共查询到20条相似文献，搜索用时 171 毫秒
1.
电感耦合等离子体发射光谱法直接测定黄铜矿中多元素 总被引：12，自引：12，他引：12
应用电感耦合等离子体原子发射光谱法直接测定黄铜矿中Cu、Fe、Cd、Co、In、Mn、Ni、Pb和Zn9种元素。试样经HCl-HNO3溶解，不需要化学分离，用干扰系数校正法消除黄铜矿中主量元素Cu和Fe对其它微量元素的干扰，以国家一级标准物质GBW 07268检验方法的准确度，结果与标准值相符，相对误差除Ni元素外，其它均小于5．00％，精密度(RSD，n=8)为2．55％～7．62％。 相似文献
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电感耦合等离子体原子发射光谱法测定硅铁中微量元素 总被引：6，自引：1，他引：6
应用电感耦合等离子体发射光谱法对硅铁中微量元素的测定进行了研究，采用基体匹配法消除了大量基体的干扰，选择了最佳激发条件，样品的加标回收率在97％－107％。方法用美国硅铁标样分析验证，测定结果与标准值吻合较好，各元素8次测定的RSD％＜7％。 相似文献
3.
微波消解-等离子体发射光谱法同时测定水中硅铁钠 总被引：1，自引：0，他引：1
讨论使用电感耦合等离子体发射光谱法测定水样中si、Fe、Na时，四种水样前处理方法对测试结果的影响。提出采用HNO3^-HF体系微波消解、H3BO3掩蔽HF的方法前处理水样，用等离子体发射光谱法可同时准确快速地测定水中Si、Fe、Na三种元素的含量。5次测定的相对标准偏差小于4％，加标回收率为89．2％-106％。 相似文献
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电感耦合等离子体发射光谱法测定煤飞灰中的主量与微量元素 总被引：6，自引：0，他引：6
应用等离子发射光谱法,选取适宜的仪器工作条件,考察了煤煤飞灰中的主量元素对测定的影响,建立了快速,准确的等离子发射光测定煤飞灰中主量元素的分析方法,微量元素加标回收率８５．７％－１００．７％,国家标准物质分析结果与推荐值一致。 相似文献
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电感耦合等离子体原子发射光谱法同时测定沉积岩中15个元素 总被引：2，自引：10，他引：2
采用电感耦合等离子体原子发射光谱法同时测定沉积岩样品中K、Na、Ca、Mg、Fe、Mn、Ni、V、Ga、Cu、Zn、Sr、Ba、Cr和B等15个元素。在应用混合酸处理样品的过程中，加入适量的甘露醇能够抑制硼的挥发。在优化选定的仪器条件中，15个元素的检出限为0．0010-0．032mg／L。对岩石国家一级标准物质GBW 07105～GBW 07108进行检测，各元素的测定值与标准值吻合。方法的回收率为93．3％～106．0％，测定结果的相对标准偏差（RSD，n=10）均小于5．2％。 相似文献
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采用发射光谱法，利用NH4F溶液作缓冲剂，通过氟化反应，改变被测元素的蒸发行为，一次完成对样品中W、Sn、Mo、Bi、Ag等多个元素的连续测定，快速、准确。 相似文献
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采用活体采样技术，对少量树木年轮样品的制备和测定方法进行了研究。使用X射线荧光光谱和透空测量方式，对树木年轮中Cl、Si、Na、Al、Mg、P、S、Ca、K、Ti、Mn、Fe、Zn、Cu、Pb、Rb、Sr、Ba等18种元素进行了分析测定，结果与其他方法相符，部分元素的精密度（RSD，n=10）为0．2％～15％。该法效果比较好，同时保证了少量树木年轮样品无损失、无化学组成变化．为后续的等离子体原子发射光谱和质谱联测创造了条件。 相似文献
11.
We have developed a rapid and accurate method to determine Zr, Nb, Hf and Ta (denoted as HFSE) in geological samples by inductively coupled plasma-mass spectrometry fitted with a flow injection system (FI-ICP-MS). The method involves sample decomposition by HF followed by HF dissolution of HFSE coprecipitated with insoluble M and Ca fluoride residues formed during the initial HF attack. This HF solution was directly nebulized into an ICP mass spectrometer. An external calibration curve method and an isotope dilution method (ID) were applied for the determination of Nb and Ta, and of Zr and Hf, respectively. Recovery yields of HFSE were > 96% for peridotite, basalt and andesite compositions, apart from Zr and Hf for peridotite (> 85%). No matrix effects for either signal intensities of HFSE or isotope ratios of Zr and Hf were observed in basalt, andesite and peridotite solutions down to a dilution factor of 100. Detection limits in silicate rocks were 40, 2, 1 and 0.1 ng g-1 for Zr, Nb, Hf and Ta, respectively. This technique required only 0.1 ml of sample solution, and thus is suitable for analysing small and/or precious samples such as meteorites, mantle peridotites and their mineral separates. We also present newly determined data for the Zr, Nb, Hf and Ta concentrations in USGS silicate reference materials DTS-1, PCC-1, BCR-1, BHVO-1 and AGV-1, GSJ reference materials JB-1, -2, -3, JA-1, -2 and -3, and the Smithsonian reference Allende powder. 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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Thomas Meisel Nina Schöner Vaida Paliulionyte Elisabeth Kahr 《Geostandards and Geoanalytical Research》2002,26(1):53-61
Data are reported for rare earth elements (REE), Y, Th, Zr, Hf, Nb and Ta in four geological reference materials using sodium peroxide (Na2 O2 ) sintering and inductively coupled plasma-mass spectrometry. The described procedure was used by students during their thesis work. A compilation of their reference material data acquired over one year of laboratory work demonstrates the ease and reliability of the method and the high reproducibility of the analytical results. Relative standard deviations of up to thirty six measurements of one reference material were lower than 5% for Y and the REE. Reproduciblities of Zr, Hf, Nb, Ta and Th were higher at between 5% and 10%, and can be attributed to the inhomogeneous distribution of zircon and other trace mineral phases and uncorrected drift effects. The concentration data are compared to reference and literature values and demonstrate that the procedure is also accurate. New data on G-3 show some systematic deviations from G-2, which are statistically significant. 相似文献
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《Chemical Geology》2003,193(1-2):109-125
Ilmenite separates from the floor (LS), roof (UBS), and wall (MBS) sequences of the Skaergaard Intrusion were analyzed for major and trace elements using DCP-AES and ICP-MS techniques. In all three sequences, FeO progressively increases, and MgO and Al2O3 progressively decrease with differentiation. Although trace element abundances are, in general, higher in UBS ilmenite than in MBS and LS ilmenite, all three sequences have similar trends for trace element abundance vs. crystallization. Ba, Cs, Rb, Sr, Th, U, Y, and the REEs are excluded elements in ilmenite, and remained at low abundances during differentiation. Cr, Ni, Sc, and V are included elements in ilmenite and other mafic phases, and decreased during differentiation. V contents in ilmenite, however, do not decrease significantly until the upper part of the middle zone, suggesting that magnetite did not begin to affect the magma differentiation trend until much later than when it first appears in the intrusion. Hf, Nb, Ta, and Zr, which are strongly excluded elements in silicates, are included elements in ilmenite. The element ratios Zr/Hf, Y/Ho, Nb/Ta, and U/Th are relatively constant in Skaergaard ilmenite from different parts of the intrusion, suggesting that fluid transport did not significantly effect these elements during differentiation or post-solidification cooling. Calculated partition coefficients for ilmenite in the Skaergaard Intrusion are similar to those reported from previous studies of lunar and terrestrial basalts and kimberlites, and for most elements are significantly lower than those reported for ilmenite in rhyolitic magma. Similar Di's for Zr, Hf, Nb, and Ta suggest that ilmenite crystallization did not significantly affect Zr/Nb or Hf/Ta in the Skaergaard magma, but the ratios of Zr, Hf, Nb, or Ta to other high field strength elements, such as Th, U, Y, or the REEs, may have been altered by ilmenite fractionation. 相似文献
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敞开酸溶和偏硼酸锂碱熔ICP-MS法测定多金属矿中的稀土元素及铌钽锆铪 总被引：2，自引：2，他引：0
用电感耦合等离子体质谱法(ICP-MS)测定地质样品中的稀土及难熔元素,混合酸敞开酸溶法和碱熔融法是两种主要的溶样方法。但地质样品组分复杂,元素之间存在相互共生的现象,对于特殊元素、特殊样品用传统酸溶法会造成部分元素消解不完全,使测定结果不准确;而碱熔法的操作过程繁琐,且溶液盐度高,易产生基体干扰和堵塞仪器进样系统。本文改进了传统四酸和五酸体系,采用氢氟酸-硝酸-硫酸敞开酸溶体系,用国家一级标准物质制作标准曲线测定15种稀土元素,方法准确度(ΔlgC)为0.001～0.027。同时改进了偏硼酸锂碱熔法,样品用偏硼酸锂碱熔提取,加入氢氧化钠调节溶液至碱性条件,所测元素与偏硼酸锂共沉淀后过滤分离熔剂,再用硝酸复溶测定15种稀土元素及铌钽锆铪。两种溶样方法的测定值与认定值的相对误差为1.09%～9.30%。将混合酸敞开酸溶法测定稀土元素、偏硼酸锂碱熔法测定铌钽锆铪的结果与其他实验室密闭酸溶法相比,两组数据的相对偏差为0.13%～15.32%。本实验表明,混合酸敞开酸溶法适用于测定地质样品中的稀土元素,偏硼酸锂碱熔法不仅适用于测定地质样品中的稀土元素及铌钽锆铪,也适用于测定如古老高压变质岩石及铝含量高的样品中的铌钽锆铪。 相似文献
17.
Sonja Aulbach Suzanne Y. O’Reilly Norman J. Pearson 《Contributions to Mineralogy and Petrology》2011,162(5):1047-1062
New trace-element data of rutile in kimberlite-borne ~1.85 Ga eclogite and pyroxenite xenoliths from the central Slave craton,
as well as ~110 Ma MARID xenoliths from the Kaapvaal craton, provide constraints on the origins of lithospheric and sublithospheric
mantle variability in high field strength element ratios. Rutiles in eclogites and pyroxenites have Zr/Hf ranging from 20
to 62 and Nb/Ta ranging from 10 to 40. Rutiles in MARID xenoliths have Zr/Hf from 24 to 33 and Nb/Ta from 10 to 41. Calculated
whole-rock Zr/Hf is suprachondritic for eclogites with suggested gabbroic protoliths and subchondritic for boninite-like eclogites;
the latter is consistent with cpx-controlled depletion in the protolith source. Within each eclogite type, positive correlations
of Zr/Hf with La/Lu and negative correlations with Lu/Hf likely reflect fractionation of cpx and/or plagioclase during crystallisation
of the protoliths. Zr/Hf–Nb/Ta relationships of some MARID-type rocks, which are products of lithospheric mantle metasomatism,
and eclogite xenoliths plot on a silicate differentiation trend, whereas other samples have higher Nb/Ta at a given Zr/Hf.
Fractionation of a few percent rutile from an HFSE-rich mafic melt can generate a trend towards strongly increased Nb/Ta at
minimally changed Zr/Hf in the residual melt. Superposition of rutile fractionation on the effects of silicate differentiation,
which fractionates Zr/Hf more strongly than Nb/Ta, can explain the Zr/Hf–Nb/Ta relationships of most eclogites from the central
Slave craton as well as those of MARID rocks, metasomatised peridotites and group II kimberlites. By contrast, Zr/Hf–Nb/Ta
relationships suggest that Group I kimberlites are mixtures between depleted peridotite and carbonatite. Thus, high Nb/Ta
is a signature of lithospheric processes and may not be important in deeply subducted eclogites that bypass extended residence
in the lithosphere. Conversely, considerable primary Zr/Hf variability was inherited by the eclogites, which is indicative
of the compositional diversity of ancient subducted oceanic crust, which is expected to have generated substantial heterogeneity
in sublithospheric basalt sources. 相似文献
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金沙江蛇绿岩带蛇纹岩中浅色岩类的成因 总被引：4，自引：0，他引：4
浅色岩类的岩石类型包括斜长岩和斜长花岗岩,它们均呈岩块状包裹于蛇纹岩中。浅色岩的正Ｅｕ异常明显,ＲＥＥ参数图解、Ｎｂ／Ｔａ和Ｚｒ／Ｈｆ值等均呈现分离结晶趋势,不相容元素Ｓｒ、Ｂａ、Ｎｂ、Ｔａ、Ｚｒ、Ｈｆ富集,相容元素Ｓｃ、Ｖ、Ｃｏ、Ｎｉ亏损,并与其寄主岩－蛇纹岩形成强烈的互补关系。这些特征表明,浅地是幔源超基性岩浆晚期结晶分异的产物。 相似文献
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三江地区澜沧江带南段半坡杂岩体锆石U-Pb年龄、岩石地球化学特征及板块构造环境 总被引：5，自引：0，他引：5
半坡杂岩体位于滇西澜沧江构造岩浆带南段,岩体主要由橄榄岩、辉石岩、辉长岩和辉长闪长岩等镁铁 超镁铁质岩组成。通过ID-TIMS锆石U-Pb年代学方法对半坡杂岩体中辉长闪长岩进行精确定年,获得其结晶年龄为(294.9±2.6) Ma,表明半坡杂岩体的形成时代为早二叠世。半坡杂岩体中不同类型岩石微量元素、稀土元素和同位素组成相似,均呈现轻稀土元素(LREEs)相对于重稀土元素(HREEs)弱到中等富集,高场强元素Nb、Ta、Zr和Hf相对亏损的特征,εNd(t=295 Ma)为正值,在+3.4~+6.6,接近亏损地幔值,这些特征与典型的大洋岛弧玄武岩的特征相似。混合计算表明,半坡杂岩体母岩浆为地幔楔部分熔融,加上约2%~7%源于大洋俯冲沉积物的富硅熔浆和蚀变洋壳流体形成的岛弧玄武质岩浆。上述年龄和同位素数据提供了早二叠世早期南澜沧江地区洋内俯冲的可靠证据。 相似文献
20.
Results are presented of the determination of Zr, Nb, Hf and Ta in 74 standard reference materials by inductively coupled plasma mass spectrometry (ICP-MS). Samples are decomposed by fusion with lithium metaborate and the analytes are separated prior to analysis by precipitation of their cupferrates. Calibration is made using synthetic solutions and internal standardization with Ru (for Zr and Nb) and Re (for Hf and Ta). Accuracy is assessed by comparison with recommended values and precision is evaluated by replicate analyses of five SRMs. 相似文献