Metrohm 860 KF User manual

860 KF Thermoprep
Manual
8.860.8003EN / 2019-12-02

Metrohm AG
CH-9100 Herisau
Switzerland
Phone [phone]
Fax [phone]
[email protected]
www.metrohm.com
860 KF Thermoprep
Manual
8.860.8003EN / 2019-12-02

Technical Communication
Metrohm AG
CH-9100 Herisau
[email protected]
This documentation is protected by copyright. All rights reserved.
This documentation has been prepared with great care. However, errors
can never be entirely ruled out. Please send comments regarding possible
errors to the address above.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents
860 KF Thermoprep ￭￭￭￭￭￭￭￭ III
Table of contents
1 Introduction 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
2 Overview of the instrument 6
3 Installation 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 instrument to the power grid ................... 8
3.3 Mounting the support rod ................................................... 9
3.4 Mounting the sample holder ............................................. 12
3.5 Mounting the needles ........................................................ 13
3.6 Mounting the heating tubing ............................................ 15
3.7 Mounting the dust filter .................................................... 16
3.8 Assembling drying flasks ................................................... 17
3.9 Assembling the air/nitrogen connector ............................ 19
3.10 Inserting the heating tube into the KF titration cell ....... 19
4 Operation 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 ......................... 24
4.4.1 Selecting from a selection list ................................................. 25
4.4.2 Modifying numerical values ................................................... 25
4.5 Parameters .......................................................................... 25
4.6 Configuration ...................................................................... 27
5 Performing a determination 28
5.1 Conditioning the system .................................................... 28
5.1.1 Preparing the KF titration cell ................................................. 28
5.1.2 Preparing the 860 KF Thermoprep ......................................... 29
5.2 Determining the blank value ............................................. 32
5.3 Determining samples ......................................................... 33
6 Operation and maintenance 35
6.1 General ................................................................................ 35
6.2 Care ...................................................................................... 35
7 Troubleshooting 36
7.1 Problems and their solutions ............................................. 36
8 Appendix 37
8.1 Practical notes .................................................................... 37
8.2 Literature ............................................................................. 38
9 Technical specifications 39
9.1 Oven ..................................................................................... 39
9.2 Gas flow .............................................................................. 39
9.3 Outlet heater ....................................................................... 39
9.4 Power connection ............................................................... 40
9.5 Ambient temperature ......................................................... 40
9.6 Reference conditions .......................................................... 40
9.7 Dimensions .......................................................................... 40
10 Accessories 41
Index 42

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of figures
860 KF Thermoprep ￭￭￭￭￭￭￭￭ V
Table of figures
Figure 1 Front 860 KF Thermoprep ................................................................. 6
Figure 2 Rear 860 KF Thermoprep ................................................................... 7
Figure 3 Loosening the adapter ....................................................................... 9
Figure 4 Mounting the support rod ............................................................... 10
Figure 5 Mounting the tubing ....................................................................... 11
Figure 6 Attaching the adapter ..................................................................... 11
Figure 7 Mounted support rod ...................................................................... 12
Figure 8 Mounting the sample holder ........................................................... 12
Figure 9 Mounting the needles ..................................................................... 14
Figure 10 Mounting the heating tubing (rear view) ......................................... 15
Figure 11 Connecting the heating tubing ........................................................ 16
Figure 12 Mounting the dust filter .................................................................. 16
Figure 13 Preparing the drying flasks ............................................................... 17
Figure 14 Mounting the tubings ..................................................................... 18
Figure 15 External gas connector .................................................................... 19
Figure 16 Coulometric KF titration cell ............................................................ 20
Figure 17 Volumetric KF titration cell ............................................................... 21
Figure 18 Power switch .................................................................................. 22
Figure 19 Keypad of the operating unit ........................................................... 22
Figure 20 Main dialog ..................................................................................... 23
Figure 21 Insert the sample vessel into the oven ............................................. 30
Figure 22 Move the guide head down ............................................................ 30
Figure 23 Insert the needle ............................................................................. 31

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction
860 KF Thermoprep ￭￭￭￭￭￭￭￭ 1
1 Introduction
1.1 Instrument description
The 860 KF Thermoprep is used wherever the heating of a sample and/or
the thermal expulsion of moisture in solids or liquids is required. In combi-
nation with a coulometric or volumetric KF titrator, the 860 KF Thermo-
prep is the ideal analysis system for water content determination in sam-
ples that contain disruptive components or from which moisture can be
removed only with difficulty.
One of its decisive advantages is reducing sample preparation to a mini-
mum. Thanks to the use of hermetically sealed sample vessels ("headspace
vials"), samples can be filled directly on-site. The PTFE-coated septa guar-
antee a constant, unaltered water content, 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 to generate the gas flow. An inlet valve is
available for nitrogen or other inert gases. The moisture can be deter-
mined in the measuring cell either coulometrically or volumetrically using
Karl Fischer titration.
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 heater
Heating tubing for preventing the condensation of moisture.
￭Support 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
water content determination using Karl Fischer titration (coulometric or
volumetric). The 860 KF Thermoprep enables the application of thermal
gas extraction technology.
This instrument is suitable for processing chemicals and flammable sam-
ples. Therefore, the use of the 860 KF Thermoprep requires the user to
have basic knowledge and experience in handling toxic and caustic sub-
stances. Knowledge regarding the application of 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 the user must follow in order to ensure safe opera-
tion of the instrument.
1.2.1 Symbols and conventions
The following symbols and formatting may appear in this documentation:
Cross-reference to figure legend
The first number refers to the figure number, the sec-
ond 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-threat-
ening 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 possible damage to
instruments or instrument parts.
NOTE
This symbol highlights additional information and
tips.
1.3 Safety instructions
1.3.1 General notes on safety
WARNING
Operate this instrument only according to the information contained in
this documentation.
This instrument 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.
Supply voltage
WARNING
An incorrect supply voltage can damage the instrument.
Only operate this instrument with a supply 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.
Do not fail to pull the power cord out of the power socket before you
set up or disconnect electrical plug connections at the rear of the
instrument.
1.3.3 Personnel safety
WARNING
Wear protective glasses and working clothes suitable for laboratory
work while operating the 860 KF Thermoprep.
WARNING
The oven and the sample vessels can reach temperatures of up to
250 °C! Avoid direct skin contact. Use the provided septum crimping
tongs or another suitable holding device to insert the sample vessels
into or remove them from the oven. Wear heat-insulating gloves, if nec-
essary.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction
860 KF Thermoprep ￭￭￭￭￭￭￭￭ 5
WARNING
The needles pose a considerable risk of injury. When inserting the
needle into the sample vessel, hold the handle of the needle adapter
with both hands. 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 (e.g., fume cup-
board).
￭Keep all sources of flame far from the workplace.
￭Clean up spilled liquids and solids immediately.
￭Follow the safety instructions of the chemical manufacturer.
1.3.5 Recycling and disposal
This product is covered by European Directive 2012/19/EU, WEEE – Waste
Electrical and Electronic Equipment.
The correct disposal of your old instrument will help to prevent negative
effects on the environment and public health.
More details about the disposal of your old instrument can be obtained
from your local authorities, from waste disposal companies or from your
local dealer.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
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 holder (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.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Overview of the instrument
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 protective packaging together with the sepa-
rately 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 and free of vibrations and which provides protection against
corrosive atmosphere and contamination by chemicals.
The instrument should be protected against excessive temperature fluctua-
tions and direct sunlight.
3.2 Connecting the instrument to the power grid
WARNING
Electric shock from electrical potential
Risk of injury by touching live components or through moisture on live
parts.
￭Never open the housing of the instrument while the power cord is
still connected.
￭Protect live parts (e.g. power supply unit, power cord, connection
sockets) against moisture.
￭Unplug the power plug immediately if you suspect that moisture has
gotten inside the instrument.
￭Only personnel who have been issued Metrohm qualifications may
perform service and repair work on electrical and electronic parts.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation
860 KF Thermoprep ￭￭￭￭￭￭￭￭ 9
Connecting the power cord
Accessories Power cord with the following specifications:
￭Length: max. 2 m
￭Number of cores: 3, with protective conductor
￭Instrument plug: IEC 60320 type C13
￭Conductor cross-section 3x min. 0.75 mm2 / 18 AWG
￭Power plug:
– according to customer requirement (6.2122.XX0)
– min. 10 A
NOTICE
Do not use a not permitted power cord!
1Plugging in the power cord
￭Plug the power cord into the instrument's power socket.
￭Connect the power cord to the power grid.
3.3 Mounting the support rod
The support 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 support rod a bit downwards by press-
ing the locking lever.
12
3
Figure 3 Loosening the adapter
2Loosen the adapter on the head of the support rod with a hex key.

3.3 Mounting the support rod ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
10 ￭￭￭￭￭￭￭￭ 860 KF Thermoprep
3Removing the adapter.
4Insert the tubing jutting out of the housing from below into the sup-
port rod.
NOTICE
This tubing conveys the gas from the flow controller upward
through the support rod to the guide head. From there, the gas is
guided to the double hollow needle (see next chapter).
4
5
Figure 4 Mounting the support rod
5Insert the support rod into the opening intended for this purpose
from above and push it downwards until it hits the stop. Observe the
orientation of the support rod.
6Pull out the tubing inside the support rod as far as possible. You
might want to use a piece of sand paper to be able to better grasp
the tubing.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation
860 KF Thermoprep ￭￭￭￭￭￭￭￭ 11
7
6
Figure 5 Mounting the tubing
7Fasten the tubing on the olive of the 4.860.4260 adapter.
8Pull out the support rod as far as possible so that the adapter rests
closely on the support rod.
10
8
9
Figure 6 Attaching the adapter
9Attach the adapter to the support rod. Fasten the screw into the sup-
port rod with the aid of a hex key.
10 Carefully push the support rod downwards.

3.4 Mounting the sample holder ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
12 ￭￭￭￭￭￭￭￭ 860 KF Thermoprep
11
Figure 7 Mounted support rod
11 Fix the support rod with the V.0434.008 hex screw following the
illustration. The screw and the corresponding hex key are enclosed
separately with the instrument.
3.4 Mounting the sample holder
6.2063.010
6.2627.000
Figure 8 Mounting the sample holder
NOTICE
The sample holder may not be inserted or removed unless it has cooled
down.