ICP-MS法测定仿真饰品中11种重金属迁移量

模拟配戴环境,研究了酸性汗液浸萃样品,建立了ICP-MS同时测定仿真饰品中11种重金属迁移量。优化了实验条件,讨论了内标选择、干扰和消除等。方法对仿真饰品进行了测定,相对标准偏差为2.4%～11%,回收率为84.5%～113.5%。     

Simultaneous determination of traces of heavy metals by solid-phase spectrophotometry

A coupling sensitive solid phase spectrophotometric (SPS) procedure for determination of traces of heavy metals (Me-SPS) and multicomponent analysis by multiple linear regressions (MA), a simple methodology for simultaneous determination of metals in mixtures was inaugurated. The Me-SPS procedure is based on sorption of heavy metals on PAN-resin and direct absorbance measurements of colour product Me-PAN sorbed on a solid carrier in a 1-mm cell. This methodology (Me-SPS-MA) was checked by simultaneous determination of metals in synthetic mixtures with different compositions and contents of metals important in pharmaceutical practice: Zn, Pb, Cd, Cu, Co, and Ni. Good agreement between experimental and theoretical amounts of heavy metals is obtained from the recovery test (78.3–110.0%). The proposed method enables determination of particular metal ion at the ng mL⁻¹ level and it was successfully applied to the determination impurities from heavy metal traces in pharmaceutical substances (Cu in ascorbic acid, Pb in glucose, and Zn in insulin). The proposed procedure could be possible contribution to the development of pharmacopoeial methodology for a heavy metals test.     

湿法消解-电感耦合等离子体质谱(ICP-MS)法测定大气降尘中7种重金属

为精准防控大气降尘污染,提供其重金属检测方法。重点考察了样品前处理中混合酸体系选择和最佳酸用量比对实验。在最优条件下建立了混合酸（硝酸、氢氟酸、盐酸和高氯酸）湿法消解大气降尘样品和电感耦合等离子体质谱仪进行7种重金属（铊、铅、镉、铬、铜、锌和镍）含量测试的实验方法。实验结果显示7种重金属在一定的浓度范围内线性关系好,线性系数均大于0.999,7种重金属方法检出限为0.02 mg/kg～2.0 mg/kg,实际样品6次测定相对标准偏差为1.1 %～5.7 %,加标回收回收率为87.7 %～108.9 %。该方法经济环保、准确快捷,可作为大气沉降重金属检测参考方法。     

Three-step extraction procedure for determination of heavy metals availability to vegetables

A three-step sequential extraction procedure was used to determine the concentration of heavy metal speciation forms in soil. The procedure allows one to identify the pool of heavy metals that can be potentially mobilised under changes in soil pH value or redox potential. It has been shown that similar portions of heavy metals are present in reducible, oxidisable and residual fractions. It was found that soil chemical properties significantly affected the distribution of heavy metals among different fractions and their uptake by vegetables. Cadmium was a dominant element which occurred in the exchangeable fraction—the most bioavailable and potentially toxic.     

Monitoring and statistical evaluation of heavy metals in airborne particulates in Cairo, Egypt

Airborne particulate material was monitored as total suspended particles and particulate matter less than 10 μm at selected sites in Cairo. The selected sites represent heavily industrial and industrial–residential areas of Cairo, Egypt. The filters were further analyzed for lead, cadmium, zinc and nickel using ion chromatography. The chosen method was modified to improve resolution and decrease the retention time. The data obtained were treated statistically using one-way analysis of variance and correlated with the anthropological and industrial activities of the sites. The concentrations of the heavy metals are studied in terms of particle size, time dependence, and safety.     

Sol-gel derived urease-based optical biosensor for the rapid determination of heavy metals

A urease optical biosensor for the determination of heavy metals based on sol-gel immobilization technique was developed. A fluorescent dye, FITC-dextran, was encapsulated and parameters including optical properties of the probe, relative enzyme activity, initial pH value and the buffer concentration for substrate preparation were investigated. In sol-gel immobilization, 1 mM Tris-HCl at pH 7.1 provided a sufficient buffer capacity for metal ion analysis as well as the enzyme activity maintenance. Also, two analytical procedures, incubated and un-incubated systems, were compared to understand the sensitivity and applicability to heavy metal analysis. The developed optical biosensor showed high reproducibility and the relative standard deviation (R.S.D.) of 5.1% (n=10) was obtained. Also, eight measurements can be completed automatically within 36 min. The biosensor has high sensitivity to Cu(II) and Cd(II) and an analytical range of 10-230 μM with a detection limit of 10 μM was achieved. Moreover, biological and environmental samples were examined to evaluate the applicability of the developed biosensor. A 19-82% of inhibition was observed when 20-45 μM metal ions were amended into tested samples, revealing that the developed system has the potential for the determination of heavy metals in real samples.     

ICP-MS法测定硅胶奶嘴中8种可溶性重金属

建立了使用电感耦合等离子体-质谱仪技术(ICP-MS)分析硅胶奶嘴中锰、镍、铜、锌、镉、铅、铬、砷溶出量的方法.应用碰撞反应界面技术(CRI)有效地消除了多原子或离子对待测金属离子的干扰;选用89 Y,115In和209Bi等元素为内标混合液校正基体效应和信号漂移,确定了实验的最佳测定条件;研究了浸泡温度、浸泡时间以及浸泡提取方式对重金属溶出量的影响.该测试方法对于锰、镍、铜、锌、镉、铅、铬、砷的仪器检出限为0.01~2.00μg/L,仪器相对标准偏差为0.4%~2.8%,加标回收率为81.4%~113.1%.该方法快速、简便,具有较好的准确度和精密度,为硅胶奶嘴中重金属含量的监控提供了途径.     

Multielement determination of trace metals in seawater by ICP-MS with aid of down-sized chelating resin-packed minicolumn for preconcentration

The multielement determination of trace metals in seawater was carried out by inductively coupled plasma mass spectrometry (ICP-MS) with aid of a down-sized chelating resin-packed minicolumn for preconcentration. The down-sized chelating resin-packed minicolumn was constructed with two syringe filters (DISMIC 13HP and Millex-LH) and an iminodiacetate chelating resin (Chelex 100, 200-400 mesh), with which trace metals in 50 mL of original seawater sample were concentrated into 0.50 mL of 2 M nitric acid, and then 100-fold preconcentration of trace metals was achieved. Then, 0.50 mL analysis solution was subjected to the multielement determination by ICP-MS equipped with a MicroMist nebulizer for micro-sampling introduction. The preconcentration and elution parameters such as the sample-loading flow rate, the amount of 1 M ammonium acetate for elimination of matrix elements, and the amount of 2 M nitric acid for eluting trace metals were optimized to obtain good recoveries and analytical detection limits for trace metals. The analytical results for V, Mn, Co, Ni, Cu, Zn, Mo, Cd, Pb, and U in three kinds of seawater certified reference materials (CRMs; CASS-3, NASS-4, and NASS-5) agreed well with their certified values. The observed values of rare earth elements (REEs) in the above seawater CRMs were also consistent with the reference values. Therefore, the compiled reference values for the concentrations of REEs in CASS-3, NASS-4, and NASS-5 were proposed based on the observed values and reference data for REEs in these CRMs.     

电感耦合等离子体质谱（ICP-MS）法测定沙虫中10种重金属

建立了密闭高压消解-电感耦合等离子体质谱快速测定了沙虫中10种重金属元素(Pb、Tl、Cd、As、Cr、Ni、V、Cu、Sn、Sb)的方法,并分析了重金属的分布特征。试样经粉碎后,以HNO3和H2O2为消解剂进行消解处理,得到的消解液使用电感耦合等离子体质谱仪测定各元素的含量。结果表明,10种重金属元素元素的方法检出限在0.05～3.4μg/kg之间,相对标准偏差（RSD,n=3）小于4%,在0.05-100μg/L线性范围内线性关系良好,相关系数均大于0.999,方法用于国家有证标准物质（GBW10050）的测定,结果与标示值相符。方法灵敏度高,重现性好,定量准确,适用于沙虫样品的检测。     

尿样中铀同位素的ICP-MS快速测量技术研究

核事故状态下的应急处理,要求对环境介质中的放射性核素进行快速分析。尿样中铀同位素测量作为内照射剂量评价的主要手段,其分析效率越高,则对核事故中涉铀人员的安全救治越及时、有效。而尿样中其它无机离子是铀含量的106倍,导致ICP-MS测量过程中尿盐堵塞进样毛细管。为降低样品的含盐量并获得较好的检测结果,本文对样品预处理过程进行优化。采用先加热氧化去除有机物,再进行1～10倍稀释后测试样品的铀同位素丰度及浓度。结果表明：将25 mL样品稀释至100 mL后效果最佳,分析方法不确定度为5.4 %,回收率95 %~105 %。     

电感耦合等离子体质谱法同时测定蔬菜中13种痕量元素

采用电感耦合等离子体质谱法同时测定蔬菜中锶、铜、硒、钼、锰、锌、钴、铬、镉、铅、镍、砷和铝等13种痕量元素。对质谱干扰和非质谱干扰进行了校正。13种重金属元素在一定的质量浓度范围内与其信号强度呈线性关系,方法的检出限(3s)在0.000 4~1.5μg·L-1之间。方法应用于蔬菜标准物质的分析,测定值与认定值相符。对芦笋样品平行测定6次,测定值的相对标准偏差在5.3%~9.6%之间。     

New trends in removing heavy metals from industrial wastewater

Innovative processes for treating industrial wastewater containing heavy metals often involve technologies for reduction of toxicity in order to meet technology-based treatment standards. This article reviews the recent developments and technical applicability of various treatments for the removal of heavy metals from industrial wastewater. A particular focus is given to innovative physico-chemical removal processes such as; adsorption on new adsorbents, membrane filtration, electrodialysis, and photocatalysis. Their advantages and limitations in application are evaluated. The main operating conditions such as pH and treatment performance are presented. Published studies of 94 cited references (1999–2008) are reviewed.It is evident from survey that new adsorbents and membrane filtration are the most frequently studied and widely applied for the treatment of metal-contaminated wastewater. However, in the near future, the most promising methods to treat such complex systems will be the photocatalytic ones which consume cheap photons from the UV-near visible region. They induce both degradation of organic pollutants and recovery of metals in one-pot systems. On the other hand, from the conventional processes, lime precipitation has been found as one of the most effective means to treat inorganic effluent with a metal concentration of >1000 mg/L. It is important to note that the overall treatment cost of metal-contaminated water varies, depending on the process employed and the local conditions. In general, the technical applicability, plant simplicity and cost-effectiveness are the key factors in selecting the most suitable treatment for inorganic effluent     

Validation of bismuth film electrode for determination of cobalt and cadmium in soil extracts using ICP-MS

A study is presented on the use of the bismuth film electrode (BiFE) operated in the anodic stripping and the cathodic adsorptive stripping voltammetry (ASV, CAdSV) modes, for the determination of two trace heavy metals (Cd and Co, respectively), in soil extract samples. Two types of BiFE were examined in this study: the in situ prepared BiFE, which was employed in ASV determination of Cd, and the ex situ prepared BiFE, which was used in CAdSV of Co with dimethylglyoxime (DMG) as complexing agent. A series of unpretreated soil extracts with varying Cd and Co concentrations were analyzed, and the results obtained compared to those determined using inductively coupled plasma-mass spectrometry (ICP-MS). The results revealed the suitability of stripping analysis at the BiFE for determination of μg l⁻¹ levels of heavy metals in soil extracts. The promising results obtained here, coupled with the non-toxic nature of bismuth (in comparison to commonly used mercury electrodes employed in stripping analysis), offer great promise in centralized and decentralized analysis of trace heavy metals in complex environmental matrices.     

黄芪口服液中8种重金属元素含量的测定

在2015年版《中国药典》的基础上,采用原子荧光光谱法和电感耦合等离子体质谱法对黄芪口服液中的铅、砷、镉、汞、铜、锌、镍和铬进行测定,并对所用试剂、器皿,赶酸时间,内标的种类和加入方式进行了优化。结果表明,在样品处理前对器皿采用硝酸(30%)处理,赶酸时间在1.5h以上,以手动方式加入单内标103 Rh溶液,可以得到较准确、稳定的测定结果,8种元素测定的相对标准偏差(RSD)均小于4%,Hg、As、Cu、Pb、Zn、Cd、Ni、Cr的检出限分别为0.089、0.21、0.45、0.15、0.45、0.025、0.35和0.39μg/L,8种元素的加标回收率在92.0%～114%。方法对于黄芪口服液中痕量元素的检测,结果稳定,过程简单,引入污染小。     

Spectrafluorimetric method for the rapid screening of toxic heavy metals in water samples

A fast and inexpensive sensitive screening test for recognising potential wastewater contamination by the presence of highly toxic heavy metals is described. The test is based on the reaction of the toxic heavy metals Hg(II), Cd(II), Pb(II) and Ag(I) with 6-mercaptopurine (6-MP) to produce highly fluorescent complexes.Optimum experimental conditions include a buffer of pH 7.2 (0.1 M citric acid/0.2 M Na₂HPO₄), a chelating reagent concentration of 6×10⁻⁴ M and the addition of 10⁻⁴ M of o-phenanthroline. The fluorescence emitted by the complexes was measured at 380 and 540 nm for excitation and emission wavelengths, respectively.Detection limits of 4, 3, 6 and 3 μg l⁻¹ were achieved for Hg, Cd, Pb and Ag. Relative standard deviation (R.S.D.) were between ±2 and ±6% of the fluorescence signals for five identical samples. Potential interference effects from other heavy metals (Zn, Mn, Co, Fe, Ni and Cu), which could affect the response of the proposed screening test was investigated. Results showed that none of these metals give rise to noticeable fluorescence signals under the above described experimental conditions.Finally, the capability of the proposed heavy metal screening test for the analysis of contaminated water samples is discussed.     

Solution extraction of transition and post-transition heavy and precious metals by chelate and macrocyclic ligands

This review focuses on compounds and methods that can be used for the extraction and separation from solution of two classes of elements that we define as heavy metals and precious metals. These elements are often targeted because they are toxic, costly, and their coordination chemistry has already been well studied, and because there is a need to develop methods of economically extracting, separating and recovering them from waste sites. This review outlines possible strategies that can be used, and reviews the present literature regarding the available methods for their extraction.     

Assessment of heavy metals leachability from metallo-organic sorbent-iron humate-with the aid of sequential extraction test

The sequential extraction test, known as a BCR procedure, was used to assess a leachability of heavy metals (Zn, Cd, Pb, Cu) from the metallo-organic sorbent—iron humate—loaded with these metals. The sequential test allowed to discriminate between various fractions of heavy metals, namely the acid-extractable fraction, the fraction bound to Fe oxides, and the fraction bound to organic matter. It was proven that the heavy metals are bound mainly to Fe oxides and organic matter, and thus they may be relatively hardly liberated into the environment. The BCR sequential extraction test exhibited a very good repeatability, when it was applied to the loaded sorbent—relative standard deviations were typically lower than 10%.     

Sources of heavy metals in the Western Bay of Izmit surface sediments

The study aimed to examine source apportionment of heavy metals of the surface sediments in the <63?µm size fraction. The sediment samples collected from 34 sites at the Western Bay of Izmit were subjected to a total digestion technique and analysed for major (total organic carbon, Al, Fe, Mg, and S) and trace (As, Cd, Co, Cr, Cu, Mn, Ni, Pb, Sn, V, and Zn) elements by inductively coupled plasma-atomic emission spectrometry. The results were compared with the marine sediment quality standards, as well as literature values reported to assess the pollution status of the sediments. A factor analysis/multiple regression (FA/MR) multivariate receptor modelling technique was used for quantitative source apportionment to estimate the contributions from each source of contamination. Source fingerprints were obtained from the literature. A varimax rotated factor analysis was applied to the whole data set, and four probable source types were identified as the iron and steel industry, paint industry, crustal and sewage for heavy metals, explaining about 84% of the total variance. Source apportionment results derived from the FA and FA/MR methods agree well with each other.     

Analysis of heavy metals in road-deposited sediments

Road-deposited sediments were analysed for heavy metal concentrations at three different landuses (residential, industrial, commercial) in Queensland State, Australia. The sediments were collected using a domestic vacuum cleaner which was proven to be highly efficient in collecting sub-micron particles. Five particle sizes were analysed separately for eight heavy metal elements (Zn, Fe, Pb, Cd, Cu, Cr, Al and Mn). At all sites, the maximum concentration of the heavy metals occurred in the 0.45-75 μm particle size range, which conventional street cleaning services do not remove efficiently. Multicriteria decision making methods (MCDM), PROMETHEE and GAIA, were employed in the data analysis. PROMETHEE, a non-parametric ranking analysis procedure, was used to rank the metal contents of the sediments sampled at each site. The most polluted site and particle size range were the industrial site and the 0.45-75 μm range, respectively. Although the industrial site displayed the highest metal concentrations, the highest heavy metal loading coincided with the highest sediment load, which occurred at the commercial site. GAIA, a special form of principal component analysis, was applied to determine correlations between the heavy metals and particle size ranges and also to assess possible correlation with total organic carbon (TOC). The GAIA-planes revealed that irrespective of the site, most of the heavy metals are adsorbed to sediments below 150 μm. A weak correlation was found between Zn, Mn and TOC at the commercial site. This could lead to higher bioavailability of these metals through complexation reactions with the organic species in the sediments.     

ICP-MS multielemental determination of metals potentially released from dental implants and articular prostheses in human biological fluids

A sector field high-resolution (HR)-ICP-MS and an octapole reaction system (ORS)-ICP-MS have been compared for the simultaneous determination of traces of metals (Ti, V, Cr, Co, Ni, and Mo) released from dental implants and articular prostheses in human biological fluids. Optimum sample treatments were evaluated to minimize matrix effects in urine and whole blood. Urine samples were diluted tenfold with ultrapure water, whereas whole blood samples were digested with high-purity nitric acid and hydrogen peroxide and finally diluted tenfold with ultrapure water. In both matrices, internal standardization (Ga and Y) was employed to avoid potential matrix interferences and ICP-MS signal drift. Spectral interferences arising from the plasma gases or the major components of urine and whole blood were identified by (HR)-ICP-MS at 3,000 resolving power. The capabilities of (HR)-ICP-MS and (ORS)-ICP-MS for the removal of such spectral interferences were evaluated and compared. Results indicate that polyatomic interferences, which hamper the determination of such metallic elements in these biological samples, could be overcome by using a resolving power of 3,000. Using (ORS)-ICP-MS, all those elements could be quantified except Ti and V (due to the polyatomic ions ³¹P¹⁶O and ³⁵Cl¹⁶O, respectively). The accuracy of the proposed methodologies by (HR)- and (ORS)-ICP-MS was checked against two reference materials. Good agreement between the given values and the concentrations obtained for all the analytes under scrutiny was found except for Ti and V when analyzed by (ORS)-ICP-MS.