Soxtherm 2000 User manual
CONTENTS
Page 1. 1.1. 1.2. 1.3. 1.4. 1.5.
General remarks Conditions of warranty Damage during transport Safety instructions Technical data Accompanying parts
17 17 17 17 17 17
2. 2.1. 2.2. 2.3. 2.4.
Operating and function elements Front view Rear view FronUrear view SOXTHERM-VARIOSTAT controller Key
17 5 6 7 18
3. 3.1. 3.2. 3.3. 3.4.
Assembly General Assembly of the extraction unit Connection to the controller Air pressure connection
19 19 19 19 19
4. 4.1. 4.2. 4.3. 4.4.
Installation General Input of date and time Selecting the display language Keyboard
20 20 20 20 21
5. 5.1. 5.2. 5.3. 5.4.
Performance Principle of operation Setting up a program Carrying out an extraction Starting the program
22 22 22 23 24
6.
Error messages
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7.
Spare parts
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Instruction manual no. E 34191
07.01.2000
1. General remarks 1.1. Conditions of warranty On the basis of our conditions of warranty Gerhardt products are guaranteed for one year. That means that the apparatus must be used in accordance with the following instructions and that the instrument is neither over or improperly used. Glass parts are excluded from warranty.
1.2. Damage during transport Please be careful when unpacking the goods and make a note of any damage! The carrier (post, rail, road) should be notified immediately and an expert's report obtained!
1.3. Safety instructions The instructions for "working with inflammable liquids" have to be observed. Before opening the apparatus, please disconnect the mains plug. 1.4. Technical data SOXTHERM extraction unit Width: Depth: Height: Weight: Type S 306 A: Weight: Typ S 306 AK: Cooling water consumption: Cooling water pressure: Power consumption:
500 mm 290 mm 650 mm 48 kg 70 kg 150 1/h > 1,5 bar 230 v /1100 240 v /1200
SOXTHERM VARIOSTAT Controller Width: 300 mm Depth: 315 mm 160 mm Height: 3,2 kg Weight:
w w
1.5. Accompanying parts 830610 830611 S 306 AK S 306A
Order no. 8213 8211 8120 8300 8310 8323 8330 8350 16100 18310
SOXTHERM extraction system, automatic SOXTHERM-VARIOSTAT controller SE-VA Compressor, 5 m tubing incl. Extraction beaker, glass, 54 x 130 mm Extraction thimbles, 33 x 80 mm (25 pc) Holder for extraction thimbles, 33 mm Insert rack for 6 extraction beakers Tongs for extraction beakers Line filter 16 A Boiling stones, 250 gr
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1 12
1 6 1 1
12 1
6 1 1
1 1
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2. Bedienungs- und Funktionselemente/ Operating and function elements 2.1. Vorderansicht I Front view
2.2. Riickansicht I Rear view
I
'10-{[
6
2
2.3.
Vorder-/Ri.ickansicht SOXTHERM·VARIOSTAT Steuergerat FronUrear view SOXTHERM-VARIOSTAT controller
32
35--e-E)
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30
~--36 Q).
..... ~--37 41
39
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2. Operating and function elements 2.1. Front view see page 5 - 2.2. Rear view see page 6 2.3. FronUrear view SOXTHERM-VARIOSTAT controller see page 7 2.4. Key
2 3 4 5 6 7 8 9 10 11 12 13 14
15 16 17 '19 20 21 22 23 24
25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41
Solvent discharge tap, consisting of: Screw-in elbow Screw-in hose tip Seal made of aluminium Ball valve, small Extraction beaker, glass, 54 x 130 mm Extraction thimble, 33 x 80 mm Holder for extraction beaker Pneumatic control switch, solvent recovery Cylinder casing with pressed in PTFE cylinder, with groove Extraction condenser, glass Clamping cylinder SZD-25/20, white Compressed air supply PTFE Pneumatic control switch, lift/lower beaker Water flow control, Liquimobil Level indicator (Inspection glass, solvent tanl<) Cover plate Hot plate, consisting of: Tubular heating element, 230V/11 DOW, 240V/1200W Aluminium plate Wobble plate, aluminium Guiding sheet metal Form tube, PTFE Distributing restrictor Ms, 90x20 Restrictor completely mounted Solvent recovery tank Cooling water outlet Cooling water inlet Resistance thermometer GF (double Pt 100) Air pressure connection (A) for compressed air piping, 6-place (11029) Cable with plug, 5-pin, 5 m, for PI 100 control system with cable guide (z-binder, 8,5 mm, with nut) Connection line heating (Cable with pin and socket connector, 5 m) Connection box, explosion-proof Display l
11079 11080 11087 11091 8300 8310 included in pas. 6 11059 40461 8129 11057 40479 11059 27401 30739 40414 12368 40402 30740 40409 40468 40460 11060 40493 30751 30750 15361 11030 11178 18708 21429 40271 11173 11750
11176
17101 21422 18703 11183 11082 11030
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3. Assembly 3.1. General The Soxtherm extraction unit must only be operated in rooms that fulfill the local regulations for working with solvents and dangerous substances. The control unit and the compressor are not explosion-proof and must therefore be installed outside the room where the extraction takes place. The cutting-through of walls for link circuits have to be sealed.
3.2. Assembly of the extraction unit The installation area for the extraction unit must be horizontal otherwise the phase for the solvent recovery is restricted. The water inlet tubing (5 m) has to be connected to the cooling water inlet (pas. 21) and the Variostat water outlet (pos.41 ). The outlet tube (pas. 20) must be placed into drain so that the water can flow away freely. Connect the corrugated hose to the air pressure connection (11029) (pas. 23) and secure with the swivel nut.
3.3. Connection to the controller The cables from the extraction unit (pas. 24, 25) or tubes (pas. 21, 23) to the control unit have to be connected to the correct sockets (pas. 36, 38, 40, 41). The diode plug of the double Pt 100 is secured by a coupling ring. The 3-pole heating connection plug is automatically locked, in case it has to be dismounted, carefully lever up the locking lug via a screw driver and pull the plug at the same time. Connect the cooling water tubing (2 m) to the cooling water inlet (pas. 35) and the tap. Connect the connection cable (pas. 37) of the control unit with a shockproof socket.
3.4. Air pressure connection Type S 306 AK No. 830610 Ace. to the enclosed instruction manual of the compressor, please change the sealing cap for the admission filter. The pressure reducer is adjusted to 5 bar at the factory. The air pressure tube should be shortened if necessary and the opposite end of the coupling be fastened with screws and connected with the coupling (pas. 39). Switch on the compressor. If the manometer of the air pressure restrictor shows "0", the black blocking tap for the air must be opened. Maintenance information can be found in the instruction manual. Type S 306 A No. 830611 If the system is connected to an existing compressed air piping a pressure control reducer has to be inserted and adjusted to 5 bar. To the coupling of the SOXTHERM-VARIOSTAT control systemair pressure tubing 4 x 6 can be connected.
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4. Installation 4.1. General The SOXTHERM-VARIOSTAT control system continually monitors air and cooling water pressure. Therefore check that the cooling water inlet is open, the compressor is switched on and the stop valve is opened before the control system is switched on.
4.2. Input of date and time The following procedure is performed: 1. Keep button "1" pressed
2. Switch on mains switch (pas. 29) 3. Let go button "1" after about 2 seconds The display shows a random date and time. In order to change this the figures have to be overwritten. Each unit (day, month etc.) has to be confirmed by pressing the ENT-key. The cursor highlights the position which can be overwritten. Altering the time and date is confirmed by pressing the ENT-key until the curser reaches the time which can then be entered. After entering the time the apparatus is in the stand-by position. Date and time are continuous, independent of the apparatus being switched on or off.
4.3. Selecting the display language
4 languages are available. To select the language required perform the following procedure:
1. Keep button "2" pressed 2. Switch on mains switch (pas. 29) 3. Let go button "2" after about 2 seconds The following can now be seen on the display: 1 =D, 2 =GB, 3 = F, 4::: NL 1 =German, 2 = English, 3 = French, 4 = Dutch By pressing the relevant button the required language is selected. The apparatus is now in stand-by position.
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4.4. Keyboard The keyboard is devided into 3 areas: 1. 2. 3.
Manual control of heating/cooling water Input keys Program correction keys
1. Manual control of heating/cooling water When the apparatus is switched on it automatically goes into AUTO-mode and the relevant LED is illuminated. If the program is started in this position, the time of the first step (boiling phase) only starts running when the temperature of the hot plate is 5° C below the programmed desired value. On automatic the program begins with a heating-up phase. If the AUTO-mode is switched off (LED is extinguished), the entered time of the boiling phase counts down independently of the hot plate temperature. The AUTO-button can only be operated in the stand-by position. As soon as a program is started the water valve is opened and the cooling water runs. In case it seems advisable to let the cooling water flow when no program is running, the valve can be switched on manually via the ON/OFF switch (pos. 34) and the corresponding LED then lights up. Switching off the cooling water during the running program is not possible.
2. Input keys Via the numbers on the keyboard (pos. 28) the data of the various program steps are entered and memorized by pressing the ENT-key. In order to look into a stored program it can be run through by pressing the ENT-key (confirmation of all data). In case it is needed to run backwards through the programming or a previous input has to be modified, the C-key has to be pressed until the desired program step is reached. The RES-key interrupts the running program and resets the system to stand-by position. Each pressing of a key is accompanied by an acoustic signal. If keys are pressed which are not applicable for a certain program step, a double acoustic signal can be heard. Pressing the dot key shows the nominal values during RUN-mode.
3. Program correction keys Depending on the sample to be extracted, the size of the extraction thimble, the solvent, the filling level and the hot plate temperature certain times must be entered for various steps. The individual length of time cannot be fixed right from the beginning as it depends on practical experience. The two keys with arrow allow intervention into the running program. By pressing the upper key once the respective step is extended by one minute, by pressing the lower key the time is reduced. During programming the standards for interval and impulse may be changed by using the arrow-keys.
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5. Performance 5.1. Principle of operation Boiling phase Solvent reduction A Extraction Solvent reduction B Solvent reduction C
range range range range range
0-99 hrs. 59 min. 0-9 intervals 0-99 hrs. 59 min. 0-30 min. 0-59 min.
During the boiling phase the sample is placed in boiling solvent which brings a large part of the extract into solution. For a complete extraction the solvent level must be reduced to a point where the separation between solvent and extraction thimble is clear (Reduction A). The evaporated solvent is cooled in the condenser and drops back into the PTFE-middle part, where 15 ml are collected before they are brought together with the sample. For the reduction compressed air is led through the condenser, which presses the solvent into the built-in collecting vessel. The time (interval) in which the solvent is recollected and the duration of the addition of compressed air (impulse) may be variably programmed (2-8 min. e.g. 1-6 sec.). After the extraction is finished the solvent is evaporated during reduction phase B, but not up to drying, to avoid a change of the extract. Reduction phase B is programmed in minutes, this makes it possible to enter the last impulse apart from the programmed interval. For example: Reduction B 11 minutes, interval 3 minutes. Every 3 minutes an impulse for reduction is given. The last impulse takes place after the reduction phase (after 2 minutes), what allows the evaporation on a volume, although the reduction on principle occurs in steps of 15ml. During reduction phase C the extraction beakers are raised away from the heating plates. Heating and cooling water are still turned on. The evaporation is minimal. The extract in not endangered, as the extraction beakers are based only in the hot air current.
5.2. Setting up a program After switching the system on the display shows the following: Date* Time Actual temperature * R = 1 * P = 2 By pressing key "2" the unit gets into the program mode. Enter the number of the program (0-99) and confirm with enter. The initializing of the security temperature of 200°C or 300°C depends on the extraction temperature, which again depends on the solvent used. The entered security temperature in connection with the position of the key-operated switch (pas. 33) only indicates a maximal value. If this value is exceeded, the heating turns off, the LED-alarm lights up and an acoustic signal is heard.
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It must be insured that when entering the extraction temperature the temperature of the heating plate must be clearly higher than the boiling temperature of the inserted solvent. The maximal temperature entered must be 5oc below the initialized security temperature (i.e. 195oc e.g. 295°C). The desired times for the following program steps of the solvent are depending on the type of sample.
Solvent e.g. Toluene n-hexane Methanol Ethanol Acetone 11 Chloroform Dichloromethane 21 Petroleumether
Extraction temperatureoc 110,6 68,9 65,0 78,5 56,2 61,7 40,0 40-60
280 180 290 290 180 190 150 150
1) Soxtherm Is equipped with Vi ton 0-rings, suitable for the usage with petroleum benzine or hexane. When working with other solvents or solvent mixtures we recommend the usage of silicone or para flour O~rings {see attached table of chemical resistance).
For the fat determination with 140 ml petroleum ether the following times have to be entered: Boiling time: Solvent reduction Extraction time: Solvent reduction Solvent reduction Solvent reduction Solvent reduction
30 minutes 5 x 15 ml 80 minutes 8 minutes 5 minutes 3 minutes* 3 seconds
A: B: C: interval: phase:
* In case of irregularities during the solvent reduction interval, which cannot be put down to the sample ( i.e. different sample portions ), this time has to be increased. When the last time step has been entered the display shows: "Program xx" finished. By pressing the ENT-key you return to stand-by position. Now either different programs can be entered or stored programs can be started.
5.3. Carrying out an extraction The extraction beakers (pas. 2) are filled with a few boiling stones and are then dried at 103° C in a drying oven. We recommend the boiling stones of JJP, type A, which are especially for vacuum distillation. Afterwards the beakers are cooled down to room temperature in a desiccator and then weighed to exactly 1 mg on an analytical balance. Make note of the weight as it is needed for the calculation. About 5 g of homogenized sample is weighed to exactly 1 mg into the extraction thimble and covered with fat-free wadding. Sample preparation like drying if necessary should be carried out as required. Push the extraction thimble holder from below over the extraction thimble so that it is level with the upper end of the thimble. Insert the extraction thimble into the extraction beaker and add approximately 140 ml of the solvent.
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The extraction timble is inserted into the extraction beaker and constantly filled with solvent. Depress the tong for the extraction beaker (pos. 4.), insert the beaker and let loose the tong. When the unit is loaded, push all beakers against the rear limit stop of the hot plate (pos. 14) in order to achieve correct positioning.
5.4. Starting the program Before the program can be started the safety temperature (200 or 300° C respectively), preset in the program, has to be adjusted via the key-operated switch (pos. 33). After having pressed key "1" the number of the desired program is entered. For the manual start this is done by pressing the ENT-key. The system takes the confirmation of the first digit as confirmation of date and time. Actual time and starting time are identical and the program runs.Date and time have to be entered for the timer-start. It is important that the first digit of the date is overwritten even if the starting date is not changed as otherwise the unit will be started manually (see above). The display now shows at the top the actual date and time and below the entered starting date and time. When they are identical, the program runs. After the termination of the program the beakers are dried at 103° C for at least 1 hour in the drying oven. Then the extraction beakers are placed into the desiccator, cooled down to room temperature and weighed to exactly 1 mg. The drying, cooling down and weighing is repeated half hourly until two successive weighings do not differ for more than 0,1 %from the weighed in material. In case the weight increases, the lower value of the weighing before must be kept. Extraction, drying and weighing have to succeed each other immediately.
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6. Error messages The following errors can be recognized and shown on the display:
*PI 100 Error
*
is shown if the Pt 100 is not connected or broken. If this error appears during the RUN-mode the program is interrupted.
Excess temperature I=XXX*C S=XXX*C
is shown if the actual temperature is more than 1 oo C higher than the programmed temperature.
Program undefined
is shown if all time steps of the entered program are zero.
Program interrupted
is shown if during the RUN-mode the beakers are raised away from the hot plate.
Right switch wrong position
is shown if at the beginning of the program start the pneumatic control switch for extraction beakers is in wrong position.
Key position
is shown if a) there is no key in the lock b) the key is in stop-position c) the programmed temperature and the limit temperature are not identical.
No water-air pressure
is shown if there is no water or air pressure or neither of the two.
XX PROGRAM FAULTY
if in an already written program only the safety temperature is changed and the program mode is then left via RES or the C-key, a consistency check of the safety temperature and the extraction temperature is carried out when the program is re-started. If these don't coincide, there will be an error message.
STOP PROG NO XX RUN=ENT ELSE·C
if the program in progress is interrupted by an error, i.e. no cooling water, the display shows the according fault for as long as it is not rectified. Afterwards the program can be restarted with the ENT-key at the position where it was interrupted or stopped with the C-key.
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7. Spare parts BASIC MODELS 11029 1'1057 11060 11067 40460 11178 12368 12708 12403 12405 15361 16601 16609 18708 21429 27401 30739 30740 40461 27301
11079 11080 11087 11091
Compressed air piping, 6-place Clamping cylinder SZD-25/20, white Restrictor, completely mounted 5/2-way valve L 25510 Airtex Distribunting restrictor Ms, 90x20 Cable with plug, 5-pin, 5 m Tubular heating element, 230V/1100W, 240V/1200W Plug w. bayonne! catch, 5-pin Rubber foot, 30x17 mm Rubber foot, 20x10 mm Resistance thermometer GF (double Pt 100) Screw cap GL 14 Tubing connection, straight with silicone seal GL 14 Z-binder, 8,5 mm, with nut Cable with pin and socket connector, 3 pin, 5 m Water fiow control, Liquimobil Inspection glass, solvent tank Wobble plate, aluminium Cylinder casing with pressed in PTFE cylinder, with groove 0-ring Viton, 75 shore, standard, built in 40461 for the following solvents: toluene, n-hexane, methanol, ethenol, dichloromethane and petroleum ether 0-ring paraflour, on request, built in 40461 especially for residue analytics and solvent mixtures, univeral usages 0-ring silicone, on request, built in 40461 especially for acetone Extraction condenser, glass Extraction beaker, glass, 54x130 mm Holder for extraction thimble 33mm Insert rack for 6 extraction beakers 8300 Solvent discharge tap - single parts: Screw-in elbow Screw-in hose tip Seal made of aluminium Ball valve, small
11061 11062 11063 11148 11149 11150 11152 11157 11167 11173 11175 11176 11187 11182 11183 11750 15350 15351 17101 18401 18703 18792 21422
Magnetic valve, 2/3-way, 230/240 V Magnetic valve, 5/2-way, 230/240 V Pneumatic-electrical transformer OVT-a-PCB for Soxtherm, 230 V OVT-a-PCB for Soxtherm, 240 V Variostat power PCB, 230 V Vapodest/Variostat display PCB Variostat power PCB, 240 V Flat cable, 250 mm, 10/10 pin Keyboard Variostat Flat cable, 160 mm, 20/20 pin Key-operated switch with cable for Soxtherm control Eprom all languages Soxt11erm Flat cable, 270 mm, 6/6 pin Flat cable Mains switch, green, 230 V Semiconductor relay WG-A5-6D25 Protective cap for 15350 Magnetic valve with pressure control, cooling water inlet Rubber foot 15-023 Mains cable, 2m, wall plug, 3x1 ,5 mm2 Z-binder, 10,5 mm Socket with catch, 3 pin
27311 27312 8129 8300 8323 8330
CONTROL SYSTEM SE-VA 8211
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