ISO 18219-2:2021 INTERNATIONAL STANDARDIULTCS/IUC 30-2:2021(E)Leather — Determination of chlorinated hydrocarbons in leather —Part 2: Chromatographic method for middle-chain chlorinated paraffins (MCCPs)

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INTERNATIONAL STANDARDIULTCS/IUC 30-2:2021(E)Leather — Determination of chlorinated hydrocarbons in leather —Part 2: Chromatographic method for middle-chain chlorinated paraffins (MCCPs)是于2021-05发布的ISO标准，适用于全球。

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标准文档类型为INTERNATIONAL STANDARDIULTCS/IUC 30-2:2021(E)Leather — Determination of chlorinated hydrocarbons in leather —Part 2: Chromatographic method for middle-chain chlorinated paraffins (MCCPs)高清PDF版本（文字版），标准文档内可进行搜索，可以复制原文，可粘贴。

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INTERNATIONAL STANDARD

IULTCS/IUC 30-2:2021(E)

Leather — Determination of chlorinated hydrocarbons in leather —

Part 2: Chromatographic method for middle-chain chlorinated paraffins (MCCPs)

1 Scope

This document specifies a chromatographic method to determine the amount of middle-chain chlorinated paraffins (MCCPs) 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/ obp

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

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

A liquid chromatography system single quad (LC-MS) or with 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 MCCPs using the GC-ECNI-MS method, the presence of sulfochlorinated paraffins and equivalent chain-length chloroalkenes can cause interference. Annex B proposes a LC-

MS/MS application method that aims to give a better resolution and eliminates 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 30-2:2021(E)

5.1 Analytical balance.

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 40KHz 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).

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) No 110-54-3.

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

6.3 Standard solutions, MCCPs, C to C , with different chlorine content, each 100 µg/ml.

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6.3.1 MCCPs C to C 52 % Cl, technical grade, CAS 85535-85-9.

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6.3.2 MCCPs C to C 57 % Cl, technical grade.

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NOTE These MCCP calibration solutions are available commercially.

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

7 Sampling

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 according to ISO 4044.

8 Sample preparation and analysis

8.1 Preparation of MCCPs calibration solution (50 µg/ml) with 55 % chlorination degree

Transfer 400 µl MCCPs C to C 52 % Cl standard solution (6.3.1) and 600 µl MCCP C to C 57 % Cl 14 17 14 17

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

The calibration standard with 55 % chlorine content shall be used for the quantification of all samples, independent of their chlorination degree (if known).

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