等温平台石墨炉原子吸收光谱法测定高纯铟中痕量杂质铅和砷

利用石墨炉原子吸收法，在等温平台条件下利用标准加入法直接测定了高纯铟中的痕量杂质铅和砷．并对石墨炉加热程序中的干燥时问、灰化温度及原子化温度进行了优化，同时也考察了介质酸度的影响．本方法中铅和砷的特征质量分别为37．8pg和40．7pg，相对标准偏差平均值分别为2．8％和2．0％，加标回收率分别为85．6％～95．4％和97．3％～105．0％，是测定高纯铟中杂质铅和砷的一种简单、快速、准确的方法．     

应用铅同位素比值和元素含量分析法识别有机鸡样品真实性

探究了鸡中铅同位素与相关元素在有机养殖和常规养殖中的差异性,以探讨有机鸡样品溯源的可能性。相同品种的鸡分别采用有机养殖和常规养殖2种不同的饲养方式,利用电感耦合等离子体质谱分别对有机鸡和普通鸡样品中的铅同位素比值和相关元素含量进行测定。方差分析结果表明,铅同位素比值²⁰⁴Pb/²⁰⁶Pb和P、Zn、Fe、Mn、Mg、Ca、Cu、Na、K元素含量具有显著性差异(p＜0.05);主成分分析初步表明,Zn、Mn、Mg、Ca、Cu、Na、K为有机鸡和普通鸡样品中的特征无机元素;聚类分析可将鸡样品分为有机养殖和常规养殖两大类,通过判别分析所得模型的初始分组正确率为100.0%,交叉验证正确率为90.0%。利用铅同位素比值(²⁰⁴Pb/²⁰⁶Pb)、相关元素(P、Zn、Fe、Mn、Mg、Ca、Cu、Na、K)含量分析能够对有机鸡进行有效溯源识别,研究结果可为有机鸡的鉴别研究提供新的方法。     

Preparation of sinapinaldehyde modified mesoporous silica materials and their application in selective extraction of trace Pb(II)

A new solid phase extractant, sinapinaldehyde (SA) modified SBA-15 mesoporous silica, was developed for selective extraction and preconcentration of trace Pb(II) from aqueous solutions. The successful immobilization of SA on SBA-15 and the strong interaction between SA-SBA-15 and Pb(II) were characterized and confirmed by FTIR spectroscopy and scanning electron microscopy. Parameters such as solution pH, shaking time, eluent condition and sample volume were optimized so that the maximum removal of Pb(II) from solution could be achieved. At pH 4.0, the maximum adsorption capacity of the sorbent for Pb(II) was found to be 33.6?mg?g^?1 and the adsorbed Pb(II) could be completely eluted using a mixed solution of 2?M HCl and 5% CS(NH₂)₂. Some common metal ions such as K(I), Na(I), Mg(II), Ca(II), Cr(III), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II) did not interfere with the adsorption of trace Pb(II). The detection limit of the present method was found to be 1.3?ng?mL^?1 and the relative standard deviation was less than 2.0% (n?=?8). These results suggested that this new sorbent is very efficient and selective for the removal of trace Pb(II) in water samples.     

Artifacts in the Determination of Trace Metal Binding Forms in Anoxic Sediments by Sequential Extraction

Abstract

The binding forms of Co, Cd, Cu, Pb, and Zn in an anoxic, sulfide-bearing sediment were investigated by performing both thermodynamic equilibrium calculations and sequential extractions. Care was taken to maintain oxygen-free conditions during the whole experiment. The calculations suggested that trace metals were bound to sulfidic minerals. Sequential extraction results, however, showed increased importance of exchangeable and reducible fractions in the order Cu < Cd < Pb < Zn < Co. Thermodynamic equilibrium calculations of the chemical reactions during extraction showed that Cd, Co, Pb, and Zn sulfides are to a significant extent soluble in the acetate-exchangeable (step 1 + 2) and oxalate-reducible (step 3) fractions. Neglecting the dissolution of sulfide minerals would lead to a misinterpretation of the experimental results.     

Trifluoroethylxanthate as an Analytical Reagent: AAS of Zinc,Antimony and Lead After Coprecipitation of Their Trifluoroethylxanthates onto Microcyrstalline Naphthalene

Abstract

A sensitive method has been developed for the direct atomic absorption spectrometric determination of zinc, antimony and lead after coprecipitation of their trifluoroethylxanthates onto microcrystalline naphthalene. The metal xanthates are quantitatively coprecipitated over the pH ranges: Zn, 5.9–8.4; Sb, 4.0–6.0 and Pb, 4.0–11.0. The solid mass consisting of the metal complex and naphthalene is dissolved in DMF. This solution is aspirated into an air-acetylene flame at 213.9, 217.6 and 217.0nm for Zn, Sb and Pb, respectively. Beer's law is obeyed in the concentration range 2–50, 3–90 and 5–60 μg of Zn, Sb and Pb, respectively in 10ml of the final DMF solution. RSDs are at the ± (0.5–0.6)% level (n=10). The concentration for 1% absorption is 0.019, 0.035 and 0.060μg/ml for Zn, Sb and Pb, respectively. The method is suitable for the preconcentration of the metals from a larger volume of the aqueous phase, and has been employed for their determination in standard reference materials. It may be employed for the simultaneous determination of Zn, Pb and Sb in a solution by pH control.     

Effect of corona discharge on cadmium sulphide and lead sulphide films

This paper describes the effect of corona discharge on cadmium sulphide (CdS) and lead sulphide (PbS) films prepared using the chemical route. The property of films before and after exposure to corona has been described in detail. The electronic properties of the CdS and PbS films have been studied by current-voltage (I-V), capacitance-voltage (C-V) measurements. The structural properties and surface morphology were studied by using X-ray diffraction and scanning electron microscopy before and after exposing to Corona discharge. The films displayed the change in surface morphology after exposure to the corona discharge. It has been found that the films showed an increase in resistivity after exposure. This change in property has been attributed to modification in surface states. Time-dependent recovery indicated that room temperature annealing is sufficient to regain the normal resistivity of the films. The experiment was carried with the aim of studying the effect of the interaction of corona discharge on the semiconductor films and its subsequent effects.     

Deep cleaning of a metallurgical zinc leaching residue and recovery of valuable metals

Huge quantities of zinc leaching residues (ZLRs) generated from zinc production are dumped continuously around the world and pose a potential environmental threat because of their considerable amounts of entrained heavy metals (mainly lead). Most ZLRs have not been properly treated and the valuable metals in them have not yet been effectively recovered. Herein, the deep cleaning of a ZLR and recovery of valuable metals via a hydrometallurgical route were investigated. The cleaning process consists of two essential stages:acid leaching followed by calcium chloride leaching. The optimum conditions for extracting zinc, copper, and indium by acid leaching were a sulfuric acid concentration of 200 g·L-1, a liquid/solid ratio of 4:1 (mL/g), a leaching time of 2 h, and a temperature of 90℃. For lead and silver extractions, the optimum conditions were a calcium chloride concentration of 400 g·L-1, a pH value of 1.0, a leaching time of 1 h, and a temperature of 30℃. After calcium chloride leaching, silver and lead were extracted out and the lead was finally recovered as electrolytic lead by electrowinning. The anglesite phase, which poses the greatest potential environmental hazard, was removed from the ZLR after deep cleaning, thus reducing the cost of environmental management of ZLRs. The treatment of chlorine and spent electrolyte generated in the process was discussed.     

Extremely Photostable Electron-Deficient Phthalocyanines that Generate High Levels of Singlet Oxygen

A robust lead-mediated synthetic procedure for the generation of phthalocyanines substituted with electron-withdrawing groups has been developed. The free-base phthalocyanine and various metal complexes were prepared without discernible degradation of the peripheral electron-withdrawing substituents. Upon irradiation with red light, some of the thus-obtained metal complexes generated high levels of singlet oxygen. In particular, a palladium complex exhibited attractive photostability upon exposure to singlet oxygen as a bleaching agent. The photostability of such complexes that may manifest concomitantly to the generation of high levels of singlet oxygen was attributed to the presence of the electron-withdrawing groups, which results in energetically low-lying highest occupied molecular orbitals.