首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献，搜索用时 421 毫秒
1.
Proposed standard reference material, coastal marine sediment (IAEA-356) recently released under the IAEA Analytical Quality Control Services programme, has been analysed by instrumental neutron activation analysis technique. Up to 32 elements have been measured using the multi-element analysis approach. The precision of measurements varied from 1.3 to 12.5% with median value of 4.9%. The quality control of the data has been validated by analysing IAEA reference material of similar matrix which shows excellent agreement with IAEA values.  相似文献   

2.
The International Atomic Energy Agency (IAEA) organised a proficiency test (PT), IAEA‐CU‐2010‐02, for the determination of elements in sewage sludge. The PT sample was analysed by semi‐absolute standardless k0‐instrumental neutron activation analysis (k0‐INAA). Results for seven elements (As, Co, Cr, Fe, Hg, Se, Zn) were submitted to the IAEA by our laboratory. All of our results were scored ‘acceptable’ by the ‘result evaluation criteria’ adopted by the IAEA. The same analytical methodology produced quantitative results for twenty‐six additional elements. In total, thirty‐six elements were determined with uncertainty varying from 4 to 11%. This paper presents the provisional mass fractions of twenty‐six additional elements (Ag, Al, Br, Ca, Ce, Cl, Dy, Eu, Ga, Hf, I, K, La, Mg, Mn, Na, Rb, Sb, Sc, Sm, Ta, Tb, Th, V, U, W) not reported by the IAEA. The analytical methodology was discussed with important sources of spectral, nuclear and fission‐product interferences. It was shown that the important components of uncertainties were the k0 factor, Q0 factor, detector efficiency, mass and counting statistics. The methodology was validated by analysing the IAEA‐S7 reference material.  相似文献   

3.
Development of new techniques, enabling simultaneous determination of large numbers of elements in environmental samples, can force analysts to use certified reference materials that do not contain all the elements of interest. In this paper, the mass fractions of forty‐six major and trace elements, including rare earth elements (REE), are presented in one soil (NCS DC 77302 also known as GBW 07410) and five sediment (Metranal‐1, IAEA 405, MESS‐3, NCS DC 73309 also known as GBW 07311 and NCS DC 75301 also known as GBW 07314) certified reference materials determined by high resolution inductively coupled plasma‐mass spectrometry. The selected certified materials represent a spectrum of geological matrices often analysed in environmental studies. Measured elements include certified elements, elements listed with information values as well as new elements absent from certificates, including REEs and some other elements. REE + Y mass fractions in the river sediment reference material Metranal‐1 are reported for the first time. The results obtained are in agreement with available certified or information values.  相似文献   

4.
INAA, ICP‐AES and ICP‐MS were used to elementally characterise four environmental reference materials – NIST SRM 1646a (Estuarine Sediment), NIST SRM 1400 (Bone Ash), IAEA‐395 (Urban Dust) and IAEA‐450 (Algae). An analytical scheme consisting of the three methods was first applied to NIST SRM 1646a to validate the methodology because it has been extensively analysed and has certified values for many elements. With repeated analyses of NIST SRM 1646a, the accuracy and measurement repeatability of the data obtained were evaluated based on two statistical calculations (zeta‐score and Horwitz ratio) and were observed to be good enough for the analytical scheme to be applied to similar sorts of environmental/geochemical samples. Applying the same approach to NIST SRM 1400, IAEA‐395 and IAEA‐450, enabled mass fractions of 29, 38 and 28 elements to be determined, respectively. Among these results, the data for rare earth elements are of particular interest, not only for IAEA‐450 but also for the other three reference samples. The data for Pr, Gd, Dy, Ho, Er and Tm in NIST SRM 1646a are newly reported in this study. By using small test portions (< 100 mg) for NIST SRM 1646a and IAEA‐395, and recommended minimum amounts for NIST SRM 1400 and IAEA‐450, sample homogeneity was evaluated.  相似文献   

5.
This paper is intended to be a constructive discussion of Fiket et al. (2017, Geostandards and Geoanalytical Research , 41 , 123–135), who dealt with the determination of major, trace and rare earth elements in several sediment and soil certified reference materials. In the present author's view, the paper by Fiket et al. (2017) suffers from a lack of reference to several publications in which somewhat similar results had already been reported. The present contribution therefore provides a comparison of previously published results with those of Fiket et al. for the CRMs soil NCS DC 77302 (GBW 07410), stream sediment NCS DC 73309 (GBW 07311), marine sediments MESS‐3 and NCS DC 75301 (GBW 07314) and estuarine sediment IAEA‐405. It is argued that this fuller consideration (a) allows critical evaluation of the quality of the results presented by Fiket et al. and (b) highlights the advantages of their work. Finally, attention is drawn to the (possible or real) problems that can arise during simultaneous determination of multiple trace elements.  相似文献   

6.
The water and bed-sediment pollution status of the Padma River was determined by analysis of representative samples for selected metals and ions. Water and bed-sediment samples were collected at a T-dam, Rajshahi, Bangladesh, for 7 months. Water and silt-metal content analysis was performed using atomic absorption spectrophotometry or other analytical methods. The data showed the variation of the metal ion-levels in water as follows: Ca 17.11–48.37 ppm, Na 17.51–20.09 ppm, K 1.00–3.60 ppm, Cr 2.80–7.00 ppm, and SO4 4.17–5.48 ppm; in bed sediment, the levels were Cr 35–1050 ppm and Pb 12–48 ppm. The occurrence of Na, K and Ca was in the normal range (US EPA permissible limit), but the levels of Cr in water were much higher than the permissible limit. The SO4 ion content was well below the pollution level. The concentration of Pb in the bed sediment was within the permissible limit for the standard International Atomic Energy Agency (IAEA) Soil-5a, but the concentration of Cr in the bed sediment was significantly higher than the permissible limit for the standard IAEA Soil-5a. Thus the Padma river water was polluted with Cr. The occurrence of some ions showed a monthly variation. Received: 19 August 1999 · Accepted: 12 October 1999  相似文献   

7.
Trace amounts (from nanogram to microgram levels) of bromine and iodine were determined by inductively coupled plasma-mass spectrometry (ICP-MS) in twenty-three geochemical reference materials issued by the GSJ, USGS, IAEA etc. The pyrohydrolysis technique was used to separate bromine and iodine from samples analysed in the form of powder. The accuracy and precision of the experimental values were assessed by the comparative analysis of well established reference materials such as USGS AGV-1, BCR-1 and IGGE GBW07312. The measured values agreed well with reported values within a 10% error range. We also report reliable new data for these elements in these geochemical reference materials.  相似文献   

8.
This study is aimed at determining the level of environmental degradation as well as the concentration of trace elements in soil and stream sediments in order to evaluate the environmental impact of the mining operation. Twenty-five (25) soils and ten (10) stream sediment samples were collected from the study area. The physicochemical parameters were determined using appropriate instrumentation with the aid of a digital pH meter (Milwaukee meter) to measure the pH and electrical conductivity, total dissolved solids, moisture content and loss on ignition of the soil and stream sediment samples. The pH of the soil sample ranged from (6.10 to 7.19); Electrical conductivity ranged from (21.3 to 279.4 µS/cm), moisture content varied from (0.60% to 7.20%), and the LOI ranged from (2.03% to 18.62%). The results of the analysis showed that the concentrations of the trace elements in the soils and stream sediment samples were slightly higher than the background values. Plots of the trace elements in stream sediment samples show moderate, consistent decrease downstream except at points where there was mine water discharge into the main river. The pollution levels of heavy metals were examined in stream sediment and soil samples using different assessable indices, such as the enrichment factor, which showed significant-moderate enrichment for Cr, Th, Nb, Zn, Pb, Y and Zr and the geo-accumulation index, which showed practically moderate contamination with Cr, Ni and Sr based on regional background reference values. Geo-accumulation index and contamination index for soils and stream sediment revealed uncontaminated to moderate contamination. Likewise, elements with moderate contamination were Cr, Ni and Sr. The Pearson correlation showed that there were significant positive associations among selected metals in soil and stream sediment samples.  相似文献   

9.
Located at the midpoint of the Asian “airborne dust corridor”, Lake Qinghai receives substantial dust annually, which may impact the biogeochemical cycles of the system. In order to determine quantitatively the flux and chemical contributions of dust to Lake Qinghai sediment, dust samples were collected monthly at two sites surrounding the lake from June 2009 to May 2011. The results demonstrate similar chemical compositions of dust samples to the local loess, implying strong representativeness of regional dust. The average dust deposition flux is 265.7 ± 55.0 g/m2/a, constituting 56.6 ± 11.7% of the modern sediment, approximating to previous estimates (∼65%). Contributions of dust-derived elements in the sediment differ substantially, with a minimum of 16.7% for Sr and a maximum of 83.9% for Cu. Among these elements, the contribution of lithophile elements (Na, Al, K, Ti, Mn, Fe and Rb) is close to that of the bulk dust; the contributions of mobile elements (Mg, Ca and Sr) are low, only 16.7% (Sr)–26.1% (Mg), whereas potentially harmful metals (Cu, Zn and Pb) have high contributions (70.3–83.9%). Seasonal variations of elemental inputs indicate that springtime contributions dominate the annual dust fluxes for all elements into the sediment, in agreement with the high dust flux in spring. These observations not only quantify the contribution of dust to the sediment of Lake Qinghai, but also highlight the important role of dust in the accumulation of various elements in the sediment, especially for potentially harmful metals.  相似文献   

10.
In the present study sediment and water samples collected from Kowsar Dam reservoir in Kohkiluye and Boyerahmad Province, southwest of Iran, are subjected to bulk digestion and chemical partitioning. The concentrations of nickel, lead, zinc, copper, cobalt, cadmium, manganese and iron in water and bed sediment were determined by atomic absorption spectrometry. The concentrations of metals bounded to five sedimentary phases were estimated. On this basis, the proportions of natural and anthropogenic elements were calculated.The anthropogenic portion of elements are as follows: zinc (96 %)> cobalt (88 %)> iron (78 %)> magnesium (78 %)> nickel (78 %)> copper (66 %)> lead (63 %)> cadmium (59 %). The results show sediment contamination by nickel, cadmium and lead, according to the world aquatic sediments and mean earth crust values. Manganese and copper have strong association with organic matter and are of high portion of sulfide bounded ions. Finally, The degree of sediment contamination was evaluated using enrichment factor, geo-accumulation index (Igeo) and pollution index (IPoll). The sediments were identified to be of high cadmium and lead pollution index. The pattern of pollution intensity according to enrichment factor is as follows; manganese (1.25) < copper (1.63) < zinc (1.93) < cobalt (2.35) < nickel (3.83) < lead (12.63) < cadmium (78.32). Cluster analysis was performed in order to assess heavy metal interactions between water and sediment. Accordingly, nickel, cadmium and copper are earth originated. Zinc, copper and manganese are dominated by pH. All the elemental concentrations in water and sediment are correlated except for sedimental copper.  相似文献   

11.
The interest in variations of barium (Ba) stable isotope amount ratios in low and high temperature environments has increased over the past several years. Characterisation of Ba isotope ratios of widely available reference materials is now required to validate analytical procedures and to allow comparison of data obtained by different laboratories. We present new Ba isotope amount ratio data for twelve geological reference materials with silicate (AGV‐1, G‐2, BHVO‐1, QLO‐1, BIR‐1, JG‐1a, JB‐1a, JR‐1 and JA‐1), carbonate (IAEA‐CO‐9) and sulfate matrices (IAEA‐SO‐5 and IAEA‐SO‐6) relative to NIST SRM 3104a. In addition, two artificially fractionated in‐house reference materials BaBe12 and BaBe27 (δ137/134Ba = ?1.161 ± 0.049‰ and ?0.616 ± 0.050‰, respectively) are used as quality control solutions for the negative δ‐range. Accuracy of our data was assessed by interlaboratory comparison between the University of Bern and the United States Geological Survey (USGS). Data were measured by MC‐ICP‐MS (Bern) and TIMS (USGS) using two different double spikes for mass bias correction (130Ba–135Ba and 132Ba–136Ba, respectively). MC‐ICP‐MS measurements were further tested for isobaric and non‐spectral matrix effects by a number of common matrix elements. The results are in excellent agreement and suggest data accuracy.  相似文献   

12.
样品用HNO3-HF高压密闭消解,电感耦合等离子体质谱测定海洋沉积物中15种稀土元素。研究了消解方法、酸体系和质谱干扰对稀土元素测定的影响。结果表明,相比于电热板消解和微波消解,高压密闭消解具有酸用量少、消解完全、消解过程损失少等优点;HNO3-HF体系能有效地分解海洋沉积物样品;利用干扰离子校正方程,能有效地校正Ba和轻稀土元素所形成的多原子离子干扰。15种稀土元素的方法检出限为3～15 ng/g。使用水系沉积物标准物质GBW 07309和GBW 07311、海底沉积物标准物质GBW 07313进行验证,测定值与标准值基本吻合,相对标准偏差和相对误差均低于5%。方法用于长江口沉积物样品的测定,精密度(RSD,n=6)小于5%,加标回收率为95.8%～104%。该方法检出限低,精密度和准确度高,适用于大批海洋沉积物样品的分析。  相似文献   

13.
This research was conducted at Samrak Park Delta of Nakdong River Basin in Busan Metropolitan City, Korea. The main objective of this study was to evaluate the interrelationship of geochemical elements in sediments and groundwater through multivariate statistical analyses and a multilayer perceptron artificial neural network model. The mean concentrations of chemical elements were Si (46%), Fe (16.9%), Al (15.7%), K (7.5%) and Ca (4.5%) in sediments, and Na (8650 mg/L), Mg (999 mg/L), Ca (432 mg/L), K (293 mg/L) and Cl (17,640 mg/L) in groundwater, respectively. The principal component analysis produced 3 kinds of factors with the variances of 63.37, 27.02 and 9.62%, respectively. It is suggested that the chemical components of sediments and groundwater were mainly originated from source rocks and seawater intrusion, with the minor impacts of irrigation and industry. Cluster analysis also showed that chemical elements were mainly controlled by the natural geogenic sources and seawater intrusion. Multilayer perceptron of artificial neural network (ANN) presented the good interrelationship between sediment and groundwater. The determination coefficients (R 2) between ANN predicted values and observed values in groundwater showed the high values of 0.61–0.97 except Mg, Mn and Sr. It is revealed that the chemical components of sediment and groundwater were derived from local geological origin and from the minor impact of anthropogenic sources. Multivariate analyses and ANN contributed to the identification of the mutual relationship between the geochemical elements of sediment and those of groundwater.  相似文献   

14.
The research project for the preparation of two polymetallic nodule (GSPN-2, GSPN-3) and two marine sediment (GSMS-2, GSMS-3) reference materials was completed in 1996. The samples were collected from the Eastern and Central Pacific Ocean and prepared to less than 74 μm fine powder. The homogeneity of the materials was tested by X-ray fluorescence spectrometry. The relative standard deviations (RSD %) of measurements of selected elements in samples taken from thirty bottles selected at random were less than 0.5%. Thirty four laboratories worldwide participated in the collaborative analysis programme. The number of elements or constituents analysed was seventy nine for nodules and eighty one for sediments. Among those, sixty three elements were certified in each sample. The sum of major elements or components is 99.7% for GSPN-2, 99.5% for GSPN-3, 99.8% for GSMS-2 and 99.8% for GSMS-3.  相似文献   

15.
Spatial distributions of trace elements in the coastal sea sediments and water of Maslinica Bay (Southern Adriatic), Croatia and possible changes in marine flora and foraminifera communities due to pollution were investigated. Macro, micro and trace elements’ distributions in five granulometric fractions were determined for each sediment sample. Bulk sediment samples were also subjected to leaching tests. Elemental concentrations in sediments, sediment extracts and seawater were measured by source excited energy dispersive X-ray fluorescence (EDXRF). Concentrations of the elements Cr, Cu, Zn, and Pb in bulk sediment samples taken in the Maslinica Bay were from 2.1 to over six times enriched when compared with the background level determined for coarse grained carbonate sediments. A low degree of trace elements leaching determined for bulk sediments pointed to strong bonding of trace elements to sediment mineral phases. The analyses of marine flora pointed to higher eutrophication, which disturbs the balance between communities and natural habitats.  相似文献   

16.
Three sediment cores were collected in the Scheldt, Lys and Spiere canals, which drain a highly populated and industrialized area in Western Europe. The speciation and the distribution of trace metals in pore waters and sediment particles were assessed through a combination of computational and experimental techniques. The concentrations of dissolved major and trace elements (anions, cations, sulfides, dissolved organic C, Cd, Co, Fe, Mn, Ni, Pb and Zn) were used to calculate the thermodynamic equilibrium speciation in pore waters and to evaluate the saturation of minerals (Visual Minteq software). A sequential extraction procedure was applied on anoxic sediment particles in order to assess the main host phases of trace elements. Manganese was the most labile metal in pore waters and was mainly associated with carbonates in particles. In contrast, a weak affinity of Cd, Co, Ni, Pb and Zn with carbonates was established because: (1) a systematic under-saturation was noticed in pore waters and (2) less than 10% of these elements were extracted in the exchangeable and carbonate sedimentary fraction. In the studied anoxic sediments, the mobility and the lability of trace metals, apart from Mn, seemed to be controlled through the competition between sulfidic and organic ligands. In particular, the necessity of taking into account organic matter in the modelling of thermodynamic equilibrium was demonstrated for Cd, Ni, Zn and Pb, the latter element exhibiting the strongest affinity with humic substances. Consequently, dissolved organic matter could favour the stabilization of trace metals in the liquid phase. Conversely, sulfide minerals played a key role in the scavenging of trace metals in sediment particles. Finally, similar trace metal lability rankings were obtained for the liquid and solid phases.  相似文献   

17.
This work tested the preferential use of fine (<63 μm) or bulk sediment (<2 mm) in environmental research of marine sediments in the Eastern Adriatic. Fine fraction sediment containing silt and clay (<63 μm), predominating in the studied area, was examined to evaluate past and present anthropogenic inputs and to test our hypothesis that investigation of bulk sediment should be preferred. Following aqua regia digestion, chemical analyses of 58 elements were performed by ICP/OES, ICP-MS and cold vapor AAS, and statistical analysis was performed. The concentrations of the majority of the analyzed elements increased with age of the sediment, except for Ag and Sn, which had higher concentrations in recent sediments. The previous main sources of metal contamination in Rijeka harbor were now abandoned municipal-sewage outflow and oil refinery, and continuing harbor activities and antifouling paint use. All activities except of antifouling paint use have been decreasing significantly. Anomalies of selected elements were determined by the box-plot method. More anomalies were found in the bulk sediment than in the fine fraction. Results of Q-modality clustering and factor analysis in the fine fraction almost correlate with that applied on bulk sediments. Thus, it can be said that the differences between the element distribution in the bulk and fine fraction are not statistically significant. Our conclusion is that analysis of bulk marine sediment gives a better insight into the state of pollution and supports previous recommendations to use bulk sediment as a chosen media for environmental studies.  相似文献   

18.
建立了激光剥蚀等离子体质谱法直接测定Li2B4O7熔融玻璃中微量元素的分析方法。详细讨论了内标元素的选择及Li2B4O7熔融玻璃的均一性、背景空白对分析测定的影响。以Li2B4O7熔融玻璃中低同位素丰度的6Li作内标，水系沉积物国家标准参考物质熔融玻璃建立多元素标准校正曲线，用于标准参考物质及水系沉积物定值样品的分析，测定值与标准值或溶液雾化等离子体质谱结果比较，具有较好的一致性。  相似文献   

19.
泛滥平原沉积物标准物质研制   总被引：6，自引：6，他引：0  
泛滥平原沉积物能代表流域内元素的平均分布规律并具有普遍的适用性,是地球化学填图工作的重要介质。目前国际上尚无泛滥平原沉积物标准物质,国外相似标准物质的研制注重于环境方面,定值成分较少;我国同类的土壤和水系沉积物标准物质受限于不同工作需要,研制目的各不相同,且多数标准物质不足。为满足需求,本文研制了长江流域、赣江流域、汉水流域、淮河流域、黄河流域、海河流域、黑龙江流域共7个泛滥平原沉积物国家一级标准物质(编号为GBW07385～GBW07391)。此系列标准物质采用X射线荧光光谱压片法测试了26种成分,主量成分的RSD小于1%,微量元素的RSD约为2%,所有成分的RSD均小于7%,方差检验的F值均小于临界值F0. 05(24,25)=1. 96,表明样品的均匀性良好。在23个月的考察期内,检验的24种成分未发现统计学意义的明显变化,证明样品的稳定性良好。由全国13家实验室采用不同原理的、可靠的多种分析方法共同完成了73种元素和化合物共511个特性成分的定值测试,除GBW07386和GBW07388的CO2未能赋值外,其余494个特性成分给出了认定值与不确定度,15个特性成分给出了参考值,是我国同类标准物质定值最为齐全的一个系列。该系列标准物质代表了各自流域元素的背景含量,适用于多目标地球化学调查、土地质量地球化学调查等样品的分析质量监控,亦可用作环境、农业等领域相关样品测试的量值和质量监控标准。  相似文献   

20.
标准物质参考值的准确性在测试仪器校准、分析数据质量监控以及方法评价等方面具有非常重要的作用.为了检验国家地质标准物质参考值的准确性,本文应用高温高压密闭溶样-电感耦合等离子体质谱法分析了国家地质标准物质的18种岩石(GBW 07103 ～ GBW 07125)、19种沉积物(GBW 07301 ～ GBW 07318)和19种土壤(GBW 07401 ～ GBW 07430)中36种痕量与稀土元素.结果表明,除个别标准样品中的几个元素(Ni、Cr、Pb、Co、Cu、Sc、Yb、Lu)外,其余国家标准物质中36种元素测定结果的相对标准偏差均小于10％;绝大部分元素测定值的相对误差小于10％,测定值与参考值能较好地吻合.将误差较大元素的测定值与其他实验室的测定值以及文献报道值进行了比较,指出已有的参考值需要修正;针对部分沉积物和土壤中的元素未提供参考值,如GBW 07306的Ni、GBW 07313的Be、Hf、Ta,GBW 07314的Li、Be,GBW 07409、GBW 07410和GBW0741 1的Hf、Ta,GBW 07426的Gd、Ta,本文给出了相应的参考值.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号