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Calcium,Na, K and Mg Concentrations in Seawater by Inductively Coupled Plasma‐Atomic Emission Spectrometry: Applications to IAPSO Seawater Reference Material,Hydrothermal Fluids and Synthetic Seawater Solutions

We report a measurement procedure to determine simultaneously the major cation concentrations (Na, Ca, K and Mg) of seawater‐derived solutions by inductively coupled plasma‐atomic emission spectrometry. The best results were obtained when the IAPSO (‘standard’) seawater reference material was diluted by thirty times with Milli‐Q^® water. We obtained an average reference value r_K (the ratio of the mass fraction of potassium to that of chlorine, i.e., (g kg^?1)/(g kg^?1)) for IAPSO seawater of 0.0205 ± 0.0006 (2.9% RSD), not significantly different from 0.0206 ± 0.0005 (2.4% RSD) for seawater composition reported in the literature. The measured Na, Ca and Mg concentrations correspond to r_Na, r_Ca and r_Mg values of 0.5406 ± 0.0026 (0.5% RSD), 0.02192 ± 0.00048 (2.2% RSD) and 0.06830 ± 0.00047 (0.7% RSD), respectively, in line with previous values measured by wet‐chemistry and atomic absorption spectrophotometry or wet‐chemical titration. Our measurement procedure was used successfully on synthetic seawater solutions and high‐temperature hydrothermal fluids.     

Sulfur Concentration in Geochemical Reference Materials by Solution Inductively Coupled Plasma‐Mass Spectrometry

With implications for the origin of ore deposits, redox state of the atmosphere, and effects of volcanic outgassing, understanding the sulfur cycle is vital to our investigation of Earth processes. However, the paucity of sulfur concentration measurements in silicate rocks and the lack of well‐calibrated reference materials with concentrations relevant to the rocks of interest have hindered such investigations. To aid in this endeavour, this study details a new method to determine sulfur concentration via high mass resolution solution inductively coupled plasma‐mass spectrometry (ICP‐MS). The method is based on an aqua regia leach, involving relatively rapid sample preparation and analysis, and uses small test portion masses (< 50 mg). We utilised two independently prepared standard solutions to calibrate the analyses, resulting in 4% accuracy, and applied the method to eight geochemical reference materials. Measurements were reproducible to within ~ 10%. Sulfur concentrations and isotopes of six reference materials were measured additionally by elemental analyser‐combustion‐isotope ratio mass spectrometry to independently evaluate the accuracy of the ICP‐MS method. Reference materials that yielded reproducible measurements identical to published values from other laboratories (JGb‐1, JGb‐2 and MAG‐1) are considered useful materials for the measurement of sulfur. Reference materials that varied between studies but were reproducible for a given test portion perhaps suffer from sample heterogeneity and are not recommended as sulfur reference materials.     

Precise and Accurate In Situ Determination of Lead Isotope Ratios in NIST,USGS, MPI‐DING and CGSG Glass Reference Materials using Femtosecond Laser Ablation MC‐ICP‐MS

Lead isotope ratio data were obtained with good precision and accuracy using a 266 nm femtosecond laser ablation (fLA) system connected to a multi‐collector ICP‐MS (MC‐ICP‐MS) and through careful control of analytical procedures. The mass fractionation coefficient induced by 266 nm femtosecond laser ablation was approximately 28% lower than that by 193 nm excimer laser ablation (eLA) with helium carrier gas. The exponential law correction method for Tl normalisation with optimum adjusted Tl ratio was utilised to obtain Pb isotopic data with good precision and accuracy. The Pb isotopic ratios of the glass reference materials NIST SRM 610, 612, 614; USGS BHVO‐2G, BCR‐2G, GSD‐1G, BIR‐1G; and MPI‐DING GOR132‐G, KL2‐G, T1‐G, StHs60/80‐G, ATHO‐G and ML3B‐G were determined using fLA‐MC‐ICP‐MS. The measured Pb isotopic ratios were in good agreement with the reference or published values within 2s measurement uncertainties. We also present the first high‐precision Pb isotopic data for GSE‐1G, GSC‐1G, GSA‐1G and CGSG‐1, CGSG‐2, CGSG‐4 and CGSG‐5 glass reference materials obtained using the femtosecond laser ablation MC‐ICP‐MS analysis technique.     

国际标准物质数据库COMAR及有证标准物质

有证标准物质（CRMs）是具有准确量值的测量标准,在分析方法研究和评价、定性和定量分析、矿产勘查、仲裁检验、质量监督检验等领域发挥着重要的作用。20世纪80年代成立的国际标准物质数据库（COMAR）是目前国际上最大的CRMs数据库,收录来自25个成员国274个生产机构提供的CRMs数量超过10200种。本文从CRMs的数量、分类、发展变化等角度全面评述了国际数据库COMAR,阐述了欧盟组织、美国、中国、日本、澳大利亚等成员国的标准物质研究情况。英、美、法、德等国家的标准物质研究开展较早,研究水平高,处于世界领先地位;中国、日本等亚洲国家标准物质的发展虽起步晚,但发展迅速,已成为向COMAR提供CRMs最多的两个国家,分别为1194种和1456种（截至2013年8月）。COMAR建立以来,工业、有色金属和物理特性三大传统应用领域的CRMs占COMA数据库总CRMs的份额一直较大,比例始终保持50%以上,其中工业领域的CRMs数量最多,占19%;有机、生物与临床类CRMs所占份额最少,仅为7%和3%。随着社会需求的增加,生物与临床、生活质量领域标准物质成为未来标准物质发展的热点方向。本文指出,未来标准物质的发展将由过去的钢铁、有色金属、物理特性等传统领域逐渐转向食品安全、环境保护、气候变化、临床医学、制药产业、生物能源等新兴领域,标准物质的研究制备、定值及不确定度将面临新的技术挑战。     

Determination of trace and rare-earth elements in Chinese soil and clay reference materials by ICP-MS

Inductively coupled plasma mass spectrometry(ICP-MS) has become a powerful tool for providing reliable analytical results in many laboratories around the word. In this study, the mixture of HF and HNO3 acids in high-temperature and high-pressure closed-vessel digestion technique were used to decompose some Chinese reference materials, and thirty seven elements were determined by ICP-MS. Most of the results for Chinese soil reference materials were found to be in reasonable agreement with the reference values, except Cs, Ta, Li, Ge, Zn, Nd, Tb and Ta whose values need to be revised. Their precisions were typically lower than 5% RSD. However, the Precisions of Chinese clay reference materials, especially for GBW03102 and GBW03102a, were significantly different with reference values, probably reflecting the existence of a coarser-grained fraction(70 μm) in samples, and the formation of fluorides in Al-rich samples during sample decomposition by using the mixture of HF and HNO3 acids. Moreover, thirty-seven trace elements covering the mass range from Li to U in four Chinese clay reference materials were firstly provided with good precision and accuracy in this study.     

基于精选基准消秩亏的GNSS参考网数据处理方法

全球导航卫星系统（GNSS）参考网多用于估计卫星轨道/钟差、监测地表形变和速度场、确定精密地球自转参数等方面。相关数据处理模式包括：双差基线解（DD）和非差精密单点定位（PPP）等。本文首先从GNSS基本观测方程出发,通过选取两组基准参数,导出了上述两模式下的列满秩观测方程,然后分析了它们的不足,例如：相位偏差在DD模式中吸收了钟差,丧失了时不变特性;模糊度在PPP模式中吸收了相位偏差,失去了整数性。基于上述分析,本文提出了一种新的参考网数据处理方案,以充分融合DD和PPP模式的优势。它的关键策略是精选基准参数,以达到消秩亏的目的,具体优点体现在：相位偏差独立可估,若合理约束为时不变参数,可充分减少参数个数,提高网解精度;待估模糊度具备整周特性,经由模糊度固定,可改善网解可靠性。     

甚长基线干涉测量天线参考点和轴线偏差监测方法探讨

高精度监测VLBI天线参考点和轴线偏差等参数,对提高VLBI台站坐标测定精度及天测、测地VLBI资料解析精度等具有重要意义.常规监测方式占用望远镜工作时间,监测效率低,所得参数精度较差.文章提出通过参数化VLBI天线的旋转运动建立天线固连合作目标在局域网中坐标数学模型的方法,有望实现全天候、全自动监测;考察了代表性数学模型,在观测方程构建、解算参数设置和约束条件选取等方面提出了新的见解.最后通过仿真分析,验证了对方程与参数所做调整的有效性,初步结论可供参考.     

几种常用平面直角坐标系与国家统一3°带坐标系转换原理、方法

开展大比例尺测图时,当测区距离国家统一3°带中央子午线较远或测区高程较大时,国家统一3°带坐标系不能满足城市建设和工程建设的需要,需要建立长度变形值不大于2．5 cmk／m 的地方平面直角坐标系。地方平面直角坐标系是国家统一3°带平面直角坐标系的变换,本文研究几种常用地方平面直角坐标系与国家统一3°带坐标系相互转换的原理与方法。     

考虑LS+AR模型基础数据量的极移预报研究

针对目前极移最小二乘(Least Square, LS)+自回归(AutoRegressive, AR)预报模型的单一数据选取方案, 提出分别考虑LS模型数据量和AR残差数据量的组合数据模式, 并对极移预报时单一数据和组合数据预报结果精度进行分析, 探讨模型输入数据量对极移预报精度的影响. 结果表明, 模型输入数据量的变化对极移预报结果影响较大. 采用组合数据预报的方式相比较于单一数据量预报方式精度更高, 特别是针对30--360 d跨度内的中长期预报, 组合数据量的极移预报精度可比单一数据量预报精度有较大改善. 结论证明组合数据在极移预报时具有一定的优势, 可为以后极移预报数据量选取提供一定的借鉴参考意义.