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Animal and vegetable fats and oils -- Preparation of methyl esters of fatty acids
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GB/T 17376-2008: PDF in English (GBT 17376-2008) GB/T 17376-2008
Animal and vegetable fats and oils - Preparation of methyl esters of fatty acids
ICS 67.200.10
X14
National Standards of People's Republic of China
GB/T 17376-2008/ISO 5509.2000
Replacing GB/T 17376-1998
Animal and vegetable fats fatty acid methyl esters prepared
(ISO 5509.2000, IDT)
Posted 2008-11-04
2009-01-20 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Foreword
This standard is equivalent to ISO 5509 Implementation.2000, "Animal and vegetable fats fatty acid methyl esters prepared" (in English).
For ease of use, the standard ISO 5509.2000 includes the following editorial changes.
--- Delete foreword international standards;
--- "This International Standard" be replaced by "this standard";
--- With a decimal point "." Instead of a comma as the decimal point "."
This standard is GB/T 17376-1998 "Animal and vegetable fats fatty acid methyl esters prepared" amendments.
This standard and GB/T 17376-1998 main differences are as follows.
--- With iso-octane (HPLC grade) in place of heptane reagent;
--- With trimethyl hydrogen sulfur (TMSH) method instead of the original standard of "no alternative to boron trifluoride";
--- Transesterification method instead of the original standard "four carbon or special preparation of four or more carbon fatty acid methyl ester";
--- The sixth chapter of the methods commonly used to analyze some of the main program and the original standards in Appendix A;
--- Increase the informative Appendix B.
Since the implementation of this standard replaces GB/T 17376-1998.
Appendix A of this standard is a normative appendix, Appendix B is an informative annex.
The standard proposed by the National Food Authority.
This standard by the National Standardization Technical Committee OILS.
This standard is drafted by. National Grain Reserve Xi'an Oil Research and Design Institute.
Involved in the drafting of this standard. Shaanxi Province Product Quality Supervision, Inspection, Anhui Daping Trade and Industry (Group) Co., Ltd.
Drafters of this standard. Meng Orange, Xiatian Wen, Chen Yong, WANG Hui-fang, xin ', Ren Chunming.
This standard replaces the standards previously issued as follows.
--- GB/T 17376-1998.
GB/T 17376-2008/ISO 5509.2000
Animal and vegetable fats fatty acid methyl esters prepared
1 Scope
This standard specifies a method for preparing the fatty acid methyl ester.
This standard covers from animal fats, fatty acids and fatty acid salts of fatty acid methyl ester preparation method. It defines three methyl ester
method.
a) boron trifluoride Act (see Chapter 3);
b) trimethyl hydrogen sulfur Act (see Chapter 4);
c) transesterification method (see Chapter 5).
This standard applies to gas chromatography, thin layer chromatography, infrared spectroscopy and other analysis required ester derivative.
2 Normative references
The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent
Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research
Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard.
GB/T 6682 analytical laboratory use specifications and test methods (GB/T 6682-2008, ISO 3696.2008, MOD)
GB/T 15687 animal and plant oils prepared sample (GB/T 15687-2008, ISO 661.2003, IDT)
3 boron trifluoride method (conventional method)
Warning. The method involves the use of hazardous reagents. Should take appropriate precautions to protect your eyes and avoid corrosive chemicals
Danger of burns. Boron trifluoride toxic, analysts recommend possible without methanol and boron trifluoride preparing methanol solution of boron trifluoride (see Appendix A
First A. Chapter 1).
3.1 Principle
Saponification glycerides, fatty acid salts, the resulting solution is reacted with boron trifluoride in methanol to methyl ester in methanol solution of sodium hydroxide. If you want to
AR fatty acids and fatty acid salts, you do not need saponification directly with boron trifluoride methyl esterification reaction.
3.2 Scope
This method is applicable to most oil and derivatives (fatty acids, fatty acid salts), does not apply creams and compounds containing the following groups.
--- Ci oxy compound (example. a ketone group, an epoxy group, a hydroxyl group, a hydroperoxy group);
--- Cyclopropane and cyclopropyl compound;
--- Acetylenic fatty acids.
If the oil contains only small amounts of these compounds (such as cottonseed oil), still the general method of Chapter 3 by esterification. Otherwise it will be taken
The method described in Chapter 4 or Chapter 5 used.
Gas chromatographic analysis using isooctane as solvent methyl ester obtained the highest recovery, but the recovery has only methyl
75%.
3.3 Reagents
Unless otherwise stated, only recognized as analytical reagents.
3.3.1 Water. should be consistent with GB/T 6682 water requirements of level 3.
3.3.2 Sodium hydroxide in methanol solution. about 0.5mol/L.
2g of sodium hydroxide dissolved in 100mL water is not more than 0.5% methanol. When the solution was stored for a long time, it may form less
Quantity of white precipitate of sodium carbonate, but do not affect the preparation of the methyl ester.
GB/T 17376-2008/ISO 5509.2000
Methanol solution of boron trifluoride 3.3.3. mass fraction of 12% to 15% 1) (see Appendix A of Section A.1 chapter).
1) Optional 14%, 20%, (MerckNO.8.01663) and 50% commercial agent, this information is only for the convenience of users of this standard, and not
An endorsement of these products.
3.3.4 iso-octane (2,2,4-trimethyl pentane). chromatography (see Appendix A, Section A.2).
Warning. isooctane flammable, explosive limit in air is 1.1% to 6.0% (volume fraction). Isooctane toxic, not eating
Or inhaled, the operation should be carried out in a fume hood.
3.3.5 Sodium chloride. saturated aqueous solution.
3.3.6 over anhydrous sodium sulfate.
3.3.7 nitrogen. oxygen content less than 5mg/kg.
3.3.8 hexane. chromatographically pure, only for the preparation of esters dry. Can also be used with petroleum ether. boiling range 40 ℃ ~ 60 ℃, bromine value less than 1, no residue (see Appendix
Section A. A's Chapter 2).
3.3.9 Methyl red. 1g/L, dissolved in a volume fraction of 60% ethanol.
3.4 Instrument
Usual laboratory equipment, and the following instruments.
3.4.1 ground-necked flask. 50mL or 100mL, with stopper.
3.4.2 reflux condenser. effective length of 200mm ~ 300mm, has a ground-necked flask (3.4.1) with the ground joint.
3.4.3 zeolite. degreasing.
3.4.4 pipette or automatic dispenser. at least 10mL.
3.4.5 Glass. a screw cap, capacity of at least 4mL.
3.4.6 separating funnel. 250mL, for the preparation of dry resin.
3.4.7 rotary evaporator.
3.4.8 Analytical Balance. Indexing is 0.001g.
3.5 Sample Preparation
The sample should be dry and liquid, transparent, according to GB/T 15687 samples were prepared. For heating of the sample, is used just above the melting point
temperature.
3.6 Procedure
Warning. toxic boron trifluoride, the following actions need to be in a fume hood, glassware after use, wash with water immediately.
3.6.1 Sample
Depending on the amount of sample required sample, according to Table 1 to select a suitable flask and the amount of reagents and solutions.
Table 1 Sample Weigh amount
Analytical method
Sample Quality /
mg
Flask
(3.4.1) /
mL
Sodium hydroxide in methanol
Solution
(3.3.2) /
mL
Boron trifluoride methanol
Solution
(3.3.3) /
mL
Solvent
(3.3.4) or
(3.3.8) /
mL
GLC
(GLC)
100 ~ 25050451 ~ 3
250 ~ 50050672 ~ 5
IR/T LC
(FTIR /
TLC)
500 ~ 750,100,894 ~ 8
~ 750 ~ 100010010127 10
3.6.2 saponification
3.6.2.1 3.6.2.2 started from grease, fatty acids and fatty acid salts from 3.6.2.3 to begin.
3.6.2.2 The sample was placed in a suitable flask (see Table 1 and Appendix A), adding an appropriate amount (see Table 1) sodium hydroxide in methanol (3.3.2)
GB/T 17376-2008/ISO 5509.2000
And zeolite (3.4.3), and then connected to the condenser (3.4.2).
If two or more double bonds in the presence of fatty acids, prior to reflow, a few quick dry nitrogen introduced into the flask (3.3.7) Air
Drain.
Reflux in a water bath until the oil droplets disappear, ~ 60s every 30s slow shake flask, in order to prevent the formation of solid sodium hydroxide attached to the wall of the bottle
on. Reflow process usually takes 5min ~ 10min, some cases may be longer (see Appendix A A.3 Chapter Chapter A.4). With shift
Methanol solution was added an appropriate amount from the top of the condenser tubes (see Table 1) of boron trifluoride (3.3.3) in solution in boiling.
The next step to perform in accordance with 3.6.3 or 3.6.4.
3.6.2.3 The sample is placed in a methanol solution of boron trifluoride suitable flask (see Table 1), adding an appropriate amount (see Table 1), (3.3.3), then take
Condenser (3.4.2).
The next step to perform in accordance with 3.6.3 or 3.6.4.
3.6.3 Preparation of methyl ester (mainly for GLC analysis)
3.6.3.1 continue to boil 3min. For oils containing long chain fatty acids, such as fish oil, continue to boil 30min.
3.6.3.2 From the top of the condenser was added an appropriate amount of iso-octane (3.3.4) in a mixed solution of boiling inside.
3.6.3.3 Remove the condenser, out of the flask. Join 20mL sodium chloride solution (3.3.5). Stoppered flask, shaking violently at least
15s.
3.6.3.4 continue to add sodium chloride solution (3.3.5) to the neck of the flask rested stratification.
3.6.3.5 draw 1mL ~ 2mL top iso-octane solution in a glass bottle (3.4.5), by adding an appropriate amount of anhydrous sodium sulfate (3.3.6) to remove dissolved
Traces of water in the liquid, and injected into the gas chromatograph in the following ways.
a) directly into the packed column (see Section A.5 of Appendix A);
b) first and then diluted with isooctane modest injection capillary column (see Appendix A of Chapter A.6 chapter);
c) For capillary columns, special circumstances may use lower boiling heptane dilution.
3.6.4 dry methyl ester (used for thin layer chromatography or infrared spectroscopy)
3.6.4.1 continue to boil 3min.
3.6.4.2 From the top of the condenser was added an appropriate amount of hexane (3.3.8) in a mixed solution of boiling inside.
3.6.4.3 Remove the condenser, out of the flask. Join 20mL sodium chloride solution (3.3.5). Stoppered flask, shaking violently at least
15s.
3.6.4.4 The mixed solution was transferred to a separatory funnel and 250mL (3.4.6). Add approximately 30mL saturated sodium chloride solution, standing stratified
Reserved hexane. Sodium chloride solution and then discharged 50mL hexane (3.3.8) twice.
3.6.4.5 The hexane extracts were combined and twice, then with 20mL of distilled water (3.3.1) and washed until the reagent with methyl red
(3.3.9) until the test is not acidic. Dried over anhydrous sodium sulfate (3.3.6) dried, filtered, treated with a stream of nitrogen in a water bath (3.3.7) or by using a rotary evaporation
Hair meter (3.4.7) the solvent was evaporated.
Part of short chain ester (C6 ~ C10) ester prepared in a dry process will be lost, less than 500mg of sample, preferably proportionally reduced sodium chloride
Liquid, solvent and distilled water volume, see Appendix A of Section A. 6.
4-trimethyl-hydrogen sulfur (TMSH) method
Warning. The method involves the use of hazardous reagents. Should take appropriate precautions to protect your eyes and avoid corrosive chemicals
Danger of burns. Trimethylhydroquinone toxic methanol solution of sulfur trioxide.
4.1 Principle
The sample was dissolved in methyl tert-butyl ether, with the methanol solution of hydrogen sulfur trioxide trimethyl ester Swapping methyl ester. Samples were analyzed
When the temperature is higher than the gasification chamber 250 ℃. If the sample contains short chain fatty acids while (C4 ~ C8), recommended the use of methyl valerate as an internal standard
(See 4.2).
4.2 Scope
This method applies only to rapid ester prepared by gas chromatography analysis of the methyl ester. This method is applicable to all oils, including milk fat and containing
GB/T 17376-2008/ISO 5509.2000
There are creamy mixture, they found no isomerization of unsaturated fatty acids.
The method is also applicable to a substance containing chemical groups listed in 3.2, but not entirely sure whether the methyl ester, free fatty acids only
70% to 80% of methyl ester.
Hydroxyl group-containing lipids partially form the corresponding o-methyl ether derivative, which may interfere with the separation of the methyl ester of GLC. Therefore, if
Samples containing more hydroxyl groups, the method is not suitable, available GC-MS analysis.
Gas-liquid chromatography, column temperature low, the method is not applicable. In addition, the method does not recommend the use of a polar stationary phase.
Analyzing the short chain fatty acids (C4 ~ C8), if recommended that no large pentanoic acid methyl ester as an internal standard.
4.3 Reagents
All reagents were of analytical grade.
4.3.1 methyl tert-butyl ether.
4.3.2 methanol solution of hydrogen sulfur trioxide trimethyl 2). 0.2mol/L. 4 ℃, this solution can be stored in a sealed tube for 2 months or more.
NOTE. If homemade preparation method see reference [3].
2) hydrogen sulfur trioxide trimethyl only by Macherey-NagelGmbH purchase, provide this information for the convenience of users of this standard, rather than
Approval of these products.
4.3.3 internal standard stock solution. Only for butyric acid or aminocaproic acid assay. Weigh approximately 250mg (accurate to 0.1mg) pentanoate in 50mL capacity
Flask with iso-octane dissolved and diluted to the mark.
4.3.4 internal standard reference solution. Only for butyric acid or aminocaproic acid assay. Take 10mL stock solution (4.3.3) in 100mL flask, with iso-octane
Dilute to the mark. Calculate the concentration (see Appendix A of Chapter A.8).
4.3.5 petroleum ether.
4.3.6 over anhydrous sodium sulfate.
4.4 Instrument
Usual laboratory equipment, and the following instruments.
4.4.1 tube. 2mL, with ground glass stopper or screw-autosampler vials.
4.4.2 pipette. 1000μL.
4.4.3 flask. 50mL and 100mL.
4.4.4 filter paper.
4.4.5 rotary evaporator.
4.5 Sample Preparation
The sample should be dry and liquid, transparent, according to GB/T 15687 samples were prepared. For heating of the sample, is used just above the melting point
temperature.
4.6 Step
4.6.1 Sample
Weigh 10mg ± 2mg samples in test tubes (4.4.1) in. If the sample is a high water content, and increase sample weight. For solid samples,
At a temperature above about 10 ℃ heated to melt. Avoid high temperature heating. With petroleum ether (4.3.5) to dissolve the sample, anhydrous sulfur
Sodium (4.3.6) drying 30min, and then filtered with filter paper, the residue was washed with petroleum ether several times, using a rotary evaporator (4.4.5) recovering
Solvent.
4.6.2 methyl ester
4.6.2.1 pipette (4.4.2) Pipette 500μL of methyl tert-butyl ether was added to the sample to dissolve the sample, if necessary, gentle heating,
The determination of butyric acid or aminocaproic acid, the Pipette 500μL internal standard reference solution (4.3.4) in place of methyl tert-butyl ether.
4.6.2.2 pipette (4.4.2) sulfur was added 250μL of trimethylhydroquinone (TMSH) solution (4.3.2), shaken violently 30s (see Appendix
Section A. A's Chapter 7).
The resulting solution 4.6.2.3 (4.6.2.2 The) can be used for gas chromatographic analysis, the gasification chamber to a temperature of at least 250 ℃. (See Appendix A of the first
GB/T 17376-2008/ISO 5509.2000
A. Section A. 2 and Appendix A of Chapter 7). If dilution using methyl tert-butyl ether (4.3.1) and methanol mixture (9 + 1), in order to avoid
Sulfur-trimethylhydroquinone (TMSH) precipitated.
5 transesterification
Warning. The method involves the use of hazardous reagents. Should take appropriate precautions to protect your eyes and avoid corrosive chemicals
Danger of burns. Toxic potassium hydroxide solution.
5.1 Principle
The oil was dissolved in iso-octane, potassium hydroxide solution was added by the transesterification of methyl, after completion of the reaction with sodium bisulfite and residual
Potassium hydroxide, in order to avoid saponification of methyl ester.
5.2 range
This method is applicable to four carbon fast or four or more carbon atoms, free fatty acid (FFA) content of not more than 2% of edible oil, but also to use the
Superscript - Determination of acid or acid gas chromatography.
Samples as high free fatty acid content, should be used in excess of potassium hydroxide solution. Since free fatty acids and potassium salts being
Esterification, so this method can only be generated in the sample portion of methyl esters.
The method is also applicable to a substance containing chemical groups listed in 3.2, but not entirely sure whether the methyl ester.
5.3 Reagents
Unless otherwise specified, reagents were of analytical grade.
5.3.1 methanol solution of potassium hydroxide. about 2mol/L. The 13.1g of potassium hydroxide was dissolved in 100mL anhydrous methanol, gentle heating can be added
Anhydrous sodium sulfate, filtered, to obtain a clear solution. The solution was stored for some time, may form a small amount of precipitation, and the supernatant was measured not
Affect.
5.3.2 iso-octane (2,2,4-trimethyl pentane). chromatography, see Appendix A. A's 2.
5.3.3 sodium bisulfate.
5.3.4 internal standard stock solution. Only for butyric acid or aminocaproic acid assay. Weigh approximately 250mg (accurate to 0.1mg) pentanoate in 50mL capacity
Volumetric flask, dissolve and dilute to volume with isooctane (5.3.2).
5.3.5 internal standard reference solution. Only for butyric acid or aminocaproic acid assay. Take 10mL stock solution (5.3.4) in 100mL flask, with iso-octane
(5.3.2) diluted to the mark. Calculate the concentration (see Appendix A of Chapter A.8).
5.4 Instrument
5.4.1 tube. 5mL, with ground glass stopper.
5.4.2 pipette or pipette. 4mL.
5.4.3 micro pipette.200μL.
5.4.4 Glass. a screw cap, at least 4mL.
5.4.5 flask. 50mL and 100mL.
5.5 Sample Preparation
The sample should be dry and liquid, transparent, according to GB/T 15687 samples were prepared. For heating of the sample, is used just above the melting point
temperature.
Step 5.6
5.6.1 Sample
Weigh 60mg samples to a stoppered test tube (5.4.1), and for determination of butyric acid or aminocaproic acid, accurate to 0.1mg.
5.6.2 methyl ester
5.6.2.1 using a pipette or pipette (5.4.2) Pipette 4mL isooctane (5.3.2) to dissolve the sample, if necessary, slightly heating the specimen
Dissolved. Measured or butyric acid, with a pipette (5.4.2) Pipette 4mL internal standard reference solution (5.3.5) in place of iso-octane sample dissolution.
5.6.2.2 After using a micro pipette (5.4.3) was added 200μL methanol solution of potassium hydroxide (5.3.1), covered with a glass stopper violently shaken 30s
It was allowed to stand until clear.
GB/T 17376-2008/ISO 5509.2000
5.6.2.3 To the solution was added about 1g of sodium hydroxide (5.3.3), violent shaking, and potassium hydroxide.
5.6.2.4 until after salt precipitation, the upper layer containing the methyl ester solution was poured into 4mL glass bottle (5.4.4), and iso-octane solution obtained methyl ester
Content of about 15mg/mL, and injected into the gas chromatograph in the following ways.
a) direct a certain amount injected packed columns (see Appendix A of Chapter A.5 chapter);
b) first and then diluted with isooctane modest injection capillary column (see Appendix A of Chapter A.6 chapter);
c) For capillary columns, special circumstances may use lower boiling heptane dilution.
6 precision
Appendix B gives the international laboratory for three kinds of methyl ester method comparison test data, because during the preparation of methyl selected column
Optional, gas chromatography and gas chromatography equipment condition value for repeatability and reproducibility values affected, so the value of the repeatability and reproducibility values does not count
Calculated.
GB/T 17376-2008/ISO 5509.2000
Appendix A
(Normative)
The main analysis program
A. Preparation of a boron trifluoride
If boron trifluoride methanol solution must be prepared as follows.
WARNING. The operation carried out in a fume hood.
Was added methanol in 1L 2L flask Weigh mass was cooled in an ice-water bath. Holding the flask in an ice water bath, so that the cylinder
Boron trifluoride methanol solution introduced via a glass tube. To avoid the return of liquid to the gas system, before the glass tube immersed in a methanol solution to
Until removed, should pass boron trifluoride gas. Gas flow rate is not too large, it can not produce white smoke.
The reagent can be stored in the refrigerator for 2 years.
A. 2 Reagents
Various agents not to gas chromatographic analysis of fatty acid methyl ester peaks interference.
In methyl GC, some agents may have some unforeseen peaks in the spectrum. Especially after long-term storage, tris
Boron trifluoride methanol solution will generate some components on C20 ~ C22 fatty acid peak area.
Thus, each new batch of reagent or solvent should be prepared pure oleic acid methyl ester, and chromatography. If extra peaks occur, these reagents
It should be discarded.
A. 3 saponification
With castor oil, for example, the oil sample was dissolved in methanol, oil droplets will not be observed.
Therefore, the solution is clear or not, it can not serve as proof of completion of the reaction.
A. 4 unsaponifiables
Unsaponifiable matter is not removed, if it is to calculate the total amount of material, it may affect the results of the analysis. If this is the case,
It is necessary to operate in accordance with the method described below to be replenished.
Available saponification solution was diluted with distilled water, and with diethyl ether, hexane or petroleum ether extraction to remove unsaponifiables, and then acidified with iso-octane or
Hexane extract fatty acids. Preparation of methyl performed in 3.6.3 or 4.6.2.
A. Storage solution of methyl 5
Methyl ester prepared should be analyzed as soon as possible. It may be methyl ester in an inert gas stored in the refrigerator.
If the storage time is longer, it can add a certain concentration will not interfere with the analysis results of antioxidants to prevent the oxidation of methyl automatically, for example.
0.05g/L of 2,6-di-tert-butyl-p-cresol (BHT) solution.
As contained methyl butyrate, methyl, should be stored in a sealed ampoule, take certain precautions to avoid filling and sealing safety
Evaporation loss ampules process.
A. 6 methyl dry storage
Dry ester should be analyzed immediately. If necessary, you can save 24h under an inert gas in the refrigerator, in cold or in a vacuum sealed tube
Tibetan library stored longer.
A. 7-trimethyl-hydrogen sulfur (TMSH) method
Free fatty acid and sulfur trioxide trimethyl hydrogen to form the corresponding salt, is converted to decomposed in the gasification chamber and methyl dimethyl sulfide.
GB/T 17376-2008/ISO 5509.2000
To prevent clogging, split mouth diameter capillary column should be wider. Such as congestion, can be heated or flush it with solvent cleaning.
If valerate do internal standard can be used methyl tert-butyl ether (0.5mg/mL ~ 1.0mg/mL) was dissolved.
A. The amount of methyl ester 8
If the internal standard - quantitative determination of fatty acid gas liquid chromatography, mass must be accurately weighed sample (accurate to 0.1mg). The results will be
Oil fatty acid composition of fat mass fraction occupied, said the results from the internal standard which is owned by a method was obtained inconsistent.
GB/T 17376-2008/ISO 5509.2000
Appendix B
(Informative)
Joint Lab test results
1995 launched an international collaborative research. In this test, there are eight different laboratories involved in the determination of free fatty acids of 8 parts
sample. The purpose of this experiment was to determine methyl ester prepared three different methods for different species and free fatty acid content of the oil application
Sex. Table B. 1 to B. 8 shows the test results, including laboratories measured the minimum essential fatty acids, maximum, mean and standard
deviation.
Table B. A refined coconut oil (free fatty acid content 0.03%)
Boron trifluoride Act (7 laboratories)
FAME Minimum Maximum Average Standard deviation
C6.0 0.3 0.6 0.5 0.1
C8.0 5.6 7.8 6.7 0.7
C10.0 5.3 6.0 5.6 0.3
C12.0 46.0 47.6 46.8 0.3
C14.0 17.7 19.1 18.3 0.4
C16.0 9.0 9.7 9.4 0.3
C18.0 2.7 3.0 2.9 0.1
C18.1 7.4 7.9 7.7 0.2
C18.2 1.9 2.2 2.0 0.1
C20.0 0.1 0.1 0.1 0.0
C20.1 0.0 0.1 0.0 0.0
Total 104.0 100.0 96.1 2.8
Trimethyl hydrogen sulfur (TMSH) France (6 laboratories)
FAME Minimum Maximum Average Standard deviation
C6.0 0.5 0.7 0.6 0.1
C8.0 7.1 8.5 7.8 0.5
C10.0 5.6 6.3 6.0 0.2
C12.0 45.8 47.6 46.7 0.7
C14.0 16.4 17.9 17.4 0.5
C16.0 8.5 9.4 8.9 0.3
C18.0 2.5 3.2 2.8 0.2
C18.1 6.8 7.9 7.4 0.4
C18.2 1.6 2.6 2.1 0.3
C20.0 0.1 0.3 0.2 0.1
C20.1 0.0 0.5 0.1 0.2
Total 104.9 100.0 95.0 3.7
GB/T 17376-2008/ISO 5509.2000
Table B. 1 (cont.)
Transesterification (7 laboratories)
FAME Minimum Maximum Average Standard deviation
C6.0 0.5 0.7 0.6 0.1
C8.0 6.5 9.3 7.4 0.6
C10.0 5.4 7.1 5.9 0.3
C12.0 45.8 52.0 46.8 0.7
C14.0 16.7 18.6 18.0 0.4
C16.0 6.6 9.5 9.1 0.3
C18.0 1.7 3.0 2.8 0.2
C18.1 4.7 8.0 7.5 0.3
C18.2 1.1 2.2 1.9 0.1
C20.0 0.0 0.1 0.1 0.0
C20.1 0.0 0.1 0.0 0.0
Total 110.7 100.0 89.1 3.1
Table B. 2 refined soybean oil (the free fatty acid content of 0.06%)
Boron trifluoride Act (7 laboratories)
FAME Minimum Maximum Average Standard deviation
C14.0 0.0 0.1 0.0 0.0
C16.0 10.4 11.0 10.6 0.2
C16.1 0.0 0.1 0.1 0.0
C17.0 0.1 0.2 0.1 0.0
C18.0 3.6 3.9 3.7 0.1
C18.1 20.7 21.0 20.9 0.1
C18.2 54.5 55.7 55.2 0.4
C18.3 7.9 9.0 8.4 0.4
C20.0 0.3 0.5 0.4 0.1
C20.1 0.2 0.3 0.2 0.1
C22.0 0.3 0.4 0.4 0.0
C24.0 0.0 0.2 0.1 0.1
Total 102.4 100.0 98.0 1.6
Trimethyl hydrogen sulfur (TMSH) France (6 laboratories)
FAME Minimum Maximum Average Standard deviation
C14.0 0.0 0.2 0.1 0.1
C16.0 10.5 11.3 10.7 0.3
C16.1 0.0 0.1 0.1 0.1
C17.0 0.0 0.2 0.1 0.1
GB/T 17376-2008/ISO 5509.2000
Table B. 2 (cont.)
Trimethyl hydrogen sulfur (TMSH) France (6 laboratories)
FAME Minimum Maximum Average Standard deviation
C18.0 3.6 3.8 3.7 0.1
C18.1 20.6 22.5 21.2 0.7
C18.2 53.4 55.7 54.8 0.9
C18.3 7.7 9.0 8.3 0.4
C20.0 0.3 0.6 0.4 0.1
C20.1 0.1 0.7 0.3 0.2
C22.0 0.3 0.5 0......
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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