GB/T 17592-2024 English PDF (GBT17592-2024)

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GB/T 17592-2024: Textiles -- Determination of the banned azo colourants
GB/T 17592-2024
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.080.01
CCS W 04
Replacing GB/T 17592-2011
Textiles - Determination of the banned azo colorants
(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, MOD)
ISSUED ON. MARCH 15, 2024
IMPLEMENTED ON. APRIL 01, 2025
Issued by. State Administration for Market Regulation;
National Standardization Administration.
Table of Contents
Foreword... 3
1 Scope... 6
2 Normative references... 6
3 Terms and definitions... 6
4 Principle... 6
5 Reagents and materials... 7
6 Instruments and equipment... 8
7 Sampling and specimen preparation... 9
8 Test steps... 10
9 Calculation and expression of results... 14
10 Test report... 15
Appendix A (Informative) Technical differences between this document and ISO
14362-1.2017... 16
Appendix B (Normative) Carcinogenic aromatic amines... 18
Appendix C (Informative) Chromatographic analysis... 19
Appendix D (Informative) Method for liquid-liquid extraction without using
diatomaceous earth column... 28
Appendix E (Informative) Judgment guide - Analysis and interpretation of results.. 31
Appendix F (Informative) Pigments... 37
Appendix G (Informative) Textiles - Determination of banned azo dyes - Extraction
method... 40
References... 44
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).
If any aromatic amine is detected, one or more chromatographic methods shall be used
for confirmation.
Note. Appendix D gives a screening method for liquid-liquid extraction without using a
diatomaceous earth column.
5 Reagents and materials
Unless otherwise specified, all reagents used are analytically pure.
5.1 Water, in accordance with GB/T 6682, grade 3.
5.2 Acetonitrile, chromatographic grade.
5.3 Methanol, chromatographic grade.
5.4 Tert-butyl methyl ether, analytical grade.
5.5 Citrate-sodium hydroxide buffer solution, c = 0.06 mol/L, pH = 6.0.
5.6 Sodium dithionite aqueous solution, effective concentration 200 mg/mL, use within
1 h after preparation.
5.7 Diatomaceous earth, porous granular, calcined at 600 °C for 4 h, stored in a
desiccator after cooling to prepare for use.
5.8 Aromatic amine standards, aromatic amines No. 1 ~ 24 (see Table B.1 in Appendix
B), aniline and 1,4-phenylenediamine, the highest purity available.
5.9 Standard solutions, see 5.9.1 ~ 5.9.5.
5.9.1 Aromatic amine standard stock solution. The aromatic amine mass concentration
is 300 μg/mL (or higher concentration), which is prepared using acetonitrile or other
suitable solvents.
Note. The standard stock solution is stored in a brown bottle with a small amount of anhydrous
sodium sulfite and stored in the freezer. The validity period is one month.
5.9.2 Aromatic amine standard working solution. The aromatic amine mass
concentration is 15 μg/mL, which is prepared by diluting the aromatic amine standard
stock solution with acetonitrile or other suitable solvents (see 5.9.1). It is prepared
before use.
5.9.3 Aromatic amine quantitative standard working solution. The aromatic amine mass
concentration is 2 μg/mL ~ 50 μg/mL, which is prepared by diluting the aromatic amine
standard stock solution with acetonitrile or other suitable solvents (see 5.9.1). It is
prepared before use. If GC-MS is used for quantitative analysis, 10 μL of internal
standard solution (see 5.9.4) needs to be added to each milliliter of solution before
injection. It is prepared before use.
Note. Select appropriate concentration points to establish a standard curve.
5.9.4 Internal standard solution (IS). ρ = 1.0 mg/mL, which is prepared with a suitable
solvent.
During GC-MS analysis, any of the following internal standards may be used.
- IS1.Naphthalene-d8, CAS number. 1146-65-2;
- IS2.2,4,5-trichloroaniline, CAS number. 636-30-6;
- IS3.Anthracene-d10, CAS number. 1719-06-8.
5.9.5 Benzidine-d8.CAS number. 92890-63-6.
Use the internal standard solution (see 5.9.4) to prepare a solution which has a mass
concentration of 0.5 mg/mL. Benzidine-d8 is a suitable indicator of late-eluting
aromatic amines in the gas chromatogram (see 8.3).
5.10 Sodium hydroxide aqueous solution. It has a mass fraction of 10%.
6 Instruments and equipment
6.1 Reactor. 20 mL ~ 50 mL, which is made of heat-resistant glass, with a sealed stopper.
6.2 Constant temperature heater. It is capable of controlling the temperature at (70 ±
2) °C.
6.3 Glass or polypropylene column. It has an inner diameter of 25 mm ~ 30 mm and a
length of 130 mm ~ 150 mm; it is filled with about 20 g diatomaceous earth (see 5.7),
with glass fiber filter at the outlet. The finished diatomaceous earth column can be used
directly, or 20 g diatomaceous earth can be filled in the glass or polypropylene column
to make the extraction column.
6.4 Vacuum rotary evaporator. It is equipped with vacuum control and water bath. Other
evaporation devices can also be used, such as nitrogen blower equipped with water bath
and nitrogen flow control.
6.5 Pipette. Choose different specifications of pipettes or adjustable pipettes as needed.
6.6 Chromatograph, optional.
6.6.1 High performance liquid chromatograph (HPLC). It is equipped with diode array
detector (DAD) or mass selective detector (MS).
6.6.2 Gas chromatograph (GC). It is equipped with mass selective detector (MS).
6.7 Polytetrafluoroethylene (PTFE) filter membrane. It has a pore size of 0.22 μm, 0.45
μm or other applicable specifications.
All colors of the sample shall be measured, including pigmented products (see
Appendix F).
Natural and uncolored fibers, yarns, fabrics are considered to be free of azo dyes and
are not measured. It shall be noted that "light-color...