加压流体萃取-GC/MS法测定土壤中半挥发性有机物

采用加压流体萃取〖CD*2〗气相色谱/质谱联用法（ASE GC/MS）测定土壤中9种半挥发性有机物,分别考察萃取条件、氮吹浓缩、硅酸镁小柱净化和浓缩定容等前处理条件对半挥发性有机物测定的影响。通过优化试验条件,使方法在100 μg/L～1 000 μg/L范围内线性良好,方法检出限为0.01 mg/kg～0.04 mg/kg。土壤样品加标回收率为72.4%～954%,4次测定结果的RSD为2.1%～6.0%。将该方法应用于测定某重点行业企业用地周边土壤,除苯并（a）芘外其余8种半挥发性有机物均为未检出。     

建设用地土壤中11种半挥发性有机物的测定

利用快速溶剂萃取-气相色谱-质谱法对建设用地土壤中11种半挥发性有机物(SVOCS)进行分析,并优化了萃取溶剂、温度和循环次数.经测定,标准曲线的相关系数(R2)>0.990,相对标准偏差(RSD)为1.7％ ～14％,加标回收率为65.0％ ～86.4％,方法检出限为0.01～0.06 mg/kg.结果表明,方法的精...     

SPE-GCMS法分析饮用水源水中痕量半挥发性有机物

采用C 18固相萃取柱富集,乙酸乙酯、二氯甲烷和丙酮混合溶剂以1∶1∶1比例洗脱、自动固相萃取的前处理方法,气相色谱质谱连用,分析水源水中33种半挥发性有机物,并与液液萃取前处理方法进行比较。结果表明:在500~5 000μg/L范围内,33种SVOC线性良好,相关系数0.990,回收率为70.1%~114.2%,相对标准偏差为2.4%~13.4%,方法检出限为0.06~0.25μg/L;而且该方法较液液萃取,检出样品种类多。适用于饮用水源水中半挥发性有机物的监测。     

地表水中半挥发性有机物的固相萃取GC-MS方法研究

利用膜式固相萃取与气相色谱-质谱联用,尽可能多的涵盖了GB 3838—2002饮用地表水80项分析中各种不同性质的半挥发性有机物,建立了地表水中半挥发性有机物的检测方法。优化的固相萃取条件:选用8270专用盘,在中性条件(pH 6～7)下,二氯甲烷淋洗2次,丙酮淋洗1次。方法检出限为0.02～0.17μg/L,各物质回收率均在EPA8270方法中所推荐的回收率范围内。     

回流萃取法提取水中有机物

通过对水中壬基酚及其聚氧乙烯醚等的提取试验，发现回流萃取是提取水中半挥发性有机物的一种很有效的方法。对提取剂进行了选择，表明环己烷效果较好，具有较好的回收率和较好的重现性。为保证高沸点壬基酚聚氧乙烯醚加合物的回收率在95％以上，取90min作为回流萃取时间。最后对回流萃取法的优点作了较详细的阐述。     

环境样品中半挥发性有机物的GC／MS定量

介绍了开展ＧＣ／ＭＳ定量必须满足的诸条件。根据环境样品定量的经验，报导开展半挥发性有机物定量工作的技术路线和注意要点。     

大气中半挥发性有机物的测定与来源分析

研究了大气中半挥发性有机物(SVOC)在滤膜、聚氨基甲酸酯泡膜(PUF)和XAD-2三层上的分布,青岛市大气中SVOC的组分和主要有机物的浓度。大气中的SVOC部分四环和五环以上的多环芳烃主要吸附在滤膜层,而大部分SVOC吸附在PUF层,XAD-2吸附的有机物主要是三甲苯和单体萘。冬季大气中主要的有机物是四环以下PAHs的烷基取代物和多种烷基酚,酚类化合物在冬夏两季的变化最大,夏季中检不出酚类化合物,酚类化合物主要来源于燃煤,而PAHs及烷基取代物来源于燃煤和交通。冬夏两季大气中均能检出与交通有关的己内酰胺。     

GC-MS法测定饮用水源水中半挥发性有机物

用固相萃取的方法对样品进行预处理,再进行GC-MS分析测定,对饮用水源水中的痕量半挥发性有机化合物进行了测定,并对结果进行了讨论。     

水污染事故中半挥发性有机物预处理方法研究

通过配制标准水样,对比液液小体积萃取法、分散液液微萃取法和固相微萃取法结合便携式气质联用仪三种预处理方法的萃取效率。结果表明,在最佳的萃取条件下,三种预处理方法对标准水样的富集效率均较高。在5~50μg/L范围内,14种SVOC线性良好,检出限为0.1~3.5μg/L,其中固相微萃取法萃取效率最高,但对酞酸酯类化合物选择性较差。分散液液微萃取法对有机磷类物质选择性较高,而液液小体积萃取法对大部分的半挥发性有机物没有特别的选择性。在进行实际水样测定时,三种方法在灵敏度、精密性和抗干扰能力等方面均满足水环境污染事故的应急监测要求。     

水污染事故中半挥发性有机物应急监测方法研究

建立了车载式气相色谱/质谱联用仪(GC/MS)结合固相微萃取(SPME)前处理技术测定水体中半挥发性有机物(SVOCs)的方法,优化了萃取头类型、萃取温度与萃取时间、离子强度、解吸温度与解吸时间、搅拌速度等影响萃取效率的因素,以及仪器分析条件.24种SVOCs、7种OPPs和17种OCPs在1.00 μg/L～40.0 μg/L范围内线性良好,检出限为0.11 μg/L～0.39 μg/L,空白加标水样平行测定的RSD≤14.3％,回收率为51.0％～98.5％.     

土壤中挥发性有机污染物现场快速监测技术应用进展

在总结我国突发性环境事故发生现状的基础上,提出了我国环境现场快速监测工作缺少规范化管理,以及标准监测技术方法不完善等问题。探讨了土壤中挥发性有机污染物快速监测技术的研究进展,重点讨论了检测管,手持式气体检测器,便携式气相色谱(配置光离子化检测器、氢火焰离子化检测器或串/并联检测器)及便携式气相色谱-质谱等技术在快速检测土壤中挥发性有机污染物方面的性能特点与应用情况,并对我国建立土壤中挥发性有机污染物现场快速监测标准方法提出了建议。     

地表水中SVOCs和氨基甲酸酯类农药同步萃取技术的探讨

采用大体积固相萃取富集地表水中SVOCs和氨基甲酸酯类农药,再以气相色谱-质谱和超高效液相色谱-串联质谱联用对目标物定性定量。通过优化固相萃取条件,使SVOCs在0.500 mg/L~10.0 mg/L之间,氨基甲酸酯类农药在1.00μg/L~100μg/L之间线性良好,方法检出限为0.002μg/L~0.009μg/L,加标回收率分别为70.5%~105%和78.5%~124%。用该方法测定某流域地表水,结果邻苯二甲酸酯类物质、多环芳烃类、酚类、硝基苯环类化合物等SVOCs,以及克百威、仲丁威等氨基甲酸酯类农药检出。     

Soil-Water Partitioning and Desorption Hysteresis of Volatile Organic Compounds from a Louisiana Superfund Site Soil

The adsorption and desorption of three volatile organic compounds (1,2- dichloroethane, 1,1,2- trichloroethane and 1,1,2,2-tetrachloroethane) from a previously uncontaminated clayey soil sample from a Superfund site in North Baton Rouge,Louisiana was studied. In the linear range of the adsorption isotherm, the partition constants were not affected by the presence of the co-solutes. The adsorption isotherms over a wide concentration range on the soil followed the nonlinearFreundlich isotherm. The desorption of the compounds showedsignificant hysteresis at all concentrations studied. Approximately 20 to 70% of the adsorbed mass of organic compounds resisted the desorption even after five months ofsuccessive desorption steps. The desorption of four compounds(1,2-dichloroethane, 1,1,2-trichloroethane, 1,4-dichlorobenzeneand hexachlorobutadiene) from a contaminated soil sample fromthe same site was also studied. The aqueous concentration declined as the successive desorption steps progressed. For hexachlorobutediene the desorption can be visualized as occurring in two stages. The first stage involved a loosely bound or reversible fraction and the second stage involveda tightly bound or resistant fraction.     

土壤中挥发性有机物的快速测定方法

本文建立了用便携式气相色谱-质谱仪快速测定土壤中VOCs的方法。该方法能够快速对土壤样品中VOCs进行定性分析和定量测定。当采样量达到5 g时,方法检出限0.02~2.11μg/L,相对标准偏差2.0%~13.5%;加标20μg/L时,回收率63%~123%。采用该方法测定北京地区5个土壤样品,总体质量浓度为0~873μg/kg。     

Soil Gas Volatile Organic Compound Concentration Contours for Locating Vadose Zone Nonaqueous Phase Liquid Contamination

Diffusion of VOC from cylindrical vadose zone domains contaminatedwith distributed nonaqueous phase liquid is examined in the steadystate approximation. The effects of first-order biodegradation and ofan extended underlying pool of LNAPL floating on the water table belowthe cylindrical domain are explored by means of an orthogonal functionsapproach. The distribution of VOC in the vadose zone above a floatingcircular LNAPL pool of finite size is explored by a numerical method.The results provide information useful in estimating the spacing anddepth at which soil gas samples should be taken in order to detect thepresence of such source areas. Comparison of model results with soilgas VOC measurements at various depths also provides insight into theextent to which natural biodegradation of the VOCs is taking place.     

Partition Constants and Adsorption/Desorption Hysteresis for Volatile Organic Compounds on Soil from a Louisiana Superfund Site

The adsorption of four volatile organic compounds (1,4-dichloro-benzene, 1,2-dichloroethane, 1,2,2-trichloroethane and 1,1,2,2,-tetrachloroethane) on three soil types from a Superfund site (Petroprocessors Inc) in Baton Rouge, LA was studied with the purpose of obtaining an overall correlation for inclusion in a groundwater transport model being developed for site remediation. The soil-water partition constant, K_d was determined using a standard ASTM procedure (E–1195–87). Using the data for different soil types (fraction organic carbon between 0.11% and 1.13%) and different mineral surface areas (7 to 45 m²/g), the organic carbon contribution (K_oc) and the mineral matter contribution (K_min) to the partition constant were determined. The soils obtained were either from the Pleistocene period or recent shallow deposits at the site. Both log K_oc and log K_min were linearly correlated to log K_ow, the octanol-water partition constant. This data provided the basis for obtaining a general correlation for K_d on different soil types at the site. The predicted values were in agreement with that for a composite soil from the same site. The desorption of compounds from the high clay soil after the 24 hour adsorption period was observed to show a biphasic behavior, namely, an easily desorbed fraction and a desorption resistant fraction. The easily desorbed fraction was found to be satisfactorily predicted using the conventional K_d as obtained from the adsorption experiment. The slowly desorbing fraction had a time constant of several weeks. The concentration in the desorption resistant compartment was found to be dependant on the initial amount of contaminant available for adsorption. The aqueous phase concentration in equilibrium with the desorption resistant fraction was found to be 8 g/L for dichlorobenzene and 12 g/L for dichloroethane.     

固相萃取-UPLC-MS/MS法测定水中全氟化合物

水样中全氟辛酸、全氟辛烷磺酸钾、全氟丁酸、全氟丁烷磺酸经弱阴离子交换固相萃取柱富集净化后,用超高效液相色谱-串联质谱法测定。通过优化样品前处理条件和仪器条件,使4种全氟化合物在0.05μg/L~10.0μg/L范围内线性良好,相关系数为0.998 9~0.999 9,方法检出限为0.27 ng/L~0.96 ng/L。空白水样3个质量浓度水平的加标回收率为73.1%~91.3%,6次测定结果的RSD为7.4%~14.3%。