GB/T 17592-2024Textiles - Determination of the banned azo colourants (English PDF)

Foreword

This document was drafted in accordance with the provisions of GB/T 1.1-2020

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

standardizing documents".

This document replaces GB/T 17592-2011 "Textiles - Determination of the banned azo

colorant". Compared with GB/T 17592-2011, in addition to structural adjustments and

editorial changes, the main technical changes are as follows.

- ADD the reagents such as acetonitrile, tert-butyl methyl ether, aromatic amine

quantitative standard working solution, sodium hydroxide aqueous solution,

benzidine-d8; SPECIFY the validity period of sodium dithionite aqueous solution;

CHANGE the concentrations of aromatic amine standard stock solution, aromatic

amine standard working solution, internal standard solution; DELETE ether (see

Chapter 5; Chapter 4 of the 2011 edition);

- ADD the pipettes, analytical balances, pH meters; ADD the mass selective

detectors (MS) and polytetrafluoroethylene filters to high performance liquid

chromatographs; ADJUST the size of glass or polypropylene columns (see Chapter

6; Chapter 5 of the 2011 edition);

- ADD the "Sampling and preparation of specimen", clarifying the requirements for

sampling by components and colors (see Chapter 7);

- CHANGE the amount of citrate-sodium hydroxide buffer solution added and the

cooling time (see 8.1; 6.1 of the 2011 edition);

- CHANGE the separation and concentration steps, extraction reagents, volume-

fixing reagents of aromatic amines; ADD the storage requirements of the sample

solution after volume fixation (see 8.2; 6.2 of the 2011 edition);

- ADD the requirements for the qualitative analysis of aniline and 1,4-

phenylenediamine (see 8.3.2);

- DELELTE the specific steps of gas chromatography/mass spectrometry qualitative

and quantitative analysis; MOVE the chromatographic analysis conditions to

Appendix C (see Appendix C; 6.3 and 6.4 of the 2011 edition);

- ADD the "Quantitative equipment and other sources related to false positive

results" (see 8.3.3);

- ADD the "verification", specifying the minimum recovery rate requirements of

aromatic amines (see 8.4);

- CHANGE the "result calculation and expression" (see Chapter 9; Chapter 7 of the

2011 edition);

- ADJUST the original Appendix A to Appendix B.

This document modifies and adopts ISO 14362-1.2017 "Textiles - Methods for

determination of certain aromatic amines derived from azo colorants - Part 1.Detection

of the use of certain azo colorants accessible with and without extracting the fibers".

Compared with ISO 14362-1.2017, this document has made the following structural

adjustments.

- Chapter 4 corresponds to Chapter 5 of ISO 14362-1.2017;

- Chapter 5 corresponds to Chapter 7 of ISO 14362-1.2017, of which 5.1 corresponds

to 7.11 of ISO 14362-1.2017 and 5.2 ~ 5.10 correspond to 7.1 ~ 7.10 of ISO 14362-

1.2017;

- Chapter 6 corresponds to Chapter 8 of ISO 14362-1.2017, of which 6.1 ~ 6.7

correspond to 8.3 ~ 8.8 of ISO 14362-1.2017, meanwhile 6.8 and 6.9 are added;

- Chapter 7 corresponds to Chapter 9 of ISO 14362-1.2017, of which 7.1 ~ 7.2

correspond to 9.1 ~ 9.2 of ISO 14362-1.2017, 7.3 corresponds to 9.6 of ISO 14362-

1.2017;

- Chapter 8 corresponds to Chapter 10 of ISO 14362-1.2017, of which 8.1 ~ 8.4

correspond to 10.3 ~ 10.6 of ISO 14362-1.2017;

- Chapter 9 corresponds to Chapter 11 of ISO 14362-1.2017; Chapter 10 corresponds

to Chapter 12 of ISO 14362-1.2017;

- Appendices C ~ F correspond to Appendix A, Appendix E, Appendix C, Appendix

G of ISO 14362-1.2017, respectively; Appendix A and Appendix G are added.

This document has technical differences, as compared with ISO 14362-1.2017, which

are marked with a vertical single line (|) in the outer margin of the clauses involved. A

list of these technical differences and their reasons is shown in Appendix A.

This document also made the following editorial changes.

- CHANGE the standard name to "Textiles - Determination of the banned azo

colorants";

- MOVE the content of Chapter 4 of the international standard to Appendix B of this

document;

- DELETE the informative Appendix B "Reliability of the method" from the

international standard.

Please note that some of the content of this document may involve patents. The issuing

agency of this document does not assume the responsibility for identifying patents.

This document was proposed by the China National Textile and Apparel Council.

This document shall be under the jurisdiction of the National Technical Committee for

Textile Standardization (SAC/TC 209).

This standard replaces the standard previously issued as follows.

- It was first published in 1998 as GB/T 17592.1 ~ 17592.3-1998;

- It was first revised in 2006 as GB/T 17592-2006;

- It was second revised in 2011 as GB/T 17592-2011;

- This is the third revision.

Textiles - Determination of the banned azo colorants

Warning - Personnel using this document shall have practical experience in formal

laboratory work. This document does not address all possible safety issues. Users

are responsible for taking appropriate safety and health measures and ensuring

that the conditions specified in relevant national laws and regulations are met.

1 Scope

This document describes the determination method of banned azo dyes that can

decompose carcinogenic aromatic amines in Appendix B in textile products.

This document is applicable to colored textile products, which are processed by dyeing,

printing, coating.

2 Normative references

The contents of the following documents constitute essential provisions of this

document through normative references in the text. Among them, for dated references,

only the version corresponding to that date applies to this document; for undated

references, the latest version (including all amendments) applies to this document.

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

GB/T 23344 Textiles - Determination of 4-aminoazobenzene

3 Terms and definitions

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

4 Principle

Under specified conditions, the specimen is placed in a citrate-sodium hydroxide buffer

solution, reduced and cleaved with sodium dithionite to produce possible aromatic

amines. The aromatic amines are extracted into tert-butyl methyl ether through a

diatomaceous earth column, concentrated and fixed to volume with a suitable solvent,

meanwhile the aromatic amines are determined by chromatography (see Appendix C).

5 Reagents and materials

Unless otherwise specified, all reagents used are analytically pure.

6 Instruments and equipment

Reactor.

Glass or polypropylene column.

Vacuum rotary evaporator.

7 Sampling and specimen preparation

Take a representative sample and cut it into small pieces of about 5 mm × 5 mm. Mix

them. Weigh about 1.0 g, accurate to 0.01 g.

If the sample is a semi-finished product, cut the specimen directly.

8 Test steps

Place the specimen in a reactor (see 6.1). Add 15 mL of citrate-sodium hydroxide buffer

solution (see 5.5), which was preheated to (70 ± 2) °C. Seal the reactor. Shake to

completely soak the specimen. Place it in a constant temperature heater (see 6.2), which

was preheated to (70 ± 2) °C, to hold for (30 ± 1) min.

Add 0.2 mL of sodium hydroxide aqueous solution (see 5.10) to the reactor. Shake

vigorously. Pipette the reaction solution to the diatomaceous earth column (see 6.3). Let

it stand for adsorption for 15 minutes.

9 Calculation and expression of results

According to 8.3, if the content of any aromatic amine measured by using the aromatic

amine standard working solution (see 5.9.2) is greater than 5 mg/kg, a standard curve

with at least 6 points (including blank) shall be established (see 5.9.3), for quantitative

analysis of the aromatic amine. Plot a standard curve of response value and known

concentration (if an internal standard is used, the response value needs to be calibrated).

The mass concentration (rhos) of the aromatic amine is obtained from the standard curve,

in micrograms per milliliter (µg/mL).

10 Test report

The test report shall include the following.

a) The number of this document, i.e., GB/T 17592-2024;

b) The source and description of the sample;

c) The date of receipt and the date of the test of the sample.

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