ISO 16181-1:2021 Footwear — Critical substances potentially present in footwear and footwear components —Part 1: Determination of phthalate with solvent extraction

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Footwear — Critical substances potentially present in footwear and footwear components —Part 1: Determination of phthalate with solvent extraction由ISO于2021-03发布，适用于全球范围。

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

Part 1: Determination of phthalate with 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 test method to determine the qualitative and quantitative presence of phthalate compounds (see Annex A) in footwear and footwear components.

NOTE 1 A list of relevant materials potentially containing phthalates can be found in ISO/TR 16178:2012, Annex A or in CEN/TR 16417.

NOTE 2 This test method can also be used to determine phthalates other than those listed in Annex A, subject to validation.

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 4787:2010, 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://w ww .iso .org/ obp

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

The test sample is extracted using toluene at 60 °C in an ultrasonic bath for 1 h. An aliquot is then analysed using a gas chromatograph (GC) with a mass selective detector (MS).

All the abbreviations of phthalates used are given in Annex A.

When compared with ISO 16181-2, the two analytical methods should give similar trends but not necessarily the same absolute result. Therefore, in cases of dispute, the method in this document shall be used in preference to ISO 16181-2.

5 Reagents

5.1 Chemicals

Unless otherwise specified, use only reagents of recognized analytical grade.

1)

5.1.1 Toluene, Chemical Abstract Service Registry Number® ( CAS RN®): 108-88-3.

5.1.2 Internal standard

Either of the following chemicals can be used as internal standard:

— Bis (2-Ethylhexyl) phtalates-3,4,5,6-D4 (CAS RN®: 93951-87-2);

— Diphenylphthalate (CAS RN® 84-62-8)

NOTE 1 Diphenylphthalate gives appropriate results in case of DEHP <1 %. In case of DEHP >1 % the results of all other phthalates can be affected because of poor resolution between DEHP and Diphenylphthalate.

NOTE 2 Other internal standards have been found convenient as Di-n-propylphthalate-3-4-5-6 D4 (CAS RN®: 358731-29-0).

5.1.3 Phthalates, see Annexes A and B.

5.1.4 Acetone, CAS RN®: 67-64-1.

5.1.5 Methanol, CAS RN®: 67-56-1.

5.1.6 Cyclohexane, CAS RN®: 110-82-7.

5.1.7 Tetrahydrofurane (THF), CAS RN®: 109-99-9.

5.1.8 n-hexane, CAS RN®: 110-54-3.

5.2 Standard solutions

5.2.1 Target phthalates — Stock solution

Based on its tasks a laboratory shall decide which phthalates from Table A.1 need to be determined.

Based on this decision, standard stock solution for each phthalate shall be available either as commercially available certified mixes, individual components in solution or self-prepared individual standard stock solutions of each phthalate in toluene (5.1.1).

Prepare, for example, standard stock solutions with concentrations of 1 000 µg/ml, weigh 50,0 mg of each phthalate depending on the purity (Table A.1) into 50 ml volumetric flasks, fill the volumetric flasks up to the mark with toluene (5.1.1) and mix thoroughly to dissolve completely the substance.

5.2.2 Internal standard — Stock solution

Prepare an internal standard stock solution that is in the same concentration range as the standard stock solutions (5.2.1) by dissolving the internal standard (5.1.2) in toluene (5.1.1) according to 5.2.1.

1) CAS Registry Number (CAS RN) is a registered trademark of the American Chemical Society (ACS). This information is given for the convenience of users of this document and does not constitute an endorsement by ISO of the product named.

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