ISO 16181-2:2021 Footwear — Critical substances potentially present in footwear and footwear components —Part 2: Determination of phthalate without solvent extraction

标准简介

Footwear — Critical substances potentially present in footwear and footwear components —Part 2: Determination of phthalate without solvent extraction由国际标准化组织于2021-06发布，适用于全球范围。

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Footwear — Critical substances potentially present in footwear and footwear components —

Part 2: Determination of phthalate without solvent extraction

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 specific phthalates (see Annex A) by pyrolyzer/thermal desorption gas chromatography-mass spectrometry (Py/TD-GC-MS). This document is applicable to all types of footwear materials except textiles.

NOTE See also CEN/TR 16417 for a list of the specific phthalates to which this document applies.

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 16181-1, Footwear — Critical substances potentially present in footwear and footwear components — Part 1: Determination of phthalate with solvent extraction

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/ obp

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

The sample is directly introduced into a pyrolyzer, the phthalates are thermally extracted under a specific heat zone and then transferred to the gas chromatograph. Phthalate compounds are separated by the gas chromatographic capillary column and detected by a mass spectrometer.

When compared to ISO 16181-1, the two analytical methods should present similar trends but at the same time, not necessarily the same absolute result. Therefore, in case of any dispute, ISO 16181-1 shall be used in preference.

5 Apparatus

5.1 Analytical balance, capable of measuring accurately to 0,000 01 g (0,01 mg).

5.2 Cryogenic grinding/ milling mill with liquid N cooling.

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5.3 Nipper (a hand tool for cutting samples).

5.4 Micro spatula.

5.5 Tweezers.

5.6 Cutter.

5.7 File.

5.8 Micro puncher.

5.9 Deactivated glass wool.

5.10 Micro syringes or automated pipettes.

5.11 Sample cup.

5.12 Volumetric flasks, 10 ml and 100 ml.

5.13 Gas chromatograph – mass spectrometer equipped with a pyrolyzer.

— Pyrolyzer/thermal desorption accessory:

A temperature rise of 1 °C to 100 °C per minute should be possible across a temperature range from 40 °C to 500 °C. The sample cup should be treated for chemical stability and should be capable of accommodating both liquid and solid samples. It should be possible to maintain the interface between the thermal pyrolysis unit and the gas chromatograph inlet up to 400 °C.

6 Reagents and materials

All reagent chemicals shall be tested for contamination and blank values prior to application as follows.

6.1 n-hexane, for preparing the phthalates standard solution, GC grade or higher.

6.2 Phthalates, see Table A.1.

6.3 Helium, purity greater than a volume fraction of 99,999 %.

6.4 Calibrants: prepare stock solutions containing 100 mg/l of each phthalate (see Annex A) in n-hexane (6.1).

NOTE A commercially available Certified Reference Materials (CRM) containing specific phthalates could be used as a calibrant.

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