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1.
《Applied Geochemistry》1999,14(3):301-317
A field filtration method for the concentration and separation of suspended particulate matter (SPM) from freshwater systems for subsequent determination of major elements (Si, Al, Ca, Fe, Mn, Mg, Na, K, P, Ti and S) is validated with respect to precision and bias. The validation comprises the whole procedure including filtration, sample digestion and instrumental analysis. The method includes two digestion procedures (microwave acid digestion and alkali fusion) in combination with inductively coupled plasma atomic emission spectrometry (ICP–AES). Total concentrations of the elements have been determined in suspended particulate matter from lake and river water with low levels of suspended solids (<2 mg l−1 DW), and a wide range of element concentrations. The precision of the method including filtration, digestion and instrumental determination ranges between 10 and 14% RSD for most elements on a dry weight basis. Non-detectable concentrations of some elements are reported due to small differences between blank filter levels and the amounts of elements present on the filters after sampling. The calculated sums of main inorganic components, expressed as oxides, ranges between 94.0 and 98.0% ash weight. The method limits of detection range between 3 and 100 μg, as estimated from the blank filter samples. These detection limits are 3–1000 times higher compared to the corresponding instrumental (ICP–AES) limits of detection.A better knowledge of the mechanisms of filter clogging in sampling of suspended matter is important in order to extend the applicability of the method. For the sample types investigated in this study, the amount of inorganic material in the suspended particulate matter (SPM) seems to be the most important factor controlling the maximum volume of filterable water, and Fe is presumably the most important clogging regulating parameter in the group of elements included in the inorganic matter.A critical evaluation of the indirect method of calculating concentrations in SPM as the difference between unfiltered-digested and filtered subsamples is also included.  相似文献   

2.
The analytical performance of laser ablation (LA) for the determination of Co, Fe, Cd, Ag, Mn, Cu and S in sphalerite was evaluated using double focusing sector field inductively coupled plasma mass spectrometry (ICP-SFMS). Samples were collected from Zinkgruvan, situated in the south central Sweden. The use of Zn for internal standardisation, together with correction for FeS impurities in sphalerite, allows straightforward quantification without using external methods for the determination of the actual Zn content. LA–ICP-SFMS results were compared with data obtained by conventional pneumatic nebulisation introduction of sample solutions following acid digestion. Good agreement between the two methods was obtained for homogeneously distributed elements. For the majority of the elements under consideration, LA–ICP-SFMS precision was better than 10% RSD.  相似文献   

3.
A total of 1785 European bottled water samples were analyzed using standard laboratory methods. The bottled water samples were purchased in 2008 at supermarkets throughout 40 European countries. The samples were analyzed for 71 chemical parameters (As, Al, As, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cs, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Hg, Ho, I, K, La, Li, Lu, Mg, Mn, Mo, Na, Nb, Nd, Ni, Pb, Pr, Rb, Sb, Sc, Se, Sm, Sn, Sr, Ta, Tb, Te, Th, Ti, Tl, Tm, U, V, W, Y, Yb, Zn, Zr, Br−, HCO3−, Cl−, F−, NH4+, NO2−, NO3−, PO43−, SO42−, SiO2, pH, and EC) by quadrupole inductively coupled emission spectroscopy (ICP-QMS, trace elements), inductively coupled plasma atomic emission spectroscopy (ICP-AES, major elements), ion chromatography (IC, anions), atomic fluorescence spectrometry (AFS, Hg), titration (alkalinity), photometric methods (NH4+), potentiometric methods (pH), and conductometric methods (specific electrical conductivity, EC). A very strict quality control procedure was followed by analysing blanks, international reference materials, an internal project standard, and duplicate analyses, as well as by analysing 23 elements by both ICP-QMS and ICP-AES. Analysis of marketed bottled water from springs, wells or boreholes, apart from the evaluation of its quality with respect to inorganic elements, it may provide a cheap alternative to obtain a first impression about groundwater chemistry at the European scale.  相似文献   

4.
电感耦合等离子体发射光谱法测定石英砂中15种杂质元素   总被引：1，自引：1，他引：0  
用氢氟酸-高氯酸消解体系分解样品,建立了石英砂中铁、钛、镁、锰、锌、铜、铅、砷、镉、镍、铬、钴、锑、铝、钡等15种杂质元素的电感耦合等离子体发射光谱测定方法。系统研究了氢氟酸-高氯酸和氢氟酸-硫酸消解体系对测定结果的影响,对氢氟酸、高氯酸试剂的用量、消解温度和仪器条件等参数进行了优化。选取石英砂样品进行加标回收试验,方法平均回收率为90.4%~110.7%,相对标准偏差(RSD,n=6)小于5.0%,检出限为0.17~0.88μg/g。方法简单、快速,样品一次前处理即可完成多种元素的检测,灵敏度高,精密度好,可满足生产企业对石英砂产品和原料杂质含量的控制。  相似文献   

5.
探讨生态地球化学评价湿沉降、悬浮物样品分析体系中,进行多元素含量测定的分析测试新方法及样品的制备技术。根据待测元素的不同,分别采用微波消解、酸溶、碱熔等方法进行样品制备,使用原子荧光光谱法、离子选择电极法、电感耦合等离子体发射光谱法、电感耦合等离子体质谱法等进行样品的测定。文章系统地建立了生态地球化学评价湿沉降、悬浮物样品的多元素分析体系,利用建立的方法对不同种类的国家标准物质进行测定,结果令人满意。  相似文献   

6.
General geochemical parameters of water, superficial sediments, and suspended particulate matter (SPM) were determined from small shallow saline lakes (soda ponds) as well as from lake Neusiedlersee in eastern Austria. Additionally, instrumental neutron activation analysis (INAA) was used to determine the distribution of major, rare earth and other trace elements in superficial sediments and SPM. Chemical results show remarkable differences in salinity and ionic strength between the investigated ponds. Anthropogenic effects, such as drawdown of ground water level and a loss of lake water due to drainage, are clearly reflected in obtained chemical and geological data. Due to a strong dependence of the complexation and scavenging behavior of the rare earth elements (REE) on ionic strength, a significant difference between REE concentrations in soda ponds with different anthropogenic impact was found. The content and composition of authigenic evaporitic minerals in superficial sediments and SPM clearly differ with a fluctuating water level and salt concentration. Furthermore, we determined the distribution of major and trace elements in superficial sediments of a nearby fluvial system. Our results show a clear correlation between REE superficial sediment concentrations in anthropogenically degraded soda ponds and fluvial system. Therefore, we assume that REE concentrations of sediments and SPM are suitable for the study of geochemical changes of inland saline lakes due to anthropogenic impacts on water balance.  相似文献   

7.
Laser ablation inductively coupled plasma mass spectrometry (LA‐ICP‐MS) is a high spatial resolution analytical method which has been applied to the analysis of silicic tephras. With current instrumentation, around 30 trace elements can be determined from single glass shards as small as ～ 40 µm, separated from tephra deposits. As a result of element fractionation during the ablation process using a 266 nm laser, a relatively complex calibration strategy is required. Nonetheless, such a strategy gives analyses which are accurate (typically within ±5%) and have an analytical precision which varies from ～ ±2% at 100 ppm, to ～ ±15% at 1 ppm. Detection limits for elements used in correlation and discrimination studies are well below 1 ppm. Examples of the application of trace element analysis by LA‐ICP‐MS in tephra studies are presented from the USA, New Zealand and the Mediterranean. Improvements in instrumental sensitivity in recent years have the potential to lower detection limits and improve analytical precision, thus allowing the analysis of smaller glass shards from more distal tephras. Laser systems operating at shorter wavelengths (e.g. 193 nm) are now more widely available, and produce a much more controllable ablation in glasses than 266 nm lasers. Crater sizes of <10 µm are easily achieved, and at 193 nm many of the elemental fractionation issues which mar longer wavelengths are overcome. By coupling a short wavelength laser to a modern ICP‐MS it should be possible to determine the trace element composition of glass shards as small as 20 µm and, providing sample preparation issues can be overcome, the determination of the more abundant trace elements in glass shards as small as 10 µm is within instrumental capabilities. This will make it possible to chemically fingerprint tephra deposits which are far from their sources, and will greatly extend the range over which geochemical correlation of tephras can be undertaken. Copyright © 2007 John Wiley & Sons, Ltd.  相似文献   

8.
The complete dissolution of representative test portions of powdered rock samples for the determination of the mass fractions of trace elements by ICP‐MS relies either on aggressive and time‐consuming acid digestions or fusion/sintering with appropriate fluxes. Here, we evaluate a microwave oven dissolution method that employs a solution of NH4HF2 and HNO3. The entire procedure occurs in a closed vessel system and takes up to 4 h. In hundreds of digestions, the precipitation of fluorides was never observed. Replicate decomposition of 100 mg of twenty‐one international reference materials (RMs) of igneous rocks, and also one of a shale presented mostly satisfactory recoveries of forty‐one trace elements. Important exceptions were Zr and Hf in G‐2 and GSP‐2 (mean recoveries of ca. 70%), although for four other felsic rock RMs, the digestion was complete. For ultramafic rock RMs, we present Cr results that indicate quantitative dissolution of Cr‐bearing phases. We discuss the findings and conclude that advances in sample preparation of geological materials for instrumental analysis would benefit from a better understanding of how specific characteristics, such as composition and crystallinity of certain minerals, may affect their reactivity.  相似文献   

9.
A fusion procedure commonly used for major element analysis of silicate rocks (1:5 sample to flux ratio, using 0.7 g of sample) was used to determine a small group of trace elements (Cu, Zn, Rb, Sr, Y, Zr, Nb) by X-ray fluorescence. Compton scatter peak ratioing was successfully used for matrix corrections, despite the thickness of the glass discs being only 1.7 mm. Precision and detection limits were compared with pressed pellet values. For most elements, routine analytical precision is better with powder pellets and detection limits are worse in glass discs, by an average factor of 2, considering all elements analyzed. Accuracy was evaluated with international reference materials and for most of the determinations, good or excellent agreement with recommended values was obtained. The main advantages of using glass discs for the trace element determination are the possibility of analyzing small amounts of sample and the suppression of any mineralogical effects in the glass discs, which can also be used to determine major elements.  相似文献   

10.
晋北-宁北煤中痕量元素的地球化学特征   总被引：2，自引：1，他引：2  
应用仪器中子活化 (INAA)、电感耦合等离子体原子发射光谱 (ICP- AES)和原子吸收光谱 (AAS)等方法测定了晋北-宁北一线 5对矿井、 2个露天矿、 5个电厂和 3个洗煤厂煤中环境敏感性痕量元素的含量;通过与中国土壤、其他地区煤以及世界范围煤中痕量元素含量进行对比,总结了研究区痕量元素的分布、富集特征,得知部分地区煤中 Hg、 Cd和 Se的含量较高,在燃烧利用过程中可能对环境造成影响.通过分析痕量元素与灰分、挥发分的相关性以及痕量元素间、痕量元素与 Al、 Fe和 Sp的相关、聚类特性,探讨了痕量元素间及其与矿物质间的亲合性及赋存特征.  相似文献   

11.
Five commercially available in Estonia brands of bottled water have been analysed for 59 chemical elements by ICP-QMS and ICP-AES techniques to assess the quality of domestic mineral waters in scope of the European Groundwater Geochemistry Project initiated by the Geochemistry Expert Group of EuroGeoSurveys. Contents of 9 cations and anions, pH and electrical conductivity (EC) were measured in the bottled mineral waters by IC, titration and photometric methods. The data showed a significant difference between natural undiluted mineral water (Värska Originaal) characterised by the highest values of pH, EC and majority of trace elements studied, and other domestic waters sold in Estonia.  相似文献   

12.
《Chemical Geology》2007,236(1-2):13-26
We examined the coprecipitation behavior of Ti, Mo, Sn and Sb in Ca–Al–Mg fluorides under two different fluoride forming conditions: at < 70 °C in an ultrasonic bath (denoted as the ultrasonic method) and at 245 °C using a Teflon bomb (denoted as the bomb method). In the ultrasonic method, small amounts of Ti, Mo and Sn coprecipitation were observed with 100% Ca and 100% Mg fluorides. No coprecipitation of Ti, Mo, Sn and Sb in Ca–Al–Mg fluorides occurred when the sample was decomposed by the bomb method except for 100% Ca fluoride. Based on our coprecipitation observations, we have developed a simultaneous determination method for B, Ti, Zr, Nb, Mo, Sn, Sb, Hf and Ta by Q-pole type ICP-MS (ICP-QMS) and sector field type ICP-MS (ICP-SFMS). 9–50 mg of samples with Zr–Mo–Sn–Sb–Hf spikes were decomposed by HF using the bomb method and the ultrasonic method with B spike. The sample was then evaporated and re-dissolved into 0.5 mol l− 1 HF, followed by the removal of fluorides by centrifuging. B, Zr, Mo, Sn, Sb and Hf were measured by ID method. Nb and Ta were measured by the ID-internal standardization method, based on Nb/Mo and Ta/Mo ratios using ICP-QMS, for which pseudo-FI was developed and applied. When 100% recovery yields of Zr and Hf are expected, Nb/Zr and Ta/Hf ratios may also be used. Ti was determined by the ID-internal standardization method, based on the Ti/Nb ratio from ICP-SFMS. Only 0.053 ml sample solution was required for measurement of all 9 elements. Dilution factors of ≤ 340 were aspirated without matrix effects. To demonstrate the applicability of our method, 4 carbonaceous chondrites (Ivuna, Orgueil, Cold Bokkeveld and Allende) as well as GSJ and USGS silicate reference materials of basalts, andesites and peridotites were analyzed. Our analytical results are consistent with previous studies, and the mean reproducibility of each element is 1.0–4.6% for basalts and andesites, and 6.7–11% for peridotites except for TiO2.  相似文献   

13.
Analytical perspective on trace element species of interest in exploration   总被引：1，自引：0，他引：1  
Analysis of soil and sediment samples, using selective extraction methods to distinguish different phases, is of particular interest in exploration geochemistry to locate deeply buried mineral deposits. There are various mechanisms of binding labile elements in the secondary environment, including physical and chemical sorption, precipitation, chelation and complexation. Phases present in soils and sediments which are likely to scavenge ‘free' elements include amorphous Mn and Fe oxides, the humic and fulvic components of humus, and clays. This paper reviews these forms of trace elements and the methods in current use to quantify them. Examples of precision data, both for control and survey samples, are given with respect to trace elements dissolved from the ‘soluble organic' component of humus, Mn oxides and amorphous Fe oxides. The high sensitivity of inductively coupled plasma mass spectrometry (ICP–MS) is required to measure accurately and precisely a large suite of trace elements, especially where only small fractions of elements are dissolved by such leaches as the commercially available Enzyme and MMI (Mobile Metal Ion) extractions. The relative standard deviations (RSD) obtained for 33 elements (e.g. Ag, Cd, In, I) in the standard reference sample (SRM), TILL-2, are in the range 0.5–8% for the hydroxylamine hydrochloride (NH2OH·HCl) leach designed to extract hydrous Fe and Mn oxides. The corresponding RSDs for elements in the reactive Mn oxide phase extracted by the Enzyme leach are in the range 3–19% except for some trace elements at levels close to detection limit (e.g. Cd, Bi). The RSDs obtained for field duplicates are inferior to those for analytical replicates (i.e. sample splits), probably a reflection of different concentrations of the host phase. In one soil survey, the Fe extracted by a 0.25 M NH2OH·HCl leach ranged conservatively from 0.2 to 1.7% whereas the Mn extracted by the Enzyme leach varied extensively, from 0.3 to >999 ppm. In contrast, precision, at 1–7% RSD, for field duplicates was found to be comparable with that for both analytical duplicates and the SRM, LKSD-4, for elements associated with the humic and fulvic component of humus samples sieved to <177 μm.  相似文献   

14.
A sequential extraction procedure, using acid digestion in a CEM MDS-81D® microwave system, is reported for the investigation of trace and minor element associations in coal in (1) mineral phases other than pyrite, (2) pyrite and (3) the organic matrix. The concentrations of sulphate, pyrite and organic sulphur can also be determined by this method. The extract solutions from each stage are rapidly analysed by ICP-AES. The association of major, minor and trace elements with mineral and organic phases is suggested for a suite of certified reference coal samples. In stage 1, a significant percentage of the total Ba, Co, Cr, Cu, Mn, Ni, Pb and Sr was extracted suggesting an association with silicate, carbonate, sulphate and phosphate minerals for these elements. In stage 2, a proportion of the Cu, Mn, Ni, Pb and Zn was dissolved implying the occurrence of these elements in pyrite. An association with the organic matrix is suggested for Cr and also for Ba and Sr in lower rank coals.  相似文献   

15.
The market for mineral water has been growing steadily over the last few years. Germany is the country with the highest number of bottled mineral water brands (908 bottled water samples from 502 wells/brands were analyzed). The per capita consumption of mineral water in Germany in 2003 was 129 L. A wide range of values of one to seven orders of magnitude was determined for 71 elements in the bottled water samples analyzed by ICP-QMS, ICP-AES, IC, titration, photometric, conductometric and potentiometric methods. A comparison of the element concentrations and the legal limits for both bottled and tap water (EU, Germany, US EPA, WHO) shows that only 70% of the 908 mineral water samples fulfill the German and EU drinking water (i.e., tap water) regulations for all parameters (not including pH) for which action levels are defined. Nearly 5% of the bottled water samples not fulfill the German and EU regulations for mineral and table water. Comparison of our results with the current German and European action levels for mineral and table water shows that only 42 of the bottled water samples exceed the limits for one or more of the following elements: arsenic, nitrate, nitrite, manganese, nickel and barium concentrations. Ten of the bottled water samples contain uranium concentrations above the 10 μg/L recommended limit.  相似文献   

16.
本文叙述了电感耦合等离子体原子发射光谱法(ICP-AES)测定硅酸盐岩石中的主要元素的分析方法及结果。我国ICP-AES对痕量分析工作已广泛开展,但在硅酸盐主要元素分析方面如何发挥仪器潜力的报导并不多。本文的目的是提供一个同时测定硅酸盐  相似文献   

17.
Particulate trace metal (Cu, Cr, Ni, Pb and Zn) and major element (Fe, Mn and Al) concentrations have been determined following intensive sampling over two consecutive spring tidal cycles in the 'turbidity maximum zone' (TMZ) of the Port Jackson estuary, Australia. Salinity, temperature, pH, dissolved oxygen, suspended particulate matter (SPM) and chlorophyll a were also determined. A three-factor analysis of variance was used to test temporal variability in concentrations of particulate trace metals and major elements as a result of tidal oscillation. Estuarine master variables, such as temperature and pH, varied within a narrow range; nevertheless, the tidal signal was clear for surface and bottom waters. In surface water, no variance was detected in SPM concentrations between consecutive tidal cycles or between tidal stages (i.e. flood, ebb and slack water). In bottom water, however, SPM concentrations were significantly higher (PА.05) at flood tide than at slack high water and ebb tide. Concentrations of particulate trace metals and major elements in surface water do not display significant variability between tidal cycles or stages. Nevertheless, differences within each tidal stage were significant (PА.05) for all elements. In bottom water, only particulate Fe and Al exhibited significant differences (PА.05) between tidal cycles, whereas particulate Ni was the only trace element that presented significant differences (PА.05) between tidal stages, following the distribution of SPM, with highest concentrations at flood tide. Among the metals studied, significant variation was found at all three temporal scales examined (i.e. from hours to consecutive tidal cycles), although the patterns of variation were different for each metal. The semi-diurnal fluctuation of SPM and particulate trace metal concentrations during spring tides is interpreted as a resuspension-deposition cycle caused by cyclical oscillations of bottom currents. The results are discussed in the context of the implications of tidal cycle influence on the geochemistry and cycling of particulate trace metals in the Port Jackson estuary.  相似文献   

18.
采用过氧化钠熔融消解样品,电感耦合等离子体发射光谱法同时测定土壤中31种常量、次量和微量元素。筛选了不同溶矿方法和仪器参数条件,测定结果的相对标准偏差(RSD,n=11)低于6.0%;经土壤国家一级标准物质分析验证,测定结果与标准值吻合。  相似文献   

19.
《Applied Geochemistry》2006,21(7):1135-1151
Trace metal adsorption to suspended particulate matter (SPM) influences bioavailability and toxicity of trace metals in natural waters. For highly contaminated urban catchments in the greater Auckland (New Zealand) area, trace metal adsorption to SPM was assessed and compared to similar data from non-urban catchments in the Auckland region, to determine whether there was any difference in the ability of the SPM to adsorb Cu, Pb and Zn. The degree of trace metal adsorption onto the SPM was assessed by way of adsorption edge experiments. It was found that the ability of the Auckland urban SPM to adsorb trace metals decreased in the order Pb > Cu > Zn. Little difference in adsorption was observed between the non-urban Waikato and Kaipara River SPM and urban SPM, or between urban SPM from different flow regimes and seasons, despite some compositional differences in the SPM. This suggests that on the basis of a single surface-binding site, metal adsorption onto SPM could be readily predicted across a range of urban and non-urban catchments in the Auckland region. Adsorption edges were modelled with a diffuse layer, surface complexation model to assess the role of Fe-oxide in adsorption. The MINTEQA2 model was used, assuming Fe-oxide (as HFO) was the only adsorbing surface. There was generally good agreement between observed and modelled adsorption for Pb, indicating the importance of Fe-oxide surfaces for Pb adsorption. However, the model did not predict Zn or Cu adsorption as well. The TOC content of the SPM, and presence of dissolved ligands and organic matter in the water column, appeared to play an important role in Cu adsorption to the SPM. For Zn, the presence of adsorbing surfaces other than HFO appeared to influence adsorption.  相似文献   

20.
Chemical weathering of basalts in the Putorana Plateau, Central Siberia, has been studied by combining chemical and mineralogical analysis of solids (rocks, soils, river sediments and suspended matter) and fluid solution chemistry in order to quantify CO2 consumption and to assess the major factors controlling basic rock weathering under permafrost-dominated taiga climate. The chemical status of  40 major and trace elements (TE) in pristine boreal rivers and interstitial solutions of permafrost soils has been investigated using in-field ultrafiltration procedure. This revealed strong relationships between concentration of TE and that of major inorganic components of colloids, i.e., Fe or Al. Decomposing plant litter and permafrost thawing are considered important sources of most major and trace elements in Arctic rivers during summertime.  相似文献   

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