Metrohm 860 KF User manual

860 KF Thermoprep
Manual
8.860.8003EN

Metrohm AG
CH-9101 Herisau
Switzerland
Phone [phone]
Fax [phone]
[email protected]
www.metrohm.com
860 KF Thermoprep
Manual
8.860.8003EN 07/2011 dm

Teachware
Metrohm AG
CH-9101 Herisau
[email protected]
This documentation is protected by copyright. All rights reserved.
Although all the information given in this documentation has been
checked with great care, errors cannot be entirely excluded. Should you
notice any mistakes please send us your comments using the address
given above.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents
860 KF Thermoprep ￭￭￭￭￭￭￭￭ III
Table of contents
1Introduction 1
1.1 Instrument description ......................................................... 1
1.1.1 Instrument components .......................................................... 1
1.1.2 Intended use ........................................................................... 2
1.2 About the documentation ................................................... 2
1.2.1 Symbols and conventions ........................................................ 2
1.3 Safety instructions ................................................................ 3
1.3.1 General notes on safety ........................................................... 3
1.3.2 Electrical safety ........................................................................ 3
1.3.3 Personnel safety ...................................................................... 4
1.3.4 Flammable samples and solvents ............................................. 5
1.3.5 Recycling and disposal ............................................................. 5
2Overview of the instrument 6
3Installation 8
3.1 Setting up the instrument .................................................... 8
3.1.1 Packaging ................................................................................ 8
3.1.2 Checks .................................................................................... 8
3.1.3 Location .................................................................................. 8
3.2 Connecting the mains cable ................................................. 8
3.3 Mounting the guidance rod ................................................. 9
3.4 Mounting the sample insert .............................................. 12
3.5 Mounting the needles ........................................................ 13
3.6 Mounting the heating tubing ............................................ 14
3.7 Mounting the dust filter .................................................... 16
3.8 Assembling the drying flask .............................................. 16
3.9 Air/nitrogen connector ....................................................... 18
3.10 Inserting the heating tube into the KF titration cell ....... 19
4Operation 22
4.1 Switching the instrument on and off ............................... 22
4.2 The keypad .......................................................................... 22
4.3 The display .......................................................................... 23
4.3.1 Display elements .................................................................... 23
4.3.2 Status display ........................................................................ 23
4.3.3 Error messages ...................................................................... 24

Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
IV ￭￭￭￭￭￭￭￭ 860 KF Thermoprep
4.4 Modifying numerical values and settings ......................... 25
4.4.1 Selecting from a selection list ................................................. 25
4.4.2 Modifying numerical values ................................................... 25
4.5 Parameters .......................................................................... 26
4.6 Configuration ...................................................................... 27
5Performing a determination 29
5.1 Conditioning the system .................................................... 29
5.1.1 Preparing the KF titration cell ................................................. 29
5.1.2 Preparing the 860 KF Thermoprep ......................................... 30
5.2 Determining the blank value ............................................. 33
5.3 Determining samples ......................................................... 34
6Handling and maintenance 36
6.1 General ................................................................................ 36
6.2 Care ...................................................................................... 36
6.3 Quality Management and validation with Metrohm ....... 36
7Troubleshooting 38
7.1 Problems and their solutions ............................................. 38
8Appendix 39
8.1 Practical instructions .......................................................... 39
8.2 Literature ............................................................................. 40
9Technical data 41
9.1 Oven ..................................................................................... 41
9.2 Gas flow .............................................................................. 41
9.3 Outlet heating ..................................................................... 41
9.4 Mains connection ............................................................... 42
9.5 Safety specifications ........................................................... 42
9.6 Electromagnetic compatibility (EMC) ................................ 42
9.7 Ambient temperature ......................................................... 43
9.8 Reference conditions .......................................................... 43
9.9 Dimensions .......................................................................... 43
10 Conformity and warranty 44
10.1 Declaration of Conformity ................................................. 44
10.2 Warranty (guarantee) ......................................................... 45

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents
860 KF Thermoprep ￭￭￭￭￭￭￭￭ V
10.3 Quality Management Principles ........................................ 46
11 Accessories 48
11.1 Scope of delivery 2.860.0010 ............................................ 48
11.2 Optional accessories ........................................................... 55
Index 56

Table of figures ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
VI ￭￭￭￭￭￭￭￭ 860 KF Thermoprep
Table of figures
Figure 1 Front 860 KF Thermoprep ................................................................. 6
Figure 2 Rear 860 KF Thermoprep ................................................................... 7
Figure 3 Connecting the mains cable .............................................................. 8
Figure 4 Loosen the adapter ........................................................................... 9
Figure 5 Mounting the guidance rod ............................................................. 10
Figure 6 Mounting tubing ............................................................................. 10
Figure 7 Fix the adapter ................................................................................ 11
Figure 8 Guidance rod mounted ................................................................... 11
Figure 9 Mounting the sample insert ............................................................. 12
Figure 10 Mounting the needles ..................................................................... 13
Figure 11 Mounting the heating tubing (view from rear) ................................. 14
Figure 12 Connecting the heating tubing ........................................................ 15
Figure 13 Mounting the dust filter .................................................................. 16
Figure 14 Preparing the drying flasks ............................................................... 16
Figure 15 Mounting the tubings ..................................................................... 17
Figure 16 External gas supply connection ........................................................ 18
Figure 17 Coulometric KF titration cell ............................................................ 19
Figure 18 Volumetric KF titration cell .............................................................. 20
Figure 19 Mains switch ................................................................................... 22
Figure 20 Keypad and operating unit .............................................................. 22
Figure 21 Main dialog ..................................................................................... 23
Figure 22 Insert the sample vessel into the oven ............................................. 31
Figure 23 Move the guide head down ............................................................ 31
Figure 24 Insert the needle ............................................................................. 32

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction
860 KF Thermoprep ￭￭￭￭￭￭￭￭ 1
1 Introduction
1.1 Instrument description
The 860 KF Thermoprep is used whenever the heating up of a sample
and/or the thermal expulsion of moisture in solid substances or liquids is
required. In combination with a coulometric or volumetric KF titrator, the
860 KF Thermoprep is the ideal analysis system for water determination in
samples that contain disruptive components or from which moisture can
be removed only with difficulty.
One of its decisive advantages is the reduction of sample preparation to a
minimum. Thanks to the use of hermetically sealed sample vessels ("head-
space vials"), the filling of the samples can be accomplished directly on-
site. The PTFE-coated septa guarantee a constant, non-falsified water con-
tent, even after prolonged holding times.
The sample heated in the oven module releases its moisture in the form of
water vapor, which is conveyed into a measuring cell with the aid of a gas
flow. An air pump is installed for the purpose of generating the gas flow.
An inlet valve is available for nitrogen or other inert gases. The determina-
tion of the moisture can be accomplished in the measuring cell either cou-
lometrically or volumetrically in accordance with Karl Fischer.
1.1.1 Instrument components
The 860 KF Thermoprep has the following components:
￭Oven
Oven module made of aluminum with software-operated temperature
control for heating the sample vessel.
￭Fan
Propeller fan for cooling the oven module.
￭Inlet valve
Valve for switching over the source of the gas flow.
￭Air pump
Pump for generating the gas flow.
￭Outlet heating
Heating tube for preventing the condensation of moisture.
￭Stand rods
Guidance device with needle adapter and tubing for the gas flow.
￭Operating unit
Monochrome LCD display and keyboard.

1.2 About the documentation ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
2￭￭￭￭￭￭￭￭ 860 KF Thermoprep
1.1.2 Intended use
The 860 KF Thermoprep is designed for usage as an auxiliary device for
sample preparation in analytical laboratories. Its main area of application is
moisture determination according to Karl Fischer (coulometric or volumet-
ric). The 860 KF Thermoprep enables the application of thermal gas
extraction technology.
The present instrument is suitable for processing chemicals and flammable
samples. The usage of the 860 KF Thermoprep therefore requires that the
user has basic knowledge and experience in the handling of poisonous
and caustic substances. Knowledge with respect to the application of the
fire prevention measures prescribed for laboratories is also mandatory.
1.2 About the documentation
Caution
Please read through this documentation carefully before putting the
instrument into operation. The documentation contains information
and warnings which have to be followed by the user in order to ensure
safe operation of the instrument.
1.2.1 Symbols and conventions
The following symbols and styles are used in this documentation:
Cross-reference to figure legend
The first number refers to the figure number, the
second to the instrument part in the figure.
Instruction step
Carry out these steps in the sequence shown.
Method Dialog text, parameter in the software
File ▶ New Menu or menu item
[Next] Button or key
Warning
This symbol draws attention to a possible life hazard
or risk of injury.
Warning
This symbol draws attention to a possible hazard due
to electrical current.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction
860 KF Thermoprep ￭￭￭￭￭￭￭￭ 3
Warning
This symbol draws attention to a possible hazard due
to heat or hot instrument parts.
Warning
This symbol draws attention to a possible biological
hazard.
Caution
This symbol draws attention to a possible damage of
instruments or instrument parts.
Note
This symbol marks additional information and tips.
1.3 Safety instructions
1.3.1 General notes on safety
Warning
This instrument may only be operated in accordance with the specifica-
tions in this documentation.
This instrument has left the factory in a flawless state in terms of technical
safety. To maintain this state and ensure non-hazardous operation of the
instrument, the following instructions must be observed carefully.
1.3.2 Electrical safety
The electrical safety when working with the instrument is ensured as part
of the international standard IEC 61010.
Warning
Only personnel qualified by Metrohm are authorized to carry out service
work on electronic components.

1.3 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
4￭￭￭￭￭￭￭￭ 860 KF Thermoprep
Warning
Never open the housing of the instrument. The instrument could be
damaged by this. There is also a risk of serious injury if live components
are touched.
There are no parts inside the housing which can be serviced or replaced
by the user.
Mains voltage
Warning
An incorrect mains voltage can damage the instrument.
Only operate this instrument with a mains voltage specified for it (see
rear panel of the instrument).
Protection against electrostatic charges
Warning
Electronic components are sensitive to electrostatic charges and can be
destroyed by discharges.
Always pull the mains cable out of the mains connection socket before
connecting or disconnecting electrical appliances on the rear panel of
the instrument.
1.3.3 Personnel safety
Warning
Wear protective goggles and working clothes suitable for laboratory
work while operating the 860 KF Thermoprep.
Warning
The oven and the sample vessels can be at a temperature of up to
250 °C! Avoid direct skin contact. Use the septum-sealing tongs sup-
plied or another suitable holding device for inserting the sample vessels
in the oven or removing them. Wear heat-insulated gloves if necessary.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction
860 KF Thermoprep ￭￭￭￭￭￭￭￭ 5
Warning
There is a considerable risk of injury connected with the needles.
Grasp the handle of the needle adapter with both hands when you
guide the needle into the sample vessel. Take care to ensure that no
other person reaches into the danger zone during this procedure.
1.3.4 Flammable samples and solvents
Warning
All relevant safety measures are to be observed when working with
flammable samples or when adding solvents.
￭Use nitrogen or another inert gas for conveying the moisture.
￭Set up the instrument in a well-ventilated location.
￭Keep all sources of flame far from the workplace.
￭Clean up spilled fluids and solids immediately.
￭Follow the safety instructions of the chemical manufacturer.
1.3.5 Recycling and disposal
This product is covered by European Directive 2002/96/EC, WEEE – Waste
from Electrical and Electronic Equipment.
The correct disposal of your old equipment will help to prevent negative
effects on the environment and public health.
More details about the disposal of your old equipment can be obtained
from your local authorities, from waste disposal companies or from your
local dealer.

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6￭￭￭￭￭￭￭￭ 860 KF Thermoprep
2 Overview of the instrument
1
2
3
4
5
6
7
8
9
10
11
12
13
Figure 1 Front 860 KF Thermoprep
1Guide head 2Needle holder (6.2049.040)
With needle adapter.
3Spring sleeve
With vessel stripper.
4Guidance rod
5Sample vessel (6.2419.007)
With 6 ml content.
6Sample insert (6.2063.010)
7Oven module
With sheet metal housing.
8Fixing lever
9Operating unit
With display and keyboard.
10 Drying flasks (6.1608.050)
With 6.1602.145 drying flask insert.
11 Drying flask holder 12 Gas inlet
With M6 thread.
13 Gas outlet
With M6 thread.

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860 KF Thermoprep ￭￭￭￭￭￭￭￭ 7
1
8
2
3
5 6
7
4
Figure 2 Rear 860 KF Thermoprep
1Air pump inlet
With 6.2724.010 dust filter.
2Mains switch
3Mains connection socket 4Type plate
Contains specifications concerning mains
voltage and serial number.
5Outlet heating connection
For the heating tube.
6Air/nitrogen connector
With M6 interior thread. Inlet for external
gassing.
7Fan
For cooling the oven module.
8Cable holder (6.2060.010)

3.1 Setting up the instrument ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
8￭￭￭￭￭￭￭￭ 860 KF Thermoprep
3 Installation
3.1 Setting up the instrument
3.1.1 Packaging
The instrument is supplied in highly protective special packaging together
with the separately packed accessories. Keep this packaging, as only this
ensures safe transportation of the instrument.
3.1.2 Checks
Immediately after receipt, check whether the shipment has arrived com-
plete and without damage by comparing it with the delivery note.
3.1.3 Location
The instrument has been developed for operation indoors and may not be
used in explosive environments.
Place the instrument in a location of the laboratory which is suitable for
operation, free of vibrations, protected from corrosive atmosphere, and
contamination by chemicals.
The instrument should be protected against excessive temperature fluctu-
ations and direct sunlight.
3.2 Connecting the mains cable
Warning
This instrument must not be operated except with the mains voltage
specified for it (see rear of the instrument).
Protect the connection sockets against moisture.
Figure 3 Connecting the mains cable

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860 KF Thermoprep ￭￭￭￭￭￭￭￭ 9
3.3 Mounting the guidance rod
The guidance rod with the guide head is enclosed separately with the 860
KF Thermoprep and must first be mounted.
Proceed as follows:
1Move the guide head of the guidance rod a bit downwards by press-
ing the fixing lever.
12
3
Figure 4 Loosen the adapter
2Loosen the adapter on the head of the guidance rod with a hexagon
key.
3Remove the adapter.
4Insert the tubing jutting out of the housing from below into the guid-
ance rod.
Note
This tubing conveys the gas from the flow controller upward
through the guidance rod to the guide head. From there the gas is
guided to the double hollow needle, see next chapter.

3.3 Mounting the guidance rod ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
10 ￭￭￭￭￭￭￭￭ 860 KF Thermoprep
4
5
Figure 5 Mounting the guidance rod
5Insert the guidance rod into the opening intended for this purpose
from above and push it downwards until it hits the stop. Observe the
orientation of the guidance rod.
6Pull out the tubing inside the guidance rod as far as possible. Eventu-
ally use a piece of sand paper in order to be able to better grasp the
tubing.
7
6
Figure 6 Mounting tubing
7Fasten the tubing on the olive of the 4.860.4260 adapter.
8Pull out the guidance rod as far as possible in order that the adapter
rests close on the guidance rod.

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860 KF Thermoprep ￭￭￭￭￭￭￭￭ 11
10
8
9
Figure 7 Fix the adapter
9Fix the adapter in the guidance rod. Fasten the screw in the guidance
rod with the aid of a hexagon key.
10 Carefully push the guidance rod downwards.
11
Figure 8 Guidance rod mounted
11 Fix the guidance rod with the V.0434.008 hexagon screw according
to the drawing. The screw and the associated hexagon key are pack-
aged separately with the instrument.

3.4 Mounting the sample insert ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
12 ￭￭￭￭￭￭￭￭ 860 KF Thermoprep
3.4 Mounting the sample insert
6.2063.010
6.2627.000
Figure 9 Mounting the sample insert
Note
The sample insert may not be inserted or removed unless it has been
cooled down.
The dimensions of the supplied sample insert are optimized for the usage
of 6 mL sample vials 6.2419.007 from Metrohm. This ensures the best
possible transfer of heat between oven and sample.
1Place the 6.2627.000 oven insert into the oven from above.
2Place the 6.2063.010 sample insert into the oven from above.
If vessels with other dimensions are to be used, then individually modified
sample inserts can be ordered. The precise vessel dimensions (including
tolerances) will be required when ordering. Non-standard sample vessels
may not exhibit dimensions outside of the following limit values:
￭Diameter 10.0…32.0 mm
￭Immersion depth 20.0…45.0 mm