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TECATOR Soxtec System, Manual

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TECATOR Soxtec System Manual Download Page 25

J

1980.01.15 RA/ML

AN 23/80

RAPID DETERMINATION OF CRUDE FAT

IN FEED STUFFS

BY USING THE SOXTEC SYSTEM

(DIETHYLETHER)

I. INTRODUCTION

The classical Soxhlet extraction with diethylether has for a long time been

used for the determination of crude fat in feed stuffs. Bowever, the method

is tedious and labour intensive. The SOXTEC SYSTEM has been developed to

eliminate the drawbacks of the original procedure. A number of determinations

have been perforraed to evaluate the SOXTEC systera in comparison with the

classical Soxhlet method.

As most fats and waxes are more soluble in hot solvents than in cold ones,

the sample in the SOXTEC EXTRACTION UNIT is first submerged in the boiling

solvent after which the remaining fat is rinsed out by the refluxing solvent

with the sample raised above the solvent surface.

Summary of Contents for Soxtec System

Page 1: ......

Page 2: ...Fix weighed extrac tion cups into Ex traction Unit nnnonn 1 Weigh extraction cups W2 Add solvent to extraction cups nnmnn Boiling extraction with thimbles in submerged boiling position 10 min i V Final extraction with thimbles in upper rinsing position 20 min followed by sol vent evaporation 5 min Remove extrac tion cups Dry extraction cups Weigh extraction f cups with extracted o Tai fat W3 W3 W2...

Page 3: ...L L Soxtec System ...

Page 4: ...11 12 12 MAINTENANCE AND SERVICE Vl 1 Vl 2 Vl 3 Vl 4 Vl 5 Vl 6 Vl 7 SERVICE UNIT 13 WATER PUMP 13 PRESSUREPUMP 13 REPLACEMENT OF HEATING ELEMENT 13 REPLACEMENT OF THERMOSTAT 15 REPLACEMENT OF CONDENSERS 16 REPLACEMENT OF SEALING MEMBRANE 16 Vl 8 REPLACEMENT OF RUBBER SLEEVE BETWEEN CONDENSER AND EXTRACTION CUP 16 Vl 9 REPLACEMENT OF HOT PLATE 18 VI 10 REPLACEMENT OF FLAT SPRING HOT PLATE 18 Vl 11 ...

Page 5: ...enient and versatile instrument whenever it comes to quantitative solvent extractions e g in the food feed and chemical pharmaceutical industries as well as in research and official laboratories The samples to be analysed are weighed into thimbles Dur ing the weighing the thimble is connected to the thimble adapter and placed in the thimble support on the balance All handling of the thimbles is do...

Page 6: ...41 011 Service Unit 1000 1461 AssemblyKit 1000 1540 Manual Extraction Unit complete comprising 1040 012 Extraction Unit 1000 1462 Extraction Cups set of 6 1000 1431 CupHolder 1000 1464 Thimble support set of 7 1000 1080 Holder for thimble support 1522 0018 Thimbles setof25 1000 1466 Thimble Adapters set of 6 1000 1467 Thimble Handler 1529 0007 Tongs for extraction cups 1000 1473 Thimble Stand 1000...

Page 7: ...Fig A Fig A 1 Fig A 2 ...

Page 8: ...als are on place Fig C It is enough to fasten the connection by hand The Service Unit must be placed close to a wall socket Never connect it without water in the tank Connect the hot water tubing from the Extraction Unit and the PVC tubing for air Seefig B If necessary the Extraction Unit can be placed further away from the Service Unit standard length of the hot water tubing is 3 m For this purpo...

Page 9: ... the tank ca 4 I with one Extraction Unit and Standard tubings Fill about 50 ml of the lubricant oil 1527 0019 into the tank this is in order to avoid unnecessary wear of the pump The thermostat is adjusted to about 90 C when the equip ment is shipped to you If you want a lower temperature use a small screw driver and turn the screw on the thermostat counter clock wise Fig E Check temperature with...

Page 10: ... provides hot water to the Extraction Unit from a built in tank The thermostat in the tank is adjustable from the outside of the Service Unit Fig E The hot water is pumped from the Service Unit to the hot plates in the Extrac tion Unit The pump can work even if the valve on the Extrac tion Unit isclosed In the Service Unit there is also a pump to give the air flow for evaporating the solvent IV 3 ...

Page 11: ......

Page 12: ...ble adapters to the magnets in the condensers of the Extraction Unit One thimble support is used on the balance when weighing sample into the thimble The thimbles are placed in the thimble stand during drying IV 6 THIMBLE HANDLER AND TONGS FOR EXTRACTION CUPS To avoid finger prints on thimbles the thimble handler is used when moving a thimble from the balance to the thimble stand or the thimble su...

Page 13: ...leased when the handler is pressed Dry in oven d After drying put defatted cotton plug above the sample and place thimbles in thimble support in holder Use thimble handler Fig J e Insert the thimbles into the condensers Raise the holder so that the support enters into the condensers Note the six knobs extraction mode should be in the rinsing posi tion Fig K f Move each extraction mode knob up to b...

Page 14: ...evaporating the solvent will be shorter but some solvent will be lost c Close the HEATING and EVAPORATION valves Release the extraction cups with the safety hook Fig N Lift out all six cups with the cup holder d Place thimble supports in holder onto the hot plates and lower the handle so the supports enter the condensers e Move extraction mode knobs so that the thimbles enter the supports f Releas...

Page 15: ...pos 4 i Loosen the four screws holding the rear part of the pump housing and remove it Fig S pos 5 j Unscrew the three screws holding the shaft seal and re place the seal Fig S pos 6 7 k Assemble the pump housing with a new O ring Fig Q Vl 3 PRESSURE PUMP 1 To increase the air flow screw clock wise on the plastic screw on the side of the air pump Fig R pos 8 2 Replacement of membrane a Unscrew the...

Page 16: ...14 ...

Page 17: ...r thermostat 18 Screw holding water pump housing 19 Watertank f Remove the cable connections g Remove the nuts holding the element Fig R pos 14 h Replace the element Fig R pos 15 Make sure that the sealings are inside the tank Vl 5 REPLACEMENT OF THERMOSTAT a Follow the procedure Vl 4 a e b c d Disconnect the two cables on the thermostat Fig R pos 16 Remove the nut on the thermostat Fig R pos 17 R...

Page 18: ...ts PVC tubings e Slide the flexible wire into the curved tube so that the magnet is free below the condenser Fig U pos 3 5 f Pull out the magnet with rod and flexible wire g Lift up recovery tube through the condenser Fig U pos 4 h Take out the old membrane To eliminate the risk of break ing the glass condenser the best way is to cut the mem brane with a knife or a scalpel i Put in the new membran...

Page 19: ...planation of symbols Knob on recovery rod Upper condenser holder Flexiblewire Recovery tube Curved tube Magnetwith holding mechanism Sealing membrane Plastic rail forslide Slide Extraction mode Knob L_ 17 ...

Page 20: ...k and disconnect the hot water tubing Explanation to symbols in from the Extraction Unit b Turn the apparatus so it is resting on the rear plate c Remove the tubing from the hotplate d Remove the snap ring Spring loaded e Lift up the hot plate f Put in the new hot plate Make sure that the flat spring is in place Replace the snap ring and connect the tubing again VI 10 REPLACEMENT OF FLAT SPRING HO...

Page 21: ...the water flow Adjust thermostat in watertank Clean the Extraction Cup Open Recovery Valve Turn counter clockwise Place Cups on center of the hot plates Replace the rubber sleeve Adjust thermostate in water tank Clean the Extraction Cup Check that evaporation valve is open and that the PVC tubing between Service and Extraction Unit is not blocked Check the pressure pump according to para Vl 3 Repl...

Page 22: ...ELECTRICAL DIAGRAM r 1041 Service Unit r 200 240V MAIN SWITCH AIR SWITCH THERMO STAT AIRPUMP WATERPUMP HEATING ELEMENT 20 ...

Page 23: ...Extraction unit comprising 1000 1461 2 ea Tubing for distribution of hot water L 0 75m inclT piececonnection 1 ea Tubing for distribution of air L 1 m 0 4 6 mm Lubricating oil for Service Unit 1527 0019 L L IX 2 SPARE PARTS For extraction Unit Condenser complete with recovery and thimble mechanism 1000 1445 Condenser glass 1000 1419 Sealing membrane in condenser 1000 1420 Knob for recovery rod 100...

Page 24: ...ir pump 1577 0008 Air pump membrane 1577 0014 Heating element 1000 1403 Thermostat 1579 0007 Strips smalI 1569 0009 Switch red 1563 0001 Switch yellow 1563 0006 Pump body to water pump 1577 0029 tecator ...

Page 25: ...r intensive The SOXTEC SYSTEM has been developed to eliminate the drawbacks of the original procedure A number of determinations have been perforraed to evaluate the SOXTEC systera in comparison with the classical Soxhlet method As most fats and waxes are more soluble in hot solvents than in cold ones the sample in the SOXTEC EXTRACTION UNIT is first submerged in the boiling solvent after which th...

Page 26: ...t should be kept in mind that the Cyclotec mill will dry the samples to some extent and that the results must be adjusted accordingly 2 Analytical balance with an accuracy 0 1 mg 3 Soxtec System M6 1040 001 complete with accessories 4 Thimbles 26 x 60 mm 1522 0018 5 Graduated cylinder 50 ml 6 Heating oven 95 100 C 7 Desiccator IV CHEMICALS 1 Diethylether anhydrous f ree from solids and peroxides S...

Page 27: ...t water to the working temperature 75 C 2 Fix thimble into thimble adaptor and place it in the thimble stand Put sorae cotton wool in the bottorn of the thimble Always use defatted thimbles and cotton wool Never handje them with your bare hands 3 Place a thimble support on the balance Use the thimble handler to transfer thimble fixed to adaptor from the stand to the support Tare support plus thimb...

Page 28: ...nd lock them in place by lowering the handle on the left of the Extraction Unit The cups will then tighten against the seals on the condensers 10 First switch on cold water through the condensers and then switch on the heating valve Preheated water 75 C from the Service Unit will then flow through the hot plates and heat the solvent to the boiling point 11 Move the thimbles to the boiling position...

Page 29: ...AND COMMENTS The 13 samples were analysed using two different times for the boiling extraction and rinsing periods respectively As can be seen in table 1 the shorter period was in most cases sufficient to achieve reliable results However there is a slight tendency to higher values on some of the samples after the longer extraction period Also the relative error was found to be slightly lower 1 36 ...

Page 30: ...ize and the duration of the extraction For ultimate accuracy the analysts are therefore requested to check the results achieved on the S O X T E C system with official results on the same samples Based on such data the extraction time in the S O X T E C system can be adjusted to get directly comparable results or a small correc tion factor can be applied The l a t t e r alternative is to be recomm...

Page 31: ... 46 2 36 3 29 5 76 6 14 2 36 4 31 16 39 8 94 3 84 11 43 2 05 X 2 23 3 44 2 35 3 30 5 79 6 10 2 39 4 34 16 28 9 02 3 81 11 43 2 08 TABLE 2 Comparison between the SOXTEC and SOXHLET results from some different laboratories SAMPLE Pig feed I Pig feed II Pig feed III Cattle feed I Cattle feed II Cattle feed III Poultry feed I Poultry feed II Coconut oil meal Cotton oil meal Oats Fish meal Corn rel err...

Page 32: ...0 9 8 10 0 14 7 15 0 2 1 2 3 5 1 5 3 10 1 10 3 15 0 15 4 2 1 2 3 5 1 5 3 10 0 10 3 14 8 15 3 correl coeff 0 9995 0 9998 0 9997 0 9993 TABLE 4 Three samples analysed by two laboratory technicians on the SOXTEC SYSTEM Duration of extrac Lab tech Sample I Sample II Sample III 30 min a 2 36 2 36 4 33 4 29 2 37 2 36 b 2 34 2 35 4 26 4 29 2 32 2 31 45 min a 2 39 2 33 4 33 4 35 2 38 2 37 b 2 36 2 35 4 31...

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