Ankom XT10 User manual
2052O’NeilRd,MacedonNY14502
Telephone:(315)986‐8090
Fax:(315)986‐8091
www.ankom.com
Operator’sManua
l
RevE4/2/12
Thispageintentionallyleftblank
TableofContents
Introduction..................................................................................................................................................................5
Warranty.......................................................................................................................................................................5
FilterBags.....................................................................................................................................................................5
OperatingEnvironment................................................................................................................................................5
ContactInformation.....................................................................................................................................................6
InstrumentDescription.................................................................................................................................................7
SafetyPrecautions........................................................................................................................................................8
InstrumentInstallation.................................................................................................................................................9
FatExtractionProcess.................................................................................................................................................10
PeriodicMaintenance.................................................................................................................................................17
Troubleshooting..........................................................................................................................................................19
AppendixA–AOCSOfficialFatExtractionProcedure................................................................................................20
AppendixB–Parts&Assemblies...............................................................................................................................22
AppendixC–ElectricalDiagram(pg.1of3)...............................................................................................................25
Thispageintentionallyleftblank
Operator’sManual
RevE4/2/12 pg.5
Introduction
ANKOM Technology designs, manufactures, and markets instruments and support products used by analytical
laboratories around the world in the environmental, agricultural, biomass, and food industries. ANKOM
Technology can provide you with products for determining or monitoring dietary fiber, detergent fiber, fat,
digestibility, microbial fermentation (anaerobic or aerobic) and more.
Committed to Total Customer Satisfaction, ANKOM designs every product based on a thorough assessment of
customer needs.
Congratulations on your purchase of theANKOMXT10 Extraction System.We are confident that this product will
effectively serve your needs.
The ANKOMXT10 Extraction System was designed to automate the process of fat extraction. This reduces
technician variation, increasing precision. By carefully following the operating instructions in this manual you will
understand the details of sample and filter bag handling as well as the instrument controls, helping you to achieve
the best possible results.
Please review the entire contents of this manual before you begin operating this
product.
Warranty
ANKOM Technology warrants the ANKOMXT10 Extraction System against any defects due to faulty workmanship
or material for one year after the original date of purchase. This warranty does not include damage to the instrument
resulting from neglect or misuse. During the warranty period, should any failure result from defects in
workmanship or materials ANKOM Technology will, at its discretion, repair or replace the instrument free of
charge.
Extended warranties are available upon request.
FilterBags
Use only ANKOM Technology filter bags (part # XT4) in your ANKOMXT10 Extraction System. Use of any other
filter mechanism will void the warranty. Filter bags can be purchased from ANKOM Technology or from your local
authorized ANKOM distributor.
OperatingEnvironment
Your ANKOMXT10 Extraction System is designed to operate within the following environments:
Ambient Temperature Range: 15°−35°C
Power: 100V−120V ~ 50/60Hz 10A / 220V−240V ~ 50/60Hz 5A
Operator’sManual
pg.6RevE4/2/12
ContactInformation
At ANKOM Technology we are committed to your total satisfaction and therefore always available to help you get
the most from your ANKOM products. We are also very interested in any comments or suggestions you may have
to help us improve.
For any questions or suggestions regarding your instrument, please contact us at:
Telephone: (315) 986-8090
Fax: (315) 986-8091
Email: [email protected]
www.ankom.com
Operator’sManual
RevE4/2/12 pg.7
InstrumentDescription
GeneralDescription
The ANKOM
XT10
Extraction System is designed to extract Crude Fat using conventional solvents, typically
petroleum ether. The compounds extracted are primarily triacylglycerols together with a small quantity of related
lipids, traditionally termed “Crude Fat.” The analysis is achieved by measuring the loss of mass due to the
extraction of fat/oil from the sample encapsulated in a filter bag. The quantitative isolation of the sample is
accomplished by surrounding the sample in a sealed filter bag with a filtering capacity in the 2 to 3 micron range.
The filter bag has sufficient porosity to permit rapid solvent passage and is composed of polymeric material that is
resistant to the higher temperatures and solvents used in the instrument.
The quantitative isolation achieved by the filter bag permits the ANKOM
XT10
Extraction System to automatically
process samples in batches of up to 15. Simply add solvent to the Extraction Vessel, place filter bags with sample in
the Extraction Vessel, add the rest of the solvent, lock the vessel in place, select the extraction time and
temperature, and press “Start.” The instrument will automatically extract the fat from the samples and recover the
solvent from the Extraction Vessel when the operation is complete.
Below is a detailed view of the ANKOM
XT10
Extraction System.
Keypad
Display
PowerSwitch(notvisible)
SafetyValveHandle
PressureGauge
ExtractionVessel
SolventRecoveryBottle
MainHandle
RefluxWaterFlowControl
Operator’sManual
pg.8RevE4/2/12
SafetyPrecautions
Flammable Hazard – Static electricity is to be avoided as it is a spark hazard.
Hot Surfaces – Do not touch the extraction vessel during operation. The surface
can exceed 70°C (158°F). Failure to observe this caution may result in injury.
Hazardous Voltages – Do not operate the instrument with the electrical
compartment open. Hazardous voltages are present during operation. Failure to
observe this caution may result in electrical shock or electrocution.
Hazardous Materials – When adding solvents, follow fill instructions
completely to avoid fire and/or explosion. Waste material will contain small
amounts of volatile solvents. Use caution when discarding. Follow safe
laboratory practices according to both local and federal regulations when
installing this instrument and when handling any organic solvents.
WARNING: Attempts to override safety features or to use this instrument in a
manner not specified by ANKOM Technology voids the warranty and may result
in serious injury or even death.
This system is designed to meet and/or exceed the applicable standards of
CE, CSA, NRTL and OSHA.
Please review the entire contents of this manual before you begin operating this
instrument.
Operator’sManual
RevE4/2/12 pg.9
InstrumentInstallation
SiteRequirements
To install and operate the ANKOM
XT10
Extraction System you will need the following:
Adjustable wrench
Chilled or tap water supply not to exceed 23°C
Adequate power (see “Operating Environment” section)
Drain
Vent Hood
InstrumentInstallationProcedure
To install the ANKOM
XT10
Extraction System, follow the procedure detailed below.
1. Remove the instrument from the shipping container and place it on a smooth level surface in an area that
is free of dust and excessive moisture and is within 6 ft. of a drain and cold water supply.
2. Place the instrument either in a Vent Hood or within 6 ft. of one.
Because the ANKOM
XT10
Extraction System is a closed system, there is very
limited exposure to solvents. When used in conjunction with a charcoal filter on
the vent line the instrument produces less than 1ml of volatiles. It is the user’s
responsibility to determine whether venting of this instrument requires placement
in a hood. Please follow both local and federal regulations when installing this
instrument.
3. Connect the tube from the top fitting to the water supply.
4. Connect the tube from the bottom fitting to the drain.
5. Connect the Solvent Recovery Bottle to the instrument.
Ensure that there are no kinks or bends in any of the tubing connected to the
instrument.
6. Plug the power cord into a grounded receptacle.
Drain
WaterSupply
VentTube
SolventRecoveryBottle
Operator’sManual
pg.10RevE4/2/12
FatExtractionProcess
CrudeFatCalculation
Crude Fat contained within a food or feed sample can be calculated using the following formula:
%CrudeFat=100x(W2–W3)
W1
Where:W1=Originalweightofsample
W2=Weightofpre‐driedsampleandfilterbag
W3=Weightofdriedsampleandfilterbag afterextraction
For meat samples with > 15% fat and plant samples with > 20% fat:
%CrudeFat=100x((W2–W4)–W3)
W1
Where:W4=Weightoftheweightin
TotalFatCalculation
If hydrolysis is done prior to fat extraction, then Total Fat contained within a food or feed sample can be calculated
using the following formula:
%TotalFat=100x(W2–(W3+(C1–C2)))
W1
Where:W1=Originalweightofsample
W2=Weightofdriedsample,filterbag,andDiatomaceousEarth(DE)afterhydrolysis
W3=Weightofdryextractedsample,filterbag,andDE
C1=Blankfilterbagdryweightafterhydrolysis
C2=Blankfilterbagweightafterextraction
FatExtractionSupportItems
The following support items are needed to perform the fat extraction procedure:
ItemRecommendedProduct
Electronic Balance with four-place readoutANKOM #TB Balance Hardware
ANKOM #TBS Balance Software
Filter BagsANKOM #XT4
Bag Holder (used for adding sample to an empty filter bag) ANKOM #101.2
Heat Sealer for sealing the filter bagsANKOM #1915 (120V), #1920 (220V)
Solvent Resistant MarkerANKOM #F08
Desiccant Pouch or Weigh Tin Desiccator for drying ANKOM #X45, #X49
Oven for drying (capable of maintaining 102°C±2°) ANKOM #RD (120V), #RDI (220V)
Ventilated oven trays to allow for sufficient oven air flow -----------------
Weigh Tins (used with samples of > 20% fat) -----------------
Sample -----------------
Spoon-----------------
Operator’sManual
RevE4/2/12 pg.11
SamplePreparationProcedureforCrudeFat–forLOWfatsamples
To prepare meat samples with ≤15% fat
by weight or plant samples with ≤20% fat by weight for fat extraction,
follow the procedure detailed below.
1. Using a Solvent Resistant Marker, number all of the empty filter bags you will use
during the fat extraction procedure. Although it is not necessary in the
determination of fat, it is recommended that you weigh and record the weights of
all the filter bags prior to filling them in order to calculate the moisture value for
the samples.
%Moisture=100x((FilterBagWeight+SampleWeight)‐Weightafterdrying)
SampleWeight
2. Place an empty filter bag in the Bag Holder in an open position.
3. Tare the weight of the empty filter bag and the holder together.
4. Add 1.5 – 2g of sample to the filter bag. Keep all particles away from the sealing
area of the filter bag.
5. Record the weight of the sample (W
1
) and tare.
6. Set the Heat Sealer dial to 6. (The setting may vary from sealer to sealer.)
7. Seal the filter bag within 4mm of its open end. Keep the
sealer arm down for 2 – 3 seconds after the red sealer light
turns off (to cool the seal). The seal can be seen as a solid
melted stripe along the top edge of the filter bag (as shown to
the right). If the seal is not strong, re-seal the bag.
8. Repeat steps 1 – 7 for all filter bags that will be used in the ANKOM
XT10
Extraction System. (Up to 15
bags can be processed during one procedure.)
9. Pre-dry all samples at 102°C±2° for 3 hours to remove moisture.
10. Remove the samples from the oven and place them in a Desiccant Pouch.
11. Allow the samples to cool to room temperature. This should take about 10 – 15 minutes.
12. Re-weigh each bag (W
2
) immediately after removing from the Desiccant Pouch.
The samples are now ready for the fat extraction procedure.
Seal
Operator’sManual
pg.12RevE4/2/12
SamplePreparationProcedureforCrudeFat–forHIGHfatsamples
To prepare meat samples with > 15% fat
by weight or plant samples with > 20% fat by weight for fat extraction,
follow the procedure detailed below.
1. Using a Solvent Resistant Marker, number all of the weigh tins and empty
filter bags you will use during the fat extraction procedure. Use one weigh tin
per filter bag. Although it is not necessary in the determination of fat, it is
recommended that you weigh and record the weights of all the filter bags
prior to filling them in order to calculate the moisture value for the samples.
%Moisture=100x((FilterBagWeight+SampleWeight)‐(Weightafterdrying‐TinWeight))
SampleWeight
2. Dry all weigh tins in an oven at 102°C±2° for 15 minutes.
3. Remove weigh tins from the oven and place them in a
Weigh Tin Desiccator or in a Desiccant Pouch.
4. Allow weigh tins to cool to room temperature.
5. Weigh and record tin weights (W
4
).
6. Place an empty filter bag in the Bag Holder in an open position.
7. Tare the weight of the empty filter bag and the holder together.
8. Add 1.5 – 2g of sample to the filter bag. Keep all particles away from the
sealing area of the filter bag.
9. Record the weight of the sample (W
1
) and tare.
10
.
Set the Heat Sealer dial to 6. (The setting may vary from sealer to sealer.)
Operator’sManual
RevE4/2/12 pg.13
11
.
Seal the filter bag within 4mm of its open end. Keep the
sealer arm down for 2 – 3 seconds after the red sealer light
turns off (to cool the seal). The seal can be seen as a solid
melted stripe along the top edge of the filter bag (as shown
to the right). If the seal is not strong, re-seal the bag.
12
.
Repeat steps 1 – 11 for all filter bags that will be used in the ANKOM
XT10
Extraction System. (Up to 15
bags can be processed during one procedure.)
13
.
Place the sealed filter bags in their corresponding weigh tins for pre-drying.
14
.
Pre-dry all samples at 102°C±2° for 3 hours to remove moisture.
15
.
Remove the weigh tins and filter bags from the oven and place them together
in a Weigh Tin Desiccator.
A Weigh Tin Desiccator is recommended because it will hold between 10 and 14
weigh tins with filter bags, depending on the size of the weigh tins. A Desiccant
Pouch will hold about 4.
16
.
Allow the samples to cool to room temperature. This should take about 10 – 15 minutes.
17
.
Re-weigh and record the weights of each weigh tin (W
4
) and filter bag (W
2
) immediately after removing
from the Weigh Tin Desiccator.
The samples are now ready for the fat extraction procedure.
Seal
Operator’sManual
pg.14RevE4/2/12
FatExtractionstep‐by‐stepprocedureusingthe
ANKOM
XT10
ExtractionSystem
To perform fat extraction on prepared samples, follow the procedure detailed below.
1. On the Display you should see “Remove/Insert Samples
Enter.”
2. Press down the Safety Valve Handle to release the Safety Valve Pin and rotate
the Main Handle upward until it stops.
3. Use the Extraction Vessel Handle to pull the Extraction Vessel out.
4. Slide the Extraction Vessel toward you far enough to remove the white Teflon
Insert.
5. Put the Bag Holder (with up to 15 bags) into the Teflon Insert.
6. Press ENTER on the Keypad.
7. On the Display you should see “Select time 60 ^…Enter.” (The number shown may not be “60.”)
8. Using the arrow keys on the Keypad, select the Extraction time. (The recommended time is 60 minutes.)
9. Press ENTER on the Keypad.
TeflonInsert
Operator’sManual
RevE4/2/12 pg.15
10
.
On the Display you should see “Heat Temp 90 ^…Enter.” (The number shown may not be “90.”)
11
.
Using the arrow keys on the Keypad, select the Temperature. (The recommended maximum temperature
is 90°C.)
12
.
Press ENTER on the Keypad.
13
.
On the Display you should see “Insert Solvent Enter.”
14
.
Ensure that the Extraction Vessel is cool.
15
.
Pour 200ml of solvent directly into the empty Extraction Vessel.
The recommended solvent for use in the ANKOM
XT10
Extraction System is
Petroleum Ether with a boiling point range of 35°C to 65°C. If you want to use
other solvents, you will need to install the XT O-ring kit for High Penetration
Solvents (part # X95) and the Valve Kit for High Penetration Solvents (part #
X73).
16
.
Put the Teflon Insert back into the Extraction
Vessel, aligning the Teflon Insert slot with the
Extraction Vessel pin.
IMPORTANT
The Teflon Insert O-ring must be in place before running the instrument.
The Extraction Vessel O-ring must be in place before running the instrument.
The Teflon Insert slot must be aligned with the Extraction Vessel pin before running
the instrument.
17
.
Pour 150ml of solvent directly into the Teflon Insert that is now back in the Extraction Vessel.
18
.
Press ENTER on the Keypad.
19
.
On the Display you should see “Close Vessel Water On Start.”
20
.
Slide the Extraction Vessel into the instrument ensuring the Extraction Vessel O-ring stays in place.
TeflonInsertO‐ring
ExtractionVesselO‐ring
Teflon
Insertslot
and
Extraction
Vesselpin
Operator’sManual
pg.16RevE4/2/12
21
.
Pull the Main Handle downward, closing and locking the Extraction Vessel in
place. You will hear a click noise when the Safety Valve Pin locks in place.
IMPORTANT
Before running the instrument, verify that the Extraction Vessel is locked in place by
attempting to rotate the Main Handle upward. If it is not locked, follow step #20 above.
22
.
Verify that the water supply is on.
23
.
Press START on the Keypad. The instrument will run through its automatic operation, showing its status
on the Display.
24
.
When the instrument has completed its automatic operation, the Display will read:
“Remove/Insert Samples Enter.”
At this time, the only light shining on the Display should be the green power
light.
25
.
When the Pressure Gauge reads zero, remove the Extraction Vessel by pushing down on the Safety Valve
Handle to release the locking pin and then rotating the Main Handle to the open position.
26
.
Use the Extraction Vessel Handle to remove the Extraction Vessel.
Warning: The Extraction Vessel interior and top will be HOT when the
extraction process is complete.
27
.
Remove the Teflon Insert from the Extraction Vessel.
28
.
Clean the fat from the bottom of the vessel using paper towel.
IMPORTANT
If too much fat accumulates in the bottom of the Extraction Vessel, an overtemp fault will
occur.
29
.
Remove the Bag Holder from the Teflon Insert.
30
.
Remove the filter bags from the Bag Holder.
31
.
Dry the samples in an oven at 102°C±2° for 30 minutes.
32
.
Remove the samples from the oven and place them in a Desiccant Pouch.
33
.
Allow the samples to cool to room temperature. This should take about 10 – 15
minutes.
34
.
Re-weigh each filter bag (W
3
) immediately after removing from the Desiccant Pouch.
Operator’sManual
RevE4/2/12 pg.17
PeriodicMaintenance
CleaningtheExtractionVessel
Some compounds extracted during the fat extraction procedure can create a black residue in the bottom of the
Extraction Vessel. The vessel can most easily be cleaned by using a drill with a long shafted stiff wire brush. This
treatment will remove a lot of the black coating that accumulates on the bottom of the vessel. When the vessel
bottom is clean, put some solvent on a cloth or paper towel and wipe down the inside of the vessel in an effort to
remove any oil residue and particles that have been loosened from the vessel bottom.
IMPORTANT
Do not use soap and/or water to clean the vessel.
When cleaning the vessel, do not damage the level sensor tip. The tip may be cleaned
with window cleaner or alcohol.
Cleaningtheexterioroftheinstrument
Wipe the outside of the instrument with window cleaner or a damp sponge as necessary.
Do not use Acetone to clean the instrument.
Cleaningthesolventfilter
If filter bags are not sealed properly and sample is lost from the bag, it will be recovered in the solvent filter in the
exhaust line.
To clean the solvent filter, follow the procedure detailed below.
1. Remove the rear cabinet of the instrument.
RearViewofinstrumentwithcabinetbackremoved
2. Unscrew the compression fitting.
3. Unscrew the filter body.
4. Unscrew and clean the metal filter screen.
5. Reassemble the filter and compression
fitting. Make sure the valve body is tight and
the Teflon washer has not come out of the
filter body.
CompressionFitting
Filter
body
Operator’sManual
pg.18RevE4/2/12
Cleaningthewaterfilter
To clean the water filter (located on the water supply line), follow the procedure detailed below.
1. Unscrew the filter from the instrument.
2. Unscrew the filter clamp from the water supply line.
3. Use compressed air to blow backwards through the
filter (blow opposite the arrow on the filter).
4. Reconnect the filter and fittings.
5. Turn on the water and check for leaks.
ReplacingtheFuses
To replace the fuses in the ANKOM
XT10
Extraction System, follow the procedure detailed below.
1. Turn off the instrument power and unplug the Power Cord from the outlet.
2. Remove the two screws on the Top Cover.
3. Swing the Top Cover down exposing the electrical compartment.
4. Locate the Fuse Holders on the terminal strip. There
are two fuses within the instrument; one for each pole
(100 – 120V 10A or 220 – 240V 5A).
5. Press the tabs to lift the Fuse Holders up.
6. Replace the fuses and close the Fuse Holders completely.
7. Close the Top Cover and secure it with the two screws that you previously removed.
Fuse
Holders
Tabtoopen
FuseHolder
Fuse
Filter
Operator’sManual
RevE4/2/12 pg.19
Troubleshooting
The ANKOM technology web site has the most current troubleshooting information. Therefore, if you have any
questions about the operation of your ANKOMXT10 Extraction System, please visit our web site at
www.ankom.com.
Operator’sManual
pg.20RevE4/2/12
AppendixA–AOCSOfficialFatExtractionProcedure
ANKOMTechnologyMethod–Version1/30/09AOCSOfficialProcedureAm5‐04
RapidDeterminationofOil/FatUtilizingHighTemperatureSolventExtraction
Definition
This method determines crude fat by extracting with petroleum ether. The compounds extracted are predominantly triacylglycerides. Small
amounts of other lipids along with minor compounds having some solubility in petroleum ether are also extracted.
Scope
This method is applicable to solid processed foods with 0-100% fat content.
Apparatus
1. Analytical Balance—capable of weighing 0.1 mg.
2. Oven—capable of maintaining a temperature of 102 ± 2°C
(ANKOMRD Dryer, ANKOM Technology).
3. Extraction instrument—capable of extracting at 90 ± 2°C.
(XT10, XT15, XT20, ANKOM Technology).
4. Filter Bags—constructed from chemically inert and heat
resistant filter media, capable of being heat sealed closed and
able to retain 1 micron particles while permitting solution
penetration (XT4, ANKOM Technology).
5. Heat sealer—sufficient for sealing the filter bags closed to
ensure complete closure (1915, ANKOM Technology).
6. Desiccant Pouch—collapsible sealable pouch with desiccant
inside that enables the removal of air from around the filter bags
(MoistureStop weigh pouch, ANKOM Technology).
7. Marking pen—Solvent and acid resistant (F08, ANKOM
Technology).
Reagents
1. Petroleum Ether (B.P. 35-65º C). Depending on the method
used, other solvents such as hexanes and ethyl ether may be
used. CAUTION: Most fat solvents are extremely flammable.
Avoid static electricity and follow safe laboratory practices
according to your local regulations when handling solvents.
Precision
Results from the collaborative study (see Table 1) indicate the
precision (Sr, RSDr, r) that the analyst should use as a benchmark for
evaluation replication in the same laboratory.
Procedure(seetheFatExtractionProcesssectionoftheOperator’s
Manualformoredetail)
1. Place a labeled filter bag on the balance and zero the balance.
2. Weigh 1.5 – 2g of sample into the bag and record the weight
(W1).
3. Heat seal the filter bag closed within 4mm of the top to
encapsulate the sample.
4. It is good practice to include a blank bag periodically,
especially when changing solvents, in order to measure any
effect on the filter bag.
5. If a meat sample has an expected fat value of > 15% or a plant
sample has an expected fat value of > 20%, then place the
filter bag with sample in a tared weigh tin (W4) during the
oven drying procedure in order to capture fat that may migrate
out of the bag during heating.
6. Place samples in the drying oven for 3 hrs (see Numbered
Note 1).
7. Cool the dried samples in the Desiccant Pouch, weigh and
record the weight (W2).
8. Place filter bags with sample into the bag holder and place in
the extractor.
9. Select the extraction time and proceed according to the
extraction instruments instructions.
10. When the extraction process is complete place the samples in
the oven for 15 – 30 minutes (see Numbered Note 2).
11. Cool in the Desiccant Pouch and weigh (W3).
Calculations
Meatsamples≤15%fatandplantsamples≤20%fatMeatsamples>15%fatandplantsamples>20%fat
%CrudeFat=100x(W2–W3) %CrudeFat=100x((W2–W4)‐W3)
W1W1
Where:W1=OriginalweightofsampleWhere:W4=Weightoftheweightin
W2=Weightofpre‐driedsamplewithfilterbag
W3=Weightofdrysamplewithfilterbagafter
extraction
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