Metrohm 832 KF Thermoprep User manual

CH-9101 Herisau/Switzerland
E-Mail [email protected]
Internet www.metrohm.com
832 KF Thermoprep
Instructions for Use
8.832.1023 10.2004/ dm

II 832 KF Thermoprep
Teachware
Metrohm AG
Oberdorfstr. 68
CH-9101 Herisau
[email protected]
These instructions are protected by copyright. All rights reserved.
Although all the information given in these instructions has been checked with great
care, errors cannot be entirely excluded. Should you notice any mistakes please
inform the author at the address given above.
© Metrohm Ltd. 2002
Printed in Switzerland

832 KF Thermoprep III
Table of contents
1Introduction 1
1.1 Description of the instrument ..........................................................1
1.2 Information about these Instructions for Use.................................2
1.3 Parts and controls ............................................................................3
1.3.1 Individual parts and standard accessories ..............................................3
1.3.2 Rear view...................................................................................................4
1.3.3 Temperature controller..............................................................................5
1.3.4 Sample holder for standard vials ..............................................................5
2Safety information 6
2.1 General ..............................................................................................6
2.2 Electrical safety ................................................................................6
3Installation 7
3.1 Instrument setup...............................................................................8
3.1.1 Packaging .................................................................................................8
3.1.2 Checks ......................................................................................................8
3.1.3 Location.....................................................................................................8
3.2 Mains connection .............................................................................8
3.3 Assembling the 832 KF Thermoprep............................................ 10
3.3.1 Assembling the needles..........................................................................10
3.3.2 Attaching the drying bottles ....................................................................11
3.3.3 Attaching the dust filter ...........................................................................11
3.4 Assembling the coulometric cell .................................................. 12
3.5 Assembling the titration vessel for volumetric KF titrators ........ 12
4Operation 13
4.1 Inserting and removing sample vials ........................................... 13
4.2 Needle penetration ........................................................................ 13
4.3 The pump ....................................................................................... 14
4.4 The temperature controller ........................................................... 15
4.4.1 Two set temperatures .............................................................................15
4.4.2 Setting a temperature..............................................................................15
4.4.3 Self-optimization of the control parameters............................................16
4.4.4 Key lock function.....................................................................................16
4.5 Working procedure........................................................................ 17
4.5.1 Preparing the 832 KF Thermoprep/756/831 Coulometer system ..........18
4.5.2 Determination with blank value subtraction............................................18
4.5.3 Determination without blank value subtraction.......................................19
4.6 Practical information ..................................................................... 20
5Maintenance information 21
6GLP validation 21

IV 832 KF Thermoprep
7Troubleshooting 22
7.1 Problems ........................................................................................ 22
8Annex 23
8.1 Technical data................................................................................ 23
8.1.1 Oven........................................................................................................23
8.1.2 Air pump..................................................................................................23
8.1.3 Temperature controller............................................................................23
8.1.4 Power supply ..........................................................................................23
8.1.5 Safety specifications ...............................................................................23
8.1.6 Electromagnetic compatibility (EMC) .....................................................24
8.1.7 Ambient temperature ..............................................................................24
8.1.8 Dimensions and materials ......................................................................24
8.2 Standard equipment ...................................................................... 25
8.2.1 832 KF Thermoprep................................................................................25
8.3 Optional accessories..................................................................... 27
8.3.1 Sample vials............................................................................................27
8.4 Warranty and conformity............................................................... 28
8.4.1 Warranty ..................................................................................................28
8.4.2 EU Declaration of Conformity for 832 KF Thermoprep ..........................29
8.4.3 Declaration of Conformity .......................................................................30
Index 31
List of illustrations
Fig. 1 Front view ................................................................................................................... 3
Fig. 2 Rear view .................................................................................................................... 4
Fig. 3 Temperature controller ...............................................................................................5
Fig. 4 Sample holder .......................................................................................................... 5
Fig. 5: 832 KF Thermoprep – peripheral devices .................................................................. 7
Fig. 6 Fuse holder.................................................................................................................9
Fig. 7 Needle assembly...................................................................................................... 10
Fig. 8 Guide head with needles.......................................................................................... 10
Fig. 9 Coulometer cell......................................................................................................... 12
Fig. 10 Volumetric KF cell ..................................................................................................... 12
Fig. 11 Crimping pliers..........................................................................................................13
Fig. 12 Loosening the guide head........................................................................................ 13
Fig. 13 Needle in lowered position .......................................................................................14

1.1 Description of the instrument
832 KF Thermoprep, Introduction 1
1 Introduction
Thanks to its reliability and simple handling, the Metrohm 832 KF Ther-
moprep is a very versatile instrument. It has been designed for use in
production and laboratories and covers a wide range of applications.
The 832 KF Thermoprep can be used wherever it is necessary to heat
up a solid or liquid sample and/or to drive off water by the application of
heat.
When combined with a coulometric or volumetric KF titrator, the 832 KF
Thermoprep forms the ideal analytical system for determining the water
content of samples which contain interfering components or which only
release their moisture slowly.
Among the decisive advantages of the KF Thermoprep is the reduction
of sample preparation to a minimum. By using hermetically sealed
sample vessels (headspace vials) the samples can be filled directly on
site. The PTFE-coated septa guarantee a constant and true water con-
tent, even when the sample have been allowed to stand for a long time.
1.1 Description of the instrument
The 832 KF Thermoprep has been designed primarily for the determina-
tion of moisture by the oven method. The samples are heated in the
oven block and release their moisture in the form of water vapor; this is
transferred to a measuring cell by a carrier gas. The carrier gas stream
is produced by a built-in air pump. An inlet valve is also provided for the
use of nitrogen or other inert gases. The determination of moisture in
the measuring cell can be carried out either coulometrically or volumet-
rically according to the Karl Fischer method.
The 832 KF Thermoprep is characterized by its compact construction;
the oven heating block, air pump, temperature controller, flowmeter and
flow controller as well as the drying bottles are already built in.

1.2 Information about these Instructions for Use
2832 KF Thermoprep, Introduction
1.2 Information about these Instructions for Use
Please read through these Instructions for Use before you start to use
the 832 KF Thermoprep.
The following notations and pictograms are used in these instructions:
35
Operating element
The operating elements are explained on
pages 3ff.
Danger
This symbol indicates a possible risk of
death or injury to the user and possible
damage to the instrument or its compo-
nents by electricity.
Danger/Warning
This symbol indicates a possible risk of
death or injury to the user and possible
damage to the instrument or its compo-
nents.
Attention
This symbol indicates important informa-
tion. Read the information provided before
you continue.

1.3 Parts and controls
832 KF Thermoprep, Introduction 3
1.3 Parts and controls
1.3.1 Individual parts and standard accessories
Fig. 1 Front view
1 Guide head 10
Temperature controller
2 Transfer tubing 6.1805.460 11
Clamping lever
3 Spacer 4.832.4190 12
Guide rod
4 Penetration and outlet needle
6.2816.070 and 6.2816.080
13
Inlet tubing 6.1805.020
5 Dosing tip 6.1543.060 14
Air/Nitrogen outlet
6 Septum stopper 6.2730.050 15
Drying bottles 6.1608.050
With 6.1602.140 inset, filled with
6.2811.000 molecular sieve
7 Sample holder 16
Bottle holder
8 Pump switch 17
Flow indicator
9 Temperature selection switch 18
Flow controller
11
1
3
2
4
5
67
12
13
8
10
917
18
16
15
14

1.3 Parts and controls
4832 KF Thermoprep, Introduction
1.3.2 Rear view
Vorsicht: Heis se Gehäuseteile
(übe r 60 °C)
Attention: H ot parts
(ab ove 60 °C)
Cuidado: Partes calientes
(mas de 60°C)
Attention: Par ties chaudes
(plu s de 60 °C)
100 - 120 V: 4 A (T)
220 - 240 V: 2 A (T)
f = 50/60 Hz
S = 35 0 VA
WARNING - Fi re Hazard -
for conti nued pro tection repl ace only
with t he same type an d rat ing o f fuse
Inlet fi lte r
Key lock
On
Off
Type 1.832.0010 Nr.
0010/01104
Made by Metrohm Switze rland
Fig. 2 Rear view
19 Tubing guide 25
Transfer tubing connection
20 Ventilation slots 26
Guide spring
21 Mains switch 27
Needle base
22 Mains connection 28
Hot air outlet
23 Fuse holder 29
Key lock switch
24 Adjustment nuts 30
Air/nitrogen outlet
Connection for dust filter (6.2724.010)
19
24
25
26
27
20
21
22
23 30
28
29

1.3 Parts and controls
832 KF Thermoprep, Introduction 5
1.3.3 Temperature controller
Fig. 3 Temperature controller
31
Actual value display
red, 4-place
35
Output status display
yellow, for outputs 1 to 3
(K1 and K3: oven heating, K2: fan)
32
Set value display
green, 4-place
36
LED for ramp/program function
green, lights if configured
33
Program key
for selecting the parameters
37
EXIT key
to exit the dialog levels
34 Decrement key
for changing values
38
Increment key
for changing values
1.3.4 Sample holder for standard vials
Fig. 4 Sample holder
The dimensions of the 6.2063.000 sample holder are optimized for the
Metrohm 6.2419.007 standard sample vials (6 mL). This ensures the
highest possible heat flow from the oven to the sample.
If other sample containers with different dimensions shall be used
custom made sample holders can be delivered. For this the precise
dimensions (incl. dimensional tolerances) must be known.
The measures of non-standard sample containers must vary within the
following dimensional limits:
Diameter 10.0 … 32.0 mm
Depth of immersion 20.0 … 45.0 mm
31
32 35
36
33 37
34 38

2.1 General
6832 KF Thermoprep, Safety information
2 Safety information
Warning!
This instrument should only be used in accordance with the information
given in these Instructions for Use.
2.1 General
This instrument left our works in perfect condition from the point of view
of its operational safety (see Technical data, safety specification). To
keep it in this condition and to continue to operate safely the following
information must be carefully observed.
2.2 Electrical safety
Please observe the following guidelines:
• Only qualified Metrohm personnel should carry out service work on
electronic components.
• Do not open the instrument housing as this could damage the in-
strument. The housing contains no components which could be
serviced or exchanged by the user.
Electrical safety when handling the instrument is guaranteed within the
scope of Standard IEC 61010. However, please observe the following
point:
Protection against electrostatic charges
Warning!
Electronic components are sensitive to electrostatic charges and can
be destroyed by a discharge. Always remove the mains connection
cable from socket 12 before making or breaking electrical connections
on the rear panel of the instrument.
Connection to the electricity supply:
This instrument must only be operated at the specified mains voltage.
Repair and maintenance:
If faults or malfunctions occur while using the 832 KF Thermoprep we
recommended that you first check that the connection to the control in-
strument has been made correctly.
The instrument must not be opened. This is reserved exclusively for
authorized service personnel.

2.2 Electrical safety
832 KF Thermoprep, Installation 7
3 Installation
This section describes the things you should pay attention to when un-
packing and starting up the 832 KF Thermoprep. It also tells you how a
complete automation system is built up.
The following illustration provides an overview of the peripheral devices
which can be used with an 832 KF Thermoprep:
Titr iermitte lTitr iermitte l
KFD 758
Titr iermitte lTitr iermitte l
KFD 758
Titriermittel
KFP 785
Titriermittel
KFP 785
756 KF756 KF
832 TP832 TP
COM 1
COM 2
LPT 1
PC
USB
COM 1
COM 2
LPT 1
PC
USB
831 KF831 KF
KFP 795KFP 795
RS232
832 Thermoprep
RS232
KF Titrino
795 / 787 / 758
KF Coulometer
831 / 756
PC Software
Tinet 2.x / VESUV 3.0
835
Titrando
KF
835
Titrando
835
Titrando
KFKF
800
Dosino
Titriermittel
800
Dosino
KF
836
Titrando
800
Dosino
Titriermittel
800
Dosino
KF
800
Dosino
Titriermittel
800
Dosino
Titriermittel
800
Dosino
KF
800
Dosino
KF
836
Titrando
836
Titrando
Titrandos
USB
PC Control tiamo
Touch ControlTouch Control
Fig. 5: 832 KF Thermoprep – peripheral devices

3.1 Instrument setup
8832 KF Thermoprep, Installation
3.1 Instrument setup
3.1.1 Packaging
The 832 KF Thermoprep and its specially packed accessories are sup-
plied in very protective special packaging. Please store this packaging
in a safe place; it is the only way in which the safe transport of the in-
strument can be guaranteed.
3.1.2 Checks
Please check that the delivery is complete and undamaged immedi-
ately on receipt (compare with delivery note and list of accessories
given in Section 8.28.2). If transport damage is evident please refer to
the information given in Section 8.4.1 “Warranty”.
3.1.3 Location
The 832 KF Thermoprep has been developed for use indoors and must
not be used in explosion-endangered surroundings.
Place the instrument on a suitable vibration-free laboratory bench, pro-
tected as much as possible from corrosive atmospheres and contami-
nation by chemicals.
Select a location in which the ambient temperature is normally between
+5 °C and +45 °C. The instrument should be protected against exces-
sive variations in temperature and direct sunshine.
If an instrument which has been stored under cold conditions is
brought into a warm room then the atmospheric humidity may con-
dense inside the instrument and form water. In order to avoid damaging
the instrument please wait for at least one hour before switching it on.
3.2 Mains connection
Please observe the following rules when connecting the instrument to
the electricity supply. If the instrument is operated with an incorrectly set
mains voltage and/or an incorrect mains fuse then it represents a fire
hazard!
Setting the mains voltage
Before you switch on the 832 KF Thermoprep for the first time please
check that the mains voltage set on the instrument (see illustration on
the following page) corresponds to your local mains voltage. If this is
not the case then you must alter the mains voltage as follows:

3.2 Mains connection
832 KF Thermoprep, Installation 9
• Pull out mains cable
Remove the mains cable from the mains supply connection of the 832
KF Thermoprep.
• Remove the fuse holder
Use a screwdriver to loosen the fuse holder beside the mains supply
connection and remove it completely.
• Check the fuse and replace it
Carefully remove the built-in fuse for the intended voltage from the fuse
holder and check its specifications (the position of the fuse in the fuse
holder is indicated by the white arrow beside the voltage range):
100…120 V 4 A (slow blow) Metrohm-No. U.600.0022
220…240 V 2 A (slow blow) Metrohm No. U.600.0019
• Insert fuse
Exchange the fuse if necessary and replace it in the fuse holder.
• Insert fuse holder
Depending on the required mains voltage, insert the fuse holder so that
the white arrow of the corresponding voltage range points to the white
bar; this is to the right of the fuse holder (see below).
220 – 240 V 100 – 120 V
220 -240 V
100 -120 V
220 -240 V
100 -120 V
Fig. 6 Fuse holder
Mains switch
Mains connection
Fuse holder

3.3 Assembling the 832 KF Thermoprep
10 832 KF Thermoprep, Installation
3.3 Assembling the 832 KF Thermoprep
3.3.1 Assembling the needles
Fig. 7
Needle assembly
• Screw spacer 3(4.832.4190, L=58 mm) into distributor 39. For special
requirements, e.g. different sample vials, custom-made spacers can
be supplied, see p. 27.
• Place PTFE distance ring 41 (supplied with the needle) on penetration
needle 42 (6.2816.070) and insert this into distributor 39 from above
(see left). Pull penetration needle 42 down as far as it will go.
• Slide hollow outlet needle 43 over penetration needle 42 from below
and fasten it to Luer-lock connector of the spacer 3.
• Connect inlet tubing 13 (6.1805.020, 52 cm) to distributor 39 from
above and fasten it. This fixes penetration needle 42 in the proper
position.
Fig. 8 Guide head with needles
To prevent possible injury the height of needle base 27, which protects
the tip of penetration needle 42, can be adjusted. Screw adjustment
nuts 44 of guide rod 12 until the needle tip is flush with the lower side of
needle base 27.
3
39
43
42
13
44
12
27
41

3.3 Assembling the 832 KF Thermoprep
832 KF Thermoprep, Installation 11
3.3.2 Attaching the drying bottles
1. Fill 6.1608.050 drying bottles 15 with 6.2811.000 molecular sieve
and place 6.1821.040 outlet tube (with 6.2821.090 filter) in
6.1602.140 screw cap. Screw the screw caps onto the drying bottles.
When attaching the tubing please
observe the following:
To filter the carrier gas before leaving
the drying bottle, it must be led
through the outlet tube to the outlet
connection.
2. Place drying bottles 15 in holder 16 of the
oven. Screw the 6.1805.180 Tubing (16 cm) to
the inlet tubing connection of the front drying
bottle. The carrier gas must enter the drying
bottle at the top of the bottle. Connect the other
end of the tubing to the air/nitrogen outlet 14
(see drawing).
3. The rear drying bottle is connected to the front
bottle using 6.1805.010 Tubing (13 cm). Screw
the tubing onto the outlet tube of the front bottle
and connect the other end to the inlet connec-
tion of the rear drying bottle. The carrier gas
must enter the rear drying bottle at the top of
the bottle.
4. Screw 6.1805.020 Tubing (52 cm) onto the
outlet tube of the rear drying bottle and lead it
through the tubing guide on the guide head of
the 832 KF Thermoprep. The free end of the
tubing is screwed onto the connection provided
for it on the guide head.
5. 6.1805.460 Transfer tubing (27 cm) is screwed onto the back of the
distributor piece. Attach 6.1543.060 Dosing tip to the other end of
the tubing and insert it into the titration vessel.
3.3.3 Attaching the dust filter
Attach 6.2724.010 Dust filter to the 'Inlet filter' connection on the rear
panel of the instrument.
If nitrogen is to be used as the carrier gas then the nitrogen inlet tubing
can be attached directly to the dust filter tubing nozzle.
14
16
15

3.4 Assembling the coulometric cell
12 832 KF Thermoprep, Installation
3.4 Assembling the coulometric cell
Fig. 9 Coulometer cell
The coulometer cell is setup for the gas inlet as
follows:
6.1543.060 Tip is screwed into the 6.1446.060 Stopper
by using the screw nipple (screw nipple of 6.2730.030
with O-ring) and the stopper is inserted into the SGJ
14/15 opening.
If simultaneous aspiration is necessary while gas is
being led in then the gas inlet tubing must be inserted
into the side inlet. This requires the use of the following
parts:
Tip 6.1543.060
Screw cap 6.2701.040
Sealing ring A.254.0104
A titration vessel with 2 side-mounted inlets is also
available: order number 6.1465.320.
3.5 Assembling the titration vessel for volumetric
KF titrators
Fig. 10 Volumetric KF cell
The titration vessel is adapted for the gas inlet in the
following way:
Instead of the 6.2730.020 Septum stopper, the
6.2730.050 Stopper is used with 6.1543.060 Tip. (Nipple
and O-ring of 6.2730.030 from the Titrino accessories.)
Generator electrode
with drying tube
Indicator electrode
6.1543.060 Tip
Screw nipple of
6.2730.030
6.1446.060 Stopper

4.1 Inserting and removing sample vials
832 KF Thermoprep, Operation 13
4 Operation
This section describes the basic principles of handling the 832 KF Ther-
moprep.
4.1 Inserting and removing sample vials
As the oven of the 832 KF Thermoprep can reach a temperature of
250 °C, vials must only be inserted in or removed from the oven by us-
ing crimping pliers or other tools. Hot vials should only be placed on
temperature-resistant surfaces.
Fig. 11 Crimping pliers
4.2 Needle penetration
Always lower guide head 1by using both hands. In this way you can
avoid injuring yourself on the needle.
Fig. 12 Loosening the guide head
Clamping lever
11

4.3 The pump
14 832 KF Thermoprep, Operation
Loosen the red clamping lever by pressing it strongly and lower the
guide head and needle by using both hands. Penetrate the vial septum
with the needle and lower the guide head until it reaches the bottom
stop.
Fig. 13 Needle in lowered position
4.3 The pump
The 832 KF Thermoprep is equipped with a powerful air pump, with
which the released humidity of the sample can be transferred to a titra-
tion cell in a constant carrier gas stream.
Atach a 6.2724.010 dust filter to the air inlet 30 on the instrument's rear
side. Avoid the intrusion of dust particles.
The dust filter must be replaced in a regular equipment service.
If thermal unstable samples, which may decompose at higher tempera-
tures are treated, the use of nitrogen as carrier gas is highly recom-
mended. Connect the nitrogen supply pipe to the hose olive of the dust
filter. The maximum pressure of the nitrogen supply must not exceed
1 bar.

4.4 The temperature controller
832 KF Thermoprep, Operation 15
4.4 The temperature controller
The best proven dTron 16.1 (JUMO) temperature controller of the 832
KF Thermoprep is very easy to use for routine operation of the instru-
ment. Fine adjustment of the control parameters is possible but not
normally necessary. Unappropriate parameters of configuration settings
may cause faults of the instrument. The default settings can be used
without any problems. The temperature controller 10 also has a com-
fortable and simple self-optimization function which can be used if nec-
essary.
4.4.1 Two set temperatures
The temperature controller of the 832 KF Thermo-
prep can store two set temperatures (T1 and T2).
You can switch between these two set tempera-
tures by using the temperature selection switch.
Temperature display
The display indicates the real value and the set
value (T1 or T2).
The oven starts to heat up as soon as the instrument is switched on
and is controlled at the set temperature (T1 or T2). If a switch is made
from one set temperature to the other one then this will be adopted im-
mediately by the temperature controller, i.e. the oven will immediately
heat up or cool down until the set temperature has been reached.
4.4.2 Setting a temperature
The desired temperature (T1 or T2) is easily set by using the two arrow
keys (increment key 38) and (decrement key 34) of the tempera-
ture controller. The set temperature can be altered at any time, regard-
less of whether the set temperature has been reached or not.
Please observe the green set value display 32. This always refers to the
set temperature T1 or T2 which has been selected. Longer pressure on
an arrow key changes the set value more quickly.
Altered set values are immediately accepted by the temperature con-
troller.
If the key lock function (tumbler switch 29 on the rear panel of the hous-
ing) is switched on then no settings can be made.

4.4 The temperature controller
16 832 KF Thermoprep, Operation
4.4.3 Self-optimization of the control parameters
Self-optimization should only be used when the set temperature cannot
be achieved by the temperature controller or when the actual tempera-
ture varies about the set temperature by more than 2…5 °C (overshoot-
ing).
Preparation
Set the same conditions as would be used in a real determination.
• Set the temperature (T1 or T2) to a value corresponding to a real
determination (e.g. 120 °C).
• Wait until the oven has reached the set temperature.
• Insert a sealed sample vial containing a sample in the oven.
• Lower the work head and completely penetrate the sample vial sep-
tum with the needle.
• Switch on the pump (or open the nitrogen valve) and set the gas
flow to a realistic value which would be used during a proper de-
termination.
Self-optimization
• Start the self-optimization process with EXIT (keep key 37 pressed
down for at least 2s!).
During the self-optimization process "tunE" blinks in the display 31.
When the blinking stops the process is finished. Self-optimization nor-
mally takes 1 to 5 minutes. The duration depends on the selected tem-
perature, i.e. the higher the temperature the shorter it takes.
•
• Save the control parameters which have been determined by press-
ing the EXIT key 37 for 2 seconds.
The self-optimization process can be canceled by pressing the EXIT
key 37 briefly.
4.4.4 Key lock function
The temperature controller settings can be protected against accidental
alteration. On the rear panel of the 832 KF Thermoprep the 'Key Lock'
tumbler switch 29 can be switched to 'On'.
If the key lock function is switched on the 'Temperature' tumbler switch
9can still be used to select the two set temperatures T1 and T2. It is
also possible to switch the pump on and off (key 8).
However, no alteration can be made to the temperature controller 10
with the key lock function switched on.