The AQSIQ Science and Technology Project "Development of a series of rapid detection kits for harmful substances in ecological textiles" completed by Shandong Inspection and Quarantine Bureau systematically studied the color determination methods of banned azo dyes in textiles , Fast, no need of large instruments and equipment, high sensitivity of dyed textiles, banned azo dye rapid screening test kit, achieved a major breakthrough in dyed textiles banned azo dye detection technology, opened up a convenient and fast, strong applicability Qualitative screening test method.
Prohibition of azo dyes refers to a class of azo dyes that may produce carcinogenic aromatic amines after cleavage and change the structure and function of human DNA through activation, which ultimately cause human disease and cancer. These dyes are one of the most important quality control items in the current international textile and apparel trade and one of the most basic quality indicators of ecological textiles.
Traditional technology is long and expensive
China's mandatory national standard GB 18401 "National Textile Product Basic Safety Technical Specifications", Germany's "Food and Consumer Goods Law", the European Union's Eco-Lable and the most widely used textile eco-label Oeko-Tex Standard 100 "Ecological Textiles Standard 100 and other domestic and foreign laws and regulations have listed it as a ban, and it has become one of the most important items for import and export textiles.
The types of carcinogenic aromatic amines currently banned have increased to 24. Among them, except for the 4-aminoazobenzene detection method, which needs to be tested separately, the other 23 kinds of aromatic amines can be tested at the same time. For the detection of banned azo dyes, the conventional method is to use gas chromatography, liquid chromatography, gas chromatography / mass spectrometry, liquid chromatography / mass spectrometry and other chromatographic instruments to determine the sample after reduction. The method is mature, accurate and highly sensitive. However, the pre-processing is complicated, the equipment needs to be precise, the inspection period is long, and the inspection cost is high. It requires professional technical personnel and harsh conditions. From the perspective of the detection of the ban of azo dyes in textiles in recent years, on the one hand, the detection business volume has increased exponentially, and the detection pressure has increased dramatically; on the other hand, the positive detection rate has decreased year by year, and the work of accurate quantitative analysis has been greatly reduced.
In view of the above problems, the establishment of a rapid screening method with simple procedures and low cost that does not depend on large chromatographic instruments is an urgent need for the detection of banned azo dyes in textiles.
Quick and inexpensive screening of aromatic amines
Prohibited azo dye detection kit technology proposes a rapid detection method for banned azo dyes in dyed textiles, which solves the dependence of traditional measurement methods on large chromatographic instruments and meets the needs of current rapid screening.
Based on the structural characteristics of aromatic amines, the kit technology introduces a diazotization-coupling color reaction mechanism to effectively optimize the conditions of the diazotization reaction and coupling reaction. The liquid-liquid extraction technology of tert-butyl methyl ether and hydrochloric acid is used to achieve aromatic amines Extraction and decolorization of the reaction solution, using o-methoxyphenol as the color reagent, the aromatic amine is determined by color development. Established a rapid screening and detection method for banned azo dyes in dyed textiles, and achieved a major breakthrough in the detection technology of banned azo dyes in dyed textiles.
This technology is compared with the current domestic and foreign methods for prohibiting the detection of azo dyes: no chromatographic instrument is required, the instrument is only a reducing water bath, and the instrument cost is less than 1% of the existing instrument detection method; the pretreatment steps are simplified to reduction and extraction Two steps of decolorization, simple operation, the time to detect one sample is only 34% to 40% of the existing method; no aromatic amine standard, diatomaceous earth extraction column, etc., the reagent consumption is small, and the cost of the required reagent is only current 3% -8% of the detection methods (Taking the Shandong Inspection and Quarantine Bureau Technology Center as an example, a total of 4,000 batches of azo samples were tested in 2011. Using this technology with only one reagent can save costs 220,000.) The method is simple, fast, and low cost. Achieve the rapid screening test of textiles banned azo dye detection.
The research results have broad application prospects
The technology has been tested on thousands of actual samples in the Technical Center of Shandong Inspection and Quarantine Bureau, and also in the Technical Center of Jiangxi Entry-Exit Inspection and Quarantine Bureau, Jiangsu Technical Center of Entry-Exit Inspection and Quarantine, Zhejiang Technical Center of Entry-Exit Inspection and Quarantine, Shanghai Tian Six units including Xiang Group, Qingdao Textile Fiber Inspection Institute and Shandong Inspection and Certification Group Shandong Inspection Co., Ltd. conducted on-site method verification. The research team brought the kit and experimenters, and took more than 20 blind samples from each daily sample for actual field testing. The test results of the kit were compared with the results of the actual instrument test. The verification result is: 42 positive samples are detected, and the detection rate of the method is 100%, without false negatives. Test 1040 negative samples, 285 samples showed false positive results, the probability of false positives was 27%.
In March 2013, at the textile professional committee working meeting and standard review meeting, the technology was introduced again due to the opening of the standard. The technical personnel of the first-line brother units engaged in the testing of textile azo dyes were extremely interested and asked for a kit to send them back to try. At present, the three units have actually applied and feedback the results. The general response method is simple, fast, and practical. It is recommended to transform it into product promotion and application as soon as possible.
The research results of this project have broad application prospects. On the one hand, for testing institutions, it can shorten the inspection cycle of textiles and clothing, reduce inspection costs, and meet the current high-throughput, low-cost inspection needs. On the other hand, the inspection of hazardous substances in textiles and clothing can be extended to factories, workshops, warehouses, cargo plants, etc. in advance. China's textile industry has the characteristics of small scale and large number of enterprises. Carrying out rapid testing is conducive to the selection of raw materials, improve product quality and improve the market competitiveness of enterprises, help enterprises to control quality, reduce losses, and protect the health of our people It is of great significance to protect foreign trade exports.
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The research group declared the national invention patent "Quick Detection Method of Prohibited Azo Dyestuffs in Dyed Textiles" and was authorized (patent number: ZL 201110350255.7). "Rapid determination of banned azo dyes in textiles-kit screening method" (2012B406) was transformed into an inspection and quarantine industry standard, and published an article in "Analytical Chemistry" with the highest impact factor in domestic chemical journals: "Based on diazotization- "Qualitative Screening Method for Prohibiting Azo Dyes in Textiles Coupling with Color Reaction" is included in SCI. With the help of patents, standards and articles, it has been widely and effectively promoted in and outside the industry. The research group was also invited to participate in the "2013 International Inspection and Testing Technology and Equipment Expo and National Inspection and Testing Academic Conference", and gave a special speech on the rapid inspection technology at the meeting.
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