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GB/T 24304-2009 PDF in English

GB/T 24304-2009 (GB/T24304-2009, GBT 24304-2009, GBT24304-2009)
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GB/T 24304-2009: PDF in English (GBT 24304-2009)

GB/T 24304-2009
Animal and vegetable fats and oils.Determination of anisidine value
ICS 67.200.10
National Standards of People's Republic of China
GB/T 24403-2009/ISO 6885..2006
Animal and vegetable fats and oils--Determination of anisidine value
(ISO 6885..2006, IDT)
Released in.2009-2009--30
2010--01-01 implementation
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
Published by China National Standardization Administration
This standard uses ISO 6885..2006 "Determination of anisidine value of animal and vegetable fats" (English version).
For ease of use, this standard has made the following editorial changes to ISO 6885..2006.
--- Delete the foreword of international standards;
--- Change "this international standard" to "this standard";
--- Replace the comma "," as the decimal point in the original text with the decimal point ".";
--- Numbered the formula.
Appendix A of this standard is an informative appendix.
This standard is proposed by the State Grain Administration.
This standard is under the jurisdiction of the National Grain and Oil Standardization Technical Committee.
This standard was drafted. National Academy of Grain Science Research Institute, Hangzhou Quality and Technical Supervision and Testing Institute, Zhengzhou Ocean Oil Engineering Technology
Co., Ltd., Zhengzhou Liangyuan Technology Co., Ltd.
The main drafters of this standard. Luan Xia, Xue Yalin, Jiang He, Wang Yingyao, Hu Hangping, Li Puxuan, Feng Rendong.
GB/T 24403-2009/ISO 6885..2006
Animal and vegetable fats and oils--Determination of anisidine value
1 Scope
This standard specifies the method for determining the anisidine value of animal and vegetable fats and oils.
This standard applies to the determination of aldehydes (mainly α, β-unsaturated aldehydes) in animal and vegetable fats and oils.
2 Normative references
The clauses in the following documents have become the clauses of this standard after being referenced. For dated references, all subsequent documents
The amendments (excluding the content of errata) or revisions are not applicable to this standard, however, all parties that have reached an agreement in accordance with this standard are encouraged to study
Is the latest version of these files available? For undated references, the latest version applies to this standard.
Samples of GB/T 5524 animal and vegetable fats and oils (GB/T 5524-2008, ISO 5555..2001, IDT)
GB/T 6682 Analytical laboratory water specifications and test methods (GB/T 6682-2008, ISO 3696. 1987, MOD)
Preparation of GB/T 15687 samples of animal and vegetable fats and oils (GB/T 15687-2008, ISO 661..2003, IDT)
3 Terms and definitions
The following terms and definitions apply to this standard.
Value, the value after 100 times expansion.
Note. Anisidine value has no unit, but the value measured by dissolving 1g sample in 100mL of solvent and reaction reagent is 1 unit of measure.
4 Principle
Absorbance, calculate anisidine value.
5 Reagents
Unless otherwise specified, the reagents used in this standard are of analytical grade. The experimental water shall meet the requirements of Grade III water in GB/T 6682.
5.1 Anhydrous sodium sulfate (Na2SO4).
5.2 Isooctane (2, 2, 4-trimethylpentane). in the wavelength range of 300nm to 380nm, the absorbance measured with water as a reference does not exceed
And filtered with medium speed filter paper to obtain a clear filtrate. The filtrate was cooled to 0 ° C and kept at this temperature for at least 4 h. Preferably in a vacuum
The crystals were filtered off and washed with a small amount of distilled water at 0 ° C. Dry in a vacuum dryer.
5.4 Glacial acetic acid. The mass fraction of water content is not more than 0.1%.
GB/T 24403-2009/ISO 6885..2006
5.5 Anisidine reagents. Considering the toxicity and instability of anisidine, only the minimum amount of reagents required for the day's analysis was prepared. For example, you can press
Avoid direct light.
Before use, check absorbance with isooctane as a blank control. If the absorbance rises above 0.2, the reagent cannot be used. in
In any case, the reagent is for the day only.
6 Instruments
General laboratory equipment, especially the following equipment.
6.1 Spectrophotometer. suitable for use in the 350nm wavelength range, with a 10mm cuvette.
For dual-beam spectrophotometry, it is recommended to use a pair of matched 10mm cuvettes.
6.2 Volumetric flask. 25mL.
6.3 Stoppered test tube. 10mL.
6.4 Pipette. 1mL and 5mL.
扦 sample
This is not the content of this standard, GB/T 5254 is recommended.
The samples received by the laboratory should be representative and not damaged or deteriorated during transportation or storage.
8 Preparation of test specimens
Prepare the sample according to GB/T 15687.
If the mass fraction of the sample water content is greater than 0.1%, use the following method to dry.
Anhydrous sodium sulfate is added at a ratio of 1g to 2g per 10g, and the sample is thoroughly mixed. If the sample is solid fat, the melting temperature
It should not be higher than 10 ° C of the melting point. Stir well and filter, keeping this temperature to prevent solidification. Because the presence of water can affect the reaction balance,
Moisture higher than 0.1% should be removed during sample preparation.
9 Operation steps
9.1 Preparation of test solution
Weigh an appropriate amount of sample (Chapter 8), accurate to 1 mg, and directly load it into a 25 mL volumetric flask. Preheat the solid sample to its melting point
Above, but not exceeding 10 ° C of melting point. Dissolve in 5 to 10 mL of isooctane (5.2) and dilute to the mark with the same solvent.
Note. The sampling volume is determined by the nature of the sample and the spectrophotometer used. The sampling volume is generally 0.4g to 4g, and the absorbance of the sample cannot be read by the instrument.
The upper and lower limits of the number.
9.2 Determination of unreacted solution
Pipette 5 mL of test solution (9.1) into a test tube (6.3) with a stopper (6.4), and add 1 mL of glacial acetic acid with a pipette (6.4).
(5.4) Solution, cap and shake well. Place in a dark place for 8 min at 23 ° C ± 3 ° C.
Transfer the solution to a clean, dry spectrophotometer cuvette within 2 min. Timing from the addition of glacial acetic acid solution, reaction time
A total of 10 min ± 1 min, then the absorbance was measured according to 9.5.
9.3 Determination of reaction solution
Pipette 5 mL of test solution (9.1) into a test tube (6.3) with a pipette (6.4) and add 1 mL of anisidine reagent with a pipette (6.4)
(5.5), cover the stopper and shake it fully. Place in a dark place for 8 min at 23 ° C ± 3 ° C.
Transfer the solution to a clean, dry spectrophotometer cuvette within 2 min. Timing from the addition of anisidine reagent, reaction time
A total of 10 min ± 1 min, then the absorbance was measured according to 9.5.
9.4 Determination of blank solution
Pipette 5mL of isooctane (5.2) into a test tube (6.3) with a pipette (6.4), and add 1mL of anisidine reagent with a pipette (6.4)
GB/T 24403-2009/ISO 6885..2006
(5.5), cover the stopper and shake it fully. Place in a dark place for 8 min at 23 ° C ± 3 ° C.
Transfer the solution to a clean, dry spectrophotometer cuvette within 2 min. Timing from the addition of anisidine reagent, total reaction time
Count 10min ± 1min, and then measure the absorbance according to 9.5.
9.5 Determination of absorbance with a spectrophotometer
Use isooctane (5.2) to calibrate the zero point of the spectrophotometer at 350 nm. Using isooctane as a control, determine the absorbance of the following solutions.
--- A1. reaction solution (9.3);
--- A0. unreacted solution (9.2);
--- A2. Blank solution (9.4).
9.6 Absorbance range
If the absorbance of A1 in the reaction solution (9.3) is not in the range of 0.2 to 0.8, it is necessary to adjust the sample sampling amount and re-measure
Elamine reagent was re-measured.
10 results
10.1 Calculate the anisidine value (A 犞) according to formula (1).
[1.2 × (A1-A2-A0)] (1)
In the formula.
犞 --- the volume of the dissolved sample, in milliliters (mL), 犞 = 25mL;
Q --- According to the definition of anisidine value, Q is the concentration of the sample in the measurement solution, the unit is gram per milliliter (g/mL), Q = 0.01 g/mL;
A0 --- absorbance of unreacted test solution (9.2);
A1 --- absorbance of reaction solution (9.3);
A2 --- absorbance of blank solution (9.4);
1.2 --- Dilute the correction factor of the test solution with 1 mL of anisidine reagent or glacial acetic acid solution.
The result remains one decimal place.
10.2 The total oxidation number is useful for evaluating the oxidative deterioration of a fat. Calculate the total oxidation value (T 犞) according to formula (2).
T 犞 = (4 × P 犞) + A 犞 (2)
In the formula.
P 犞 --- the peroxide value of the sample, the unit is millimoles per kilogram (mmol/kg);
A 犞 --- Anisidine value of the sample.
11 precision
11.1 Interlaboratory test results
Appendix A summarizes the interlaboratory testing of the precision of this method. These test results may not apply to other ranges and tests
11.2 Repeatability
In the same laboratory, the same operator uses the same equipment, uses the same test method, and measures the same object in a short time.
Over 5%.
11.3 Reproducibility
In different laboratories, different operators use different equipment and use the same test method to independently test the same object.
GB/T 24403-2009/ISO 6885..2006
In cases where the absolute difference between the two independent test results obtained by the tests is greater than the reproducibility limit (R) given in Table 1, it should not exceed 5%.
A 犞 (average of two determinations) 0 to 100.034A + 0.31 0.19A + 1.41
12 test report
The test report should state.
--- All relevant information of the sample;
--- If the sampling method is known, indicate;
--- Standard methods and literature cited in this standard;
--- details not specified or selected in this standard, and all operational details that may affect the results;
---Test Results;
--- If a repeatability test is performed, the final result is provided.
GB/T 24403-2009/ISO 6885..2006
Appendix A
(Informative appendix)
Interlaboratory test results
French ITERG completed the latest international-level laboratory test comparison in.2004. Nine countries (Argentina, Canada,
France, Germany, Hungary, the Netherlands, Portugal, the United Kingdom, and the United States) 18 laboratories participated in this test, and one sample was measured twice. Statistics
The results (calculated according to ISO 5725-2 statistics) are shown in Table A. 1.
Table A. 1 Inter-laboratory test results
Sample soybean oil, rapeseed oil, walnut oil, fish oil, fish oil, poultry oil, anhydrous cream
Frying oil
After removing outliers
Number of laboratories
16 17 17 16 16 17 15 15 14 16
Average 3.46 0.95 6.86 25.46 31.54 4.59 0.333 96.80
Repeatability coefficient of variation /% 2.6 8.2 2.5 1.2 2.3 2.3 6.0 19.9 1.3
0.225 0.22 0.48 0.86 2.02 0.78 0.19 3.43
Reproducible standard deviation, 狊 R 0.27 0.39 0.52 1.75 3.79 1.79 1.80 6.17
Reproducibility coefficient of variation /% 7.9 41.4 7.6 6.9 12.9 39.3 49.5 7.0
Reproducibility limit, R
(2.8 × 狊 R)
0.77 1.10 1.46 4.89 10.61 5.05 0.54 0.58 8.86
GB/T 24403-2009/ISO 6885..2006
[1] ISO 5555. Animatedvegetableslabs-following-Sampling.
[2] ISO 5725-1. Accuracy (truensesandprecipion) ofmeanssurgentsmeanshodsandresults-Part 1. Gen-
[3] ISO 5725-2. Accuracy (truensesandprecipion) ofmesurancemeetingmeanshodsandresults-part 2. Basic
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GB/T 24403-2009/ISO 6885..2006
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.