土壤和河流沉积物中六六六和滴滴涕残留的测定

采用密闭微波提取、超声波提取、索氏提取对土壤和河流沉积物进行前处理,提取液经弗罗里硅土柱净化或浓硫酸净化.通过回收率实验和精密度实验对三种提取方法和两种净化方法进行比较,建立了微波提取土壤和河流沉积物中六六六和滴滴涕,浓硫酸净化,气相色谱一质谱测定的分析方法,方法回收率在84%～110%之间,精密度(RSD)在2.8%～9.9%之间.采用该方法对阜阳市废弃农药厂周围的土壤和河流沉积物中六六六和滴滴涕进行了监测.     

两相分配式生物反应器处理高盐废水中的苯酚

采用新型两相分配式生物反应器(TPPB)和前期研究得到的高效苯酚降解菌对高盐废水中苯酚的降解进行研究,研究中确定煤油为反应系统的最佳有机溶剂,并考察了废水苯酚含量、废水盐度以及搅拌器搅拌速度对苯酚降解的影响。结果表明,反应系统能正常降解苯酚含量为1 000～2 500 mg/L的高盐苯酚废水;反应系统在含盐量为100 g NaCl/L、搅拌速度为50 r/min的运行工况条件下,降解时间缩短为52 h,总酚去除率为20.58 mg/(L.h)。     

Applicability of microwave-assisted extraction combined with LC-MS/MS in the evaluation of booster biocide levels in harbour sediments

A new sample treatment method for the determination of four common booster biocides (Diuron, TCMTB, Irgarol 1051 and Dichlofluanid) in harbour sediment samples has been developed that uses liquid chromatography-tandem mass spectrometry (LC-MS/MS) after microwave-assisted extraction, followed by clean-up and a solid phase extraction preconcentration step (MAE-SPE). The effects of different variables on MAE-SPE were studied. The recoveries obtained were greater than 75%, and the relative standard deviation was less than 7%. The detection limits ranged between 0.1 and 0.3 ng g⁻¹. The developed methodology was successfully applied to the evaluation of the presence of booster biocides in sediment samples from different harbours and marinas of Gran Canaria Island (Canary Islands, Spain).     

Fractionation of plutonium in environmental and bio-shielding concrete samples using dynamic sequential extraction

Fractionation of plutonium isotopes (²³⁸Pu, ^239,240Pu) in environmental samples (i.e. soil and sediment) and bio-shielding concrete from decommissioning of nuclear reactor were carried out by dynamic sequential extraction using an on-line sequential injection (SI) system combined with a specially designed extraction column. Plutonium in the fractions from the sequential extraction was separated by ion exchange chromatography and measured using alpha spectrometry. The analytical results show a higher mobility of plutonium in bio-shielding concrete, which means attention should be paid to the treatment and disposal of nuclear waste from decommissioning.     

采油废水回注处理技术的现状及展望

阐述了目前采油废水回注处理的技术及工艺现状，重点探讨了膜分离技术在采油废水回注处理中的研究及应用情况，分析了各技术存在的问题，并展望了采油废水回注处理技术的发展趋势。     

Microwave extraction of incurred salinomycin from chicken tissues

Abstract

A rapid, accurate, environmentally friendly and cost‐effective microwave extraction technique was developed for the extraction of spiked and incurred salmomycin from chicken tissues (kidney, liver, muscle, ovarian yolk and fat). Extraction of salinomycin from various tissues was achieved by irradiating the sample in absolute ethanol and 2‐propanol (15+2) for 9 sec. in a common household microwave oven. The extract was analysed without further cleanup by HPLC on a C₁₈ column (5 μm) and detected at 592 nm via post‐column reaction with 4‐dimethylaminobenzaldehyde (DMABA) in a heated reactor coil at 86° C. Recoveries of salinomycin from spiked tissues at 30 ng/g level ranged between 87 and 100%. The limit of quantitation was found to be 10 ng/g. The developed method was applied for the analysis of incurred tissues and ovarian yolk of laying chickens given sodium salinomycin in feed at different levels for 14 consecutive days followed by withdrawal periods. Residues were detected in all tissues and ovarian yolk at 0 withdrawal time but declined during the withdrawal period. Highest residue were found in fat and ovarian yolk.     

Kinetic extractions to assess mobilization of Zn, Pb, Cu, and Cd in a metal-contaminated soil: EDTA vs. citrate

Kinetic EDTA and citrate extractions were used to mimic metal mobilization in a soil contaminated by metallurgical fallout. Modeling of metal removal rates vs. time distinguished two metal pools: readily labile (QM1) and less labile (QM2). In citrate extractions, total extractability (QM1+QM2) of Zn and Cd was proportionally higher than for Pb and Cu. Proportions of Pb and Cu extracted with EDTA were three times higher than when using citrate. We observed similar QM1/QM2 ratios for Zn and Cu regardless of the extractant, suggesting comparable binding energies to soil constituents. However, for Pb and Cd, more heterogeneous binding energies were hypothesized to explain different kinetic extraction behaviors. Proportions of citrate-labile metals were found consistent with their short-term, in-situ mobility assessed in the studied soil, i.e., metal amount released in the soil solution or extracted by cultivated plants. Kinetic EDTA extractions were hypothesized to be more predictive for long-term metal migration with depth.     

Determination of 10 particle-associated multiclass polar and semi-polar pesticides from small streams using accelerated solvent extraction

A new analytical method using accelerated solvent extraction was developed for the determination of 10 particle-associated polar and semipolar pesticides. In addition, six deuterated analogues of the target compounds were evaluated as internal standards. The method yielded acceptable accuracy (73–103% recovery) and precision (<25% relative standard deviation) for eight compounds. Using size exclusion chromatography (SEC) as cleanup step resulted in higher recoveries compared to solid phase extraction (SPE) cleanup.

Deuterated standards with 10 or more deuterium atoms performed well as internal standards concerning similar recovery and correlation with the target analytes.

The method was employed to extract particle-associated pesticides from 16 streams located in an area with intense agriculture in France. Acetochlor, pirimicarb, tebuconazole, fenpropidin, -endosulfan and chlorfenvinphos were detected at concentrations up to 1 mg kg⁻¹ dry weight. A comparison with aquatic toxicity data indicated potential risk to the benthic fauna exposed to these concentrations of pirimicarb, -endosulfan and chlorfenvinphos.

We suggest that the method presented here be used for the extraction and quantitation of particle-associated polar pesticides.     

Extraction of labile metals from solid media by dilute hydrochloric acid

Extraction of labile metals from solid media is environmentally more meaningful than a total digestion. A variety of reagents have been introduced in the literature, but dilute HCl has received the greatest attention. We compare metal concentrations liberated by a dilute HCl leach with the sum of the 3-step optimized (standardized) BCR sequential extraction procedure. This is the first study to compare these procedures over a range of grain sizes. Road-deposited sediments from 10 sites in Honolulu were fractionated into six grain size classes. Aliquots of individual fractions were digested with dilute HCl, the 3-step BCR procedure (‘labile’), and a 4-acid (total) procedure. Results indicated that the weighted labile concentrations of Al, Cu, Fe, Mn, Ni, Pb and Zn were statistically greater than those from the dilute HCl leach. However, regression analysis indicated strong statistically significant relationships between the two partial extraction procedures for all metals. On a whole-sample basis, the toxicity classifications for anthropogenic-enhanced metals (Cu, Pb and Zn) were similar between extractions. Taken together, results suggest that the application of dilute HCl to solid media provides a rapid, cost-effective, and environmentally meaningful approach for contaminant monitoring.     

泄漏检测与维修技术在芳烃抽提装置的应用研究

采用泄漏检测与维修（ LDAR）技术进行了全面检测和统计分析，分析泄漏的原因并通过维修减少泄漏。结果表明：芳烃抽提装置容易泄漏的元件主要为连接件和阀门，主要分布在泵区；SV≥5000μmol／mol的泄漏密封点占总密封点数的0.57％，对总泄漏量的贡献达到了82％，是造成泄漏排放的主要部分。设备管阀件泄漏造成的加工损失率为0.0009％，泄漏点停工维修修复率为83％，停工维修后整体泄漏率为0.03％；VOCs减排率为71％。