毛细柱气相色谱法测定废水中的三氯乙醛

讨论了用毛细柱气相色谱法测定废水中三氯乙醛的方法。该方法用(2+1)石油醚-乙醚萃取废水中的三氯乙醛,方法的相对标准偏差4.9％,回收率91.2％～101.1％,最低检出限4×10~(-2)ng。     

Determination of organophosphorus pesticides and related compounds in water samples by membrane extraction and gas chromatography

A membrane extraction-gas chromatography method was developed fordetermination of organophosphorus pesticides and related compounds including methamidophos, DDVP, dimethoate, methyl parathion, parathion, thiophosphoric acid trimethyl ester, and thiophosphoramidic acid dimethyl ester in water samples. In thismethod, surface-modified acetic cellulose membranes were used to extract the target analytes in water samples, the extracted analytes were back-extracted into a small amount of methanol, andgas chromatography with pulsed flame photometric detector (GC-PFPD) was used to determine the concentrations of targetanalytes in the extracts. The recoveries obtained for thetarget analytes spiked into the water samples ranged from 66to 94%. The method detection limit for each target analyte was 0.05 g L^-1. The method developed in this study had shown the advantages of being cheap, simple, fast, and reliable. It had been used successfully to determine the concentrations of target analytes in river water samples.     

微波萃取-气相色谱/质谱法测定土壤中的有机氯农药

通过微波萃取提取土壤中的有机氯农药,萃取溶液经浓硫酸脱色、佛罗里硅土柱净化,最后用气相色谱/质谱法分析.以石英砂为基体进行加标回收测定,有机氯农药的回收率在75.5%～103%之间,检出限为0.01μg/kg.     

固相萃取富集高效液相色谱法测定环境水样中的重金属元素

研究了用固相萃取富集高效液相色谱法测定环境水样中痕量重金属镍、铜、银、铅、镉和汞的方法。环境水样中的镍、铜、银、铅、镉和汞用四 -(对二甲氨基苯基 ) -卟啉 (T4 -DMAPP)柱前衍生 ,用C18固相萃取小柱萃取富集镍、铜、银、铅、镉和汞的T4 -DMAPP络合物 ,富集倍数为 1 0 0倍 ,然后用甲醇和四氢呋喃梯度洗脱为流动相 ,WatersXter raTMRP18( 3 9mm× 1 5 0mm)色谱柱为固定相分离 ,用二极管矩阵检测器检测。镍、铜、银、铅、镉和汞的检测限分别为3、2、4、3、1 5ng/L和 3ng/L。方法相对标准偏差为 1 8%— 3 2 % ,标准回收率为 92 %— 1 0 7%。该方法用于测定环境水样中的痕量重金属 ,结果令人满意     

固相萃取-气相色谱法测定水中硝基苯类有机污染物的方法研究

建立了固相萃取、毛细柱气相色谱-电子捕获检测器定量分析水中硝基苯类化合物的分析方法。通过对固相萃取柱的选择、固相萃取条件(样品溶液的pH值、上样速度、上样体积、洗脱液选择及配比)的优化,得出了最佳实验条件。穿透体积可达1.5L,回收率在80%~105%,最小检出浓度在0.00037~0.072μg/L之间,均大大低于GB13194-91的规定。相对标准偏差在0.7%~5.3%之间。该方法准确、简单,重现性好、回收率高,污染小。     

玄武湖沉积物中磷的形态分布特征

利用分级提取法分析了玄武湖的沉积磷形态,在玄武湖沉积物中,铝结合态磷的含量较低,平均值为64 mg/kg,其余形态磷中,铁结合态磷为241 mg/kg,有机磷为335 mg/kg,钙结合态磷为394 mg/kg.在环境变化的条件下,铁结合态磷可以释放到间隙水和上层水体中,是湖泊产生富营养化的重要因素;铝结合态磷由于含量少,对湖泊富营养化影响很小;钙结合态磷相对稳定且很难被生物利用,对湖泊富营养化影响不大;有机磷对水体有机负荷影响较大,并影响水体富营养化程度.     

萃取-催化氧化光度法测定生物体中H2O2含量研究

提出萃取-催化氧化光度法测定生物体中H2O2含量的新方法.用稀土催化H2O2产生羟基自由基以氧化二苯基碳酰二肼,生成红色二苯基碳酰腙,其最大吸收波长为563.0nm;当二苯基碳酰二肼浓度一定时,△A563与H2O2含量呈量效关系.在0～30μmol/L H2O2 含量范围内,该法能简单、快速、精确地测定生物样品中H2O2实际含量.     

Fractionation of Cu, Pb and Zn in certified reference soils SRM 2710 and SRM 2711 using the optimized BCR sequential extraction procedure

Sequential extraction of metals from solid media is a common analytical tool used in environmental and exploration geochemistry. A number of procedures exist, but without harmonization and standardization, meaningful comparisons are tenuous without baseline data. A newly developed, standardized sequential extraction procedure (optimized BCR) was applied to two contaminated certified reference soils from Montana, US (SRM 2710 and SRM 2711) for Cu, Pb and Zn. Four operationally defined fractions were isolated, acid extractable, reducible, oxidizable, and residual (by aqua regia). Fraction-specific concentrations, percentages and recoveries for Cu, Pb and Zn were used to explore differences between the optimized BCR procedure and three other sequential extraction schemes with published data for SRM 2710 and 2711 (i.e. Tessier scheme, Geological Survey of Canada scheme and the original BCR scheme). Results indicate significant differences between the four schemes, even for schemes that are closely associated (i.e. the original and optimized BCR schemes). Order-of-magnitude fraction-specific concentration differences were observed, especially for Pb in the reducible fraction. Differences between schemes are worrisome because trends varied between metals, between fractions and between reference soils. These data reinforce the need for increased adoption of standardized sequential extraction procedures and further examination of different solid media.     

石油亚砜萃取巯基醋酸的研究

对石油亚砜(PSO)萃取巯基醋酸的条件和影响进行了实验研究,确定了石油亚砜通过氢键和巯基醋酸形成的萃合物的组成.为从废水中回收巯基醋酸以及石油硫醚的综合利用提供了依据.     

超声波－蒸汽蒸馏萃取技术富集沉积物样品中的氯代农药和多氯联苯

为方便快速分离沉积物中含氯农药和多氯联苯，将超声波技术和蒸汽蒸馏萃取技术相结合，萃取沉积物中的微量含氯农药和多氯联苯，所得萃取物不需进一步的净化和浓缩，可直接用于色谱分析．实验表明，在进行蒸汽蒸馏萃取之前，使用辅助的超声波技术可将大部分待测物的回收率提高２０％－３０％，较好地解决了由于沉积物的吸附作用而导致的蒸汽蒸馏萃取回收率偏低的缺陷．该法使沉积物样品中的氯代农药和多氯联苯的蒸汽蒸馏萃取富集成为可能．