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《华北地质》2019,(4)
以铜、铅、锌为主,富含多种有色金属的矿床,其所含矿物种类较多,通过矿石主量成分的分析,可对矿床评价与利用起到重要作用。多金属矿石的主量元素检测多采用传统化学方法进行各项指标的测定,需使用多种方法,实验过程复杂,且人为误差影响较大。本文建立了一种敞口酸溶-电感耦合等离子体发射光谱法测定多金属矿中的铝锰钾钠钙镁硫的方法。以氢氟酸-硝酸-高氯酸敞口酸溶样品,使用电感耦合等离子体发射光谱仪进行同时测定,标准曲线线性良好,相关系数均大于0.999 0%,方法检出限为0.000 3%~0.004 1%,测定结果相对标准偏差(RSD)为0.82%~7.93%,方法准确、可靠,满足地质样品的分析需求,且测试过程简单,相较传统分析方法更加省时高效。 相似文献
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约翰斯顿岛附近海山富钴锰结壳的元素组成及地球化学特征 总被引:5,自引:1,他引:4
采用波长色散X射线荧光光谱(WDXRF)、电感耦合等离子体光谱(ICPAES)、电感耦合等离子体质谱(ICPMS)、原子荧光光谱(AF)和化学等多种现代化分析技术,研究测定了我国“海洋四号”船1987年采自约翰斯顿岛附近海山上的富钴锰结壳样品化学组成;获得了主、次和痕量(包括全部稀土元素REE)共52个组分的含量,并以地壳元素丰度的新数据计算了各元素的富集因数ef(enrichmentfactor)。与大洋多金属结核相比,该结壳样的主要地球化学特征是:Co和Pt的质量分数较高(分别达1.2%和0.37×1 相似文献
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《矿产与地质》2020,(2)
研究建立了稀氨水-微波消解-电感耦合等离子体质谱法(ICP-MS)测定生态地球化学生物样品中碘的方法。通过采用稀氨水代替硝酸对样品进行消解,较好地解决了测定结果不稳定及记忆效应严重现象;同时,采用离线内标加入法,有效地消除了检测过程中因操作因素等引起的误差和基体效应干扰。进行条件优化实验后,该方法的检出限为0.005μg/g,测定范围0.05~12.5μg/g。使用国家一级生物成分分析标准物质验证,相对误差(RE)为0.53%~7.17%,相对标准偏差(RSD)(n=8)为0.87%~5.81%。实际样品测定加标回收率在94.0%~96.7%之间。建立的方法能有效满足生态地球化学生物样品中碘的测试需求。 相似文献
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本文以敞开式四酸溶样,电感耦合等离子体质谱测定了新疆、青海区调样品中的Co、Mo、W、Pb等元素,并把ICP-MS、ICP-AES和XRF三个大型仪器对新疆卡克-色帕巴衣地区样品的测定结果进行了比较,确定了区调样品元素分析方法的配套方案,并对溶样过程进行了一系列的优化,其方法检出限和精密度均符合DZ0130.4-2006及补充说明中1﹕5万化探样品标准要求。经国家标准物质验证,结果与标准值相符。优化的分析方法快速灵敏度高,能用于地球化学填图计划中分析测试任务, 同时也用于日常大规模多元素分析。 相似文献
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Nick Belshaw 《岩矿测试》2007,26(1):55-60
无机地球化学研究的进展通常依赖于新的技术开发。电感耦合等离子体质谱(ICP—MS)技术可以进行高精度的同位素比值分析,使以前很难测定的元素的分析成为可能。牛津大学地球科学系已经越来越多地开展多接收器电感耦合等离子体质谱分析,着重于解决从宇宙至环境化学领域的诸多问题。目前主要研究Cr同位素,确定Cr对Jurassic—Triassic边界可能产生的影响事件,以及采用铀系列同位素进行海洋学研究。 相似文献
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在农业生态环境地球化学调查与评价中,植物的化学组成是重要的直接指标,因此对植物样品元素含量进行准确测定具有重要意义.本研究的主要目的是开发一种利用电感耦合等离子体发射光谱(ICP-OES)测定植物样品中多元素的分析方法,同时不需要在光谱测定之前进行费力而繁琐的样品前处理.采用微波消解、电热板消解及超声消解3种方法处理植物样品,利用ICP-OES分别测定植物样品中Ca、Cr、Cu、Fe、Mg、Mn、Ni、Pb、Sr、Zn等10种元素的含量,并对3种方法的消解效果进行比较.结果表明:3种方法的检出限分别为0.042×10-6~0.239×10-6、0.046×10-6~0.237×10-6、0.026×10-6~0.232×10-6;测定待测元素的相对标准偏差均低于10%;相对误差分别为-11%~+13.8%,-22.1%~+8.7%,-13.3%~+8.9%.其中超声消解表现出更低的检出限和较好的准确度,满足DD2005-03《生态地球化学评价样品分析技术要... 相似文献
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ICP发射光谱法测定硅酸盐岩石中主要元素 总被引:1,自引:0,他引:1
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岩石及类似样品的十种主要元素的方法及结果。方法的精密度和准确度均能满足地球化学工作的要求。 实验部分 光谱仪及工作条件 相似文献
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《矿物岩石地球化学通报》2018,(5)
微区原位同位素分析是近年来同位素地球化学研究的前沿领域。其中,激光剥蚀系统与多接收电感耦合等离子体质谱联用技术(LA-MC-ICP-MS)被广泛应用于不同同位素体系和不同天然矿物的微区原位同位素测定。铅同位素作为有效的地球化学示踪手段被广泛用于岩石成因和演化、成矿时代、成矿物质来源、环境污染物源示踪和考古学等研究。目前多利用LA-MC-ICP-MS测定硅酸盐矿物、硫化物矿物和包裹体Pb同位素组成。该方法省略了冗长的化学处理流程,提高了工作效率,并且通过对不同矿物或同一矿物中不同结构部位进行微区原位Pb同位素分析,可揭示微米尺度上的Pb同位素组成变化,为解决地质问题提供了重要的证据。本文评述了近年来地质样品中LA-MC-ICP-MS测定Pb同位素的方法改进及其在部分地球科学研究中的应用。 相似文献
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20世纪80年代至今,中国已研制了9种茶叶成分标准物质。中国地质调查局于2004年下达中国地质科学院地球物理地球化学勘查研究所研制的一套适用于覆盖区农业生态地球化学评价的生物地球化学系列标准物质,其中包括两种茶叶标准物质,定值组分60余项,包括植物营养元素、有毒、有害元素和重金属污染元素以及人们关心的一些微量营养元素等,满足了相关食品卫生安全及生物样品成分检验分析的需要,取得了显著的社会效益。随着农业生态地质调查工作全面部署和展开,对生物样品的分析测试任务加大,对相应地球化学标准物质的需求也随之增加。本文复制了GBW10016a和GBW10052a两种茶叶标准物质,候选物分别为福建武夷山乌龙茶和江西上饶市婺源绿茶。研制过程严格按照JJG 1006—1994、JJF 1343—2012和JJF1646—2017等相关规范要求,侯选物经粗碎、干燥、细碎、过筛、混匀等步骤制备而成,经统计学检验,样品均匀,稳定性良好,定值采用多家实验室合作定值的方式进行,优选国内技术实力较强、仪器设备先进、且有相关标准物质定值测试经验的11家实验室,采用电感耦合等离子体质谱/发射光谱法(ICP-MS/OES)... 相似文献
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电感耦合等离子体质谱联用技术在元素形态分析中的应用进展 总被引:1,自引:0,他引:1
电感耦合等离子体质谱(ICP-MS)作为一种高灵敏度的分析技术在痕量超痕量无机元素分析方面已被广泛应用,其与色谱分离技术相结合为元素形态分析提供了强有力的检测工具。本文阐述了近年来利用不同ICP-MS联用技术进行元素形态分析的研究进展,主要包括:(1)气相色谱-电感耦合等离子体质谱联用技术(GC-ICP-MS);(2)毛细管电泳-电感耦合等离子体质谱联用技术(CE-ICP-MS);(3)离子色谱-电感耦合等离子体质谱联用技术(IC-ICP-MS);(4)高效液相色谱-电感耦合等离子体质谱联用技术(HPLC-ICP-MS)。在此基础上归纳总结了中国元素形态分析领域的主要研究情况,对元素形态分析发展前景作了展望。这些联用技术中,GC-ICP-MS的灵敏度高,样品传输率接近100%,但其适用于易挥发或中等挥发性样品的分离,应用范围相对较窄;CE-ICP-MS的分离效率高,样品和试剂消耗量少,但受到其进样量限制使得最低检出浓度较大;IC-ICP-MS主要分析阴离子和阳离子及小分子极性化合物,是液相色谱的有益补充,具有分离效果好和快速方便等优点,但离子色谱流动相中的盐类会造成ICP-MS进样管和采样锥的堵塞,使得基体效应严重;HPLC-ICP-MS以其广泛的应用范围、简单的接口技术,成为元素形态分析研究中应用最广泛的联用技术。本文认为,元素形态分析研究中开展复杂基体样品前处理方法研究,研制系列元素形态分析标准物质,建立多元素形态同时分析方法是元素形态分析领域的发展方向。 相似文献
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Jon D. Woodhead 《Geostandards and Geoanalytical Research》2005,29(1):26-36
This annual review documents developments and applications in the field of isotope ratio determination, as reflected in the literature for the Earth and environmental sciences for the year 2003. Particular emphasis is placed upon the relationship between the two dominant analytical techniques-thermal ionisation mass spectrometry (TIMS) and multi-collector inductively coupled plasma-mass spectrometry (MC-ICP-MS)-and the rapidly changing nature of their roles in isotope analysis. Additionally, the review covers developments in single-collector ICP-MS and TOF technologies, new sample preparation procedures and the characterisation of isotopic reference materials, together with fundamental investigations of mass spectrometer performance. 相似文献
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Jean S. KANE 《Geostandards and Geoanalytical Research》1985,9(2):181-190
A simultaneous multi-element method is described for the determination of six elements of importance in geochemical investigations of mineralization processes in granites. After a mixed acid sample digestion, the elements Be, Li, Nb, W, Mo and Sn are determined by inductively coupled plasma spectrometry. Possible sources of bias due to incomplete sample dissolution and from spectral interferences were investigated. Analysis of 16 geological reference standard samples and a number of enriched samples demonstrates the accuracy and precision of the method for the study of mineralized granites and for several other geochemical sample types as well. 相似文献
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A field filtration method for the concentration and separation of suspended particulate matter (SPM) from freshwater systems and the subsequent determination of minor, trace and ultra trace elements (As, Ba, Be, Cd, Co, Cr, Cs, Cu, Ga, Hf, Mo, Nb, Ni, Pb, Rb, Sb, Sc, Sn, Sr, Ta, Th, Tl, U, V, W, Zn and Zr) is validated with respect to detection limits, 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) and inductively coupled plasma quadrupole mass spectrometry (ICP-QMS). Total concentrations of these 27 trace and minor elements have been determined in suspended particulate matter (SPM) 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 8% and 18% RSD for most elements on a dry weight basis. Higher recovery after acid digestion is found for some elements, probably because of volatilization or retention losses in the fusion procedure. Other elements show higher recovery after fusion, which is explained by more efficient decomposition of refractory mineral phases relative to the non-total acid digestion. 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 method limits of detection range between 0.7 ng and 2.65 μg, as estimated from the blank filter samples. These detection limits are 10–550 times higher compared to the corresponding instrumental limits of detection. The accuracy and bias of the overall analytical procedure was assessed from replicate analysis of certified reference materials. A critical evaluation of the instrumental capabilities of the ICP-QMS instrumentation in comparison with a double focusing sector field plasma mass spectrometry technique (ICP-SFMS) is also included. It was found that a modified microwave acid digestion procedure in combination with ICP-SFMS could replace ICP-AES determinations and fusion digestions for most of the investigated elements. Guidelines and limitations for this time- and labour- efficient procedure, offering accurate results for the majority of elements studied are discussed. 相似文献
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Reference Minerals for the Microanalysis of Light Elements 总被引:2,自引:0,他引:2
M. Darby Dyar Michael Wiedenbeck David Robertson Laura R. Cross Jeremy S. Delaney Kurt Ferguson Carl A. Francis Edward S. Grew Charles V. Guidotti Richard L. Hervig John M. Hughes John Husler William Leeman Anne V. McGuire Dieter Rhede Heike Rothe Rick L. Paul Ian Richards Martin Yates 《Geostandards and Geoanalytical Research》2001,25(2-3):441-463
The quantitative determination of light element concentrations in geological specimens represents a major analytical challenge as the electron probe is generally not suited to this task. With the development of new in situ analytical techniques, and in particular the increasing use of secondary ion mass spectrometry, the routine determination of Li, Be and B contents has become a realistic goal. However, a major obstacle to the development of this research field is the critical dependence of SIMS on the availability of well characterized, homogeneous reference materials that are closely matched in matrix (composition and structure) to the sample being studied. Here we report the first results from a suite of large, gem crystals which cover a broad spectrum of minerals in which light elements are major constituents. We have characterized these materials using both in situ and wet chemical techniques. The samples described here are intended for distribution to geochemical laboratories active in the study of light elements. Further work is needed before reference values for these materials can be finalized, but the availability of this suite of materials represents a major step toward the routine analysis of the light element contents of geological specimens. 相似文献
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A. M. Sulej-Suchomska Ż. Polkowska A. Przyjazny Z. J. Kokot J. Namieśnik 《International Journal of Environmental Science and Technology》2016,13(6):1475-1488
Determination of xenobiotics in samples of airport runoff water is both a complex and indispensable task due to an increasing threat resulting from the activities of numerous airports. The aim of this study was to develop, optimize, and validate a procedure based on liquid–liquid extraction (LLE) coupled with gas chromatography–mass spectrometry (GC–MS) for the determination of polycyclic aromatic hydrocarbons (PAHs). So far, no procedure was available that would ensure reliable data about concentration levels of these toxic pollutants in a new type of environmental samples, such as airport stormwater. The most difficult step in the analytical procedure used for the determination of fuel combustion products in airport stormwater samples is sample preparation. In this work, eight different protocols of sample preparation were tested. The evaluation of the LLE demonstrated that the best extraction conditions were as follows: dichloromethane (extraction solvent), solvent volume of 15 mL and sample volume of 250 mL. The percent recovery values ranged from 66 to 106 %, which shows that the LLE technique is a powerful method for extracting PAHs from airport runoff water samples with a complex matrix composition. Moreover, the developed procedure was characterized by satisfactory selectivity and a relatively low LOQ (0.17–0.52 μg/L). The procedure has been successfully applied to the analysis of stormwater samples collected from different sites at international airport in Poland. The procedure can thus be used as a tool for tracking the environmental fate of these compounds and for assessing the environmental effect of airports. 相似文献