Characterisation of a Natural Quartz Crystal as a Reference Material for Microanalytical Determination of Ti,Al, Li,Fe, Mn,Ga and Ge

A natural smoky quartz crystal from Shandong province, China, was characterised by laser ablation ICP‐MS, electron probe microanalysis (EPMA) and solution ICP‐MS to determine the concentration of twenty‐four trace and ultra trace elements. Our main focus was on Ti quantification because of the increased use of this element for titanium‐in‐quartz (TitaniQ) thermobarometry. Pieces of a uniform growth zone of 9 mm thickness within the quartz crystal were analysed in four different LA‐ICP‐MS laboratories, three EPMA laboratories and one solution‐ICP‐MS laboratory. The results reveal reproducible concentrations of Ti (57 ± 4 μg g^?1), Al (154 ± 15 μg g^?1), Li (30 ± 2 μg g^?1), Fe (2.2 ± 0.3 μg g^?1), Mn (0.34 ± 0.04 μg g^?1), Ge (1.7 ± 0.2 μg g^?1) and Ga (0.020 ± 0.002 μg g^?1) and detectable, but less reproducible, concentrations of Be, B, Na, Cu, Zr, Sn and Pb. Concentrations of K, Ca, Sr, Mo, Ag, Sb, Ba and Au were below the limits of detection of all three techniques. The uncertainties on the average concentration determinations by multiple techniques and laboratories for Ti, Al, Li, Fe, Mn, Ga and Ge are low; hence, this quartz can serve as a reference material or a secondary reference material for microanalytical applications involving the quantification of trace elements in quartz.     

The stress field and rupture feature in compound model containing typical cracks system and hard-inclusion

IntroductionMet(1995,1996)presentedhard-inclusionearthquakepreparationmodebasingonintraplatemacroseismicityandtempo-spatialevolutioncharacteristicsofprecursoryabnormalfieldssuchasseismicitygapandhighQvalueappearinginawideareaaroundepicenterbeforestrongearthquakes.Somedeepstructure,mechanicalanalysisandrockmechanicaltestconcernedhaveprovidedsupportingevidenceforthemode.Oneofthemostimportantachievementsofmodernseismologyisconfirmingthatearthquakes(especiallyforshallowfocusshocks)causedbyfaultext…     

Determination of Zr and Hf in a Flux-Free Fusion of Whole Rock Samples using Laser Ablation Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS) with Isotope Dilution Calibration

Isotope dilution calibration has been applied to the determination of Zr and Hf in whole rocks by laser ablation (LA)-ICP-MS. Enriched isotopes were added during the preparation of flux-free, synthetic whole rock glasses and homogenised through a combination of grinding and fusion. This method avoids problems, such as solution instability and the chemical resistance of minerals such as zircon, inherent in acid digestion sample preparation. The use of isotope dilution removes the need for external calibration using certified reference material glasses such as NIST SRM 612 for which certified Zr and Hf values are not available. The precision of Zr and Hf determinations were found to be < 1% and 3.5% respectively, limited by Poisson counting statistics which contributed to 50% of the final precision of analysis. Measured values correlate closely with compiled literature values.     

测量学教学体系改革的深层构想——面向资源环境与城乡规划管理专业的理性思考

从资源环境与城乡规划管理专业的学科定位对测量学课程进行定性,从更新教育观念的角度提出教学体系改革的指导思想,以此确定测量学课程的培养目标与课程规格并指导教学体系的设计。提出了测量学教学体系的系统结构模式,并按教学理论与教学实践两大部分,经典测量学、测绘新技术与测量学应用三个模块构建了教学体系的基本内容。     

Nickel Isotope Variations in Terrestrial Silicate Rocks and Geological Reference Materials Measured by MC‐ICP‐MS

Although initial studies have demonstrated the applicability of Ni isotopes for cosmochemistry and as a potential biosignature, the Ni isotope composition of terrestrial igneous and sedimentary rocks, and ore deposits remains poorly known. Our contribution is fourfold: (a) to detail an analytical procedure for Ni isotope determination, (b) to determine the Ni isotope composition of various geological reference materials, (c) to assess the isotope composition of the Bulk Silicate Earth relative to the Ni isotope reference material NIST SRM 986 and (d) to report the range of mass‐dependent Ni isotope fractionations in magmatic rocks and ore deposits. After purification through a two‐stage chromatography procedure, Ni isotope ratios were measured by MC‐ICP‐MS and were corrected for instrumental mass bias using a double‐spike correction method. Measurement precision (two standard error of the mean) was between 0.02 and 0.04‰, and intermediate measurement precision for NIST SRM 986 was 0.05‰ (2s). Igneous‐ and mantle‐derived rocks displayed a restricted range of δ^60/58Ni values between ?0.13 and +0.16‰, suggesting an average BSE composition of +0.05‰. Manganese nodules (Nod A1; P1), shale (SDO‐1), coal (CLB‐1) and a metal‐contaminated soil (NIST SRM 2711) showed positive values ranging between +0.14 and +1.06‰, whereas komatiite‐hosted Ni‐rich sulfides varied from ?0.10 to ?1.03‰.     

Abundances of Sulfur,Selenium, Tellurium,Rhenium and Platinum‐Group Elements in Eighteen Reference Materials by Isotope Dilution Sector‐Field ICP‐MS and Negative TIMS

Geological reference materials (RMs) with variable compositions and NIST SRM 612 were analysed by isotope dilution mass spectrometry for bulk rock concentrations of chalcogen elements (sulfur, selenium and tellurium), rhenium and platinum‐group elements (PGEs: Ru, Pd, Os, Ir and Pt), including the isotope amount ratios of ¹⁸⁷Os/¹⁸⁸Os. All concentrations were obtained from the same aliquot after HCl‐HNO₃ digestion in a high pressure asher at 320 °C. Concentrations were determined after chemical separation by negative TIMS, ICP‐MS and hydride generation ICP‐MS (Se, Te). As in previous studies, concentrations of the PGEs in most RMs were found to be highly variable, which may be ascribed to sample heterogeneity at the < 1 g level. In contrast, S, Se and Te displayed good precision (RSD < 5%) in most RMs, suggesting that part of the PGE budget is controlled by different phases, compared with the chalcogen budget. The method may minimise losses of volatile chalcogens during the closed‐system digestion and indicates the different extent of heterogeneity of chalcogens, Re and PGEs in the same sample aliquot. OKUM, SCo‐1, MRG‐1, DR‐N and MAG‐1 are useful RMs for the chalcogens. NIST SRM 612 displays homogenous distribution of S, Se, Te, Pt and Pd in 30 mg aliquots, in contrast with micro‐scale heterogeneity of Se, Pd and Pt.     

Barium Isotopic Compositions of Geological Reference Materials

The interest in variations of barium (Ba) stable isotope amount ratios in low and high temperature environments has increased over the past several years. Characterisation of Ba isotope ratios of widely available reference materials is now required to validate analytical procedures and to allow comparison of data obtained by different laboratories. We present new Ba isotope amount ratio data for twelve geological reference materials with silicate (AGV‐1, G‐2, BHVO‐1, QLO‐1, BIR‐1, JG‐1a, JB‐1a, JR‐1 and JA‐1), carbonate (IAEA‐CO‐9) and sulfate matrices (IAEA‐SO‐5 and IAEA‐SO‐6) relative to NIST SRM 3104a. In addition, two artificially fractionated in‐house reference materials BaBe12 and BaBe27 (δ^137/134Ba = ?1.161 ± 0.049‰ and ?0.616 ± 0.050‰, respectively) are used as quality control solutions for the negative δ‐range. Accuracy of our data was assessed by interlaboratory comparison between the University of Bern and the United States Geological Survey (USGS). Data were measured by MC‐ICP‐MS (Bern) and TIMS (USGS) using two different double spikes for mass bias correction (¹³⁰Ba–¹³⁵Ba and ¹³²Ba–¹³⁶Ba, respectively). MC‐ICP‐MS measurements were further tested for isobaric and non‐spectral matrix effects by a number of common matrix elements. The results are in excellent agreement and suggest data accuracy.     

识别断层活动和失稳的热场标志——实验室的证据

利用一套双向伺服系统对含压性和张性雁列断层的标本进行变形实验,实验中应用红外热像仪和接触式测温仪同步记录岩石变形过程中热红外辐射的亮度温度场和温度场的变化;使用数字CCD相机同步采集标本表面的数字图像,并利用数字散斑方法对采集到的图像进行分析得到位移场和应变场的演化过程。实验结果表明:1)在断层贯通前压性雁列岩桥区温度最高,而张性雁列岩桥区温度最低;数字散斑结果显示压性岩桥区平均应变最高,而张性岩桥区平均应变最低。温度场对两类雁列断层在岩桥区相反的受力状态有清晰的响应,可以为判断断层应力状态提供标志。2)雁列断层经历了从岩桥区应力积累、破坏到断层失稳错动两个变形阶段,升温机制也由应变升温变为摩擦升温;伴随升温机制的转变,在岩桥区观测到断层失稳错动前的破坏降温、温度快速起伏以及升温脉冲等现象,是观测失稳前兆的最佳部位。3)在雁列岩桥区裂纹端点附近观测到升温脉冲,表现为温度快升快降,随后即出现断层带的快速升温。升温脉冲现象可能与裂纹端部的应力奇异集中和破裂扩展引起的应力释放有关。裂纹端部的扩展是断层失稳错动的条件,随后断层带的升温正是断层失稳错动造成的。断层带开始升温发生在失稳前2～3s内,岩桥区的降温发生在失稳     

Developments at ISO/REMCO and its Impact on the Production and Use of Geological Reference Materials

During the past decade the work of ISO/REMCO, the International Organization for Standardization’s Technical Committee on Reference Materials, was dedicated to achieving global harmonisation, and true involvement of the member countries. The first major accomplishment was the clarification of the terminology in the definitions for reference material and certified reference material, which were published as an amendment to ISO Guide 30 in 2008. The next milestone was the recognition that ISO Guide 34 (‘General requirements for the competence of reference material producers’) be used in conjunction with ISO/IEC 17025 for the accreditation of reference material producers. The third edition of ISO Guide 34 published in November 2009, clarifies the acceptable procedures for the certification of reference materials. This paper will discuss the role of ISO/REMCO in formalising the procedures for the accreditation of reference material producers and the evolution of the terms reference material and certified reference material. The paper will conclude with a case study, where a primary method in a single laboratory – one of the recognised acceptable metrologically valid procedures according to ISO Guide 34 – was used for the certification of reference materials. The reference materials are South African Reference Material SARM 2 (Syenite), SARM 3 (Lujavrite) and SARM 4 (Norite) from the suite of six NIMROCs that were originally certified by the Council for Mineral Technology (MINTEK) in South Africa in the 1970s.