The Determination Of Organic Halogen Compounds In Textiles By Ion Chromotography Method

The organic halogen compounds in textile has a growing influence on human health and the environment, and thus many countries and institutions has issued numerous restrictions, regulations and testing standards on the organic halogen compounds. However the current determination methods can hardly meet the testing requirements due to the variety of organic halogen compounds. In this paper, an efficient detection method was established. While performing this method, the organic halogen compounds were oxidized and cracked into inorganic halide ions, and then the ions was analyzed by ion chromatography (IC). Total organic halogen compounds (TOX) can be determined accurately via this method, including total organic chlorine (TOC1) and total organic bromine (TOBr). Therefore this TOX-determination method has important significance in the evaluation of ecological textiles.First of all, oxygen bomb combustion - ion chromatography method was established to determine total organic chlorine (TOC1) in textiles. After comparing the organic halide’s recovery rate between oxygen bomb combustion method and tube furnace combustion method, it’s been found that the recoveries of spiked samples were low and unstable when using tube furnace combustion method. Comparatively oxygen bomb combustion method takes less time and the recoveries are above 70%, which obviously meets the detection requirements.Taking pentachlorophenol (PCP) as the research object, the accumulated oxygen bomb combustion-ion chromatography method was established. Regarding the fluctuation test results of samples in low concentration, accumulated oxygen bomb combustion method was used to increase the tested samples’mass, thus to improve the stability of the samples’test results in low concentration. Results showed that, when the sample was added 5 times, the detection limit has extended from 250μg/L to 10μg/L. In the detection range of this method (10-1000μg/L), the recoveries of the sample are between 88.68% -106.58%. And the results of repeatability and reproducibility test under different concentrations showed that the sample recoveries were 87.54%-129.36% and 86.66%-125.32% respectively, and the relative standard deviation (RSD) were 9.29%-16.03% and 8.80%-11.16% separately. The accumulated oxygen bomb combustion - ion chromatography method was used to determine the content of Pentachlorobenzene (PCB), tetrachlorophenol (TeCP) and trichlorophenol (TriCP), and the results also meet testing requirements.Second, the oxygen bomb combustion - ion chromatography method was established to determine TOBr in textiles. Taking hexabromocyclododecane (HBCDD), tetrabromobisphenol A (TBBPA) and 2,2’,6,6’-tetrabromobisphenol A diallylether as the research objects, determining samples’contents with the same method used in TOCl’s determination, all the TOBr’s recoveries were around 50%. After a systematic analysis of redox properties among oxygen, bromine and chlorine, an improved oxygen bomb combustion - ion chromatography method was established. In the new method, the step of using oxygen driving out air from bottle was removed, and the optimum oxygen pressure for the highest recoveries of TOBr is 2.5 MPa. When determining the content of HBCDD via this method, the detection range is 100-1000 μg/L, and the recoveries is 75.44%-101.51%. The results of repeatability and reproducibility test under different concentrations showed that HBCDD recoveries are 70.82%-109.17% and 71.54%-110.08% respectively, and the relative standard deviation (RSD) are 4.12%-15.36% and 5.96%-16.77% separately, which proved the experimental data stable. The extended test results of TBBPA and 2,2’,6,6’-tetrabromobisphenol A diallylether showed that the single standard and mixed standard samples’recoveries are 72.01%-93.13% and 89.94%-102.96%, which comply with testing requirements. To sum up, the improved method is suitable for determining various TOBr in textiles.Finally, fabric sample added with mixed PCP/HBCDD standard solution was treated with accumulated oxygen bomb combustion method. The recovery rate of PCP was detected by IC. When the sample is added 5 times, the recovery of PCP is 98.39%-107.98%, and RSD is 4.02%. When the fabric sample is treated with oxygen bomb combustion method without driving out air in bottle, HBCDD’s recovery is 85.96%-98.40%, and RSD is 5.22%. The results above proved that the methods established in this paper are suitable for determination of TOC1 and TOBr in textiles.