气相色谱法测定土壤中挥发性硫化物

采用带硫化学发光检测器的气相色谱(GC-SCD),同时分离并测定土壤中硫化氢、羰基硫、甲硫醇、甲硫醚、二硫化碳和二甲基二硫等6种挥发性硫化物。通过优化仪器工作条件,使该方法在0.521μg/L~65.7μg/L范围内线性良好,方法检出限为0.58μg/L~1.76μg/L,标准气体5次测定结果的RSD为0.9%~8.3%。用该方法分析土壤在强还原条件下挥发性硫化物的排放量,结果表明,上述6种挥发性硫化物均有产生,且随培养时间的延长排放速率增加,硫化氢是其主要气体产物,占挥发性硫化物排放总量的79.1%。     

固相萃取-GC/MS法测定地表水中3-甲基吲哚

采用微球硅胶键合C_(18)固相萃取柱萃取水样中的3-甲基吲哚,并用气质联用法测定,方法在0 mg/L~10.0 mg/L范围内线性良好,方法检出限为0.2μg/L。空白水样3个质量浓度水平的加标回收率为89%~94%,7次测定结果的RSD为2.3%~6.9%。用该方法测定7个实际地表水样品,其中4个地表水样品检出3-甲基吲哚,地表水样的加标回收率为81.5%~97.0%。     

顶空气相色谱法测定漓江底泥中的三氯乙烯和四氯乙烯

采用Na Cl溶液提取,顶空气相色谱法测定底泥中的三氯乙烯和四氯乙烯,方法在0.098 ng/L~1.03 ng/L范围内线性良好,三氯乙烯和四氯乙烯的方法检出限分别为0.013 ng/g和0.016 ng/g。对空白样品做3个质量比水平的加标回收试验,7次测定结果的RSD为2.0%~3.8%,平均加标回收率为94.0%~109%。将该方法用于桂林市漓江底泥样品的测定,结果三氯乙烯和四氯乙烯均为未检出,实际样品加标回收率为92.0%~107%。     

溶剂效应对有机氯农药测定的影响研究

采用气相色谱-质谱法(GC-MS)研究了不同溶剂对有机氯农药测定的影响。结果表明,有机氯农药在不同溶剂中的GC-MS响应值是有差异的,但保留时间不变,且随着有机氯农药质量浓度的增加,这种溶剂效应对大部分有机氯农药的作用减弱。经分析溶剂的极性对有机氯农药测定有显著的影响。     

Mathematical Modeling of Column and Field Dense Nonaqueous Phase Liquid Tracer Tests

Mathematical models for the simulation of dense nonaqueous phase liquid tracer tests (DTTs) in laboratory columns and in the field are developed and examined. The DTT technique is a means of estimating the quantity of dense nonaqueous phase liquid (DNAPL) in a domain of interest in an aquifer. The two-dimensional field DTT model uses the Method of Principal Directions and an asymmetrical upwind algorithm for describing advective transport. Both models include diffusion transport of tracer into and from low-permeability porous structures such as clay lenses, as well as the mass transport kinetics of partitioning tracer to and from the DNAPL droplets. The dependence of the effluent tracer concentration curves on the parameters of the models is explored, and conclusions are drawn regarding the applicability of, and several possible problems with, the DTT technique. Model results indicate that the DTT performs well at locating distributed droplets of DNAPL, but is unlikely to be useful in the assessment of pooled DNAPL.     

单柱阳离子色谱快速分析白云石中高含量钙镁

采用离子色谱法同时测定白云石中高含量钙镁,该法与目前使用的络合滴定法相比,具有准确可靠、操作简便快速、无干扰等特点。对样品测定取得了满意的结果,氧化钙与镁瓣含量分别为３１．９９％和２１．４７％,相对标准偏差分别为０．８１％和０．６５％,平均回收率分别９９．９％和１０２％。     

宁波市饮用水源地爆发蓝藻水华时微囊藻毒素的污染分析

通过固相萃取净化,建立了超高效液相色谱-串联四极杆质谱法测定水中微囊藻毒素MC-LR和MC-RR的方法,并用该方法监测了宁波市两个饮用水源地爆发蓝藻水华时水体中的微囊藻毒素.监测结果表明,姚江水体中的微囊藻毒素污染水平低,MC-LR和MC-RR没有被检出;梅湖水库水体中MC-RR也未被检出,采取措施后,虽MC-LR有时被检出,但最高时也低于国家标准值(1.0μg/L).     

超声波提取-GC/MS法测定生物体内硝基苯类化合物

以洪泽湖中6种代表性生物为研究对象,采用超声波法提取样品中硝基苯类化合物,用凝胶色谱净化、浓缩,气相色谱／质谱联用法测定。该法与索氏提取法在同等试验条件下进行加标回收试验,前者回收率高且稳定,简便可行。方法检出限为0．008μg／g～0．030μg／g,平均加标回收率为76．5％～109％,重复测定3次的RSD为1．5％～13．0％。     

碳包覆Pd/Al2O3催化剂催化4-溴苯酚加氢脱溴的活性和稳定性调控研究

在污染物液相催化加氢脱卤过程中,提高催化剂的稳定性至关重要.以水热合成法制备了不同碳包覆量的Pd/Al₂O₃@C催化剂,对催化剂进行了系列表征,并将催化剂应用于4-溴苯酚(4-BP)污染物的催化加氢脱溴反应.表征结果显示碳层提高了Pd/Al₂O₃的表面疏水性,有利于4-BP在催化剂上的吸附.并且在Pd/Al₂O₃@C催化剂的碳化过程中,碳还原部分Pd颗粒,并保留部分正价态Pd活性位,增强了4-BP中C-Br键的活化.与Pd/Al₂O₃相比,碳涂层提高了催化剂的催化活性.但当碳包覆量超过最佳包覆量后,暴露的Pd粒子随碳包覆量的增加而减少,导致活性下降.此外,碳层修饰后,催化剂的稳定性显著提高,从而大大抑制了Pd粒子的团聚和损耗.Pd/Al₂O₃@C表面的碳涂层对卤素具有较高的耐受性,从而减轻了液相催化加氢脱卤反应中活性中心的中毒.     

Comparison of Three Extraction Methods for 17 β-Estradiol in Sand,Bentonite, and Organic-Rich Silt Loam

Extraction is an important procedure for samples that contain soil because other compounds in soil may affect analysis of estrogens. This study was conducted to evaluate three different extraction methods for 17β-estradiol in soil. Sand, bentonite, and organic-rich silt loam were spiked with 1 mg kg^{? 1} of 17β-estradiol as a model compound of estrogens. 17β-estradiol and its metabolites, estrone and estriol, were extracted using (i) a modified Bligh and Dyer extraction, (ii) a pressurized fluid extraction, and (iii) a diethyl ether extraction, and measured by liquid chromatography tandem mass spectrometry. There were significant differences in the extraction efficiency for 17β-estradiol among the extraction methods and the soils: the efficiencies ranged from 10% to 97%. Overall, the diethyl ether extraction method had the largest efficiency of 17β-estradiol with 45% and 57% for bentonite and silt loam, respectively. Transformation of 17β-estradiol to estrone and estriol in the different extraction methods was less than 3.6% during the extraction procedures. This study underlined the importance of sample preparation for estrogen analysis in soil samples.