ISO 18219-1:2021 INTERNATIONAL STANDARDIULTCS/IUC 30-1:2021(E)Leather — Determination of chlorinated hydrocarbons in leather —Part 1: Chromatographic method for short-chain chlorinated paraffins (SCCPs)

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INTERNATIONAL STANDARDIULTCS/IUC 30-1:2021(E)Leather — Determination of chlorinated hydrocarbons in leather —Part 1: Chromatographic method for short-chain chlorinated paraffins (SCCPs)由国际标准化组织(International Organization for Standardization，简称ISO)于2021-05发布，适用于全球范围。

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INTERNATIONAL STANDARD

IULTCS/IUC 30-1:2021(E)

Leather — Determination of chlorinated hydrocarbons in leather —

Part 1: Chromatographic method for short-chain chlorinated paraffins (SCCPs)

1 Scope

This document specifies a chromatographic method to determine the amount of short-chain chlorinated paraffins (SCCPs) C to C in processed and unprocessed leathers.

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2 Normative references

The following documents are referred to in the text in such a way that some or all of their content constitutes requirements 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.

ISO 2418, Leather — Chemical, physical and mechanical and fastness tests — Sampling location

ISO 4044, Leather — Chemical tests — Preparation of chemical test samples

3 Terms and definitions

No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso. org/o bp

— IEC Electropedia: available at http:// www .electropedia .org/ 4 Principle

The test sample is extracted using n-hexane at 60 °C in an ultrasonic bath for 60 min. After sulfuric acid clean-up, an aliquot is then analysed using a gas chromatograph fitted to a mass selective detector with chemical ionization (GC-ECNI-MS).

A liquid chromatography system with single quad (LC-MS) or triple quad mass spectrometry (LC-

MS/MS), as described in Annex B, can also be used if the user has demonstrated that the accuracy of measurement is equivalent to that of the GC-ECNI-MS method.

In some cases when determining SCCPs using the GC-ECNI-MS method, the presence of sulfochlorinated paraffins and equivalent chain-length chloroalkenes causes interference. The Annex B procedure with a LC-MS/MS method aims to give a better resolution and eliminate possible false positives determined with the GC-ECNI-MS method.

5 Apparatus and materials

Use normal laboratory apparatus and, in particular, the following.

IULTCS/IUC 30-1:2021(E)

5.1 Analytical balance, weighing to an accuracy of 0,1 mg.

5.2 Sealable vessel, with lid, 20 ml, suitable for extraction with n-hexane.

5.3 Ultrasonic bath, with controllable heating capable of maintaining a temperature of (60 ± 5) °C.

NOTE A frequency of 40 KHz is suitable.

5.4 Pipette, 1 ml to 10 ml capacity.

5.5 Volumetric flask, 2 ml.

5.6 Gas chromatograph and mass selective detector with chemical ionization, (GC-ECNI-MS).

NOTE An example of GC-ECNI-MS equipment is given in Annex A.

5.7 Shaker or agitator, ensuring an efficient mixing of the phases.

6 Reagents

If not otherwise defined, analytical reagent grade chemicals shall be used.

6.1 n-hexane, Chemical Abstracts Service (CAS) CAS No 110-54-3.

6.2 Internal standard solution, lindane, CAS No 58-89-9, 1 000 µg/ml.

6.3 Standard solutions, SCCPs, C to C , with different chlorination degree, each 100 µg/ml.

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6.3.1 SCCPs C to C , 55,5 % Cl, technical grade.

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6.3.2 SCCPs C to C , 63 % Cl, technical grade, CAS No 85535-84-8.

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NOTE These SCCPs calibration solutions are available commercially.

6.4 Concentrated sulfuric acid, (ρ = 1,84 g/ml at 20 °C).

7 Sampling

Take a sample in accordance with ISO 2418. If sampling in accordance with ISO 2418 is not possible (e.g. leathers from finished products like shoes, garments), provide details about sampling together with the test report. Glue residuals shall be mechanically removed from leather samples.

Prepare the leather samples in accordance with ISO 4044.

8 Sample preparation and analysis

8.1 Preparation of the SCCPs calibration solution (50 µg/ml) with 59 % chlorine content

Transfer 533 µl of SCCPs C to C 55,5 % Cl standard solution (6.3.1) and 467 µl SCCPs C to C 63 % 10 13 10 13

Cl standard solution (6.3.2) into a 2 ml volumetric flask (5.5). Add 20 µl of internal standard solution (6.2). Fill the flask up to the volume with n-hexane (6.1).

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