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GB/T 40263-2021 English PDF (GBT40263-2021)

GB/T 40263-2021 English PDF (GBT40263-2021)

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GB/T 40263-2021: Textiles - Determination of short chain chlorinated paraffins

This document specifies the method for the determination of short-chain chlorinated paraffins (C10-C13) in textiles, by gas chromatography-tandem mass spectrometry. This document applies to all types of textile products.
GB/T 40263-2021
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 59.080.01
CCS W 04
Textiles - Determination of short chain chlorinated
paraffins
ISSUED ON: MAY 21, 2021
IMPLEMENTED ON: DECEMBER 01, 2021
Issued by: State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and definitions ... 4
4 Principles ... 4
5 Reagents and materials ... 4
6 Instruments ... 5
7 Preparation of specimen ... 6
8 Measurement steps ... 6
9 Calculation and expression of results ... 8
10 Quantification limit and precision ... 9
11 Test report ... 9
Appendix A (Informative) Chromatogram of short-chain chlorinated paraffin standards ... 10
Textiles - Determination of short chain chlorinated
paraffins
Warning: The personnel using this document shall have practical
experience in formal laboratory work. This document does not point out
all possible safety issues. The user is responsible for taking appropriate safety and health measures AND ensuring compliance with relevant
national regulations.
1 Scope
This document specifies the method for the determination of short-chain chlorinated paraffins (C10-C13) in textiles, by gas chromatography-tandem mass spectrometry.
This document applies to all types of textile products.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
There are no terms and definitions, that need to be defined in this document. 4 Principles
The specimen is added to the n-hexane-acetone solution AND ultrasonically extracted. The extract is purified by a graphitized carbon black solid phase extraction column and a silica gel solid phase extraction column; followed by concentration and making its volume reach to the mark; determined by a gas chromatography-tandem mass spectrometer (GC-MS/MS); quantified by
external standard method.
5 Reagents and materials
Unless otherwise stated, all reagents used are of analytical grade.
temperature 35 ??C.
6.5 Nitrogen blowing instrument: It is equipped with water bath heating device, temperature 40 ??C.
7 Preparation of specimen
Take representative specimens. Cut them into slices, which are less than 5 mm ?? 5 mm. Mix them evenly.
8 Measurement steps
8.1 Extraction
Weigh about 1 g of the specimen, which was prepared according to Chapter 7 (accurate to 0.01 g). Place it in a 250 mL Erlenmeyer flask (5.11). Add 20 mL of extraction solvent (5.4). Ultrasonically extract it for 30 min, at room temperature. The filtrate is filtered by qualitative filter paper (5.10). Respectively use 10 mL of extraction solvent to wash the residual sample and filter paper, for 3 times. Combine the above filtrates in a pear-shaped bottle (5.12). Rotate it in a 35 ??C water bath to evaporate it nearly dryness. Use 2 mL of n-hexane (5.1) to dissolve it. Make it ready to be purified.
8.2 Purification
Completely transfer the extract, which is obtained in 8.1, into the activated graphitized carbon black solid phase extraction column (5.6). Then use 8 mL of n-hexane (5.1) to wash the pear-shaped bottle twice, 4 mL for each washing. Transfer the washing liquid on the solid phase extraction column. The obtained effluent is then passed through the activated silica gel solid phase extraction column (5.7). Discard the effluent. Use 15 mL of elution solvent (5.5) to elute it. Collect the eluate in a glass tube (5.13). In a water bath at 40 ??C, use nitrogen to blow it to near dryness. Use n-hexane to make its volume reach to 1 mL, for GC-MS/MS detection.
8.3 Determination by gas chromatography-tandem mass spectrometry
8.3.1 Gas chromatographic conditions
Because the test result depends on the instrument used, it is impossible to give the general parameters of gas chromatography analysis. The following
operating conditions have been proved to be suitable for testing.
a) Chromatographic column: DB-5 quartz capillary column (30 m ?? 0.25 mm ?? 0.25 ??m) or equivalent;
Xi - The content of short-chain chlorinated paraffins in the specimen, in milligrams per kilogram (mg/kg);
Ai - The peak area of short-chain chlorinated paraffin in the sample solution; A0 - The peak area of short-chain chlorinated paraffin in the blank sample solution;
Ais - The peak area of short-chain chlorinated paraffin in standard working solution;
ci - The mass concentration of short-chain chlorinated paraffins in the standard working solution, in micrograms per milliliter (??g/mL);
V - The final constant volume of the sample solution, in milliliters (mL); m - The mass of the specimen, in grams (g).
10 Quantification limit and precision
10.1 Limit of quantification
The limit of quantification of short-chain chlorinated paraffins in textiles, by this method, is 20.0 mg/kg.
10.2 Precision
In the same laboratory, when the same operator uses the same equipment, according to the same test method, to carry out independent test on the same tested object, within a short period of time, THEN the absolute difference between the two test results is not greater than the arithmetic mean of the two determinations values by 15%.
11 Test report
The test report shall include at least the following:
a) The number of this document;
b) Sample description;
c) Test results;
d) Any deviation from the prescribed procedures;
e) Test date.

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