Study On The Determination Method And Content Of Fluorine Compounds In Sewage And Sludge From Textile Factory

Perfluorinated compounds(PFCs)are a kind of organic compounds composed of fluorine and carbon atoms,which are widely used in textile,leather,printing and dyeing and other pillar industries of national economy.PFCs in the environment mainly include perfluoropolymers,perfluoroamides,perfluorosulfonic acids,perfluorocarboxylic acids,etc.Existing reports have confirmed that PFCs are widespread in environmental media such as water and soil.There are many textile enterprises in the Yangtze River Delta,with a large output.The existing standard test methods for sewage sludge cover a narrow range,usually more than ten kinds,and the detection limit is high.It is of great significance to research and develop high sensitivity,fast and efficient methods for the effective monitoring of PFC emissions of enterprises.The method of 33 fluorine-containing compounds in sewage sludge of textile factory were established,and a perfect detection system was established.The main results are as follows:(1)For PFC compounds,solid-phase extraction method was used,then elution with methanol solution,constant volume,separation and determination by HPLC/MS/MS.Linear and working range:1 μg/L～30 μg/L,R2>0.99;for wastewater sample,recovery range:51%～99.0%,precision range:5%～19%,MDL range:0.0017-0.005 μg/L;LOR range:0.068-0.02 μg/L;for soil after drying,recovery range:51-101%,precision range:7%-25%,MDL range:0.023-0.15 ng/kg,LOR range:0.091-0.58 ng/kg.(2)For FTOH/FTA perfluorocarbons,the extract was concentrated,catalysed by 4-2-methylaminopyridine,derivatized by acetic anhydride,and determined by GCMS.Linearity and working range are 20 μg/L～2000 μg/L,R2>0.990;for wastewater samples,the recovery range is 60%～140%,precision range is 3.0%～17%,MDL range is 0.0070～0.0240 μg/L,LOR range is 0.027～0.096 μg/L;for soil samples,the recovery range is 60%～140%,precision range is 3.4～20%,and MDL range is 0.00029～0.00078 mg/kg,LOR range:0.0012～0.0031 mg/kg.(3)Several hundred times of influent and effluent from ten factories,33 kinds of PFCs in influent and effluent before and after sewage treatment and sludge discharged were tested,which fully verified that the detection method has the advantages of wide range of detection concentration,strong applicability,high efficiency and low detection limit.