共查询到20条相似文献，搜索用时 78 毫秒
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介绍了一个适合于电感耦合等离子体质谱直接测定土壤、沉积物和生物样品中碘、溴的快速简单的样品前处理方法。样品在φ(NH3·H2O)=10%的水溶液中,于190℃下密封分解18h,溶液适当稀释后放置澄清,用电感耦合等离子体质谱法直接测定溶液中的碘、溴。选用126Te作为内标,补偿基体效应和仪器漂移对分析结果的影响。碘、溴的方法检出限(10σ,DF=100)分别为0.01μg/g、0.04μg/g。用土壤、水系沉积物以及头发等标准物质验证了方法的准确度及精密度,绝大多数样品分析结果在标准值的允许误差范围内。对国家一级标准物质10次测定的RSD为2.0%～8.6%。但方法分析岩石样品结果偏低,不适用于岩石样品的分析。 相似文献
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电感耦合等离子体质谱法同时测定地质样品中锗碘 总被引：2，自引：8，他引：2
样品用NaOH全熔,热水提取,分取部分溶液通过强酸性阳离子交换树脂,分离溶液中大量的钠离子后,采用电感耦合等离子体质谱法同时测定锗和碘。方法的检出限Ge、I分别为0.043μg/g和0.22μg/g,经土壤国家一级标准物质分析验证,结果与标准值相符,12次测定的RSD均小于10%。 相似文献
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碱性模式氢化物发生—原子荧光光谱法测定土壤中的痕量硒 总被引：3，自引：1，他引：3
土壤样品经王水分解，转化成HCl溶液，再用NaOH溶液调至碱性，样品溶液首先与KBH4混合，然后与酸作用完成氢化物发生，用原子荧光光谱法测定样品中的痕量硒。方法检出限为0.01μg/g。线性范围为1－200μg/L，样品中硒的含量为0.082μg/g和0.34μg/g时，RSD（n=12)分别为4.9%和2.9%。方法经土壤国家一级标准物质中硒的测定验证，结果与标准值相符。 相似文献
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电感耦合等离子体质谱法测定地球化学样品中的硼碘锡锗 总被引：4，自引：3，他引：1
在多目标的配套方法中,硼、碘、锡、锗四个元素的分析涉及三个配套方法,发射光谱法测定硼、锡,原子荧光光谱法测定锗,分光光度法或电感耦合等离子体质谱法(ICP-MS)测定碘,分析成本高、检测效率低。本文建立了一种ICP-MS同时测定地球化学样品中硼、碘、锡、锗的方法。样品用过氧化钠熔矿,使难熔元素锡分解完全,熔盐经水提取后加入铼内标,再用阳离子交换树脂分离大量钠盐及大部分阳离子,保证了盐分满足质谱测定的要求。方法检出限分别为硼0.92μg/g、碘0.10μg/g、锡0.29μg/g、锗0.09μg/g,满足多目标测试要求。用国家一级标准物质验证,测定值与认定值一致,相对标准偏差(RSD,n=12)≤5%,适用于批量地球化学样品中硼、碘、锡、锗的测定,样品处理过程简便,检测效率高。 相似文献
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分析地质样品中的溴碘,目前常用的提取方法有半熔法、稀氨水密封溶样法和热解法,但由于元素含量低、易损失,样品分解和溴碘的提取过程是主要的误差来源。本文改进了传统热解法的吸收装置,用液氮冷凝吸收代替常规的碱溶液吸收,提取地质样品中的溴碘,用电感耦合等离子体质谱法测定其含量。以标准偏差的10倍计算,稀释倍数为50,溴碘的检出限分别为0.06μg/g、0.01μg/g,低于传统热解法和半熔法,略高于稀氨水密封溶样法;精密度(RSD)为6.4%~21.0%。本方法相对于传统的碱溶液吸收热解法,减少了碱试剂的引入,降低了基体空白和稀释倍数,提高了精密度,操作较半熔法简便,可作为稀氨水密封溶样法的一种补充方法。因此,对于土壤和水系沉积物,宜采用稀氨水密封溶样法;对于岩石以及采用稀氨水密封溶样法难以完全提取的样品,可采用本方法。 相似文献
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Carius管溶样-标准加入电感耦合等离子体质谱法测定土壤中碘 总被引：2，自引：0，他引：2
建立了利用Carius管提取与标准加入电感耦合等离子体质谱法测定土壤中碘的方法。样品用φ=10%的NH.H2O溶液于密封的Carius管中150℃提取4 h,溶液适当稀释后离心分离沉淀,取出5等份样品上清液,分别加入不同浓度的碘标准储备液,用电感耦合等离子体质谱法测定溶液中的碘,以126Te作为内标。应用该方法分析了土壤国家一级标准物质GBW07404、GBW 07406、GBW 07407中碘的含量分别为(9.58±0.02)μg/g、(19.83±0.01)μg/g和(18.88±0.03)μg/g。分析结果与标准值相符。碘的检出限为0.02μg/g。 相似文献
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《华北地质》2019,(4)
准确测定砷和锑的含量是化探样品测定中的重要内容。本文介绍了测定这两种元素的一种新方法,笔者基于原子荧光光谱仪,试样经氢氟酸-盐酸-硝酸混酸微波消解,高氯酸-硫酸混酸蒸发除去氢氟酸,由盐酸-酒石酸混合溶液定容,从而得到样品中准确的砷、锑含量。本方法砷、锑校准曲线的线性相关系数均大于0.999;检出限分别为砷0.039μg/L、锑0.005 8μg/L。按照实验方法测定水系沉积物、土壤标准物质中砷、锑,结果的相对误差砷为1.52%～6.77%,锑为1.25%～7.17%;相对标准偏差(RSD,n=6)砷为2.27%～5.15%、锑为1.88%～5.81%。本方法适用于化探样品中砷含量在0.05～500μg/g、锑含量在0.05～300μg/g之间的样品测定。 相似文献
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多目标地球化学填图是多目标区域地球化学调查中重要的区域性基础性工作之一,为了更好地反映出地球化学背景变化,要求分析方法具有更高的准确度、精密度以及更低的检出限。地球化学调查样品中的硼锗溴钼锡碘钨主要采用单独或分组熔矿的方法进行制备和测定,操作流程长且涉及6种测定方法。本文基于前人研究,对以上7种元素的分析方法进行系统总结,采用过氧化钠-氢氧化钠碱熔,分取溶液加入柠檬酸,利用阳离子交换树脂,静态交换2～3h,除去溶液中大量的阳离子减少基体干扰,利用电感耦合等离子体质谱法(ICP-MS)测定硼锗溴钼锡碘钨含量。结果表明：7种元素的检出限分别为0.66、0.096、0.78、0.11、0.15、0.29、0.27μg/g,相对标准偏差(RSD,n=11)在2.1%～7.5%之间,均小于10%。该方法操作简便、快速,应用成本低,并且整合了相关6种分析配套方法,应用于测定厚覆盖区地球化学调查样品,精密度和准确度均满足《多目标区域地球化学调查规范(1∶250000)》(DZ/T 0258—2014)要求。 相似文献
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Most sulfide-rich magmatic Ni-Cu-(PGE) deposits form in dynamic magmatic systems by partial melting S-bearing wall rocks with variable degrees of assimilation of miscible silicate and volatile components, and generation of barren to weakly-mineralized immiscible Fe sulfide xenomelts into which Ni-Cu-Co-PGE partition from the magma. Some exceptionally-thick magmatic Cr deposits may form by partial melting oxide-bearing wall rocks with variable degrees of assimilation of the miscible silicate and volatile components, and generation of barren Fe ± Ti oxide xenocrysts into which Cr-Mg-V ± Ti partition from the magma. The products of these processes are variably preserved as skarns, residues, xenoliths, xenocrysts, xenomelts, and xenovolatiles, which play important to critical roles in ore genesis, transport, localization, and/or modification. Incorporation of barren xenoliths/autoliths may induce small amounts of sulfide/chromite to segregate, but incorporation of sulfide xenomelts or oxide xenocrysts with dynamic upgrading of metal tenors (PGE > Cu > Ni > Co and Cr > V > Ti, respectively) is required to make significant ore deposits. Silicate xenomelts are only rarely preserved, but will be variably depleted in chalcophile and ferrous metals. Less dense felsic xenoliths may aid upward sulfide transport by increasing the effective viscosity and decreasing the bulk density of the magma. Denser mafic or metamorphosed xenoliths may also increase the effective viscosity of the magma, but may aid downward sulfide transport by increasing the bulk density of the magma. Sulfide wets olivine, so olivine xenocrysts may act as filter beds to collect advected finely dispersed sulfide droplets, but other silicates and xenoliths may not be wetted by sulfides. Xenovolatiles may retard settling of – or in some cases float – dense sulfide droplets. Reactions of sulfide melts with felsic country rocks may generate Fe-rich skarns that may allow sulfide melts to fractionate to more extreme Cu-Ni-rich compositions. Xenoliths, xenocrysts, xenomelts, and xenovolatiles are more likely to be preserved in cooler basaltic magmas than in hotter komatiitic magmas, and are more likely to be preserved in less dynamic (less turbulent) systems/domain/phases than in more dynamic (more turbulent) systems/domains/phases. Massive to semi-massive Ni-Cu-PGE and Cr mineralization and xenoliths are often localized within footwall embayments, dilations/jogs in dikes, throats of magma conduits, and the horizontal segments of dike-chonolith and dike-sill complexes, which represent fluid dynamic traps for both ascending and descending sulfides/oxides. If skarns, residues, xenoliths, xenocrysts, xenomelts, and/or xenovolatiles are present, they provide important constraints on ore genesis and they are valuable exploration indicators, but they must be included in elemental and isotopic mass balance calculations. 相似文献
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针对兖州煤田下组煤深部开采受奥灰高承压水威胁以及当地大型煤化工企业生产用水量大的现状,在已进行的水文地质勘探及放水试验基础上,评价奥灰富水性,并采用有限差分法进行奥灰疏水降压数值模拟研究,提出水煤共采观点。研究结果表明:兖州煤田深部奥灰水压高,合理布置水煤共采孔,可以实现奥灰水位的有效疏降,疏降中心区水位最大降深可达110 m,突水系数显著下降,提高了下组煤开采的安全性;同时可提供煤化工43200 m3/d的供水量,能达到可持续的、水资源保护性的供水效果,实现下组煤的水煤共采。 相似文献
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《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
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Hirokazu Fujimaki 《Contributions to Mineralogy and Petrology》1986,94(1):42-45
Concentration ratios of Hf, Zr, and REE between zircon, apatite, and liquid were determined for three igneous compositions: two andesites and a diorite. The concentration ratios of these elements between zircon and corresponding liquid can approximate the partition coefficient. Although the concentration ratios between apatite and andesite groundmass can be considered as partition coefficients, those for the apatite in the diorite may deviate from the partition coefficients. The HREE partition coefficients between zircon and liquid are very large (100 for Er to 500 for Lu), and the Hf partition coefficient is even larger. The REE partition coefficients between apatite and liquid are convex upward, and large (D=10–100), whereas the Hf and Zr partition coefficients are less than 1. The large differences between partition coefficients of Lu and Hf for zircon-liquid and for apatite-liquid are confirmed. These partition coefficients are useful for petrogenetic models involving zircon and apatite. 相似文献
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The distribution of Cu, Co, As and Fe was studied downstream from mines and deposits in the Idaho Cobalt Belt (ICB), the largest Co resource in the USA. To evaluate potential contamination in ecosystems in the ICB, mine waste, stream sediment, soil, and water were collected and analyzed for Cu, Co, As and Fe in this area. Concentrations of Cu in mine waste and stream sediment collected proximal to mines in the ICB ranged from 390 to 19,000 μg/g, exceeding the USEPA target clean-up level and the probable effect concentration (PEC) for Cu of 149 μg/g in sediment; PEC is the concentration above which harmful effects are likely in sediment dwelling organisms. In addition concentrations of Cu in mine runoff and stream water collected proximal to mines were highly elevated in the ICB and exceeded the USEPA chronic criterion for aquatic organisms of 6.3 μg/L (at a water hardness of 50 mg/L) and an LC50 concentration for rainbow trout of 14 μg/L for Cu in water. Concentrations of Co in mine waste and stream sediment collected proximal to mines varied from 14 to 7400 μg/g and were highly elevated above regional background concentrations, and generally exceeded the USEPA target clean-up level of 80 μg/g for Co in sediment. Concentrations of Co in water were as high as in 75,000 μg/L in the ICB, exceeding an LC50 of 346 μg/L for rainbow trout for Co in water by as much as two orders of magnitude, likely indicating an adverse effect on trout. Mine waste and stream sediment collected in the ICB also contained highly elevated As concentrations that varied from 26 to 17,000 μg/g, most of which exceeded the PEC of 33 μg/g and the USEPA target clean-up level of 35 μg/g for As in sediment. Conversely, most water samples had As concentrations that were below the 150 μg/L chronic criterion for protection of aquatic organisms and the USEPA target clean-up level of 14 μg/L. There is abundant Fe oxide in streams in the ICB and several samples of mine runoff and stream water exceeded the chronic criterion for protection of aquatic organisms of 1000 μg/L for Fe. There has been extensive remediation of mined areas in the ICB, but because some mine waste remaining in the area contains highly elevated Cu, Co, As and Fe, inhalation or ingestion of mine waste particulates may lead to human exposure to these elements. 相似文献
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E. M. Prasolov S. A. Sergeev B. V. Belyatsky E. S. Bogomolov K. A. Gruzdov I. N. Kapitonov R. Sh. Krymsky V. O. Khalenev 《Geochemistry International》2018,56(1):46-64
This paper reports the first results of a study of 11 isotope systems (3He/4He, 40Ar/36Ar, 34S/32S, 65Cu/63Cu, 62Ni/60Ni, 87Sr/86Sr, 143Nd/144Nd, 206–208Pb/204Pb, Hf–Nd, U–Pb, and Re–Os) in the rocks and ores of the Cu–Ni–PGE deposits of the Norilsk ore district. Almost all the results were obtained at the Center of Isotopic Research of the Karpinskii All-Russia Research Institute of Geology. The use of a number of independent genetic isotopic signatures and comprehensive isotopic knowledge provided a methodic basis for the interpretation of approximately 5000 isotopic analyses of various elements. The presence of materials from two sources, crust and mantle, was detected in the composition of the rocks and ores. The contribution of the crustal source is especially significant in the paleofluids (gas–liquid microinclusions) of the ore-forming medium. Crustal solutions were probably a transport medium during ore formation. Air argon is dominant in the ores, which indicates a connection between the paleofluids and the atmosphere. This suggests intense groundwater circulation during the crystallization of ore minerals. The age of the rocks and ores of the Norilsk deposits was determined. The stage of orebody formation is restricted to a narrow age interval of 250 ± 10 Ma. An isotopic criterion was proposed for the ore-bearing potential of mafic intrusions in the Norilsk–Taimyr region. It includes several interrelated isotopic ratios of various elements: He, Ar, S, and others. 相似文献
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Todd Dunn 《Contributions to Mineralogy and Petrology》1987,96(4):476-484
The crystal/liquid partition coefficients of Lu, Hf, Ti, Mn and Ca have been measured between olivine, clinopyroxene and basaltic melt. The Ti, Mn, and Ca partition coefficients were determined at natural abundance levels. The Lu and Hf partition coefficients were determined at doping levels ranging from 0.5 to 1.5 wt% “trace element” as oxide in order to allow analysis by electron microprobe. Olivine/liquid partition coefficients for Lu, Hf, Ti, Mn, and Ca were determined at 1 bar and temperatures from 1150 to 1177° C. Clinopyroxene/liquid partition coefficients were determined for Lu, Hf, Ti, and Mn at pressures of 10, 15, and 20 kbars and temperatures from 1250 to 1290° C. The olivine/liquid partition coefficients of Hf, Lu, Ti, and Ca are small. D(Hf-ol) is zero within the analytical uncertainty. Both D(Lu-ol) and D(Mn-ol) decrease with increasing temperature, but D(Ti-ol) and D(Ca-ol) are constant over the narrow temperature range studied. The partition coefficient results are summarized below.
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Stratiform quartz-sulphide lodes in Ingladhal occur in a typical Precambrian green-stone-belt environment comprising metabasalts, tuff, chert and cherty iron-sulphide formation. Unusually high cobalt contents of metavolcanics and of sulphide minerals in orebodies suggest a consanguinity between ores and rocks. 90% of total nickel, 70% of total cobalt but only 30% of total copper in rocks occur in silicate phases and thus indicate an early separation of copper from cobalt and nickel. Unusually high non-sulphide copper in barren bedded cherts implies availability of Cu-rich solution prior to their lithification. Pyrite in sediments, in volcanics, and in orebodies is characterized by a distinctive pattern of Co-Ni distribution in each case. Partitioning of Co and Ni between coexisting sulphide pairs is complex, but gross equilibrium is indicated. Very high trace metal content of orebody pyrite sharply contrasts with very low such values in pyrite from adjacent sediments and points to a higher temperature of formation of orebodies. 相似文献
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