background image

 

Operator’s

 

Manual

 

 

 

 

 

 

 

 

pg.

 

20

 

   

Rev

 

E

 

4/2/12

 

 

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 
(ANKOM

RD

 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 (S

r

, RSD

r

, 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 
(W

1

). 

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 (W

4

) 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 (W

2

). 

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 (W

3

). 

 

Calculations

 

Meat

 

samples

 ≤ 

15%

 

fat

 

and

 

plant

 

samples

 ≤ 

20%

 

fat

 

Meat

 

samples

 

>

 

15%

 

fat

 

and

 

plant

 

samples

 

>

 

20%

 

fat

 

%

 

Crude

 

Fat

 

=

 

100

 

x

 

(W

2

 

 

W

3

)

   

%

 

Crude

 

Fat

 

=

 

100

 

x

 

((W

2

 

 

W4)

 ‐ 

W

3

)

 

 

 

 

W

1

 

 

 

 

 

W

1

 

 

Where:

 

W

1

 

=

 

Original

 

weight

 

of

 

sample

 

Where:

 

W

4

 

=

 

Weight

 

of

 

the

 

weigh

 

tin

 

 

W

2

 

=

 

Weight

 

of

 

pre

dried

 

sample

 

with

 

filter

 

bag

 

 

 

 

 

W

3

 

=

 

Weight

 

of

 

dry

 

sample

 

with

 

filter

 

bag

 

after

 

extraction

 

 

 

 

 

 

 
 
 

Summary of Contents for XT10

Page 1: ...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 ...

Page 2: ...This page intentionally left blank ...

Page 3: ...tact Information 6 Instrument Description 7 Safety Precautions 8 Instrument Installation 9 Fat Extraction Process 10 Periodic Maintenance 17 Troubleshooting 19 Appendix A AOCS Official Fat Extraction Procedure 20 Appendix B Parts Assemblies 22 Appendix C Electrical Diagram pg 1 of 3 25 ...

Page 4: ...This page intentionally left blank ...

Page 5: ...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 da...

Page 6: ...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 service ankom com www ankom com ...

Page 7: ...rmit 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 ANKOMXT10 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 t...

Page 8: ...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...

Page 9: ...ument either in a Vent Hood or within 6 ft of one Because the ANKOMXT10 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 loca...

Page 10: ...e 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 readou...

Page 11: ...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 ...

Page 12: ...illing 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...

Page 13: ...d 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...

Page 14: ...in 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 ...

Page 15: ...ation 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 wi...

Page 16: ... 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...

Page 17: ...l 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 recove...

Page 18: ...es To replace the fuses in the ANKOMXT10 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...

Page 19: ...g 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 ...

Page 20: ...afe 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 balan...

Page 21: ...0 72 1 09 R 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 food crackers turkey ham beef ground chicken breast soybean B safflower potato chips hot dog sausage corn B cheese curls corn silage Number of laboratories 12 10 12 9 11 11 11 9 11 12 11 12 12 12 Number of replicates 24 20 24 1...

Page 22: ...5 O ring kit for High Penetration Solvents X86 Teflon Insert Assembly with Wave Spring Bag Holder 983 7 Wave Spring Bag Holder X88 Splat Controller X90 Splat Display X72 Safety Valve Assembly X73 Valve Kit for High Penetration Solvents X91 Valve Plunger Assembly 5604 Pressure Gauge 146 1 Solvent Filter Element X97 Water Filter ...

Page 23: ...X98 RFI Filter 206 Fuse 10A 5578 Fuse 5A X96 Thermister Assembly 460 120V Relay 461 220V Relay 97 20A Relay 963 Power Supply 5653 On Off Switch 24 XT Burkert Valve 5 16 orifice 414 24V Burkert Valve 1 8 orifice Z132 Valve Seals 1 per valve ...

Page 24: ... 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 ...

Page 25: ...Operator s Manual Rev E 4 2 12 pg 25 Appendix C Electrical Diagram pg 1 of 3 ...

Page 26: ...Operator s Manual pg 26 Rev E 4 2 12 Appendix C Electrical Diagram pg 2 of 3 ...

Page 27: ...Operator s Manual Rev E 4 2 12 pg 27 Appendix C Electrical Diagram pg 3 of 3 ...

Page 28: ...hod AOCS Am 5 04 Fully automatic Solvent recovery at 97 or greater Batch process up to 15 samples at one time RF Gas Production System High sensitivity pressure measurement Applications include Ruminant Nutrition Human Digestion Yeast Activity Beer Wine Fermentation Biomass to Energy analysis e g Ethanol Biodegradability Soil respiration BOD etc Wireless Computer control and data storage Chemicals...

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