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2052 O’Neil Rd, Macedon NY 14502 Telephone: (315) 986‐8090 Fax: (315) 986‐8091 www.ankom.com Operator’s Manual Rev E 4/2/12
2052 O’Neil Rd, Macedon NY 14502 Telephone: (315) 986‐8090 Fax: (315) 986‐8091 www.ankom.com
Operator’s Manual
Rev E 4/2/12
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Table of Contents
Introduction .................................................................................................................................................................. 5
Warranty ....................................................................................................................................................................... 5
Filter Bags ..................................................................................................................................................................... 5
Operating Environment ................................................................................................................................................ 5
Contact Information ..................................................................................................................................................... 6
Instrument Description ................................................................................................................................................. 7
Safety Precautions ........................................................................................................................................................ 8
Instrument Installation ................................................................................................................................................. 9
Fat Extraction Process ................................................................................................................................................. 10
Periodic Maintenance ................................................................................................................................................. 19
Troubleshooting .......................................................................................................................................................... 21
Appendix A – AOCS Official Fat Extraction Procedure ................................................................................................ 23
Appendix B – Parts & Assemblies ............................................................................................................................... 25
Appendix C – Electrical Diagram ................................................................................................................................. 28
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Operator’s Manual
Rev E 4/2/12 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 the ANKOMXT15 Extraction System. We are confident that this product will effectively serve your needs.
The ANKOMXT15 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 ANKOMXT15 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.
Filter Bags
Use only ANKOM Technology filter bags (part # XT4) in your ANKOMXT15 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.
Operating Environment
Your ANKOMXT15 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’s Manual
pg. 6 Rev E 4/2/12
Contact Information
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’s Manual
Rev E 4/2/12 pg. 7
Instrument Description
General Description
The ANKOMXT15 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 ANKOMXT15 Extraction System to automatically process samples in batches of up to 15. With the solvent reservoir filled, simply place filter bags with sample in the Extraction Vessel, lock the vessel in place, select the extraction time and temperature, and press “Start.” The instrument will automatically fill the Extraction Vessel with solvent, extract the fat from the sample, and recycle the solvent.
Below is a detailed view of the ANKOMXT15 Extraction System.
Keypad
Display
Power Switch (not visible)
Safety Valve Handle
Pressure Gauge
Extraction Vessel
Solvent Fill Port
Main Handle
Solvent Sight Level Reflux Water Flow Control
Operator’s Manual
pg. 8 Rev E 4/2/12
Safety Precautions
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 – The ANKOMXT15 Extraction System comes equipped with a charcoal filter which traps any residual vapor in the vent system. By properly maintaining the charcoal filter, volatiles will not escape the vent system. We recommend replacement of the filter every 3 months or after 100 extraction runs. Trace amounts of vapor may also be present when samples are removed. It is recommended that the ANKOMXT15 Extraction System be placed in a well ventilated environment, away from any heat or ignition sources. Organic solvents may be flammable. 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’s Manual
Rev E 4/2/12 pg. 9
Instrument Installation
Site Requirements
To install and operate the ANKOMXT15 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
Instrument Installation Procedure
To install the ANKOMXT15 Extraction System, follow the procedure detailed below.
1. Remove the instrument from the shipping container and place in an area that is free of dust and excessive moisture, and is well ventilated (away from any heat or ignition sources).
Because the ANKOMXT15 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.
2. Connect the tube from the top fitting to the water supply and the one from the bottom fitting to the drain.
Ensure that there are no kinks or bends in any of the tubing connected to the instrument.
3. Connect the vent flask to the Vent Flask Connector on the instrument and run the tubing to the inline charcoal filter. Periodically check the vent line to verify that it is free from any blockage or kinks. Generally, there should not be any significant solvent in the vent flask. Any solvent visible in the flask may indicate a problem with the water supply to the instrument.
Change the Charcoal Filter every 3 months or after 100 extraction runs.
4. Plug the power cord into a grounded receptacle.
Charcoal Filter
Water Supply
Drain
Vent Flask Connector
Operator’s Manual
pg. 10 Rev E 4/2/12
Fat Extraction Process
Crude Fat Calculation
Crude Fat contained within a food or feed sample can be calculated using the following formula:
% Crude Fat = 100 x (W2 – W3) W1
Where: W1 = Original weight of sample W2 = Weight of pre‐dried sample and filter bag W3 = Weight of dried sample and filter bag after extraction
For meat samples with > 15% fat and plant samples with > 20% fat:
% Crude Fat = 100 x ((W2 – W4) – W3) W1
Where: W4 = Weight of the weigh tin
Total Fat Calculation
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:
% Total Fat = 100 x (W2 – (W3 + (C1 – C2))) W1
Where: W1 = Original weight of sample W2 = Weight of dried sample, filter bag, and Diatomaceous Earth (DE) after hydrolysis W3 = Weight of dry extracted sample, filter bag, and DE C1 = Blank filter bag dry weight after hydrolysis C2 = Blank filter bag weight after extraction
Fat Extraction Support Items
The following support items are needed to perform the fat extraction procedure:
Item Recommended Product
Electronic Balance with four-place readout ANKOM #TB Balance Hardware
ANKOM #TBS Balance Software
Filter Bags ANKOM #XT4
Bag Holder (used for adding sample to an empty filter bag) ANKOM #101.2
Heat Sealer for sealing the filter bags ANKOM #1915 (120V), #1920 (220V)
Solvent Resistant Marker ANKOM #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’s Manual
Rev E 4/2/12 pg. 11
Solvent preparation procedure
To fill the solvent reservoir follow the procedure detailed below.
1. Unscrew the Fill Cap.
2. Pour solvent into the Fill Port up to the dark blue level mark on the Solvent Sight Level. Do not add solvent up to the top of the Solvent Sight Level tube or it will start flowing into the Vent Flask.
If using Diethyl Ether or a solvent mixture that includes Diethyl Ether (such as the Mojonnier Mixture), you will need the O-ring Kit for High Penetration Solvents (part # X95) to replace the standard O-rings on the top of the Extraction Vessel and the Valve Kit for High Penetration Solvents (part # X55).
Warning: Do NOT use Acetone in this instrument because it will cause damage to the valves.
Operator’s Manual
pg. 12 Rev E 4/2/12
Sample Preparation Procedure for Crude Fat – for LOW fat samples
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 = 100 x ((Filter Bag Weight + Sample Weight) ‐ Weight after drying) Sample Weight
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 (W1) 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 ANKOMXT15 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 (W2) immediately after removing from the Desiccant Pouch.
The samples are now ready for the fat extraction procedure.
Seal
Operator’s Manual
Rev E 4/2/12 pg. 13
Sample Preparation Procedure for Crude Fat – for HIGH fat samples
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 = 100 x ((Filter Bag Weight + Sample Weight) ‐ (Weight after drying ‐ Tin Weight)) Sample Weight
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 (W4).
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 (W1) and tare.
10. Set the Heat Sealer dial to 6. (The setting may vary from sealer to sealer.)
Operator’s Manual
pg. 14 Rev E 4/2/12
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 ANKOMXT15 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 (W4) and filter bag (W2) immediately after removing from the Weigh Tin Desiccator.
The samples are now ready for the fat extraction procedure.
Seal
Operator’s Manual
Rev E 4/2/12 pg. 15
Fat Extraction step‐by‐step procedure using the ANKOMXT15 Extraction System
To perform fat extraction on prepared samples with solvent in the reservoir, 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 or to put the Bag Holder directly into Teflon Insert while it remains in the Extraction Vessel.
It is not necessary to remove the white Teflon Insert from the Extraction Vessel in order to put the Bag Holder in place.
5. Put the Bag Holder (with up to 15 bags) into the Teflon Insert.
Teflon Insert
Operator’s Manual
pg. 16 Rev E 4/2/12
6. If you removed the Teflon Insert, put it 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.
7. Slide the Extraction Vessel into the instrument ensuring the Extraction Vessel O-ring stays in place.
8. 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 #7 above.
9. Press ENTER on the Keypad.
10. On the Display you should see “Select time 60 ^…Enter.” (The number may not be “60.”)
11. Using the arrow keys on the Keypad, select the Extraction time. (The recommended time is 60 minutes.)
12. Press ENTER on the Keypad.
13. On the Display you should see “Heat Temp 90 ^…Enter.”
14. Using the arrow keys on the Keypad, select the Temperature. (The recommended maximum temperature is 90°C.)
15. Press ENTER on the Keypad.
16. On the Display you should see “Close Vessel Water On Start.”
17. Verify that the water supply is on.
18. Press START on the Keypad. The instrument will run through its automatic operation, showing its status on the Display.
Teflon Insert O‐ring
Extraction Vessel O‐ring
Teflon Insert slot and Extraction Vessel pin
Operator’s Manual
Rev E 4/2/12 pg. 17
19. 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.
20. 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.
21. 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.
22. Remove the Teflon Insert from the Extraction Vessel.
23. 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.
24. Remove the Bag Holder from the Teflon Insert.
25. Remove the filter bags from the Bag Holder.
26. Dry the samples in an oven at 102°C±2° for 30 minutes.
27. Remove the samples from the oven and place them in a Desiccant Pouch.
28. Allow the samples to cool to room temperature. This should take about 10 – 15 minutes.
29. Re-weigh each filter bag (W3) immediately after removing from the Desiccant Pouch.
Operator’s Manual
pg. 18 Rev E 4/2/12
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Operator’s Manual
Rev E 4/2/12 pg. 19
Periodic Maintenance
Cleaning the Extraction Vessel
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.
Cleaning the exterior of the instrument
Wipe the outside of the instrument with window cleaner or a damp sponge as necessary.
Do not use Acetone to clean the instrument.
Cleaning the solvent filter
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.
Rear View of instrument with cabinet back removed
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.
Compression Fitting
Filter body
Operator’s Manual
pg. 20 Rev E 4/2/12
Cleaning the water filter
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.
Replacing the Fuses
To replace the fuses in the ANKOMXT15 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.
Replacing the Charcoal Filter
The Charcoal Filter should be replaced every 3 months, or after 100 extraction operations using the instrument. To replace the filter, remove the old one from the vent line and install the new one.
Fuse Holders
Tab to open Fuse Holder
Fuse
Filter
Operator’s Manual
Rev E 4/2/12 pg. 21
Troubleshooting
The ANKOM technology web site has the most current troubleshooting information. Therefore, if you have any questions about the operation of your ANKOMXT15 Extraction System, please visit our web site at www.ankom.com.
Operator’s Manual
pg. 22 Rev E 4/2/12
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Operator’s Manual
Rev E 4/2/12 pg. 23
Appendix A – AOCS Official Fat Extraction Procedure
ANKOM Technology Method – Version 1/30/09 AOCS Official Procedure Am 5‐04
Rapid Determination of Oil/Fat Utilizing High Temperature Solvent Extraction
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 (see the Fat Extraction Process section of the Operator’s Manual for more detail)
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
Meat samples ≤ 15% fat and plant samples ≤ 20% fat Meat samples > 15% fat and plant samples > 20% fat
% Crude Fat = 100 x (W2 – W3) % Crude Fat = 100 x ((W2 – W4) ‐ W3)
W1 W1
Where: W1 = Original weight of sample Where: W4 = Weight of the weigh tin
W2 = Weight of pre‐dried sample with filter bag
W3 = Weight of dry sample with filter bag after extraction
Operator’s Manual
pg. 24 Rev E 4/2/12
Numbered Notes
1. Pre-drying time of the samples in the filter bags can be greatly reduced by using a microwave oven. However, microwave ovens vary in energy output and samples vary in water and fat composition. You will need to experiment with your microwave oven to determine the proper conditions for use. Contact ANKOM Technology for further information.
2. Some samples with large amounts of carbohydrates (starches and cellulose) may bind small quantities of solvent and require additional post drying. To remove bound solvent, dry at 100°C for 1 – 3 hrs or at 125°C for 30 minutes.
Sample ID oat
mea
l
bro
wni
e m
ix
soy
bean
A
can
ola
soy
bean
mea
l
cor
n A
pou
ltry
star
ter
cat
tle
feed
pig
sta
rter
alf
alfa
cat
foo
d
coo
kies
bkf
t cer
eal
tort
illa
chi
ps
Number of laboratories 12 12 11 9 12 12 11 10 11 11 12 11 12 12Number of replicates 24 24 22 18 24 24 22 20 22 22 24 22 24 24
Filter Bag Average, % Crude Fat 5.8 8.7 20.9 39.0 1.6 3.3 3.3 3.2 5.6 2.4 6.3 22.7 2.3 19.9
Certified Labs Averagea 5.7 8.7 21.1 39.7 1.6 3.6 3.5 3.0 5.5 2.2 6.2 23.1 2.3 20.0AOCS Am 2-93 Avg. for Oilseeds 21.9 44.8 3.6
Sr 0.36 0.20 0.35 0.23 0.14 0.31 0.24 0.18 0.20 0.39 0.27 0.20 0.26 0.39
SR 0.54 0.31 0.63 0.68 0.27 0.42 0.42 0.20 0.28 0.50 0.30 0.20 0.36 0.48
RSDr, % 6.2 2.3 1.7 0.6 8.5 9.5 7.3 5.6 3.6 16.1 4.2 0.9 11.4 2.0
RSDR, % 9.4 3.5 3.0 1.7 16.3 12.7 12.6 6.1 5.0 20.7 4.7 0.9 15.7 2.4
r 0.99 0.56 0.98 0.65 0.39 0.88 0.68 0.51 0.56 1.08 0.75 0.56 0.72 1.09R 1.52 0.86 1.76 1.90 0.75 1.18 1.16 0.55 0.78 1.39 0.83 0.56 1.00 1.35
HORRAT 3.05 1.21 1.19 0.76 4.38 3.87 3.77 1.83 1.61 5.92 1.56 0.35 4.45 0.95
Sample ID dog
foo
d
cra
cker
s
turk
ey
ham
bee
f gr
ound
chi
cken
bre
ast
soy
bean
B
saf
flow
er
pot
ato
chip
s
hot
dog
sau
sage
cor
n B
che
ese
curl
s
cor
n si
lage
Number of laboratories 12 10 12 9 11 11 11 9 11 12 11 12 12 12Number of replicates 24 20 24 18 22 22 22 18 22 24 22 24 24 24
Filter Bag Average, % Crude Fat 6.8 23.8 3.2 11.6 23.8 2.8 19.4 22.5 32.0 39.5 25.7 3.4 30.6 2.3
Certified Labs Averagea 6.9 24.0 3.2 11.3 23.5 2.7 19.7 23.2 32.0 39.0 25.0 3.7 30.5 2.3AOCS Am 2-93 Avg. for Oilseeds 20.8 24.7
Sr 0.35 0.23 0.21 0.30 0.24 0.33 0.38 0.53 0.48 0.35 0.34 0.39 0.48 0.23
SR 0.35 0.23 0.34 0.30 0.36 0.33 0.62 0.83 0.52 0.59 0.51 0.41 0.69 0.51
RSDr, % 5.23 0.96 6.57 2.59 1.01 11.89 1.97 2.36 1.49 0.89 1.33 11.48 1.59 9.87
RSDR, % 5.23 0.96 10.84 2.59 1.49 11.89 3.19 3.69 1.61 1.49 1.98 11.93 2.27 22.45
r 0.99 0.64 0.58 0.84 0.67 0.94 1.07 1.49 1.34 0.98 0.96 1.10 1.36 0.63R 0.99 0.64 0.96 0.84 0.99 0.94 1.73 2.33 1.45 1.65 1.43 1.14 1.94 1.44
HORRAT 1.74 0.39 3.22 0.94 0.6 3.47 1.25 1.48 0.68 0.65 0.81 3.59 0.95 6.36
aAOCS Official Methods Ba 3-38, AOAC 920.39 or equivalent
Table 1. A summary of the statistical analysis of the international collaborative study of the Filter Bag Technique for the proposed Official AOCS Method, “Rapid Determination of Oil/Fat Utilizing High Temperature Solvent Extraction” is presented in this table. Included in the summary is a comparison of the Filter Bag Technique with the results of analysis by AOCS certified laboratories using official AOCS or AOAC methods
Operator’s Manual
Rev E 4/2/12 pg. 25
Appendix B – Parts & Assemblies
X84 – Extraction Vessel Assembly X87 – O‐ring Kit for Pet Ether X95 – O‐ring kit for High
Penetration Solvents
X86 – Teflon Insert Assembly with Wave Spring Bag Holder
983.7 – Wave Spring Bag Holder X96 – Thermister Assembly X99 – Level Sensor Assembly
X72 – Safety Valve Assembly X91 – Valve Plunger Assembly 5604 – Pressure Gauge
X89 – Splat Controller X90 – Splat Display 146.1 – Solvent Filter Element
Operator’s Manual
pg. 26 Rev E 4/2/12
X83 – Charcoal Filter X97 – Water Filter X98 – RFI Filter
206 – Fuse 10A 5578 – Fuse 5A X55 – Valve Kit for High Penetration Solvents
460 – 120V Relay 461 – 220V Relay 462 – 24V Relay
97 – 20A Relay 963 – Power Supply 5653 – On/Off Switch
Operator’s Manual
Rev E 4/2/12 pg. 27
24 – XT Burkert Valve 5/16” orifice 414 – 24V Burkert Valve 1/8” orifice Z132 – Valve Seals (1 per valve)
101.2 – Bag Holder X49 – Weigh Tin Desiccator X45 – Desiccant Pouch
5605 – Vent Flask SH – High Fat Check Sample SL – Low Fat Check Sample
TCH1 – Chiller Assembly 120V with Bypass and Alarm
TCH2 – Chiller Assembly 220V with Bypass and Alarm
X93 – By‐pass Assembly for Chiller
Operator’s Manual
pg. 28 Rev E 4/2/12
Appendix C – Electrical Diagram
Operator’s Manual
Rev E 4/2/12 pg. 29
Appendix C – Electrical Diagram (continued)
Operator’s Manual
pg. 30 Rev E 4/2/12
Appendix C – Electrical Diagram (continued)
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