GB/T 17592-2011 English PDF (GBT17592-2011)

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GB/T 17592-2011: Textiles -- Determination of the banned azo colorant
GB/T 17592-2011
GB
ICS 59.080.01
W 04
NATIONAL STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
Replacing GB/T 17592-2006
Textiles - Determination of the Banned
Azo Colourants
ISSUED ON. DECEMBER 30, 2011
IMPLEMENTED ON. SEPTEMBER 1, 2012
Jointly issued by. General Administration of Quality Supervision,
Inspection and Quarantine of the People's Republic of
China (AQSIQ);
Standardization Administration of China (SAC).
Table of Contents
Foreword ... 3 
1 Scope ... 5 
2 Normative References ... 5 
3 Principle ... 5 
4 Reagents and Materials ... 5 
5 Equipment and Instruments ... 7 
6 Analytical Procedures ... 7 
7 Result Calculation and Expression ... 10 
8 Lower Limit of Determination ... 11 
9 Test Report ... 11 
Appendix A (Normative) Carcinogenic Aromatic Amine Names and GC/MS Qualitative
Selected Characteristic Ion of Their Standard Substances ... 13 
Appendix B (Informative) Pre-treatment Method for Polyester Sample ... 15 
Appendix C (Informative) Chromatogram of Carcinogenic Aromatic Amine Standard
Substances ... 17 
Foreword
This Standard is drafted in accordance with regulations given in GB/T 1.1-2009.
This Standard is the revision of GB/T 17592-2006 "Textiles - Determination of the
banned azo colourants". Compared with GB/T 17592-2006, the main technical
changes are as follows.
- The normative reference GB/T 23344 "Textiles-Determination of
4-aminoazobenzene" has been added (See Chapter 2);
- In Chapter 5, temperature-control ultrasonic generator has been deleted (See 5.1
of the 2005 edition);
- The pre-treatment provisions for polyester products have been deleted, which act
as the notes in 6.1 (See 6.1.1 of 6.1 in the 2006 edition);
- Preparation methods for mixing standard working solution have been added (See
4.5.4);
- The expressions of gradient i) in the analysis methods for HPLC/ DAD have been
amended (See 6.4.1; 6.4.1 of 2006 edition);
- Footnote a in Appendix A has been added; Note 2 has been amended (See
Appendix A);
- Appendix B has been changed into informative appendix (See Appendix B;
Appendix B of 2006 edition);
- The liquid chromatogram of carcinogenic aromatic amines standard substance
has been added (See Appendix C).
This Standard was proposed by China National Textile and Apparel Council.
This Standard shall be under the jurisdiction of basic standard subcommittee of
Technical Sub-Committee on Textiles of Standardization Administration of China
(SAC/TC 209/SC 1).
Drafting organizations of this Standard. Shanghai Textile Science Research Institute,
Standardization Institute of Textile Industry, and Standardization Institute of Textile
Industry.
Chief drafting staffs of this Standard. Chen Yun, Zheng Yuying, Yang Haiying, Zhu
Ying, and Zhang Xiaoyan.
Textiles - Determination of the Banned Azo Colourants
WARNING. The personnel using this Standard shall have practical experiences
in regular laboratory work. This Standard does not point out all the possible
safety problems. The users shall be responsible for taking appropriate safety
and health measures and ensure to comply with the conditions specified in the
relevant laws and regulations of the nation.
1 Scope
This Standard specifies the detection methods for the banned azo colourants (in
textile products) which can decompose carcinogenic aromatic amines (see Appendix
A).
This Standard is applicable to the textile products after dyeing and printing.
2 Normative References
The following documents are essential to the application of this document. For dated
references, only the dated edition of the document is applicable to this Standard. For
undated references, the latest edition (including all the amendments) of the document
is applicable to this Standard.
GB/T 6682 Water for analytical laboratory use - Specification and test methods
GB/T 23344 Textiles-Determination of 4-aminoazobenzene
3 Principle
Textile sample uses sodium dithionite for reduction and decomposition to generate
potential carcinogenic aromatic amine in the medium of citrate buffer solution; extract
aromatic amine in the solution with proper solution - solution partition column. And
scale the volume with appropriate organic solvent after concentrating; carry out
determination with gas chromatograph (GC/MSD) which is equipped with mass
selective detector. If necessary, select another method or more methods to determine
the isomer. Carry out quantification with high pressure liquid chromatography - diode
array detector (HPLC /DAD) or gas chromatography - mass spectrograph.
4 Reagents and Materials
4.1 General rules
disodium hydrogen phosphate in 1000 mL of Grade 2 water, pH =6.9;
i) Gradient. at starting, use 15% mobile phase A and 85% mobile phase B; then
linearly change the gradient into 80% mobile phase A and 20% mobile phase B.
Maintain for 5 min.
Accurately transfer 1 mL of methanol or other appropriate solvent to add it into the
round-bottom flask (6.2.2) that has been concentrated to nearly dry. Mix the solution
uniformly. Stand at still. Then take 1 μL of standard working solution (4.6.2) and
sample solution respectively. Inject them in the chromatograph. Operate according to
the above-mentioned conditions. Carry out qualitative determination by external
standard method.
Note. When the above-mentioned analytical conditions are adopted, chromatogram of
carcinogenic aromatic amine standard substance HPLC is detailed in Figure C.2 in Appendix
C.
6.4.2 GC/MSD analysis method
Accurately transfer 1 mL of internal standard solution to add it into the round-bottom
flask (6.2.2) that has bee concentrated to nearly dry. Mix the solution uniformly. Stand
at still. And then take 1 μL of mixing standard working solution and sample solution
respectively. Inject them into the chromatograph. Operate according to the conditions
of 6.3.1. Ion mode may be selected to carry out thee qualitative determination.
Grouping of internal standard quantitative is detailed in Appendix D.
7 Result Calculation and Expression
7.1 External standard method
The aromatic amine i content separated from the sample shall be calculated
according to Formula (1).
mA
VcAX
iS
i 
 (1)
Where.
Xi - Content of aromatic amine i separated from the sample, (mg/kg);
Ai - Peak area (or peak height) of aromatic amine i in sample solution;
ci - Concentration of aromatic amine i in standard working solution, (mg/L);
V - Final volume of sample solution, (mL);
AiS - Peak area (or peak height) of aromatic amine i in standard working solution;
m - Sample mass, (g).
7.2 Internal standard method
The aromatic amine i content separated from the sample shall be calculated
according to Formula (2).
iSSiS
iSCii
i AmA
AVcAX 
 (2)
Where,
Xi - Content of aromatic amine i separated from the sample, (mg/kg);
Ai - Peak area (or peak height) of aromatic amine i in sample solution;
ci - Concentration of aromatic amine i in standard working solution, (mg/L);
V - Final volume of sample solution, (mL);
AiSC - Peak area of internal standard in standard working solution;
AiS - Peak area (or peak height) of aromatic amine i in standard working solution;
m - Sample mass, (g).
AiSS - Peak area of internal standard in sample solution.
7.3 Result expression
Test results shall be expressed with the inspection results of various aromatic amines.
The calculated results shall ...