共查询到20条相似文献，搜索用时 218 毫秒
1.
Adam J.R. Kent Benjamin Jacobsen David W. Peate Tod E. Waight Joel A. Baker 《Geostandards and Geoanalytical Research》2004,28(3):417-429
We present data for the concentrations of eleven rare earth elements (La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Er, Yb, Lu) in eleven international geochemical reference materials obtained by isotope dilution multi-collector inductively coupled plasma-mass spectrometry (MC-ICP-MS). We have analysed both rock powders and synthetic silicate glasses, and the latter provide precise data to support the use of these as reference materials for in situ trace element determination techniques. Our data also provide precise measurements of the abundance of mono-isotopic Pr in both glasses and powders, which allows more accurate constraints on the anomalous redox-related behaviour of Ce during geochemical processes. All materials were analysed in replicate providing data that typically reproduce to better than one percent. Sm/Nd ratios in all these materials also reproduce to better than 0.2% and are accurate to < 0.2% and can thus be used as calibrants for Sm-Nd geochronology. Our analyses agree well with existing data on these reference materials. In particular, for NIST SRM 610, USGS BHVO-2, AGV-1 and AGV-2, our measured REE abundances are typically within < 2% (and mostly 1%) of REE concentrations previously determined by isotope dilution analysis and thermal ionisation mass spectrometry, consistent with the higher degree of precision and accuracy obtained from isotope dilution techniques. Close agreement of results between basaltic glass reference materials USGS BHVO-2G and BCR-2G and the BHVO-2 and BCR-2 powders from which they were created suggests that little fractionation, concentration or dilution of REE contents occurred during glass manufacture. 相似文献
2.
Isotope dilution mass spectrometry has been used to measure copper, zinc, cadmium and lead in the marine sediments SD-M-2/TM and BCSS-1 and dogfish muscle DORM-1. The measured values for the metals in the latter two materials are in agreement with the certified values except for zinc where the certified values are slightly higher. Sample SD-M-2/TM, which has only recently become available, has a composition similar, although not identical to BCSS-1. 相似文献
3.
Data were obtained for rubidium in six geological reference materials by isotopic dilution thermal ionisation mass spectrometry (ID-TIMS) and wavelength dispersive X-ray fluorescence spectrometry (WD-XRF). The results found by one technique compare very well with the other within the respective analytical uncertainties and are also in good agreement with data from previously published values. The particular case of low Rb determinations in reference sample BIR-1 is discussed. 相似文献
4.
M.D. Norman W.P. Leeman D.P. Blanchard§ J. G. Fitton† D. James† 《Geostandards and Geoanalytical Research》1989,13(2):283-290
Element concentration data for a set of silicate igneous rocks have been determined by four independent analytical methods: inductivelycoupled plasma emission spectroscopy (ICP), instrumental neutron activation analysis (INAA), x-ray fluorescence (XRF), and isotope dilution mass spectrometry (ID). The results show excellent agreement among elements determined by more than one technique, and demonstrate the suitability of commercially available ICP instrumentation for the routine analysis of geologic material compared to other standard methods. 相似文献
5.
Ingrid Raczek Brigitte Stoll Albrecht W. Hofmann Klaus Peter Jochum 《Geostandards and Geoanalytical Research》2001,25(1):77-86
Different batches of the new US Geological Survey (USGS) reference materials (RMs) BCR-2, BHVO-2, AGV-2, DTS-2 and GSP-2 and the original USGS RMs BCR-1, BHVO-1, AGV-1, DTS-1 and GSP-1 have been analysed by isotope dilution using thermal ionisation mass spectrometry (ID-TIMS) and by multi-ion counting spark source mass spectrometry (MIC-SSMS). The concentrations of K, Rb, Sr, Ba and the rare earth elements were determined with overall analytical uncertainties of better than 1% (ID-TIMS) and 3% (MIC-SSMS). The analyses of different aliquots and batches of BCR-2, BHVO-2, AGV-2 and GSP-2, respectively, agree within 1%, i.e. approximately the analytical uncertainties of the data. This indicates an homogeneous distribution of the trace elements in these RMs. Differences in element concentrations of up to 17% in different aliquots of the depleted RM DTS-2 are outside the analytical uncertainty of our data. They may be attributed to a slightly heterogeneous distribution of trace elements in this dunite sample. Our trace element data for BCR-2, BHVO-2, AGV-2 and GSP-2 agree within about 3% with preliminary reference values published by the USGS. They also agree within 1-6% with those of the original RMs BCR-1, BHVO-1, AGV-1 and GSP-1. Large compositional differences are found between DTS-2 and DTS-1, where the concentrations of K, Rb, Sr and the light REE differ by factors of 2 to 24. 相似文献
6.
AG-MP-1M阴离子交换树脂分离-表面热电质谱法测定沉积物中的铅同位素组成 总被引：2，自引：1，他引：1
利用新型阴离子交换树脂分离沉积物中的重金属Pb,采用表面热电离质谱法(TIMS)测定了沉积物样品中的Pb同位素组成。新型树脂为大孔径阴离子树脂AG-MP-1M,淋洗液采用低浓度的盐酸,避免了使用难以纯化的氢溴酸,可有效地降低试剂空白。通过对铅同位素标准物质NIST NBS-981的重复测试,方法的精密度(<0.5%,2s)和准确度均达到了应用研究的要求。对5个实际沉积物样品中的铅同位素组成进行测定,获得了理想的分析效果。 相似文献
7.
Martin Rosner Lary Ball Bernhard Peucker-Ehrenbrink Jerzy Blusztajn Wolfgang Bach Jörg Erzinger 《Geostandards and Geoanalytical Research》2007,31(2):77-88
We report a new approach to conduct fast and accurate lithium isotope ratio measurements by MC-ICP mass spectrometry after wet chemical sample preparation. In contrast to most previously published methods our MC-ICP-MS set-up did not use a desolvating system to achieve appropriate ion beam intensities and, therefore, was less affected by matrix-induced shifts of the instrumental mass bias. As the total lithium background and build-up in the sample introduction system was low, previous sample residues could be washed out by an extended uptake of the new sample. Elimination of a nitric acid rinse step increased the sample throughput by a factor of two and allowed the instrumental mass bias drift to be tracked more precisely. δ7 Li values of powdered silicate rock reference materials and seawater obtained in this study revealed good accuracy and an overall analytical uncertainty of typically 0.5‰ (2s). On the basis of a comparison between our lithium isotope data and compiled literature data, we recommend preliminary average δ7 Li values for seawater (+30.8‰) and several silicate rock reference materials (BHVO-1: +5.0‰; JA-1: +5.6‰; JB-2: +4.8‰). The compilation of published δ7 Li values for seawater suggests that the observed large lithium isotope differences are due to inter-method and/or interlaboratory bias. Most recently published δ7 Li values for seawater show little variation and confirm a constant lithium isotope composition (at the sub ‰ level) of seawater in well mixed ocean basins. 相似文献
8.
Trace element concentrations in BIR-1 basalt have been determined by isotope dilution-spark source mass spectrometry, high performance liquid chromatography and laser ionization mass spectrometry. Of particular interest are the low abundance elements Nb, Ta, Zr, Hf, Th, U, Rb, Cs for which published data vary extremely. Our analyses of most trace elements in four different batches of BIR-1, however, agree within 10% indicating that these large differences cannot be caused by heterogeneities of the powders but may be attributed to analytical problems. Based on own and recently published data, an attempt is made to assign "preferred values" for BIR-1 which are at variance with several published consensus or working values by as much as a factor of 110. 相似文献
9.
Isotope dilution (ID) mass spectrometry is a primary method of analysis suited for the accurate and precise measurement of several trace elements in geological matrices. Here we present mass fractions and respective uncertainties for Cr, Cu, Ni, Sn, Sr and Zn in 10 silicate rock reference materials (BCR‐2, BRP‐1, BIR‐1, OU‐6, GSP‐2, GSR‐1, AGV‐1, RGM‐1, RGM‐2 and G‐3) obtained by the double ID technique and measuring the isotope ratios with an inductively coupled plasma‐mass spectrometer equipped with collision cell. Test portions of the samples were dissolved by validated procedures, and no further matrix separation was applied. Addition of spikes was designed to achieve isotope ratios close to unity to minimise error magnification factors, according to the ID theory. Radiogenic ingrowth of 87Sr from the decay of 87Rb was considered in the calculation of Sr mass fractions. The mean values of our results mostly agree with reference values, considering both uncertainties at the 95% confidence level, and also with ID data published for AGV‐1. Considering all results, the means of the combined uncertainties were < 1% for Sr, approximately 2% for Sn and Cu, 4% for Cr and Ni and almost 6% for Zn. 相似文献
10.
11.
Cadmium has been determined in a range of silicate rock standards using the stable isotope dilution technique incorporating solid source mass spectrometry. Our recommended values are, in general, lower than the previously reported data. 相似文献
12.
Joy E. Reid Ingo Horn Henry P. Longerich Lance Forsythe George A. Jenner 《Geostandards and Geoanalytical Research》1999,23(2):149-155
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. 相似文献
13.
We have developed a rapid and accurate method to determine Zr, Nb, Hf and Ta (denoted as HFSE) in geological samples by inductively coupled plasma-mass spectrometry fitted with a flow injection system (FI-ICP-MS). The method involves sample decomposition by HF followed by HF dissolution of HFSE coprecipitated with insoluble M and Ca fluoride residues formed during the initial HF attack. This HF solution was directly nebulized into an ICP mass spectrometer. An external calibration curve method and an isotope dilution method (ID) were applied for the determination of Nb and Ta, and of Zr and Hf, respectively. Recovery yields of HFSE were > 96% for peridotite, basalt and andesite compositions, apart from Zr and Hf for peridotite (> 85%). No matrix effects for either signal intensities of HFSE or isotope ratios of Zr and Hf were observed in basalt, andesite and peridotite solutions down to a dilution factor of 100. Detection limits in silicate rocks were 40, 2, 1 and 0.1 ng g-1 for Zr, Nb, Hf and Ta, respectively. This technique required only 0.1 ml of sample solution, and thus is suitable for analysing small and/or precious samples such as meteorites, mantle peridotites and their mineral separates. We also present newly determined data for the Zr, Nb, Hf and Ta concentrations in USGS silicate reference materials DTS-1, PCC-1, BCR-1, BHVO-1 and AGV-1, GSJ reference materials JB-1, -2, -3, JA-1, -2 and -3, and the Smithsonian reference Allende powder. 相似文献
14.
Ruthenium, palladium and iridium have been determined in 27 international reference rocks, ores and related materials by inductively-coupled plasma mass spectrometry using isotope dilution and sample introduction by solution nebulization and electrothermal vaporization, after chemical separation by co-precipitation with tellurium. The accuracy of the procedure is discussed by comparison of the results obtained with synthetic solutions and standard samples. 相似文献
15.
Horst R. Marschall Christian Meyer Bernd Wunder Thomas Ludwig Wilhelm Heinrich 《Contributions to Mineralogy and Petrology》2009,158(5):675-681
Tourmaline synthesised in an experiment with low boron excess was analysed in situ by secondary ion mass spectrometry. It
revealed significant B isotope zonation with 11B/10B ratios increasing in the growth direction of the crystals. Trend, magnitude and absolute values strongly support results
from high-B-excess isotope fractionation experiments. Furthermore, the closed system B-isotopic evolution of the experimental
fluid was modelled by Rayleigh fractionation. The model results are in excellent agreement with the measured B-isotope composition
of the run-product fluid. Consequently, low-element-excess experiments are proposed as an ideal approach to determine fluid-solid
isotope fractionation factors for systems that are characterised by Rayleigh fractionation. 相似文献
16.
Molybdenum concentrations in eleven USGS geochemical reference materials AGV-1, BCR-1, BHVO-1, BIR-1, DNC-1, DTS-1, G-2, GSP-1, MAG-1, PCC-1 and W-2 were measured by isotope dilution thermal ionisation mass spectrometry (ID-TIMS). In every case but one, the concentrations determined in this study were significantly lower than the current consensus values. Molybdenum concentrations determined by ID-TIMS are inherently more accurate and precisions may be up to an order of magnitude higher than those measured by other analytical techniques. 相似文献
17.
Iwan Roelandts 《Geostandards and Geoanalytical Research》1987,11(1):49-74
Nine rare earth elements have been determined by inductively coupled plasma spectrometry (ICP) in eight USGS reference samples, MAG-1, SCo-1, SDC-1, BIR-1, DNC-1, W-2, BCR-1 and BHVO-1 and in the ANRT Glauconite, GL-O. Along with these new data, updated compilations are presented for these samples. Good agreement is observed between the present work and the compiled values. 相似文献
18.
A thermal ionisation mass spectrometric technique enabled the abundance of Zn in geological and biological reference materials and water samples to be measured by double spiking isotope dilution mass spectrometry enriched in the 67Zn and 70Zn isotopes. In the past, thermal ionisation mass spectrometry proved to be difficult for low-level zinc isotopic measurements. The size of Zn samples used for isotopic determination, in particular the biological RMs, represents an important breakthrough. These results represent the most accurate and precise concentrations measured for Zn in these samples. The maximum fractional uncertainty was that for TILL-3 (2%), while the minimum fractional uncertainty was 0.7% for both BCR-1 and W-2. The inhomogeneity of Zn in HISS-1 was revealed while other reference materials appeared homogeneous at the 95% confidence uncertainty. The certified concentration of Zn in HISS-1 and IMEP-19 by their producers are 28% and 3.8% higher than the values measured in this work. These are the first Zn concentration measurements in these materials by the isotope dilution-TIMS technique, except for BCR-1, NIES No 9 and IMEP-19. Reducing the blank enabled accurate measurement in water at the ng g-1 level demonstrating the applicability of the technique for low-level Zn samples. 相似文献
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20.
Taeko Shinonaga Helmuth Aigner Dilani Klose Peter Spinder Heinz Fröschl David Donohue 《Geostandards and Geoanalytical Research》2008,32(1):93-101
The recommended concentrations of 239Pu, 240Pu and 239+240Pu in reference material IAEA‐315 (marine sediment) were estimated by three analytical methods: isotope dilution thermal ionisation mass spectrometry (TIMS), isotope dilution inductively coupled plasma‐mass spectrometry (ICP‐MS) and alpha spectrometry. The determination of 239Pu and 240Pu (239+240Pu by alpha spectrometry) was carried out with samples from randomly selected bottles using each method. Plutonium‐238 was also measured by alpha spectrometry. A plutonium‐242 reference material was used as a spike for the quantitative analysis. The influence of 242Pu in the samples was therefore calculated; however, this contribution was less than the range of uncertainty and did not influence the final results. The obtained data were statistically analysed using variance component analysis and paired comparison. The combined standard uncertainties from “method/measurement”, “bottle” and “sub‐sample” were in the order of 3 to 6%. The main contributions to the uncertainty were from the material heterogeneity and from systematic differences between methods. Based on this study with twenty‐seven analyses using 10–14 g sample mass, concentrations of (38 ± 3) Bq kg?1, (28 ± 3) Bq kg?1 and (66 ± 4) Bq kg?1 are proposed as recommended values for 239Pu, 240Pu and 239+240Pu, respectively, and (9.5 ± 0.4) Bq kg?1 for 238Pu as an information value in reference material IAEA‐315. In mass concentration units, these amount to (16.4 ± 1.2) ng kg?1, (3.3 ± 0.4) ng kg?1 and (0.015 ± 0.003) ng kg?1 for 239Pu, 240Pu and 238Pu, respectively. The certified reference materials NIST 4350B and NIST 4354 were also analysed by TIMS for quality assurance of the method used in this study. 相似文献