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This standard was proposed by the China National Textile and Apparel Council.
This standard is under the jurisdiction of the National Technical Committee on Textiles of Standardization Administration of China (SAC/TC 209).
Textiles — Determination of short chain chlorinated paraffins
WARNING - Persons using this standard shall be familiar with normal laboratory practice. This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health measures and to ensure compliance with any national regulatory conditions.
1 Scope
This standard specifies the determination of short chain chlorinated paraffins (C10-C13) by gas chromatography-tandem mass spectrometry method for the textiles.
This standard is applicable to various textiles.
2 Normative references
There are no normative references in this standard.
3 Terms and definitions
No terms and definitions are listed in this standard.
4 Principles
Add a specimen into the n-hexane-acetone solution for ultrasonic extraction; purify the extraction liquid by running through the solid phase extraction column with graphitized carbon black and following by solid phase extraction column with silica gel; then concentrate and drip to constant volume; determine with gas chromatography-tandem mass spectrometer (GC-MS/MS); and quantify by external standard method.
5 Reagents and materials
Unless otherwise specified, analytical reagents shall be adopted.
5.1 N-hexane, analytical reagents for extraction and purification, and chromatographically-pure reagents for constant volume.
5.2 Acetone.
5.3 Dichloromethane.
5.4 Extraction solvent: n-hexane (5.1) and acetone (5.2) are mixed evenly in a volume ratio of 1:2.
5.5 Elution solvent: n-hexane (5.1) and dichloromethane (5.3) in a volume ratio of 1:2.
5.6 Solid phase extraction column with graphitized carbon black: 500 mg, 6 mL. Activate with 5 mL of n-hexane (5.1) before being use, and discard the effluent.
5.7 Solid phase extraction column with silica gel: 500 mg, 3 mL. Activate with 5 mL of n-hexane (5.1) before being use, and discard the effluent.
5.8 Short chain chlorinated paraffin (C10-C13) standards: 100 μg/mL, with the average chlorine content of 51.5%, 55.5% and 63% respectively.
5.9 Short chain chlorinated paraffin (C10-C13) standard working solution: It shall be prepared immediately before use, prepared from mixing the short chain chlorinated paraffin standards (5.8) with different chlorine content for 1 mL respectively and making the total concentration of short chain chlorinated paraffin in the mixed standard solution to be 100 μg/mL, and then diluting with n-hexane (5.1) served as the solvent to a series of standard working solutions.
5.10 Qualitative filter paper: with a diameter of 10 cm.
5.11 Erlenmeyer flask: with the capacity of 250 mL.
5.12 Pear-shaped flask: with the capacity of 250 mL.
5.13 Glass tube: with the capacity of 25 mL.
Foreword i
1 Scope
2 Normative references
3 Terms and definitions
4 Principles
5 Reagents and materials
6 Apparatus
7 Preparation of specimens
8 Determination procedures
9 Calculation and expression of results
10 Limit of quantitation and precision
11 Test report
Annex A (Informative) Chromatogram of short chain chlorinated paraffin reference
