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Rapid determination method for content of banned azo dye

A technology that prohibits azo and fast determination, is used in measurement devices, material separation, analysis materials, etc. It can solve the problems of long test process and shorten the analysis time of gas chromatography-mass spectrometer, achieve low column bleed, overcome the problem of instrument Long analysis process and good selectivity

Inactive Publication Date: 2013-04-10
SGS STANDARD TECHNICAL SERVICES SHANGHAI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the above-mentioned deficiencies, and to provide a rapid determination method for prohibiting the content of azo dyes, which greatly shortens the analysis time of the gas chromatography-mass spectrometer, and solves the existing testing process of the current domestic and foreign testing standards. long question

Method used

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  • Rapid determination method for content of banned azo dye
  • Rapid determination method for content of banned azo dye
  • Rapid determination method for content of banned azo dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1) Preparation of sample spiked solution: Take 1 gram of blank cotton fabric without 24 kinds of aromatic amines in the reactor, add aromatic amines, and the prepared content is 30mg / kg;

[0019] 2) Reduction and extraction: Add 15ml of citrate buffer solution preheated to 70°C in the reactor, seal the reactor and keep it at 70±2°C for 30±1min, then add 3.0ml of 200mg / ml azo component Put the aqueous solution of sodium dithionite, the reducing cleavage agent, into the reactor, shake vigorously and directly keep it at 70±2°C for 30±1min, remove the reactor and cool it to room temperature within 2min;

[0020] Then, add 0.2ml of 10% m / m sodium hydroxide solution to the reaction solution and shake vigorously, transfer the reaction solution to a diatomaceous earth column, and let it fully absorb for 15min, and at the same time add 10ml of methyl tert-butyl ether to the reactor After 15 minutes, transfer the methyl tert-butyl ether and the fiber to the top of the column, col...

Embodiment 2

[0038] 1. Preparation of standard solution: Weigh 0.0100g of 24 kinds of standard aromatic amines, and set the volume to 100ml to obtain a mixed standard solution of 24 kinds of aromatic amines with a solubility of 100mg / L, and then use this solution to reconstitute the concentration of 1mg / L, 5mg / L, 30mg / L three standard solutions;

[0039] 2. Same as Example 1, analysis and qualitative and quantitative test results are shown in Table 2, and the analysis time is 9.15 minutes.

[0040] Table 2: Standard solution recovery rate

[0041]

[0042]

[0043] From above embodiment 1 and embodiment 2 as can be seen, adopt forbidden azo dye content measuring method of the present invention, its analysis time only needs 9.15 minutes, and adopt traditional testing method then need time spent 40-50 minutes, it can be seen The invention can greatly shorten the analysis time of the gas chromatography-mass spectrometer, and it can be judged from the test results that the recovery rat...

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Abstract

The invention relates to a rapid determination method for content of a banned azo dye. The method comprises the following steps that a sample solution is prepared and subjected to reduction and extraction; a sample concentrated solution is obtained; for gas chromatography and mass spectrometry conditions, helium serves as carrier gas, and a gradient temperature rise mode is adopted; a DB-35 capillary column serves as a chromatographic column; an EI (electron impact) serves as an ion source, and an ionization mode serves as a normal mode; the flow velocity is 1ml / min, and the split ratio is 15:1; a full scan mode serves as a data acquisition mode; and the sample concentrated solution is injected into a gas chromatography and mass spectrometry instrument, subjected to qualitative analysis according to retention time of a banned azo compound on the chromatographic column and a mass spectrogram, and then subjected to quantitative analysis by an internal standard method according to a peak area of the banned azo compound on the chromatographic column. Compared with the traditional detection technique, the rapid determination method greatly shortens the analysis time of the gas chromatography and mass spectrometry instrument, solves the problem of long testing flow existing in domestic and foreign detection standards at present, and achieves good separation; the selectivity is good; and the recovery rate meets the requirements.

Description

[technical field] [0001] The invention relates to the technical field of textile azo dye detection, in particular to a rapid determination method for prohibited azo dye content. [Background technique] [0002] Azo dyes (AZO for short) are the most widely used synthetic dyes in the printing and dyeing process of textiles and clothing. They are used for dyeing and printing of various natural and synthetic fibers, and are also used for coloring paint, plastic, rubber, etc. Under special conditions, azo dyes can decompose and produce more than 20 kinds of carcinogenic aromatic amine compounds. cancer. [0003] In 1994, the German government officially banned the use of certain azo dyes in consumer products that have long-term contact with the skin in the "Food and Daily Consumer Products" regulations. In 2002, my country also drafted the national standard of "Basic Safety Technical Requirements for Textiles". On September 11, 2002, the European Commission issued Order No. 61,...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 施冲杰郑爱明汪慧春
Owner SGS STANDARD TECHNICAL SERVICES SHANGHAI CO LTD
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