Karl Fischer Coulometer
Karl Fischer Coulometer
C20/C30
Table of Contents
1 Introduction 7
2 Safety Notes 8
2.1 Definition of Signal Warnings and Symbols 8
2.2 Product Specific Safety Notes 8
3 Karl Fischer Water Determination - Measuring Principle 10
4 Fundamentals of Coulometric Water Content and Bromine Index Determination 11
4.1 Fundamentals of coulometric water content determination 11
4.2 Coulometric bromine index determination 11
4.3 Generator electrodes 11
5 Description of Functions 13
5.1 Layout of the Terminal 13
5.2 Operating the Touchscreen 13
5.3 The Homescreen 13
5.4 The User Interface 13
5.4.1 Entering Data in the User Interface 14
5.4.2 Shortcuts and Direct Shortcuts 14
5.4.3 The Start analysis dialog 15
5.4.4 Online Dialog 15
5.4.4.1 Pretitration 15
5.4.4.2 Standby 16
6 Setup 18
6.1 Hardware 18
6.1.1 Sensors 18
6.1.2 Pump 19
6.1.3 Peripherals 19
6.1.3.1 Balance 19
6.1.3.2 Barcode reader 20
6.1.3.3 USB-Stick 20
6.1.3.4 Printer and USB data export 20
6.1.3.5 PC settings 22
6.1.3.6 Network settings 22
6.1.3.7 Fingerprint reader 22
6.1.3.8 LevelSens 23
6.1.4 Titration stands 24
6.2 Global settings 24
6.2.1 System 24
6.2.2 User Management 25
6.2.3 Analysis and resources behavior 26
6.2.3.1 Monitoring the Expiration Date and Life Span of Resources 28
6.2.4 Reagent control 29
6.3 User settings 30
6.3.1 Language 30
6.3.2 Screen 30
6.3.3 Beep 31
6.3.4 Shortcuts 31
6.3.5 Keyboards 31
6.4 Maintenance & Service 31
6.4.1 MT service 31
6.4.2 Import/Export 31
Table of Contents 3
6.4.3 Reset to factory settings 32
6.4.4 Titrator firmware history 32
6.4.5 Board firmware 32
6.4.6 Terminal 32
6.4.7 Board data 32
6.4.8 Upgrade 33
6.4.9 Update 33
6.4.10 Delete Mettler method template 33
6.5 Values 33
6.5.1 Blanks 33
6.5.2 Auxiliary values 33
7 Manual operations 35
7.1 Stirrer 35
7.2 Pump 35
7.3 Sensor 36
7.3.1 Polarized sensor 36
8 Methods 38
8.1 METTLER TOLEDO Methods 38
8.2 Creating Methods 39
8.2.1 Method Templates 40
8.3 Modifying or Deleting Methods 40
8.4 Starting Methods 41
8.5 Terminate method 41
8.6 Method Syntax – Rules for Establishing a Method 41
8.6.1 Possible Number of Method Functions 42
8.6.2 Types and Possible Number of Loops 42
8.6.3 Sample loops 43
8.6.4 Method Functions Within a Loop 43
8.6.5 Method Functions Outside of a Loop 44
8.7 Overview of method functions 44
8.8 Method functions 45
8.8.1 Title 45
8.8.2 Drift determination 46
8.8.3 Sample (KF) 46
8.8.4 Titration stand 48
8.8.5 Mix time 49
8.8.6 Titration (KF Coul) 49
8.8.7 Titration (EP Coul) 50
8.8.8 Auxiliary value 51
8.8.9 Blank 51
8.8.10 Instruction 52
8.8.11 Calculation 52
8.8.12 Report 53
8.8.13 End of sample 54
8.8.14 Standby 54
8.8.15 Hidden method functions 54
9 Series Templates 55
9.1 Sample series 55
9.2 Sample parameters 55
4 Table of Contents
10 Results 57
10.1 Results proposal lists 57
10.1.1 Internal calculations 59
10.2 All results 59
10.3 Add result 60
10.4 Statistics 60
10.4.1 Outlier test 60
10.5 Samples 61
10.6 Undo changes 61
10.7 Delete all results 62
11 Analysis Sequences 63
11.1 Starting an Analysis 63
11.2 KF Analysis sequence 64
11.2.1 Series analyses with the "Stromboli" oven sample changer 66
11.2.2 External extraction 67
11.2.3 Switching between determination types 67
11.2.4 Replacing the reagent solution 67
12 Analysis data 68
13 Evaluate and calculate 69
13.1 Indexing of method functions 69
13.2 Naming conventions for using analysis data in calculations 69
13.3 Formulas 71
13.3.1 Using analysis data in formulas 71
13.3.2 Mathematical functions and operators 72
Index 73
Table of Contents 5
1 Introduction
Simple and compact
The devices in METTLER TOLEDO's Titration Compact Line are modern, compact titrators for use in a wide vari
ety of application areas. They can be used, for example, in quality control as well as in research and develop
ment and satisfy the most demanding of requirements.
The titrators in the Titration Compact Line perfectly combine simple, easy-to-understand operation with an
extremely high level of precision and outstanding reliability. Thanks to automatic titrant recognition (Plug &
Play burettes), the titrator independently identifies which titrant is required without intervention from the operator.
Settings no longer need to be adjusted manually, even when connecting a printer or a Stromboli oven sample
changer.
Titration Compact devices can either be controlled by touchscreen or by using LabX PC software. The large col
or touchscreen allows intuitive control by the user and flexibility in its adjustment options. All functions can be
activated directly from the home screen via shortcuts which can be freely created, making everyday use
extremely easier. The touchscreen control of the titrator and all adjustable parameters are described in detail in
the operating instructions.
The separate installation information explains all the necessary steps for installing and commissioning your
device. The enclosed "Quick Guide" then guides you through the first titration using a practical example. If you
have any additional questions, METTLER TOLEDO is always available to assist you.
Introduction 7
2 Safety Notes
2.1 Definition of Signal Warnings and Symbols
Safety notes are marked with signal words and warning symbols. These show safety issues and warnings.
Ignoring the safety notes may lead to personal injury, damage to the instrument, malfunctions and false results.
Signal words
WARNING for a hazardous situation with medium risk, possibly resulting in severe
injuries or death if not avoided.
CAUTION for a hazardous situation with low risk, resulting in damage to the device or
the property or in loss of data, or minor or medium injuries if not avoided.
Warning symbols
General hazard Electrical shock
Acid / Corrosion
Location
The instrument has been developed for indoor operation and may not be used in explosive
environments.
Place the instrument in a location which is suitable for the operation, protected from direct
sunlight and corrosive gases. Avoid powerful vibrations, excessive temperature fluctuations
and temperatures below 5 °C and above 40 °C.
8 Safety Notes
Protective Clothing
It is advisable to wear protective clothing in the laboratory when working with hazardous or toxic substances.
A lab coat should be worn.
Use appropriate gloves when handling chemicals or hazardous substances, checking their
integrity before use.
Safety notes
WARNING
WARNING
Risk of corrosion
Leaks in tubing connections and loose titration vessels are a safety risk.
a) Tighten all connections well by hand, avoid applying excessive force to tubing connec
tions.
b) Always test the titration vessel for firm seating in the titration head.
WARNING
Flammable solvents
All relevant safety measures must be observed when working with flammable solvents and
chemicals.
a) Keep all sources of flame away from the workplace.
b) When using chemicals and solvents, comply with the instructions of the producer and
the general lab safety rules.
WARNING
Chemicals
All relevant safety measures are to be observed when working with chemicals.
a) Set up the instrument in a well-ventilated location.
b) Any spills should be wiped off immediately.
c) When using chemicals and solvents, comply with the instructions of the producer and
the general lab safety rules.
Safety Notes 9
3 Karl Fischer Water Determination - Measuring Principle
The Karl Fischer procedure is a titration method used for the quantitative determination of water content in liq
uids and solids. Karl Fischer titration is used in a variety of areas, e.g. for determining the water content of gro
ceries, chemicals, pharmaceuticals, cosmetics and mineral oils.
To determine the water content, first sulfur dioxide and water react with iodine:
2 H2O + SO2 + I2 SO42− + 2 I− + 4 H+
The addition of alcohol (e.g. methanol, ethanol), causes a preliminary reaction to take place in which sulfur
dioxide forms an acidic ester, which is then neutralized by the addition of a base (e.g. imidazole, referred to in
the following as "RN"):
CH3OH + SO2 + RN (RNH)·(CH3OSO2)
In the presence of water, the alkyl sulfite anion is oxidized to alkyl sulfate by the iodine. This process reduces
the yellow-brown iodine to colorless iodide:
(RNH)·(CH3OSO2) + I2 + H2O + 2 RN (RNH)·(CH3OSO3) + 2 (RNH)·I
The overall reaction proceeds as follows:
H2O + I2 + SO2 + CH3OH + 3 RN [RNH]SO4CH3 + 2 [RNH]I
The reaction runs until all the water has been consumed and hence free iodine is detected in the titration solu
tion. The end point is determined using bivoltametric indication, i.e. the potential at the polarized double-plat
inum-pin electrode falls below a certain value (e.g. 100mV).
7
7
8
8
Generator electrode Generator electrode
with diaphragm without diaphragm
You can press these buttons any time, regardless of which dialog you are currently using.
The Reset button acts as an "EMERGENCY STOP" switch. If the titrator malfunctions or there is an operating
error, you can stop all current tasks by pressing the reset button. Afterward, for each task, you can decide
whether to end it completely or continue.
See also
● Shortcuts and Direct Shortcuts (page 14)
Description of Functions 13
● The scroll bar on the right-hand side of the screen becomes visible if the content of the screen extends
beyond the viewable area. If this occurs, use either the arrows or the area in between them to move the
viewable area of the screen up or down.
● Five buttons are located at the bottom of the screen. The function of these buttons varies and depends on
the context of the current dialog.
Text input fields A Any text comprised of letters, numbers and symbols can be
BC entered into these fields.
Number input fields 1 Numbers, formulas and auxiliary values can be entered into
23 these fields. In some fields an auxiliary value can be selected
from the Auxiliary Values list by pressing the "H" button.
Drop-down lists Selecting these fields opens a drop-down list from which you can
select an entry.
List fields Selecting these fields opens a menu list in a new window.
Menu fields Selecting these fields opens a new dialog with a number of addi
tional menu options.
Formula fields A formula must be entered in these fields. You can enter these
manually or access a menu list by pressing the "Proposal" soft
key.
Info field The values in deactivated input fields are displayed as informa
i tion only and cannot be edited in the corresponding dialog.
In addition to the input fields there are checkboxes that can be checked in order to select certain functionalities.
Checkboxes can affect the scope of the corresponding dialog, i.e. input fields can be hidden or visible depend
ing on whether the checkbox is checked.
Sorting Lists
All of the lists displayed in the user interface can be sorted alphabetically or numerically by column in ascend
ing or descending order. To do this, simply touch the parameter in the header row by which you would like to
sort the list. A small arrow in the header row indicates the parameter by which the list is sorted and whether it is
sorted in ascending or descending order.
Dialog: Tasks (C30 only)
The Tasks dialog is accessed using the Tasks button (on the top right of the screen). It provides an overview of
all running tasks. Selecting an individual task from the list displays the relevant online dialog box, from where
you can exit the task.
The list contains a maximum of 10 running tasks.
14 Description of Functions
The titrator supports two types of shortcuts. Direct shortcuts which, when selected, start the task immediately
without warning (only if the other settings allow this), and normal shortcuts which take you to the correspond
ing start dialog from which you can start the task.
Shortcuts for methods, series or manual operations that take you
to the corresponding start dialog.
Shortcuts are managed in Setup > User settings. Here you can delete or modify shortcuts, or change their
position on the homescreen (see "User settings: Shortcuts").
Tasks started using the shortcuts can begin immediately without warning. Therefore, always make sure that all
tubes are connected to suitable vessels prior to using a shortcut.
● Once the maximum number of shortcuts (12) has been created in the Homescreen, the button AddToHome
is deactivated in the start dialog for methods, series and manual operations.
The Start analysis dialog is always the first dialog that appears after you choose "Start" or the relevant short
cut.
When a direct shortcut is activated, the Start analysis dialog does not appear and the respective method starts
immediately, provided that the other settings allow this.
The parameters for the previously used method or series appear in the Start analysis dialog so that the same
method can immediately be restarted.
Of course, all of the settings can also be adjusted prior to pressing "Start" The type and number of settings dis
played in the Start analysis dialog depends on the type of analysis to be started and the resources used.
5.4.4.1 Pretitration
Immediately following the start of a Karl Fischer titration, the online window for pretitration appears. In this win
dow, the following buttons are available:
Results
Select the Results button to display the results and statistics for the samples to be analyzed following the
analysis. The system displays the results of the active determination type (sample, blank value). Furthermore,
Description of Functions 15
the "Results" dialog also contains the following buttons: Add Result, Recalculate, Undo Changes, Perform
Outlier Test.
Samples
You can change sample and series data. However, the number of samples cannot be changed while a blank
determination is in progress. For changes to the sample data, refer to the analysis sequences:Starting an analy
sis
More
The More button provides you with additional functions. Using the More button in Pretitration mode, you can
perform the following:
End series
You can end a series if all predefined samples have been processed. Any changes made in the Start analysis
dialog or later are no longer taken into account. After the series has ended, you return to the pretitration or
standby mode and the series can be restarted again. A new series is entered in the results. The system then
uses the original sample parameters.
● The End series function triggers printouts defined Per series.
Stop method
The current method is stopped immediately. No printout is generated.
● Before actually stopping the process, the system displays a system message asking you to confirm the
action.
Save series data
The analysis of a series is saved in its entirety under a name freely chosen by the titrator in the form "SeriesXY".
Only sample data is included in the series. Blank value data is not included in the generated series. If the maxi
mum number of permitted series has already been reached, the series is not saved.
Axes
You can select the units for the horizontal and vertical axes from a list.
Sample size calculation
The optimum sample size can be calculated from the standby of an analysis.
The determined limits for the sample size do not have any impact on the lower and upper limits in the method
or for the sample data memory.
You can determine the following parameters:
Parameters Description Values
Content Expected water content of the sample. 0 .. 106
Unit Unit for the content. [%] | [ppm]
Use the Calculate button to obtain the upper and lower sample size limits for optimum titration.
5.4.4.2 Standby
If the drift drops below a predefined value, the system automatically switches from pretitration to Standby
mode (see "Analysis flows: Analysis flow diagram").
In Standby mode, you can start the drift determination or sample analysis, or conduct a blank determination for
the "external extraction" method type. The following buttons are available for this:
Start drift
For a drift determination, at least one increment of titrant must be generated.When the determination has been
completed successfully, the determined drift value is entered in the setup of the titration stand. The system then
generates an automatic printout containing the sample data, raw results, and resource data.
Start sample
This button is used to perform a sample analysis. When you press this button, an Info dialog is displayed
prompting you to add the sample.
Once a sample has been added and the analysis started, you can use the Samples button to enter the sample
size (see Method Function: Sample (KF) > Sample.
16 Description of Functions
Start blank determination
Blank value determination can be performed for the method type Ext. Extraction. No predispensing is per
formed. The determined blank value or the mean value for a series of blank determinations is entered in the Set
up for the relevant titrant, if this falls within the limits. If the mean value falls outside the specified limits, this is
not transferred to the Setup, but the system still switches to Standby. After the blank value has been determined
successfully,you receive a printout. If the value is not transferred to Setup, the system issues a message to
inform you of this. When you tap this button, an Info dialog is displayed prompting you to add the sample.
Measured values
You can use the More and Measured values buttons to display a table of measured values during an analysis
as an alternative to the online dialog.
Samples
You can use this button to change the sample size of the sample currently being processed or to define the
sample size for a new sample.
Cancel determination
You can use this button to cancel the measurement immediately during a sample or blank determination.
Before actually terminating the process, the system displays a system message asking you to confirm the ter
mination.
Description of Functions 17
6 Setup
This section tells you how to set up the titrator in accordance with your requirements so that you can carry out
titration.
Hardware Sensors
Pumps
Peripherals
Titration Stands
User settings Language
Screen
Beep
Shortcuts
Keyboard
Global settings System
User management
Analysis and resources behavior
Reagent Control
Values Blank
Auxiliary values
Mainten. & Service MT-Service
Import / Export
Reset to factory settings
Titrator firmware history
Board firmware
Terminal
Board data
Update
Expired Resources
Navigation: Home > Setup
Resources for which monitoring was selected in the settings can expire. Tap [Expired Resources] to open an
overview of all expired resources with the type, name and date of expiry of the respective resource.
6.1 Hardware
Navigation: Setup > Hardware
In this dialog window you can configure all the hardware components connected to the titrator, such as:
● Sensors
● Pump
● Peripherals (devices such as printers or balances)
● Titration stands (KF stand and additional Stromboli TTL for C30)
6.1.1 Sensors
Navigation: Setup > Hardware > Sensors
In this dialog you can configure and manage the sensors to be used with the titrator.
A polarized sensor is used for the Karl Fischer titration. The unit of measure can be set to [mV] or [µA].
To create a new sensor in the titrator, open the Sensor parameters dialog using the New button in the Sensors
dialog. You can determine the following parameters:
Parameters Description Values
Name Specify a descriptive name of your choice. Arbitrary
Serial number The serial number of the relevant device type. Arbitrary
18 Setup
Monitoring life Specifies whether the life span of the resource is to be monitored. Yes | No
span
● If a PnP sensor is connected to the sensor input, this automatically generates an entry in the setup. The
titrator updates all the details (sensor name, type or inputs).
6.1.2 Pump
Navigation: Setup > Hardware > Pumps
The Reagent manager is predefined in the Setupand cannot be configured individually. A connected Reagent
manager creates the relevant entry.
The parameters Type, Name and Pump output are displayed in the information fields in the Pump parameters
window.
6.1.3 Peripherals
Navigation: Home > Setup > Hardware > Peripherals
These settings encompass all input and output devices that belong to the titrator environment but that are not
essential instruments for processing an analysis (peripherals cannot be accessed in methods). The computer
also counts as a peripheral device. The list of all peripheral instruments defined in the titrator, together with the
parameters of each individual instrument can be printed out by a printer.
6.1.3.1 Balance
Navigation: Home > Setup > Hardware > Peripherals > Balance
Before defining a balance, you need to select the balance type. The titrator supports the following types of bal
ance:
Balance type Supported balances
Mettler AB | PB | PB-S | AB-S | PB-E | AB-E | College-S | SB | CB | GB | College-B |
HB | AG | PG | PG-S | SG | HG | XP | XS | XA | XPE | XSE | XVE | AX | MX |
UMX | PR | SR | HR | AT | MT | UMT | PM | AM | SM | CM | MS | ML
Sartorius Sartorius
More --
Setup 19
Data bit Defines the number of data bits. 7|8
Stop bit Defines the number of stop bits. (2 stop bits can only be selected 1|2
if 7 data bits are also selected at the same time.)
Parity Defines the parity protocol. Even | Odd | None
Handshake Data transmission via the RS-232 interface. (Only the handshake None | Xon-Xoff
option "Xon-Xoff" is available for serial connections on the ana
log and conductivity board in conjunction with a baud rate of
9600.)
● The settings for the baud rate, data bit, stop bit, parity, and handshake must agree for the balance and titra
tor!
● If None is selected as balance type that means that no balance is to be connected to the titrator.
6.1.3.3 USB-Stick
Navigation: Home > Setup > Hardware > Peripherals > USB-Stick
Commercially available USB sticks from USB Version 1.1 are supported.
You can assign a relevant name to the USB stick.
20 Setup
Methods List printout
Parameter printouts
Series List printout
Parameter printouts
● The compact printer does not generate the automatic printouts generated by the method functions Instruc
tion and Calculation during the analysis. It also does not support all languages.
● For Karl Fischer determinations, manual concentration, drift and blank value analyses are printed out auto
matically.
Define the following parameters:
Parameters Description Values
Printer type Selection of a printer, USB printer | USB
The USB compact printer does not support all languages. This compact printer | USB
printer can only print out a limited quantity of analysis data and data export
results.
For USB data export, the data is transmitted regardless of the
selected language. Only a limited quantity of data and results are
exported.
Information on the USB data export
● In the method function Record, the parameter Summary must be activated (Record = outside loop) or Per
sample or Per series (Record = inside loop). The other settings in Record have no effect.
• If the method function Record is inserted outside the loop, the data from the preceding loop and the data
between the End of sample and method functions Record are output.
● For a KF method in the method function Record (within the loop), the parameter Summary should be
selected with the value Per sample or Per series.
If data export is activated, the following data is transmitted:
● The most important sample data and results, either per sample or per series, according to the parameter
setting in Summary of the method function Record.
● Automatic reports for drift, blank value and concentration determination in a Karl Fischer water content
determination if the global setting Print autom. KF protocols is also activated
Navigation: Home > Setup > Global settings > Analysis and resources behavior > Analysis sequence
settings
Depending on the selected printer type, the following parameters appear in the printer dialog box:
● USB printer and USB compact printer
Parameters Description Values
Status Indicates whether the selected printer type is installed. Installed
Name Specify a descriptive name of your choice. Arbitrary
Serial number The serial number of the relevant device type. Arbitrary
Connection Information on the USB port to which the printer is connected. MB1/USB1 | PnP
PnP is displayed if the printer is not connected to the titrator.
● USB data export
The USB data export box is required for USB data export. If it is connected to the titrator using the USB interface,
the box is automatically detected (PnP detection).
Parameters Description Values
USB data export Indicates whether the USB data export box is installed (info field). Installed | Not
box installed
Connection The USB port to which the USB data export box is connected (info USB | PnP
field). PnP is displayed if the box is not connected to the titrator.
Baud rate The baud rate for data transmission via the USB interface. 1200 | 2400 | 4800 |
9600 | 19200
Data bit Information on the number of data bits is displayed. 8
Stop bit Information the number of stop bits is displayed. 1
Parity Defines the parity protocol. Even | Odd | None
Setup 21
Handshake Data transmission via the USB interface. None | Xon-Xoff
The max. Xoff duration for outgoing data is around 30s.
6.1.3.5 PC settings
Navigation: Home > Setup > Hardware > Peripherals > PC settings
Configure these settings if you have your instrument connected to the PC software LabX.
● The PC with LabX installed must always be connected to the PC (USB) or Ethernet port on the rear panel.
● After the settings have been modified, it may be necessary to restart the instrument.
Parameters Description Values
Connect to LabX If this parameter is activated, a connection to LabX will be estab Yes | No
at start-up lished on startup.
Connection type Defines how the titrator is connected to the PC, either via the net Network | USB
work connection or via the USB connection.
Status Information on the connection status from the instrument to LabX. Connected | Discon
nected
Port number Defines the port for a network connection of the titrator to LabX. 1024…65535
Only appears for Connection type = Network.
22 Setup
4 Place the preferred finger on the fingerprint reader and repeat the step as prompted.
When completed, the message Registration successful. appears.
5 Confirm the message with the [OK] to return to the User data window.
6 Confirm with [OK] to return to the homescreen.
The next time you log on, the Fingerprint login window will appears. To log on, place the appropriate finger
on the fingerprint reader.
● You can only log on using the fingerprint reader if Activate fingerprint reader is selected.
Navigation: Home > Setup > Hardware > Peripherals > Fingerprint reader
● You are still able to log on using a password. To do this, tap [Password login].
6.1.3.8 LevelSens
Navigation: Home > Setup > Hardware > Peripherals > LevelSens
The level sensor (LevelSens) can be used either to monitor the fill level of titration or solvent vessels or to pre
vent the overflow of waste vessels.
The level sensor is connected to the "LevelSens box", which is connected to the titrator via the CAN interface.
The titrator automatically recognizes up to two of these boxes (PnP recognition). These appear in the settings.
Navigation: Home > Setup > Hardware > Peripherals > LevelSens
1 In LevelSens, tap on a "LevelSens box".
The windows to edit the parameters opens.
2 The parameters Level, Waste or Inactive can be defined for the relevant sensor type
Activating level monitoring
● At the start of a method or a manual operation.
The level is checked for all activated and connected sensors, regardless of whether they are used in the
method.
● At the start of each sample (GT).
● After completion of a Karl Fischer analysis (KF).
● Before the start of a KF Stromboli method.
● Before replacing the solvent.
● During the course of the following manual operations: Burette (Rinse, Rinse multiple burettes, Dispense,
Manual titration), Pump, Auxiliary instrument (output 24V), Sample changer (Pump, Rinse).
If the fill level is not reached or exceeded, a message appears with a prompt either to empty or fill the vessel
(depending on the Setup setting: Waste or Level). The analysis is interrupted during this time. After the vessel
has been emptied or filled and the message has been confirmed, the analysis is resumed.
● Only two LevelSens boxes can be entered in the settings. Additional boxes do not generate an additional
entry.
● Entries in the settings can only be deleted if the corresponding LevelSens box is not installed.
● The sensor must be fitted in such a way that when the maximum fill level is reached, the analysis of a sam
ple, the entire loop of a Stromboli method or a solvent replacement can be performed.
● The fill level is only checked before a sample analysis, at the start of a Stromboli method or before a solvent
replacement.
Parameters Description Values
Name Information on the designation of the LevelSens box. -
In the settings, the first detected box is entered as LevelSens Box
1, the second as LevelSens Box 2.
Chip ID Information on the Chip-ID of the detected LevelSens box. -
Position Information on the position of the LevelSens box connected to the PnP | PnP1 | PnP2
titrator.
Sensor 1 Specifies the sensor type to be used. Level | Waste | Inactive
type…Sensor 4
type
Setup 23
6.1.4 Titration stands
Navigation: Setup > Hardware > Titration Stands
In this dialog, you can add new titration stands or select existing stands that are connected to the titrator and
change their parameters. You can also print the list of entered titration stands. You can also delete individual
titration stands.
You can create the following titration stands:
● Stromboli TTL
● Karl Fischer stand
Choose the New button in the Titration stands dialog to open the Titration stand parameters dialog box.
To configure the new titration stand you have just created, you can determine the following parameters:
Parameters Description Values
Type The type of the titration stand to be used. KF stand | Stromboli
TTL
Name Specify a descriptive name of your choice. Arbitrary
Stirrer output Defines the stirrer output. MB/Stirrer1 | MB/Stir
rer2 | AB1/Stirrer |
Internal stirrer | More
depending on configu
ration
● The Stromboli oven sample changer is connected to the TTL port of the mainboard.
6.2.1 System
Navigation: Home > Global settings > System
Titrator identification
You can enter and assign any ID consisting of at least four characters to the titrator.
Parameters Description Values
Titrator ID Define the instrument identification. -
Titrator Indicates the titrator type. T50 | T70 | T90
Serial number Information on the serial number of the instrument. -
Titrator FW ver Information on the firmware version of the instrument. -
sion
Date / Time
You can define the format used to display the date and time and set the titrator date and time.
Parameters Description Values
Date format Defines the format for displaying the date. mm/dd/yyyy |
dd/mm/yyyy
24 Setup
Time format Defines the format for displaying the time. 24h | a.m./p.m.
Date Enter the current date. -
Time Enter the current time. -
Header and footer
Define whether all printouts generated by the titrator should have a header or footer. The content of these head
ers and footers can be entered directly into the respective setting.
As part of the end of record, signature fields are appended to the respective printout consisting of a declaration
(e.g. Approved by) followed by an empty line. A personal signature can be then be entered on this line.
Parameters Description Values
Header Activates the header on print outs. Yes | No
Text Defines the text for the header. Arbitrary
Only for Header = Yes.
Footer Activates the footer on print outs. Yes | No
Text Defines the text for the footer. Arbitrary
Only for Footer = Yes.
End of report Select the information to be printed at the end of a report. Created by | Modified
by | Checked by |
Approved by
Data storage
In the T50 and T70, the system only saves the results from the last analysis (series or individual sample). In
the T90 select [Select Series] to select the results from the last two analyses.
Parameters Description Values
Delete data on Define if analysis data is to be deleted from the titrator memory Yes | No
shut down when the titrator is shut down.
Setup 25
Enforce pass If activated, the user is forced to change their password the next Yes | No
word change time they log on to the titrator.
Only appears if Enforce password/fingerprint = Yes is selected
in Account Policies.
● If the parameter Reset password is activated, the parameter Enforce password change will be automatical
ly activated.
● The default password for this user (User ID: "Administrator") is "123456" (do not enter inverted commas).
User group
Two fixed user groups are defined in the titrator: Experts and Routine-User. Any user can belong to one of the
user groups (with different authorizations). User management for "x20" models only contain the Experts group.
1 In User management select [Groups].
The two fixed defined groups are listed in this window.
2 Select one of these groups to access the Group parameters dialog.
This is where the parameters and authorization rights of the user groups are defined.
● Users in the Experts (system administrators) group have all the rights listed below:
• Editing methods Users can create methods in the Method editor and have full editing rights.
• Editing series and samples Users can create series templates and samples and have full editing rights.
• Editing resources and peripherals Users can create resources and peripherals and have full editing rights.
• Editing global and analysis sequence settings: Users can edit the global settings in Setup.
• Editing user-specific settings: Users can edit the user-specific settings in Setup.
• Editing results: Users can edit the saved results.
• Starting methods and series: Users can start methods from the method list or the Start analysis dialog.
• Executing manual operations: Users can execute manual operations.
● Users in the Routine-User (operators) group can start methods and series and execute manual operations.
*Basic functions: Starting drift or blank determination.
Account Policies
In Account Policies define the actions of the titrator when it is started up.
Parameters Description Values
Enforce pass If this parameter is activated, the titrator always starts with the Yes | No
word/fingerprint login screen (even if only one user is defined for the instrument).
The user name must always be entered in the login screen man
ually (the corresponding input box is always initially empty).
● If this option is selected for an instrument with factory settings, the titrator will demand the password for the
predefined user (User ID: "Administrator") the next time it is booted up. This password is "123456" (do not
enter inverted commas).
Min. no. of char Specifies the minimum number of characters required for user Yes | No
acters passwords. If this parameter is changed, then users whose pass
word does not meet this requirement will be requested to change
their password accordingly the next time that they log in.
26 Setup
Analysis sequence settings
The analysis sequence settings can only be modified if no tasks are currently being performed by the titrator.
You can make the following settings that influence the sequence of an analysis.
Parameters Description Values
Show required When an analysis is started a screen appears displaying all Yes | No
resources at resources required for the analysis and their status (available,
start not-available, locked or in use). If an individual entry is selected
from this screen then the user receives additional information
about the respective resource.
However, if "no" is selected, then the required resources are still
checked when the analysis is started and if necessary, an appro
priate error message is issued.
Show SOP If an SOP (standard operating procedure) has been defined in the Yes | No
Title method function then this will be displayed before the
method is started provided that "yes" has been selected.
● If Show required resources at start and Show SOP parameters were set to "Yes" at the start of a job series,
all SOPs and subsequently all resources for the individual sample series must be confirmed before the job
series is started. In this way a job series can be performed after it has been started without any further inter
ruption.
LabX: Warning If "yes" is selected then a warning is issued when the analysis is Yes | No
when not con started if there is no connection to LabX.
nected
Show results If a manual or external titration stand is being used, then the Yes | No
after analysis results for a sample are automatically displayed after they have
been analyzed and must be acknowledged by the user before the
analysis can be continued. With Auto stand the results are dis
played for a certain period and are not to be confirmed.
The activated parameter is valid for the following functions:
Analysis: the results for a sample are shown
Calibration/Loop: The results of the calibration are shown
(slope, zero point)
Sensor test: The results of the test are shown (slope, zero point,
drift and sensor test OK / not OK)
Check local When selected, the availability of a printer is checked at the Yes | No
printer connec beginning of the method.
tion and wait If not selected and no printer is connected, the method function
Record is skipped. If a printer is connected, the method function
Record is executed even if this parameter is not selected.
Print autom. KF Controls the printouts in manual drift or blank determination. Yes | No
protocols
Save results Defines if date, time, user, Methods ID, sample ID, results, result To USB-Stick | No
unit per sample is saved in a file. If this parameter is activated
and the stick is not detected during the data writing process, you
can stop the process or you can plug in another USB-stick for the
data writing and to continue the method run.
Only for Check USB-Stick connection and wait = Yes.
Check USB-Stick If this parameter is activated, the presence of a USB - Stick is val Yes | No
connection and idated at the start of the analysis.
wait
Resources behavior
Use the following parameters to configure how the titrator responds to the deletion of resources and its response
to the automatic identification of PnP resources.
Setup 27
Action when exceeding usable life
If it is determined by the titrator that the expiration dates of a resource have been exceeded, then the titrator may
perform various actions.
Warning The user is warned that the resource's usable life has been exceeded and the raw results and
results determined with the respective resource will be labeled accordingly.
Block The user is notified that the usable life of the resource has been exceeded and it is no longer
possible to start the analysis with the affected resource. (Methods that result in renewal of
this resource can however still be started.)
None If you select "none" then the analysis is started without message in spite of the exceeded
usable life. The expiry of the expiration date will, however, be logged.
Parameters Description Values
Auxiliary values This action is performed if the system determines at the start of None | Warning | Block
an analysis that the usable life of an auxiliary value that is to be
used in the analysis has been exceeded.
Blank values This action is performed if the system determines at the start of None | Warning | Block
an analysis that the usable life of a blank value that is to be used
in the analysis has been exceeded.
Action when exceeding life span
If, at the start of an analysis, it is determined that the life span of a resource to be used for the analysis has
expired, the titrator can set various actions.
Warning The user is warned that the resource life span has been exceeded and the raw results and
results determined with the respective resource will be labeled accordingly.
Block The user is notified that the life span of the resource has been exceeded and it is no longer
possible to start the analysis with the affected resource.
None The analysis is started in spite of the exceeded life span.
Parameters Description Values
Sensors The action is executed if the system determines at the start of an None | Warning | Block
analysis that the usable life of a sensor has been exceeded.
Whether the expiration dates should be monitored can be defined in the setup for each individual resource.
If monitoring is activated then additional parameters become available in the respective resource with which the
duration of the expiration dates can be determined. In addition a reminder may optionally be issued by the titra
tor before the expiration dates expire.
You can define the following parameters:
Parameters Description Values
Time period Specifies the time range. Days | Hours
Usable life Defines the time span of the expiration dates either in days or Days: 1…1000
hours (depending on: Time period). Hours: 1…104
Reminder Determines whether the titrator should issue a warning before the Yes | No
service life or usable life of a resource elapses.
Days before Determines the number of days before the service life of the 0…1000
expiration resource that the titrator should issue a warning. The value
entered must be less than the value in Usable life.
Only if Time period = Days and Reminder = Yes.
28 Setup
If a resource is updated, the Date/Time field in Setup of the affected resource is automatically adjusted and the
expiration date (or time) is recalculated.
In the "Global settings" under "Analysis and resources behavior", you can define how the titrator deals with the
relevant resource if the expiration dates have been exceeded at the start of the analysis (see "Action when
exceeding usable life (page 28)").
To monitor the reagent solution, the time, water volume, and number of samples is recorded and added for
each titration. When the defined monitoring parameters have been reached, a system message is displayed.
The user then has an opportunity to replace the reagent solution. The Solvent manager is started to pump the
reagent solution away.The cell is then filled with new solution. All counters are reset to zero (see Manual opera
tions: Pump).
For sample analysis using the Stromboli oven sample changer, the reagent solution can only be replaced in
Standby mode before analysis of the first sample, or at the end of the series, if the titrator returns to Standby
mode.
You can choose the Reagent control button in the Global settings to open the Reagent control dialog.
In this window, you can define the following parameters for solvent replacement:
Parameters Description Values
Monitoring Specifies whether the reagent solution is to be monitored. Yes | No
usable life of
reagent
Usable life Defines the time interval in days for the use of the reagent solu 1…10000
tion.
Enforce replace Forces the user to replace the reagent solution immediately after Yes | No
ment when the prompt to do so.
exceeding
usable life
Monitoring Specifies whether the capacity is to be monitored. Yes | No
capacity of
reagent
Setup 29
Max. amount of The maximum volume of water in [mg] for a reagent. 0...1000000
water Only if Monitoring capacity of reagent = Yes.
Enforce replace Forces the user to replace the reagent solution immediately after Yes | No
ment when the prompt to do so.
exceeding
capacity
Monitoring no. Specifies whether the system should monitor the number of sam Yes | No
of samples ples.
Max. no. of Maximum number of samples (not including the blank value) 0...120
samples after which the reagent is to be replaced.
Enforce replace Forces the user to replace the reagent solution immediately after Yes | No
ment at max. the prompt to do so.
no. of samples
Stir Enables the stirrer during solvent exchange. Yes | No
See also
● Monitoring the expiration date of a resource (page 28)
6.3.1 Language
Navigation: Home > Setup > User settings > Language
Define the following parameters:
Parameters Description Values
Touchscreen Defines the language for operation of the terminal. German | English |
French | Italian | Span
ish | Chinese | Russian |
Polish | Korean
Record Defines the language in which the protocols are to be printed out. German | English |
French | Italian | Span
ish | Chinese | Russian |
Polish | Korean
● For the Chinese and Korean language settings, it is not possible to print using the USB-P25 tape printer.
● For Polish, records can be printed on the USB-P25 tape printer without special characters.
6.3.2 Screen
Navigation: Home > Setup > User settings > Screen
Define the following parameters:
Parameters Description Values
Primary color Here various color schemes for the user interface can be select Gray | Blue | Green |
ed. Red
Brightness Specifies the display brightness in [%]. 50 | 60 | 70 | 80 | 90 |
100 [%]
Button shape Defines whether to display the buttons in the menus with square Rounded | Square
or rounded corners.
Screen saver Here you can define whether the screen saver should be used. Yes | No
Wait time Defines how long in [min] the system should wait after the user's 1…1000
last action on the terminal before activating the screen saver.
30 Setup
6.3.3 Beep
Navigation: Home > Setup > User settings > Beep
Define the following parameter:
Parameters Description Values
At push of a but Enables a beep when tapping on the touch screen. Yes | No
ton
6.3.4 Shortcuts
Navigation: Home > Setup > User settings > Shortcuts
Each user can manage the shortcuts that they have created. Individual shortcuts can be selected and deleted
and the following parameters of a shortcut can be changed:
Parameters Description Values
Description Any name for the shortcut. Arbitrary
Immediate start The method, series, or manual operation can be started immedi Yes | No
ately. This enables you to start the analysis without any interfer
ing dialog.
Homescreen You can select the free position for the shortcut on the Home 1…12
position screen.
6.3.5 Keyboards
Navigation: Home > Setup > User settings > Keyboards
In this dialog, you can define the layout for the alphanumeric and the numeric input fields. The following set
tings are available:
Parameters Description Values
ABC keyboard Determines the layout of the alphanumeric input field. English | French | Ger
man
123 keyboard Defines the organization of the keys for the numeric input field. Calculator | Phone
6.4.1 MT service
Select the MT service button to open the Last MT services dialog box.
In this dialog, you can view and print out a list of the most recent (max. 10) METTLER TOLEDO services. Under
each date, the user name of the METTLER TOLEDO service technicians and the date and time of the service
appointment are displayed. The most recently performed service always appears at the top of the list.
The Settings button in the Last MT services dialog window opens the Service data dialog, in which you can
change the service life (in days) of the last service date and configure the titrator to issue a warning at a
defined time before the service life elapses (requires administrator rights). You can define the following parame
ters:
Parameters Description Values
Service life Defines the service life (in days) of the most recently performed 0…104
service.
Reminder Determines whether the titrator should issue a warning before the Yes | No
service life or usable life of a resource elapses.
Days before expi Determines the number of days before expiry of the service life 0...1000
ration that the titrator should issue a warning.
The value entered here must be smaller than the service life.
(Appears only if "Reminder" is activated.)
6.4.2 Import/Export
You can use this function to save titrator data on a USB stick (export) and reload the data back to a titrator later
on (import).
Setup 31
Thus is it possible to create a backup of most data that has been changed from the titrator's default settings.
Uploading data from a backup copy results in the existing data in the titrator being overwritten. In this way you
can immediately duplicate the status of one titrator in another one or restore titrator settings after repair.
The following two rules should be observed:
● Memory copies can only be imported from the same type.
● Memory copies can only be imported from the same or from a lower software version.
You can select whether you want to export or import a backup copy, an individual method or the user manage
ment.
A backup copy includes, for example:
● All parameters of methods, series and firmware updates
● Setup inclusive of all resources
● All shortcuts
The backup copy does not contain all saved results, data saved on a PnP component and the default parame
ters for manual operations.
When you import/export an individual method you can select which method is to be exported or imported. You
require the right to edit methods.
When you import/export user management settings the entire user management settings with all users and
their properties are exported or imported.
In the Maintenance & Service dialog, open the Import / Export dialog window.
– In this dialog, you can define the following parameters:
Parameters Description Values
Action Here you can select whether you wish to export the titrator data to Export | Import
a memory stick or to import it from a memory stick to a titrator.
Data In this box you can select the data that you wish to export or Export | Import
import. You can select whether you want to export or import a
backup copy, an individual method or the user management.
Method ID Here you can select the Method ID for the relevant method. Method list
6.4.6 Terminal
You use the Terminal button to display the chip in the terminal.
32 Setup
6.4.8 Upgrade
You use this dialog to upgrade a titrator from a lower to a higher model. To do this, you will need a product key
that you can obtain from your METTLER TOLEDO Representative. You will need the data displayed in the screen
to order the product key:
You can easily transfer the data from this screen by pressing the "Print" softkey.
If you have received your product key, you can enter it via the "Product Key" softkey and perform an upgrade.
6.4.9 Update
You use the Update button to update the titrator firmware using a USB stick.
6.5 Values
Navigation: Home > Setup > Values
Blanks and auxiliary values can be created, edited and deleted and the list of defined blanks or auxiliary values
can be viewed and printed out. It is also possible to print out the individual values with their parameters.
Settings Explanation
Blanks Blank values can be used in formulas for calculations.
Auxiliary values You can use auxiliary values in formulas.
6.5.1 Blanks
Navigation: Home > Setup > Values > Blanks
Blanks can be used in formulas for calculations. They can either be created manually with the aid of their vari
ous parameters or generated as the result of a method. A resulting blank (or calculated mean value) can then
be assigned to a blank using the method function Blank. The blank will then appear under the assigned name
in the Blank list in Setup.
Adding a blank value
– In Blanks choose [New].
The windows to edit the parameters opens.
Setup 33
value by means of the "Auxiliary Value" method function. The auxiliary value then appears under the assigned
name in the auxiliary values list in the Setup.
Adding an auxiliary value
– In Auxiliary values choose [New].
The windows to edit the parameters opens.
34 Setup
7 Manual operations
You can use manual operations to access various titrator functions that are not directly connected to the execu
tion of an analysis, but that might be useful during the sample preparation, for example.
You can call up the following manual operations from here with the relevant titrator components:
Hardware com Possible manual operations Possible usages
ponents
Stirrer Stir Dissolve a solid sample
Pump Pump Fill, empty, or replace liquids.
Sensor Measure Voltametric indication
● Manual operations can also be executed while an analysis is running, if the hardware components that you
want to operate manually are not already being used by the analysis.
● The resource parameters in all editable fields can be changed temporarily (only for the execution of the
manual operation in question) and can vary from the setup settings. The changes made will not be copied
over to the setup, however.
7.1 Stirrer
To switch a connected stirrer (Rod stirrer or magnetic stirrer) on or off for a definable time interval and at a
definable stirring speed, select the following:
Navigation: Home > Manual > Stirrer
1 Make a selection in Titration stand.
2 Select the desired stirrer in Stirrer output and enter the speed in [%].
3 Enter the stir time in [sec] or select "∞" for an infinite duration.
4 Tap [Start] to start the stirrer.
The stirrer starts. Tap [Stop] to stop the stirrer at any time (terminating the manual operation).
7.2 Pump
Navigation: Home > Manual > Pump
You can use the Pump operation to fill or drain (depending on the hose connections) any volume of liquid from
the titration beaker using the Solvent manager.
Proceed as follows to start a pump process:
1 Choose the action that you want to perform (empty, fill, replace solvent).
2 Enter the duration of the relevant action in [sec].
3 Tap [Start] to start the measurement.
4 Tap [Stop] to terminate the procedure at any time.
You can determine the following parameters:
Manual operations 35
Parameters Description Values
Action Determines the actions for the pump process. Drain | Fill | Replace
reagent
Drain time Defines the pumping time for draining a fluid. 0...1000 | ∞
The duration of the drain operation for the tubes should be as
long as possible to ensure that the tubes are completely free of
liquids following draining.
Fill time Defines the pumping time for filling a liquid. 0...1000 | ∞
Reset counter If this parameter is set, all counters are reset when cell filling Yes | No
commences (applies to current capacity per number of sam
ples). The fill date for the cell is also reset.
Stirrer A stirrer can be switched on. Yes | No
Only for Action = Fill or Drain.
Titration stand The name of the titration stand. List of titration stands
only if stirrer is activated.
Stirrer output Specifies the stirrer output at the relevant board (only available if Internal stirrer | More
Stirrer is activated). depending on configu
ration
Speed Speed in [%]. 0…100
Only if stirrer is activated.
7.3 Sensor
Navigation: Home > Manual > Sensor
1 Select the sensor you want to use from the list of sensors defined in the settings.
2 Determine the polarization current.
3 Select the relevant titration stand.
4 Select the stirrer output for the stirrer and enter a speed.
5 Enter the duration of the measurement in [sec].
6 Select whether to output a record on the printer.
7 If you want to output a record on the printer, use dt [sec] to define the time interval between measurements.
8 Tap [Start] to start the measurement.
9 Tap [Stop] to terminate the procedure at any time.
During the measurement, the system will display the online curve (measured values in the selected unit versus
time). You can also tap [Measured values] to display a table of measured values instead of the curve.
You can define the following parameters for polarized sensors:
36 Manual operations
Record If activated, the measured values will be printed out. Yes | No
dt Defines the time interval in [sec] for outputting measured values 1…6000
to the printer.
Only appears if Record = Yes was selected.
Changes made in this dialog will only be applied to the manual operations "Sensor" and have no effect on the
settings made in the Setup.
Manual operations 37
8 Methods
To carry out an analysis with the titrator, you require a method. A method is an analysis program and consists
of a sequence of method functions (some with method subfunctions), which are processed by the titrator in
sequence.
In this chapter, you will learn how to access and define methods.
The basic building blocks of a titration method consist of sample preparation, stirring and wait times, the actual
titration, result calculation and a record. The titrator defines these partial steps as functions that consist of para
meters whose values can be changed.
Types of Methods
The titrator distinguishes between the following method types with different objectives:
● KF coul
Method for coulometric water content determination with the Karl Fischer method (according ASTM
D1492).
● Bromine Index
Method for coulometric Bromine Index (BI) determination.
● External Extraction
"External extraction" is a KF method for samples with extremely inhomogeneous water dissipation. It is also
used for insoluble solids which only release water slowly, even if broken into smaller pieces.
● Stromboli
Method for selecting the Stromboli oven sample changer as the titration stand.
Preloaded Methods
A number of methods have already been stored in the device. These methods were developed by METTLER
TOLEDO for specific uses and can be used immediately for the corresponding analysis.
You can change these methods in line with your requirements and save them as user methods.
When creating methods you can revert to method templates, which, according to their objective, specify the
structure of the method, and whose parameters already contain the most suitable default values.
Method ID
You can distinguish between different types of method and single methods of the same type using their ID:
● Each method has its own unique method ID.
● The method ID of the Mettler method for coulometric Karl Fischer titration, consisting of "KFC" followed by a
sequential number (KFC01, KFC02...).
● You can enter a name of your choice for the method ID for a user method, however it cannot begin with
"KFC" followed by a number.
38 Methods
ID Type Title Description
M391 KF coul Toluene dry Water content determination of a
sample with a water content in the
ppm range
M392 KF coul Nitrogen gas Water content determination of a
gaseous sample with a water content
in the ppm range
M393 KF coul Acetone dry Water content determination of a
ketone-containing sample with a
water content in the ppm range
M394 KF coul external extraction Sugar (external extrac External extraction of a sample with a
tion) water content in the ppm range
M395 KF coul PET granulates (manual Manual gas phase extraction of a
oven) sample with a water content in the
ppm range, using the DO308 oven
M396 KF coul Stromboli Temp.ramp (Stromboli) Automatic gas phase extraction with
one blank loop and 13 sample loops
with different temperatures: From 120
°C to 300 °C in 15° increments. Pro
posal: Polycarbonate or polyamide
as sample.
M397 Bromine index (1 loop) Bromine index Bromine index determination in
mg/100g using a blank value
M398 Bromine index blank Bromine index Determining the blank value of an
electrolyte
M399 Bromine index (2 loops) Bromine index Bromine index determination with
one conditioning loop and one loop
for determining the bromine index of
the sample
The polarizable electrode DM143-SC is used as a sensor.
Methods 39
11 After inserting all required method functions, tap [Save].
The method is saved under the method ID and appears in the list of available methods.
● When establishing a new method, follow the rules specified by the instrument.
40 Methods
8 Modify the individual parameters of the method function.
The new method function appears in the method.
1 To delete a method function, select the function in question and then choose Delete.
2 After you have made all of the necessary adjustments, you can store the method in the titrator by choosing
Save.
Deleting Methods
You can easily delete user-defined methods from the titrator. Select:
Home > Methods
1 Select the method that you want to delete.
2 Choose Delete method to delete the method from the titrator's memory.
You can use the method editor to start any method stored in the titrator.
1 From the displayed list in the Methods dialog, select the method that you wish to start (Home > Methods).
2 As soon as the method functions of the selected method appear on the screen, you can open the Start
analysis screen by choosing Start.
3 Choose Start again to reach an overview screen on the resources required for the method. (Only if this was
defined in the analysis sequence settings.)
4 To execute the method, confirm the screen by choosing OK.
Methods 41
8.6.1 Possible Number of Method Functions
The following table shows the method functions for the Karl Fischer method types (KF coul, external extraction,
Stromboli and Bromine index). The maximum number of functions per method is listed.
Number of functions per method for KF coul, external extraction, and Stromboli
Method function Max. number per method for Max. number for Stromboli
all KF method types except methods (for C30 only)
Stromboli
C20 C30
Title 1 1 1
Sample (KF) 1 1 14
Titration stand 1 1 14
Titration (KF coul) 1 1 14
Calculation 3 40 40
End of sample 1 1 14
Auxiliary value - 30 30
Blank - - 10
Instruction 1 10 10
Report 1 10 14
Drift determination - - 14
Mix time 1 1 15
Homogenizer - - -
Standby (Stromboli) - - 1
Number of functions for Bromine Index (BI)
Number of functions Max. number for BI
Title 1
Sample 3
Titration stand 3
Titration (EP coul) 3
Calculation 40
End of sample 3
Auxiliary value 30
Blank 10
Instruction 10
Report 10
Mix time 3
Different numbers of KF loops are allowed within a method, depending on the method type:
Method type Maximum number of loops per method
KF coul 1
External extraction 1 (for C30 only)
Stromboli 14 (for C30 only)
Bromine index 3 (for C30 only)
42 Methods
8.6.3 Sample loops
Stromboli
Two templates exist for the "Stromboli (KF coul)" method type; one with and one without a blank value. The
template for the KF sample loop with the "Blank value" method function is shown below (for C30 only):
Sample loop (KF): Sample (KF)
Titration stand (Stromboli)
Mix time
Titration (KF Coul)
Calculation
Report
End of sample
Blank
Bromine Index
Three templates exist for the "Bromine index" method type:
Sample loop: Sample
Titration stand (KF)
Mix time
Titration (EP Coul)
Calculation
Report
End of sample
The following method functions are only available for the "Stromboli" method type (for C30 only):
● Blank
● Drift determination
Methods 43
Bromine index
The following method functions are permitted within a bromine index method:
● Titration stand (KF stand | External KF stand)
● Mix time
● Titration (EP coul)
● Auxiliary value
● Instruction
● Record
● Calculation
● Blank
The selection option depends on the sequence of the KF method (see above) .
The "Standby" method function must be in the final position in the method.
Method type "Bromine index"
For the method type "Bromine index", you can use the following method functions:
● Calculation
● Auxiliary value
● Blank
● Instruction
● Record
44 Methods
Functions Explanation Within loop Outside loop
Auxiliary value Assigns a result or an Yes Yes
arbitrary value to an auxil
iary value and updates
the value stored in Setup.
Instruction Halts the analysis and Yes Yes
displays instructions on
the screen for the user.
Record Defines the record data to Yes Yes
be output to the printer.
Drift determination Determines the drift for Yes Yes
Karl Fischer titrations
(only for method type
"Stromboli").
Blank Assigns a result or an Yes Yes
arbitrary value to a blank
and updates the value
saved in the setup (only
for method type
"Stromboli").
Calculation Converts the analysis Yes Yes
results.
End of sample Concludes a sample loop. End of loop Yes
Standby Returns the titrator to No Yes
standby mode on comple
tion of the "Stromboli"
series, so that new series
can be started quickly.
The following sequence must be observed within the Karl Fischer loop:
1. Sample
2. Titration stand
3. Drift determination (only for Stromboli)*
4. Mix time
5. Titration
6. Calculation*
7. Record*
8. End of sample
9. Standby*(only for Stromboli)
8.8.1 Title
Defines the title and type of a method of a method, and manages properties such as the creation and change
date, the author, and whether or not the method is to be protected.
Parameters Description Values
ID Unique ID of the method. arbitrary (cannot start
with "M" followed by a
numeric character)
Title Title of the method. Arbitrary
Protect Protects the method against changes and Yes | No
deletion by any user other than the author or the administrator.
Methods 45
SOP Standard operating procedure None | Text | Link
(SOP: (SOP)
SOP-Text Text for a standard operating procedure Arbitrary text
(if "SOP" = "text" is selected.)
SOP ID ID for the link to a standard operating procedure (if "SOP" = "link" Arbitrary
is selected.)
46 Methods
Solvent weight Quantity of solvent in [g] in which the sample was extracted or 0...1000
dissolved.
Only for method type = Ext. Extraction.
Wt. extracted Total weight of sample in [g] which was extracted or dissolved in 0...1000
sample the solvent.
Only for method type = Ext. Extraction.
Correction factor Any correction factor that can be used in calculations. 0.0001…106
Temperature The temperature in [°C] during the analysis. -20…200
Autostart If activated, KF titration starts following a significant signal Yes | No
increase within 30 seconds after the start of the analysis (not for
Stromboli methods).
If deactivated, the sample addition must be confirmed before
titration can begin.
Analysis start If Automatic is selected, the analysis begins without any user Automatic | Manual
confirmation if the value falls below the maximum start drift and
the defined stability criterion Drift stability/dt and the set temper
ature are reached.
If the standby is executed by the method function Standby (only
for Stromboli), the automatic start is not performed (affects the
2nd, 3rd....series).
If the analysis is started manually, the Stromboli series must be
started explicitly in the Standby dialog.
Drift stability Maximum permitted drift difference in [µg/min]. 0...1000
Only for "Stromboli" method type and if Analysis start = Auto
matic is selected.
dt dt in [sec] is the time taken to determine the drift stability. The 1…1000
time recording can begin before the set temperature is reached
and before the value falls below the maximum start drift.
Only for "Stromboli" method type and if Analysis start = Auto
matic is selected.
Entry Determines the input time for the sample size. Arbitrary | After addi
Before: The sample size must be entered before the titration. tion
Arbitrary: The sample size will have to be entered at any time
during the titration (no later than when it is used during the cal
culations). Only appears if for Entry type no "Fixed" values are
selected.
After addition: You are prompted to enter the sample data once
the sample has been added. The sample size - even during the
method execution - can be entered later on (however, no later
than when required for use in formulas).
Subfunction: Blank value (for method type: external extraction)
The "Blank value" method function assigns a determined water content to the solvent. The blank can be a fixed
value, can be taken from the setup, or can be requested by the system.
You can determine the following parameters:
Parameters Description Values
Source for blank Setup: After the blank value is determined, the value and the unit Setup | Fix value [%] |
of the blank are transferred to the settings. Fix value [ppm] |
Fix: The value defined in the method is used. Request [%] | Request
[ppm]
Request: The blank value in the relevant unit is requested before
each sample.
The specified blank value is labeled with "B" in the method func
tion Calculation.
Value Here you can enter a numerical value. 0...106
Only appears if for Entry type "Fixed" values are selected.
Blank The blank value assigned to the solvent to be determined. Value from the settings
You can select a blank value defined in the settings.
Methods 47
Unit Defines the unit in which the blank value is calculated and used % | ppm
in a calculation. The unit for calculation with a blank value must
be the same as the unit set here.
Applies for the Setup option only.
Entry type Defines whether the sample should be added with a defined Weight | Fixed weight |
mass or defined volume. The sample data query will then adjust Volume | Fixed volume
according to the unit of measurement.
For Fixed weight or Fixed volume, the sample mass and the
sample volume are entered as parameters in the method function
and not requested in the sequence of the method.
Lower limit Defines the lower limit for the variable entry of sample data in 0...1000
[mL] or [g]. The unit will depend on the setting for Entry type
parameter.
Applies only for Entry type = Weight and Volume.
Upper limit Defines the upper limit for the variable entry of sample data in 0...1000
[ml] or [g]. The unit will depend on the setting for the Entry type
parameter.
Applies only for Entry type = Weight and Volume.
Weight Weight in [g]. 0…1000
Appears only if Entry type = Fixed weight was selected.
Volume Volume in [mL]. 0…1000
Appears only if Entry type = Fixed volume was selected.
Density The density of the liquid sample in [g/mL] for Entry type = Vol 0…1000
ume or Fixed volume.
Mix time The duration of stirring in [s] with the defined "Stir" speed. 0…104
Autostart If activated, KF titration starts following a significant signal Yes | No
increase within 30 seconds after the start of the analysis (not for
Stromboli methods).
If deactivated, the sample addition must be confirmed before
titration can begin.
Entry Determines the input time for the sample size. Arbitrary | After addi
Before: The sample size must be entered before the titration. tion
Arbitrary: The sample size will have to be entered at any time
during the titration (no later than when it is used during the cal
culations). Only appears if for Entry type no "Fixed" values are
selected.
After addition: You are prompted to enter the sample data once
the sample has been added. The sample size - even during the
method execution - can be entered later on (however, no later
than when required for use in formulas).
Limits Determines whether limits should be taken into account for Yes | No
acquisition of a value. If the value is outside these limits, the val
ue is not transferred to Setup.
Upper limit Defines the upper blank limit. Appears only if "limits" = "yes" was 0...106
selected. Outside these limits, the blank value is not entered in
the setup.
See also
● Blanks (page 33)
48 Methods
Source for drift Online (not for Stromboli): For calculations, the drift determined Online | Determination
in the online procedure is used. | Fix value | Request
Determination: The drift saved in the titration stand setup for the
KF titration stand selected in the method is used.
Fix value: The drift value determined in the method.
Request: The drift value is requested before each sample or
Stromboli series.
Drift Value of the drift in [µg/min]. 0...1000
Max. start drift The maximum drift for which a sample determination can still be 0...1000
started.
Oven tempera Temperature setting in [°C] for the "Stromboli" oven sample 50...300
ture changer.
Only for Titration stand = Stromboli TTL.
Methods 49
Generator cur You can select whether the pulse strength is regulated automati Automatic | Fix
rent cally or whether the user enters a required fixed pulse strength.
Current The current can be selected with fixed generator currents. 400 | 300 | 200 | 100
Subfunction: Termination
Parameters Description Values
Type Termination of titration following defined drift and if the value falls Drift stop relative |
below the end-point value (EP). Drift stop absolute |
Drift stop relative: Actual drift stop value = online drift + drift Delay time
Drift stop absolute: Actual drift stop value = drift
Delay time: Termination after a delay time below the EP.
Drift The drift value in [µg/min] for the termination criterion drift stop 1.0 ... 106
relative or drift stop absolute.
Delay time Time in [s] from the time the end point is first reached until the 0...6000
termination of the titration.
Min. time Titration is not to be terminated before this time in [s] is reached 0...108 | Auxiliary value
(exception: the maximum volume has been reached).
Max. time Maximum duration of the titration (without post-consumption 0...108 | ∞ | Auxiliary
measurement). value
50 Methods
Subfunction: Termination
Parameters Description Values
Type Termination of titration following defined drift and if the value falls Drift stop relative |
below the end-point value (EP). Drift stop absolute |
Drift stop relative: Actual drift stop value = online drift + drift Delay time
Drift stop absolute: Actual drift stop value = drift
Delay time: Termination after a delay time below the EP.
Drift The drift value in [µg/min] for the termination criterion drift stop 1.0 ... 106
relative or drift stop absolute.
Delay time Time in [s] from the time the end point is first reached until the 0...6000
termination of the titration.
Min. time Titration is not to be terminated before this time in [s] is reached 0...108 | Auxiliary value
(exception: the maximum volume has been reached).
Max. time Maximum duration of the titration (without post-consumption 0...108 | ∞ | Auxiliary
measurement). value
8.8.9 Blank
This method function assigns a result or an arbitrary value to a blank value, including units (only for methods
of type "Stromboli").
Parameters Description Values
Name Specify a descriptive name of your choice. Arbitrary
Value B= Here you can enter a formula that will be used to convert the Formula (see "Evalua
sample loop result to the blank. You can also enter a number or tion and Calculation
an auxiliary value. (page 69)") | Auxiliary
Value | Number
Unit The units in which the blank is specified. Arbitrary
Limits Determines whether limits should be taken into account for Yes | No
acquisition of a value. If the value is outside these limits, the val
ue is not transferred to Setup.
Interruption out Determines whether the method should be interrupted if a value Yes | No
side limits lies outside the defined limits (only appears if the "Limits" para
meter has been activated).
A message (which must be acknowledged) appears advising
that the process has been interrupted during the time that the
message is displayed.
Lower limit Appears only if "limits" = "yes" was selected. -108 … 108
Methods 51
Upper limit Appears only if "limits" = "yes" was selected. -108 … 108
8.8.10 Instruction
Interrupts the analysis and outputs an on-screen instruction to the user. Either the user has to confirm the
instructions or they will disappear automatically after a certain period.
Parameters Description Values
Instruction The text of the instructions to be output to the display. Arbitrary, including
This text can also contain a formula or auxiliary values, enclosed enclosed formula (con
in percent symbols. trol characters: %)
Example: "Add %VEQ*m/z% g".
Continue after Confirmation: The analysis will continue as soon as the user Confirmation | Time
confirms the instructions. interval
Time interval: The analysis is continued after the defined time
period has elapsed.
Time interval The time period, in [sec], during which the analysis is terminated 0…106
and the instructions are displayed on the screen.
Only appears if Continue after = Time interval is selected.
Print If selected, the instructions will be output to a connected printer. Yes | No
8.8.11 Calculation
For converting the titration results.
Parameters Description Values
Result type If the result type "Automatic" is selected, a predefined result from Automatic | User defined
the proposal list is used. The parameters "Result", "Unit", "Formu
la", and "Constant" are adjusted automatically in accordance
with the entry type selected in the method function sample (KF)
and cannot be changed.
If "User defined" is selected, all parameters can be edited. You
can also select a predefined result type from the results proposal
list.
● The "Result type" parameter is not available for KF titrators in the 20 series, and is set to "Automatic".
● "Result type" is hidden for the "Stromboli" method type and is fixed to "user-defined".
Result After selecting a result from the dropdown list, the system will Results list | Arbitrary
automatically set the "Result unit", "Formula" and "Constant"
parameters. But you will be able to make any changes to them
that you would like without having the system adjust the other
parameters. You can also enter any number.
Result unit The unit of the result. (Is not automatically adjusted after changes Device list | Arbitrary
to "Formula" or "Constant".) You can also use "Proposal" to
select from a predefined suggestion list.
Formula The formula for calculating the result. You can use "Results pro Formula list | Arbitrary
posals" to select from a predefined suggestion list.
Constant Definition of the C constant which can be used in the calculation. Constants list | Arbitrary
The constant can itself be a formula. You can also use
"Proposal" to select from a predefined suggestion list.
Decimal places The number of decimal places for the result. 0…6
Result limits Defines whether limits should be observed for the result. If this Yes | No
function is activated, there will be a message in the record if the
result falls outside the defined limits.
Lower limit Defines the lower result limit. -108 … 108
Appears only if "result limits" = "yes" was selected.
Upper limit Defines the upper result limit. -108…108
Appears only if "result limit" = "yes" was selected.
52 Methods
Interruption out Determines whether the method should be interrupted if a value Yes | No
side limits lies outside the defined limits (only appears if the "Limits" para
meter has been activated).
A message (which must be acknowledged) appears advising
that the process has been interrupted during the time that the
message is displayed.
Record statistics Specifies whether statistics should also be issued with the results Yes | No
in the report along with the result.
The statistics are not printed, if in the method function "Protocol"
the parameter "Results" = "No" is selected.
Extra statistical You can use this parameter to switch on extra statistical func Yes | No
functions tions. For example, this will allow you to define a maximum val
ue for the relative standard deviation which, if violated, will cause
individual results to be listed in the record. The settings for this
parameter will only be taken into consideration if the "Calcula
tion" method function is used within a sample loop.
Multiple determi This function helps you do statistical evaluations of sample Yes | No
nation groups.
The sample groups are defined with the "Number of samples"
parameter.
Appears only if "additional statistic functionalities" = "yes" was
selected.
Max. srel If the relative standard deviation for the calculated result is above 0…100
the "Max. srel", the system will output a corresponding message
in the record. Appears only if "Extra statistical functions" = "Yes"
was selected (and if available "Multiple determination" = "Yes").
Number of sam Defines the sample groups for a multiple determination. For 2…9
ples example, a value of 3 means that the system will run a statistical
evaluation on three consecutive samples.
Appears only if "Extra statistical functions" and "Multiple determi
nation" = "Yes" were selected.
Interruption Specifies whether an analysis series should be terminated as Yes | No
above max. srel soon as the relative standard deviation of a sample group within
a multiple determination is above the "Max. srel".
Appears only if "Extra statistical functions" and "Multiple determi
nation" = "Yes" were selected.
Record If "yes" is selected for "Record", the multiple determination func Yes | No
tion will create a record listing the groups after a double determi
nation whose relative standard deviation lies above a "Max. srel"
number defined in the method.
Appears only if "Extra statistical functions" and "Multiple determi
nation" = "Yes" were selected.
8.8.12 Report
This method function defines the type and scope of the data to be output for a report using the printer (see
"Hardware>Peripherals: Printer").
If the method function "Record" is placed within a sample loop, the record will include all previous method
functions within the current sample loop.
If the method function "Record" is placed outside of a sample loop, the record will include all previous method
functions listed after the last sample loop in the method procedure. A few settings are not available outside of a
loop.
Parameters Description Values
Overview States whether or not a short summary of the results should No | Per sample | Per
appear at the top of the protocol. series out of loop: No |
Yes
Results The results from the "Calculation" method functions. Any statistic within loop: Per Sam
selected will be recorded after the last sample of a series or mul ple | Per Series | No Out
tiple determination. of Loop: No | Yes
Methods 53
Raw results The raw results produced during the determination within loop: Per Sam
ple | Per Series | No Out
of Loop: No | Yes
Measured value The table of measured values of the current sample (not avail Yes | No
table able out of loop).
Sample data The sample data of a sample loop. (Not available outside of Per sample | Per
loop) series | No
Resource data All data in the setup regarding the resources used in the method. Per Sample | Per
Series | Non Per Sample
| Per Series | No
E-C Titration curve of the current sample. The potential is plotted Yes | No
against the load (not available out of loop).
E–t Titration curve of the current sample. The potential is plotted ver Yes | No
sus the time (not available outside of loop).
C-t Titration curve of the current sample. The load is plotted against Yes | No
the time. (not available outside of loop)
H2O -t Titration curve of the current sample. The water content is plotted Yes | No
against the time (not available out of loop).
Drift-t The titration curve "Drift" against "Time" (not available out of Yes | No
loop).
H2O-t & Drift-t Two overlaid titration curves "H2O – t" and "Drift-t" of the current Yes | No
sample (not available out of loop).
C - t & Drift - t Two overlaid titration curves "C-t" and "Drift-t" of the current sam Yes | No
ple (not available out of loop).
8.8.14 Standby
The "Standby" method function can only be inserted in methods of the type Stromboli after the method function
"End of sample". This method function determines whether the method is terminated at the end of the series, or
if the method remains active and then enters standby mode for the first loop.
54 Methods
9 Series Templates
Series templates are used for a sequential series of samples processed using the same method (templates for
sample series (SAS)).
Using series templates, you can group multiple (up to 120) individual samples into one sample series, so
that all the samples in the series can be analyzed consecutively using a defined method.
The list of series templates shows you all the series templates defined in the titrator. Each series template is
shown in the list with its type (SAS = Sample series) and name.
If you select a series template from this list, you can change its parameters or delete the entire template.
● You can create a shortcut on the Home screen for all series templates.
● A maximum of 60 sample series can be saved in the titrator.
● Series templates cannot be created for blank samples.
Series Templates 55
Solvent weight Quantity of solvent in [g] in which the sample was extracted or 0...1000
dissolved.
Only for method type = Ext. Extraction.
Wt. extracted Total weight of sample in [g] which was extracted or dissolved in 0...1000
sample the solvent.
Only for method type = Ext. Extraction.
ID 2…ID 3 The name defined here will be used as the default name for the Arbitrary
respective sample on the sample loop.
Only appears subject to the settings made for Number of IDs.
Comment You can enter a brief comment about the series. Arbitrary
Correction factor Any correction factor that can be used in calculations. 0.0001…106
Temperature The temperature in [°C] during the analysis. -20…200
For entering the sample parameters, particularly for numerous samples, the titrator provides you with assis
tance in the entry windows of the "ID 1" and "Sample size" parameters:
These extra icons are a quick, direct way to jump to the entry window of the previous sample or next sample.
56 Series Templates
10 Results
The Results dialog can be accessed directly from Home using the relevant button.
● In the C20, only the results of the last analysis are saved, in the C30, the results of the last two analyses
can be selected by pressing the Select series button.
● When you start a new analysis, you will lose the results from the previous analysis.
● You can view results immediately after they have been recorded (for the same determination type:sample or
blank determination).
You can use the various buttons in the "Results" dialog to call up different functions. You can, for example,
● view all results of the last analysis (C20) or the last two individual samples or series (C30).
● add a supplementary result calculation both within the loop (for all samples in the analysis), and outside a
loop (once for the entire analysis).
● view statistics, perform an outlier test and if necessary, exclude samples from the statistics.
● perform recalculations for results in which certain raw data (e.g. sample sizes) have to be adapted retro
spectively for a single sample or for all samples in a series.
● view and print the status and the calculated results of each individual sample.
Results are stored until new results are generated by methods. The results of the "older" of the two sample
series are replaced.
In KF methods, the End series function can be used to generate a new result entry during the execution of a
method. After the series is finished, the original sample parameters are used, i.e. the changes made in the Start
analysis dialog or later are not taken into account. A new series is entered in the results.
In Karl Fischer (KF) titrations, the results are divided into the determination types:Sample and blank. All options
for managing results only have an effect on the determinations of one particular determination type.
While an analysis is running, only the current determination type is available.
If a determination type ("Sample", "Blank") is started for a second time, existing data is overwritten.
All the changes performed on the saved results can be reversed with the "Undo changes" button.
Changes to results are indicated by an asterisk in the record. Example: Changes to the results are marked by
an asterisk in the record, e.g., VEQ*.
Results 57
Result Unit Replace "m" Formula R = Constant
according to entry
type
Content mg -- R= C = 1,000
µg -- (ICEQ/10.712-TIME*DRIFT)/C C=1
% g R=(ICEQ/10.712- C = 10,000
ppm ml: m*d TIME*DRIFT)/(C*m) C=1
mg/g pc: m*wp C = 1,000
g/kg C = 1,000
µg/ml ml C=1
mg/ml g: m/d C = 1,000
mg/pc pc C = 1,000
µg/l ml C = 0.001
g: m/d
g/ml ml C = 1,000,000
g: m/d
58 Results
Result Unit Replace "m" Formula R = Constant
according to
entry type
Content blank value mg -- R=(ICEQ/10.712–TIME*DRIFT- C = 1,000
compensated (B in µg -- B[Blank Stromboli])/C C=1
µg) % g R=(ICEQ/10.712– C = 10,000
ppm ml: m*d TIME*DRIFT- C=1
mg/g pc: m*wp B[Blank Stromboli])/(C*m) C = 1,000
g/kg C = 1,000
µg/ml ml C=1
mg/ml g: m/d C = 1,000
mg/pc pc C = 1,000
µg/l ml C = 0.001
g: m/d
g/ml ml C = 1,000,000
g: m/d
Results 59
10.3 Add result
You can use the Add result button to add a subsequent result calculation to your analysis results. To do that,
you will first have to specify whether the calculation should be run inside or outside a loop. For calculations
within a loop, the result will be added for all the samples (of the same loop) of a series. You may still be able
to select the required loop. The other parameters must be entered in accordance with the "Calculate" method
function. (See "Method Function Settings").
You can use the Calculate button to calculate the additional result and add it to your analysis results. If you are
missing raw data or raw results for the calculation and cannot calculate the result for that reason, the result
"NaN" (Not a number) will be added.
Predefined results (see "Evaluation and calculation>Formulas>Results proposal lists") for the volumetric Karl
Fischer titration, you can view the following by selecting the Results proposals button in the Add result dialog.
10.4 Statistics
For results within a sample loop, you can display and print out statistics.
● The statistics are only created if more than one sample was analyzed in the corresponding loop.
● If you selected "Statistics functionalities" = "Yes" and "Multiple determination" = "Yes" in the associated
"Calculate" method function, the system will create the statistics for the entire series and also individually for
multiple samples within the series.
The following calculated values will be displayed as statistical components:
● Mean value x of a result Rx (Mean [Rx])
● Standard deviation s
● Relative standard deviation srel
● Number of samples per loop nTOT
If a result was excluded from the statistics, all the results from that sample will always be excluded as well. The
system will then recalculate the statistics without the excluded sample and label them accordingly. If the sam
ple's results are then put back into the statistical evaluation, the label will be removed from the statistics.
From the Statistics dialog, you also have the following additional options:
● Samples View, print, or exclude the results of an individual sample
● Results View or print all results
● Outlier test Perform a test for outliers in the statistical evaluation.
x* - x
PG =
s
60 Results
The test variable [PG] is then compared with the corresponding value in the Grubbs table G (N, 90%), which
in turn depends on the number of measured values N:
N (number of samples) 1 2 3 4 5 6 7 8 9 10
90 % - - 1.15 1.46 1.67 1.82 1.94 2.03 2.11 2.18
N (number of samples) 11 12 13 14 15 16 17 18 19 20
90 % 2.23 2.29 2.33 2.37 2.41 2.44 2.48 2.5 2.53 2.56
N (number of samples) 21 22 23 24 25 26 27 28 29 30
90 % 2.58 2.6 2.61 2.63 2.65 2.67 2.69 2.7 2.72 2.74
N (number of samples) 31 32 33 34 35 36 37 38 39 40
90 % 2.75 2.77 2.78 2.79 2.81 2.82 2.83 2.84 2.86 2.87
N (number of samples) 41 42 43 44 45 46 47 48 49 50
90 % 2.88 2.89 2.9 2.91 2.92 2.92 2.93 2.94 2.95 2.96
N (number of samples) 51 52 53 54 55 56 57 58 59 60
90 % 2.97 2.97 2.98 2.99 3 3 3.01 3.02 3.02 3.03
N (number of samples) 61 62 63 64 65 66 67 68 69 70
90 % 3.03 3.04 3.04 3.05 3.05 3.06 3.06 3.07 3.07 3.08
N (number of samples) 71 72 73 74 75 76 77 78 79 80
90 % 3.08 3.08 3.09 3.09 3.1 3.1 3.11 3.11 3.12 3.12
N (number of samples) 81 82 83 84 85 86 87 88 89 90
90 % 3.12 3.13 3.13 3.14 3.14 3.15 3.15 3.16 3.16 3.17
N (number of samples) 91 92 93 94 95 96 97 98 99 100
90 % 3.17 3.17 3.18 3.18 3.19 3.19 3.2 3.2 3.21 3.21
N (number of samples) 101 102 103 104 105 106 107 108 109 110
90 % 3.21 3.22 3.22 3.22 3.23 3.23 3.23 3.23 3.24 3.24
N (number of samples) 111 112 113 114 115 116 117 118 119 120
90 % 3.24 3.22 3.25 3.25 3.26 3.26 3.26 3.26 3.27 3.27
If the calculated test variable PG is greater than the corresponding value taken from the table, the measured val
ue x* is identified as an outlier and marked accordingly.
After an outlier has been identified, the test is repeated with the remaining measured values (without the already
identified outlier) using the newly calculated mean value and new standard deviation. This process is repeated
continually until no further outlier can be identified.
It is then the user's responsibility to exclude any identified outliers from the statistics. After confirmation, the
entire sample is excluded and the statistics are recalculated without the identified and excluded outliers.
10.5 Samples
You can use the Samples button to display and print the status and calculated results for each individual sam
ple. The same applies for a series of additional data sets that can be accessed via "Data". This will let you view
and print the sample, method and resource data for each sample and view and print the raw results and the
measured values.
You can use the Exclude button in the Results: Samples dialog to exclude individual samples from the statisti
cal evaluation. The system will not delete the results of the samples excluded in this way but merely label them
as excluded. They will no longer be included in the statistics. Samples that have been excluded can be returned
to the statistics at any time by choosing "Include".
After a sample is excluded, all affected calculations (inside and outside of loops) are performed again. In KF
titrations, the new calculations refer only to the current determination type.
If you exclude a sample from a sample group in a multiple determination, no more statistics will be generated
for that group. The system will continue to create individual statistics for the remaining sample groups and for
all the remaining samples overall.
Results 61
10.7 Delete all results
You can use this button to delete all the data (raw data, raw results, and results) saved by the titrator in the
results area. The deletion only ever refers to one determination type. If the last determination type in the sample
series is deleted, the whole sample series is automatically deleted.
62 Results
11 Analysis Sequences
11.1 Starting an Analysis
An analysis, whether it be a single or multiple determination, can be started on the titrator in several different
ways:
1. By choosing the following options:
• Start from the method editor
• Start from "Home"
• Start from the "Series" dialog
2. Using a user-specific shortcut or a direct shortcut from "Home".
When you create a shortcut by choosing AddToHome (see "Description of Functions > The User Interface >
Shortcuts and Direct Shortcuts"), the following parameters are available:
Parameters Description Values
Description Any name for the shortcut. Arbitrary
Immediate start The method, series, or manual operation can be started immedi Yes | No
ately. This enables you to start the analysis without any interfer
ing dialog.
Homescreen You can select the free position for the shortcut on the Home 1…12
position screen.
After you create the shortcut, it appears in the selected position in "Home", from where you can select it by tap
ping the touchscreen.
When you start an analysis, whether by using a button or with a shortcut, the system always opens the Start
analysis dialog (see "Descripton of Functions > The User Interface > The Start Analysis Dialog"). The only
exceptions are direct shortcuts ("Immediate start" = "Yes"), whose selected settings permit a direct start.
At the start of an analysis, you can still make changes to various settings in the Start analysis dialog. It is
therefore possible, for example, to modify the sample size and define the number of samples to be determined.
If the analysis you want to start is a single determination, you can enter the sample size or sample ID directly
as a parameter in the Start analysis dialog.
In general, the sample data can be entered for each individual sample using the Samples button in the Start
analysis dialog. In the Sample data dialog that opens when you choose this button, a list of the individual
samples is displayed.
In addition, the status is displayed for every sample (regardless of the loop type) in the Sample data dialog.
The following status levels can be assigned to a sample:
● Idle: The sample is not yet running and the sample data can still be edited
● Running: The sample is running but the sample data can still be edited
● Active: The sample is running and the sample data can no longer be edited
● Done: Done – the sample has run and concluded and the sample data can no longer be edited
If you select a sample, you can define the following sample data.
Parameters Description Values
ID 1 The ID for the first or only sample of an analysis. Arbitrary
Sample size You can enter the sample size here. 0…1000 [g] | [mL]
For fixed entry types, this field only appears as an info field. 0…106 [pcs.]
Density You can enter the sample's density, in [g/mL], here. 0…100
Does not appear for the Entry type = Pieces and Fixed pieces.
Weight per The weight in [g] per pirece. 0 … 1000
piece Appears only if Entry type = Pieces or Fixed pieces was select
ed.
Solvent weight Quantity of solvent in [g] in which the sample was extracted or 0...1000
dissolved.
Only for method type = Ext. Extraction.
Analysis Sequences 63
ID 2…ID 3 The name defined here will be used as the default name for the Arbitrary
respective sample on the sample loop.
Only appears subject to the settings made for Number of IDs.
Comment You can enter a brief comment about the series. Arbitrary
Correction factor Any correction factor that can be used in calculations. 0.0001…106
Temperature The temperature in [°C] during the analysis. If temperature moni -20…200
toring is activated in a titration function, the system will ignore
the sample temperature given here.
You can enter the following parameters in the Start analysis dialog, depending on the type of analysis to be
started and the resources used:
Parameters Description Values
Number of sam Defines the number of samples to be analyzed. 1…120
ples
ID 1 The ID for the first or only sample of an analysis. Arbitrary
Sample size You can enter the sample size here. 0…1000 [g] | [mL]
For fixed entry types, this field only appears as an info field. 0…106 [pcs.]
Continuous run After each termination of the analysis (using series or methods) Yes | No
the analysis is automatically restarted (this is done until the
process is canceled manually).
(Only for method type "Bromine index")
● All the parameters that can be edited in the Start analysis dialog or the sample data dialog will overwrite
the settings defined in the method for the same parameters.
● All non-editable parameters that are displayed as an info field are only shown for orientation purposes and
list the settings from the method.
● If the sample size must be entered before the analysis but the user does not do so, the user will be required
to enter it immediately before the start of the analysis.
Dialog: Start analysis This dialog can be switched off for a start using the "Shortcut
parameters" dialog and the "Immediate start" parameter when
creating or managing a shortcut.
64 Analysis Sequences
<Start>
Check: Resources Can be switched off with the "Display required resources at start"
parameter in the analysis sequence settings. (An error message
will appear if the resources have already been allocated or are
missing.)
<OK>
Online dialog: Pretitration Selection of function options: Terminate method, Samples (for
changing samples and series data), End series, Save series
data, Results, Axes,
(see " Description of functions>User
interface>Online dialog").
Automatic switch between Pretitration and Standby.
Online dialog: Standby Selection of function options: Start sample, Start blank (for
external extraction, Samples (for changing samples and series
data), Start drift determination, End series, Terminate method,
Save series data, Results*, Axes, Sample size calculation
(see " Description of functions>User
interface>Online dialog ").
<Start sample> | <Start blank> If the maximum number of samples or blank determinations has
been reached and a measurement has been started, a message
appears informing you that a new series can be started.
From the start of the first sample analysis in a predefined series
to the processing of the last sample in the series, the blank deter
mination function cannot be selected in the "Standby" dialog.
If the voltage value of the measuring sensor is too low at the start
of a sample, drift, or blank determination, when the user presses
Start, they are informed that the system is overtitrated.
<OK>
Online dialog: Mix time Displays the time remaining and stirrer speed.
Online dialog: Titration (KF coul) You have the following options during an analysis: To cancel the
sample, drift, or blank determination or the method, you can
modify sample data, view results or measured values, save a
series, or specify the axes of the measurement diagram.
Analysis Sequences 65
Online dialog: Standby
*During Standby or Pretitration mode, you can access the results of the current determination type (sample or
blank determination). Here you can perform the following actions (see "Results"):
● Recalculate (can only be changed for individual samples, and not for a whole loop)1
● Exclude samples1
● Perform outlier test1
● Results
● Display statistics
● Undo changes
1For titrations using the "Stromboli" oven sample changer, these functions are only available at the start of the
series or in Standby mode and with Start analysis "manual".
Drift determination
There are several different ways to determine the drift:
1. Using the "Drift determination" method function. Here you can enter the duration of determination. The
method function can be inserted outside the loop (in determination per series) or inside the loop (in deter
mination per sample) (only for KF methods of the type "Stromboli").
2. Spontaneous drift determinations: The drift can be determined from Standby mode of any KF method. The
drift determined here is used if the "Source for drift" parameter in the "Titration stand" method function is set
to "Setup".
3. Online drift determination: The drift that is constantly determined during standby operation is the current and
correct drift value which is used in the calculations. To enable this, the "Source for drift" parameter in the
"Titration stand" method function must be set to "Online" (see "Method functions: Titration stand").
Once the titration is complete, Standby mode is active until the end of the loop in the current sample beaker. If
the system is switched to Pretitration mode during this time, the sample changer returns to the start position
(beaker in the drift position) and performs the pretitration followed by the standby titration.The analysis of the
next sample is then continued automatically when the maximum start drift value is reached. If the last sample
in a loop has been processed and further loops still remain, the current position (sample or drift beaker) is
maintained until the next sample is approached. The current drift is reviewed before the start of the next sample.
The following is a description of the behavior when particular actions are performed:
Start analysis
Each analysis starts in position 1, immediately after the "Drift" position.
When using Stromboli, no positions can be controlled. The sample changer always moves forward by one
position and performs an analysis or a blank determination in that position. Stromboli only returns to the "Drift"
position to perform a drift determination.
66 Analysis Sequences
Cancel method
The method is terminated with no further action. The temperature control and the pump are switched off imme
diately. Stromboli returns to the "Drift" position.
Before actually canceling the process, the system displays a system message asking you to confirm the termi
nation.
Drift determination
The manual drift determination and the drift determination via method functions always take place in the "Drift"
position. After manual drift determination, the sample changer remains in this position. In contrast, with drift
determination using the method function, the sample changer moves to the next planned sample position.
Canceling the drift determination
Because the drift and concentration determination is performed in the drift beaker, terminating the process has
no effect on the actions of the sample changer. The standby titration is started again.
Pressing Reset
If the Reset button is pressed while a KF analysis or manual operations are active, all Karl Fischer methods and
manual operations are terminated. For Stromboli, this means that the pumps are switched off, the titrator
returns to the resting position (via the drift beaker), and the heating is turned off. If a KF analysis (method or
sample series) is terminated, the system continues with the pending analyses from the list. The sample data for
the terminated samples or sample series (such as weigh-ins, etc.) are still saved with the results.
Analysis Sequences 67
12 Analysis data
The "Analysis data" include different types of data that can be used at various times during the planning and
execution of an analysis.
The system differentiates between the following types of analysis data:
Displaying raw data Raw data is defined when you create a method or series. It is
automatically generated and stored during the analyses. Raw
data is always created for each analysis and cannot be influ
enced by the user.
Method data All data for the method run.
Series data All data from the series run, such as e.g. the series ID and the
number of samples.
Sample data All data from the analyzed samples, such as e.g. the sample
size, sample density and sample ID.
Resource data Data for all resources used during the execution of an analysis
(for example, titration stand, blank value). The data for a
resource are copied from the setup at the time when it is used in
an analysis.
Table of measured values Tables of measured values are created by some method func
tions during an analysis and can be output in the record.
Raw results Raw results are data determined by the titrator during an analy
sis, such as the drift value, or coulometric consumption to the
end point (ICEQ).
The raw results can be converted to the actual analysis results as
a part of the "Calculation" method function using suitable sym
bols and formulas.
Some raw results are always created automatically, while others
are only generated if used during a calculation.
Results Results are the results of the conversions of raw results run within
the "Calculate" method function. The results of an analysis can
be influenced by the user.
Of these, the following can be used in calculations:
● Sample data (such as the sample size or the sample density)
● Resource data (e.g. blank value variable)
● Raw results (e.g. auxiliary value, blank)
● Results (the results of a calculation can then be used in a subsequent calculation.)
68 Analysis data
13 Evaluate and calculate
13.1 Indexing of method functions
The "KF titration" method functions return their own raw results within a method.
These raw results are saved in the titrator in the order in which the generating method functions are processed
within the method. To ensure that any time these method functions are used more than once, the raw results
can still be given a unique assignment to their individual method functions, they are divided into different
groups:
If method functions from a group are used multiple times within a method, they are given indexes (beyond the
loop limits). This group index allows unique referencing of the raw results during calculations.
If the structure of a method is changed, the group indices are automatically updated, guaranteeing the serial
numbering at all times.
● Make sure your calculations take this into consideration!
● Calculations can be used independently of the method functions that generated the results. For the results,
we suggest using the IDs R1...Rn, following the sequence of the calculations in the method.
● Multiple loops are only permitted for the Stromboli method type.
● The group index "1" can be omitted because when a group index is missing, the system automatically
assigns the group index "1".
Method function Group index Result
Title
Sample (KF)
Titration stand (Stromboli)
Mix time
Titration (KF coul) 1
Calculation R1
Calculation R2
Calculation R3
End of sample
Sample (KF)
Titration stand (Stromboli)
Mix time
Titration (KF coul) 2
Calculation R4
End of sample
Calculation R5
[mg/pc]
[%]
[ppm]
Rx Arbitrary -- Rx Result x.
C -- -- C A constant that uniquely
belongs to the result Rx. It can
not be used in this form for the
calculations of other results.
Mean Arbitrary Rx Mean[Rx] Mean value of a result Rx
s Arbitrary Rx s[Rx] Standard deviation of a result
Rx
srel [%] Rx srel[Rx] The relative standard deviation
of the result Rx.
n -- -- n Sample number
13.3 Formulas
Calculation formulas can be used in the "Calculate" and "Condition" method functions. Some parameters within
method functions can also be defined in the form of formulas.
Formulas within the "Calculation" method function
A typical example of a formula within the "Calculation" method function would be the expression R=ICEQ in the
"Formula" parameter, where R represents the coulometric consumption in [mC] until the end point is reached.
All the symbols can be used for analysis data in relations like this. The analysis data to be used must be gener
ated by the method before the "Calculate" method function.
Conditions
A condition is a formula whose result comes in the form of "true" or "false". Conditions can be used in various
method functions in the "Condition" parameter (or subfunction). Depending on the condition's result, the
method function in question will be executed (condition true) or not executed (condition false).
● Auxiliary values and blanks defined in the setup can generally be used in formulas in the same manner as
symbols. The general form for an auxiliary value is: H[Name] (as defined in the setup).
● Likewise, results from other "Calculation" method functions can be referenced in the "Calculation" method
function (e.g. R3 = R2+R1). (What is important in this case is to make sure that the results used must
already be in existence at the time they are to be used!)
Index 73
Info button 13 Method syntax 41
Instruction 52 Method Templates 40
Internal calculations Method types 38
Blank determinations 59 Methods
More 59 Creating 39
Modify 40
K Preprogrammed 38
Karl Fischer stand METTLER TOLEDO balances 19
Setting up 24 METTLER TOLEDO Methods 38
Karl Fischer titration Mix time 49
Measurement principle 10 Monitoring
Keyboard layout Usable life and life span 28
Define 31
N
L Naming conventions for calcula 69
Language, setting 30 tions
Layout of terminal 13 Network settings 22
Level sensor 23
LevelSens 23 O
Activate 23 Online Dialog 15
Life span 28 Open series 64
Life span monitoring 29 Operation of the touchscreen 13
Loops 42 Outlier test 60
M P
Managing groups 26 PC settings 22
Manual operations Peripherals 19, 19
Pump 35 Balance 19
Sensor 36 Balances 20
Solvent manager 35 Barcode reader 20
Stirrer 35 Fingerprint reader 22
Mathematical functions and 72 Printer 20
operators USB data export 20
Measured Values 17 USB stick 20
Method Polarized sensors 18
Delete 41 Preloaded Methods 38
Start 41 Pretitration
Method editor 38 Automatic switch 16
Method functions Online dialog 16
Hidden method functions 54 Printer 20
Out of loop 44 Setup 20
Overview 44 USB data export 20, 20
Possible number 42 Protective clothing 9
Within loop 43 Pump
Method functions, hidden Manual operations 35
Pretitration 54
Standby 54 R
Method functions, Parameters Reagent manager 29
Auxiliary value 51 Setup 19
Blank value 51 Reagents
Calculation 52 Monitoring 29
Drift determination 46 Registration
End of sample 54 Fingerprint reader 22
Instruction 52 Reset button 13
Mix time 49 Reset to factory settings 32
Record 53 Results
Sample (KF) 46 Deleting 62
Title 45 Display 15-16
Titration (EP Coul) 50 Results proposals 60
Titration (KF Coul) 49 Routine 26
Titration stand 48 Running tasks 14
Method ID 38
74 Index
S Time and date 24
Safety Information Title
General 8 Parameter 45
Protective clothing 9 Titrant
Signal words 8 Replacement 67
Warning Symbols 8 Titrant replacement 67
Sample (KF) 46 Titration
Sample analysis 16 Network settings 22
Sample data PC settings 22
Change 16 Titration (EP Coul) 50
Sample Results 61 Titration (KF Coul) 49
Sample series Titration stand 48
Sample parameters 55 Setting up 24
Sample size 16 Titrator identification 24
Standby 17 U
Screen, setting 30
Sensor Undo Changes 61
Polarized 37 Updating 33
Sensors Upgrading 33
Configure 18 Usable life 28
Series analysis 66 Usable life and life span
Series data Monitoring 28
Save 16 USB compact printer 20
Series templates 55 USB data export 20, 20
Service & Maintenance USB data export box 20
Board data 32 USB-Stick 20
Board firmware 32 User Interface 13
Data Import/Export 31 Input Fields 14
Reset to factory settings 32 User management
Terminal 32 Managing groups 26
Titrator Firmware History 32 User rights
Update 33 Experts 26
Upgrade 33 Routine 26
Settings User settings
global 24 Keyboards 31
Shortcuts 14 Language 30
Manage 31 Screen 30
Signal words 8 Shortcuts 31
Solvent capacity 29 V
Solvent manager
Values
Manual operations 35
Auxiliary 33
Sorting lists 14
Blank 33
Standby 16
Automatic switch 16 W
Online dialog 16 Warning Symbols 8
Start analysis dialog 15
Starting an Analysis 63
Starting analysis 64
Statistics 60
Stirrer 35
Stop method 16
Stopping methods 41
Stromboli
Analysis sequence 66
Stromboli TTL
Setting up 24
Symbol list 69
System settings 24
T
Tape printer 20
Tasks menu 14
Index 75
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