GB/T 23344-2009 PDF English
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| GB/T 23344-2009 | English | 70 |
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Textiles -- Determination of 4-aminoazobenzene
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GB/T 23344-2009: Textiles -- Determination of 4-aminoazobenzene---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT23344-2009
GB
ICS 59.080.01
W 04
NATIONAL STANDARD
GB/T 23344-2009
Textiles - Determination of
4-aminoazobenzene
Issued on. MARCH 19, 2009
Implemented on. FEBRUARY 1, 2010
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... 4
2 Normative References... 4
3 Principles... 4
4 Reagent... 5
5 Equipment and Instruments... 6
6 Analytical Procedures... 6
7 Result Calculation and Expression... 9
8 Detection Lower Limit, Recovery Rate and Precision... 10
9 Test Report... 11
Annex A... 12
Annex B... 14
Annex C... 15
Annex D... 16
Foreword
Annex A, Annex B, Annex C and Annex D in this Standard are informative.
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. Jiangsu Entry-Exit Inspection and Quarantine
Bureau of the people's republic of china, Standardization Research Institute of Textile
Industry, and Jiangsu High Hope International Group.
Chief drafting staffs of this Standard. Cao Xizhong, Ding Youchao, Xu Xinhua, Feng
Quanbing, Qian Kai, Tian Shu, Zhou Jia, and Chen Xiaoding.
Textiles - Determination of 4-aminoazobenzene
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 test methods for determination of the 4-aminoazabenzene
decomposed from some azo dyes in textile products by gas chromatography - mass
spectrogram detection method (GC /MSD) and high performance liquid
chromatography method (HPLC/DAD).
This Standard is applicable to various textile products after dyeing and printing.
2 Normative References
The following documents contain provisions which, through reference in this text,
constitute provisions of this Standard. For dated reference, subsequent amendments
(excluding correction) or revisions of these publications do not be applied. However,
the parties who enter into agreement according to these specifications are
encouraged to research whether the latest editions of these references are applicable.
For undated references, the latest edition of the normative document is applicable to
these specifications.
GB/T 6682 "Water for analytical laboratory use - Specification and test methods"
(GB/T 6682-2008, ISO 3696.1987, MOD)
GB/T 7592 "Textiles ― Determination of the banned azo colourants"
3 Principles
The samples is reduced with sodium dithionite in alkaline medium; the decomposed
4-aminoazobenzene shall be extracted by appropriate liquid-liquid distribution method;
4 Reagent
Except otherwise specified, the reagents used shall be analytically pure, and water
shall be grade 3 water in accordance with those specified in GB/T 6682.
4.1 Sodium chloride
4.2 Tertiary butyl methyl ether (CAS No.. 1634-04-4).
Note. if tertiary butyl methyl ether is not available, fresh ethyl ether may be used to replace it.
Preparation method of fresh ethyl ether. take 500mL of ethyl ether and put it in 1000mL
separating funnel. Add 100mL of 5% ferrous sulfate solution. Shake it violently. Discard the
water layer. Put it in the all-glass device to distill it. Collect the distillate of 33.5°C ~34.5°C.
4.3 Acetonitrile (HPLC Grade).
4.4 Sodium hydroxide solution, 20g/L.
4.5 Sodium dithionite solution (200mg/mL). take sodium dithionite (content of
Na2S204 ≥ 85%), dissolve it with water. Prepare the fresh solution.
4.6 Standard solution
4.6.4 Anthracene-d10 internal standard working solution (2 mg/L). prepare it with
tertiary butyl methyl ether (4.2); this solution shall be prepared when using.
4.6.5 Mixed standard working solution. prepare it with tertiary butyl methyl ether
(4.2).
5 Equipment and Instruments
5.1 Reactor. made of hard glass in shape of tubes with airtight plug, about 65mL.
5.2 Thermostatic water-bath. temperature may be controlled at (40±2)°C.
5.3 Mechanical oscillator. oscillation frequency is about 150 times/min.
6 Analytical Procedures
6.1 Preparation and reduction treatment of specimen
Take representative samples; cut them into the chips of 5 mm× 5 mm; Mix them well;
weigh 1.0g of the mixed sample, accurate to 0.01g;
6.2 Extraction
6.2.1 For gas chromatographic analysis
Add accurately 10mL of anthracene - d10 internal standard working solution (4.6.4) in
the above reactor; add again 7g of sodium chloride (4.1); seal the reactor well; shaken
forcibly for mixing completely; shake for 45min in mechanical oscillator (5.3); Stand at
still; after two-phase layering, take the supernatant liquor for GC/MSD analysis.
6.2.2 For high performance liquid chromatography analysis
Add 10mL of tertiary butyl methyl ether (4.2) in above reactor; add again 7g of sodium
oxide (4.1); seal the reactor; shake for 45min in mechanical oscillator after it is shaken
for mixing; Stand at still; after two-phase layering, take the supernatant liquor through
0.45μm organic filter membrane for HPLC/DAD analysis.
6.3 Gas chromatography - mass spectrometry method
6.3.2 Qualitative and quantitative analysis
Isometric cross injection shall be carried out to the mixed standard working solution
(4.6.5) and the sample test solution (6.2.1); gas chromatograph (5.4) shall be adopted
for its testing and analysis according to the requirements in 6.3.1.
6.4.1 HPLC/DAD analysis conditions
As test result depends on the used instrument, so the general parameters of
chromatographic analysis are impossible to be provided. It has proved that it is
suitable to adopt the following operation conditions in the test.
6 4.2 Qualitative and quantitative analysis
Isometric cross injection shall be carried out to 4-aminoazobenzene standard working
solution (4.6.3) and sample test solution (6.2.2); high performance liquid
chromatograph shall be adopted for its testing and analysis according to the
requirements of 6.4.1.Carry out the qualitative analysis through comparison of the
retention time between the sample and the standard sample, and ultraviolet
spectrogram.
7 Result Calculation and Expression
7.1 External standard method
7.3 Expression of results
Test results shall be expressed in the concentration of 4-aminoazobenzene. The
calculated results shall be expressed to its integer.
8 Detection Lower Limit, Recovery Rate and
Precision
8.1 Detection Lower limit
The detection lower limit in this method is 5 mg/kg.
8.2 Recovery rate
See Annex D.
8.3 Precision
The tests are carried out in the same laboratory; in mutual independence; on the
same tested object;
9 Test Report
The following contents at least shall be given in test report.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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