Static headspace analysis of volatile organic compounds in soil and vegetation samples for site characterization

Traditional methodologies for the characterization of volatile organic compounds (VOCs) in subsurface soil are expensive, time-consuming processes that are often conducted on samples collected at random. The determination of VOCs in near-surface soils and vegetation is the foundation for a more efficient sampling strategy to characterize subsurface soil and improve understanding of environmental problems.In the absence of a standard methodology for the determination of VOCs in vegetation and in view of the high detection limits of the method for soils, we developed a methodology using headspace gas chromatography with an electron capture detector for the determination of low levels (parts-per-billion to parts-per-trillion) of VOCs in soils and vegetation. The technique demonstrates good sensitivity, good recoveries of internal standards and surrogate compounds, good performance, and minimal waste. A case study involving application of this technique as a first-step vadose-zone characterization methodology is presented.     

Solid phase extractive preconcentration of uranium(VI) using quinoline-8-ol anchored chloromethylated polymeric resin beads

A new chelating polymeric sorbent has been developed using Merrifield chloromethylated resin anchored with quinoline-8-ol (HQ). The modified polymeric resin was characterized by FT-IR spectroscopy and elemental analysis. The HQ anchored resin showed superior binding affinity for U(VI) over Th(IV) and La(III). The influence of various physicochemical parameters on the recovery of U(VI) were optimized by both static and dynamic methods. The phase exchange kinetic studies performed for U(VI) revealed that <5 min was sufficient for reaching equilibrium metal ion sorption. The maximum sorption capacity of HQ anchored resin for U(VI) was found to be 120.30 mg g⁻¹ of resin which is higher than other solid phase extraction sorbents reported so far excepting N,N-dibutyl, N′-benzoyl thiourea sorbed Amberlite XAD-16. The developed HQ anchored polymeric resin is highly selective as none of the extraneous species were found to have any deleterious effect. Solid phase extraction (SPE) studies performed using HQ anchored polymeric resin offered enrichment factor of 100 and the lowest concentration below which recoveries become non-quantitative is 5 μg l⁻¹. The accuracy of the developed SPE method in conjunction with Arsenazo III procedure was tested by analyzing marine sediment (MESS-3) and soil (IAEA–Soil 7) reference materials. Furthermore, the above procedure has been successfully employed for the analysis of real soil and sediment samples.     

Supercritical Fluid Extraction of Organochlorine Pesticides from Soil

Abstract

A supercritical fluid extraction (SFE) method was developed for the extraction of 21 organochlorine (OC) pesticides from soil using dichloromethane as cosolvent and magnesium sulfate as drying agent. Average recoveries of spiked OCs from six different soils generally ranged from 70 to 95%, with an average replicate precision of ± 13%. For the extraction of two soils containing “native” OCs, the SFE method gave generally similar or higher concentrations compared to Soxhlet extraction. The precision of replicate analyses of native OCs using SFE and Soxhlet extraction was ± 0.009 and ± 0.007 ug/g, with 24 and 13 degrees of freedom respectively.     

中国不同类型土壤中稀土元素的形态分布特征

采用中子活化分析地中国不同地带土壤中的稀土元素含量分布模型及其赋存形态进行了系统的研究。结果表明，黄棕壤，褐土，淋溶黑钙土及白浆土中稀土元素的分布均为轻稀土富集，Ｅｕ亏损型，砖红壤，红壤为轻稀土富集，Ｃｅ亏损型。     

新乐工业新区土壤中多种元素的测定

采用湿法消解对不同厂区的土壤进行前处理,应用电感耦合等离子体原子发射光谱法(ICP-OES)测定土壤中的金属元素含量,使用原子荧光光谱法AFS测定砷的含量,测定的相对标准偏差为0.8%～3.0%,回收率为89.0%～105.5%。实验表明,方法简单快速、准确,较高的灵敏度和较低的检出限,均能满足土壤中多元素分析的要求。     

微波消解-FAAS测定皖南茶园土壤中矿质元素含量

采用微波消解-FAAS测定了皖南休宁县茶园不同深度土壤中的矿质元素Cu、Cd、Mn、Zn、Fe、Pb的含量,分析了不同深度土壤中矿质元素的分布特征,结果表明,皖南土壤中矿质元素Cu、Cd、Mn、Zn、Pb 5元素含量随土壤深度呈递减趋势,土壤表层的矿质元素(Cu、Cd、Mn、Zn、Pb)含量高于深层的,这与施肥有关,土...     

超高效液相色谱-质谱法检测土壤中的羟基化多溴联苯醚

建立了土壤中8种羟基化多溴联苯醚(Hydroxylated polybrominated diphenyl ethers,OH-PBDEs)的Qu ECh ERS-超高效液相色谱串联质谱(UPLC-MS/MS)分析方法。样品前处理采用Qu ECh ERS方法,土壤样品用水浸润之后,以甲酸和乙腈提取目标物,C18填料和正丙基乙二胺(PSA)净化,C18色谱柱分离,乙腈和水梯度洗脱,多反应监测负离子模式扫描。在最佳实验条件下,8种目标物在9 min内分离良好,并在2~200μg/L范围内线性良好,相关系数范围在0.9936~0.9990,检出限范围为0.23~1.21 ng/g。在5.0和50 ng/g 2个浓度水平6次平行加标实验中,8种OH-PBDEs平均回收率为73.2%~117.7%,相对标准偏差为5.6%~19.7%。本方法操作简便,灵敏度高,适用于大批量样品的快速分析。