Investigation of the solubilization of car-emitted Pt,Pd and Rh in street dust and spiked soil samples

A sequential extraction procedure (three-step), proposed by the Standards, Measurements and Testing Programme (formerly BCR) of the European Union, was applied to street dust and spiked soil samples for the determination of PGEs. Analyses were carried out using inductively coupled plasma-mass spectrometry (ICP-MS). The results indicate that up to 5% from Pt, 70% from Pd and 14% from Rh are in mobile forms in street dust. The results for the soil samples spiked with crushed catalytic converter are significantly lower indicating that PGEs are oxidised more efficiently in natural conditions. Additionally Pt and Pd bound to humic acids were investigated.     

Evaluating the mobility of toxic metals in untreated industrial wastewater sludge using a BCR sequential extraction procedure and a leaching test

The distribution and speciation of toxic metals in industrial wastewater sludge (IWS) was investigated. In this work, the modified BCR three-stage sequential extraction procedure was applied to the fractionation of Cr Pb Ni, and Cd in untreated industrial wastewater sludge from industrial sites in Hyderabad (Pakistan). The extracts were analyzed using electrothermal atomic absorption spectrometry. The procedure was evaluated using a certified reference material for soil mixed with sewage sludge BCR 483. The results from the partitioning study indicate that more easily mobilized forms (acid exchangeable) of Cd were dominant. The oxidizable fraction was dominant for all four toxic metals. Metal recovery was good, with <4% difference between the total metal recovered through the extractant steps and the total metal determined after microwave digestion. Lixiviation tests (DIN 38414-S4) were used to evaluate the leaching of toxic species from IWS, and it was observed that levels of leachable toxic metals were low compared to the amount of metal extracted in the exchangeable fraction of the BCR protocol.     

Electrochemical biosensor based on nanogold-modified poly-eriochrome black T film for BCR/ABL fusion gene assay by using hairpin LNA probe

A novel electrochemical biosensor is described for detection of breakpoint cluster region gene and a cellular abl (BCR/ABL) fusion gene in chronic myelogenous leukemia (CML) by using thiolated-hairpin locked nucleic acids (LNA) as the capture probe. The hairpin LNA probe was immobilized on the nanogold (NG)/poly-eriochrome black T (EBT) film-modified glassy carbon electrode (GCE). The immobilized LNA probe could selectively hybridize with its target DNA on LNA/NG/EBT/GCE surface. The immobilization and hybridization of the LNA probe were characterized with cyclic voltammetry and electrochemical impedance spectroscopy. The hybridization of the immobilized LNA probe with the target DNA was detected by differential pulse voltammetry with the electroactive methylene blue as an indicator. The results indicated this new method has excellent specificity for single-base mismatch and complementary after hybridization, and a high sensitivity. This novel electrochemical biosensor has been used for assay of PCR real sample with satisfactory result.     

黄河甘宁蒙段表层沉积物中重金属元素含量及其形态分析

到目前为止,关于水环境中重金属浓度和形态分布的研究有许多报道。但是关于黄河上游,特别是对黄河甘宁蒙段区域重金属的研究报道仍需进一步深入。在相关研究工作的基础上,使用HR-ICP-MS和BCR连续提取法主要对2011年丰水期黄河甘宁蒙段12个采样点表层沉积物Cd,Pb,Cr,V,Co,Ni,Cu和Zn重金属元素的含量,形态和潜在风险进行测定与分析。结果表明：所有采样点各重金属元素含量顺序相同：Cr>V>Zn>Cu>Ni>Pb>Co>Cd,与各采样点所在区域土壤中背景值相比,S5采样点Cd元素的含量水平最高(1.30 μg·g-1) 约为背景值(0.103 μg·g-1)的13倍。通过I_geo对重金属进行污染评价,结果显示S5采样点Cd元素为强污染水平(I_geo=3.08),内蒙古段四个采样点(S1—S4)Cd表现为中强度污染水平,I_geo位于2.02~2.90之间;此外,富集因子(EF)评价结果发现,研究区域表层沉积物中八种重金属均受到人为活动的污染。根据潜在生态风险指数(RI)结果,S5和S3采样点为高生态风险,其他采样点为中等生态风险。BCR连续提取法结果显示Cd的有效性最高,其次为Co和Ni,V和Cr有效性最低。根据形态分析风险评估准则 (RAC),Cd在S1—S4采样点有高风险,在S5采样点有很高风险;而对于Ni和Co来说,12个采样点中均表现为中等风险。研究结果和结论可为相关政府部门提供重要的研究信息。     

基于BCR和HG-ICP-AES的矿区土壤重金属污染特征分析

建立了基于BCR法(连续提取法)和HG-ICP-AES技术的土壤重金属形态含量的检测方法。在选定的实验条件下,HG-ICP-AES对Hg, Pb和As的检测限分别达到0.6,1.5和0.8 ng·mL-1。对国家标准沉积物样品中Hg,Pb和As的含量进行对照测定,检测结果与推荐值一致,标准物质中Hg, Pb和As多次重复测定的RSD均<8%。应用本法实测了湘西某有色金属矿区土壤中Hg, Pb和As各形态的含量,发现矿区土壤中Hg, Pb和As均以残渣态为主,有机态和Fe-Mn氧化态次之,酸交换态含量较少;与对照区相比,矿区土壤中酸交换态、Fe-Mn氧化态、有机态、残渣态Hg, Pb和As的含量分别增加1.2, 3.0, 47, 272倍(Hg); 1.2, 4.6, 8.1, 4.5倍(Pb); 1.5, 2.9, 3.3, 2.2倍(As); 表明湘西矿区土壤同时存在Hg, Pb和As的复合污染。     

Comparison of original and modified BCR sequential extraction procedures for the fractionation of copper, iron, lead, manganese and zinc in soils and sediments

This article describes a detailed comparison between the original BCR sequential extraction procedure, step 2 of which involves treatment with 0.1 mol l⁻¹ hydroxylammonium chloride at pH 2, and the revised BCR procedure (step 2: 0.5 mol l⁻¹ hydroxylammonium chloride at pH 1.5). An intermediate protocol was also evaluated in which 0.5 mol l⁻¹ hydroxylammonium chloride at pH 2 was used. The procedures were applied to five soil and sediment substrates: a sewage sludge-amended soil, two different industrially contaminated soils, a river sediment and an inter-tidal sediment. Extractable iron and manganese concentrations were measured to assess the effects of the procedural modifications on dissolution of the reducible matrix components. Trace elements copper, lead and zinc were also determined. Statistical analysis (two-tailed t-tests at 95% confidence interval) indicated that recovery of iron in step 2 was not markedly enhanced when the intermediate protocol was used. However, significantly greater amounts were isolated with the revised BCR scheme than with the original procedure. Copper behaved similarly to iron. Lead recoveries were increased by use of both modified protocols, with the greatest effect occurring for the revised BCR extraction. In contrast, manganese and zinc extraction did not vary markedly between procedures. The work indicates that the revised BCR sequential extraction provides better attack on the iron-based components of the reducible matrix for a wide range of soils and sediments.     

Determination of molybdenum in extracts of soil and sewage sludge CRMs after fractionation by means of BCR modified sequential extraction procedure

A modified three-step sequential extraction procedure proposed by the Commission of European Communities Bureau of Reference (BCR) was applied to certified reference materials of three different soil groups (rendzina, luvisol, and cambisol) and sewage sludge of different compositions originating from a municipal water treatment plant in order to assess potential mobility and the distribution of molybdenum in the resulting fractions. In the soils examined, molybdenum was present almost entirely in the mineral lattice, the content of molybdenum in the fractions of the studied reference materials of sludges was predominant in the fraction, represents Mo bound to organic matter and sulphide.The internal check of accuracy was performed on the results of the sequential extraction by comparing of the extractable amounts of molybdenum in the sequential procedure with the results of the pseudototal digestion of original samples. The recovery ranged from 96 to 101% and the precision (RSD) in the extracts was below 10%.     

Certification of trimethyl‐lead in an urban dust reference material (CRM 605)

In order to control the quality of trimethyl‐lead determination in urban dust, the Standards, Measurements and Testing Programme (formerly BCR) of the European Commission organized interlaboratory studies of which the final aim was to certify a Reference Material. This paper describes the preparation of an urban dust reference material (CRM 605), the homogeneity and stability studies, and the analytical work performed for the certification of the trimethyl‐lead content (7.9 ± 1.2 μg kg⁻¹ by mass). Copyright © 1999 John Wiley & Sons, Ltd.     

Modelling of chemical fractionation patterns of metals in soils by two-way and three-way principal component analysis

The ‘pseudo-total’ contents and the chemical fractionation pattern of eight toxic elements (As, Cd, Co, Cu, Cr, Ni, Pb and Zn) have been determined in 12 soil samples collected around a coal-fuelled power plant (Velilla del Río Carrión, Spain) by using, respectively, the US-EPA 3051 norm and the modified BCR (SM&T) chemical fractionation procedure. The ‘pseudo-total’ dataset has been analyzed by classical two-way principal component analysis (PCA) finding a PC accounting for the metal ‘pollution’ of the area. On the other hand, the three-dimensional (samples × metals × fractions) X array obtained after application of the modified BCR SM&T procedure, has been studied by matrix augmentation (MA-PCA) and three-way principal component analysis (3-PCA) using PARAFAC and TUCKER3 models. Whereas both MA-PCA and PARAFAC originated two-factor models biased towards the different chemical fractionation of the samples, the best TUCKER3 model [1, 2, 2] takes into account simultaneously both the ‘pseudo-total’ contents and the chemical fractionation of the soil samples. Therefore, the TUCKER3 originated a better representation of the global environmental impact caused by the power plant, and the plotting of the soil samples loadings, A1, in the physical space allowed to locate the most potentially hazardous areas.