Concentrations of Trace Elements in Carbonate Reference Materials Coral JCp-1 and Giant Clam JCt-1 by Inductively Coupled Plasma-Mass Spectrometry

Trace elements in the Geological Survey of Japan carbonate reference materials Coral JCp-1 and Giant Clam JCt-1 were determined by inductively coupled plasma-mass spectrometry after digestion with 2% v/v HNO₃. A standard addition method was adopted in this determination in order to neutralise the Ca matrix effect. In addition, Sc, Y, In and Bi were used as internal standards to control the matrix effect and correct instrumental drift. Of the eighteen elements measured in JCp-1, precisions for fourteen elements, including Cu, Cd and Ba, were better than 10% RSD and concentrations ranged from 0.002 μg g^-1 (Cs) to 8.02 μg g^-1 (Ba). The concentrations of measured trace elements in JCt-1, except for Cu, were lower than those in JCp-1. Precisions for all elements with concentrations higher than 0.04 μg g^-1 in JCt-1 were also better than 10% RSD and concentrations were found to be between 0.001 μg g^-1 (Cs) and 4.84 μg g^-1 (Ba). The concentrations of more than fifteen trace elements in the aragonite reference materials are reported here for the first time. Both reference materials are suitable for use in geochemical studies of environmental reconstruction based upon biogenic carbonate materials.     

The Preparation and Characterisation of Two New Geological Survey of Japan Geochemical Reference Materials: Copper ore JCu-1 and Zinc ore JZn-1

Two new geochemical reference materials, copper ore JCu-1 and zinc ore JZn-1 have been prepared by the Geological Survey of Japan (GSJ) for the determination of major and minor elements and isotopic compositions. JCu-1 is a sample of Cu-bearing sulfide ore typical of the Kamaishi mine in Iwate Prefecture, Japan, and is composed mainly of hedenbergite, chalcopyrite, quartz and calcite. Pyrrhotite, magnetite and actinolitic amphibole were also commonly found. The Zn-rich ore, JZn-1 is a crude ore from the Kamioka Pb-Zn mine in Gifu Prefecture, Japan. The sample consists of hedenbergite, quartz, calcite, sphalerite and epidote as main crystalline phase. Homogeneity test results showed that all studied constituents including ore elements such as Cu, Pb and Zn can be considered to be homogeneously distributed. Provisional collaborative analyses were carried out in ten laboratories, and the data were evaluated using a robust statistical method using z-scores. Recommended values for a number of major elements including TiO₂, Al₂O₃, MnO, MgO, CaO, Na₂O, K₂O, Fe (total), Zn, Cu and Pb were established. In addition, information values for eighteen major, minor and trace elements are presented to support future collaborative analyses.     

Uranium and Thorium Content of Reference Samples from the Geological Survey of Japan "Igneous Rock Series 1986"

Improved determinations of uranium and thorium by fission track and moderating neutron techniques are presented for the rock reference samples of the Geological Survey of Japan (GSJ) "Igneous rock series 1986". The non-homogenous distribution of uranium and thorium has been detected in the samples JF-1, JG-2 and JG-1a caused by the presence of highly radioactive accessory minerals.     

海泡石化学成分分析标准物质研制

海泡石是一种十分重要的非金属矿，被广泛应用于航空、畜牧、化工环保等领域中，贸易活动十分活跃。鉴于中国一直没有海泡石标准物质，国际上的海泡石标准物质定值组分少，为了满足相关研究需求，本文研制了湖南湘潭的海泡石标准物质（GBW07138）。对Ba、Be、Bi、Cd、Ce、Co、Cr、Cs、La、Li、Lu、U、Nb、Nd、Ni、Pb、SiO₂、Al₂O₃、Fe₂O₃、MgO、CaO、Na₂O、K₂O、TiO₂共24种组分进行均匀性和稳定性检验。针对不同含量、不同性质的组分，采用合理的国家标准方法检验了20种组分的RSD小于3%，其余4种组分Bi、La、Lu、Mo的RSD略大于3%，方差检验的F值均小于列表临界值[F_0.05（29，60）=1.65]，表明该标准物质均匀性良好。在稳定性考察期内，24种组分的含量无统计学上的明显变化，表明该标准物质稳定性良好。由9家实验室采用重量法、容量法、X射线荧光光谱法、电感耦合等离子体质谱法等传统化学分析方法和现代仪器分析方法协作定值，最终定值组分63种，涵盖了主量、微量及全部稀土元素，其中海泡石特征组分MgO和烧失量（LOI）的含量分别为18%±0.2%和8.55%±0.19%，这两种组分与现有的标准物质形成一定阶梯性，能够更好地满足海泡石成分分析测试需求。该海泡石标准物质可用于地质找矿、地球化学调查、地质矿产产品测试以及其他行业相关领域样品测试的质量监控标准。而且在研制该标准物质过程中，改良或开发的一些新方法可为后续开发海泡石标准物质提供技术支持。     

New Reference Material of Dunite Rock, NGRI-UMR: Preparation and Evaluation

A dunite reference material has been prepared as part of the reference materials programme at the National Geophysical Research Institute, Hyderabad, India. The scarcity of reference materials for undertaking the chemical analysis of ultramafic rocks for major and trace elements justified the preparation of such a rock reference material. A 300 kg sample of starting material was collected from an active quarry near the town of Salem in Tamil Nadu, southern India. The sample was homogenized and an invitation for round robin participation was published in Geostandards Newsletter (October 1995). A total of twenty seven international laboratories participated in the study, providing information on the total element concentration of major, minor, trace and rare earth elements. Following data compilation, outlier rejection, and statistical analysis, proposed and indicative total element concentrations are reported for twenty four elements.     

The Preparation and Characteristics of the Geochemical Certified Reference Material BEM (Emeishan Basalt)

A basaltic certified reference material BEM, prepared by Chengdu University of Technology, has recently been approved as a Primary Grade Reference Material (GBW07126) by the General Administration of Quality Supervision, Inspection and Quarantine of China. BEM was sampled from the Emeishan Basalts in China, which is one of the largest basalt provinces in the world. After successfully completing homogeneity and stability tests, collaborative analyses were carried out in seventeen Chinese institutes and laboratories and two American laboratories. More than ten reliable analytical methods based on different principles of measurement were adopted, of which ICP-MS, NAA and ICP-AES contributed 60.5% of all results. Fifty-four elements and oxide components were characterised as certified values, four elements as recommended values and nine elements as information values. A minimum sampling mass of 40 mg for most elements is recommended for use.     

Reference Materials for Geochemical Studies: New Analytical Data by ICP-MS and Critical Discussion of Reference Values

Abundances of twenty four trace elements, including Y and fourteen rare earth elements (REE), are reported for eighty six geological reference materials and four proficiency testing samples. Analytical data were obtained by ICP-MS using solution nebulisation after mixed acid digestion (HF-HClO₄) under pressure. Analysed samples cover a wide range of element concentrations and mineralogical compositions, including samples for which there are few previously published data. Precision for elemental determinations in nearly 90% of the samples analysed is better than 5%. Accuracy, estimated by comparison with data from compilations is better than 6% for well characterized reference materials. Results obtained for samples that are low in trace elements are often significantly lower than compiled reference values. A critical discussion of the compiled data sets, especially for Y and the REEs, indicates that some reference values seem to be erroneous.     

New Series of Rock and Sediment Geochemical Reference Materials

Certified or reference values for sixty six to sixty seven elements and element oxides are given for geochemical reference materials recently prepared by the Institute of Geophysical and Geochemical Exploration (IGGE), including limestone (GSR-13), granitic gneiss (GSR-14), amphibolite (GSR-15), lake sediment (GSS-9) and stream sediments (GSD-1a, GSD-13, GSD-14). These samples supplement the GSR 1-6, GSD1-8 and GSD 9-12 certified reference materials already prepared and characterized by the IGGE.     

Rhenium‐Osmium Isotope Measurements of Geological Reference Material BIR‐1a: Evaluation of Homogeneity and Implications for Method Validation and Quality Control

To evaluate the homogeneity of geological reference material BIR‐1a (basalt; United States Geological Survey, USGS) for Re‐Os isotopic studies at the 0.2–1.0 g test portion size level, sixty‐three precise measurement results of Re and Os mass fractions and isotope amount ratios were obtained over an 18‐month period. These data reveal that the reference material has higher Re (0.691 ± 0.022 ng g^?1, 2s, n = 63) and lower Os mass fractions (0.343 ± 0.089 ng g^?1, 2s, n = 63) than UB‐N (serpentinite, CRPG) and is homogeneous in ¹⁸⁷Os/¹⁸⁸Os isotope amount ratio (0.13371 ± 0.00092, 2s, n = 63) at the 0.2–1.0 g test portion size level. The results are essentially consistent with previous views indicating that BIR‐1a gives precise measurement results for Re‐Os isotope amount ratio measurements at the 1 g test portion size level (Ishikawa et al., Chemical Geology, 2014, 384, 27–46; Meisel and Horan, Reviews in Mineralogy and Geochemistry, 2016, 81, 89–106). Based on these new Re‐Os data and previous studies, we propose BIR‐1a as a useful reference material that can be used in method validation and quality control and interlaboratory comparisons for studies dealing with mafic geological samples at test portion sizes of > 0.4 g.     

抗战内迁北碚的中央地质调查所与中国西部科学院

抗战时期,中央地质调查所内迁重庆北碚,中国西部科学院帮助其在纷乱的战时安定下来,开始相对稳定的科研工作,主要在西部地区开展调查、从事科研。地调所的科研血脉得以传承,成为战时国内矿产资源调查研究中心。     

土壤中总有机碳环境标准样品研制

土壤环境标准样品是土壤生态环境监测质量控制的重要技术工具.目前,土壤中总有机碳环境标准样品仍为中国环境标准样品体系的空缺,特别是配套燃烧氧化-非分散红外法的土壤标准样品一直未曾问世.本文以有机碳含量较高的农用地土壤为原材料,经干燥、研磨、混匀、装瓶、灭菌等加工步骤,制备获得土壤中总有机碳环境标准样品.分层随机抽取10瓶...     

Homogeneity of the Geochemical Reference Material BRP-1 (Paraná Basin Basalt) and Assessment of Minimum Mass

Reference materials (RM) are required for quantitative analyses and their successful use is associated with the degree of homogeneity, and the traceability and confidence limits of the values established by characterisation. During the production of a RM, the chemical characterisation can only commence after it has been demonstrated that the material has the required level of homogeneity. Here we describe the preparation of BRP-1, a proposed geochemical reference material, and the results of the tests to evaluate its degree of homogeneity between and within bottles. BRP-1 is the first of two geochemical RM being produced by Brazilian institutions in collaboration with the United States Geological Survey (USGS) and the International Association of Geoanalysts (IAG). Two test portions of twenty bottles of BRP-1 were analysed by wavelength dispersive-XRF spectrometry and major, minor and eighteen trace elements were determined. The results show that for most of the investigated elements, the units of BRP-1 were homogeneous at conditions approximately three times more rigorous than those strived for by the test of "sufficient homogeneity". Furthermore, the within bottle homogeneity of BRP-1 was evaluated using small beam (1 mm²) synchrotron radiation XRF spectrometry and, for comparison, the USGS reference materials BCR-2 and GSP-2 were also evaluated. From our data, it has been possible to assign representative minimum masses for some major constituents (1 mg) and for some trace elements (1-13 mg), except Zr in GSP-2, for which test portions of 74 mg are recommended.     

Ban-1 Zircon: A New Natural Zircon Reference Material for LA-MC-ICP-MS Zr and Hf Isotopic Determinations

New zircon reference materials for in situ zircon radiogenic Hf isotope and stable Zr isotopic determinations made by laser ablation multi-collector inductively coupled plasma-mass spectrometry (LA-MC-ICP-MS) are required due to high data productivity and consequently high reference material consumption rate. This study examines a new natural zircon for Zr isotope ratios by double spike thermal ionisation mass spectrometry (TIMS), and for Hf isotopes by bulk solution nebuliser (SN)-MC-ICP-MS with both Zr and Hf determined by LA-MC-ICP-MS. A total of five zirconium isotope measurements from drilled zircons, determined by TIMS, yield a mean δ^94/90Zr_IPGP-Zr value of -0.09 ± 0.06‰ (2s). Five and eight hafnium isotope measurements for powders from the drilled zircons and Ban-1-4 by SN-MC-ICP-MS, yield mean ¹⁷⁶Hf/¹⁷⁷Hf ratios of 0.282985 ± 0.000011 (2s) and 0.282982 ± 0.000007 (2s), respectively. The mean δ^94/90Zr_IPGP-Zr value and ¹⁷⁶Hf/¹⁷⁷Hf ratio determined by LA-MC-ICP-MS analyses are -0.06 ± 0.09‰ (2s, n = 504) and 0.282985 ± 0.000035 (2s, n = 327), respectively. The isotopic homogeneities suggest that the Ban-1 zircon is a suitable reference material for microbeam Zr and Hf isotopic measurements.     

MK‐1 Apatite: A New Potential Reference Material for (U‐Th)/He Dating

The (U‐Th)/He dating technique has been widely used for several decades to constrain the timing of low temperature geological processes. Recent research has shown that the commonly used reference material (the Durango apatite) often yields dispersed fragment dates that are beyond analytical uncertainties. Here, we report a new apatite (U‐Th)/He dating reference material, MK‐1, which was collected from the Mogok metamorphic belt in Burma. Electron probe microanalysis and backscattered electron images of two randomly selected fragments indicate that this apatite is chemically and structurally homogeneous. We performed single‐grain (U‐Th)/He dating on thirty randomly selected fragments of this material. (U‐Th)/He dating results from multiple laboratories show that fragments of the MK‐1 apatite megacryst yielded reproducible results, with a mean date of 18.0 ± 0.2 Ma. The Th/U ratio of this apatite is homogeneous. Nine randomly selected fragments registered a narrow range of effective uranium (eU) mass fractions (326–354 μg g^?1), with a mean value of 336.6 ± 10.3 μg g^?1. Twenty‐four in situ (U‐Th)/He dates yielded a mean value of 18.0 ± 0.2 Ma (MSWD = 0.41), indistinguishable from the results obtained by the conventional method. All the results suggest that this apatite has the potential to become a new reference material for (U‐Th)/He geochronology.     

Stevns Klint Fish Clay (FC-1): Preparation of, and Preliminary Results for, a Candidate Reference Material

The collapse of a section of the cliff at Stevns Klint, Denmark in 1986 provided a unique opportunity to collect about 50 kg of Fish Clay representing the Cretaceous-Tertiary (K-T) boundary layer. In this paper, details of the preparation of this sample are presented, together with preliminary analytical results to support the development of this sample as a reference material, particularly for the determination of iridium and the other platinum-group elements in clays and sediments associated with K-T boundary studies and in other environmental samples collected to study the effects of automobile exhaust catalysts.     

中国地质学的产生与发展——写在地质调查所创建100周年之际

中国的地质学非我国自有,而是在传播和引入西方近代科学文化的过程中逐渐形成的,是"西学东渐"的结果。在欧美等西方国家,至19世纪中叶,便建立并完善了近代地质学的理论和方法体系,完成了学科体制化建设,比中国至少早一个世纪。从16世纪后半叶的"西学东渐",西方近代地学传入中国进行第一次启蒙,到引进、消化、吸收和本土化,最后建立中国地质学理论和方法体系,完成学科建制,中国地质事业历经了长达三个半世纪艰辛曲折并充满坎坷的历史进程。创建于1913年的地质调查所是中国近代第一个科研机构,在章鸿钊、丁文江、翁文灏等第一代地质学家的领导下,筚路蓝缕、艰苦奋斗,在短短的二、三十年里,全面开创和奠定了中国近代地质事业,培养了一大批早期地质学家,取得了举世瞩目的成果,赢得国内外学术界的广泛赞誉。地质调查所的成功及其所取得的成就远远超出了地质学,对我国古生物学、地理学、地震学、地球物理学、土壤学、考古、古人类学、燃料和地图等诸多学科领域都产生了深远影响。     

Certificate of Analysis of the Reference Material BRP-1 (Basalt Ribeirão Preto)

Reference materials (RM) are essential to achieve traceability of measurements. Specific uses of RM in analytical laboratories are the validation of methods, the calibration of instruments, the quality control and the demonstration of proficiency. This paper describes the certification of a new geochemical reference material, named BRP-1 (Basalt Ribeirão Preto), and acts as the certificate of analysis for this RM. The rock sample was crushed and pulverised at the USGS (Denver, USA), homogenised and split into 1920 bottles, with 55 g each. BRP-1 was transported back to Brazil and the homogeneity between and within bottles was assessed to demonstrate sufficient homogeneity for certification. The chemical characterisation was performed by twenty-five laboratories. Each laboratory received two bottles of BRP-1 and one of BCR-2 (Basalt Columbia River) used for quality control (QC). Reference values and uncertainties were calculated for forty-four constituents of BRP-1, following ISO Guide 35 recommendations and the IAG Protocol. The calculation of each reference value included data of proven traceability from at least ten laboratories using two or more analytical techniques and the uncertainties combines the characterisation and between bottle homogeneity contributions.     

中国科学院地质研究所的成立与中央地质调查所的传承

1913年成立的中央地质调查所（成立时称农商部地质调查所）是中国建立的第一个国家级科研机构,代表了中国现代科学的起始,在中国现代科学发展史上具有举足轻重的地位。在它成立后的几十年间,中央地质调查所在区域地质调查、矿产资源勘查、大地构造学、地震学、土壤学、古生物与古人类学等众多领域,取得了一系列举世瞩目的学术成就,是民国时期我国最享有国际声誉的研究单位。1951年,中央地质调查所被正式改组为中国科学院地质研究所。根据当时新中国地质工作"一元化"的要求,原中央研究院地质研究所和原国民政府资源委员会矿产测勘处的部分地质研究人员也一同并入该研究所,使其成为当时我国最大的地质研究机构。1952年6月开始,刚成立不久的中国科学院地质研究所的科技人员开始分流。首先是研究所的古生物研究人员分流到新成立的中国科学院古生物研究所（即现在的中国科学院南京地质古生物研究所）,它是在原中央研究院地质研究所基础上成立的。1952年9月,研究所土壤研究室扩充建设为中国科学院土壤研究所。1952年底左右,因新中国大规模经济建设的需求,大批科技人员分流到刚成立的地质部及所属的地质勘探队。从这一脉络可以看出,中国科学院地质研究所是中央地质调查所的传承和延续,而学术界大多认为中央地质调查所已于解放初期解体或撤销的观点与史实并不相符。