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GB/T 23344-2009 English PDF (GBT23344-2009)

GB/T 23344-2009 English PDF (GBT23344-2009)

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GB/T 23344-2009: Textiles -- Determination of 4-aminoazobenzene

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.
GB/T 23344-2009
GB
ICS 59.080.01
W 04
NATIONAL STANDARD
OF THE PEOPLE REPUBLIC OF CHINA
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; carry out qualitative determination by using the gas chromatograph (GC/MSD) with mass selective detector; if necessary, select high performance liquid chromatography - diode array detector (HPLC/DAD) to carry out the determination of isomer. Carry out the quantitation by gas chromatography - mass spectrogram internal standard method or high performance liquid chromatography external standard method.
Annex A
(Informative)
Reduction treatment method after specimen extraction
A.1 Reagent
A.1.1 Chlorobenzene, analytically pure.
A.1.2 Dimethylbenzene (isomer mixture), analytically pure.
A.1.3 Methanol.
A.2 Instruments and equipment
A.2.1 Extraction device. adopt the extraction device specified in GB/T 17592. A.2.2 Vacuum rotary evaporator.
A.2.3 Ultrasonic bath. frequency is 40 kHz.
A.3 Sample pre-treatment
A.3.1 Pre-treatment of the sample
Take representative sample; cut it into strip-shape of 40 mm?? 5 mm or other proper sizes; mix them. Weigh 1.0g (to 0.01g) of the mixed sample; tighten it with colourless yarn; place it in the extraction device (A.2.1) to make that condense solvent is able to flow through the sample.
A.3.2 Extraction
Add 25mL of chlorobenzene (A.1.1); heat it to make chlorobenzene to boil slightly; extract for 30min. Or extract for 45min with dimethylbenzene (A.1.2). Cool the raffinate to room temperature; remove solvent in vacuum rotary evaporator (A.2.2); transfer its residue with 7mL of methanol (A.1.3) into the reactor (5.1). Note. Transfer extract liquor to the rotary evaporator for concentration (suggested at 45??C ~60??C ) to near dry; transfer in quantitative residues with 7mL of methanol in several times to the reaction flask; ultrasonic bath may be adopted for auxiliary dissolution. A.3.3 Reduction decomposition
Add 9.0mL of sodium hydroxide solution (4.4) in the reactor; seal the reactor; and shake it forcibly. Unwrap the bottle cap; add again 1.0mL of sodium dithionite solution (4.5); seal the reactor and shake it slightly to make solution well mixed. Place it in thermostatic water-bath (5.2); maintain the temperature for 30 min; take out and cool Annex D
(Informative)
Recovery rate
In the direct reduction treatment of specimen (according to 6.1), add 5 mg/kg~100mg/kg 4-aminoazobenzene in the sample. The method?€?s recovery rate is 60%~80%.
In the reduction treatment (according to Annex A) after the specimen is extracted and dyed, add 5 mg/kg~100mg/kg 4-aminoazobenzene in the extracted dye, the method?€?s recovery rate is 90%~100%.

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