Contents
Karl Fischer titration
Introduction to Karl Fischer titration
Volumetric KF titrators
Volumetric KF titrators – overview
890/901 Titrando
870 KF Titrino Plus
KF.3
KF.4
KF.5
KF Coulometer
Coulometric KF titrators – overview
851/852 Titrando
756/831 KF Coulometer
KF.6
KF.7
KF.8
KF sample preparation
874 USB Oven Sample Processor
860 KF Thermoprep
KF Evaporator
Polytron PT 1300 D
KF.9
KF.10
KF.10
KF.11
KF automation
Automated coulometric KF titrations
Automated volumetric KF titrations
Automated volumetric KF titration including sample preparation
KF.12
KF.12
KF.13
5 — KF
Karl Fischer titration
Introduction to Karl Fischer Titration
Karl Fischer water determination is one of the most frequently used laboratory methods world-wide. In contrast to other water determination methods it is specific, fast and the amount of instrumentation required
is very small.
With an application range of 0.1% to 100% water,
volumetric Karl Fischer titration is used in a wide
variety of industries. The advantage of volumetry is that
not only liquid samples but also solid or pasty samples
can be put directly into the titration vessel. No matter
whether you want to determine water in food, cosmetics or pharmaceutical products, with Metrohm KF
titrators you are always right.
As far as quantities in the trace range (10 g to 10 mg
water absolute) are concerned, coulometry is the
optimal method to determine water in liquids, solids
and gases. Coulometry is also an absolute method and
therefore requires no titer determination.
6 — KF
For difficult samples, we offer intelligent solutions for
sample preparation, e.g. the KF oven technique or
sample pulverisation with a homogeniser included in
the system.
Due to high sample throughput the use of automated
systems pays for itself very quickly. Metrohm KF automation offers you sophisticated techniques for both
volumetric and coulometric KF titration.
Karl Fischer titration
Volumetric KF titrators – overview
Technical specications
Volumetric Karl Fischer titration (KFT)
Titration to preset pH/mV endpoints (SET)
870 KF
Titrino plus
890
Titrando
901
Titrando
yes
yes
yes
yes
yes
Real-time curve display
yes
yes
yes
Predened methods
yes
yes
yes
yes (tiamoTM)
Exchange Unit
Exchange Unit
Dosing Unit
pH calibration and pH measurements (CAL, MEAS)
Parallel titration
Dosing drive for titration
Inputs, interfaces
Second, galvanically separated measuring interface
option
Automated reagent exchange with Dosino (option)
yes
yes
MSB-port for connection of further Dosinos (addition of auxiliary solution, …)
3
4
MSB-port for connection of further Dosinos (Titration)
3
yes
yes
yes
yes
yes
Attachment of stirrer
Sample changer connection
Attachment of printer, balance, ...
yes, USB
yes, USB
yes, USB
optional RS 232C
yes, USB
yes, USB
tiamoTM
yes (1.3 or higher)
yes (2.0 or higher)
Touch Control
yes
yes
Optional interfaces
Software
7 — KF
Karl Fischer titration
Karl Fischer Titrando
890/901 Titrando
Karl Fischer titrators for the modern titration lab
Due to their simple and intuitive user guidance,
the KF Titrandos are the optimal instruments both for
routine work and for demanding applications in
development laboratories. With the KF Titrando you
have a titration system that can be adapted to meet all
imaginable requirements without any compromises at
all.
An electrode test and the specially created parameter
«Safety stop» prevent the cell from overflowing during
conditioning, i.e. conditioning is stopped after a certain
time or the addition of a certain amount of KF reagent
(Laboratory safety). The sophisticated control algorithm of the Titrando is adapted to the characteristics
of the Karl Fischer reaction and guarantees results of
outstanding precision.
Choose your favorite! Both the 901 Titrando and
the 890 Titrando can be used either as a stand-alone
system with the 900 Touch Control or via a PC using
the tiamo™ software.
901 Titrando
In addition to the Karl Fischer mode (KFT), the 901
Titrando also features the SET mode, allowing titrations
to a predefined endpoint. With the high-resolution,
galvanically separated measuring interface with additional digital measuring input for intelligent electrodes «iTrodes» it is also capable of performing highprecision pH measurements.
Ordering information
2.890.0110 890 Titrando with Touch Control
2.890.0210 890 Titrando with tiamoTM light
2.901.0010 901 Titrando
Options
2.803.0010
2.900.0010
6.6056.221
6.6056.222
6.6056.223
6.3026.150
6.3026.210
6.3026.220
2.800.0010
6.3032.120
6.3032.150
6.3032.210
6.3032.220
6.2061.010
803 TI Stand with stirrer and pump
900 Touch Control
tiamo™ 2.2 light
tiamo™ 2.2 full
tiamo™ 2.2 multi
Exchange Unit 5 mL
Exchange Unit 10 mL
Exchange Unit 20 mL
800 Dosino
Dosing Unit 2 mL
Dosing Unit 5 mL
Dosing Unit 10 mL
Dosing Unit 20 mL
Bottle holder for Dosinos
Thanks to the four MSB connections, up to four 800
Dosino dosing systems can be connected to the 901
Titrando. These can be used for titration, but also for
the automated addition of sample, standard and auxiliary solutions such as solubility promoters. All liquid
handling commands are also available.
Because of its special properties the 800 Dosino is the
optimal dosing system for KF titration. Thanks to the
«Empty» command the Dosino can be completely emptied; as a result opening and cleaning the dosing unit is
no longer necessary. In contrast to the exchange unit,
repeated rinsing before titre adjustment is no longer
necessary; you save both time and reagents.
890 Titrando
The 890 Titrando offers the same high-end features as
the 901 Titrando (except digital measuring input), but
is limited to the KF mode and titrates only with the
well-proven exchange unit. In addition up to three 800
Dosino dosing systems can be connected and used for
the automated addition of sample, standard and auxiliary solutions.
901 Titrando with 803 Ti Stand and Touch Control
8 — KF
Karl Fischer titration
Karl Fischer Titrino plus
870 KF Titrino Plus
• Straightforward installation
• Easy operation due to predefined methods
• Excellent precision thanks to the high-resolution
measuring input
• Live curve for recognizing side-reactions
• Overflow protection for increased operating safety
• Compact USB printer as an option
The competitively priced 870 Titrino plus is a titrator
for volumetric water determination. It can be used
to determine water contents from a few ppm up to
100% reliably and accurately in solid, liquid and gaseous samples. With its operating interface designed
for routine users, the 870 Titrino plus is so easy to use
that hardly any familiarization is needed at all. Due to
its robustness, it is also the ideal titrator for routine
determinations. Titration vessel and electrode are
included.
Very simple installation
Installation of the 870 Titrino plus is simple. As soon
as they are connected, the exchange unit, stirrer and
compact USB printer are recognised and configured
automatically.
Ready-to-use methods simplify your work
You only have to decide whether you want to carry
out a titre, blank value or water determination and
then start the titration by pressing just one key. Parameters need only be adjusted in exceptional cases.
Ordering information
2.870.0010 870 KF Titrino
2.870.1010 870 KF Titrino
2.870.1020 870 KF Titrino
2.870.2010 870 KF Titrino
moprep
plus
plus complete
plus with printer
plus and 860 KF Ther-
Mouse or keyboard – choose your favorite!
The 870 Titrino plus is the first titrator that can be controlled either by mouse-click or keyboard – the choice
is yours.
Highest precision thanks to new measuring
input
Just like the Titrando high-end titrator, the new KF
titrator is also equipped with a high-resolution measuring input that guarantees results of outstanding precision.
Live curve allows recognition of side-reactions
Metrohm KF titrators feature a display with live curve
as standard. This allows the user to recognise sidereactions in good time and take measures to suppress
them.
New parameters improve working safety
Great importance has been given to working safety:
The new titrator allows safe handling of hazardous Karl
Fischer reagents. The new safety parameter «Conditioning options» prevents the titration cell from overflowing.
Optional:
Intelligent Exchange Unit for more convenience
The chip of the intelligent Metrohm Exchange Unit
automatically provides the titrator with the data (cylinder volume, type of KF reagent, expiration date of titre,
etc.) that are necessary to carry out an error-free titration. This means that you always titrate under optimal
conditions.
The 803 KF Titration Stand
The 803 KF Titration Stand is used for stirring and for
exchanging the used working medium. The built-in
pump aspirates off the used titration solution and adds
new working medium there being no need to open
the cell.
9 — KF
Karl Fischer titration
Coulometric KF titrators – overview
Technical specications
852 Titrando
756 KF Coulometer
831 KF Coulometer
851 Titrando
Coulometric Karl Fischer titration (KFC)
yes
yes
yes
yes
Volumetric Karl Fischer titration (KFT)
yes
Bromine index (BRC)
yes
yes
Titration to preset mV endpoints (MET Ipol, SET Upol)
yes
Monotonic equivalence point titration (MET Ipol, MET Upol)
yes
Water/time real-time curve display
yes
yes
yes
yes
Predened methods
yes
yes
yes (with tiamoTM)
yes
yes
yes
yes
yes
yes
3
Parallel titration
Automatic reagent exchange with Dosino (option)
Automatic titration start for coulometry
Inputs, interfaces
MSB-port for connection of further Dosinos (titration)
MSB-port for connection of further Dosinos (dosing)
Attachment of stirrer
Sample changer connection
yes
yes
yes
yes
yes
yes
yes
yes
yes
yes
Attachment of printer and balance
RS 232C
RS 232C
USB (2)
USB (2)
Optional interfaces
RS 232C
RS 232C
RS 232C
RS 232C
yes
yes
yes (2.1 or higher)
yes (2.1 or higher)
yes
yes
Software
tiamoTM
Touch Control
10 — KF
Karl Fischer titration
KF Coulometers
851/852 Titrando
Coulometry is the ideal method for water determination in the trace range (10 g to 10 mg water absolute) for analysing liquids, solids and gases. Furthermore, coulometry is an absolut method, which is why
no titer determination is necessary.
With the 851 Titrando, coulometric titrations can
be performed rapidly and easily. The 852 Titrando
enables not only coulemetric but also volumetric Karl
Fischer titrations.
Bromine index
The bromine index can be determined with the 851
Titrando and the 852 Titrando. No additional accessory parts are required for the measurements. The
conventional coulometric titration cell and the generator electrode with diaphragm can also be used for the
bromine index determination. Only the anolyte and the
catholyte need to be adjusted.
Automatic titration start
It can easily happen that the sample is injected into the
titration vessel before starting the titration beforehand.
In such cases, the water in the sample is conditioned
away and the measurement must be repeated. You
don’t have to worry about this potential problem with
the 851 Titrando or the 852 Titrando. The instrument starts the titration automatically, as soon as the
sample is added. Thus, you will save on reagents,
sample and, above all, on valuable time.
Ordering information
2.851.0010 851 Titrando with generator electrode
with diaphragm
2.851.0020 851 Titrando with diaphragm-generator electrode and Touch Control operating unit
2.851.0110 851 Titrando with diaphragmless generator electrode
2.851.0120 851 Titrando with diaphragmless generator electrode and Touch Control
operating unit
2.852.0050 852 Titrando with generator electrode
with diaphragm
2.852.0060 852 Titrando with generator electrode
with diaphragm and Touch Control
2.852.0150 852 Titrando with generator electrode
without diaphragm
2.852.0160 852 Titrando with diaphragm-less generator cell and Touch Control operating
unit
Options
2.801.0010
2.803.0010
2.800.0010
2.900.0010
6.3032.120
6.3032.150
6.3032.210
6.3032.220
6.3032.250
6.6056.221
6.6056.222
6.6056.223
801 Magnetic Stirrer
803 TI Stand with stirrer and pump
800 Dosino
900 Touch Control
Dosing Unit 2 mL
Dosing Unit 5 mL
Dosing Unit 10 mL
Dosing Unit 20 mL
Dosing Unit 50 mL
tiamo™ 2.2 light
tiamo™ 2.2 full
tiamo™ 2.2 multi
Dosing Unit and Dosino
Dosinos and Dosing Units can be connected to the
new coulometer at one of the four MSB ports. In
combination with the two Titrandos, these can be
used for the adding of sample, standard or auxiliary
solutions such as solubility promoters. In addition, the
replacement of reagents can be automated, which
means that the cell does not need to be opened, thus
eliminating the possibility of moisture entering it. As a
result, long conditioning times following a change of
reagent are avoided.
Coulometric and volumetric titrations
If the water content of the samples should be too high
for coulemetric determination, this is not a problem
when the 852 Titrando is used. The instrument enables
analysis of samples with water content levels ranging
from a few micrograms all the way up to 100%.
852 Titrando with coulometric and volumetric titration cell
11 — KF
Karl Fischer titration
KF Coulometers
756/831 KF Coulometer
The Metrohm KF Coulometers are suitable for precise
water determinations in the trace range (1 ppm...10%).
They are available with two different types of generator electrodes. The diaphragm-less generator electrode
requires only one reagent and is practically maintenance-free. The use of the generator electrode with
diaphragm is preferred for the following applications:
very low water content (< 100 g water absolute),
when ketone reagents are used or with a high content
of solubility promoter (> 10%).
Ordering information
2.756.0010 756 KF Coulometer including generator
electrode with diaphragm
2.756.0110 756 KF Coulometer including diaphragmless generator electrode
2.831.0010 831 KF Coulometer including generator
electrode with diaphragm
2.831.0110 831 KF Coulometer with diaphragmless
generator electrode
With or without printer – choose as you prefer! The
756 KF Coulometer is equipped with a built-in thermal printer. However, just like the 831 KF Coulometer,
you can also connect an external printer or connect
the instrument to a PC, in which case you can choose
between the Metrodata Vesuv and tiamo™ software.
Options
2.728.0010
2.703.0010
6.5617.000
2.700.0020
2.140.0200
Our KF Coulometers come with a complete titration
cell and many accessories. KF Coulometers with the
diaphragm generator electrode are delivered with the
728 Magnetic Stirrer as part of the accessories.
User benefits:
728 Stirrer without stand
703 Ti Stand with stirrer and pump
Reagent changing equipment
700 Dosino
Impact printer CUSTOM DP40-S4N
• Possibility of connecting a PC keyboard and barcode
reader
• Optional: automatic reagent exchange using Dosing
Unit and Dosino
• Live curve for early recognition of possible side
reactions
• Simple operation due to dialogue in German, English,
French, Spanish, Italian, Portuguese and Swedish
• Expert or routine mode selectable
• Memory for up to 100 methods
• With 2 x RS 232C (DB9) data interfaces for connection of balance, printer and PC
756 KF Coulometer with 728 Stirrer and additional equipment for
automatic reagent exchange
12 — KF
Karl Fischer titration
Thermal sample preparation
874 USB Oven Sample Processor
The 874 Oven Sample Processor opens up new possibilities for water determinations in samples that are
either insoluble, cause side reactions or for any other
reasons cannot be placed directly into the titration vessel. Using the oven method, these problems can be
avoided, as the water is separated from the sample
matrix.
How the oven technique works: The samples are
placed in the oven in hermetically sealed sample vials.
Heating the sample releases the water, which is transferred in a stream of carrier gas to the KF cell, where
the Karl Fischer titration takes place.
Sample preparation: Sample preparation for the oven
technique is very simple. All that has to be done is
weighing out the sample into the vial and then sealing it. Hermetically sealing the vial with a septum also
reliably prevents moisture absorption from the atmosphere.
Field of application: The oven method is suitable for
liquid and solid samples and can be used with both
volumetric and coulometric KF titrators.
Advantages of the oven method at a glance:
• Reproducible analysis conditions for each sample –
benefit: much higher precision of results
• Reduction of manual preparation steps to a minimum
• Considerable savings in time
• No contamination of the oven by the sample, so no
carryover or memory effects
Ordering information
2.874.0010 874 USB Oven Sample Processor
2.874.0020 874 USB Oven Sample Processor
customized
• Improved water release from the sample, because
the carrier gas does not just pass over the sample
but is led directly through it
• Lower reagent consumption, as the titration solution
needs to be changed only at infrequent intervals
874 USB Oven Sample Processor
• USB device – If the 874 USB Oven Sample Processor
is connected to a PC the instrument is recognised
automatically
• Optimal oven temperature – Running a temperature
gradient enables the optimal oven temperature to be
defined for each individual sample
• Reagent exchange – an 800 Dosino can be attached
directly to one of the MSB ports of the Sample
Changer. With a Dosino and a Dosing Unit the
reagent exchange can be carried out automatically
With tiamo™ full software and extensive accessories, consisting of: 100 sample vials 100 septum seals, 1 crimping tongs.
874 USB Oven Sample Processor, 851 Titrando
13 — KF
Karl Fischer titration
860 KF Thermoprep
• Simple handling of the instrument thanks to a clearly
arranged menu
• Identical and reproducible conditions for all samples
during analysis ensures precise results
• No contamination of the oven and therefore no carryover and memory effects
• Simple and fast sample preparation
Ordering information
2.860.0010 860 KF Thermoprep
The 860 KF Thermoprep is designed for thermal sample
preparation in Karl Fischer titration.
Numerous substances cannot be analysed by direct
Karl Fischer titration as they are not soluble, react with
the Karl Fischer reagent or release their water only very
slowly or not until heated to high temperatures. Using
tightly sealed sample vials, the sample is inserted in the
oven. The samples can be subsequently analysed by
any volumetric or coulometric KF titrator.
860 KF Thermoprep with 756 KF Coulometer
KF Evaporator
The KF Evaporator is used for sample preparation in
Karl Fischer titration by means of azeotropic distillation.
Ordering information
2.136.0200 KF Evaporator
As with the oven method, the water is separated from
the sample matrix. Because the sample itself remains in
the evaporation chamber, the titration vessel and the
electrodes are not contaminated. Furthermore, unwanted side reactions and matrix effects are avoided.
KF Evaporator
14 — KF
Karl Fischer titration
KF homogenizer
Polytron PT 1300 D
With the PT 1300 D you can pulverise and homogenise
samples directly in the titration cell. Because sample
preparation is carried out directly in the sealed titration vessel, any change of the water content caused
by atmospheric humidity is eliminated. Depending on
the dispersing tool and type of sample, rotor speeds
between 7000 and 30’000 rpm can be set steplessly
and exactly. As the Polytron 1300 D is controlled
directly either by the Metrohm tiamo™ software or
the Touch Control the speed can be varied during the
measurement; as a result stirring with an additional
magnetic stirrer is not necessary.
Examples of applications for the Polytron 1300
D in sparingly soluble substances:
Candies
Water content is a critical factor during the manufacture of candy, even though it is not one of its major
components. It determines both the properties of the
candy and its taste.
Ordering information
2.136.0100 Polytron PT 1300 D
Options
6.9012.000
6.9012.010
Dispersing aggregate for Polytron,
125 mm
Dispersing aggregate for Polytron,
157 mm
Pharmaceuticals
The water content of drugs influences their active substance release. In pharmaceutical analyses it is therefore an important parameter. With the Titrando/Polytron system, tablets are dissolved in the KF reagent in
a short time regardless of their coating in a way which
immediately releases their water content.
Meat
Meat usually has a high water content which is normally enclosed in cells. This water can only be released
by comminution with a high-frequency homogeniser.
Dried plant material
In plant material, such as tobacco, the majority of the
water is enclosed in cells. The easiest way to release it
is by using a high-frequency homogeniser.
15 — KF
Karl Fischer titration
Automated coulometric KF titrations
MATi 4 is a fully automated system for coulometric
KF titrations with high sample throughput. The sample
rack of the Sample Processor accommodates up to
160 samples in 6-mL-vials. The samples are transferred
to an external coulometric cell where KF titration is
carried out. The system is controlled by the tiamo™
titration software.
Ordering information
MATi 04
Automated coulometric KF titrations
The system consists of:
1 x 815 Robotic USB Sample Processor XL
1 x 786 Swing Head
1 x 851 Titrando
1 x 800 Dosino
1 x 801 Stirrer
Automated volumetric KF titrations
Fully automated system for volumetric Karl Fischer
water determination in up to 24 samples. The system
is controlled by tiamo™ and consists of an 814 USB
Sample Processor, an 901 Titrando and numerous
accessories.
The samples are weighed out into beakers, sealed to
protect them against atmospheric moisture and placed
on the rack. Prior to titration the samples are dissolved
in a known amount of KF working medium and the
water content is then titrated in a second step.
This method is particularly suitable for samples that
dissolve quickly in the KF working medium. The solubility can also be improved by using a suitable solubility
promoter.
The system consists of:
1 x 814 USB Sample Processor
1 x 901 Titrando
2 x 800 Dosino
1 x 741 Stirrer
16 — KF
Ordering information
MATi 10
Automated volumetric KF titrations
Karl Fischer titration
Automated volumetric KF titration including
sample preparation
Fully automated system for volumetric Karl Fischer
water determination in up to 53 samples. The system
is controlled by tiamo™ and consists of an 815 USB
Sample Processor XL, an 901 Titrando and numerous
accessories.
Ordering information
MATi 11
Automated volumetric KF titration
including sample preparation
The samples are weighed out into beakers, sealed to
protect them against atmospheric moisture and placed
on the rack. Prior to titration a known amount of KF
reagent is added and the sample crushed using a Polytron. In a second step the water content is titrated.
With the Polytron the samples are crushed into small
pieces and the contained water is released. This
method is also suitable for the analysis of hardly soluble samples (e.g. tablets). In many cases solubility promoters can thus be avoided.
The system consists of:
1 x 815 USB Sample Processor XL
1 x 901 Titrando
1 x Polytron
1 x 772 Pump Unit
2 x 800 Dosino
2 x 786 Swing Head
1 x 6.9903.048 Electrode
1 x 6.9914.139 Titration head
1 x 6.9914.140 Robotic arm
1 x 6.9920.141 Sample rack
17 — KF