ICP-MS法测定不同类型水体可滤态与总量结果比对分析

本文运用电感耦合等离子体质谱(ICP-MS)法对不用类型水体(地下水、地表水、水库水和污水)中的10种重金属元素进行了测定和比对分析。结果显示地下水除钴元素可滤态与总量测定结果相当之外总量均大于可滤态、地表水总量均大于可滤态、水库水除锰元素和镍元素可滤态与总量测定值有较差别外其它8种元素总量与可滤态测定值均无明显差异、污水除钛元素外其余9种元素总量与可滤态测定值均无明显差异。其中,地表水与污水钛元素可滤态均未检出,总量测定值为检出限的1倍至3倍,结果可信。此结果证明对于本次用于检测的样品中的钛元素,全部来源于悬浮于水中的直径大于0.45μm的微粒上,其它元素无此特性。     

ASD-ICP-MS联合快速测定《土壤环境质量标准》中的金属元素简

采用HNO3-HCl-HF-HClO4体系在全自动消解仪消解土壤样品,以50.0μg/L的Rh作内标,用电感耦合等离子体-质谱仪同时测定《土壤环境质量标准》的7种元素Cd、 As、Cu、 Pb、 Cr、 Zn、 Ni。结果表明,土壤标样的测定值与标准值吻合,各元素对应的检出限和相对标准偏差分别为： Cd：0.002 mg/kg和3.6%, As：0.05 mg/kg和5.5%, Cu：0.10 mg/kg和2.9%, Pb：0.18 mg/kg和4.7%, Cr：0.25 mg/kg和2.2%, Zn：0.40 mg/kg和3.4%, Ni：0.20 mg/kg和3.8%。该方法简便快捷,灵敏度高,重现性好。     

Real time alteration of a nuclear waste glass and remobilization of lanthanide into an interphase

The development of predictive models for the long term evolution of nuclear waste glass requires the complete knowledge of the glass dissolution at the laboratory scale. A new approach was developed to determine the initial reaction during the first steps of experience, a new concept was developed, based on the combination of dynamic leaching test and the characterization of the altered materials. With this experimental set-up it is possible to follow in real time the glass alteration process at a fine temporal scale. The results put in evidence a singular behaviour of the lanthanide, shown by a concentration peak of La, Nd and Ce after 2 h and a quick decrease of their concentration measured on line in the solution during the leaching test. This fact is directly linked to the development of an interphase (altered layer which differs from the initial solid by its texture, structure and chemical composition) at the interface of the glass surface and the leaching solution. This work is an attempt to integrate the formation of the alteration products (here the interphase) during leaching into the dissolution mechanisms of a nuclear waste glass. A model is proposed and discussed.     

Metals and organic pollutants in snow surrounding an iron factory

To estimate air pollution snow samples were collected in March 2001 at six sites in the vicinity of the Kostomuksha factory in Karelia. Seventy-two chemical elements and more than 200 individual organic compounds were identified by inductively coupled plasma mass spectrometry (ICP-MS) and gas chromatography mass spectrometry (GC-MS). It was found that the levels of Li, B, Al, Fe, Ni, Cu, Zn, Hg, Mn, Mo as well as hydrocarbons, phthalates and phenols exceeded the existing maximum allowable concentrations. A list of toxicants emitted with the factory exhausts and a list of priority pollutants for Kostomuksha were compiled. The impact of the exhausts of the Kostomuksha factory on the environment in Finland is relatively small. Electronic Publication     

Ligand exchange rate of metal-nom complexes by EDTA

Metal complexation by natural ligands is important for metal transport and distribution in surface and ground water. The goal of the work was to study the ligand exchange rate for two important metal ions in natural aquatic systems (Al, Fe) was determined using EDTA and natural organic matter (NOM) of humic type as ligands. After adding EDTA to a solution containing metal-NOM complexes, these complexes dissociated and metal-EDTA complexes were formed. Metal-NOM complexes were separated from metal-EDTA complexes with the help of size-exclusion chromatography and detected by on-line inductively coupled plasma-mass spectrometry (ICP-MS). Injecting the samples into the system over time after addition of EDTA allowed us to measure the rate of the exchange of NOM by EDTA. The experiments could be well described with a first-order rate law assuming that the dissociation of the metal-NOM complexes is the rate-determining step. The exchange rate of Fe was found to be faster than that of Al. This corresponds well with the exchange rate of water molecules from the coordination sphere of the metal ions, which is also faster for Fe than for Al. Furthermore, the UV and the fluorescence signal of the chromatograms were measured. The results indicate that no disaggregation of NOM molecules took place, although about 75-85% of the aggregate-forming metal ions exchanged NOM by EDTA in their coordination sphere. This suggests clearly the fundamental role of NOM in colloidal transport of metals and in their bioavailability.     

珠江三角洲养殖鱼塘水体中重金属污染特征和评估

为了解珠江三角洲主要养殖环境中重金属含量及潜在生态危害程度,用电感藕合等离子质谱法和原子荧光法测定了肇庆、广州、惠州和茂名4市14个样点沉积物中7种元素的水体及底泥总量,并对底泥中主要重金属污染状况及潜在生态风险进行了评价。结果表明：养殖鱼塘水体中Cr质量浓度范围是nd-0.1011 mg·L-1,超标率为7.1%,Cu质量浓度范围为nd-0.1438 mg·L-1,超标率为64.3%,As质量浓度范围是0.0112-0.0812 mg·L-1,超标率为24.1%,Hg质量浓度范围是0.00004-0.00458 mg·L^-1,超标率为35.7%,Pb质量浓度范围为nd-0.0973 mg·L^-1,超标率为6.8%,其余Ni、Zn和Cd质量浓度范围分别为nd-0.0218、nd-0.0232和nd-0.00319 mg·L^-1,均未超渔业水质标准;底泥中重金属元素Cr、Cu、Zn、As、Hg、Cd和Pb的平均值分别为83.86、46.19、242.16、32.38、0.64、1.00和60.06 mg·kg^-1,地积累指数评价结果显示,表层沉积物重金属污染程度顺序为Cd＞Hg＞Zn＞Pb＞As＞Cu＞Cr,其中,Cd污染程度为中-强,是底泥污染最严重的元素。潜在生态风险指数分析,单项潜在生态风险指数生态风险均值排列顺序为 Hg＞As＞Cd＞Pb＞Cu＞Zn＞Cr。对区域综合潜在生态风险指数RI的贡献率最大的元素为Hg、As和Cd。4个市底泥潜在生态风险综合指数（RI）比较,惠州（290.13）＞广州（240.54）＞茂名（193.23）＞肇庆（116.40）。Hg和Cd是该水域污染和潜在生态风险最大的元素。     

ASD—ICP—MS联合快速测定土壤中部分金属元素

土壤环境质量例行监测正在全国展开,如何准确快速分析土壤中的金属含量成为当务之急。采用HNO3-HCl-HF—HClO4体系在全自动消解仪（ASD）上对土壤进行前处理,以50．0μg／L的铑作内标,电感耦合等离子体-质谱仪同时测定《土壤环境质量标准》的7种元素：Cd、As、Cu、Ph、Cr、Zn、Ni。各元素的方法检出限为0．003～0．40mg／kg,相对标准偏差小于6．0％,土壤标样的测定值与标准值吻合。该方法简便快捷、灵敏度高、重现性好,为大批量土壤重金属元素含量的快速测定提供了可靠地消解-分析方法。     

U and Th in some brown coals of Serbia and Montenegro and their environmental impact

GOAL, SCOPE AND BACKGROUND: The objective of this paper is to determine and compare the concentrations of U and Th in soft to hard brown (lignite to sub-bituminous) coals of Serbia and Montenegro. It also presents comparison of the obtained data on U and Th concentrations with the published data on coals located in some other countries of the world. Almost the whole coal production of Serbia and Montenegro is used as feed coals for combustion in thermal power plants. METHODS: Channel samples from open pit and underground mines and core samples were collected for hard and soft brown coals. For the analysis the samples were decomposed using microwave technique. Obtained solutions containing U and Th were analyzed by inductively coupled plasma mass spectroscopy (ICP-MS) using NIST standards. RESULTS: Concentration of U from the investigated basins and the corresponding mine fields ranges within 0.60-70.10 mg/kg, 0.65-3.20 mg/kg, 0.95-6.59 mg/kg, 1.20-6.05 mg/kg, 0.80-6.66 mg/kg, 0.18-89.90 mg/kg, 0.19-4.14 mg/kg, and 0.28-3.52 mg/kg for the Kostolac, Kolubara, Krepoljin, Sjenica, Soko Banja, Bogovina East field, Senje-Resavica and Pljevlja basins, respectively. Concentration of Th ranges within 0.20-2.60 mg/kg, 0.84-6.57 mg/kg, 1.48-6.48 mg/kg, 0.12-2.71 mg/kg, 0.13-4.95 mg/kg, 0.14-3.48 mg/kg, 0.29-3.56 mg/kg, and 0.17-1.89 mg/kg for the Kostolac, Kolubara, Krepoljin, Sjenica, Soko Banja, Bogovina East field, Senje-Resavica and Pljevlja basins, respectively. DISCUSSION: Brown coal from Senje-Resavica, Kolubara, Kostolac and Pljevlja is characterized by low U concentration. Coals form the Krepoljin, Soko Banja and Sjenica basins have slightly higher U concentrations than the mentioned group. The highest concentration of U is characteristic for the coal from the Bogovina East field. Concentration of Th in coals from Serbia and Montenegro has proved to be low. Out of all investigated coal basins, only the coal from the Krepoljin and Kolubara basins has high concentration of Th. The hydrothermally altered rocks of the Timok dacite-andesite complex, representing the basement of the Bogovina basin, could be a potential source of U, especially at the bottom part of the Lower seam of the Bogovina East field. CONCLUSIONS: This study shows that brown coals in Serbia and Montenegro (soft to hard brown coals or lignite to sub-bituminous) contain low levels of U (5.30 mg/kg, average value and 2.10 mg/kg geometric mean value) and Th (1.80 mg/kg, average value and 1.12 mg/kg geometric mean value). There are some obvious differences in concentration of U and Th in coals from different basins in Serbia and Montenegro. The approximate value for U and Th release mainly from power plants was 644.33 t and 983.46 t, respectively within the period 1965-2000 for the studied mines in Serbia, and 23.76 t and 15.05 t for the Potrlica mine (Montenegro) within the period 1965-1997. RECOMMENDATIONS: The coals in Serbia and Montenegro show no identifiable unfavourable impact on the surrounding environment, due to low natural radioactive concentration of U and Th, but further investigations concerning human health should be performed. PERSPECTIVES: Preliminary research revealed that in some Serbian coals (and, particularly, parts of the coal seam) U and Th content are rather high. Such coals should be carefully studied, as well as U and Th concentrations in ash, fly ash, waste disposals, nearby soil and ground water. Further studies should include determination of the radioactivity of all these products, and estimation of possible health impact.     

衡山PM_（2.5）中痕量金属元素的分析

建立了微波消解-电感耦合等离子体质谱法同时测定PM2.5中12种痕量金属元素的方法。对不同消解体系进行了讨论,确定采用HNO3＋H2O2消解体系。方法检出限在0.01～6.4 ng/m3之间,精密度为0.5%～8.9%,加标回收率在69.2%～92.6%之间。应用该方法测定了衡山PM2.5中痕量金属元素的含量,讨论了痕量元素的浓度分布特征,对各元素进行了相关性分析,并应用富集因子法对来源进行了分析。     

珠江下游河段沉积物中重金属含量及污染评价

为了解珠江下游出海河道沉积物中重金属含量及各污染物的潜在生态危害程度,用电感耦合等离子质谱法和原子荧光法测定了21个样点沉积物中13种元素的总量,及对底泥中主要重金属污染状况和潜在生态风险进行了评价.结果表明,珠江下游河道总Fe、总Mn含量分别为41 658.73 mg.kg-1和1 104.73 mg.kg-1,微量元素Cr、Co、Ni、Cu、Zn、As、Se、Cd、Sb、Pb和Hg的平均值分别为86.62、18.18、54.10、80.20、543.60、119.55、4.28、10.60、20.26、104.58和0.520 mg.kg-1,地积累指数评价结果显示,表层沉积物重金属污染程度顺序为：Cd〉As≈Zn〉Hg〉Pb≈Cu≈Cr,潜在生态风险程度大小顺序：Cd〉Hg〉As〉Cu〉Pb〉Zn〉Cr,Cd是该水域污染和潜在生态风险最大的元素,单项潜在生态风险与区域综合潜在生态风险一致.珠江下游河道底泥Cd、Hg和Pb污染受输入影响北江大于西江和东江.聚类分析结果表明,研究站位潜在生态风险可分5类,基本反映了站位分布及沉积物环境污染变化特征.总体而言,重金属污染和生态风险程度较高的江段有陈村-沙湾段、陈村-顺德港段及外海-虎跳门段,北江及相关河道污染程度和潜在生态风险指数高于区域其他江段.