860 KF Thermoprep: Manual
860 KF Thermoprep: Manual
860 KF Thermoprep: Manual
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]
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
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
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
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
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
1 Introduction
CAUTION
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.
WARNING
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.
WARNING
WARNING
Supply voltage
WARNING
WARNING
WARNING
WARNING
WARNING
WARNING
1 8
5
9
6
10
7 11
12
13
13 Gas outlet
With M6 thread.
2
3
7
4 5 6
Figure 2 Rear 860 KF Thermoprep
3 Installation
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.
WARNING
This instrument may only be operated with the specified supply voltages
(see rear of the instrument).
Protect the connection sockets against moisture.
1 Move the guide head of the support rod a bit downwards by press-
ing the locking lever.
1 2
2 Loosen the adapter on the head of the support rod with a hex key.
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).
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
8 Pull out the support rod as far as possible so that the adapter rests
closely on the support rod.
10
9 Attach the adapter to the support rod. Fasten the screw into the sup-
port rod with the aid of a hex key.
11
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.
6.2063.010
6.2627.000
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.
6.1805.100
4 4
6.2816.070 3
1
6.2049.040
6.2816.080
2
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.
6.2060.010 2 6.1830.030
1
3
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.
NOTE
6.2724.010
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:
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
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).
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
6.1808.040
6.1808.050
WARNING
■ 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
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
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.
■ 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
1 Guide the upper part of the septum stopper over the tip of the
6.1830.030 heating tube as shown in the illustration.
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
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.
4 Operation
3
4
2
5
5 Status display
Shows status and error messages.
Icon Meaning
An error has occurred. The error type is shown in the
status display.
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.
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
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.
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
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.
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:
2 Align the tip of the heating tube against the vessel wall.
NOTE
NOTE
Caution! The oven is hot. Use the crimping tongs to insert the
sample vessel.
1 Grip the guide head with both hands and press the fixing lever.
2 Move the guide head down and insert the needle into the sample
vessel.
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.
3 Using the arrow keys [▶] or [◀], select pump or valve (if you are
using an external carrier gas) and confirm by pressing [OK].
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.
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.
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.
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.
NOTE
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.
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.
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
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.
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.
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.
7 Troubleshooting
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.
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.
8 Appendix
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.
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.
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
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
9.7 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)
10 Accessories
NOTE
1 6.2739.000 Wrench
For tightening connectors
Length (mm): 68
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