微波消解—ICP-MS法测定鲤鱼和河蚌中汞和砷

采用微波消解样品,电感耦合等离子体质谱检测,以Rh作为内标物进行基体干扰校正,同时测定了鲤鱼和河蚌中Hg和As的含量。结果表明:建立的方法简便、快速、准确,标准曲线的线性关系均大于0.9990,样品加标回收率在97.9%～104%之间。     

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.     

水中钴测定方法的比对研究

通过对石墨炉原子吸收法、电感耦合等离子体质谱法、比色法测定水中钴的方法性能进行比对研究,分析了各自的优缺点,为实验人员对钴分析方法选择提供良好的技术依据。当测定钴含量为5.00%~99.5μg/L时,石墨炉原子吸收法的RSD为2.6%~3.9%,加标回收率为93.5%~101.4%;ICP-MS法的RSD为2.0%~3.3%,加标回收率为95.6%~97.1%;5-CI-PADAB光度法的RSD为3.8%~4.8%,加标回收率为91.6%~103.8%。     

Microwave assisted digestion followed by ICP-MS for determination of trace metals in atmospheric and lake ecosystem

The study of trace metals in the atmosphere and lake water is important due to their critical effects on humans,aquatic animals and the geochemical balance of ecosystems. The objective of this study was to investigate the concentration of trace metals in atmospheric and lake water samples during the rainy season(before and after precipitation)between November and December 2015. Typical methods of sample preparation for trace metal determination such as cloud point extraction,solid phase extraction and dispersive liquid–liquid micro-extraction are time-consuming and difficult to perform; therefore,there is a crucial need for development of more effective sample preparation procedure. A convection microwave assisted digestion procedure for extraction of trace metals was developed for use prior to inductively couple plasma-mass spectrometric determination. The result showed that metals like zinc(133.50–419.30 μg/m~3)and aluminum(53.58–378.93 μg/m~3)had higher concentrations in atmospheric samples as compared to lake samples before precipitation.On the other hand,the concentrations of zinc,aluminum,chromium and arsenic were significantly higher in lake samples after precipitation and lower in atmospheric samples. The relationship between physicochemical parameters(pH and turbidity)and heavy metal concentrations was investigated as well. Furthermore,enrichment factor analysis indicated that anthropogenic sources such as soil dust,biomass burning and fuel combustion influenced the metal concentrations in the atmosphere.     

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。     

Hazardous and essential trace elements profile in the different soft tissues of Lithophaga lithophaga (Linnaeus, 1758) from Southern Adriatic Sea (Italy)

A characterization study of 7 hazardous (Hg, Pb, Cd, As, Cr, U, and Ni) and 11 essential (Co, Mo, Se, Cu, Zn, V, Ca, Al, Sr, Mn, and Fe) trace elements in date mussels (Lithophaga lithophaga,Linnaeus, 1758) was carried out by inductively coupled plasma mass spectrometer. Date mussels (231 individuals), caught in the Gulf of Manfredonia (Southern Italy), were divided into 4 size-related groups. The different tissues (muscle, stomach, hepatopancreas and rest of soft tissues) were separated and analyzed to study the capability of absorption of this species. No particular differences were reported on the basis of the shell size; the soft tissues play an important role on the accumulation levels of hazardous and essential trace elements. These marine animals may be considered a good bioindicator of marine environmental pollution for their longevity and habitat permanence peculiarities.     

京津冀地区城市环境空气颗粒物及其元素特征分析

于2013年四个季度,选择京津冀3个主要城市和1个对照点,以及4个全国大气背景站,同步采集环境空气颗粒物PM10和PM2.5样品,采用微波消解ICP-MS法分析样品中的68种元素.结果表明,京津冀3个城市四个季度PM10和PM2.5均超过国家二级标准限值,且采暖季高于非采暖季.全年PM2.5/PM10比值大于0.5,细颗粒物污染占主导.元素在PM2.5中所占比例高于PM10.而背景点颗粒物浓度低于标准限值,远低于城市点,且四个季节变化不大.在检出的57种元素中, Na、Mg、Al、S、K、Ca、Fe、Zn在0.1~10 μg/m3之间,P、Ti、Mn、Ni、Cu、Ba、Pb在10~100ng/m3之间,其他含量较低元素如Cd、Co、Ge、Ga、Zr、Sr、V等在0.01~10ng/m3之间.元素S、Na、K、Al、Fe、Mg、Ca等含量大于1%,P、Zn、Pb、Cu、Ba等其他元素含量介于0.1%~1%.富集因子分析结果提示,K、Ca、Cr、Fe、Cu、Zn、As、Cd和Pb等9种元素主要来源于人为污染,采暖季与非采暖季富集因子比值在1.1~3.5之间.因子分析提示,燃煤、工业污染源、燃油等是颗粒物污染的主要贡献因素.     

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。