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81.
本文采用P507萃取树脂-盐酸体系色谱法对高纯氧化镱中14种稀土杂质元素进行分离、富集,用ICP-AES法测定其稀土元素含量。当上柱量为200mgYb2O3时,所能达到的测定下限:Eu2O3为1μgg-1;Y2O3,Gd2O3,Dy2O3,Ho2O3,Tm2O3,Lu2O3为2μgg-1;La2O3,Er2O3为4μgg-1;Pr6O11,Nd2O3,Sm2O3,Tb4O7为8μgg-1;CeO2为16μgg-1。5次取样分离,加入试验回收率在88%—112%之间,相对标准偏差<10%。本方法可适用于纯度为99.95%—99.99%的氧化镱中14种稀土杂质元素的测定。 相似文献
82.
Le Zhang Jia‐Lin Wu Jia‐Run Tu Dan Wu Nan Li Xiao‐Ping Xia Zhong‐Yuan Ren 《Geostandards and Geoanalytical Research》2020,44(1):133-145
Matrix‐matched reference materials are necessary for accurate microbeam U‐Pb dating and Hf isotopic determination. This study introduces the RMJG rutile as a new potential reference material, which was separated from Palaeoproterozoic pelitic granulites collected in Hebei Province, China. LA‐ICP‐MS measurements indicate the RMJG rutile has extremely low Th (< 0.003 ± 0.01 µg g?1) and common Pb contents, but high Hf (102 ± 34 µg g?1), U (61 ± 11 µg g?1), and radiogenic Pb (~ 20 µg g?1) contents. Moreover, the rutile yields relatively constant U‐Pb ages and Hf isotopic data. The LA‐ICP‐MS analyses suggest that this rutile has a concordant U‐Pb age with a statistical mean 206Pb/238U and 207Pb/235U ages of 1749.9 ± 32.1 Ma and 1750.0 ± 26.4 Ma, respectively (2s), which are statistically indistinguishable from its ID‐TIMS ages (1750.6 ± 8.4 and 1750.1 ± 4.7 Ma). Precise determination of the 176Hf/177Hf ratio by MC‐ICP‐MS in solution mode (0.281652 ± 0.000006) is in good agreement with the statistical mean of the LA‐MC‐ICP‐MS measurements (0.28166 ± 0.00018). Therefore, the limited variations of RMJG U‐Pb age and Hf isotopic composition together with its extremely low common Pb and high Hf, U and Pb contents make it an ideal calibration and monitor reference material for LA‐ICP‐MS measurements. 相似文献
83.
Michael Weber Federico Lugli Bodo Hattendorf Denis Scholz Regina Mertz‐Kraus Damien Guinoiseau Klaus Peter Jochum 《Geostandards and Geoanalytical Research》2020,44(1):69-83
The in situ measurement of Sr isotopes in carbonates by MC‐ICP‐MS is limited by the availability of suitable microanalytical reference materials (RMs), which match the samples of interest. Whereas several well‐characterised carbonate reference materials for Sr mass fractions > 1000 µg g?1 are available, there is a lack of well‐characterised carbonate microanalytical RMs with lower Sr mass fractions. Here, we present a new synthetic carbonate nanopowder RM with a Sr mass fraction of ca. 500 µg g?1 suitable for microanalytical Sr isotope research (‘NanoSr’). NanoSr was analysed by both solution‐based and in situ techniques. Element mass fractions were determined using EPMA (Ca mass fraction), as well as laser ablation and solution ICP‐MS in different laboratories. The 87Sr/86Sr ratio was determined by well‐established bulk methods for Sr isotope measurements and is 0.70756 ± 0.00003 (2s). The Sr isotope microhomogeneity of the material was determined by LA‐MC‐ICP‐MS, which resulted in 87Sr/86Sr ratios of 0.70753 ± 0.00007 (2s) and 0.70757 ± 0.00006 (2s), respectively, in agreement with the solution data within uncertainties. Thus, this new reference material is well suited to monitor and correct microanalytical Sr isotope measurements of low‐Sr, low‐REE carbonate samples. NanoSr is available from the corresponding author. 相似文献
84.
Meng‐Shu Liu Qun Zhang Yingnan Zhang Zhaofeng Zhang Fang Huang Hui‐Min Yu 《Geostandards and Geoanalytical Research》2020,44(1):169-182
This study presents a high‐precision Cd isotope measurement method for soil and rock reference materials using MC‐ICP‐MS with double spike correction. The effects of molecular interferences (e.g., 109Ag1H+, 94Zr16O+, 94Mo16O+ and 70Zn40Ar+) and isobaric interferences (e.g., Pd, In and Sn) to Cd isotope measurements were quantitatively evaluated. When the measured solution has Ag/Cd ≤ 5, Zn/Cd ≤ 0.02, Mo/Cd ≤ 0.4, Zr/Cd ≤ 0.001, Pd/Cd ≤ 5 × 10?5 and In/Cd ≤ 10?3, the measured Cd isotope data were not significantly affected. The intermediate measurement precision of pure Cd solutions (BAM I012 Cd, Münster Cd and AAS Cd) was better than ± 0.05‰ (2s) for δ114/110Cd. The δ114/110Cd values of soil reference materials (NIST SRM 2709, 2709a, 2710, 2710a, 2711, 2711a and GSS‐1) relative to NIST SRM 3108 were in the range of ?0.251 to 0.632‰, the δ114/110Cd values of rock reference materials (BCR‐2, BIR‐1, BHVO‐2, W‐2, AGV‐2, GSP‐2 and COQ‐1) varied from ?0.196‰ to 0.098‰, and that of the manganese nodule (NOD‐P‐1) was 0.163 ± 0.040‰ (2s, n = 8). The large variation in Cd isotopes in soils and igneous rocks indicates that they can be more widely used to study magmatic and supergene processes. 相似文献
85.
John B. Creech Bruce F. Schaefer Simon P. Turner 《Geostandards and Geoanalytical Research》2020,44(2):223-229
Recent developments in amplifier hardware enable low‐noise measurements of exceedingly small ion beams in isotope ratio analysis, yielding higher precision from smaller samples than ever before. To date, these amplifiers have largely been employed in thermal ionisation instruments, with few applications using plasma‐source (i.e., MC‐ICP‐MS) instruments. Here, we demonstrate the utility of these new generation 1013 Ω amplifiers in MC‐ICP‐MS, employing Pt isotopes as a case study, a system that could greatly benefit from the promised advances. The data demonstrate that for samples with low Pt abundance, for a modest increase in uncertainties, the amount of sample required can be reduced by a factor of 50–100. This technique thereby opens up new possibilities for analysis of samples that have low Pt mass fractions or were otherwise impossible to obtain in sufficient quantities. 相似文献
86.
Characterisation of Apatites as Potential Uranium Reference Materials for Fission‐track Dating by LA‐ICP‐MS 下载免费PDF全文
Cleber J. Soares Regina Mertz‐Kraus Sandro Guedes Daniel F. Stockli Thomas Zack 《Geostandards and Geoanalytical Research》2015,39(3):305-313
We report homogeneity tests on large natural apatite crystals to evaluate their potential as U reference materials for apatite fission‐track (AFT) thermochronology by laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS). The homogeneity tests include the measurements of major element concentrations by electron probe microanalysis (EPMA), whereas for U concentration, isotope dilution (ID) ICP‐MS and laser ablation (LA) ICP‐MS were employed. Two apatite crystals are potential reference materials for LA‐ICP‐MS analysis: a 1 cm3 fraction of a Durango crystal (7.5 μg g?1 U) and a 1 cm3 Mud Tank crystal (6.9 μg g?1 U). The relative standard deviation (1 RSD) of the U concentration determined by ID‐ICP‐MS of both apatite crystals was ≤ 1.5%, whereas 1 RSD for the LA‐ICP‐MS results was better than 4%, providing sufficient homogeneity for fission‐track dating. The results on the U homogeneity for two different apatite samples are an important step towards establishing in situ dating routines for AFT analysis by LA‐ICP‐MS. 相似文献
87.
An Evaluation of the Effects of Primary and Cross‐Contamination during the Preparation of Rock Powders for Chemical Determinations 下载免费PDF全文
José P. Sertek Sandra Andrade Horstpeter H. Ulbrich 《Geostandards and Geoanalytical Research》2015,39(3):381-397
Quartz crystals from the Batatal site, Minas Gerais, southern Brazil, were used to determine quantitatively primary contamination when submitting the samples to milling processes. Crushing devices used were a primary steel jaw crusher (br1), a secondary tungsten carbide (WC) crusher (br2) and a hydraulic press with stainless steel plates (pr). Fragments with suitable sizes were then ground in different Fritsch planetary mills, equipped with agate, WC and chromium‐steel rings for 7, 4 and 3 min, respectively. Solutions of the powders were analysed initially with the TotalQuant? method in a quadrupole ICP‐MS instrument, providing semi‐quantitative results for seventy‐five elements. Contamination from crushers and mills was visible in major and minor elements such as Fe, Mn and Ti, and noticeable in trace elements such as Cr, Co, Ni, Cu and also V, Zr, Sc; significant contamination was observed from W, Mo, Co, Ta and Nb (mainly by use of the WC devices). Little or no contamination was observed for Pb, REE, Sr and Rb, elements that are important in routine isotopic determinations. Cross‐contamination was tested by grinding either a granite or a basalt sample, followed by conventional cleaning with mica‐free quartz sand, before the working quartz powder was prepared. 相似文献
88.
Yimin Wang Xiaohong Wang Wenjun Qu Yushu Gao Tiexin Gu Xingtao Fan S.I. Andreev Xuefa Shi 《Geostandards and Geoanalytical Research》2011,35(3):341-352
Two Co‐rich seamount crust reference materials, MCPt‐1 and MCPt‐2, were prepared using ultra‐fine particle size milling technique and characterised for the platinum‐group elements (PGEs). The raw material for these two reference materials was collected separately from the Magellan seamounts of the western Pacific Ocean and the seamounts of the central Pacific Ocean by Russian and Chinese scientists. First, they were ground by ball mill to a ?200 mesh powder, then further processed by ultra‐fine jet mill and well‐mixed. The particle size distributions of the samples were tested by a laser particle analyser; the average particle size was 1.8 and 1.5 μm (equal to about 2000 mesh) respectively. The homogeneity of six major and minor elements in these two materials was tested at the milligram level of sampling mass by high‐precision wavelength dispersive X‐ray fluorescence (XRF) spectrometry and at the microgram level of sampling mass by electron probe microanalyser. The homogeneity of more than forty trace elements, including Pt, was tested at the microgram level of sampling mass by LA‐ICP‐MS. Except for Rh, all PGEs were determined by isotope dilution‐ICP‐MS. Platinum in MCPt‐1 and MCPt‐2 was characterised as certified values, whereas the other five PGEs in MCPt‐1 and MCPt‐2 were reported as reference values. In addition, the information values of sixty‐two major, minor and trace elements were obtained by XRF, ICP‐AES and ICP‐MS. The minimum sampling mass for the determination of PGEs was 1 g, while the minimum sampling mass for the determination of the other elements was 2–5 mg. 相似文献
89.
Mg/Ca and Sr/Ca ratios in calcium carbonate are important components of many palaeoclimate studies. We present an isotope dilution method relying on a single mixed spike containing 25Mg, 43Ca and 87Sr. Dozens of samples per day, as small as 10 μg of carbonate, could be dissolved, spiked and run in an ICP‐MS with a precision of 0.8% (2 RSD). Two instruments types, a sector field and a quadrupole ICP‐MS, were compared. The best long term precision found was 0.4% (2 RSD), although this increased by up to a factor of two when samples of very different Mg or Sr content were run together in the same sequence. Long term averages for the two instruments concurred. No matrix effects were detected for a range of Ca concentrations between 0.2 and 2 mmol l‐1. Accuracy, tested by measuring synthetic standard solutions, was 0.8% with some systematic trends. We demonstrate the strength of this isotope dilution method for (a) obtaining accurate results for sample sets that present a broad Mg and Sr range and (b) testing solid carbonates as candidate reference materials for interlaboratory consistency. Mg/Ca and Sr/Ca results for reference materials were in good agreement with values from the literature. 相似文献
90.
Germain Bayon Dominique Birot Claire Bollinger Jean Alix Barrat 《Geostandards and Geoanalytical Research》2011,35(1):145-153
We report on an improved method for determining trace element abundances in seawater and other natural waters. The analytical procedure involves co‐precipitation on iron hydroxides after addition of a Tm spike, and measurement by inductively coupled plasma‐sector field mass spectrometry (ICP‐SFMS). The validity of the method was assessed through a series of co‐precipitation experiments, using ultra‐diluted solutions of a certified rock reference material (BIR‐1). Results obtained for four natural water reference materials (NASS‐5, CASS‐4, SLEW‐3, SLRS‐4) are in agreement with published working values for rare earth elements, yttrium, vanadium and, when available, for hafnium, zirconium, thorium and scandium. A set of proposed values with uncertainties typically better than 8% RSD is proposed for Hf, Zr and Th. 相似文献