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％。     

铬渣中铬的浸出行为

采用BCR法连续浸提研究铬渣中铬的存在形态,结果表明:铬渣中总铬和六价铬主要以残渣态和可氧化态形式存在;通过铬渣动态连续浸提实验与静态浸提实验研究了浸提剂和活性炭对铬渣中铬浸出行为的影响,研究发现p H值为3.1的醋酸浸提剂浸出液中铬浓度最低,且添加活性炭后的静态浸出液中铬的浓度有不同程度降低。     

超高“Z型”中庭高度对自燃排烟特性影响的数值模拟研究

超过12m的超高中庭发生火灾时,常规排烟方法不能完全满足实际需求。通过FDS软件对某超高"Z型"中庭进行数值模拟,研究中庭高度对自然排烟特性的影响。该"Z型"中庭底层南面是自然进风口,顶层北面是自然排烟口,以烟气最先到达指定楼层人员危险时间值为到达危险时间。实验条件下模拟结果表明:无风情况下,中庭高度增加,到达危险时间增加,自然排烟效果增强。到达危险时间t与中庭高度h之间满足一定指数增长关系:t=y0+Aexp(h/α),中庭火源位置和中庭宽度对y0、A和α有一定影响。有风情况下,外界风向与进风口方向一致时,中庭自然排烟效果优于无风状况,中庭越高效果越强。在外界风向与排烟口方向相反时,烟气倒灌进中庭,自然排烟效果较弱。