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This standard is drafted in accordance with the rules given in the GB/T 1.1-2009.
This standard has been redrafted and modified adoption of International Standard ISO 18219:2015 Leather — Determination of Chlorinated Hydrocarbons in Leather — Chromatographic Method for Short-chain Chlorinated Paraffins (SCCP).
There are structural changes between this standard and the International Standard ISO 18219:2015. A list of the clauses in this standard and the equivalent clauses in ISO 18219:2015 is given in Annex A.
There are technical deviations between this standard and the International Standard ISO 18219:2015. A complete list of technical deviations, together with their justifications, is given in Annex B.
For the purposes of this standard, the following editorial changes have also been made:
— the standard name is changed to Leather and Fur — Chemical Tests — Determination of Short-chain Chlorinated Paraffins.
This standard was proposed by the China National Light Industry Council.
This standard is under the jurisdiction of the National Technical Committee 252 on Leather Industry of Standardization Administration of China (SAC/TC 252).
Leather and Fur — Chemical Tests — Determination of Short-chain Chlorinated Paraffins
1 Scope
This standard specifies a chromatographic method to determine the amount of residues of short-chain chlorinated paraffins (SCCP) C10-C13 in leathers and furs.
This standard is applicable to the determination of SCCP content in various leathers, furs and their products.
2 Normative References
The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB/T 6682 Water for Analytical Laboratory Use — Specification and Test Methods (GB/T 6682-2008, ISO 3696:1987, MOD)
QB/T 1267 Leather — Chemical, Physical and Mechanical and Fastness Tests — Sampling Location (QB/T 1267-2012, ISO 2418:2002, MOD)
QB/T 1272 Fur — Preparation of Chemical Test Samples (QB/T 1272-2012, ISO 4044:2008, MOD)
QB/T 2706 Leather — Chemical, Physical and Mechanical and Fastness Tests — Sampling Location (QB/T 2706-2005, ISO 2418:2002, MOD)
QB/T 2716 Leather — Preparation of Chemical Test Samples (QB/T 2716-2018, ISO 4044:2008, MOD)
3 Principle
The test sample is extracted using n-hexane at the specified conditions in an ultrasonic bath. After SPE clean up, an aliquot is then analyzed using a gas chromatograph fitted to a mass selective detector with chemical ionization (GC-ECNI-MS).
4 Reagents
Unless otherwise specified, all reagents are analytically pure.
4.1 Water, Grade 3 according to GB/T 6682, for test purpose.
4.2 n-hexane, CAS No.: 110-54-3, chromatographically pure.
4.3 Dichloromethane, CAS No.: 75-09-2, chromatographically pure.
4.4 Internal standard solution, 1,1,1,3,10,11-hexachloroundecane, CAS No: 601523-28-8, 1000 µg/mL. The solvent is n-hexane.
Note: Other suitable internal standard can be used.
4.5 Standard solutions, SCCP, C10-C13, with different chlorine content, each 100 µg/ml. The solvent is n-hexane.
SCCP C10-C13 55.5% Cl, industrial grade.
SCCP C10-C13 63.0% Cl, industrial grade.
Note: These SCCP calibration solutions are available commercially.
4.6 SCCP standard solution (50 µg/mL, with 59% chlorination). 533 µL of SCCP C10-C13 55.5% Cl standard solution and 467 µL SCCP C10-C13 63% Cl standard solution are transferred into a 2 mL volumetric flask. 20 µL of internal standard solution is added and the flask filled up to the volume with n-hexane.
4.7 Nitrogen: with a purity of 99.9% or better.
4.8 Helium: with a purity of 99.999% or better.
4.9 Methane: with a purity of 99.9995% or better.
Foreword II
1 Scope
2 Normative References
3 Principle
4 Reagents
5 Apparatus and Equipment
6 Sampling and Sample Preparation
7 Analytical Procedures
8 Calculation of Result
9 Test Report
Annex A (Informative) Structural Changes of This Standard with Respect to ISO 18219:
Annex B (Informative) Technical Deviations between This Standard and ISO 18219:2015 and Their Justifications