【作者】 史春丽；

【导师】 高楼军；

【作者基本信息】 延安大学 ， 分析化学， 2011， 硕士

【摘要】 本文采用溶剂浮选法对石化地区水体中的烷基酚(壬基酚、辛基酚)、双酚A、氯苯类(对二氯苯、三氯苯、六氯苯、对氯苯酚)7种环境激素进行分离富集,并用高效液相色谱法对其各组分进行定量分析。在溶剂浮选条件优化实验中,分别考察了浮选溶剂、试液pH、氮气流速、浮选时间及离子强度调节剂NaCl等因素对溶剂浮选效率的影响。在高效液相色谱的条件优化实验中,考察了流动相组成及比例、温度等的影响。采用溶剂浮选法分离富集水体中壬基酚、辛基酚和双酚A,优选出最佳浮选条件为:浮选溶剂为正辛醇,试液pH为3,氮气流速为60 mL/min,浮选时间为70 min,不加电解质。高效液相色谱优化的最佳条件为:流动相为甲醇-水(体积比为85:15),采用等度洗脱,流速为1.0 mL/min,检测波长为220 nm,温度为20℃,进样量20μL。采用所述方法对石化地区(延安炼油厂)的水样进行测定,测得双酚A,辛基酚,壬基酚检出限(LOD)分别为0.03μg/L,0.25μg/L,0.21μg/L,样品加标回收率为83.1%～110.4%,RSD为4.2～5.9 %。同时将该测定方法用于测定石化地区水体中氯苯类环境激素。主要研究对象为对二氯苯,1,2,4─三氯苯,六氯苯和对氯苯酚四种环境激素。实验得出最佳浮选条件为:浮选溶剂为石油醚,试液pH为3,氮气流速为70 mL/min,浮选时间为80 min,不加电解质。最佳色谱检测条件为:流动相为乙腈-水(80:20),采用等度洗脱,流速为1.0 mL/min,检测波长为220 nm,温度为40℃,进样量20μL。采用所述方法对石化地区附近五个采样点的水样进行测定,测得对氯苯酚的检出限为0.0475μg/L(n=9);对二氯苯的检出限为0.0198μg/L(n=9);1,2,4-三氯苯的检出限为0.018μg/L(n=9);六氯苯的检出限为3.91 ng/L(n=9)。样品加标回收率为82.9%～98.6%,RSD为0.82%～3.42%。本文所建立的溶剂浮选-高效液相色谱法(Solvent Sublation-High Performance Liquid Chromatography)同时测定水体中的环境激素的方法,实现了对石化地区水体中酚类和氯苯类化合物含量的测定。方法简便快速,成本低廉,灵敏度高,准确度好,具有实际应用价值。更多还原

【Abstract】 In this paper, Separation and Enrichment of alkylphenols(nonylphenol and octylphenol), bisphenol A and chlorobenzene (p-dichlorobenzene, hexachlorobenzene, chlorophenol, trichlorobenzene) organic pollutants in water by solvent sublation. and quantitative analysis of active ingredients by high performance liquid chromatography. In the experiment, Optimization of solvents, test solution pH, nitrogen flow rate, sublation time and ionic strength and other factors . Optimization of HPLC conditions in the experiment, investigated the proportion of mobile phase composition and temperature and other effects.Separation and enrichment of Nonylphenol, Octylphenol and Bisphenol A in water by solvent sublation , determination of content of each component with high performance liquid chromatography. Sublation conditions of parameters were optimized, octanol of sublation solvent , test solution pH of 3 , Nitrogen flow rate of 60 mL/min, sublation time was 70 min, without electrolyte. The best optimization of HPLC conditions: mobile phase was methanol - water (85:15), using is ocratic elution, flow rate was 1.0 mL/min, detection wavelength was 220 nm, temperature 20℃, injection Volume of 20μL.The method was used for determination of petrochemical refinery water of Yanan , measured bisphenol A, octylphenol, nonylphenol limit of detection (LOD) were 0.03μg/L, 0.25μg/L, 0.21μg/L, the recovery rate was 83.1%~110.4%, RSD 4.2~5.9%.Determination of both the petrochemical area of chlorobenzenes in water environment hormone. Main object of study for the p-dichlorobenzene, 1,2,4─trichlorobenzene, hexachlorobenzene, and p-chlorophenol of four representatives of the organic pollutants. The optimized sublation experimental conditions: solvent sublation of petroleum ether, the test solution pH 3, the nitrogen flow rate of 70 mL/min,sublation time was 80 min, without electrolyte. Optimal chromatography conditions were: mobile phase of acetonitrile - water (80:20), using isocratic elution, flow rate 1.0mL/min, detection wavelength was 220 nm, temperature 40℃, the injection volume was 20μL.In the vicinity of petrochemicals of five water samples were determined by this method , the chlorophenol detection limit was 0.0475μg/L(n=9); dichlorobenzene detection limit was 0.0198μg/L(n=9); 1,2,4-trichlorobenzene detection limit is 0.018μg/L (n=9); HCB detection limit 3.91 ng/L (n=9) . The recovery rate was 82.9%~98.6%, RSD was 0.82%~3.42%.The method which determined petrochemical area of environmental hormones in water by sublation solvent- High Performance Liquid Chromatography was established, Efficient determination of phenols and chlorobenzenes in water. Method is simple, low cost, high sensitivity, good accuracy has practical value.更多还原