大连近岸海域双壳贝类重金属污染调查与评价

采用电感耦合等离子体质谱法(ICP-MS)对大连近岸海域虾夷扇贝(Patinopecten yessoensis)、紫贻贝(Mytilus edulis)、菲律宾蛤仔(Ruditapes philippinarum)、缢蛏(Sinonovacula constricta)、赤贝(Arkshell)、牡蛎(Oyster)等双壳经济贝类体内Pb、Cd、Hg、Cr、Cu、Zn、Mn、Ni等重金属污染状况进行调查,对其重金属含量进行了初步评价。结果表明:虾夷扇贝中重金属存在组织间差异性,Cd、Cu在闭壳肌中含量明显低于其他组织,Cr、Ni在各组织间差异较小;双壳贝类中重金属存在明显的种间差异性,Zn、Cu在牡蛎中含量相对其他贝类较高;调查海区内双壳贝类中重金属大多符合我国《无公害食品水产品中有毒有害物质限量》等卫生要求,部分双壳贝类品种Cd、Pb含量超标。     

混酸微波辅助萃取ICP-MS测定不同性质土壤中的重金属元素

比较了硝酸(HNO3)、硝酸-盐酸(HNO3∶HCl=3∶1)、硝酸-盐酸-双氧水(HNO3∶HCl∶H2O2=3∶1∶1)和硝酸-盐酸-高氯酸(HNO3∶HCl∶HCl O4=3∶1∶1)等4种消解液对土壤中铅(Pb)、镉(Cd)、砷(As)、铬(Cr)、镍(Ni)、铜(Cu)和锌(Zn)等7种重金属元素的萃取效率.结果表明,硝酸-盐酸-高氯酸混合液的萃取效果最好,硝酸-盐酸混合液次之.通过对6种土壤标准物质的分析发现,除了Cr之外,其他重金属元素在土壤中的混酸微波可提取态含量与总含量接近.土壤中的Cr有一部分是以铬铁矿的形式存在,在环境中相对较为稳定,采用混酸微波可提取态的Cr来评估其对环境的危害能够获得更加准确的结果.重金属与土壤的结合强弱与成土母质相关,冲积母质的土壤中Pb、Zn和Cu的结合较强,萃取相对较难,Cd、Ni和As与土壤的结合强弱则与成土母质关系不大.采用最优的消解液萃取矿区河流底泥和土壤中的重金属,ICP-MS分析结果表明,底泥中重金属含量较高,应为尾砂冲积而成,矿区周边的土壤也受到不同程度重金属的污染.     

ICP-MS对再生水灌溉区土壤重金属含量的测定

采用ICP-MS(电感耦合等离子光谱)对北京市3个再生水灌溉区8种土壤重金属含量进行分析测定,并将其分别与当地井灌区土壤重金属含量作对比,探究再生水灌溉对土壤重金属含量的影响。结果表明:3个再生水灌区均存在不同程度的汞污染,土壤中的Cd、Ni、Cu和As含量均符合国家土壤环境质量一级标准,而Pb、Zn和Cr含量的最大值(39.90、103.1和120.3 mg/kg)未超过国家土壤环境质量二级标准;Ni和Hg在多数采样点出现重金属向土壤深层移动的趋势;与对照区(井灌区)相比,Cd在3个再生水灌区的土壤中含量均无显著变化,Hg含量仅在通州区大北关井灌区超过再生水灌区,其余6种重金属则呈现不同程度的重金属累积现象。再生水灌溉区土壤重金属污染并非一定由再生水灌溉所致,早期的污水灌溉和有机肥施用等也是不可忽视的因素。     

ICP-MS的安装调试和日常维护的注意事项

ICP-MS广泛的用于环境监测系统。本文主要围绕ICP-MS的安装调试、维护保养以及在日常检测工作中应注意的事项展开了讨论。并结合笔者自身经验提出了如何减少故障的办法。     

原子荧光法和电感耦合等离子体质谱法测定水中锑的比较

分别用原子荧光法(AFS)和电感耦合等离子体质谱法(ICP-MS)测定水中锑。AFS法和ICP-MS法均线性良好,相关系数分别为0.999 8和0.999 9,检出限分别为0.17和0.03μg/L,相对标准偏差均1.15%,加标回收率分别为96.6%~111.9%和95.4%~111.5%,2种方法均能很好地用于水中锑的测定。其中,ICP-MS法适合较清洁地表水和地下水样品中锑的分析,AFS法则对地表水、地下水和废水样品均适用。     

微波消解体系与聚四氟乙烯滤膜对PM2.5中重金属测定的影响

采用4种微波消解体系对聚四氟乙烯(PTFE)材质滤膜采集的PM2.5样品进行消解,利用电感耦合等离子体质谱(ICP-MS)测定样品中Cr、Mn、Cu、As、Cd 5种重金属元素含量,并计算其空白加标和样品加标回收率,建立了测定PTFE材质滤膜采集的PM2.5样品中重金属元素的最优微波消解体系。结果表明,4种消解体系下,空白加标回收率和样品加标回收率均处于合理范围,分别为95.3%~116.3%和93.3%~118.5%。其中,HNO3放置过夜+H2O2消解体系具有空白值低、测定稳定性强、操作简便、绿色环保、对人体健康危害小等优点,能够满足大批量PM2.5样品中重金属总量的快速、高效、准确分析的要求。     

微波消解-ICP-MS测定土壤和底泥中的12种金属元素

以20.0μg/L铟作内标,采用硝酸-氢氟酸-过氧化氢体系微波消解,ICP-MS(电感耦合等离子体质谱法)同时测定土壤和底泥中的12种金属元素,各元素方法检出限为0.003～0.2μg/g,相对标准偏差小于6.1%,土壤标准样品的测定值与标准值吻合。方法简便快捷,灵敏度高,重现性好,是分析大批量土壤和底泥样品中多元素的可靠、高效方法。     

铅在植物-环境体系中的吸收、分布和迁移规律的稳定同位素示踪法研究

以低浓度的稳定铅同位素为示踪剂,采用电感耦合等离子质谱法,通过盆栽实验,考察了在不同的pH值环境和不同铅源引入方式下,茶树植株对铅的吸收情况以及铅在植株体内的分布及迁移规律.结果表明:茶树植株对大气铅源污染的反应比土壤铅源污染灵敏;大气铅源污染有往顶端(芽)迁移的趋势,而土壤铅源污染则主要聚集在根部;低pH条件增强植株对铅的吸收且能促使植株体内的铅的往高处迁移.本实验方法危害小,更接近植株承受低浓度污染的实际情况,能区分实验引入铅源和环境引入铅源.     

Determination of total organic halogen (TOX) in humic acids after microwave-induced combustion

Chemically chlorinated organic matter as well as natural background humic acids contain significant amounts of organically bound halogens that must be determined for assessment of environmental pollution. In this work the use of ion chromatography (IC) and inductively coupled plasma mass spectrometry (ICP-MS) is proposed for the determination of total organic Cl, Br and I concentration in humic acids extracted from various forest soil horizons after a single digestion by microwave-induced combustion (MIC). Samples were pressed as pellets and combusted using 20 bar of oxygen and ammonium nitrate solution as igniter. Analytes were absorbed in diluted alkaline solution (50 mM (NH₄)₂CO₃) and a reflux step was applied after combustion to improve analyte recoveries (5 min, microwave power of 1400 W). The accuracy was evaluated using certified reference materials (CRM) and spiked samples. Using MIC the agreement with CRM values and spike recoveries was higher than 97% for all analytes. As an advantage over conventional procedures, using MIC it was possible to digest up to eight samples in only 25 min, obtaining a single solution suitable for all halogens determination in humic acids samples by different techniques (IC and ICP-MS). The limit of detection (3σ) for Cl, Br and I obtained by IC was 1.2, 2.5 and 4.3 μg g⁻¹ and by ICP-MS it was 1.4, 0.03 and 0.002 μg g⁻¹, respectively.     

A rapid isotope ratio analysis protocol for nuclear solid materials using nano-second laser-ablation time-of-flight ICP-MS

The analysis of the isotopic composition of nuclear or non-nuclear solid materials is performed in a variety of fields, e.g., for quality assurance in the production of nuclear fuels, as signatures in forensics, nuclear safeguards, and non-proliferation control, in material characterization, geology, and archeology. We have investigated the capability of laser ablation (New Wave Research, 213 nm) coupled to time-of-flight (TOF) ICP-MS (GBC OptiMass 8000) as a rapid analytical protocol for multi-isotope screening of nuclear and non-nuclear solid samples. This includes natural and non-natural isotopic compositions for elements including Cu, Zr, Mo, Cd, In, Ba, Ta, W, Re, Pt, Pb, and U, in pure metals, alloys, and glasses. Without correcting for mass bias (mass fractionation), an overall precision and accuracy of about 4% (1σ) can be achieved by minimizing the deposited laser power and thus fractionation (mass removal based on thermal properties). The precision and accuracy in combination with literally no or minimized sample preparation enables a rapid isotope screening of solid samples that is of particular interest to support nuclear forensic and safeguard analysis.