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GB/T 5534-2024 PDF English

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GB/T 5534-2024: Animal and vegetable fats and oils - Determination of saponification value
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GB/T 5534: Evolution and historical versions

Standard IDContents [version]USDSTEP2[PDF] deliveryName of Chinese StandardStatus
GB/T 5534-2024English275 Add to Cart 0-9 seconds. Auto-delivery Animal and vegetable fats and oils - Determination of saponification value Valid
GB/T 5534-2008English160 Add to Cart 0-9 seconds. Auto-delivery Animal and vegetable fats and oils -- Determination of saponification value Valid
GB/T 5534-1995English199 Add to Cart 3 days Animal and vegetable oils and fats--Determination of saponification value Obsolete
GB 5534-1985English199 Add to Cart 2 days Inspection of vegetable oils--Methods for determination of saponification value Obsolete

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GB/T 5534-2024: Animal and vegetable fats and oils - Determination of saponification value

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GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 67.040 CCS X 04 GB/T 5534-2024 / ISO 3657.2023 Replacing GB/T 5534-2008 Animal and Vegetable Fats and Oils – Determination of Saponification Value (ISO 3657.2023, IDT) Issued on: OCTOBER 26, 2024 Implemented on: MAY 1, 2025 Issued by. State Administration for Market Regulation; Standardization Administration of the People’s Republic of China.

Table of Contents

Foreword... 3 1 Scope... 4 2 Normative References... 4 3 Terms and Definitions... 4 4 Principle... 5 5 Reagents... 5 6 Instruments and Equipment... 6 7 Sampling... 6 8 Preparation of Specimen... 6 9 Operating Procedure... 6 10 Calculation of Results... 7 11 Precision... 8 12 Test Report... 8 Appendix A (Informative) Interlaboratory Test Results... 9 Appendix B (Informative) Calculation of Saponification Values from Fatty Acid Composition Data... 10 Bibliography... 14

Foreword

This Document was drafted as per the rules specified in GB/T 1.1-2020 Directives for Standardization – Part 1.Rules for the Structure and Drafting of Standardizing Documents. This Document replaced GB/T 5534-2008 Animal and Vegetable Fats and Oils - Determination of Saponification Value. Compared with GB/T 5534-2008, the major technical changes of this Document are as follows besides the structural adjustments and editorial modifications. --- Add the ethanol concentration, and make accurate concentration of potassium hydroxide- ethanol solution (see 5.1, 5.2 of this Edition; 5.1 of the 2008 Edition); --- Add the specifications of the analytical balance and the weighing accuracy of the samples (see 6.6 of this Edition; 6.6 of the 2008 Edition). This Document equivalently adopted ISO 3657.2023 Animal and Vegetable Fats and Oils - Determination of Saponification Value. Please note some contents of this Document may involve patents. The issuing agency of this Document shall not assume the responsibility to identify these patents. This Document was proposed by National Food and Strategic Reserves Administration. This Document shall be under the jurisdiction of National Technical Committee on Grains and Oils of Standardization Administration of China (SAC/TC 270). Drafting organizations of this Document. Wuhan Polytechnic University; COFCO Yellowsea Oils and Grains Industries (Shandong) Co., Ltd.; Shenzhen Academy of Metrology & Quality Inspection; Wuhan Institute for Food and Cosmetic Control; COFCO Fortune Food Sales & Distribution Co., Ltd.; and Wuhan Institute of Standardization. Chief drafting staffs of this Document. Zhou Li, Gao Pan, Wang Jie, Liu Peilian, Jiang Xiaoming, Yu Lei, Huang Qing, and Zhang Sihong. The historical editions replaced by this Document are as follows. --- GB/T 5534-1995 was first-time published in 1995; first-time revised in 2008; --- It is second-time revised hereby. Animal and Vegetable Fats and Oils – Determination of Saponification Value

1 Scope

This Document describes the method for determining the saponification value of animal and vegetable fats and oils. The saponification value is an indicator of determining the content of free fatty acids and glycerides in oils or fatty acids. This Document applies to refined animal and vegetable fats and oils, and crude animal and vegetable oils. This Document does not apply to products containing inorganic acids unless the inorganic acids can be determined separately. The saponification value can also be calculated from fatty acid data obtained by gas chromatography analysis as shown in Appendix B. For this calculation, it shall be ensured that the sample is free of impurities or thermal degradation products.

2 Normative References

The provisions in following documents become the essential provisions of this Document through reference in this Document. For the dated documents, only the versions with the dates indicated are applicable to this Document; for the undated documents, only the latest version (including all the amendments) is applicable to this Document. ISO 661 Animal and vegetable fats and oils – preparation of test sample NOTE. GB/T 15687-2008 Animal and vegetable fats and oils - Preparation of test sample (ISO 661.2003, IDT)

3 Terms and Definitions

For the purposes of this Document, the following terms and definitions apply. 3.1 Saponification value; IS The number of milligrams for potassium hydroxide that are needed to saponify 1 g of fats and oils.

4 Principle

The test sample was saponified by using an excess of potassium hydroxide-ethanol solution under reflux boiling conditions, and then the excessive potassium hydroxide was titrated with a hydrochloric acid standard titration solution.

5 Reagents

Unless otherwise specified, all reagents used in this Document are of analytical reagents; and the used water is distilled water or demineralized water of equivalent purity. 5.1 Ethanol. Volume fraction φ = 95%. 5.2 Potassium hydroxide-ethanol solution. c(KOH) = 0.5 mol/L. The potassium hydroxide-ethanol solution is colorless or pale yellow. A stable colorless solution can be obtained by any of the following methods. a) Reflux 1 L of ethanol (5.1) with 8 g of potassium hydroxide and 5 g of aluminum granules for 1 h; then immediately distill. Dissolve the required amount of potassium hydroxide (approximately 35 g) in the distillate. Let stand for several days; then pour the clear supernatant from the precipitated potassium carbonate into a brown glass bottle. b) Add 4 g of aluminum tert-butoxide to 1 L of ethanol and allow the mixture to stand for several days. Pour off the supernatant and dissolve the required amount of potassium hydroxide in it. Let it stand for several days, then pour the clear supernatant from the precipitated potassium carbonate into a brown glass bottle. 5.3 Hydrochloric acid standard solution. c(HCl) = 0.5 mol/L. 5.4 Alkali blue 6B solution. ρ = 2.5 g/100 mL ethanol solution (5.1). 5.5 Phenolphthalein solution. ρ = 0.1 g/100 mL ethanol solution (5.1). Phenolphthalein is classified as a carcinogenic, teratogenic, or reproductively toxic (CMR) substance and should only be used when no alternative is available. 5.6 Boiling promoters.

6 Instruments and Equipment

Common laboratory instruments, especially the following shall be used. 6.1 Erlenmeyer flask. 250 mL capacity, made of alkali-resistant glass, with a ground glass neck. 6.2 Reflux condenser. Equipped with a ground glass connector for connection to the Erlenmeyer flask (6.1). 6.3 Heating device. Such as a water bath, hot plate, or other suitable device; open flame heating is prohibited. 6.4 Burette. 50 mL capacity, with a minimum graduation of 0.1 mL, or an automatic burette. 6.5 Pipette. 25 mL capacity, or an automatic pipette. 6.6 Analytical balance. Minimum graduation of 0.0001 g, weighing accuracy of 0.001 g.

7 Sampling

Sampling is not a specific content of this Document; ISO 5555 is recommended. It is crucial that the samples received by the laboratory are representative and have not been damaged or altered during transportation or storage period.

8 Preparation of Specimen

Perform according to the provisions of ISO 661. If insoluble impurities are present in the specimen, mix thoroughly, filter, and note this in the test report.

9 Operating Procedure

9.1 Weighing Weigh approximately 2 g of the sample (Clause 8) into an Erlenmeyer flask (6.1), accurate to 0.005 g Based on a saponification value (by KOH) of 170 mg/g to 200 mg/g and the 2 g of sample size, for samples with different saponification values, the sample size should be varied as needed to ensure that approximately half of the potassium hydroxide-ethanol solution is neutralized. Recommended sample sizes are shown in Table 1. Table 1 -- Sample sizes 9.2 Determination 9.2.1 Pipette (6.5) 25.0 mL of potassium hydroxide-ethanol solution (5.2) to the specimen; and add some boiling promoters (5.6). Connect the reflux condenser (6.2) to the Erlenmeyer flask; and place the Erlenmeyer flask on a heating device (6.3) to slowly boil; shake occasionally; maintaining boiling for 60 min. For samples with high melting points and difficult saponification, boil for 2 h. 9.2.2 Add 0.5 mL to 1 mL of indicator (5.4 or 5.5) to the hot solution; and titrate with hydrochloric acid standard solution (5.3) until the indicator color just disappears. If the solution color is dark, phenolphthalein (5.5) shall not be used as an indicator. 9.3 Blank test Following the requirements of 9.2, without adding a sample, a blank determination was performed using 25.0 mL of potassium hydroxide-ethanol solution (5.2).

10 Calculation of Results

The saponification value IS was calculated according to Formula (1). Where. V0 – volume of hydrochloric acid standard solution (5.3) consumed in the blank test, in mL; V1 - volume of hydrochloric acid standard solution (5.3) consumed in the specimen test, in mL; c - actual concentration of the hydrochloric acid standard solution (5.3), in mol/L; m - mass of the specimen (9.1), in g. For repeatability meeting the requirements of 11.2, the arithmetic mean of two tests shall be taken as the test result. Estimated saponification value (by KOH) Sample size/g Results shall be expressed as integers, by KOH, and in mg/g.

11 Precision

11.1 Interlaboratory test In 2000, the German Institute for Standardization (DIN) organized interlaboratory test involving 22 laboratories (see Appendix A). Each sample was tested twice; and statistical results were provided (evaluated according to ISO 5725-1 and ISO 5725-2). The statistical results are shown in Table A.1. 11.2 Repeatability In the same laboratory, by the same operator using the same equipment and the same test method, the absolute difference between two independent tests of the same test subject conducted within a short period of time shall not exceed 5% of the repeatability limit r shown in Table A.1. 11.3 Reproducibility In different laboratories, by different operators using different equipment and the same test method, the absolute difference between two independent tests of conducted the same test subject shall not exceed 5% of the reproducibility limit R shown in Table A.1.

12 Test Report

The test report shall include. a) All relevant information required for the test sample; b) If the sampling method is known, indicate it; c) Whether filtration is required for the test sample; d) The used test method document, such as GB/T 5534-2024; e) A description of the used indicator (5.4 or 5.5); f) Any details not specifically stated in this Document or considered optional, and all operational details that may affect the results; g) The determination results, and if repeatability tests were performed, the final results shall be listed.

Appendix A

(Informative) Interlaboratory Test Results An international joint test was conducted on 5 samples by 22 laboratories in 8 countries. --- A. Coconut oil; --- B. Palm oil; --- C. Rapeseed oil; --- D. Medium-chain triglyceride (MCT) oil; --- E. A mixture of 60% A and 40% D. In 2000, the German Institute for Standardization (DIN) organized the joint test and performed a statistical analysis of the data accuracy according to ISO 5725-2.The results are shown in Table A.1. Table A.1 -- Statistical analysis of test results The number of laboratories retained after removing outliers, n Parameters Rapeseed oil Palm oil Coconut oil 60% coconut oil+40% medium-chain triglyceride oil Medium-chain triglyceride oil The number of participating laboratories, N The number of independent test results for each sample from all laboratories, z Average value𝐼S̅(by KOH)/(mg/g) Repeatability standard deviation, sr Repeatability coefficient of variation CVr /% Repeatability limit r Reproducibility standard deviation, SR Reproducibility coefficient of variation CVR /% Reproducibility limit R

Appendix B

(Informative) Calculation of Saponification Values from Fatty Acid Composition Data B.1 Overview The Formulas in B.3~B.6 provide a mathematical method for calculating the saponification values of oils and their constituent acylglycerols from a given fatty acid composition of fatty acids, fatty acid methyl esters, or other fatty acid esters. Therefore, the given Formulas are well-suited for computer use. B.7 provides an example that can be calculated manually. The determination of fatty acid methyl esters shall be performed according to ISO 12966-2, ISO 12966-3, and ISO 12966-4. B.2 Symbols CF(i). Carbon number of the ith fatty acid or fatty acid ester; CT(i). Carbon number of the ith triglyceride; i. Specific fatty acid, fatty acid ester, or triglyceride; ISC. Calculated saponification value; k. Integer constant of fatty acid derivative; 𝑀ഥ. Average relative molecular mass of all fatty acids in the specimen; MCH2.Relative molecular mass of CH2 (14.026 7); MH2.Relative molecular mass of H2 (2.015 9) MHCOOH. Relative molecular mass of HCOOH (46.025 5) MF(i). Relative molecular mass of the ith fatty acid or fatty acid ester; MT(i). Relative molecular mass of the ith triacylglycerol; nF(i). The number of double bonds in the ith fatty acid or fatty acid ester; nT(i). The number of double bonds in the ith triacylglycerol; wF(i). Mass fraction of the ith fatty acid or fatty acid ester; wT(i). Mass fraction of the ith triacylglycerol; wU. Mass fraction of unsaponifiable matter; xF(i). Mole fraction of the ith fatty acid or fatty acid ester; xT(i). Mole fraction of the ith triacylglycerol. B.3 Calculation of the relative molecular mass of fatty acids or fatty acid esters Where. k = 0, representing an acid; k = 1, representing a methyl ester; k = 2, representing an ethyl ester; k = 3, representing a propyl ester; k = 4, representing a butyl ester. Or, applicable to the relative molecular mass of the acid given by the user. B.4 Calculation of the relative molecular mass of triacylglycerols B.5 Calculation of the average relative molecular mass of triacylglycerols Equal to. Equal to. B.6 Calculation of saponification value According to the definition of saponification value, for triacylglycerols. For diacylglycerols, factor 3 is replaced by 2; for fatty acids and monoacylglycerols, factor 3 is replaced by 1. B.7 Examples B.7.1 Fatty acid methyl ester composition of samples Samples using the following methyl ester compositions. 16.0 (10.6% mass fraction), 18.0 (4.2% mass fraction), 18.1 (22.7% mass fraction), 18.2 (54.5% mass fraction), 18.3 (8.0% mass fraction). B.7.2 Calculation of the relative molecular mass of methyl esters (k = 1) Some relative molecular masses are shown below. Palmitic acid. 270.45; Stearic acid. 298.51; Oleic acid. 296.49; Linoleic acid. 294.47; Linolenic acid. 292.46. B.7.3 Calculation of the relative molecular mass of triacylglycerol (k = 1) The relative molecular mass of triacylglycerol (TAG) is the sum of the masses of the three fatty acid methyl esters minus the mass of four hydrogen atoms (4.0318). For a 16.0 triglyceride ratio, the result is 270.45 + 270.45 + 270.45 − 4.0318 = 807.32. For an 18.0 triglyceride ratio, the result is 298.51 + 298.51 + 298.51 − 4.0318 = 891.50. For an 18.1 triglyceride ratio, the result is 296.49 + 296.49 + 296.49 − 4.0318 = 885.44. For an 18.2 triglyceride ratio, the result is 294.47 + 294.47 + 294.47 − 4.0318 = 879.38. For an 18.3 triglyceride ratio, the result is 292.46 + 292.46 + 292.46 − 4.0318 = 873.35. B.7.4 Calculation of average relative molecular mass In manual calculations, to save workload, it is assumed that Wx(0) = WR(0), which is equivalent to the mass fraction of triacylglycerols being the same as the mass fraction of fatty acid methyl esters. The average relative molecular mass of all triacylglycerols is. B.7.5 Calculation of saponification value NOTE. Results are expressed as positive numbers. B.8 Correction for free fatty acids, partial glycerol, and unsaponifiable matters For free fatty acids and partial glycerol, their appropriate relative molecular masses and saponification values are calculated by Formulas B.3~B.6.Their total relative molecular mass and saponification reaction are calculated by mass conservation for a given ratio of free fatty acids to glycerol. Bibliography ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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