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61.
A range of independently characterised reference materials (RMs) for LA‐ICP‐MS, used for the determination of the platinum‐group elements (PGE) and Au in a sulfide matrix, were analysed and compared: 8b, PGE‐A, NiS‐3, Po727‐T1, Po724‐T and the Lombard meteorite. The newly developed RM NiS‐3 was used as the RM for the calibration of all LA‐ICP‐MS analyses and the measured concentrations of the other RMs compared against their published concentrations. This data were also used to assess the consistency of concentrations calibrated against the different RMs. It was found that Po727‐T1 and 8b produced results that were comparable, within uncertainty, for all elements. Po727‐T1 also produced consistent results with NiS‐3 for all elements. All other RMs showed differences for some elements, especially Ru in Po724‐T, and Os, Ir and Au in PGE‐A. The homogeneity of the PGE and Au in each RM was assessed, by comparing the precision of multiple LA‐ICP‐MS spot analyses with the average uncertainty of the signal. Po724‐T, Po727‐T1 and the Lombard meteorite were found to be homogeneous for all elements, but 8b, PGE‐A and NiS‐3 were heterogeneous for some elements. This is the first direct comparison between a range of independently characterised PGE and Au LA‐ICP‐MS RMs.  相似文献   
62.
Research into natural mass‐dependent stable isotope fractionation of cadmium has rapidly expanded in the past few years. Methodologies are diverse with MC‐ICP‐MS favoured by all but one laboratory, which uses thermal ionisation mass spectrometry (TIMS). To quantify the isotope fractionation and correct for instrumental mass bias, double‐spike techniques, sample‐calibrator bracketing or element doping has been used. However, easy comparison between data sets has been hampered by the multitude of in‐house Cd solutions used as zero‐delta reference in different laboratories. The lack of a suitable isotopic reference material for Cd is detrimental for progress in the long term. We have conducted a comprehensive round‐robin assay of NIST SRM 3108 and the Cd isotope offsets to commonly used in‐house reference materials. Here, we advocate NIST SRM 3108 both as an isotope standard and the isotopic reference point for Cd and encourage its use as ‘zero‐delta’ in future studies. The purity of NIST SRM 3108 was evaluated regarding isobaric and polyatomic molecular interferences, and the levels of Zn, Pd and Sn found were not significant. The isotope ratio 114Cd/110Cd for NIST SRM 3108 lies within ~ 10 ppm Da?1 of best estimates for the Bulk Silicate Earth and is validated for all measurement technologies currently in use.  相似文献   
63.
等离子体发射光谱法测定大气颗粒物中的无机元素   总被引:14,自引:4,他引:10  
建立了用等离子体发射光谱(ICP-AES)测定大气颗粒物中无机元素的分析方法,包括样品消解体系的选择,仪器的操作条件及采样滤膜的选择,产对自行采样分析测得的无机元素数据作了初步的讨论。实验结果表明:采用HNO3-HClO4消解体系,操作方便,样品消解较完全;选用石英滤膜查减低空白值,保证测定质量以及同时在一张滤膜上测定大气颗粒物中的有机碳、元素碳及无机元素;内标法可有效降低由于仪器漂移等因素对测定  相似文献   
64.
报道了用王水-HF溶样,ICP-AES同时测定海洋沉积物中18种常量、微量元素的方法.该方法简便、快捷,其准确度、精密度及检出限均好.  相似文献   
65.
66.
万洋山岩体位于湘赣两省交界地带,为加里东期多阶段岩浆活动的复式岩体,花岗岩主要岩石类型有黑云母二长花岗岩、黑云母花岗闪长岩和二云母二长花岗岩,以黑云母二长花岗岩分布面积最广。对岩体中黑云母二长花岗岩中的锆石样品进行激光剥蚀—多接收器电感耦合等离子体质谱(LA-ICP-MS)U-Pb定年,锆石的16个测点206Pb/238U的加权平均年龄为(446.0±3.4)Ma(n=16,MSWD=0.15)(95%置信度),反映该岩体形成于晚奥陶世至早志留世。岩石地球化学表明岩体中Si O2的含量为65.91%~73.35%,K2O的平均含量为4.20%,Na2O+K2O为5.90%~7.88%,K2O/Na2O平均值为1.64,Al2O3平均值为13.81%,ASI平均值为1.09%,总体属于高钾钙碱性过铝质花岗岩。微量元素组成中Ba、K、Sr、P、Ti表现出明显的亏损,Rb、Th、U、Nb、Zr、Hf等则相对富集,稀土元素总量中等(159.71×10-6~262.78×10-6),轻稀土富集LREE/HREE=6.16~10.01,(La/Yb)N=6.37~12.17,具明显的负Eu异常(δEu=0.30~0.59)。岩体的[n(87Sr)/n(86Sr)]i值为0.71223~0.72509,εSr(t)值为117.5~299.9Ma,εNd(t)值为-9.39~-7.30,两阶段Nd模式年龄(TDM2)为1.77~1.94 Ga。根据上述岩石地球化学特征表明万洋山岩体为来源于地壳的S型花岗岩,花岗岩氧化物和微量元素构造环境判别图解指示岩体形成于后碰撞构造环境。结合前人对华南加里东期岩体的研究成果,推断华南加里东期花岗岩岩体的具体形成机制为:在全球板块构造的影响,华夏板块与扬子板块拼接后,板块间的强烈挤压应力相对松弛、压力降低的后碰撞构造环境下,因地壳增厚而升温的中上地壳岩石减压熔融并向上侵位。  相似文献   
67.
陈井胜  李斌  姚玉来  刘淼  杨帆  邢德  李伟  汪岩 《地质学报》2016,90(10):2733-2746
辽宁东北部桓仁—吉林南部通化地区分布有大面积的中生代火山岩,分别属于果松组、林子头组及小岭组。通过野外地质调查发现,这三个组的火山岩组合自下而上均显示为酸性—中性—酸性的岩石组合,在岩石组合上具有可对比性。对这三个组的典型火山岩进行LA-ICP-MS锆石U-Pb测年,结果显示果松组安山岩(GS-1-TWS)和流纹岩(GS-2-TWS)年龄为130.83±0.8Ma和118.5±1.1Ma;林子头组安山质凝灰岩(LZT1)和安山岩(LZT2)年龄为123.24±0.91Ma和126.0±2.9Ma;小岭组流纹岩(P03-29)和安山岩(P03-30)年龄为126.3±1.3Ma和129.0±1.4Ma,表明三个含有中生代火山岩的地层形成时代一致,均为早白垩世产物。辽西地区含有中生代火山岩的地层为义县组,其形成时代为133~118Ma之间,本文辽宁桓仁—吉林通化地区中生代火山岩形成时代为130~118Ma,二者为同时产物;并且二者均产有相同的热河生物群化石,所以辽东北—吉南果松组、林子头组、小岭组与辽西义县组可对比。!  相似文献   
68.
A two‐step Th isolation protocol, involving micro‐columns of TRU‐Spec extraction chromatography material and AG1 resin, was evaluated. The MC‐ICP‐MS procedure included 232Th tailing characterisation and correction, and calibrator bracketing using an in‐house standard solution (ThS1) to correct for instrumental mass bias and Faraday cup to secondary electron multiplier relative gain. Repeated analyses of reference solutions (UCSC Th ‘A’, WUN, OU Th ‘U’, IRMM‐36) were consistent with published data. Six reference materials (A‐THO, BCR‐2, AGV‐2, BHVO‐2, BE‐N and BIR‐1) were processed. The average 230Th/232Th values obtained for these samples are in excellent agreement with published data. In addition, we report the first 230Th/232Th values for BE‐N and BIR‐1. The intermediate precisions for rock samples ranged from ± 0.24 to ± 0.49% (2 RSD) and were similar to those achieved for synthetic solutions, thereby supporting the overall validity of the chemical separation, data acquisition and reduction procedures. Counting statistics on the 230Th isotope was the most significant source of uncertainty. The intermediate precision of the mean 230Th/232Th for the Th‐depleted BIR‐1 (5.64 × 10?6 ± 0.27%, 2 RSD) is in the range of the analyses of other reference materials analysed in this study.  相似文献   
69.
Trace element concentrations in gold grains from various geological units in South Africa were measured in situ by field emission‐electron probe microanalysis (FE‐EPMA), laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS) and synchrotron micro X‐ray fluorescence spectroscopy (SR‐μ‐XRF). This study assesses the accuracy, precision and detection limits of these mostly non‐destructive analytical methods using certified reference materials and discusses their application in natural sample measurement. FE‐EPMA point analyses yielded reproducible and discernible concentrations for Au and trace concentrations of S, Cu, Ti, Hg, Fe and Ni, with detection limits well below the actual concentrations in the gold. LA‐ICP‐MS analyses required larger gold particles (> 60 μm) to avoid contamination during measurement. Elements that measured above detection limits included Ag, Cu, Ti, Fe, Pt, Pd, Mn, Cr, Ni, Sn, Hg, Pb, As and Te, which can be used for geochemical characterisation and gold fingerprinting. Although LA‐ICP‐MS measurements had lower detection limits, precision was lower than FE‐EPMA and SR‐μ‐XRF. The higher variability in absolute values measured by LA‐ICP‐MS, possibly due to micro‐inclusions, had to be critically assessed. Non‐destructive point analyses of gold alloys by SR‐μ‐XRF revealed Ag, Fe, Cu, Ni, Pb, Ti, Sb, U, Cr, Co, As, Y and Zr in the various gold samples. Detection limits were mostly lower than those for elements measured by FE‐EPMA, but higher than those for elements measured by LA‐ICP‐MS.  相似文献   
70.
Moss samples (Pleurozium schreberi) exposed to traffic‐related emission of Pd, Pt and Rh were analysed in this study. Successful elimination of interferences was achieved in the determination of Pd, Pt and Rh mass fractions in these samples using inductively coupled plasma‐tandem mass spectrometry (ICP‐MS/MS). Based on the results, a reliable determination of Pd, Pt and Rh mass fractions in microwave‐digested moss samples was obtained using ammonia (10% NH3 in He) in the collision/reaction cell when 103Rh was measured either on‐mass (103→103) or with mass‐shift (103→171) and mass‐shifts for 108Pd (108→159) and 195Pt (195→229) were used. The ICP‐MS/MS procedure was validated using BCR‐723 (road dust) as a reference material. In addition, a good agreement between the ICP‐MS/MS results and the results obtained with cloud point extraction and quadrupole ICP‐MS was observed for the moss samples.  相似文献   
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