共查询到19条相似文献，搜索用时 158 毫秒
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1：20万岩石化探测量碳酸盐岩分析方法研究—等离子体质谱为主的配套分析方法 总被引：6，自引：3，他引：3
研究了碳酸盐岩中基体元素Ｃａ和Ｍｇ对测定痕量元素的影响及消除办法,建立了用等离子体质谱法测定碳酸盐岩石中２６个痕量元素的３个分析流程;采用用Ｘ射线荧光光谱、石墨炉原子吸收光谱、原子荧光光谱等方法配套测定了碳酸盐石中１５种主、次量元素。配套方法的检出限、精精密、准确度均符合１：２０万岩石化探测量碳酸盐岩分析指标要求。方法经标样及碳酸盐岩石样品分析验证,共结果不同实验室、不同方法测定结果相符． 相似文献
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用百分总和检查硅酸盐岩石全分析数据的质量是分析工作者的传统做法,但对于微量元素含量较高的样品,采用X射线荧光光谱法(XRF)进行测定,如果不考虑微量元素的含量及其对主量元素基体效应的影响,往往会使主量元素含量更加偏离真实值。本文针对Sr、Ba含量较高的硅酸盐样品,通过人工配制标准样品,扩大了Sr、Ba校准曲线的定量范围,主量元素校准中加入Sr、Ba的基体校正系数,达到了主量元素定量更加准确可靠的实际效果。采用此方法分析国家标准物质,各主量元素的精密度(RSD)均小于2%;分析不参加回归的标准物质和人工配制的标准样品,主量元素的测量值与标准值(或参考值)基本一致。该方法可以满足硅酸盐的测定要求,主量元素各项结果的加和能够达到《地质矿产实验室测试质量管理规范》的一级标准(99.3%～100.7%)。 相似文献
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在区域地球化学调查样品多元素分析测试中,通常将XRF、ICP-OES、ICP-MS、AFS等仪器相互配套使用,但由于XRF测定20多个元素,与其他仪器测定速度并不同步,影响了项目的整体进度。本方法对配套方案进行了优化,调整了XRF部分测量元素的分析方法,即将基体校正和谱线重叠校正涉及Na_2O、MgO、V的数据由ICP-OES法测量;Cu、Pb、Zn、Mn、Th的数据由ICP-MS法测量;As、Bi的数据由AFS法测量。优化后的XRF方法测量元素减少为16个:SiO_2、Al_2O_3、Ca O、TFe_2O_3、K_2O、Ti、P、Sr、Ba、Zr、Nb、Y、Rb、Br、Ga、Cl。通过设计的XRF数据处理程序,实现了这些不同方法的测量数据共享,利用ICP-OES、ICP-MS、AFS等测量数据对XRF数据进行基体效应和谱线重叠干扰校正。本方法精密度(RSD,n=12)为0.55%~8.22%,准确度(ΔlogC)为0.000~0.031,用国家标准物质及实际样品验证的结果满足区域地球化学调查样品分析测试质量规范要求。本方案减少了XRF直接测量元素的数量,提高了多种仪器协同的分析效率。 相似文献
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熔融制样-X射线荧光光谱法测定稀土矿石中的主量元素和稀土元素 总被引：3，自引：3，他引：0
应用熔融制样-X射线荧光光谱法(XRF)分析矿石样品具有定量准确、试剂用量少、重现性好等优点,但由于目前稀土标准物质较少,不能满足复杂稀土矿石类样品的准确定量要求。本文采用配置人工标准样品,解决了现有稀土标准物质较少的问题,加入高纯稀土氧化物La2O3、Ce O2、Y2O3扩展了La、Ce、Y的线性范围,利用人工标准样品和现有稀土标准物质、碳酸盐标准物质制作工作曲线,建立了XRF测定稀土矿石、矿化样品中25种主量元素和稀土元素的分析方法。针对主量元素采用理论α系数法校准,稀土元素采用经验系数法校准,对有谱线重叠的元素进行干扰校正,使绝大多数主量元素的相对标准偏差(RSD,n=13)小于1.5%,稀土元素含量在300"g/g以上时RSD(n=13)在0.69%~6.94%之间。通过未知样品考核,主量元素、稀土元素和烧失量的加和结果为99.41%~100.63%,满足《地质矿产实验室测试质量管理规范》的一级标准。 相似文献
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电气石是一类含硼的铝硅酸盐矿物,化学成分复杂、化学稳定性强,不易湿法分解,B_2O_3含量较高,导致其主次量元素的同时测定存在一定困难。本文采用熔融法制样,建立了X射线荧光光谱法测定电气石Na_2O、MgO、Al_2O_3、SiO_2、P_2O_5、K_2O、CaO、TiO_2、V_2O_5、Cr_2O_3、MnO、TFe_2O_3等主次量元素的分析方法。样品与四硼酸锂-偏硼酸锂-氟化锂(质量比为4.5∶1∶0.4)混合熔剂的稀释比例为1∶10,消除了粒度效应和矿物效应;在缺少电气石标准物质的情况下,选择土壤、水系沉积物及多种类型的地质标准物质绘制校准曲线,利用含量与电气石类似的标准物质验证准确度,测定结果的相对标准偏差小于4.2%。采用所建方法测定四种不同类型电气石实际样品,测定值与经典化学法基本吻合。本方法解决了电气石不易湿法分解和硼的干扰问题,测定结果准确可靠,与其他方法相比操作简便,分析周期短。 相似文献
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硅酸盐岩石化学组成的ICPAES和ICPMS准确测定:酸溶与碱熔分解样品方法的对比 总被引：63，自引：8，他引：63
报道了采用酸溶和碱熔分解硅酸盐岩石样品，用ICP-AES和ICP-MS联合测定岩石的主元素和微量元素的分析方法，酸溶方法检出限低，能准确分析除SiO2以外的其他主元素和40余种微量元素；碱熔方法一次分解样品可以直接测定所有的主元素和30多种微量元素，但方法检出限增高，不能准确分析一些检出限高而含量低的元素，因此，根据不同的岩石类型，所需分析的元素种类以及研究目的，采用适当的样品分解方法，用ICP-AES和ICP-MS分析可以获得准确的主元素和微量元素数据。 相似文献
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《物探化探计算技术》2021,(1)
以X射线荧光光谱分析技术(XRF)为基准,对那阿地区的花岗岩和变质岩样品进行测试分析。以实验室所测得的主量元素结果为标准,将PXRF所测得的粉末状岩石样品数据与其对比。在处理样品中Al_2O_3、CaO、Fe_2O_3、MgO、SiO_2、TiO_2这六个主量元素的数据时,发现Spearman方法优于Pearson方法。根据不同时间变量下XRF与PXRF所测样品相关系数值(ρ)来看,90 s是4个时间点(90 s、80 s、70 s、60 s)中最优的时间点;以90 s为基准,对比变质岩与花岗岩的相关数据发现:除CaO、MgO的变质岩ρ值大于其花岗岩ρ值之外,其余主量元素的变质岩的ρ值均小于花岗岩的ρ值,在变质岩中除了SiO_2、TiO_2不具有明显的正相关与负相关性外,其余主量元素均可以进行半定量甚至是定量测量。在花岗岩中除SiO_2具有弱正相关性外,其余主量元素的正相关性均显著,因此在样品为粉末态的前提下PXRF的野外现场测试具有可行性。 相似文献
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本文针对岩石特性,按岩性分类,按含量高低分段求取工作曲线常数,并因元素而异选用不同的基体校正模式,确立一种岩石地球化学样品多元素的快速、简便的分析方法.基本能适应包括超基性、基性到中酸性岩岩石样中主、次、痕量元素分析,为岩石化探分析提供了切实可行的配套方案. 相似文献
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采用氢化物发生技术测定地质样品中的硒时,需要考虑样品的溶解、Se价态的预还原以及抑制共存离子的干扰。本文采用硝酸-盐酸-氢氟酸-高氯酸体系快速溶解样品,直接加入浓盐酸煮沸将六价硒还原为四价硒,将氢化物发生器与电感耦合等离子体发射光谱仪联用测定了铀矿地质样品中的痕量硒。样品中除了Cu2+其他离子的含量均不干扰硒的测定,通过在试液中加入铁盐溶液或在硼氢化钠还原剂中加入铁氰化钾抑制了Cu2+的干扰。方法检出限为0.12μg/L,精密度(RSD)小于5%。与前人报道的方法相比,本方法检出限较低,操作简单快速,冲洗30 s可消除记忆效应,适合批量铀矿地质样品中痕量硒的测定。 相似文献
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Jing Wang Ben-Xun Su Bing-Yu Gao Wen-Jun Li Meng-Meng Cui Xia Liu Yang Luo Qi-Qi Pan Li-Hui Jia Li Su Kai-Yun Chen 《Geostandards and Geoanalytical Research》2023,47(3):683-695
Four natural chromite samples (LBS13-04, LBS13-06 and LBS13-13) from the Luobusa ophiolite (China) and 16SW2-6 from the Stillwater Complex (USA) were developed as reference materials for in situ element microanalysis. Approximately 8 g of chromite fragments with grain sizes of 0.5–1.5 mm from each chromite sample were separated under a binocular microscope and analysed by EPMA, XRF, LA-ICP-MS and solution nebulisation ICP-MS techniques for major and trace elements at six laboratories. The results show that the four chromite samples are homogeneous with respect to MgO, Al2O3, Cr2O3, FeO, Sc, Ti, V, Mn, Co, Ni, Zn and Ga. These samples are thus suitable to be used as reference materials for in situ microanalysis. 相似文献
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Major element compositions of 36 bulk samples and 41 clay samples, which were obtained from 47 topsoils collected in monsoonal eastern China, were investigated with conventional wet chemistry and X-ray fluorescence (XRF) spectrometry, respectively. Based on major element analyses, the mobility of major elements and latitudinal distributions of SiO2/Al2O3 ratio, chemical index of alteration (CIA), chemical index of weathering (CIW) and weathering index of Parker (WIP) were analyzed. Meanwhile, the suitability of these chemical weathering indices to topsoils in monsoonal eastern China and its controls were discussed.These investigations indicate that Na, K, Ca, Mg, and Si are relatively depleted, while Mn, P, Fe and Ti are relatively enriched in topsoils of the study area by comparison with their contents in the upper continent crust (UCC), and that alkali metal (Na, K) and alkaline earth metal (Ca, Mg) elements are generally easier to be depleted from their parent materials than other major elements during chemical weathering. The latitudinal distributions of CIA, CIW and WIP show that they are suitable to both bulk and clay samples, but SiO2/Al2O3 is only suitable to clay samples, not suitable in bulk ones. All these investigations indicate a significant dependence of grain-size in major element abundance and latitudinal distributions of SiO2/Al2O3, CIA, CIW and WIP, but parent rock type has little effect on them, except its impact on the latitudinal distribution of WIP in clay samples. The significant grain-size dependence probably indicates the presence of unaltered minerals in bulk samples, thus we suggest that clay samples are more suitable to investigating chemical weathering of sediments on continents than bulk samples. The trivial effect of parent rock type probably indicates a relatively uniform chemical weathering on various parent rocks. Correlation analyses indicate that climate is the dominant control of chemical weathering of topsoils in the study area, and the significant latitude effect indicated by the spatial distributions of chemical weathering indices actually reflect the climate control on chemical weathering of topsoils.Chemical weathering indices actually reflect the integrated weathering history in the study area. Besides the dominant control of climate, other factors like tectonics, parent rock, biology, landform and soil depth and age might also have some effect on the chemical weathering of topsoils in the study area, which needs further research. 相似文献
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本文应用电子微探针(EPMA)、扫描电镜(SEM)在阿尔金地区的榴闪岩中发现了一种微米级含铀氧化物矿物,结合光学显微镜、拉曼光谱和电子背散射衍射(EBSD)技术对该矿物的化学成分、赋存状态、物理及光学性质、晶体结构等矿物学特征进行了研究。结果表明,该矿物在空间上与钛铁矿关系密切且主要产于其边部,为一种不透明矿物;主要化学组成为TiO2、ZrO2和UO2,实验化学式为(Zr,U)Ti2O6,其中U与Zr互为类质同象替代;具独特的拉曼光谱特征,初步确定为斜方晶系且具有序的铌钙矿结构。通过电子微探针U-Th-Pb定年获得等时线年龄为451±49Ma,可能代表了寄主岩石的退变质年龄。将该矿物与化学成分类似的晶体进行对比,发现与斯里兰卡石等已知天然矿物存在差异,而与一种人工合成晶体Zr5Ti7O24在化学成分和晶体结构上较为相似,可以初步推断Ti-Zr-U氧化物为一种未被人们发现的新矿物。 相似文献
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Jaya K. Gurung Hiroaki Ishiga Mohan S. Khadka Nav R. Shrestha 《Environmental Geology》2007,52(3):503-517
The geochemical analyses of fluvial-lacustrine aquifer sediments of the Kathmandu Valley have been made as a step in assessing
the environment for the mobilization of arsenic in groundwater. Elements measured by X-ray fluorescence (XRF) include 4 major
oxides (Fe2O3, TiO2, CaO, P2O5) and 14 trace elements (As, Pb, Zn, Cu, Ni, Cr, V, Sr, Y, Nb, Zr, Th, Sc and TS). Elution tests of 15 selected core samples
were also carried out to determine the potential leaching of arsenic from the sediments. The XRF results show that average
bulk concentrations of the major oxides and trace elements are similar to modern unconsolidated sediments and average upper
continental crust. However, the abundance of elements varies with grain size, with higher concentrations in finer-size grades.
Variations in elemental abundances within the basin are strongly controlled by sediment facies. The elution tests show that
greater amounts of arsenic are generally eluted from the fine sediments, although the rates are variable. The results overall
suggest that As concentrations in the bulk sediments are not a controlling factor for elevated As in the Kathmandu Basin groundwater,
and the roles of other factors such as redox conditions and organic matter contents are likely to be more significant. 相似文献
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Lüyun Zhu Yongsheng Liu Zhaochu Hu Qinghai Hu Xirong Tong Keqing Zong Haihong Chen Shan Gao 《Geostandards and Geoanalytical Research》2013,37(2):207-229
Fused glass prepared without the addition of a flux is generally more homogeneous than a pressed powder pellet and thus ideal for analysis of bulk samples by LA‐ICP‐MS. In this work, a new glass‐making method using a boron nitride crucible was developed to prepare homogenous glass samples from silicate rock powder. The apparatus consisted of a small boron nitride vessel with net volume of about 34 mm3 and two molybdenum strips. Applying the summed metal oxide normalisation technique, both major and trace element contents in the fused glass were measured by LA‐ICP‐MS. Analyses of five geochemical reference materials (spanning the compositional range basalt–andesite–rhyolite) indicated that the measured SiO2, Al2O3 and P2O5 contents matched the preferred values to within 5%, and the other major elements generally matched the preferred values to within 8%. Except for the transition metals, the measured trace element contents generally matched the preferred values to within 10%. Compared with the iridium heater method developed by Stoll et al. (2008), element volatilisation during high‐temperature melting was effectively suppressed in our method, but metal segregation caused by reduction of BN may cause loss of Cr, Ni and Cu. Although analysis with a large spot size has the advantage of improving counting statistics, matrix effects induced by mass loading of the ICP may hamper the accurate determination of some elements. 相似文献
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铜矿石类型繁多,矿石赋存状态各异,成分复杂。在现有的铜矿石熔融制样X射线荧光光谱（XRF）分析方法中,选取标准物质个数和矿石类型少、分析范围宽,与实际样品类型相差太大,且制备的熔融片质量不高。本文选用铜含量既有良好浓度变化范围,又符合铜矿石常见含量的包括铜金银铅锌钼铜镍等各类矿石的24个标准物质,以四硼酸锂-偏硼酸锂-氟化锂为混合熔剂,熔剂与样品质量比为30：1,以溴化锂为脱模剂,改进样品预处理方式,将通常采用样品预氧化后或熔融中加入脱模剂的方式,改进为加入脱模剂后再用混合熔剂完全覆盖的方法制备了高质量的熔融片,建立了XRF测定铜矿石中铜锌铅硅铝铁钛锰钙钾镁钼铋锑钴镍16种元素的分析方法。分析铜矿石国家标准物质GBW 07164、GBW 07169,各元素的精密度（RSD）为0.1%~5.4%。分析国家标准物质GBW 07163（多金属矿石）、GBW 07170（铜矿石）的测定值与标准值相符;分析实际铜矿石样品,铜锌铅钼铋锑钴镍的测试结果与电感耦合等离子体发射光谱法和其他方法的测定值相符。本文方法扩大了基体的适应性,提高了实际应用价值。 相似文献
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Principal components analysis is used to study the chemical compositions of pyroxenes of five Apollo 12 specimens. Important correlations recognized in the variation of oxide weight per cent are: MGO, Al2O3, SiO2| CaO, TiO2, FeO MgO, Al2O3, SiO2| FeO MgO, SiO2, FeO | Al2O3, CaO, TiO2 where the oxides on one side of the bar are correlated positively with each other and negatively with the oxides on the other side. Several other similarly distinct relationships with significantly less variance could be noted. These correlations indicating substitutional relationships can be interpreted as representative of stable and metastable trends of crystallization by using crystal-chemical and thermodynamic information. The per cent variance of pyroxene groups with characteristic trends in each specimen can be evaluated and interpreted in terms of history of crystallization. Distribution of Fe and Mg in certain pairs of olivine and pyroxene, which are found in contact in the rock and which may have crystallized simultaneously, is useful in recognizing the tendency towards chemical equilibrium in FeMg distribution during a limited interval in the liquidus or subsolidus stages. 相似文献