Application Of GC-MS Technology To The Detection Of Short Chain Chlorinated Paraffins In Textiles

With the increasing prosperity of international trade,the security of the textile import and export has attracted more and more attention.In recent years,a number of import and export of textiles have been detected in the banned hazardous substances,and their ecological security problems caused the textile industry and their related testing agencies of great concern.Short chain chlorinated paraffins?SCCPs?because of their flame resistance,fire resistance,low vapor pressures,low volatility and other characteristics,in the textile is often used as a flame retardant,but it also has remote mobility,persistence,bioaccumulation and toxicity,long-term exposure will be teratogenic,carcinogenic and mutagenic,therefore it has been the EU classified into the prohibit the use of persistent organic pollutants,many countries have limited or banned.At present,the detection technology of short chain chlorinated paraffin in textile is less,and the testing instruments used in each laboratory are different,the validity can't be compared.In this paper,we developed new methods for the detection of short chain chlorinated paraffins in textiles,the first was pretreatment by ultrasonic extraction with n-hexane and purification used florisil column activated by n-hexane,the second was GC/MS detection method in selective ion scanning mode,the third was quantitative analysisi method by qualitative and quantitative ion monitored,manual integratio,and standard curve quantitation.Focused on the research of the quantitative analysis method in SCCPsof different chlorine content.The methods was validated byrecovery and precision,intra-day and inter-day reproducibility,detection limit and quantification limit.The detection method established in this paper was as follows: the conditions of ultrasonic extraction were 30 m L n-hexane,500 W,50 ? and 35 min.The purification was by Florisil column?activated with 4m L n-hexane in advance?,and elution with n-hexane and methylene chloride?V/V,1:1?.GC-MS detective methods was used DB-5 chromatography column,high purity N₂,inlet temperature 270 ?,mass end temperature 280?,ion source temperature 240?;splitless injection,sample volume1?L,carrier gas flow 2.0ml/min;selective ion scanning mode,select the monitoring ions 75,89,95,105;oven temperature program maintained at 90 ? for 1min after heating rate of 40?/min to 280?,for 6min.Quantitative method for the quantitative monitoring of ions under the manual integration,the corresponding standard curve quantitative.Linear detection method in this paper was good,the linear correlation coefficient can reach more than 0.990,the recovery rate was in the range of 92.11%⁹8.95%,the relative standard deviation?RSD/%?were less than 5%,the intra-day and inter-day reproducibility was good,their relative standard deviation was in 4.90%⁵.11% and6.01%⁶.24%,the detection limit was 0.5mg/kg;quantitative limit was 3.5mg/kg.The method established in this paper was simple,rapid,accurate,high sensitivity,and can be used in the detection of SCCPs in textile,which provides a practical technical means for the detection of SCCPs in textiles.