Remobilization of selected metal ions from Nile sediment (Egypt) according to sequential extraction and metal–EDTA complex

River sediments are basic components of our environment, providing nutrients for living organisms and serving as sinks for deleterious chemical species. The metal contents may be remobilized and released back into waters with changes in environmental conditions, thus affecting living organisms and human activities. This paper aims to determine the effect of a synthetic anthropogenic chelating agent (EDTA) as industrial discharges on the remobilization of several metals (Cu, Zn, Cd, and Pb) in River Nile sediments (at Aswan and Mansoura cities) under different concentrations and pH values, and to investigate the influence of metal–EDTA complexes on this remobilization. For these purposes, sequential extraction and experiments on the effect of pH and metal EDTA complex were carried out on the two representative sediment samples south and north of the River Nile in Egypt. The results of sequential extraction show that most of metal contents present in the residual form (Cu, 11.36–72.34%; Pb, 29.64–66.67%; and Zn, 43.76–50.09% at Aswan and Mansoura, respectively). Non-residual fractions which may be available for the remobilization by EDTA represented anthropogenic (industrial, agriculture, and domestic discharges) and lithiopogenic (metals bound to Fe and Mn oxides) sources. A clear increase was detected for Cu and Zn remobilization from the increase in EDTA concentrations, in contrast, Cd independent of the EDTA concentration and slight influence on Pb content. The remobilization of metals as a function of pH exhibited. The metals were greatly remobilized under the complexing action of EDTA, showing that some of these elements were adsorbed on the sediments. The remobilization rate of metals was dependent upon the added metal–EDTA complex (with the exchange rate being in the order Ca–EDTA>Zn–EDTA>Cd–EDTA>Cu–EDTA>Pb–EDTA), due to the stability constant of the metal–EDTA complex. The results of these experiments showed that heavy metals are greatly remobilized under the complexing action of EDTA when it is present in excess, so all precautions should be taken to prevent any wastewater containing EDTA or any chelating agents discharging directly or indirectly via the River Nile stream because most EDTA remains in the aquatic phase. The ability of this portion to remobilize metals from sediments should be taken into account.     

Spatial distribution of perfluorooctane sulfonate (PFOS) in major rivers in southwest Nigeria

Concentrations of perfluorooctane sulfonate (PFOS) were measured for the first time in major rivers within southwest, Nigeria. PFOS was concentrated from water and sediment using solid-phase extraction, identified and quantified with high-performance liquid chromatography coupled with tandem mass spectrometry. Concentrations of PFOS ranged from 1.71 to 16.19 ng L^?1 in water, and from 1.64 to 10.29 ng g^?1 in sediments across all locations. Comparatively, the concentrations of PFOS observed in this study were within the range ever measured in the environment. Field-based sediment water distribution coefficients (log K_d, L kg^?1) ranged from 2.08 to 3.56. While no correlation was observed between K_d and organic carbon contents, there was significant positive correlation between K_d and salinity (r² = 0.7867), which suggested that activities capable of increasing salinity can enhance PFOS removal from the environment.     

Determination of pentachlorophenol in human urine using solid phase extraction and GC‐MS analysis with stable isotope dilution

A method for the determination of pentachlorophenol (PCP) in human urine was developed. Urine samples were fortified with ¹³C₆‐IabeIed PCP and hydrolyzed with sulfuric acid prior to extraction. The urine samples were then passed through preconditioned solid phase extraction cartridges containing octadecylsilane adsorbent. The PCP was subsequently eluted from the cartridge with ethyl acetate and converted to pentachloroanisole prior to GC‐MS analysis. GC‐MS quantitation was performed using the technique of stable isotope dilution. Percent recoveries averaging 100, 97, and 111% were obtained for replicate urine samples fortified with approximately 2, 20, and 200 ng/mL of PCP, respectively. The method detection limit was estimated to be 0.2 ng/mL.     

Online solid phase preconcentration using EGDMA–MAA copolymer for lead determination by FAAS

A Ethylene glycol dimethacrylate (EGDMA) methacrylic acid (MAA) resin was used for preconcentration of lead at trace levels in water samples. For this purpose, a flow-injection, solid phase extraction method was developed for the determination of lead by flame atomic absorption spectrometry. Lead ions were sorbed on a EGDMA–MAA column at pH 4, followed by an elution step using 288 µL of 4.0 M nitric acid solution and determination by flame atomic absorption spectrometry. Optimum conditions for quantitative sorption involving the pH, sample volume, loading and elution flow rates, eluent type, and volume were investigated. A 868-fold enrichment factor could be reached. The detection limit for the water samples, estimated from the noise on the signal obtained for 250 mL of 10 µg L^?1 loaded at 4.9 mL min^?1 was 1.04 µg L^?1. The method was applied for lead determination in river water samples collected in Edirne, Turkey. Recoveries of spiked solutions (10 µg L^?1) to river water samples were quantitative. Finally, the method was validated by the analysis of certified reference material SRM 2704 (Buffalo River Sediment).     

A new procedure combining GC-MS with accelerated solvent extraction for the analysis of phthalic acid esters in contaminated soils

An optimized procedure based on gas chromatography-mass spectrometry (GC-MS) combined with accelerated solvent extraction (ASE) is developed for the analysis of six phthalic acid esters (PAEs), which are priority soil pollutants nominated by United States Environmental Protection Agency (USEPA). Quantification of PAEs in soil employs ultrasonic extraction (UE) (USEPA 3550) and ASE (USEPA 3545), followed by clean up procedures involving three different chromatography columns and two combined elution methods. GC-MS conditions under selected ion monitoring (SIM) mode are described and quality assurance and quality control (QA/QC) criteria with high accuracy and sensitivity for target analytes were achieved. Method reliability is assured with the use of an isotopically labeled PAE, di-n-butyl phthalate-d4 (DnBP-D4), as a surrogate, and benzyl benzoate (BB) as an internal standard, and with the analysis of certified reference materials (CRM). QA/QC for the developed procedure was tested in four PAE-spiked soils and one PAE-contaminated soil. The four spiked soils were originated from typical Chinese agricultural fields and the contaminated soil was obtained from an electronic waste dismantling area. Instrument detection limits (IDLs) for the six PAEs ranged 0.10–0.31 μg·L^-1 and method detection limits (MDLs) of the four spiked soils varied from a range of 20–70 μg·kg^-1 to a range of 90– 290 μg·kg^-1. Linearity of response between 20 μg·L^-1 and 2 mg·L^-1 was also established and the correlation coefficients (R) were all>0.998. Spiked soil matrix showed relative recovery rates between 75 and 120% for the six target compounds and about 93% for the surrogate substance. The developed procedure is anticipated to be highly applicable for field surveys of soil PAE pollution in China.     

土壤宏蛋白质组学蛋白质提取方法及其应用

土壤宏蛋白质组学在揭示土壤微生物功能、代谢与环境相互作用方面具有广阔的应用前景,但由于土壤样品的特殊性,土壤蛋白质提取步骤是限制土壤宏蛋白质组学大规模应用的瓶颈之一.本文从样品制备、提取方法、影响因素等方面综述了土壤蛋白提取方面的研究进展.一般来说,根据实验目的、蛋白种类及后续研究方法设计相应的分组成收集策略才能取得较好的提取效果.土壤总蛋白、胞内蛋白与胞外蛋白分别有不同的提取方法.总蛋白提取一般采用直接提取法;胞外蛋白不需要裂解;胞内蛋白提取方法有直接提取法和间接提取法等.裂解、浓缩、去除腐殖质的方法以及提取液、pH值的选择等也会影响提取效果.此外,简单介绍了土壤宏蛋白质组学的应用,并对今后的研究工作提出展望.表1参36     

水中痕量阿特拉津的测定方法研究

采用固相萃取与高效液相色谱结合的方法测定了水样中痕量阿特拉津的含量,研究了最佳固相萃取条件:选择洗脱液为乙腈,过样流速为5.0 mL/min。最佳的色谱条件:流动相为乙腈和水,温度为25℃,流速为1.0 mL/min,检测波长为222 nm。阿特拉津质量浓度在0.05～5 mg/L范围内线性关系良好,回归方程y=219.71x+2.2343,回收率平均值为98.46%,将该方法应用于实际环境水样的分析测定,操作简单,结果准确。     

固体吸附剂控制燃煤重金属排放的实验研究

在滴管炉上进行了烟煤添加固体吸附剂的燃烧实验研究了硫酸钙、石灰石、铝土矿3种吸附剂对重金属元素Pb、Cd、Cu、Co、Ni排放的控制,并采用形态逐级提取法,将排放颗粒物中重金属分为吸附态、离子可交换态、碳酸盐结合态、硫酸盐结合态和残渣态从粗粒灰渣及细微粒子中重金属元素含量的分布和细微粒子中残渣态稳定形态含量增加2个方面说明添加吸附剂对煤中重金属的排放具有一定的捕获力.对不同的重金属,由于吸附剂本身物理化学特性的差异,所表现出的吸附能力也各不相同.硫酸钙对Pb、Cd、Cu的排放有控制作用;石灰石对Pb、Cd、Cu、Nj的排放有控制作用;铝土矿对5种重金属元素的排放都有控制作用吸附剂粒径越小,对重金属的吸附效果越好.     

基于非线性渗流模型采空区漏风流场数值模拟

针对采空区非线性渗流模型中颗粒平均粒径的取值问题,利用专业的流体力学软件fluent对刘庄矿151305工作面采空区不同颗粒粒径下的漏风流场进行了模拟,以此确定合适的平均粒径,并利用该采空区颗粒平均粒径对工作面供风量及采空区漏风的影响进行了模拟与分析。结果表明,采空区内平均粒径的取值对工作面风量分布影响较大,瓦斯抽采负压也相差一个数量级;通过与实测工作面风量及实际的瓦斯抽采负压作对比,当采空区颗粒平均粒径取0.1 m时,模拟结果与现场实际最为吻合;工作面供风量越大,采空区的漏风量也越大,两者为二次函数关系。该研究方法为工作面采空区漏风流场数值模拟提供了理论指导。     

北京地区地表水中OCPs和PCBs的污染分析

在夏、冬两季对北京地区密云,潮白河,玉渊潭和通惠河等地表水中17种有机氯农药（OCPs）和84种多氯联苯（PCBs）的含量进行了分析及来源解析.实验结果表明,OCPs总量在7.86～53.1ng/L之间,平均值为（16.9±14.6）ng/L.PCBs总量在2.99～32.7ng/L之间,平均浓度为（10.9±10.4）ng/L.HCHs,硫丹,DDTs和HCB是主要的OCPs污染物,其含量分别为（13.9±11.5）ng/L,（2.20±2.01）ng/L,（0.63±1.51）ng/L和（0.12±0.14）ng/L.α-HCH/γ-HCH平均比值为1.53,小于工业HCH中比值4～7,表明北京地区地表水中存在林丹的使用.而DDT/（DDD+DDE）比值<1.22,表明北京地区并无新的DDTs污染源输入环境.PCBs以低氯代联苯为主,其中二氯,三氯,四氯和五氯联苯总和占∑₈₄PCBs总量的79.2%.北京地区地表水中不同氯取代数PCBs组成与我国历史PCB产品组成相符,均以低氯代联苯为主,表明北京地区地表水中PCBs污染来源为历史使用.相比于国内其他区域水质而言,北京地区地表水OCPs和PCBs污染水平较低.