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1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
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1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
Table of Contents
1 PRECAUTIONS AND PROCEDURES
1.1 Intended use..............................................................................................1
1.2 Safety precautions.................................................................................1
2 INTRODUCTION
2.1 Performance data...................................................................................3
3 PREPARATIONS FOR USE
3.1 Unpacking and checking ....................................................................4
3.2 Installation .................................................................................................5
3.2.1 Installation requirements ............................................................................5
3.2.2 Fuses .................................................................................................................5
3.2.3 Installation instructions................................................................................5
4 OPERATION
4.1 Preliminary preparation.....................................................................6
4.2 Pre-extraction ...........................................................................................7
4.3 Hydrolysis ..................................................................................................8
4.4 Drying............................................................................................................9
4.5 Solvent extraction .................................................................................9
4.6 Calculation................................................................................................10
5 MAINTENANCE
5.1 Change of vacuum valve ................................................................11
5.2 Change of condenser .........................................................................11
5.3 Change of filter seal, upper ..........................................................11
5.4 Change of the lower thimble holder........................................12
5.5 Change of the vacuum tube ..........................................................12
5.6 Change of fuses.....................................................................................12
6 TECHNICAL SPECIFICATIONS
6.1 Safety...........................................................................................................13
6.2 Environmental conditions...............................................................13
6.3 Lifting instructions..............................................................................13
7 Foss Tecator APPLICATION NOTES SYSTEM
8 ACCESSORIES AND SPARE PARTS
8.1 Accessories ...............................................................................................15
8.2 Spare parts ...............................................................................................15
8.3 Manufacturer’s name and address............................................15
9 SAFETY INFORMATION 1047 (GB) ................................17
9 SICHERHEITSINFORMATIONEN 1047(DE) ..............20
9 SIKKERHEDSINFORMATION 1047(DK) .....................24
9 INFORMACION DE SEGURIDAD 1047 (ES)............28
1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
9 TURVALLISUUSOHJEET 1047 (FIN)................................32
9 INSTRUCTIONS DE SECURITE 1047(FR)....................36
9ËÇØÇ ÌÅÔÑÙÍ ÁÓÖÁËÅÉÁÓ 1047 (GR)......................40
9 ÖRYGGISLEIÐBEININGAR 1047(IS)..............................45
9 INFORMAZIONI DI SICUREZZA 1047(IT).................48
9 VEILIGHEIDSINFORMATIE 1047(NL)...........................52
9 SIKKERHETSINFORMASJON 1047(NO).....................56
9 INFORMAÇÕES DE SEGURANÇA 1047(PT) ...........59
9 SÄKERHETSINFORMATION 1047(SE)..........................63
1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
2INTRODUCTION
Crude Fat is generally defined as sample constituents soluble in
appropriate organic solvents, such as diethyl ether, petroleum
ether or chloroform. The main constituents in Crude Fat are
triglycerols and free fatty acids. In certain Sample types, however,
some of the fat, or lipids, are bound as lipoproteins,
liposaccharides or metal salts. Solvents are not capable of
breaking such bonds, therefore hydrolysis is used to transform
these lipids into extractable forms.
The 1047 Hydrolyzing Unit in combination with Soxtec System
HT enables total fat extractions to be performed in a simple way
in a variety of Sample types.
2.1 Performance data
Sample size 0.5-5 g
Measuring range 0-100% fat
Capacity per batch 6 per unit
Speed of hydrolyzing cycle 20-60 min
1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
3
STEC004A
Fig. 1 The procedure for fat determination with 1047 Hydrolyzing Unit and 1043 Soxtec Extraction Unit.
3PREPARATIONS FOR USE
3.1 Unpacking and checking
Unpack the 1047 Hydrolyzing Unit and its accessories with care.
Remove all packing material.
Use the parts list, packed together with the instrument and check
that you have received all parts. Use Fig.2 to identify the
different parts. If any parts are missing, contact your Foss Tecator
representative.
1. Hydrolyzing Unit 2. Sample Tube (set of 6)
3. Glass Thimbles (set of 6) 4. Glass Thimble Holder (set of 6)
5. Water Spray Device 6. Beaker
7. Tube Stand 8. Reflector
9. Cleaning rod 10. Glass Thimble adaptor (set of 6)
11. Celite 12. Tube 8/11 L= 2 m
13. Tube 6/11 L= 2 m 14. Spray bottle, red
15. Cotton 16. Glass Thimble seals (set of 6)
17. Water Aspirator Pump 18. Hydrolysis Stand
19. Manual 22. Mains cable
1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
4
1047011A
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15 16
17
18
19
22
Fig. 2
3.2 Installation
All text in this section is translated in
local language.
3.2.1 Installation requirements
Power supply 110 or 200-230V, 50-60 Hz
Power consumption 975W
Dimensions L xDxH 61x31x85cm
Weight 23 kg
Water supply Tap water approx. 2 l/min
(cooling). Tap water for vacuum
pump.
Ventilation Fume hood is recommended.
Place the unit on the laboratory bench near
suitable power, water and drainage.
3.2.2 Fuses
External: 230V: Two fuses T 6,3 A.
110V: Two fuses T 10 A.
3.2.3 Installation instructions
Before connecting to an earthed power supply,
make sure that the mains voltage agrees with
the voltage quoted at the rear of the unit.
Connect tubes to the rear of the unit
according to fig. 3.
1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
5
1047012A
1
2
3
4
5
VACCUM
WATER
DRAIN
!
Fig. 3 1. Equipotential screw, 2. Mains and fuses, 3. Vacuum (water aspirator
pump), 4. Cooling water inlet, 5. Drain.
4OPERATION
Total fat determinations according to most
accepted procedures include the following
main steps:
·Hydrolysis with boiling acid
·Cooling of solution with solubilized fat
·Filtration
·Drying of hydrolyzed sample residue
·Solvent extraction
·Drying of extracted matter
·Weighing and calculation
Due to local reference methods, variations in
e.g. acid strength, hydrolysis time, type of
solvents etc. do occur.
Samples rich in fat (>10 %) are generally
recommended to be pre-extracted before
hydrolysis.
The following description of how to operate
the 1047 Hydrolyzing Unit in conjunction with
1043 or 1045 Soxtec Extraction Systems, is
generally based. For more detailed
information on specific types of samples,
please ask your local Foss Tecator dealer for
"Application Notes".
4.1 Preliminary preparation
In order to achieve as good results as
possible, all samples must be homogenized in a
proper way before chemical treatment.
Sample Type of milI
Dry product, e.g. Cyclone mill e.g.
grains, foods,
granulates
1093 Cyclotec.
Products high in
moisture,
Knife homogenizer e.g.
fat or fibrous samples. 1094 Homogenizer or
Moulinex.
In order to make wet samples e.g. meat
products more lyphilic, a short predrying
before extraction is recommended.
1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
6
4.2 Pre-extraction
As high fat levels can prevent effective
hydrolysis, samples with 10% fat content
should be pre-extracted with the same type of
solvent as used in the final extraction.
1.Weight in the sample with a precision of
1000 ±2 mg. Load the glass thimble with 1 g
celite and the sample. Do not cover with
cotton.
2.Fit adapters on the thimbles, by
introducing them into the thimbles in such a
way that the circlip is compressed
progressively into the thimble, (i.e. the
closed side of the circlip is pressed in
first and then working towards the open
side), and insert them into the Soxtec HT
Extraction Unit.
3.Add solvent and extract for 10 minutes in
"Rinsing" position.
4.After the extraction, dry the extraction
cups in an oven at 100°C for 30 minutes. Let
them cool down and weigh them. Calculate
percentage extracted fat. If the fat
content is high, 20% , it is recommended to
use a second extraction cup for the final
extraction.
5.Remove the thimble holders from the glass
thimbles. Transfer the pre-extracted sample
as quantitatively as possible from the
glass thimble to a sample tube for acid
hydrolysis. Proceed from step 2 of the
hydrolysis part.
Note: Use the same glass thimbles for the filtration after
hydrolysis (see 4.3 position 4 )
1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
7
1047013A
Fig. 4 Insert the tube with sample and
celite into the Hydorlyzing Unit.
4.3 Hydrolysis
1. Weigh the samples with a precision of
1000 ±2 mg and transfer them to the sample
tubes.
2. Add 1-2 g of celite and 100-120 ml of the
acid solution to each sample tube. The
level of the acid solution must be over
the top of the cover of the heaters.
3. Insert the tubes into position in the
1047 Hydrolyzing Unit (Fig. 4). Lower the
suction tubes to the fume exhaust
position by pulling the handle upwards
(Fig. 5). The teflonpart should rest on
the top of the sample tubes and the
suction tubes should be about one
centimeter down in the sample tubes.
4. Place the glass thimbles into the thimble
supports (Fig. 6) and insert them into
the Hydrolyzing Unit(Fig. 7).
Note: If pre-extraction according to section 4.2 has been
carried out, check that the thimbles are used for the same
samples as in pre-extraction.
5. Start the water aspirator pump for the
fume exhaust system. Open vacuum valves
(Fig. 7) under each thimble. Adjust
during boiling for low fume exhaust.
6. Turn on the heater to maximum effect and
place the reflector in front of the
sample tubes. When the solution starts
boiling, adjust to a gently boiling speed
with the heater control (Fig. 8).
7. At the end of the hydrolysing period,
turn off the heater and remove the
reflector.
8. Open the cold water tap for the
condensers (approximately 2 l/m).
9. Pull down the suction tube handle to
pos. 1 (Fig. 5). Dilute the acid solution
in each tube with some 100 ml of 20-25°C
distilled water. Close the vacuum valve
(Fig. 7) under each thimble.
10. Lower the suction tubes to pos. 2
(Fig. 5). Open the vacuum valve (Fig. 7)
under one thimble and suck up the sample
solution and as much as possible of the
solid particles in the solution. Close
the valve and repeat in the same way with
the rest of the tubes.
1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
8
1047014A
2
1
Fig. 5 Pull the handle up (to pos 2) to
lower the suction tubes.
1047015A
Fig. 6 Use gloves when handling thimbles
to minimize contamination.
1047016A
Fig. 7 Turn the knob to open/close the
vacuum valve.
11. Wash each tube by opening the vacuum
valve and spray 5x50 ml of approximately
50°C distilled water, by using the water
sprayer (Fig. 9).
12. Raise the suction tubes and take out one
of the sample tubes. Cover the cleaning
rod with a thin layer of defatted
cottonwool and wet it with acetone. Clean
the inside of the tubes by gently pushing
and pulling the cleaning rod up and down
in the tube (Fig. 10). Take a small piece
of the cottonwool and clean the outside
of the suction tube if necessary. Place
each pad of the cottonwool on the top of
the sample residue in the glass thimble.
Note: Do not have the valves in closed position when the
Hydrolysing Unit is shut down.
4.4 Drying
To make the wet sample residue lyophilic and
achieve effective solvent extraction, the
residue and thimble must be dried.
Alt. 1: Dry overnight at 60-80°C in a oven.
Alt. 2: Dry in a microwave oven with
turntable at medium power for 30-60
minutes.
Most samples can be dried in a microwave oven,
except meat and fish products.
1WARNING!
Do not use a microwave oven if residues of organic
solvents are present.
4.5 Solvent extraction
1.Fit the adapters, as written in 4.2:2, to
each thimble and insert them into the Soxtec
HT Extraction Unit.
2.Extract and analyse the samples according
to the Soxtec HT Extraction Unit
instructions, see Soxtec HT manual.
1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
9
1047017A
Fig. 8
1047018A
Fig. 9 Wash the tubes with the sprayer to
suck up the residues of the sample solution.
1047019A
Fig. 10 Clean the tube with the cleaning
rod and defatted cotton.
4.6 Calculation
Calculate the fat content according to the
formula below.
W3 = The extraction cup weight after fat
extraction and cooling in desiccator.
W2 = Clean and predried extraction cup.
W1 = Sample weight.
% Fat = W3-W2 x 100
W1
If a pre-extraction was required, using two
extraction cups, add the two results that have
been calculated, and the sum is the total fat
in the sample.
F1 = Fat content after pre-extraction.
F2 = Fat content in final extraction.
% Fat/Oil = F1 + F2
1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
10
5MAINTENANCE
5.1 Change of vacuum valve
1. Loosen all neoprene tubings carefully that are connected to
the suction tubes, by removing the plastic straps.
2. Lower the suction tubes down the horizontal plate, so the
suction tubes rest against the bottom of the oven.
3. Unscrew the 3 screws that are placed on the white plate on
the backside of the hydrolyzing unit. Unscrew the 3 screws
that are on the bottom of the white plate.
4. Take away the white plate.
5. Loosen the 6 metal clips on the neoprene tubings connected
to the connection tube and then loosen the neoprene tubes
from the connection tube.
Note: Do not take away the neoprene tube that is situated
to the far right.
6. Fold the connection tube to the right.
7. Carefully loosen and take away the filter seal that is
connected on the top of the vacuum valve to be changed.
8. Turn the vacuum valve knob counter clockwise until it
disengages.
9. The vacuum valve is now free and is drawn out from the
rear of the hydrolyzing unit.
10. Fit the new vacuum valve and put together in reverse order.
5.2 Change of condenser
1. Take away the plastic straps on the 3 neoprene tubings that are
connected to the condenser and loose the tubings from the
condenser.
2. Loosen carefully the condenser from the filter seal and pull the
condenser right up.
3. Assemble the new condenser and connect the tubes in the same
way as for the old condenser.
5.3 Change of filter seal, upper
1. Loosen the condenser according to paragraph 5.2 Pos. 1-3
1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
11
2. Carefully loosen and pull out the old filter seal. Press gently
down the new filter seal.
Note: Check carefully the correct positioning of the new
filter seals.
5.4 Change of the lower thimble
holder
1. Loosen the old thimble holder by gently easing and pulling it
upwards.
2. Press down the new thimble holder and check that it fits
correctly.
5.5 Change of the vacuum tube
1. Remove the plug from the wall socket.
2. Unscrew the instrument panel with the heating control knob.
3. Remove the white plate on the back of the hydrolyzing unit
according to paragraph 5.1 Pos. 1- 4.
4. Remove the plastic strap on the neoprene tube that is situated
to the far right on the connection tube.
5. Unscrew the nipple on the back of the hydrolyzing unit that is
marked "vacuum".
6. Pull out the tube with the nipple through the instrument hole.
7. Cut the new vacuum tube to 450 mm and assemble the nipple
from the old tube.
8. Assemble the rest in reverse order.
5.6 Change of fuses
1. The 2 pole fuse holder is located under the mains cable. Push
the middle button and change the fuses.
1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
12
1047012A
1
2
3
4
5
VACCUM
WATER
DRAIN
!
Fig. 11 Pos 2: 2 pole fuse holder and mains
6TECHNICAL
SPECIFICATIONS
6.1 Safety
The insulation of external, inaccessible
circuits is reinforced.
6.2 Environmental conditions
The equipment is designed to be safe at least
under the following conditions:
·Indoor use
·Altitude up to 2000 m.
·Temperature 5°C to 40°C.
·Maximum relative humidity 80% for
temperatures up to 31°C decreasing linearly
to 50% relative humidity at 40°C.
·Mains supply voltage fluctuations not
exeeding ±10% of the rated voltage.
·Transient overvoltage is according to
category II, which is normal for this type
of equipment.
·Pollution degree 2.
6.3 Lifting instructions
This instrument is not equipped with handles
or grips. One or two persons are needed to
lift the instrument, following the
instructions below:
1. Tilt the instrument slightly backwards,
lift and support the instrument as shown
in fig.12 to simplify and ensure a safe
lift.
2. Weight 23 kg.
1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
13
1047021a
Fig. 12
7Foss Tecator
APPLICATION NOTES
SYSTEM
For information about preparation of chemicals and the Solvent
Extraction (with hydrolysis) method. please see the Application
Note AN 301.
In Foss Tecators extensive list of Application Sub Notes you will
find information on how to analyse the sample of your choice.
Please contact your Foss Tecator representative for more details.
1047 Soxtec System Hydrolyzing Unit, User Manual, Rev. 2.2, Part no 1000 3315, Foss Tecator AB, Sweden
14
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