| Through fiber processing,spinning,weaving,dyeing,as well as finished product processing and a series of production links,textiles can be converted from fiber raw materials into finished products.Ethylenediaminetetraacetic Acid(EDTA)and Diethylenetriaminepentaacetic Acid(DTPA)are used in industrial production of complexing agent(commonly used sodium salt).In the textile production,it is mainly used to remove calcium and magnesium ions in water,and is also used for softening water quality,stabilizing agent and cleaning agent.They are very stability in the environment,and are not easy to be degraded,remaining in the environment in a long time,which caused harm to human health and ecological environment.Oeko-tex standard 1000 explicitly states that EDTA and DTPA are to be detected and the European Commission on textiles eco label(Eco-label)(2002/371/EC resolution)requires textiles shall not contain EDTA and DTPA At present,the most commonly used pretreatment method for Ethylene Diamine Detraacetic Acid(EDTA)and diethylenetriaminepentaacetic acid(DTPA)is combined with heavy metal ions to form a stable chelate,and then use a liquid chromatography for qualitative and quantitative analysis.But this method not only has long complexing time,but also has a high salt content in the liquid sample analysis,and it can be used seriously for a long time.Aiming at the finishing agent of harmful substances in EDTA and DTPA deficiency of current detection methods,this study establishes two kinds of pretreatment method:(1)The pretreatment of dyeing and finishing auxiliaries was carried out by acidification and esterification,and the methods for the determination of EDTA and DTPA were established by gas chromatography-mass spectrometry.The results show that this method has good reproducibility,high sensitivity,can replace the existing defects of the instrument has been contaminated by liquid chromatography,EDTA and DTPA for other areas to provide reference data;the application of the method to the analysis of common dyeing and finishing auxiliaries samples in some samples detected by EDTA.The method quantification limit of EDTA was 0.194 mg/kg and DTPA was 9.62 mg/kg.The recovery rate was 91.6%~94.9%,the relative standard deviation(RSD)was 3.5%~5.2%,which was in accordance with the technical requirements of residue analysis.(2)In boiling water,a pretreatment method for esterification of EDTA and DTPA in dyeing and finishing auxiliaries with n-butyl alcohol / acetyl chloride mixed solution as esterifying agent.An apparatus for the determination of EDTA and DTPA acetylation by gas chromatography-mass spectrometry has been developed.The recoveries are between 91.9%~101% in negative samples,the relative standard deviation was less than 9 %(n=8),the method of quantitative limit of EDTA was 0.498 mg/kg and DTPA was 4.86 mg/kg.This method is accurate,stable,can be used for the determination of EDTA and DTPA in textile dyeing and finishing auxiliaries.The results of this study showed that the detection limit of EDTA and DTPA in dyeing and finishing auxiliaries are not lower than the national and international standards,can effectively get rid of foreign technical barriers,promote China’s textile exports and protect the health of consumers.The precision,recovery rate,linear range of technical indicators reached the requirements of chemical analysis of residues,stable method reliable,accurate,and can be used for determination of qualitative and quantitative analysis of toxic and harmful substances in the dyeing and finishing auxiliaries,and provides strong technical support for textile quality control. |
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