Method for quickly screening and detecting azo dyes forbidden in textile materials, leathers and dyes using gas chromatography mass spectrometry

A gas chromatography and azo-free technology, applied in the field of chemical analysis and detection, can solve the problems of large detection scale, high reagent consumption, low positive rate, etc., achieve the effect of large consumption of reagents and materials, and shorten the processing time

Active Publication Date: 2012-11-28
南京海关工业产品检测中心
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is aimed at the low positive rate and large detection scale of banned azo dyes in products such as textiles, leather and dyes, as well as the long detection time, many detection standard methods, high c

Method used

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  • Method for quickly screening and detecting azo dyes forbidden in textile materials, leathers and dyes using gas chromatography mass spectrometry
  • Method for quickly screening and detecting azo dyes forbidden in textile materials, leathers and dyes using gas chromatography mass spectrometry
  • Method for quickly screening and detecting azo dyes forbidden in textile materials, leathers and dyes using gas chromatography mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] Embodiment 1: Actual sample detection

[0080] (1) Reagent preparation:

[0081] Sodium citrate buffer (0.06 mol / L, pH=6): Take 12.526 g of citric acid and 6.320 g of sodium hydroxide, dissolve in water, and dilute to 1000 mL.

[0082] 20 mg / L 2,4,5-trichloroaniline internal standard working solution: Dissolve 20 mg 2,4,5-trichloroaniline in ethyl acetate, and dilute to 1000 mL.

[0083] 2 mg / L 2,4,5-trichloroaniline internal standard working solution: draw 1 mL of 2,4,5-trichloroaniline internal standard working solution with a concentration of 20 mg / L into a 10 mL volumetric flask, and use Dilute to the mark with ethyl acetate and mix well.

[0084] 22 kinds of aromatic amine standard substance concentrations are 20 mg / L mixed standard working solution: 24 kinds of prohibited aromatic amine standard substances (shown in Table 1) except o-aminoazotoluene, 5-nitro - 21 kinds of prohibited aromatic amine standard substances and aniline except o-toluidine and 4-aminoaz...

Embodiment 2

[0110] Embodiment 2: Detection of 4-aminoazobenzene

[0111] Using the method of the present invention, although o-aminoazotoluene and 5-nitro-o-toluidine can be further decomposed and difficult to be directly detected, they can be decomposed by a detector to produce o-toluidine and 2,4-diaminotoluene in the form of Indirect method detection. For 4-aminoazobenzene, the amount of aniline detected by the detection method of the present invention is used to determine whether to further use the existing 4-aminoazobenzene detection standard for detection.

[0112] Table 5 Contains 4-aminoazobenzene positive sample to detect aromatic amine value through detection method of the present invention and standard method

[0113]

[0114] At present, the limit of 4-aminoazobenzene in the European Union is 30 mg / kg, and the limit of 4-aminoazobenzene in my country is stricter - 20 mg / kg. In Table 5, when the content of 4-aminoazobenzene is lower than 20 mg / kg, its decomposition product...

Embodiment 3

[0115] Embodiment 3: comparison of technical parameters

[0116] Table 6 Comparison of technical parameters for the detection of prohibited azo dyes in samples

[0117]

[0118] Through the standard recovery test and the analysis of Examples 1-2, the method of the present invention can be used as 14 standards such as the detection of azo dyes and the detection of 4-aminoazobenzene in 3 types of products commonly used at home and abroad, such as textiles, leather and dyes. Compared with the standard method, the method of the present invention has the advantages of high sensitivity, high recovery rate and high extraction efficiency.

[0119]Through the comparison of the method of the present invention in Table 6 with the representative EU standard EN 14362:2003 on the technical parameters of sample pretreatment, it is found that the method of the present invention also has the following advantages: 1), single-sample detection cost (excluding The labor cost saved) was reduced...

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Abstract

The invention discloses a method for quickly screening and detecting azo dyes forbidden in textile materials, leathers and dyes using gas chromatography mass spectrometry, which comprises the following steps: 1) preparing a sample, 2) subjecting the sample to reduction reaction, 3) extracting the sample, 4) performing the gas chromatography mass spectrometry on the sample, 5) screening decision: compared with the GC-MS analysis result of a standard solution, if the retention time and the mass spectrum of the aromatic amine in the sample keep with standards, the sample is judged as a suspicious positive sample, otherwise it is a negative sample and directly judged as a qualified sample. The sample pre-treatment time is shortened, the cost is reduced, the detection time is shortened, the operation step is simple, the operation is convenient, the operation time is short, the operation cost is low, the detection efficiency is improved; the aromatic amine in the sample is detected by a gas chromatography mass spectrometer, color interference problem is not existed, the sample matrix is effectively prevented from being infected, and the judgment accuracy is high, thus the method is not only suitable for textile materials, but also suitable for other products such as leathers and dyes.

Description

technical field [0001] The invention relates to the technical field of chemical analysis and detection, in particular to a rapid screening and detection method for prohibited azo dyes in textiles, leather and dyes by using gas chromatography-mass spectrometry (GC-MS). technical background [0002] Banning azo dyes is one of the earliest and most important safety items. The "Food and Consumer Goods Act (Second Amendment)" promulgated by the German government on July 15, 1994 prohibits the use of azo dyes that can be decomposed to generate carcinogenic aromatic amines in daily necessities such as textiles and leather. The European Union formulated Directive 2002 / 61 / EC in 2002, stipulating that the content of 22 banned aromatic amines that can be decomposed by azo dyes used in daily consumer products shall not exceed 30mg / kg. my country's mandatory standard GB 18401-2003 "National Basic Safety Technical Specifications for Textile Products" limits the content of 24 prohibited a...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 丁友超曹锡忠钱凯
Owner 南京海关工业产品检测中心
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