GB/T 15688-2024_English: PDF (GB/T15688-2024)
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Animal and vegetable fats and oils - Determination of insoluble impurities content
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Animal and vegetable fats and oils -- Determination of insoluble impurities content
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Animal and vegetable oils and fats--Determination of insoluble impurities content
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| Standard ID | GB/T 15688-2024 (GB/T15688-2024) | | Description (Translated English) | Animal and vegetable fats and oils - Determination of insoluble impurities content | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | X04 | | Classification of International Standard | 67.040 | | Word Count Estimation | 12,181 | | Date of Issue | 2024-08-23 | | Date of Implementation | 2024-08-23 | | Administrative Organization | National Technical Committee on Grain and Oil Standardization (SAC/TC 270) | | Proposing organization | National Grain and Material Reserves Administration | | Issuing agency(ies) | State Administration for Market Regulation, National Standardization Administration | | Standard ID | GB/T 15688-2008 (GB/T15688-2008) | | Description (Translated English) | Animal and vegetable fats and oils. Determination of insoluble impurities content | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | X04 | | Classification of International Standard | 67.040 | | Word Count Estimation | 8,871 | | Date of Issue | 2008-11-04 | | Date of Implementation | 2009-01-01 | | Older Standard (superseded by this standard) | GB/T 15688-1995 | | Quoted Standard | GB/T 15687 | | Adopted Standard | ISO 663-2007, MOD | | Drafting Organization | Huazhong Agricultural University | | Administrative Organization | National Standardization Technical Committee Agri | | Regulation (derived from) | National Standard Approval Announcement 2008 No.17 (Total No.130) | | Proposing organization | National Food Authority | | Issuing agency(ies) | Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China; Standardization Administration of China | | Summary | This standard specifies the determination of plant and animal oils and fats insoluble impurities content. This standard applies to animal fat. If soaps (especially calcium soaps) or oxidation of fatty acids is not as insoluble impurities content calculated using different solvents should and method of operation. The measurement of insoluble impurities content complies with the relevant requirements. | | Standard ID | GB/T 15688-1995 (GB/T15688-1995) | | Description (Translated English) | Animal and vegetable oils and fats--Determination of insoluble impurities content | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | X14 | | Classification of International Standard | 67.2 | | Word Count Estimation | 3,347 | | Date of Issue | 1995/8/17 | | Date of Implementation | 1996/1/1 | | Adopted Standard | ISO 663-1992, MOD | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 17 of 2008 (No. 130 overall) | | Proposing organization | People Republic of China Ministry of Internal Trade | | Issuing agency(ies) | State Bureau of Technical Supervision |
GB/T 15688-2024 Chinese.Determination of insoluble impurities in animal and vegetable fats and oils
GB/T 15688-2024 English. Animal and vegetable fats and oils - Determination of insoluble impurities content
National Standard of the People's Republic of China
Replace GB/T 15688-2008
Released on 2024-08-23
2025-03-01 Implementation
State Administration for Market Regulation
The National Standardization Administration issued
Preface
This document is in accordance with the provisions of GB/T 1.1-2020 "Guidelines for standardization work Part 1.Structure and drafting rules for standardization documents"
Drafting is required.
This document replaces GB/T 15688-2008 "Determination of insoluble impurities in animal and vegetable fats and oils". Compared with GB/T 15688-2008,
In addition to structural adjustments and editorial changes, the main technical content changes are as follows.
Added the scope of non-application (see Chapter 1). a)
This document is equivalent to ISO 663.2017 "Determination of insoluble impurities in animal and vegetable fats and oils".
Please note that some of the contents of this document may involve patents. The issuing organization of this document does not assume the responsibility for identifying patents.
This document was proposed by the State Administration of Grain and Material Reserves.
This document is under the jurisdiction of the National Technical Committee on Standardization of Cereals and Oils (SAC/TC 270).
This document was drafted by. Wuhan Standardization Research Institute, Wuhan Food and Cosmetics Inspection Institute, Wuhan University of Technology, Yihai Kerry Golden Dragon Fish
China Cereals, Oils and Foodstuffs Corporation Limited, Gansu Provincial Institute of Standardization.
The main drafters of this document are. Huang Yong, Jiang Xiaoming, Huang Qing, Zhang Sihong, Wang Geping, Yang Yi, Fang Weixing, Ren Wenjing, Yang Yong,
Xiang Xiaoxue and Xiao Ronghui.
The previous versions of this document and the documents it replaces are as follows.
First published in.1995 as GB/T 15688-1995, first revised in.2008; -
This is the second revision. -
Determination of insoluble impurities in animal and vegetable fats and oils
1 Scope
This document describes a method for the determination of the content of insoluble impurities in animal and vegetable fats and oils.
This document applies to animal and vegetable fats and oils. If soaps (especially calcium soaps) or oxidized fatty acids are not included in the calculation of insoluble impurities,
Calculate and use different solvents and operating methods to ensure that the determination of insoluble impurities content meets relevant requirements.
This document does not apply to milk and dairy products (referring to fats and oils extracted from milk and dairy products).
2 Normative references
The contents of the following documents constitute the essential clauses of this document through normative references in this document.
For referenced documents without a date, only the version corresponding to that date applies to this document; for referenced documents without a date, the latest version (including all amendments) applies.
in this document.
ISO 661 Animal and vegetable fats and oils-Preparation of test samples
sample）
Note. GB/T 15687-2008 Preparation of animal and vegetable fat samples (ISO 661..2003, IDT)
3 Terms and definitions
The following terms and definitions apply to this document.
3.1
Insoluble impurities content
The amount of material insoluble in n-hexane or petroleum ether and foreign impurities under the conditions specified in this document.
Note 1.Content is expressed in mass fraction.
Note 2.These impurities include mechanical impurities, minerals, carbohydrates, nitrogen-containing compounds, various resins, calcium soaps, oxidized fatty acids, fatty acid lactones and
(Part) alkali soaps, hydroxy fatty acids and their glycerides, etc.
4 Principle
Dissolve the sample with excess n-hexane or petroleum ether and filter the resulting solution. Rinse the residue and filter paper with the same solvent to make it
Dry at 103 °C to constant weight.
5 Reagents
Warning - Use proper operating rules for handling hazardous materials and follow all technical, organizational and personal safety measures.
5.1 n-hexane or petroleum ether, the distillation range of petroleum ether is 30℃～60℃, and the bromine value is less than 1.Any of the above solvents, every 100 mL
The residue after evaporation should not exceed 0.002 g.
5.2 Diatomaceous earth, purified and calcined, with a mass loss of less than 0.2% at 900 °C (red heat).
5.3 All reagents were of analytical grade.
6 Instruments
6.1 Analytical balance. graduation value 0.001 g.
6.2 Electric oven. can be controlled at 103℃±2℃.
6.3 Conical flask. capacity 250 mL, with ground glass stopper.
6.4 Dryer. Contains effective desiccant.
6.5 Ashless filter paper. The maximum residue mass fraction of ashless filter paper after combustion is 0.01%. The interception rate of particles larger than 2.5 µm is
Alternatively, choose a glass fiber filter with a diameter of 120 mm, together with a metal (preferably aluminum) or glass container with a lid.
These can be used in place of the crucible filters described in 6.6 for filtering all products except acid oils.
6.6 Crucible filter. glass, P16 grade (pore size 10 µm to 16 µm), diameter 40 mm, volume 50 mL, with vacuum bottle.
Replace the filter described in 6.5 to filter all products including acidic oils.
7 Sampling
The samples received by the laboratory should be representative and should not be damaged or altered during transportation or storage. Sampling is not covered by this document.
For capacity, ISO 5555 should be adopted.
8 Sample preparation
The test specimens were prepared according to ISO 661.
9 Operation steps
9.1 Specimen
In a conical flask (6.3), weigh about 20 g of the sample (Chapter 8) to the nearest 0.01 g.
9.2 Determination
9.2.1 Place the ash-free filter paper (6.5) and the container with a cover or the crucible filter (6.6) in an electric oven (6.2) at a temperature of 103 °C.
Heat and dry. Cool in a desiccator (6.4) and weigh to the nearest 0.001 g. For acidic oils, prepare the crucible according to 9.2.7, and then
Follow the procedures in 9.2.2.
9.2.2 Add.200 mL of n-hexane or petroleum ether (5.1) to the conical flask containing the sample (9.1), cover it with a stopper and shake it.
Oil can increase the amount of solvent for easier operation, so a larger conical flask can be used. Place at 20 °C for 30 min.
9.2.3 Filter through ash-free filter paper in a suitable funnel and, if necessary, filter through a crucible filter with suction. When cleaning the conical flask, ensure that all
The impurities are washed into the filter paper or crucible. Use a small amount of solvent (9.2.2) to clean the filter paper or crucible filter until the solvent is free of grease.
If necessary, heat the solvent appropriately, but the temperature should not exceed 60°C, to dissolve some of the solidified fat on the filter paper.
9.2.4 If ash-free filter paper is used, move the filter paper from the funnel to a container and allow it to stand to allow most of the solvent on the filter paper to evaporate in the air.
The solvent was completely evaporated in an electric oven at 103 °C, then the mixture was taken out of the oven, covered with a lid, cooled in a desiccator (6.4) and weighed.
Measure accurately to 0.001 g.
9.2.5 If a crucible filter is used, place the crucible filter in a fume hood to allow most of the solvent to evaporate in the air and heat at 103 °C.
The solvent is completely evaporated in an oven, then cooled in a desiccator (6.4) and weighed to the nearest 0.001 g.
9.2.6 If the content of organic impurities is to be determined, it is necessary to use pre-dried and weighed ash-free filter paper. In this case, the ash containing
For filter paper containing insoluble impurities, the mass of the filter paper ash is subtracted from the mass of the insoluble impurities being measured.
The organic impurity content is expressed as mass fraction and needs to be multiplied by 100/m0 in the calculation formula. m0 represents the mass of the sample in grams (g).
9.2.7 If acidic oils are to be analyzed, the glass crucible filter should be coated with diatomaceous earth (5.2) as follows.
Mix 2 g of diatomaceous earth and 30 mL of petroleum ether (5.1) into a paste. Pour the paste mixture into a crucible filter under reduced pressure to make the glass
A layer of diatomaceous earth is attached to the filter.
Place the crucible filter coated with diatomaceous earth in an electric oven (6.2) and dry it at 103 °C for 1 h before transferring it to
Cool in a desiccator (6.4) and weigh to an accuracy of 0.001 g.
The same sample (Chapter 8) is measured twice using the above method.
10 Results
11.Precision
11.1 Interlaboratory testing
Appendix A summarizes interlaboratory testing of the precision of this method. The values obtained from these tests may not be applicable to other concentration ranges.
surrounding and other test objects.
11.2 Repeatability
In the same laboratory, under the same conditions, by the same operator using the same equipment, according to the same test method, and in a short period of time
The absolute difference between the two independent test results of an object under test is greater than the repeatability limit given in Table A.1.
(r) does not exceed 5%.
11.3 Reproducibility
In different laboratories, different operators use different equipment and the same test method to test the same object independently.
The absolute difference between the two independent test results obtained shall not exceed 5% of the reproducibility limit (R) given in Table A.1.
12 Test Report
The test report should detail.
All relevant information required for testing the samples;-
If the sampling method is known, please state it;-
Test methods used and referenced standards;-
Solvents used;-
Anything not specifically described in this document, or considered optional, and all operational details that may affect the results;
Determination results. If repeated tests were performed, state the results of the two determinations and the average result. -
......
GB/T 15688-2008
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 67.040
X 04
Replacing GB/T 15688-1995
Animal and Vegetable Fats and Oils -
Determination of Insoluble Impurities Content
(ISO 663:2007, MOD)
ISSUED ON: NOVEMBER 04, 2008
IMPLEMENTED ON: JANUARY 01, 2009
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of PRC.
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 ... 5
7 Sampling ... 6
8 Preparation of Specimen ... 6
9 Operating Procedures ... 6
10 Result Expression ... 7
11 Precision ... 7
12 Test Report ... 8
Appendix A (Informative) Inter-Laboratory Test Results ... 9
Bibliography ... 10
Animal and Vegetable Fats and Oils -
Determination of Insoluble Impurities Content
1 Scope
This Standard specifies the method for the determination of insoluble impurities
content in animal and vegetable fats and oils.
This Standard is applicable to animal and vegetable fats and oils. If soaps (especially
calcium soaps) or oxidized fatty acids are not calculated as insoluble impurities,
different solvents and operating methods shall be used to make the determination of
insoluble impurities meet the relevant requirements.
2 Normative References
The provisions in following documents become the provisions of this Standard through
reference in this Standard. For dated references, the subsequent amendments
(excluding corrigendum) or revisions do not apply to this Standard, however, parties
who reach an agreement based on this Standard are encouraged to study if the latest
versions of these documents are applicable. For undated references, the latest edition
of the referenced document applies.
GB/T 15687 Oils And Fats－Preparation of Test Sample (GB/T 15687-1995, eqv
ISO 661:1989)
3 Terms and Definitions
For the purpose of this Standard, the following terms and definitions apply.
3.1 Insoluble impurities content
Under the conditions specified in this standard, the amount of substances and foreign
impurities insoluble in n-hexane or petroleum ether.
NOTE 1: The content is expressed by mass fraction.
NOTE 2: These impurities include mechanical impurities, minerals, carbohydrates, nitrogen
compounds, various resins, calcium soaps, oxidized fatty acids, fatty acid lactones and (partial)
alkaline soaps, hydroxy fatty acids and their glycerides, etc.
7 Sampling
The sampling is not the content of this Standard, it is recommended to use GB/T 5524.
The samples received by the laboratory shall be representative and shall not be
damaged or changed during transportation or storage.
8 Preparation of Specimen
Prepare the specimen according to the method in GB/T 15687.
9 Operating Procedures
9.1 Specimen
In a conical flask (6.3), take about 20g of the specimen (Clause 8), accurate to 0.01g.
9.2 Determination
9.2.1 Put the filter paper and filter with lid (6.5) or crucible filter (6.6) in the oven (6.2);
the temperature of the oven is 103°C; heat, bake and dry. Cool in a dryer (6.4) and
weigh it, accurate to 0.001g. For acid oils, prepare the crucible according to 9.2.7; and
then operate according to 9.2.2.
9.2.2 Add 200mL of n-hexane or petroleum ether (5.1) to the conical flask containing
the specimen (9.1); cover the stopper and shake. For castor oil, the amount of solvent
may be increased to facilitate operation; so that a larger conical flask may be used.
Stand at 20°C for 30min.
9.2.3 Filter through ashless filter paper in a suitable funnel; and suction filter through a
crucible filter if necessary. When cleaning the conical flask, make sure that all
impurities are washed into the filter paper or crucible.
Clean the filter paper or crucible filter by a small amount of solvent (9.2.2) until the
solvent is free of grease. If necessary, properly heat the solvent, but the temperature
shall not exceed 60°C, so to dissolve some solidified fat on the filter paper.
9.2.4 Move the filter paper from the funnel to the filter (6.5); let it stand; make most of
the solvent on the filter paper evaporate in the air; and completely evaporate the
solvent in the oven at 103°C. Then take it out from the oven; cover the lid; cool in a
dryer (6.4) and weigh it, accurate 0.001g.
9.2.5 If using a crucible filter, make most of the solvent on the crucible filter evaporate
in the air; and completely evaporate the solvent in an oven at 103°C; and then cool
Appendix A summarizes the inter-laboratory test conditions of the precision of this
method. The values obtained from these tests may not be applicable to other
concentration ranges and other test objects.
11.2 Repeatability
In the same laboratory, the same operator uses the same equipment, according to the
same test method, and the same test object is tested independently in a short time.
The condition that the absolute difference between the two independent test results is
greater than the repeatability limit (r) given in Table A.1 does not exceed 5%.
11.3 Reproducibility
In different laboratories, different operators use different equipment and use the same
test method to test the same test object independently of each other. The condition
that the absolute difference between the two independent test results is greater than
the reproducibility limit (R) given in Table A.1 does not exceed 5%.
12 Test Report
The test report should explain in detail for the following:
--- All relevant information required for the test sample;
--- If the sampling method is known, please indicate it;
--- The adopted inspection method and reference standard;
--- The used Solvent;
--- Not specifically stated in this Standard, or considered optional, and all
operational details that may affect the results;
---The measurement results. If a repeatability test is carried out, the results of the
two measurements and the average result shall be stated.
......
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