870 KF Titrino Plus: Manual
870 KF Titrino Plus: Manual
870 KF Titrino Plus: Manual
Manual
8.870.8005EN
Metrohm AG
CH-9100 Herisau
Switzerland
Phone +41 71 353 85 85
Fax +41 71 353 89 01
[email protected]
www.metrohm.com
Manual
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
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
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
9 Troubleshooting 67
9.1 Karl Fischer titration .......................................................... 67
9.2 Miscellaneous ..................................................................... 68
10 Appendix 70
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
11.9 Dimensions .......................................................................... 86
12 Warranty (guarantee) 87
13 Accessories 89
13.1 Scope of delivery ................................................................ 89
13.2 Optional accessories ........................................................... 94
Index 97
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
1 Introduction
1.1.2 Connectors
The instrument is equipped with the following connectors:
■ MSB connector (Metrohm Serial Bus)
For connecting a stirrer.
■ USB (OTG) connector
The 6.2151.100 adapter can be used to connect, for example, a
printer, a USB flash drive or a USB keyboard.
■ Electrode connector
For connecting polarizable electrodes.
■ Remote connector
For connecting instruments with a remote interface.
CAUTION
NOTE
This symbol highlights additional information and
tips.
WARNING
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.
WARNING
WARNING
Mains voltage
WARNING
WARNING
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.
Check the connections regularly for leakage. If the instrument is used
mainly in unattended operation, then weekly inspections are manda-
tory.
WARNING
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.
1
2
3
3 Coupling 4 Display
For switching the flat stopcock.
5 Keypad
1 3
4
2 5
Control range
EP
V/mL
t/s
V/mL
Initial Continuous
dosing dosing
I/µA
KFT Upol
EP
Control range
V/mL
Figure 3 Reagent dosing for KFT
4 Installation
4.1.2 Checks
Immediately after receipt, check whether the shipment has arrived com-
plete 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.
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 fluctu-
ations and direct sunlight.
NOTE
CAUTION
Make sure that the flat side of the plug matches the marking on the
socket.
6.2151.100
CAUTION
NOTE
Most of the USB devices need a so-called hub in order to work cor-
rectly.
A USB hub is a distributor to which several USB devices can be connec-
ted. 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.
Examples:
Figure 9 Connecting the 6.2147.000 USB keyboard with USB stick and
printer
USB stick
Printer
Figure 10 Connecting the USB hub with USB stick, printer and the
6.2148.030 RS-232/USB Box (for connecting balances).
1 Slide the exchange unit from the front onto the 870 KF Titrino plus
and push all the way to the rear.
It must snap in audibly.
5 Operation
Proceed as follows:
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 set-
tings (see "PREP warning", page 41).
The main dialog is displayed:
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:
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 cor-
ner:
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 func-
tions contained therein can be selected with the arrow keys [⇦] or [⇨]
and executed with [OK].
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:
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 con-
figured except for a few parameters.
The following method templates can be selected:
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 cal-
culation.
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.
KFT Upol–Blank Method with adjustable polarization voltage.
The blank value is taken into account for the cal-
culation.
2 Select a method
■ Select the desired method.
NOTE
2 Select a method
■ Select the desired method.
ID1
Sample identification.
Entry max. 10 characters
Default value empty
ID2
Sample identification.
Entry max. 10 characters
Default value empty
Sample size
Sample size.
Input range –999999999 - 9999999999
Default value 1.0
Unit
Unit of the sample size.
Selection g | mg | µg | mL | µL | pieces | User-defined
Default value g
User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined.
2 Starting conditioning
■ Press [START].
Conditioning starts. Conditioning not OK is displayed until the
endpoint is reached. The working medium is titrated to the endpoint.
This is indicated by Conditioning OK. The status is kept stable.
The stirring rate can be modified with the Stirrer function. The fol-
lowing 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].
3 Adding sample
NOTE
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.
NOTE
5.7 Results
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.
Curve
Display the curve of the current determination.
Recalculate
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).
The arrow keys [⇦] and [⇨] can be used to move to the individual measur-
ing points. A cross hair is used to show the current position on the curve.
The data (volume, measured value, time, etc.) for the respective measur-
ing point is indicated on the right-hand side.
Recalculating
NOTE
All of the results are recalculated with the Recalculate function. This is
necessary if, for example, the calculation, the titer or the sample size has
been modified.
5.8 Statistics
Menu ▶ Results ▶ Statistics
The statistical overview of a determination series can be displayed in the
Results dialog with the Statistics function.
NOTE
The mean value (Mean), the absolute and the relative standard deviation
(s abs and s rel) are displayed in the overview. For the mean value, the
number of individual results from which it has been calculated is displayed
in parentheses. In this example, it is 3. The Statistics line shows how
many determinations have already been carried out and how many deter-
minations are to be carried out in total. All three determinations were car-
ried out in this example.
Details
Display additional data.
Reset
Delete all statistics data.
Increase
Add a further determination to the determination series.
The result and the sample size of each determination are shown.
On/Off
Remove the selected determination from the statistics. The line will then
be marked with an asterisk (*), the statistics will be recalculated automati-
cally.
The available subfunctions are listed for each function in the function bar.
NOTE
5.10.1 Dosing
The following dosing functions are available in the manual control:
Prepare the buret Rinse the cylinder and tubings of the buret unit
unit (PREP) (see Chapter 10.1.2, page 70).
Continuous dosing Dose while the [START] key is pressed.
(DOS)
Dose a fixed vol- Dose a specified volume.
ume (ADD)
Proceed as follows:
CAUTION
Make sure that the buret tip is directed into a vessel that can
accommodate the cylinder volume of your buret unit several times
over.
NOTE
■ The dosing and filling rates should be decreased for viscous liq-
uids.
■ The maximum dosing and filling rates depend on the cylinder
volume (see Chapter 10.1.1, page 70).
4 Start dosing
■ Press [START].
The status changes to busy, the dosed volume is displayed. When
the volume of one cylinder has been dosed, the dosing cylinder will
be refilled automatically.
NOTE
■ The dosing and filling rates should be decreased for viscous liq-
uids.
■ The maximum dosing and filling rates depend on the cylinder
volume (see Chapter 10.1.1, page 70).
4 Start dosing
■ Press [START].
The status changes to busy, the dosed volume is displayed. When
the volume of one cylinder has been dosed, the dosing cylinder will
be refilled automatically.
5.10.2 Stirring
You can control a connected stirrer manually.
Proceed as follows:
6 System settings
User name
A user name can be entered here for the report. This parameter will only
be printed if a user has been defined.
Entry max. 12 characters
Default value empty
Instrument name
A instrument name can be entered here for the report. This parameter will
only be printed if a designation has been defined.
Entry max. 10 characters
Default value empty
Serial number
Serial number of the instrument. This is printed as a part of the instrument
identification in the report header.
Program version
Version number of the instrument software. This is printed as a part of the
instrument identification in the report header.
Time
Current time. Only valid numbers can be entered.
Format: hh:mm:ss
Date
Current date. Only valid numbers can be entered.
Format: YYYY:MM:DD
Language
Setting the dialog language. An additional language can be selected
besides English.
NOTE
Dialog type
The user dialog can be limited for routine operations. One can operate
normally with methods in the limited dialog. However, no settings can be
made or methods deleted.
The resetting of the dialog will take effect as soon as you exit the main
menu.
The limitation of the dialog results in the following:
■ The menu items System and Parameters are not shown in the main
menu.
■ Methods can only be loaded, but not deleted, exported or created.
NOTE
If the limited dialog for routine operation is activated, then the expert
dialog cannot be activated during ongoing operation. To change the
dialog type, the 870 KF Titrino plus must be switched off and then back
on again. The expert dialog can be forced as soon as the instrument is
started up again. Then it is possible to enter whatever settings one
wishes, e.g. the changing of the dialog type. If the instrument is
switched off again without changing the dialog type, then the routine
dialog will remain activated.
Routine
Limited dialog for routine operations.
Contrast
The contrast of the display can be adjusted with the arrow keys [⇦] and
[⇨].
■ [⇦]: the contrast will be decreased by one step each time the key is
pressed.
■ [⇨]: the contrast will be increased by one step each time the key is
pressed.
Input range 150 - 240
Default value 212
NOTE
Beep
If this parameter is activated, then a short beep will sound in the following
cases:
■ When a key is pressed.
■ At the end of the determination.
■ When the system remains conditioned without interruption for 10 sec-
onds.
Selection on | off
Default value on
PREP warning
If this parameter is activated, then the recommendation will be made to
carry out the function PREP (Preparing):
■ After the instrument is switched on.
■ Each time a buret unit is attached.
All tubing and the cylinder are rinsed with this function (see Chapter
10.1.2, page 70).
Selection on | off
Default value on
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 solu-
tions in buret units with data chip can be added to the solution list. The
number of solutions in buret units without data chip is limited to 10 items.
Meaning of the type:
■ EU: exchange unit without data chip
■ IEU: exchange unit with integrated data chip
not defined is the standard solution. It can be used to carry out determi-
nations without having configured a solution. If you carry out a titer deter-
mination 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
Edit the data of the selected solution, see following chapter.
New
Add a new solution to the list, see following chapter.
Delete
Delete the selected solution from the list.
Type
The model of the buret unit is displayed.
Cylinder volume
Cylinder volume of the buret unit in mL. The cylinder volume is automati-
cally read out with intelligent buret units.
Selection 1 | 5 | 10 | 20 | 50
Default value 20
Concentration
Concentration of the solution.
Input range –999999999 - 9999999999
Default value 1.000
Concentration unit
Unit of the concentration.
Selection µmol/mL | mmol/L | mol/L | g/L | mg/L | mg/mL |
µg/L | ppm | % | mEq/L | User-defined
Default value mol/L
User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined. A blank entry can be generated this way as well.
Titer
Titer of the solution.
Input range –999999999 - 9999999999
Default value 1.000
Titer unit
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
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.
Monitoring
Activating and deactivating the titer monitoring.
Selection on | off
Default value off
Time interval
This parameter is visible only when Monitoring = on.
You will be notified that this time interval (in days) has elapsed when start-
ing a method. You can then select whether or not you would still like to
start the method.
Input range 1 - 999 d
Default value 999 d
NOTE
This menu item is visible only if a USB flash drive has been connected as
an external storage medium.
Methods can be imported and deleted from a USB flash drive in this dia-
log. Only methods located in the Files directory are displayed in the list
(see "Directory structure on the USB flash drive", page 45).
A backup of the system can be created (all data and settings). Similarly, an
existing backup can be reloaded.
Import
Import the selected method.
Delete
Delete the selected method.
Backup
Create a backup of all data and settings on the USB flash drive.
NOTE
Only one backup can be created on the same USB flash drive.
If a backup is already stored on the flash drive, then this will be over-
written as soon as the function is performed once again.
Restore
Load the backup from a connected USB flash drive.
PC/LIMS report
Specification of the storage location for the PC/LIMS report. The PC/LIMS
report is a machine-readable report with all of the important data for a
determination. It can be saved as follows:
■ as a TXT file on a USB flash drive.
■ to a LIMS via an RS-232 interface. The 6.2148.030 RS-232/USB Box is
required for this purpose.
Selection COM2 | USB Stick
Default value USB Stick
COM2
The report is sent via the serial COM2 interface. The interface parame-
ters set in the dialog COM2 settings are used (see "Editing the COM2
settings", page 48).
USB Stick
The report will be saved as a TXT file on the USB flash drive in the
folder pc_lims_report.
Printer
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
Adjust the width of the curve to be printed out to the paper width of the
printer to be used. The default value depends on the selected printer. The
height of the curve is 2/3 of the width.
Input range 100 - 3000 Pixels
Keyboard layout
A commercially available USB keyboard can be connected to make it eas-
ier to enter text and numbers. Specify the country-specific keyboard lay-
out.
Balance
If you have connected a balance, then you must define the balance type
here.
Selection AND | Mettler | Mettler AT | Mettler AX |
Ohaus | Precisa | Sartorius | Shimadzu
Default value Sartorius
The following table indicates the balance type that needs to be selected
for the balance model:
Baud rate
Transfer rate in characters per second.
Selection 1200 | 2400 | 4800 | 9600 | 19200 | 38400 |
57600 | 115200
Default value 9600
Data bits
Number of data bits.
Selection 7|8
Default value 8
Stop bits
Number of stop bits.
Selection 1|2
Default value 1
Parity
Type of parity testing.
Selection even | none | odd
Default value none
Handshake
Type of the data transfer protocol.
Selection hardware | software | none
Default value hardware
NOTE
Program files
They are instrument-specific. The file name has the following structure:
5XXXyyyy.bin where
XXX = Instrument type (e.g. 848 for the 848 Titrino plus)
yyyy = 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 struc-
ture:
5848xxxxYY.bin where
Loading a file
Proceed as follows:
7 Parameters
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.
Selection on | off
Default value on
Start drift
Conditioning OK will be displayed as soon as this volume drift has been
reached and the titration can be started.
Input range 1 - 999 µL/min
Default value 20 µL/min
Drift correction
The endpoint volume can be corrected by taking the drift value into
account. For this, the volume drift is multiplied with the drift correction
time and this value is then subtracted from the endpoint volume. The drift
correction time is the time interval between the end of conditioning and
the end of the determination.
Selection auto | manual | off
Default value off
auto
The value of the current volume drift is applied automatically at the
start of the titration.
manual
If the volume drift is known throughout a prolonged period of time,
then this can be entered manually.
off
No drift correction takes place.
Drift value
This parameter is visible only when Drift correction = manual.
Volume drift for manual drift correction.
Input range 0.0 - 99.9 µL/min
Default value 0.0 µL/min
Start volume
Volume that is dosed prior to the start of the titration.
Input range 0.00000 - 9999.99 mL
Default value 0.00000 mL
Dosing rate
Rate at which the start volume is dosed. The maximum dosing rate
depends on the cylinder volume (see Chapter 10.1.1, page 70).
Input range 0.01 - 166.00 mL/min
Selection max.
Default value max.
Pause
Waiting time, e.g. in case of a slow response of the electrode after the
start or reaction time after the dosing of a start volume.
Input range 0 - 999999 s
Default value 0s
Request sample ID
Selection of the sample identification that is queried in the method run.
Selection off | ID1 | ID2 | ID1&ID2
Default value off
Hold at request
If this parameter is switched on, then the method run will be paused dur-
ing the query. If the parameter is switched off, the titration will be started
in the background.
Selection on | off
Default value on
Endpoint at
Measured value for the endpoint.
Titration rate
Three predefined sets of parameters can be selected for the titration rate.
Selection slow | optimal | fast | user
Default value optimal
slow
For samples with a low water content or samples which release their
moisture only slowly.
optimal
For all standard titrations. The parameters have been optimized for the
most frequent applications.
fast
For uncritical samples with high water content.
user
The individual titration parameters can be modified.
The settings of the individual titration rates are listed in table 1, page
55.
Dynamics
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 vol-
ume 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.
Max. rate
This parameter is visible only when Titration rate = user.
Rate at which dosing is carried out outside of the control range. The maxi-
mum dosing rate depends on the cylinder volume (see Chapter 10.1.1,
page 70) .
Input range 0.01 - 166.00 mL/min
Selection max.
Default value max.
Min. increment
This parameter is visible only when Titration rate = user.
Minimum volume increment that is dosed at the beginning of the titration
and in the control range at the end of the titration. This parameter has a
decisive influence on the titration rate and thus also on the accuracy. The
smaller the selected minimum increment, the slower the titration.
Input range 0.1 - 99.90 µL
Selection min.
Default value min.
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.
Stop drift
This parameter is visible only when Stop criterion = drift.
Titration is stopped when the endpoint and the stop drift have been
reached.
Input range 1 - 999 µL/min
Default value 20 µL/min
Delay time
This parameter is visible only when Stop criterion = time.
When the endpoint is reached, the specified time is allowed to elapse
after the last dosing and the titration is then stopped.
Input range 0 - 999 s
Default value 10 s
Solution
Selection of the solution from the solution list. We recommend always
selecting the solution. This ensures that the correct data (titer, concentra-
tion, etc.) is always used for the calculation. Solutions are defined under
System ▶ Solutions.
For buret units with integrated data chip, a check is made in the method
run to verify whether the correct solution has been attached and whether
the type of dosing drive matches. For buret units without integrated data
chip, the cylinder volume and the type of dosing drive are checked. The
validity of the titer is checked for the selected solution at the start of the
determination.
Selection Selection of configured solution | not defined
Default value not defined
not defined
No check takes place.
I(pol)
The polarization current is the current that is applied to a polarizable elec-
trode during the voltametric measurement. This parameter is available
only with I(pol) determinations.
Input range –125 - 125 µA (Increment: 1)
Default value 50 µA
U(pol)
The polarization voltage is the voltage applied to the polarizable electrode
during an amperometric measurement. This parameter is available only
with U(pol) determinations.
Input range –1250 - 1250 mV (Increment: 10)
Default value 400 mV
Electrode test
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) determina-
tions.
Selection on | off
Default value off
Stirrer
When this parameter is switched on, then the stirrer is switched on at the
start of the determination.
Selection on | off
Default value on
Stirring rate
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-
tional speed is specified in chapter 10.2, page 71. The optimum stirring
rate can be tested in the manual control.
The algebraic sign of the stirring rate changes the direction in which the
stirring is done. When the stirrer is viewed from above, this means:
■ "+": counterclockwise rotation
■ "–": clockwise rotation
Input range –15 - 15
Default value 8
Temperature
Manually entered titration temperature.
Input range –20.0 - 150.0 °C
Default value 25.0 °C
Extraction time
Minimum duration of the titration. The titration will not be stopped during
the extraction time, even if the endpoint has already been reached. The
titration is however stopped if a stop condition is fulfilled during this time
(see Chapter 7.1.5, page 58). The entering of an extraction time is e.g.
recommended with samples that release water slowly or if a Karl Fischer
oven is used.
Input range 0 - 999999 s
Default value 0s
Stop volume
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.
Stop time
The titration is stopped when the specified time has elapsed following the
termination of the start conditions.
Input range 0 - 999999 s
Selection off
Default value off
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
70).
Input range 0.01 - 166.00 mL/min
Selection max.
Default value max.
Calculation formula
EP1*FCT
Factor (FCT)
If a larger amount of solvent is used for determining the blank value than
is later used for the sample, then this factor must be used to convert the
endpoint volume accordingly.
Input range –999999999 - 9999999999
Default value 1.0
Decimal places
Number of decimal places used to display the result.
Input range 0-5
Default value 2
Result unit
The result unit is displayed and saved together with the result. It cannot
be modified.
Selection mL
Calculation formula
(C00*FCT)/EP1
Factor (FCT)
Conversion factor, see table above.
Input range –999999999 - 9999999999
Default value 1.0
Decimal places
Number of decimal places used to display the result.
Input range 0-5
Default value 4
Result unit
The result unit is displayed and saved together with the result.
Selection % | ppm | mg/mL | g | mg | mL | mg/piece |
User-defined
Default value mg/mL
User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined. A blank entry can be generated this way as well.
Factor (FCT)
Conversion factor, see table above.
Input range –999999999 - 9999999999
Default value 0.1
Divisor (DIV)
Conversion factor, see table above.
Input range –999999999 - 9999999999
Default value 1.0
Titer
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 for-
mula. The calculation will then provide a correct result only if the unit
of the titer is mg/mL.
Blank (CV01/2)
This parameter is visible only with the methods KFT Ipol–Blank and KFT
Upol–Blank.
This value is calculated with the blank value determination (methods
Blank Ipol and Blank Upol) and entered here. The value can also be
modified manually.
Input range –999999999 - 9999999999 mL
Default value 0.0 mL
Decimal places
Number of decimal places used to display the result.
Result unit
The result unit is displayed and saved together with the result.
Selection % | ppm | mg/mL | g | mg | mL | mg/piece |
User-defined
Default value %
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.
7.1.9 Statistics
Menu ▶ Parameters ▶ Statistics
The statistics calculation of a multiple determination is switched on under
Statistics and it is defined how many determinations the series contains.
Statistics
If this funtion is switched on, then statistics calculations will be carried out
for all of the defined results.
Selection on | off
Default value off
For the methods "Titer Ipol" and "Titer Upol" the
default value is on.
Number of samples
The number of determinations that are carried out for the statistics calcu-
lations.
If an additional determination must be added to the determination series,
because one determination was incorrect, for example, then this can be
accomplished in the statistical overview (see Chapter 5.8, page 30).
Input range 2 - 20
Default value 3
7.1.10 Reports
Menu ▶ Parameters ▶ Reports
The reports that will be printed out automatically in connection with a
determination are defined under Reports.
Results
The result report contains the calculated results, equivalence points and
endpoints, sample data, etc.
Selection on | off
Default value off
Curve
Curve report. The width of the curve is defined in the system settings (see
"Graphics width", page 46).
Selection on | off
Default value off
Calculations/Statistics
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 on | off
Default value off
Parameters
All of the parameters of the current method are printed out with the para-
meter report.
Selection on | off
Default value off
PC/LIMS
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 on | off
Default value off
Qualification
Please contact your local Metrohm representative for support in qualifica-
tion of instruments and software. The Installation Qualification (IQ)
and Operational Qualification (OQ) are offered by Metrohm represen-
tatives as a service. They are carried out by trained employees using stan-
dardized qualification documents and in accordance with the currently
applicable requirements of the regulated industry. Further information on
this can be found in the brochure "Analytical Instrument Qualifica-
tion – Confidence in quality with IQ/OQ".
Maintenance
The electronic and mechanical functional groups of Metrohm instruments
can and should be checked by specialist personnel from Metrohm as part
of a regular preventive maintenance schedule. Please ask your local
Metrohm representative regarding the precise terms and conditions
involved in concluding a corresponding maintenance agreement. Further
information on this can be found in the brochure "Metrohm Care Con-
tracts – Protect your investment the smart way" available from your
local Metrohm representative.
9 Troubleshooting
9.1 Karl Fischer titration
Problem Cause Remedy
The drift is very high The titration cell is leaking. ■ Check seals and septum. If necessary,
during conditioning. replace.
■ Replace molecular sieve.
The drift becomes The sample releases water ■ Adjust the method.
greater after each very slowly. ■ Add solubilizer.
titration. ■ Increase the temperature (possibly using a
KF oven).
■ See technical literature.
The titration will not The titration cell is leaking. ■ Check seals and septum. If necessary,
be finished. replace.
■ Replace molecular sieve.
The minimum increment is Define Titration rate = user and increase the
too low. minimum volume increment (Min. incre-
ment) (see Chapter 7.1.3, page 53).
The stop criterion is unsuit- Adjust the control parameters (see Chapter
able. 7.1.3, page 53):
The electrode may be cov- Wipe off the electrode with ethanol or a suita-
ered. ble solvent.
The endpoint is The dosing rate outside the Define Titration rate = user and reduce the
reached too quickly. control range is too high. dosing rate (Max. rate) (see Chapter 7.1.3,
page 53).
9.2 Miscellaneous
Problem Cause Remedy
No report is printed. The printer is not recog- ■ Switch the 870 KF Titrino plus off and on
nized by the instrument. again.
■ Use a hub on the USB connector and con-
nect the printer to the hub.
The USB keyboard The keyboard or mouse is ■ Switch the 870 KF Titrino plus off and on
or the PC mouse not recognized by the again.
does not function. instrument. ■ Use a hub on the USB connector and con-
nect the keyboard or mouse to the hub.
The keyboard or the mouse Use a model which fulfills the required specifi-
is not compatible. cations (see Chapter 10.4, page 72).
The display is no The contrast is set incor- Adjust the contrast correctly (see Chapter 6.1,
longer readable. rectly. page 39).
Mettler XP balances The automatic calibration Switch off the automatic calibration.
send "R" or "O ----" of the balance is switched
as ID1. on.
Message 020-511 The USB stick is no longer 1. Connect the USB stick.
"Action not possi- connected. 2. Switch the instrument off and on again.
ble" is displayed.
The USB stick is full. ■ Use a different USB stick.
■ Delete files with the aid of a PC.
10 Appendix
Example:
Stirring rate set: 8
Rotational speed in rpm = 125 · 8 = 1000
r/min
2000
1500
1000
500
-15 -10 -5 0 5 10 15
Figure 15 Rotational speed depending on stirring rate
10.3 Balance
The sample size and the associated unit can be sent from a connected bal-
ance. The sample size is transmitted as a number with up to ten charac-
ters (including algebraic sign and decimal point).
Sample size and unit are sent as a single character string. They are separa-
ted by a space character. The string is terminated with the ASCII charac-
ters CR and LF.
If the balance sends a negative sample size (e.g. when you are reweighing
a sample), then the algebraic sign is adopted. The algebraic sign is, how-
ever, 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 identifica-
tion 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
NOTE
NOTE
The lettering of the USB keyboard may differ from above lettering,
depending on the country-specific keyboard used.
10.4.3 PC mouse
In order to make navigating in the dialog of the 870 KF Titrino plus easier,
a PC mouse can be connected.
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 select-
ing 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.
CAUTION
All user data (methods, solutions, etc.) are deleted if a system initializa-
tion is carried out. Afterwards, the instrument will have the factory set-
tings again.
We recommend creating a backup of the system at regular intervals in
order to avoid data losses.
NOTE
9 6
6 9
Figure 16 Pin assignment of remote socket and remote plug
The above figure of the pin assignment applies for all Metrohm instru-
ments with 9-pin D-Sub remote connector.
Inputs
+5 V approx. 5 kΩ Pull-up
tp
tp > 100 ms
active = low, inactive = high
Outputs
Open Collector
tp
tp > 200 ms
active = low, inactive = high
IC = 20 mA, VCEO = 40 V
+5 V: maximum load = 20 mA
Output 1
Titr/Determ Output 2
condOK Output 3
Error Output 4
Start Input 0
Stop Input 1
[STOP]
6.2134.040
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, adjust the interface parameters under
Menu ▶ System ▶ External devices ▶ COM2 settings.
Transfer protocol
The data communication is synchronous. On each command there is an
acknowledgement by the instrument.
A command must be sent to the instrument with the control characters
CR LF as terminator. The acknowledgements of the instrument will also
be transferred with CR LF as terminator.
The instrument does not send spontaneous messages.
Variable Comment
C00 Sample size
EP1 Volume of the endpoint EP1
CI# Sample identification (# = 1…2)
R1 Result
CV01 Common variable (blank value at KFT Ipol)
CV02 Common variable (blank value at KFT Upol)
SMN1 Mean value of result R#
TITER Titer of selected solution
Variable Comment
CONC Concentration of selected solution
FCT Factor
DIV Divisor
MCV End volume, i.e. total dosed volume at the end of the titration
EM1 Measured value of the endpoint EP1
ED1 Time at the endpoint EP1
MSV Start volume
DD Duration of the entire determination
The values of the variables are only available after the end of a determina-
tion (in the status 'ready').
Acknowledgement of Comment
the instrument
OK Command executed
E1 Method not found
E2 Invalid variable
E3 Invalid command
Rounding-off process
Measured values and results are rounded to the defined number of deci-
mal places (commercial rounding, in accordance with the US Pharmaco-
peia USP). If the digit at the first dropped decimal place is 1, 2, 3 or 4,
then it will be rounded off; if this digit is 5, 6, 7, 8 or 9, then it will be
rounded up. Negative digits will be rounded in accordance with their
amount, i.e. away from zero.
Examples:
2.33 yields 2.3
2.35 yields 2.4
2.47 yields 2.5
–2.38 yields –2.4
–2.45 yields –2.5
Statistics
The arithmetic mean value and the absolute and relative standard devia-
tions of results are calculated:
You can statistically evaluate a maximum of five results (1 ≤ k ≤ 5) calcu-
lated in a determination. A statistical series can contain a maximum of 20
determinations (1 ≤ n ≤ 20).
The following convention applies to the subsequent formulas:
1 ≤ n ≤ 20 and 1 ≤ k ≤ 5.
Mean value:
Explanations
The individual values are incorporated in the statistics with full accuracy.
15 significant places are yielded when the 64 bit numerical format is
applied for the floating-point number in decimal presentation.
The accuracy can be controlled by the selection of the prefix of the unit
(milli, micro) and the number of decimal places.
Example:
NOTE
11 Technical specifications
11.1.1 Polarizer
A measuring input (Pol.) for polarizable electrodes.
Measuring mode Determination with adjustable polarization current.
Ipol
Polarization –120 - +120 µA (increment: 1 µA)
current –125 - –121 µA / +121 - +125 µA: non-guaranteed values, dependent
on reference voltage +2.5 V
Measuring –1,200 - +1,200 mV
range
Resolution 0.1 mV
Measuring ±0.2 mV
accuracy (±1 digit, without sensor error, under reference conditions)
11.3 Interfaces
USB (OTG) connec- For connecting USB devices.
tor
MSB connector For connecting a stirrer.
Remote connector For connecting instruments with a remote interface.
Design and testing According to EN/IEC/UL 61010-1, CSA-C22.2 No. 61010-1, protection
class I, EN/IEC 60529, degree of protection IP40.
Safety instructions This document contains safety instructions which have to be followed
by the user in order to ensure safe operation of the instrument.
Immunity
Standards fulfil- ■ EN/IEC 61326-1
led ■ EN/IEC 61000-6-2
■ EN/IEC 61000-4-2
■ EN/IEC 61000-4-3
■ EN/IEC 61000-4-4
■ EN/IEC 61000-4-5
■ EN/IEC 61000-4-6
■ EN/IEC 61000-4-11
■ EN/IEC 61000-4-14
11.9 Dimensions
Material of hous- Polybutylene terephthalate (PBT)
ing
Material of display Glass
cover
Width 142 mm
Height 164 mm
Depth 310 mm
Weight 2,950 g
12 Warranty (guarantee)
Metrohm guarantees that the deliveries and services it provides are free of
defects in materials, design or manufacturing.
The general warranty period is 36 months (exclusions below) from the
date of delivery or 18 months in the event of continuous operation. The
warranty remains valid on the condition that the servicing is provided by a
service organization authorized by Metrohm at defined intervals and with
a defined scope.
The warranty period for anion suppressors of the type "MSM" is 120
months from the date of delivery or 60 months in the case of continuous
operation.
The warranty period for IC separation columns is 90 days after start-up.
For third-party components that are recognizable as such, the manufac-
turer's warranty regulations apply.
Consumables and materials with limited storage life and glass breakage in
the case of electrodes or other glass parts are excluded from the warranty.
Warranty claims cannot be asserted if the ordering party has failed to
meet its payment obligations according to schedule.
During the warranty period, Metrohm undertakes either to replace free of
charge or to credit the purchaser for any modules or components that can
be shown to be faulty. Any transport or customs fees that may apply are
the ordering party’s responsibility.
The precondition for this is that the ordering party has to specify the arti-
cle number, the article designation, an adequate error description, the
delivery date and (if applicable) the serial number or chip data in the Sup-
port Tracker. Metrohm then decides whether a replacement or a credit
note is to be issued or whether the faulty part has to be returned using
the Return Material Authorization (RMA). If a replacement or credit note is
issued, the ordering party undertakes to store the faulty part for at least
24 months in accordance with the current storage directives (in compli-
ance with ESD guidelines) and to hold it in readiness for onsite inspection
or for return shipment to Metrohm. Metrohm reserves the right to invoice
the ordering party for these articles, including retroactively, in the event of
noncompliance with these preconditions.
The same warranty periods that are specified for a corresponding new
part apply to parts that are replaced or repaired within the above-men-
tioned warranty periods. However, replacement or repair of a part does
not extend the warranty period of the entire system.
13 Accessories
NOTE
3 6.2730.030 Stopper
Complete with nipple and E.301.0043 O-ring. For 6.1414.030 titra-
tion vessel lid. For KF instruments, VA measurement stands, VA Com-
putrace and IC Dilution.
Length (mm): 38
1 6.2739.010 Wrench
For exchange units.
Length (mm): 190
Index
A Expert dialog ............................ 40 Numerical input ........................ 19
Adapter
Connect ............................. 11 F O
Filling rate Operation
B Maximum ........................... 70 General .............................. 17
Backup ..................................... 44
Balance .................................... 71 G P
Connect ............................. 11 GLP .......................................... 66 Parameter
Interface parameters ........... 47 Graphics width ......................... 46 KFT ..................................... 51
Balance type ............................. 47 Guarantee ................................ 87 Parameters
Buret unit Modify live ......................... 28
Prepare (PREP) .................... 33 I PC/LIMS report ......................... 46
Initialization .............................. 74 Pin assignment ......................... 76
C Instrument PREP
Calculation Switch off ........................... 17 Parameters ......................... 70
KFT ......................... 59, 60, 61 Switch on ........................... 16 Preparing
Numerical format ............... 80 Instrument diagnosis ................ 49 Parameters ......................... 70
Rounding-off process ......... 81 Print ......................................... 31
Conditioning K Printer ................................ 46, 74
KFT ..................................... 51 Keyboard Connect ............................. 11
Contrast ................................... 41 Connect ............................. 11 Program crash .......................... 74
Control parameters Key assignment ............ 72, 73 Program version
KFT ..................................... 53 Keyboard layout ....................... 46 Update ............................... 49
Curve ....................................... 29 KFT ........................................ 1, 8
Parameter ........................... 51 Q
D Quality Management ................ 66
Determination L
Cancel ................................ 26 Language ................................. 39 R
Carry out ............................ 24 Language file Recalculate ............................... 29
Result ................................. 29 Load ................................... 49 Remote
Diagnosis ................................. 50 Live modifications ..................... 27 Connector ............................ 7
Dialog language ....................... 39 Live parameters ........................ 28 Interface ............................. 76
Load ................................... 49 Pin assignment ................... 76
Dialog type ............................... 40 M Status diagram ................... 77
Directory structure .................... 45 Mains voltage ............................. 3 Remote cable
Dosing Maintenance Agreement .......... 66 Connect ............................. 14
Continuous (DOS) ............... 35 Manual control Remote control ........................ 77
Fixed volume (ADD) ............ 36 Dosing ............................... 33 Report
Dosing rate Stirring ............................... 37 Print manually .................... 31
Maximum ........................... 70 Method .................................... 20 Reports .................................... 63
Delete ................................ 44 Result ....................................... 29
E Export ................................ 21 Recalculate ......................... 30
Electrode Import ................................ 44 Rounding-off process ......... 81
Connect ............................... 9 Load ................................... 21 Routine dialog .......................... 41
Electrode connector Save ................................... 21 RS-232
Polarizable electrode ............. 7 MSB Interface parameters ........... 48
Electrostatic charge .................... 4 Connector ............................ 7 RS-232 connection ................... 77
End of Determination EOD ....... 77
Exchange unit N S
Attach ................................ 15 Navigate ................................... 18 Safety instructions ...................... 3