860 KF Thermoprep: Manual

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860 KF Thermoprep

Manual
8.860.8003EN
Metrohm AG
CH-9100 Herisau
Switzerland
Phone +41 71 353 85 85
Fax +41 71 353 89 01
[email protected]
www.metrohm.com

860 KF Thermoprep

Manual

8.860.8003EN 11/2016
Technische Dokumentation
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

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 power cord ................................................. 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 ............................................ 14
3.7 Mounting the dust filter .................................................... 16
3.8 Assembling drying flasks ................................................... 16
3.9 Assembling the air/nitrogen connector ............................ 18
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

860 KF Thermoprep ■■■■■■■■ III


Table of contents ■■■■■■■■■■■■■■■■■■■■■■

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

5 Performing 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

6 Operation and maintenance 36


6.1 General ................................................................................ 36
6.2 Care ...................................................................................... 36
6.3 Quality management and qualification with Metrohm . . 37

7 Troubleshooting 38
7.1 Problems and their solutions ............................................. 38

8 Appendix 39
8.1 Practical notes .................................................................... 39
8.2 Literature ............................................................................. 40

9 Technical specifications 41
9.1 Oven ..................................................................................... 41
9.2 Gas flow .............................................................................. 41
9.3 Outlet heater ....................................................................... 41
9.4 Power connection ............................................................... 42
9.5 Ambient temperature ......................................................... 42
9.6 Reference conditions .......................................................... 42
9.7 Dimensions .......................................................................... 42

10 Accessories 43
10.1 2.860.0010 scope of delivery ............................................ 43
10.2 Optional accessories ........................................................... 50

Index 51

IV ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ Table of figures

Table of figures
Figure 1 Front 860 KF Thermoprep ................................................................. 6
Figure 2 Rear 860 KF Thermoprep ................................................................... 7
Figure 3 Connecting the power cord ............................................................... 8
Figure 4 Loosening the adapter ...................................................................... 9
Figure 5 Mounting the support rod ............................................................... 10
Figure 6 Mounting the tubing ....................................................................... 10
Figure 7 Attaching the adapter ..................................................................... 11
Figure 8 Mounted support rod ...................................................................... 11
Figure 9 Mounting the sample holder ........................................................... 12
Figure 10 Mounting the needles ..................................................................... 13
Figure 11 Mounting the heating tubing (rear view) ......................................... 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 connector .................................................................... 18
Figure 17 Coulometric KF titration cell ............................................................ 19
Figure 18 Volumetric KF titration cell .............................................................. 20
Figure 19 Power switch .................................................................................. 22
Figure 20 Keypad of the 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

860 KF Thermoprep ■■■■■■■■ V


■■■■■■■■■■■■■■■■■■■■■■ 1 Introduction

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.

860 KF Thermoprep ■■■■■■■■ 1


1.2 About the documentation ■■■■■■■■■■■■■■■■■■■■■■

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.

2 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 1 Introduction

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

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.

860 KF Thermoprep ■■■■■■■■ 3


1.3 Safety instructions ■■■■■■■■■■■■■■■■■■■■■■

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 supply cable 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
necessary.

4 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 1 Introduction

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 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.

860 KF Thermoprep ■■■■■■■■ 5


■■■■■■■■■■■■■■■■■■■■■■

2 Overview of the instrument

1 8

5
9
6

10
7 11

12

13

Figure 1 Front 860 KF Thermoprep

1 Guide head 2 Needle holder (6.2049.040)


With needle adapter.

3 Spring sleeve 4 Guidance rod


With vessel stripper.

5 Sample vessel (6.2419.007) 6 Sample holder (6.2063.010)


With 6 ml content.

7 Oven module 8 Fixing lever


With sheet metal housing.

9 Operating unit 10 Drying flasks (6.1608.050)


With display and keyboard. With 6.1602.145 drying flask insert.

11 Drying flask holder 12 Gas inlet


With M6 thread.

13 Gas outlet
With M6 thread.

6 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 2 Overview of the instrument

2
3
7

4 5 6
Figure 2 Rear 860 KF Thermoprep

1 Air pump inlet 2 Mains switch


With 6.2724.010 dust filter.

3 Mains connection socket 4 Type plate


Contains specifications concerning mains
voltage and serial number.

5 Outlet heating connection 6 Air/nitrogen connector


For the heating tube. With M6 interior thread. Inlet for external
gassing.

7 Fan 8 Cable holder (6.2060.010)


For cooling the oven module.

860 KF Thermoprep ■■■■■■■■ 7


3.1 Setting up the instrument ■■■■■■■■■■■■■■■■■■■■■■

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, 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 power cord

WARNING

This instrument may only be operated with the specified supply voltages
(see rear of the instrument).
Protect the connection sockets against moisture.

Figure 3 Connecting the power cord

8 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 3 Installation

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:

1 Move the guide head of the support rod a bit downwards by press-
ing the locking lever.

1 2

Figure 4 Loosening the adapter

2 Loosen the adapter on the head of the support rod with a hex key.

3 Removing the adapter.

4 Insert the tubing jutting out of the housing from below into the sup-
port rod.

NOTE

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).

860 KF Thermoprep ■■■■■■■■ 9


3.3 Mounting the support rod ■■■■■■■■■■■■■■■■■■■■■■

Figure 5 Mounting the support rod

5 Insert 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.

6 Pull 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.

7
6

Figure 6 Mounting the tubing

7 Fasten the tubing on the olive of the 4.860.4260 adapter.

8 Pull out the support rod as far as possible so that the adapter rests
closely on the support rod.

10 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 3 Installation

10

Figure 7 Attaching the adapter

9 Attach 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.

11

Figure 8 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.

860 KF Thermoprep ■■■■■■■■ 11


3.4 Mounting the sample holder ■■■■■■■■■■■■■■■■■■■■■■

3.4 Mounting the sample holder

6.2063.010

6.2627.000

Figure 9 Mounting the sample holder

NOTE

The sample holder may not be inserted or removed unless it has cooled
down.

The dimensions of the supplied sample holder are optimized for the usage
of 6.2419.007 6-mL sample vials by Metrohm. This ensures the best possi-
ble transfer of heat between oven and sample.

1 Place the 6.2627.000 oven insert into the oven from above.

2 Place the 6.2063.010 sample holder into the oven from above.

If vessels with other dimensions are to be used, then individually modified


sample holders can be ordered. The precise vessel dimensions (including
tolerances) are required. 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

12 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 3 Installation

3.5 Mounting the needles


The length of the needle holder defines how deep the needle for the gas
inlet enters the sample vessel. The 6.2049.040 needle holder with a
length of 58 mm ensures that the needle penetrates the liquid or powdery
sample. The carrier gas flows through the sample and efficiently removes
the contained moisture.
If the heated sample may block the needle, use the 6.2049.050 needle
holder with a length of 73 mm. In this case, the needle for the gas inlet
enters the sample vessel slightly more than the outlet needle and it does
not have any contact with the sample. The 6.2049.050 needle holder can
be ordered at Metrohm if required.
Needle holders with the dimensions required for situations calling for spe-
cial sample vessels can be supplied by Metrohm upon request.

6.1805.100

4 4

6.2816.070 3

1
6.2049.040

6.2816.080
2

Figure 10 Mounting the needles


Mount the needles as follows:

1 Screw the 6.2049.040 needle holder into the distributor on the


guide head.

860 KF Thermoprep ■■■■■■■■ 13


3.6 Mounting the heating tubing ■■■■■■■■■■■■■■■■■■■■■■

2 Screw the 6.2816.080 outlet needle onto the Luer connector of


the needle holder.

3 Carefully guide the 6.2816.070 needle for gas inlet into the
opening of the distributor from above and allow it to drop down.

NOTE

Ensure that the white PTFE seal sits firmly on the needle.

4 Screw the 6.1805.100 FEP tubing onto the opening of the distri-
butor by hand. Screw the other end of the tubing onto the opening
on the upper side of the support rod.

3.6 Mounting the heating tubing

6.2060.010 2 6.1830.030
1
3

Figure 11 Mounting the heating tubing (rear view)


Proceed as follows:

1 Screw the M6 connector of the 6.1830.030 heating tubing into


the lateral opening of the distributor on the guide head.

2 Use the accompanying knurled screw to screw the 6.2060.010


cable holder tightly onto the guide head from below.

14 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 3 Installation

3 Guide the heating tubing cable through the eyelet of the cable
holder.

NOTE

The cable holder prevents the cable of the heating tubing from
coming into contact with parts of the housing that are hot.

4 Connect the heating tubing cable to the Outlet heater connector


on the rear of the instrument.

Figure 12 Connecting the heating tubing


Rotate the plug in such a way that the three contact pins correspond
to the sequence of the corresponding socket openings. Press the
plug towards the socket and rotate the front knurled screw clock-
wise.

NOTE

The heating jacket of the heating tubing is heated up to approx.


40 to 50 °C as soon as the instrument is switched on. This pre-
vents condensation of moisture in the tubing when it is removed
from the sample and transferred to a KF titration cell with a carrier
gas.

860 KF Thermoprep ■■■■■■■■ 15


3.7 Mounting the dust filter ■■■■■■■■■■■■■■■■■■■■■■

3.7 Mounting the dust filter


The installed air pump must be protected from dust. For this reason, a
6.2724.010 dust filter must be placed on the air inlet (Inlet filter) on
the right-hand side of the housing..

6.2724.010

Figure 13 Mounting the dust filter


The dust filter should be replaced once a year.

3.8 Assembling drying flasks


Two drying flasks with desiccant are integrated into the gas flow to dry
the supplied gas. Dust (e.g. from the desiccant) must be prevented from
finding its way into the sample vessel.

6.1602.145

6.1821.040 3
2

1
6.2811.000

6.1608.050
Figure 14 Preparing the drying flasks
Prepare the two drying flasks as follows:

1 Fill both 6.1608.050 drying flasks with 6.2811.000 molecular


sieve.

2 Screw one 6.1821.040 filter tube into each of the 6.1602.145


drying flask caps from below. Tighten the filter tubes by hand.

16 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 3 Installation

3 Screw the two drying flask caps with the filter tubes onto the drying
flasks. Tighten the caps by hand.

NOTE

If drying flask caps or filter tubes are not tightened well, the gas
flow may not be precise and regular. The error message "Flow rate
error" usually occurs when screw connections are not tight.

6.1805.010
6.1805.080
6.1805.080 4

3
2

1
1
3

Figure 15 Mounting the tubings


Mount the FEP tubings as follows:

1 Insert the two drying flasks that have been prepared into the holders,
see illustration.

2 Screw one 6.1805.080 FEP tubing (25 cm length) to the gas outlet
(at the front, labeled 1). Screw the other tubing end on the front dry-
ing flask to the M6 connector without point marking (see left-hand
arrow).

3 Screw the second 6.1805.080 FEP tubing (25 cm length) to the gas
inlet (at the rear, labeled 2). Screw the other tubing end on the rear
drying flask to the M6 connector with point marking (see right-hand
arrow).

860 KF Thermoprep ■■■■■■■■ 17


3.9 Assembling the air/nitrogen connector ■■■■■■■■■■■■■■■■■■■■■■

4 Screw the 6.1805.010 FEP tubing (13 cm length) tightly onto the
remaining M6 connectors of the drying flasks.
The Drying flask marking on the right-hand side of the instrument
displays the diagram for the tubing.

NOTE

Tighten the screw connections well by hand.

3.9 Assembling the air/nitrogen connector


If compressed air, nitrogen or another gas is to be used for transferring
the expelled moisture, then a separate connector is available at the rear of
the instrument.
A tube with M6 thread can be connected directly to the Air/N2 in con-
nector. Enclosed with the instrument is the 6.1808.040 M6/M8 tubing
adapter for a tubing with an M8 thread. The 6.1808.050 M8/tubing
olive can additionally be put in place in order to connect a simple tubing.

6.1808.040

6.1808.050

Figure 16 External gas connector

WARNING

If gas is fed from a pressure line or a pressure vessel, a pressure reduc-


tion valve must be activated. The gas pressure must not exceed 0.3 bar
of overpressure.

18 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 3 Installation

3.10 Inserting the heating tube into the KF titration cell


The 860 KF Thermoprep can be used in combination with a KF coulometer
or a volumetric KF titrator. The mounting of the tip of the heating tube is
accomplished in different ways for the respective KF titration cells.

Coulometric KF titration cell

■ Remove the protective cover from the tip of the heating tube and the
E.3010.032 O-ring.
■ Disassemble the accompanying 6.1446.170 heating tube stopper
into three parts.

6.1830.030
1 6.1446.170
2

Figure 17 Coulometric KF titration cell


Proceed as follows:

1 Guide the upper part of the heating tube stopper over the tip of the
6.1830.030 heating tube as shown in the illustration.

2 Guide the O-ring of the heating tube stopper over the heating tube.

3 Guide the lower part of the heating tube stopper over the heating
tube and screw the three parts together (not too tightly).

4 Insert the stopper with the tip of the heating tube into one of the
two SGJ openings of the KF titration cell

860 KF Thermoprep ■■■■■■■■ 19


3.10 Inserting the heating tube into the KF titration cell ■■■■■■■■■■■■■■■■■■■■■■

5 Shift the tip vertically in such a way that the outlet opening of the
tubing is immersed as deeply as possible. The tip must not however
be permitted to get in the way of the stirring bar in the KF titration
cell. Afterwards give the heating tube stopper its final tightening.

Volumetric KF titration cell

■ Remove the protective cover from the tip of the heating tube and the
E.3010.032 O-ring. The latter you will still need.
■ A 6.2730.020 septum stopper is enclosed with every KF titrator
made by Metrohm. Disassemble this septum stopper into three parts
and remove the septum. It will not be required.

6.1830.030

1 6.2730.020

E.3010.032 2
3

Figure 18 Volumetric KF titration cell


Proceed as follows:

1 Guide the upper part of the septum stopper over the tip of the
6.1830.030 heating tube as shown in the illustration.

2 Guide the E.3010.032 O-ring over the heating tube.


This O-ring is also part of the 6.1244.040 set of seals that is enclosed
with each KF titrator. It cannot be reordered individually.

3 Guide the lower part of the septum stopper over the heating tube
and screw the three parts together (not too tightly).

4 Insert the stopper with the tip of the heating tube into the front
opening of the KF titration cell

20 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 3 Installation

5 Shift the height of the tip of the heating tube vertically in such a way
that the outlet opening of the tubing is immersed as deeply as possi-
ble. The tip must not however be permitted to get in the way of the
stirring bar in the KF titration cell. Afterwards give the septum stop-
per its final tightening.

860 KF Thermoprep ■■■■■■■■ 21


4.1 Switching the instrument on and off ■■■■■■■■■■■■■■■■■■■■■■

4 Operation

4.1 Switching the instrument on and off


The toggle switch for switching on and off is located on the rear of the
instrument.

Figure 19 Power switch


The oven is switched on automatically after the instrument has been
switched on and it is heated to the temperature that was set last. At the
same time, the outlet heating of the heating tubing is also switched on.

4.2 The keypad

Figure 20 Keypad of the operating unit

Key functions in the main dialog


[FLOW] Switches the gas flow on or off.
[TEMP] Switches between the two target temperatures.
[QUIT] No function.
[OK] Opens parameter menu.

22 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 4 Operation

[◀] Reduces the gas flow by 1 mL/min during operation.


Press the key shortly.
[▶] Increases the gas flow by 1 mL/min during operation.
Press the key shortly.
[▲] Reduces the brightness of the display.
[▼] Increases the brightness of the display.

4.3 The display


4.3.1 Display elements

3
4
2
5

Figure 21 Main dialog

1 Temperature display 2 Icon of the status display


Shows the measured oven temperature.

3 Gas flow display 4 Target temperature


Shows the set gas supply and the flow rate. Shows the set specification (temp. 1 or
temp. 2).

5 Status display
Shows status and error messages.

4.3.2 Status display


Table 1 Icons of the status display
Icon Meaning
The oven is heated.

The oven is cooled.

The predefined temperature has been reached.

860 KF Thermoprep ■■■■■■■■ 23


4.3 The display ■■■■■■■■■■■■■■■■■■■■■■

Icon Meaning
An error has occurred. The error type is shown in the
status display.

4.3.3 Error messages


Table 2 Error messages
Error message Cause Remedy
Flow rate error The tubing system Tighten all tubing connec-
is leaking or the tions and screws of the
flow rate is set too drying flasks.
high.
Check the function of the
pump.
The pressure is too Regulate the pressure of
low or too high the external gas to 0.1 -
during external gas 0.3 bar.
supply.
The flow sensor is Contact a service engineer.
defective.
Max. temp. The oven tempera- Switch off the instrument
reached ture is higher than immediately and let the
265 °C. The tem- oven cool down.
perature control
If the error reoccurs again
might be defective.
when switching the instru-
ment on, contact a service
engineer.
Adj. data missing The adjustment The instrument must be
data of the instru- adjusted again. Contact a
ment is not cor- service engineer.
rect.

24 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 4 Operation

4.4 Modifying numerical values and settings


The settings of the instrument can be modified in two ways:
■ Selection of predefined values from a list. Parameters with selection
lists are marked with a colon (:).
■ Modifying numerical values.
The various parameters can be selected using the [▼] and [▲] arrow keys.
The current line will be displayed reversed.

4.4.1 Selecting from a selection list


You can modify parameters with selection lists (e.g. Flow source:) using
the [▶] or [◀] arrow keys. The next value in the selection list is usually dis-
played.
Apply the modified value with the [OK] key.

4.4.2 Modifying numerical values


Modify parameters with numerical values using the arrow keys:

1 Use the [▶] or [◀] arrow keys to select a digit of the numerical value.
The selected digit is displayed in black on white. The colors for the
rest of the line remain reversed.

2 Modify the digit using the [▲] or [▼] arrow keys.

3 Select the next digit and modify it, etc.

4 Apply the modified value with the [OK] key.


Press [QUIT] if the previous value is to be restored.

860 KF Thermoprep ■■■■■■■■ 25


4.5 Parameters ■■■■■■■■■■■■■■■■■■■■■■

4.5 Parameters
[OK]
The instrument parameters can be set in a menu which can be opened
with the [OK] key. Quit the parameter menu with [QUIT].

NOTE

Modified values are applied by pressing [OK]. A modification is discar-


ded with [QUIT].

Temp. 1
Default value for temperature 1.
Input range 50 - 250 °C (Increment: 1)
Default value 100 °C

Temp. 2
Default value for temperature 2.
Input range 50 - 250 °C (Increment: 1)
Default value 100 °C

Gas flow
Default value for the gas flow.
Input range 10 - 150 mL/min (Increment: 1)
Default value 50 mL/min

Gas type
Selection of the gas.
Selection air | nitrogen | other
Default value air
other
A measuring factor must be specified for the gas used when selecting
other. The measuring factor is used for the correct measurement of
the flow rate.

Meas. factor
Measuring factor for measuring the flow rate of the gas. This setting is
only possible if other was selected as gas. For air and nitrogen, the corre-
sponding measuring factor is inserted automatically.

26 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 4 Operation

Only if 'gas type' = 'other'.


Input range 0.001 - 2.000 (Increment: 0.001)
Default value 1.000

Flow source
Selection of the gas supply.
Selection pump | valve
Default value pump
pump
Built-in air pump.
valve
Inlet valve for inert gas.

4.6 Configuration
[TEMP]
The basic settings of the instrument can be configured in the setup menu.
You can open the menu by pressing the [TEMP] key while switching the
instrument on. Press [QUIT] to close the menu.

NOTE

The setup menu can be opened even if the key lock is on.

Lock keys
Key lock. The [OK], [◀] and [▶] keys can be locked. With this, you can
prevent that changes are made in the parameter menu or that the gas
flow is changed during a determination. If this function is enabled (on),
you can only switch between temperature 1 and temperature 2 and
switch the gas flow on or off. The brightness of the display can still be
adjusted.
Selection off | on
Default value off

Temp.corr
Temperature correction. The default value for the temperature control of
the oven can be influenced by this correction value. In this way, you can
adjust a temperature difference between the oven module and the sample
in the vessel if required.
Input range -10 - 10 °C (Increment: 1)
Default value 0 °C

860 KF Thermoprep ■■■■■■■■ 27


4.6 Configuration ■■■■■■■■■■■■■■■■■■■■■■

The determination of the necessary temperature correction can be accom-


plished with a special oven insert and should be performed by a service
engineer. Contact your responsible Metrohm supplier.

28 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 5 Performing a determination

5 Performing a determination
Moisture determinations according to the heating method require the
conditioning of the entire tubing system and of the KF titration cell before
a determination can be carried out. Because the sample vials and the sep-
tum seals may contain small amounts of moisture, three to five blank
value determinations must be carried out with sealed, empty vessels.
Solid or liquid samples are weighed out into sample vials, which are then
sealed. We recommend the use of 6.2419.007 sample vials with
6.1448.057 septum seals. The silicone septum of the aluminum cap resists
temperatures of up to 250 °C and has proven itself to be an optimum
solution.

5.1 Conditioning the system


The entire system must be conditioned prior to use, i. e. it must be abso-
lutely water-free. The oven must be heated to the desired working tem-
perature for this purpose. The needle must be inserted into a sealed sam-
ple vessel (conditioning vessel) in order to flush the entire tubing system
with the carrier gas. The gas supply is thus connected with the heating
tube.

5.1.1 Preparing the KF titration cell

Filling the KF titration cell

The KF titration cell must remain filled with conditioned working medium
when not in use. The working medium must be replaced from time to
time, even though the sample is not transferred into the working medium
during the heating-out process.
Prepare the KF titration cell as follows:

1 Fill the KF titration cell with working medium. We recommend


approximately 150 mL of working medium when using a Coulometer
cell and approximately 35 mL with a volumetric KF titration cell. The
shaft of the heating tube should, however, not be immersed.

2 Align the tip of the heating tube against the vessel wall.

3 Switch on the stirrer. Set the stirring rate to high.

860 KF Thermoprep ■■■■■■■■ 29


5.1 Conditioning the system ■■■■■■■■■■■■■■■■■■■■■■

It is advantageous to have air bubbles stirred into the working


medium and forcefully broken up in the process. The air in the KF
titration cell must also be dried.

Conditioning the working medium

1 Load a conditioning method on the KF titrator and begin the condi-


tioning by pressing the [Start] key.
You will find the necessary settings in the KF titrator manual.

NOTE

It is imperative that an extraction time of at least 300 seconds


be set for a determination using the heating method.

5.1.2 Preparing the 860 KF Thermoprep

Switch on the 860 KF Thermoprep and select the tempera-


ture

The necessary settings on the 860 KF Thermoprep:

1 Switch on the instrument.

2 Select one of the preset temperatures using the [TEMP] key.


If you would like to change Temp. 1 or Temp. 2, press [OK].

Inserting the conditioning vessel

1 Seal an empty sample vessel tightly with a septum seal. To do this,


use the crimping tongs.

2 Insert the sample vessel into the oven.

NOTE

Caution! The oven is hot. Use the crimping tongs to insert the
sample vessel.

30 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 5 Performing a determination

Figure 22 Insert the sample vessel into the oven

Inserting the needle

1 Grip the guide head with both hands and press the fixing lever.

Figure 23 Move the guide head down

2 Move the guide head down and insert the needle into the sample
vessel.

860 KF Thermoprep ■■■■■■■■ 31


5.1 Conditioning the system ■■■■■■■■■■■■■■■■■■■■■■

Figure 24 Insert the needle

Switching on the gas flow

1 Press the [OK] key and adjust the flow rate (Gas flow), e. g.
50 mL/min. Use the arrow keys [▶] or [◀] to select the number of
decimal places, and then [▲] or [▼] to change the value.

2 Confirm the entry by pressing [OK] and select Flow source.

3 Using the arrow keys [▶] or [◀], select pump or valve (if you are
using an external carrier gas) and confirm by pressing [OK].

4 Close the Parameters menu by pressing [QUIT].

5 Press the [FLOW] key.


The gas flow is switched on. The flow rate gradually approaches the
level set.

NOTE

The carrier gas should emerge from the tip of the heating tube into the
working medium as tiny bubbles and be spun there forcefully. Alter the
stirring rate if necessary. The tip of the tubing should be immersed until
it reaches the bottom of the KF titration cell and be rotated against the
vessel wall.

Allow the system to condition for a few minutes and swirl the KF titration
cell now and again in order to remove the last traces of moisture. Check
whether the set oven temperature has been reached.

32 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 5 Performing a determination

NOTE

The signal drift on the KF titrator should be less than 20 µg/min (or
µL/min) and remain stable for at least 2 minutes before the blank value
determination can be started.

5.2 Determining the blank value


Because the surface of the sample vessels and the air enclosed in the ves-
sel could contain moisture, it is imperative that three to five blank value
determinations be carried out. One determination with an empty, tightly
sealed sample vessel is carried out in each case. The result is calculated as
the quantity of water expelled from the sample vessel. The titration
parameters used for a regular sample must also be applied to blank value
determinations. Select a relative stop drift of 5 µg/min (or µL/min) as the
stop criterion.

Preparing the blank

The system should already be conditioned. A conditioning vessel must be


in the oven at this stage and the needle must already be inserted.

1 Seal three to five sample vessels tightly with the crimping tongs.

2 Check that the oven temperature and the gas flow rate correspond
to the values which have been set.

3 Wait until the working medium in the KF titration vessel has been
conditioned and the signal drift is stable.

Starting the blank value determination

1 Start the determination by pressing the [Start] key on the KF titrator.

2 Use both hands to move the guide head of the 860 KF Thermoprep
upward while pressing the fixing lever.
Refer to the illustrations on pages 31 ff.

3 Remove the conditioning vessel from the oven with the crimping
tongs.

860 KF Thermoprep ■■■■■■■■ 33


5.3 Determining samples ■■■■■■■■■■■■■■■■■■■■■■

NOTE

Caution! The vessel is hot.

4 Place the blank into the oven using the crimping tongs.

5 Use both hands to move the guide head downward and insert the
needle into the blank.

Waiting for the determination

1 Wait until the determination is finished. Conditioning will then be


resumed automatically.

2 Repeat the blank value determination with the next blank.

5.3 Determining samples


The blank value must be subtracted from the calculated consumption
when determining a sample.

Preparing the KF titrator

1 Load a suitable method.

2 Start the conditioning by pressing the [Start] key.

Preparing the sample

1 Weigh the sample into a sample vessel and seal it tightly with the
crimping tongs.

2 Check that the oven temperature and the gas flow rate correspond
to the values which have been set.

3 Wait until the working medium in the KF titration vessel has been
conditioned and the signal drift is stable.

34 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 5 Performing a determination

Starting the sample determination

1 Start the determination by pressing the [Start] key on the KF titrator.

2 Use both hands to move the guide head of the 860 KF Thermoprep
upward while pressing the fixing lever.
Refer to the illustrations on pages 31 ff.

3 Remove the blank from the oven with the crimping tongs.

NOTE

Caution! The vessel is hot.

4 Place the sample vessel into the oven using the crimping tongs.

5 Use both hands to move the guide head downward and insert the
needle into the sample vessel.

Waiting for the determination

1 Wait until the determination is finished. Conditioning will then be


resumed automatically.

2 Repeat the determination with the next blank.

860 KF Thermoprep ■■■■■■■■ 35


6.1 General ■■■■■■■■■■■■■■■■■■■■■■

6 Operation and maintenance

6.1 General
The 860 KF Thermoprep requires appropriate care. Excess contamination
of the instrument may result in malfunctions and a reduction in the service
life of the sturdy mechanical and electronic components.
Severe contamination can also have an influence on the measured results.
Regular cleaning of exposed parts can prevent this to a large extent.
Spilled chemicals and solvents must be removed immediately. In particular,
the power plug should be protected from contamination.

6.2 Care
■ Replace exhausted molecular sieve promptly. You should replace the
molecular sieve as soon as increased drift values appear in the Karl
Fischer cell.
■ Check all tubing connections regularly for leaks.
■ Rinse the tubing connections from time to time. Carefully dry the tub-
ing afterward. The tubing must be replaced after prolonged usage.
■ Replace the dust filter once a year.
■ Clean the sample holder regularly.

WARNING

Clean the oven only with the instrument switched off and while it is
cold.

36 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 6 Operation and maintenance

6.3 Quality management and qualification with


Metrohm
Quality management
Metrohm offers you comprehensive support in implementing quality man-
agement measures for instruments and software.

Qualification
Please contact your local Metrohm representative for support in qualifica-
tion of instruments and software. The Installation Qualification (IQ)
and Operational Qualification (OQ) are offered by Metrohm represen-
tatives as a service. They are carried out by trained employees using stan-
dardized qualification documents and in accordance with the currently
applicable requirements of the regulated industry.

Maintenance
The electronic and mechanical modules of Metrohm instruments can and
should be checked by specialist personnel from Metrohm as part of a reg-
ular preventive maintenance schedule. Please ask your local Metrohm rep-
resentative regarding the precise terms and conditions involved in con-
cluding a corresponding maintenance agreement.
For detailed information on this topic, please visit www.metrohm.com.

860 KF Thermoprep ■■■■■■■■ 37


7.1 Problems and their solutions ■■■■■■■■■■■■■■■■■■■■■■

7 Troubleshooting

7.1 Problems and their solutions


Problem Cause Remedy
The drift is very high Molecular sieve of drying Replace molecular sieve.
during conditioning. flasks and/or the titration
cell exhausted.

The titration cell is leaking Check seals. If necessary, replace.

The titration time is The sample is non-homo- Reduce the size of the sample before weighing
too long. genous in.

Not the entirety of the Select more stringent switch-off criteria on the
moisture expelled. KF titrator: lower stop drift, higher switch-off
delay time.

Tubing connections leaking Inspect tubing and replace as necessary.

The results are Molecular sieve of drying Replace molecular sieve.


spread widely. flasks exhausted.

Condensate in the heating ■ Dry the tubing.


tube. ■ Reduce the gas flow.
■ Perhaps lower the oven temperature.

Gas flow too high. Reduce the gas flow.

The sample is non-homo- Reduce the size of the sample before weighing
genous in.

Selected gas flow is System is leaking Check all tubing connections and drying flasks
not achieved. for leaks.

Pressure from external gas Adjust gas pressure (max. 0.3 bar).
supply either too low or
too high.

Pump defective Contact a service technician.

38 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 8 Appendix

8 Appendix

8.1 Practical notes


Carrier gas selection
If the hot sample is sensitive to air or oxygen (decomposition) and if it
releases substances that disrupt the KF reaction, then nitrogen (N2) should
be used as the carrier gas.

Temperature setting
The temperature selected should be as high as the sample allows (high
temperature = shorter analysis time). The sample may not, however,
decompose. It must only release water and not any oxidizable substances.
The temperature displayed refers to the temperature in the heating block
and not to the sample temperature. Depending on the vial size used, the
gas flow and the temperature setting, the actual temperature of the sam-
ple can deviate up to 10%.

Gas flow
Once the needle is inserted into the sample vessel until it stops, the gas
flow moves through the sample and then through the outlet needle into
the titration vessel where the moisture is titrated. If the needle is not per-
mitted to immerse into the sample, then a longer needle holder can be
used.
The gas flow should be kept as low as possible. Particularly in the case of
very moist samples, care must be taken to ensure that water is not
released too quickly and in excessively large quantities into the titration
vessel. In addition, there is the danger of condensate formation in the
heating tubing. The working medium in the cell must be able to absorb
the moisture that is expelled without delay. Normally, a flow rate of 40 to
60 mL/min is optimal.
The tolerances for gas flow measurement depend on the system: They
depend on the pressure, temperature, measuring system and the gas
itself, and a deviation of 20% is possible.
The gas flow measurement is calibrated with air; other gases deviate more
or less strongly from that.
If required, the flow rate of the gas can be checked using a flow measur-
ing instrument at the local pressure and current temperature. An individ-
ual measuring factor can be entered with the Meas. factor parameter so
that the corrected gas flow is displayed. At the same time, however,
other must be selected for the Gas type parameter.

860 KF Thermoprep ■■■■■■■■ 39


8.2 Literature ■■■■■■■■■■■■■■■■■■■■■■

Extraction time
An extraction time of min. 5 minutes should be set on the titrator in order
to prevent the titration from being canceled before the sample has
released its water.

Conditioning the system


The system must be conditioned with an empty, sealed sample vial (condi-
tioning vial) before a determination is made.

8.2 Literature
■ E. Scholz, Hydranal® Manual, Riedel-de Haën
■ P. Bruttel, R. Schlink, Water Determination by Karl Fischer Titration
Monograph, Metrohm, 2006, Order no. 8.026.5013

40 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 9 Technical specifications

9 Technical specifications

9.1 Oven
Temperature 50 - 250 °C
range
Accuracy ±3 °C
Correction range –10 - +10 °C
Heating cartridges 165 W (typical)
performance Dependent on supply voltage
Heating rate Typically 15 °C/min (at 80 - 180 °C, 230 V)
Dependent on temperature, supply voltage, sample amount and vessel
dimensions
Cooling rate Typically 9 °C/min (at 180 - 80 °C)
Dependent on temperature, sample amount and vessel dimensions

9.2 Gas flow


Flow range 10 - 150 mL/min
Under normal conditions, calibrated with air at approx. +25 °C and
1,013 mbar.
Deviations of gas amount per time unit of ±20% are possible.

9.3 Outlet heater


Socket connection U = 16 ±1 V
I ≤ 0.8 A
Typical tubing approx. 50 °C
temperature

860 KF Thermoprep ■■■■■■■■ 41


9.4 Power connection ■■■■■■■■■■■■■■■■■■■■■■

9.4 Power connection


Potential 100 - 120 / 220 - 240 V
Frequency 50 / 60 Hz
Power consump- 200 W
tion
Fuse 2.0 ATH

9.5 Ambient temperature


Nominal function 5 - 45 °C
range Humidity < 80%
Storage –20 - 70 °C
Transport –40 - 70 °C

9.6 Reference conditions


Ambient tempera- 25 °C (±3 °C)
ture
Relative humidity ≤ 60%
Supply voltage 230 V

9.7 Dimensions
Width 0.44 m
Height 0.18 m (without support rod)
0.50 m (with support rod)
Depth 0.23 m
Weight (without 8.17 kg
accessories)
Material
Housing Cover and bottom: Steel sheet, stove-enameled
Oven covering PTFE
Operating unit Polycarbonate / Acrylonitrile butadiene styrene (PC/ABS)

42 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 10 Accessories

10 Accessories
NOTE

Subject to change without notice.

10.1 2.860.0010 scope of delivery

Qty. Order no. Description


1 1.860.0010 860 KF Thermoprep
Instrument for the expulsion of moisture from solid and liquid sam-
ples

1 6.1446.170 Heating tube stopper


For coulometric KF vessels in connection with heatable tubing con-
nection
Material: PP
Height (mm): 34
Outer diameter (mm): 13

1 6.1448.057 Aluminum septum cap / 100 pieces


Including Al seal.
Material: Aluminum
Material 2: Silicone
Height (mm): 7.4
Outer diameter (mm): 20.7

2 6.1602.145 Drying flask cap


Drying flask cap with GL45 thread for 6.1608.050

860 KF Thermoprep ■■■■■■■■ 43


10.1 2.860.0010 scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


2 6.1608.050 Drying flask / 100 mL / GL 45

Material: Clear glass


Height (mm): 100
Outer diameter (mm): 56
Volume (mL): 100

1 6.1805.010 FEP tubing / M6 / 13 cm


With light protection and protection against kinks.
Material: FEP
Inner diameter (mm): 2
Length (mm): 130

2 6.1805.080 FEP tubing / M6 / 25 cm


With light protection and protection against kinks.
Material: FEP
Inner diameter (mm): 2
Length (mm): 250

44 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 10 Accessories

Qty. Order no. Description


1 6.1805.100 FEP tubing / M6 / 40 cm
With light protection and protection against kinks.
Material: FEP
Inner diameter (mm): 2
Length (mm): 400

1 6.1808.040 Adapter M6 outer / M8 inner


Thread M6 outer, M8 inner.
Material: PCTFE

1 6.1808.050 Tubing adapter olive / M8


1 M8 outer thread and 1 tubing olive, e.g. for the thermostat casing
of exchange units and stability measuring instruments.
Material: PVDF
Length (mm): 31.5

860 KF Thermoprep ■■■■■■■■ 45


10.1 2.860.0010 scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


2 6.1821.040 Filter tube
Filter tube for 6.1608.050 drying flask. For Rancimats and Karl
Fischer ovens.
Length (mm): 112

1 6.1830.030 Heatable outlet tubing


Heatable outlet tubing for the 860 KF Thermoprep.

1 6.2048.030 Guidance rod


Guidance rod for 860 KF Thermoprep.

1 6.2049.040 Needle holder with Luer lock for 860 KF


Thermoprep
Length (mm): 58

46 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 10 Accessories

Qty. Order no. Description


1 6.2060.010 Cable holder
Used with 860 KF Thermoprep.

1 6.2063.010 Sample holder for 6.2419.007 6 mL sample


vials

1 6.2419.007 Sample vial 6 mL / 100 pieces


Suitable for the 6.1448.057 septum. Utilization for KF determinations
with oven.
Volume (mL): 6

1 6.2621.110 Septum crimping tongs


Septum crimping tongs for sealing 6 mL sample vessels (6.2419.000,
6.2419.007).
Length (mm): 210

860 KF Thermoprep ■■■■■■■■ 47


10.1 2.860.0010 scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1 6.2621.120 Hex key 1.5 mm

1 6.2621.130 Hex key 2 mm

1 6.2627.000 Oven insert


Used with 860 KF Thermoprep.

1 6.2724.010 Dust filter


Dust filter for Rancimats and for Karl Fischer ovens.
Outer diameter (mm): 44
Length (mm): 53

1 6.2739.000 Wrench
For tightening connectors
Length (mm): 68

48 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ 10 Accessories

Qty. Order no. Description


1 6.2811.000 Molecular sieve
Molecular sieve. Bottle containing 250 g. Pore size: 0.3 nm. Without
moisture indicator. For Rancimats and Karl Fischer instruments.

1 6.2816.070 Needle for gas inlet


For 832 KF Thermoprep.
Material: Stainless steel (AISI 304)

1 6.2816.080 Outlet needle


For KF Thermoprep Oven Sample Processor.
Material: Stainless steel (AISI 304)

1 6.2122.0x0 Power cord with IEC-60320-C13 line socket


Cable plug according to customer requirements.
Switzerland: Type SEV 12
6.2122.020
Germany, …: Type CEE(7), VII
6.2122.040
USA, …: Type NEMA/ASA
6.2122.070

1 8.860.8003DE 860 KF Thermoprep manual

860 KF Thermoprep ■■■■■■■■ 49


10.2 Optional accessories ■■■■■■■■■■■■■■■■■■■■■■

10.2 Optional accessories

Order no. Description


6.1448.050 Aluminum septum caps / 1000 pieces
Including Al sealing.
Material: Aluminum
Material 2: Silicone
Height (mm): 7.4
Outer diameter (mm): 20.7

6.2049.050 Needle holder with Luer-lock for 860 KF Thermoprep


Length (mm): 73

6.2419.000 Sample vial 6 mL / 1000 pieces


For 6.1448.050 septum caps.
Height (mm): 38
Outer diameter (mm): 22
Volume (mL): 6

50 ■■■■■■■■ 860 KF Thermoprep


■■■■■■■■■■■■■■■■■■■■■■ Index

Index
6.2627.000 oven insert ............ 12 Gas inlet ..................................... 6 Needle holder ........................... 13
Gas outlet .................................. 6 Numerical input ........................ 25
A Gas supply ................................ 27
Arrow button ........................... 23 Gas type ................................... 26 O
Arrow key ................................ 25 Guidance rod ............................. 6 Operational qualification .......... 37
Assembling Guide head .......................... 6, 31 Outlet heater ............................ 15
Drying flasks ....................... 16 outlet needle ............................ 14
H Oven module ............................. 6
B Heating tube ............................ 19 Oven temperature .............. 23, 26
Basic settings ............................ 27 Heating tubing ......................... 14
Blank value ............................... 33 P
Brightness ................................ 23 I Parameters ............................... 26
Icon ......................................... 23 Personnel safety ......................... 4
C Injection needle ........................ 14 Power connection ...................... 8
Cable holder ......................... 7, 14 Inlet Power cord ................................. 8
Carrier gas ................................ 39 Air pump .............................. 7
Colon ....................................... 25 Inlet filter .................................. 16 Q
Conditioning ............................ 29 Installation qualification ............ 37 Quality management ................ 37
Conditioning vessel .................. 30
Connector K S
Air/nitrogen .................... 7, 18 Keys ......................................... 22 Safety instructions ...................... 3
Outlet heating ...................... 7 KF titration cell ................... 19, 29 Sample determination .............. 34
Crimping tongs. ........................ 30 Coulometric ....................... 19 Sample holder ...................... 6, 12
Volumetric .......................... 20 Sample vessel ............................. 6
D Selection .................................. 25
Display ..................................... 23 L Selection list ............................. 25
Drying flask .................... 6, 16, 18 Lock keys ................................. 27 Serial number ............................. 7
Dust filter ............................. 7, 16 Service ....................................... 3
M Setup ....................................... 27
E Main dialog .............................. 22 Signal drift ................................ 33
Electrostatic charge .................... 4 Maintenance ............................ 36 Solvents ..................................... 5
Error message .......................... 24 Maintenance agreement .......... 37 Status ....................................... 23
External gas connector ............. 18 Molecular sieve ........................ 16 Supply voltage ............................ 4
Extraction time ......................... 40 Mount Support rod ................................ 9
Dust filter ........................... 16
F Heating tubing ................... 14 T
Fan ............................................. 7 Support rod .......................... 9 Temperature ................. 23, 26, 39
Fixing lever ........................... 6, 31 Tubings .............................. 17 Temperature correction ............ 27
Flow rate .................................. 23 Mounting Tubings .................................... 17
Flow rate error ......................... 17 KF titration cell ................... 19 Type plate .................................. 7
Flow source .............................. 27 Needle ............................... 13
Sample holder .................... 12 V
G Valve ........................................ 27
Gas flow ....................... 23, 26, 39 N
Needle ..................................... 13

860 KF Thermoprep ■■■■■■■■ 51

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