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GB/T 24279.2-2021Textiles - Determination of certain flame retardants - Part 2: Phosphorus flame retardants (English PDF)

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

May 21, 2021

Implementation date

December 1, 2021

Scope

GB/T 24279.2-2021 (Textiles - Determination of certain flame retardants - Part 2: Phosphorus flame retardants) is available as an English-translated PDF.

GB/T 24279.2-2021 — This Part specifies the test method that uses the high-performance liquid chromatography-tandem mass spectrometer (HPLC-MS/MS) to determine certain phosphorus flame retardants in textiles. This Part is applicable to various textiles.

Document preview — GB/T 24279.2-2021

National Standard of the People's Republic of China

Issued by: SAMR; SAC

Contents

  • Foreword...3
  • Introduction...5
  • 1 Scope...6
  • 2 Normative references...6
  • 3 Terms and definitions...6
  • 4 Principle...6
  • 5 Reagents...7
  • 6 Instruments and materials...7
  • 7 Test steps...7
  • 8 Result calculation...9
  • 9 Precision...9
  • 10 Test report...9
  • Annex A (informative) HPLC-MS/MS detection parameters...11

Foreword

This Part was drafted in accordance with the rules given in GB/T 1.1-2020

"Directives for standardization - Part 1: Rules for the structure and drafting of

standardizing documents".

This Part is Part 2 of GB/T 24279 "Textiles - Determination of certain flame

retardants". The following parts of GB/T 24279 have been issued:

- Part 1: Brominated flame retardants;

- Part 2: Phosphorus flame retardants.

This Part uses redrafting method to modify and adopt ISO 17881-2:2016

"Textiles - Determination of certain flame retardants - Part 2: Phosphorus flame

retardants".

The structural differences between this Part and ISO 17881-2:2016 are as

follows:

- added "Normative references" as Clause 2;

- added "Terms and definitions" as Clause 3;

- added "Precision" as Clause 9.

The technical differences between this Part and ISO 17881-2:2016 are as

follows:

- In Clause 5, changed analytically pure to chromatographically pure, added

the purity of the tested standard substance for liquid chromatography

analysis; according to the relevant requirements of prohibited flame

retardants, added the test substance "Di-(2,3-dibromopropyl) phosphate";

- in 5.8, added GB/T 6682 as a reference; specified the requirements for

water used;

- in 6.7, added the balance with a division of 0.01g for weighing textile

specimen;

- in Clause 8, added the provisions that dilution factors and calculation results

are kept to one decimal place, so as to make the calculation and

expression of results clearer;

- in Clause 9, according to relevant domestic standards, added relevant

description on precision.

This Part made the following editorial modifications:

Textiles - Determination of certain flame retardants -

Part 2: Phosphorus flame retardants

WARNING - Personnel using this document should have practical

experience in formal laboratory work. This document does not indicate all

possible security issues. The user is responsible for taking appropriate

safety and health measures and ensuring compliance with the conditions

stipulated by relevant national laws and regulations.

1 Scope

This Part specifies the test method that uses the high-performance liquid

chromatography-tandem mass spectrometer (HPLC-MS/MS) to determine

certain phosphorus flame retardants in textiles.

This Part is applicable to various textiles.

2 Normative references

The following documents are essential to the application of this document. For

the dated documents, only the versions with the dates indicated are applicable

to this document; for the undated documents, only the latest version (including

all the amendments) is applicable to this standard.

GB/T 6682, Water for analytical laboratory use - Specification and test

methods (GB/T 6682-2008, ISO 3696:1987, MOD)

3 Terms and definitions

There are no terms and definitions that need to be defined in this document.

4 Principle

Use acetone as extractant. Extract flame retardant from textile specimens in

ultrasonic generator. Use HPLC-MS/MS to determine flame retardant. Use

external standard method to quantify.

Use acetonitrile (5.6) as solvent to respectively prepare standard stock solution

of each flame retardant (5.1~5.4). The concentration is 1000µg/mL.

7.1.2 Standard working solution

Use acetonitrile to prepare the mixed standard solution. According to the needs,

use acetonitrile to dilute step by step into a series of mixed standard working

solutions of suitable concentration. Choose at least five standard dilution

solutions of appropriate concentration to establish the standard working curve.

Conduct HPLC-MS/MS analysis.

NOTE: Store the standard stock solution in the dark at 0°C~4°C. The validity is 6 months.

Store the standard working solution in the dark at 0°C~4°C. The validity is 3 months.

7.2 Specimen preparation

Take respective specimen from the sample. After cutting and mixing well, use

the balance (6.7) to weigh (1.00+/-0.01)g of specimen.

7.3 Ultrasonic extraction

Place the specimen in a stoppered glass reaction flask (6.4). Add 20mL of

acetone (5.5). Extract in 40°C ultrasonic generator (6.2) for 40min. Collect the

extract in a 100mL concentrating bottle (6.5). Add another 20mL of acetone to

the reaction flask. Extract 20min at about 40°C. Combine and collect the

extracts in a 100mL concentrating flask (6.5).

Use a rotary evaporator (6.3) to concentrate until the residue is nearly dry. Take

2mL of acetonitrile (5.6) to dissolve the residue. Filter through organic filter

membrane (6.6). The resulting filtrate is used for the determination of flame

retardants.

7.4 Determination

Use HPLC-MS/MS(6.1) to determine the flame retardant in the filtrate obtained

in 7.3. Annex A gives examples of detection parameters for HPLC-MS/MS

determination of flame retardants. Carry out a blank test. Subtract the blank

value.

When the flame retardant concentration is too low, appropriately increase the

specimen mass so that the detection concentration is within the linear range of

the instrument's response value.

When the flame retardant concentration is higher than the linear range of the

instrument response value, the solution is appropriately diluted.

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — all pages — is available in the English PDF.

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