diagram of the remote interface .................................. 77
10.7 Remote control via an RS-232 connection ....................... 77
10.7.1 Commands and variables ....................................................... 78
10.8 Arithmetic algorithms in the 870 KF Titrino plus ............ 80
11 Technical specifications 83
11.1 Measuring inputs ................................................................ 83
11.1.1 Polarizer ................................................................................ 83
11.2 Dosing drive ........................................................................ 84
11.3 Interfaces ............................................................................. 84
11.4 Mains connection ............................................................... 84
11.5 Safety specifications ........................................................... 84
11.6 Electromagnetic compatibility (EMC) ................................ 85
11.7 Ambient temperature ......................................................... 85
11.8 Reference conditions .......................................................... 86
870 KF Titrino plus
11.9 Dimensions .......................................................................... 86
12 Warranty (guarantee) 87
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V
Table of contents
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13 Accessories 89
13.1 Scope of delivery ................................................................ 89
13.2 Optional accessories ........................................................... 94
Index 97
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VI
870 KF Titrino plus
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Table of figures
Figure 1 Front 870 KF Titrino plus ................................................................... 6
Figure 2 Rear 870 KF Titrino plus .................................................................... 7
Figure 3 Reagent dosing for KFT ..................................................................... 8
Figure 4 Connecting a polarizable electrode .................................................... 9
Figure 5 Connecting a stirrer ......................................................................... 10
Figure 6 Connecting a balance ...................................................................... 11
Figure 7 Connecting USB devices .................................................................. 12
Figure 8 Connecting the USB stick ................................................................ 13
Figure 9 Connecting the 6.2147.000 USB keyboard with USB stick and
printer ............................................................................................. 13
Figure 10 Connecting the USB hub with USB stick, printer and the 6.2148.030
RS-232/USB Box (for connecting balances). ...................................... 14
Figure 11 Connecting a remote cable ............................................................. 14
Figure 12 Attaching the exchange unit ........................................................... 15
Figure 13 Keypad 870 KF Titrino plus .............................................................. 17
Figure 14 Directory structure on the USB flash drive ........................................ 45
Figure 15 Rotational speed depending on stirring rate .................................... 71
Figure 16 Pin assignment of remote socket and remote plug .......................... 76
Figure 17 Remote status diagram .................................................................... 77
Figure 18 Connecting the RS-232/USB Box to the PC ...................................... 78
Table of figures
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VII
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1 Introduction
1.1 Instrument description
The 870 KF Titrino plus is an instrument used for volumetric water content
determination according to Karl Fischer. There are method templates
available which are already configured except for a few parameters. If
parameters are changed, then these will be saved automatically. The
methods can be exported to a connected USB flash drive. This function
makes it possible for you to copy methods quickly and easily from one
instrument to another.
1.1.1 Titration and measuring modes
The following titration and measuring modes are supported:
￭ KFT
Volumetric water content determination according to Karl Fischer.
Measuring modes:
– Ipol (voltametric measurement with selectable polarization cur-
rent)
– Upol (amperometric measurement with selectable polarization
voltage)
1 Introduction
1.1.2 Connectors
The instrument is equipped with the following connectors:
￭ MSB connector (Metrohm Serial Bus)
￭ USB (OTG) connector
￭ Electrode connector
￭ Remote connector
1.1.3 Intended use
The 870 KF Titrino plus is designed for usage as a titrator in analytical laboratories. Its main application field is volumetric titration.
This instrument is suitable for processing chemicals and flammable samples. The usage of the 870 KF Titrino plus therefore requires that the user
have basic knowledge and experience in the handling of toxic and caustic
substances. Knowledge with respect to the application of the fire prevention measures prescribed for laboratories is also mandatory.
For connecting a stirrer.
The 6.2151.100 adapter can be used to connect, for example, a
printer, a USB flash drive or a USB keyboard.
For connecting polarizable electrodes.
For connecting instruments with a remote interface.
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1.2 About the documentation
1.2 About the documentation
CAUTION
Please read through this documentation carefully before putting the
instrument into operation. The documentation contains information
and warnings which the user must follow in order to ensure safe operation of the instrument.
1.2.1 Symbols and conventions
The following symbols and formatting may appear in this documentation:
Cross-reference to figure legend
The first number refers to the figure number, the second to the instrument part in the figure.
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Instruction step
Carry out these steps in the sequence shown.
Method Dialog text, parameter in the software
File ▶ New Menu or menu item
[Next] Button or key
WARNING
This symbol draws attention to a possible life-threatening hazard or risk of injury.
WARNING
This symbol draws attention to a possible hazard due
to electrical current.
WARNING
This symbol draws attention to a possible hazard due
to heat or hot instrument parts.
WARNING
This symbol draws attention to a possible biological
hazard.
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2
CAUTION
This symbol draws attention to possible damage to
instruments or instrument parts.
870 KF Titrino plus
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1.3 Safety instructions
1.3.1 General notes on safety
WARNING
This instrument may only be operated in accordance with the specifications in this documentation.
This instrument has left the factory in a flawless state in terms of technical
safety. To maintain this state and ensure non-hazardous operation of the
instrument, the following instructions must be observed carefully.
1.3.2 Electrical safety
The electrical safety when working with the instrument is ensured as part
of the international standard IEC 61010.
1 Introduction
NOTE
This symbol highlights additional information and
tips.
WARNING
Only personnel qualified by Metrohm are authorized to carry out service
work on electronic components.
WARNING
Never open the housing of the instrument. The instrument could be
damaged by this. There is also a risk of serious injury if live components
are touched.
There are no parts inside the housing which can be serviced or replaced
by the user.
Mains voltage
WARNING
An incorrect mains voltage can damage the instrument.
870 KF Titrino plus
Only operate this instrument with a mains voltage specified for it (see
rear panel of the instrument).
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3
1.3 Safety instructions
Protection against electrostatic charges
WARNING
Electronic components are sensitive to electrostatic charges and can be
destroyed by discharges.
Do not fail to pull the mains cable out of the mains connection socket
before you set up or disconnect electrical plug connections at the rear
of the instrument.
1.3.3 Tubing and capillary connections
CAUTION
Leaks in tubing and capillary connections are a safety risk. Tighten all
connections well by hand. Avoid applying excessive force to tubing
connections. Damaged tubing ends lead to leakage. Appropriate tools
can be used to loosen connections.
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Check the connections regularly for leakage. If the instrument is used
mainly in unattended operation, then weekly inspections are mandatory.
1.3.4 Flammable solvents and chemicals
WARNING
All relevant safety measures are to be observed when working with
flammable solvents and chemicals.
￭ Set up the instrument in a well-ventilated location (e.g. fume cup-
board).
￭ Keep all sources of flame far from the workplace.
￭ Clean up spilled liquids and solids immediately.
￭ Follow the safety instructions of the chemical manufacturer.
1.3.5 Recycling and disposal
This product is covered by European Directive 2002/96/EC, WEEE – Waste
from Electrical and Electronic Equipment.
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4
The correct disposal of your old equipment will help to prevent negative
effects on the environment and public health.
870 KF Titrino plus
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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.
870 KF Titrino plus
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5
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
870 KF Titrino plus
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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.
870 KF Titrino plus
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EP
KFT Ipol
KFT Upol
EP
V/mL
Continuous
dosing
Initial
dosing
V/mL
V/mL
U/mV
t/s
I/µA
Control range
Control range
3 Water determination according to Karl Fischer
(KFT)
Karl Fischer Titration is a method for volumetric water determination. Conditioning is carried out automatically both before and after the actual titration. The reagent dosing is controlled in such a way that a predefined
endpoint is reached as quickly and as accurately as possible. The volume
steps and the rate of reagent dosing are regulated by the difference
between the current measured value and the predefined endpoint. This
means that titration is performed more slowly in the control range and
that smaller volumes are added. The titration is stopped at the endpoint
either drift-controlled or after a waiting time. The volume dosed until the
endpoint is used to calculate the water content of the sample.
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8
Figure 3
Reagent dosing for KFT
870 KF Titrino plus
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4 Installation
4.1 Setting up the instrument
4.1.1 Packaging
The instrument is supplied in highly protective special packaging together
with the separately packed accessories. Keep this packaging, as only this
ensures safe transportation of the instrument.
4.1.2 Checks
Immediately after receipt, check whether the shipment has arrived complete and without damage by comparing it with the delivery note.
4.1.3 Location
The instrument has been developed for operation indoors and may not be
used in explosive environments.
4 Installation
Place the instrument in a location of the laboratory which is suitable for
operation, free of vibrations, protected from corrosive atmosphere, and
contamination by chemicals.
The instrument should be protected against excessive temperature fluctuations and direct sunlight.
4.2 Connecting a sensor
Connecting a polarizable electrode
Figure 4
Connecting a polarizable electrode
870 KF Titrino plus
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9
4.3 Connecting a stirrer
NOTE
The electrode cable is protected against accidental disconnection of the
cable by means of a pull-out protection feature. If you wish to remove
the plug, then you must first retract the outer plug sleeve.
4.3 Connecting a stirrer
You can connect the following stirrers:
￭ 801 Stirrer
￭ 803 Ti Stand
￭ 804 Ti Stand (requires rod stirrer)
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Figure 5
Connecting a stirrer
CAUTION
Make sure that the flat side of the plug matches the marking on the
socket.
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10
870 KF Titrino plus
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4.4 Connecting a balance
Balances are equipped with a serial RS-232 interface as a rule. To connect
a balance, you require a 6.2148.030 RS-232/USB Box.
Figure 6 Connecting a balance
When a 6.2151.020 USB cable is used, then the 6.2148.030 RS-232/USB
Box can be connected to the 870 KF Titrino plus by means of a USB hub
or a 6.2151.100 adapter (see Chapter 4.5, page 11).
4 Installation
Connect the 9-pin plug of the respective balance connecting cable to the
RS 232/1 connector. Consult the user manual of the balance in order to
select the correct connecting cable.
The parameters for the RS-232 interface on the instrument must match
those on the balance (see "Editing the COM1 settings", page 47). Additionally consult the user manual of the balance.
4.5 Connecting a keyboard, printer and other USB devices
The 870 KF Titrino plus has a USB (OTG) connector. Use the provided
6.2151.100 adapter USB MINI (OTG) - USB A for connecting USB devices
as e.g. printers, keyboards or USB sticks, see the following figure.
870 KF Titrino plus
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11
4.5 Connecting a keyboard, printer and other USB devices
6.2151.100
Figure 7 Connecting USB devices
CAUTION
Switch the instrument off before connecting or disconnecting a USB
device or a USB stick.
The 870 KF Titrino plus can only recognize the device immediately after
switching on.
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The following devices can be operated directly on the USB connector
with the 6.2151.100 adapter:
￭ USB sticks (for the backup or storing of methods)
￭ 6.2147.000 numerical USB keypad
￭ 6.2148.030 RS-232/USB Box (for connecting balances or for the
RS-232 remote control)
￭ USB hub (with or without an own power supply)
The 6.2147.000 numerical USB keypad serves for comfortable numerical input and for navigating in the dialog. In addition, it provides two USB
connectors. Connect additional USB devices to the keypad.
NOTE
Most of the USB devices need a so-called hub in order to work correctly.
A USB hub is a distributor to which several USB devices can be connected. USB hubs are available in specialty stores in a number of different
models.
The USB (OTG) connector of the 870 KF Titrino plus has no such hub.
The 6.2147.000 numerical USB keypad has a USB hub and two USB
connectors.
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12
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
4 Installation
The following devices can only be connected to a 6.2147.000
numerical keypad or to a USB hub:
￭ Printer (with USB connector, use the 6.2151.020 connecting cable)
￭ Barcode reader (with USB cable)
￭ Mouse (PC mouse with USB cable, for navigating in the dialog)
The following devices can only be connected to a USB hub:
￭ PC keyboard (with USB cable, for the comfortable input of letters and
numbers)
￭ Keypad with numerical keypad (with USB cable)
If you wish to connect several different instruments without own
power supply, then you must possibly use a USB hub with own power
supply (self powered). The USB (OTG) connector of the 870 KF Titrino plus
is not designed for supplying power to several devices with elevated electricity requirements.
Also observe the instructions in chapter 10.4, page 72.
Examples:
Figure 8
Connecting the USB stick
Figure 9 Connecting the 6.2147.000 USB keyboard with USB stick and
printer
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4.6 Connecting instruments to the remote connector
USB MINI (OTG)-USB
USB stick
USB-Hub
RS-232/USB Box
6.2148.030
6.2151.100
Printer
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Figure 10 Connecting the USB hub with USB stick, printer and the
6.2148.030 RS-232/USB Box (for connecting balances).
4.6 Connecting instruments to the remote connector
The 870 KF Titrino plus can be integrated in an automation system with
the aid of a remote cable.
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14
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).
870 KF Titrino plus
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4.7 Attaching the exchange unit
4 Installation
Figure 12 Attaching the exchange unit
To attach the exchange unit, proceed as follows:
Slide the exchange unit from the front onto the 870 KF Titrino plus
1
and push all the way to the rear.
It must snap in audibly.
870 KF Titrino plus
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15
5.1 Switching the instrument on and off
5 Operation
5.1 Switching the instrument on and off
Switching on the instrument
Proceed as follows:
￭ Press the red [STOP] key.
1
The instrument is initialized and a system test performed. This
process takes some time.
￭ If a buret unit has been attached, then a request appears to carry
out the PREP function:
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All tubings and the cylinder are rinsed with the PREP (Preparing)
function. The preparing of the buret unit is described in chapter
"Preparing the buret unit (PREP)", page 33.
￭ Confirm the message with [OK].
The display of this message can be deactivated in the system settings (see "PREP warning", page 41).
The main dialog is displayed:
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16
870 KF Titrino plus
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Switching off the instrument
The instrument is switched off with the [STOP] key. The fact that the key
needs to be pressed down for an extended time prevents accidental
switch off.
Proceed as follows:
￭ Keep the red [STOP] key pressed down for at least 3 s.
1
A progress bar is displayed. If the key is released during this time,
then the instrument will not be switched off.
5.2 Fundamentals of operation
5.2.1 The keypad
5 Operation
Figure 13
Keypad 870 KF Titrino plus
BACK Apply the input and exit the dialog.
⇧ ⇩ Move the selection bar either up or down by one
line at a time. Select the character to be entered
in the text editor.
⇦ ⇨ Select the character to be entered in the text and
number editor. Select the individual functions in
the function bar.
OK Confirm the selection.
STOP Stop an ongoing method run or a manual func-
tion. Switch the instrument on or off.
START Start a method run or a manual function.
870 KF Titrino plus
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17
5.2 Fundamentals of operation
5.2.2 Structure of the dialog windows
The current dialog title is displayed on the left-hand side of the title bar.
The current status of the system is displayed in the upper right-hand corner:
ready The instrument is in normal status.
cond.busy The working medium is being conditioned.
cond.ok The working medium is conditioned.
busy A method has been started.
Some dialogs have a so-called function bar on the bottom line. The functions contained therein can be selected with the arrow keys [⇦] or [⇨]
and executed with [OK].
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5.2.3 Navigating in the dialog
The selection bar is displayed in inverted style. Use the arrow keys [⇧] and
[⇩] to move the selection bar upward or downward one line at a time. If
a dialog text is marked with "＞", then additional settings are available in
a subordinate dialog. Use [OK] to access this dialog.
Example: System settings
Use the [BACK] key to return to the next higher level.
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870 KF Titrino plus
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
5.2.4 Entering text and numbers
In the editing dialog for text input or numerical input, select the individual
characters with the arrow keys. Use [OK] to apply the character in the
input field. The following functions are available:
5 Operation
Editing function
Description
Accept The modification is applied and the editing dialog
is exited.
Cancel The editing dialog is exited without applying the
modification.
Clear The content of the input field is deleted com-
pletely.
The character left of the cursor is deleted (backspace).
Text editor only
The cursor within the input field is shifted to the
left by one character each time that [OK] is
pressed.
Text editor only
The cursor within the input field is shifted to the
right by one character each time that [OK] is
pressed.
870 KF Titrino plus
[BACK] The modification is applied and the editing dialog
is exited.
The [BACK] key has the same function as Accept.
A commercially available USB keyboard can be connected to make it easier to enter text and numbers. The assignment of the keys on the PC keyboard is described in chapter 10.4.2, page 73.
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5.3 Methods
5.2.5 Selecting from a selection list
In a selection list, select the individual entries with the arrow keys [⇧] and
[⇩]. Accept the selection with [OK] or [BACK].
5.3 Methods
5.3.1 Method templates
The 870 KF Titrino plus contains method templates which are already configured except for a few parameters.
The following method templates can be selected:
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KFT Ipol Method with adjustable polarization current.
The blank value is not taken into account for the
calculation.
Titer Ipol Titer determination with adjustable polarization
current.
Blank Ipol Blank value determination with adjustable polari-
zation current.
KFT Ipol–Blank Method with adjustable polarization current.
The blank value is taken into account for the calculation.
KFT Upol Method with adjustable polarization voltage.
The blank value is not taken into account for the
calculation.
Titer Upol Titer determination with adjustable polarization
voltage.
Blank Upol Blank value determination with adjustable polari-
zation voltage.
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KFT Upol–Blank Method with adjustable polarization voltage.
The blank value is taken into account for the calculation.
870 KF Titrino plus
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