ISO 16186:2021 Footwear — Critical substances potentially present in footwear and footwear components — Determination of dimethyl fumarate (DMFU)

标准简介

Footwear — Critical substances potentially present in footwear and footwear components — Determination of dimethyl fumarate (DMFU)由ISO于2021-05发布，适用于世界范围。

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标准部分原文

Footwear — Critical substances potentially present in footwear and footwear components — Determination of dimethyl fumarate (DMFU)

WARNING — The use of this document can involve hazardous materials, operations and equipment. It does not purport to address all of the safety or environmental problems associated with its use. It is the responsibility of users of this document to take appropriate measures to ensure the safety and health of personnel and the environment prior to application of the document, and to determine the applicability of regulatory limitations for this purpose.

1 Scope

This document specifies a method for the determination of the content of dimethyl fumarate (DMFU) by gas chromatograph with single quadrupole mass spectrometer (GC-MS) or tandem quadrupole mass spectrometer (GC-MS/MS).

This document is applicable to all types of footwear and footwear components except metal parts.

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 4787, Laboratory glassware — Volumetric instruments — Methods for testing of capacity and for use

3 Terms a nd definiti ons

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://w ww.e lectropedia .org/ 4 Principle

The sample is extracted using acetone (see precaution for the solvent in Annex C) at 60 °C in an ultrasonic bath. At this step, two different procedures can be used, depending on the material being tested:

a) The “standard procedure,” without purification and concentration of the extracted solution, can be used for samples giving a simple chromatogram, for example, textile footwear components.

b) The “procedure for complex matrix”, with purification and concentration of the extract, can be used for samples with a complex matrix effect, such as leather.

An aliquot of the extract is analysed using a gas chromatography with single quadrupole mass spectrometry (GC-MS) or tandem quadrupole mass spectrometry (GC-MS/MS).

5 Reagents and materials

The substances shall be used at a defined purity grade. If not otherwise defined, analytical reagent grade chemicals shall be used.

1)

5.1 Acetone, CAS RN® : 67-64-1.

5.2 n-Hexane, CAS RN®: 110-54-3.

5.3 Dimethyl fumarate (DMFU), CAS RN®: 624-49-7.

5.4 Dimethyl maleate (DMMA), CAS RN®: 624-48-6.

5.5 Internal standard, deuterated Dimethyl fumarate-2,3-d (d -DMFU), CAS RN®: 23057-98-9.

2 2

5.6 Standard solutions.

5.6.1 Internal standard - stock solution (1 000 mg/l).

Weigh (10 ± 0,1) mg of d -DMFU (5.5) into a 10 ml volumetric flask (6.6) and fill to the mark with acetone 2

(5.1). Transfer the content into an amber 10 ml vial (6.8) with cap and keep it at 4 °C.

5.6.2 Internal standard - working solution (10 mg/l).

Prepare this solution by means of 1:100 dilution of the internal standard stock solution (5.6.1) with acetone (5.1).

5.6.3 Target compounds - stock solution (1 000 mg/l).

Weigh (50 ± 0,1) mg of DMFU (5.3) and (50 ± 0,1) mg of DMMA (5.4), with an accuracy of 0,1 mg, in a 50 ml volumetric flask (6.6), and fill to the mark with the acetone(5.1).

5.6.4 Target compounds - working solution(1 mg/l).

Prepare this solution by means of 1:1 000 dilution of the standard stock solution (5.6.3) with acetone (5.1).

6 Apparatus

The usual laboratory equipment and laboratory glassware, in accordance with ISO 4787, shall be used, in addition to the following:

6.1 Analytical balance, with a precision of at least 0,1 mg.

6.2 Glass vial, with screw cap that can be tightly sealed (e.g. volume of 40 ml).

6.3 Ultrasonic bath, with adjustable temperature, suitable for operation at about 60 °C.

6.4 PTFE membrane filter, with a pore width of 0,45 µm.

6.5 GC vial, with cap (e.g. volume of 2 ml).

1) CAS Registry Number® (CAS RN®) is a trademark of CAS corporation. This information is given for the convenience of users of this document and does not constitute an endorsement by ISO of the product named. Equivalent products may be used if they can be shown to lead to the same results.

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