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21.
German Velásquez Anastassia Y. Borisova Stefano Salvi Didier Béziat 《Geostandards and Geoanalytical Research》2012,36(3):315-324
Gold and copper concentrations were determined in natural pyrite by near‐infrared femtosecond LA‐ICP‐QMS, using both sulfide reference materials (pyrrhotite Po‐726 and in‐house natural chalcopyrite Cpy‐RM) and NIST SRM 610 as external calibrators. Firstly, using NIST SRM 610 as the external calibrator, we calculated the Au concentration in Po‐726 and the Cu concentration in Cpy‐RM. The calculated concentration averages for Au and Cu were similar to the values published for Po‐726 and Cpy‐RM, respectively. Secondly, we calculated Au and Cu concentrations taking NIST SRM 610 as an unknown sample and using Po‐726 and Cpy‐RM as external calibrators. Again, the average values obtained closely reflected the preferred concentrations for NIST SRM 610. Finally, we calculated Au and Cu concentrations in natural pyrite using sulfide and silicate reference materials as external calibrators. In both cases, calculated concentrations were very similar, independent of the external calibrator used. The aforementioned data, plus the fact that we obtained very small differences in relative sensitivity values (percentage differences are between 5% and 17% for 57Fe, 63Cu and 197Au) on analyses of silicate and sulfide RMs, indicate that there were no matrix effects related to the differences in material composition. Thus, it is possible to determine Au and Cu in natural sulfides using NIST silicate glasses as an external calibrator. 相似文献
22.
Mohammad Wasim Mohammad Arif Sajid Iqbal Muhammad Daud 《Geostandards and Geoanalytical Research》2013,37(1):87-93
The International Atomic Energy Agency (IAEA) organised a proficiency test (PT), IAEA‐CU‐2010‐02, for the determination of elements in sewage sludge. The PT sample was analysed by semi‐absolute standardless k0‐instrumental neutron activation analysis (k0‐INAA). Results for seven elements (As, Co, Cr, Fe, Hg, Se, Zn) were submitted to the IAEA by our laboratory. All of our results were scored ‘acceptable’ by the ‘result evaluation criteria’ adopted by the IAEA. The same analytical methodology produced quantitative results for twenty‐six additional elements. In total, thirty‐six elements were determined with uncertainty varying from 4 to 11%. This paper presents the provisional mass fractions of twenty‐six additional elements (Ag, Al, Br, Ca, Ce, Cl, Dy, Eu, Ga, Hf, I, K, La, Mg, Mn, Na, Rb, Sb, Sc, Sm, Ta, Tb, Th, V, U, W) not reported by the IAEA. The analytical methodology was discussed with important sources of spectral, nuclear and fission‐product interferences. It was shown that the important components of uncertainties were the k0 factor, Q0 factor, detector efficiency, mass and counting statistics. The methodology was validated by analysing the IAEA‐S7 reference material. 相似文献
23.
Wafa Abouchami Stephen J. G. Galer Tristan J. Horner Mark Rehkämper Frank Wombacher Zichen Xue Myriam Lambelet Melanie Gault‐Ringold Claudine H. Stirling Maria Schönbächler Alyssa E. Shiel Dominique Weis Philip F. Holdship 《Geostandards and Geoanalytical Research》2013,37(1):5-17
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
24.
Molybdenum Mass Fractions and Isotopic Compositions of International Geological Reference Materials
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Pei‐Pei Zhao Jie Li Le Zhang Zhi‐Bing Wang De‐Xin Kong Jin‐Long Ma Gang‐Jian Wei Ji‐Feng Xu 《Geostandards and Geoanalytical Research》2016,40(2):217-226
The double‐spike method with multi‐collector inductively coupled plasma‐mass spectrometry was used to measure the Mo mass fractions and isotopic compositions of a set of geological reference materials including the mineral molybdenite, seawater, coral, as well as igneous and sedimentary rocks. The long‐term reproducibility of the Mo isotopic measurements, based on two‐year analyses of NIST SRM 3134 reference solutions and seawater samples, was ≤ 0.07‰ (two standard deviations, 2s, n = 167) for δ98/95Mo. Accuracy was evaluated by analyses of Atlantic seawater, which yielded a mean δ98/95Mo of 2.03 ± 0.06‰ (2s, n = 30, relative to NIST SRM 3134 = 0‰) and mass fraction of 0.0104 ± 0.0006 μg g?1 (2s, n = 30), which is indistinguishable from seawater samples taken world‐wide and measured in other laboratories. The comprehensive data set presented in this study serves as a reference for quality assurance and interlaboratory comparison of high‐precision Mo mass fractions and isotopic compositions. 相似文献
25.
Precise and Accurate Doping of Nanoporous Silica Gel for the Synthesis of Trace Element Microanalytical Reference Materials
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William O. Nachlas 《Geostandards and Geoanalytical Research》2016,40(4):505-516
This study presents an experimental procedure to fabricate high‐purity silica glass containing a selected element at a specified mass fraction. The procedure was used to prepare glasses doped with trace‐level mass fractions of Ti with the goal of improving analytical confidence when measuring trace elements in quartz. Systematic tests were performed to determine the ideal conditions and procedures for doping nanoporous silica gel with the highest efficiency of dopant recovery. Silica gel was cleaned in concentrated HCl, immersed in a non‐polar doping medium at a controlled pH and doped with precise quantities of ICP‐MS standard solution. Using liquids composed of longer chain molecules as the doping medium diminishes recovery, suggesting that large molecules could obstruct nanopores to inhibit capillary uptake of the dopant. A control experiment using crystalline quartz reinforced the effectiveness of nanoporous silica gel for doping with trace‐level precision. Layered aggregates of silica gel doped with different Ti mass fractions were hot‐pressed to create multi‐layered reference materials that were analysed with multiple techniques at a variety of spatial scales. Analyses at the intra‐grain scale (cathodoluminescence scanning electron microscopy, electron probe microanalysis), at the single grain scale (SIMS), at the sample layer scale (EPMA, laser ablation‐ICP‐MS) and at the bulk scale (ICP‐OES) demonstrated acceptable homogeneity at sample volumes characteristic of most microanalysis techniques and show that nanoporous silica gel holds promise as a highly retentive doping substrate for preparing reference materials for laser‐, electron‐ and ion‐beam microanalysis. 相似文献
26.
Elimination of Interferences in the Determination of Palladium,Platinum and Rhodium Mass Fractions in Moss Samples using ICP‐MS/MS
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Terhi Suoranta Syed N. H. Bokhari Thomas Meisel Matti Niemelä Paavo Perämäki 《Geostandards and Geoanalytical Research》2016,40(4):559-569
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
27.
Qiaoyun Wang Akio Makishima Eizo Nakamura 《Geostandards and Geoanalytical Research》2010,34(2):175-183
A method to determine F and Cl in silicate materials by employing pyrohydrolysis and ion chromatography (IC) is described. Pyrohydrolysis involved mixing a pulverised sample (∼ 40 mg) with V2O5 (∼ 160 mg) and heating to 1100 °C under a wet oxygen flow in a quartz tube. Recovery yields of F and Cl were ∼ 97% using a NaF + NaCl standard solution. Detection limits of the pyrohydrolysis-IC method for silicate samples were 0.36 and 0.69 μg g-1 for F and Cl, respectively. Fluorine and Cl concentrations were determined in the reference materials JB-2, JB-3 and JA-1 from the GSJ; BCR-2, BHVO-1, BHVO-2, AGV-1 and AGV-2 from the USGS; and NIST SRM 610, 612 and 614 glasses. Precisions (RSD) for determinations of F were 1–13% (except NIST SRM 614) and 2–19% for Cl, and were dependent on the concentration and blank correction. Most results obtained in this study were in good agreement with those of previous studies. In comparison, the Na2CO3 + ZnO fusion method at 900 °C showed that the yields of F and Cl by alkaline fusion systematically decreased with fusion duration time. The yields were 84% and 83% for JB-3, inferring that F and Cl were lost in this alkaline fusion. 相似文献
28.
Michael A.W. Marks Roberta L. Rudnick Thomas Ludwig Horst Marschall Thomas Zack Ralf Halama William F. McDonough Detlef Rost Thomas Wenzel Edward P. Vicenzi Ivan P. Savov Rainer Altherr Gregor Markl 《Geostandards and Geoanalytical Research》2008,32(3):295-310
Two large pegmatitic crystals of sodic pyroxene (aegirine) and sodic amphibole (arfvedsonite) from the agpaitic igneous Ilímaussaq Complex, south Greenland were found to be suitable as reference materials for in situ Li isotope determinations. Lithium concentrations determined by SIMS and micro‐drilled material analysed by MC‐ICP‐MS generally agreed within analytical uncertainty. The arfvedsonite crystal was homogeneous with [Li] = 639 ± 51 μg g?1 (2s, n = 69, MC‐ICP‐MS and SIMS results). The aegirine crystal shows strongly developed sector zoning, which is a common feature of aegirines. Using qualitative element mapping techniques (EPMA), the homogeneous core of the crystal was easily distinguished from the outermost sectors of the crystals. The core had a mean [Li] of 47.6 ± 3.6 μg g?1 (2s, n = 33) as determined by SIMS. The seven micro‐drilled regions measured by solution MC‐ICP‐MS returned slightly lower concentrations (41–46 μg g?1), but still overlap with the SIMS data within uncertainty. Based on MC‐ICP‐MS and SIMS analyses, the variation in δ7Li was about 1‰ in each of the two crystals, which is smaller than that in widely used glass reference materials, making these two samples suitable to serve as reference materials. There was, however, a significant offset between the results of MC‐ICP‐MS and SIMS. The latter deviated from the MC‐ICP‐MS results by ?6.0 ± 1.9‰ (2s) for the amphibole and by ?3.9 ± 1.9‰ (2s) for the aegirine. This indicates the presence of a significant matrix effect in SIMS determinations of Li isotopes for amphibole and pyroxene relative to the basalt glasses used for calibration. Based on the MC‐ICP‐MS results, mean δ7Li values of +0.7 ± 1.2‰ (2s, n = 10) for the arfvedsonite crystal and of ?3.7 ± 1.2‰ (2s, n = 7) for the core of the aegirine crystal were calculated. Adopting these values, SIMS users can correct for the specific IMF (instrumental mass fractionation) of the ion probe used. We propose that these two crystals serve as reference materials for in situ Li isotope determinations by SIMS and pieces of these two crystals are available from the first author upon request. 相似文献
29.
Zhizhong Cheng Mei Liu Hongku Huang Tiexin Gu Weidong Yan Hongli Wen 《Geostandards and Geoanalytical Research》2015,39(2):221-232
The preparation and characterisation of three nickel ores and two nickel concentrate certified reference materials are described in this paper. The samples of nickel ore and nickel concentrate were collected from the Hongqiling nickel deposit in Jilin province. The raw materials were crushed and passed through a 2.0‐mm sieve. The rough samples were then ground for 48 hr in a high‐alumina ball mill to a final size of < 0.074 mm. Homogeneity of the samples was tested by X‐ray fluorescence spectrometry (WD‐XRF) and inductively coupled plasma‐atomic emission spectrometry (ICP‐AES). The relative standard deviations (RSD) of results on mass fraction measurements by WD‐XRF were < 1.0% m/m for eighteen components. F‐tests showed that all five samples were homogeneous. Nineteen laboratories contributed with measurement results (2127 in total) for the certification of mass fractions for twenty‐three elements and compounds. Twenty‐three components in the nickel ores and twenty components in the nickel concentrates were characterised as certified values, while the Ni mass fractions ranges from 0.1 to 9.02% m/m in these certified reference materials. These five samples were approved as national certified reference materials by the National Organisation of Reference Materials of China in 2012. 相似文献
30.
Characterisation of Apatites as Potential Uranium Reference Materials for Fission‐track Dating by LA‐ICP‐MS
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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