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1.
Sphalerite (ZnS) is an abundant ore mineral and an important carrier of elements such as Ge, Ga and In used in high‐technology applications. In situ measurements of trace elements in natural sphalerite samples using LA‐ICP‐MS are hampered by a lack of homogenous matrix‐matched sulfide reference materials available for calibration. The preparation of the MUL‐ZnS1 calibration material containing the trace elements V, Cr, Mn, Co, Ni, Cu, Ga, Ge, As, Se, Mo, Ag, Cd, In, Sn, Sb, Tl and Pb besides Zn, Fe and S is reported. Commercially available ZnS, FeS, CdS products were used as the major components, whereas the trace elements were added by doping with single‐element ICP‐MS standard solutions and natural mineral powders. The resulting powder mixture was pressed to pellets and sintered at 400 °C for 100 h using argon as an inert gas. To confirm the homogeneity of major and trace element distributions within the MUL‐ZnS1 calibration material, measurements were performed using EPMA, solution ICP‐MS, ICP‐OES and LA‐ICP‐MS. The results show that MUL‐ZnS‐1 is an appropriate material for calibrating trace element determination in sphalerite using LA‐ICP‐MS.  相似文献   

2.
An efficient, clean procedure for the measurement of element mass fractions in bulk rock nanoparticulate pressed powder pellets (PPPs) by 193 nm laser ablation ICP‐MS is presented. Samples were pulverised by wet milling and pelletised with microcrystalline cellulose as a binder, allowing non‐cohesive materials such as quartz or ceramics to be processed. The LA‐ICP‐MS PPP analytical procedure was optimised and evaluated using six different geological reference materials (JP‐1, UB‐N, BCR‐2, GSP‐2, OKUM and MUH‐1), with rigorous procedural blank quantification employing synthetic quartz. Measurement trueness of the procedure was equivalent to that achieved by solution ICP‐MS and LA‐ICP‐MS analysis of glass. The measurement repeatability was as low as 0.5–2% (1s, n = 6) and, accordingly, PPP homogeneity could be demonstrated. Calibration based on the reference glasses NIST SRM 610, NIST SRM 612, BCR‐2G and GSD‐1G revealed matrix effects for glass and PPP measurement with NIST SRM 61×; using basalt glasses eliminated this problem. Most significantly, trace elements not commonly measured (flux elements Li, B; chalcophile elements As, Sb, Tl, In, Bi) could be quantified. The PPP‐LA‐ICP‐MS method overcomes common problems and limitations in analytical geochemistry and thus represents an efficient and accurate alternative for bulk rock analysis.  相似文献   

3.
Three synthetic reference glasses were prepared by directly fusing and stirring 3.8 kg of high‐purity oxide powders to provide reference materials for microanalytical work. These glasses have andesitic major compositions and are doped with fifty‐four trace elements in nearly identical abundance (500, 50, 5 µg g?1) using oxide powders or element solutions, and are named ARM‐1, 2 and 3, respectively. We further document that sector‐field (SF) ICP‐MS (Element 2 or Element XR) is capable of sweeping seventy‐seven isotopes (from 7Li to 238U, a total of sixty‐eight elements) in 1 s and, thus, is able to quantify up to sixty‐eight elements by laser sampling. Micro‐ and bulk analyses indicate that the glasses are homogeneous with respect to major and trace elements. This paper provides preliminary data for the ARM glasses using a variety of analytical techniques (EPMA, XRF, ICP‐OES, ICP‐MS, LA‐Q‐ICP‐MS and LA‐SF‐ICP‐MS) performed in ten laboratories. Discrepancies in the data of V, Cr, Ni and Tl exist, mainly caused by analytical limitations. Preliminary reference and information values for fifty‐six elements were calculated with uncertainties [2 relative standard error (RSE)] estimated in the range of 1–20%.  相似文献   

4.
Microanalysis of native gold specimens has been hampered by the lack of a suitable reference material (RM) known to be sufficiently homogeneous at the scale of microanalytical sampling. The suitability of gold reference material AuRM2 for microanalysis was assessed. This RM was created for bulk analysis of refined gold and was only certified for homogeneity at the bulk scale. However, it contains trace elements in appropriate mass fraction ranges for analysis of native gold. This study was not intended to provide alternative mass fractions from the original certified values, only to assess its suitability for microanalytical methods. Micro‐scale (~ 3.4 μg sample mass) heterogeneity was calculated from measurement repeatability of LA‐ICP‐MS analyses of AuRM2 by factoring in signal (represented by counting statistics) and instrument set‐up‐specific variability (determined using measurement variability of a reference material known to be homogeneous). Elements determined to be homogeneous or to have minor heterogeneity (< 10% calculated heterogeneity RSD) are Mg, Al, Ti, Fe, Ni, Cu, Zn, Se, Rh, Sn, Sb, Pt and Pb. Elements with moderate heterogeneity (10–20% heterogeneity RSD) are: Mn, As, Pd, Te and Bi. Correlation of element mass fractions indicates that micro‐scale inclusions of chalcophile‐rich phases along grain boundaries may be responsible for some of the chemical heterogeneity. However, the level of heterogeneity is statistically negligible compared with the ranges of chemical signatures observed in sample populations of native gold. Therefore, AuRM2 is shown to be sufficiently homogenous at a micro‐scale for use as a RM for microanalysis of native gold.  相似文献   

5.
Seven ilmenite (FeTiO3) megacrysts derived from alnöite pipes (Island of Malaita, Solomon Islands) were characterised for their major and trace element compositions in relation to their potential use as secondary reference materials for in situ microanalysis. Abundances of thirteen trace elements obtained by laser ablation ICP‐MS analyses (using the NIST SRM 610 glass reference material) were compared with those determined by solution‐mode ICP‐MS measurements, and these indicated good agreement for most elements. The accuracy of the LA‐ICP‐MS protocol employed here was also assessed by repeated analysis of MPI‐DING international glass reference materials ML3B‐G and KL2‐G. Several of the Malaitan ilmenite megacrysts exhibited discrepancies between laser ablation and solution‐mode ICP‐MS analyses, primarily attributed to the presence of a titano‐magnetite exsolution phase (at the grain boundaries), which were incorporated solely in the solution‐mode runs. Element abundances obtained by LA‐ICP‐MS for three of the ilmenite megacrysts (CRN63E, CRN63H and CRN63K) investigated here had RSD (2s) values of < 20% and therefore can be considered as working values for reference purposes during routine LA‐ICP‐MS analyses of ilmenite.  相似文献   

6.
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   

7.
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   

8.
Silicon is a beneficial element for many plants and is deposited in plant tissue as amorphous bio‐opal called phytoliths. The biochemical processes of silicon uptake and precipitation induce isotope fractionation: the mass‐dependent shift in the relative abundances of the stable isotopes of silicon. At the bulk scale, δ30Si ratios span from ?2 to +6‰. To further constrain these variations in situ, at the scale of individual phytolith fragments, we used femtosecond laser ablation multi‐collector inductively coupled plasma‐mass spectrometry (fsLA‐MC‐ICP‐MS). A variety of phytoliths from grasses, trees and ferns were prepared from plant tissue or extracted from soil. Good agreement between phytolith δ30Si ratios obtained by bulk solution MC‐ICP‐MS analysis and in situ isotope ratios from fsLA‐MC‐ICP‐MS validates the method. Bulk solution analyses result in at least twofold better precision for δ30Si (2s on reference materials ≤ 0.11‰) over that found for the means of in situ analyses (2s typically ≤ 0.24‰). We find that bushgrass, common reed and horsetail show large internal variations up to 2‰ in δ30Si, reflecting the various pathways of silicon from soil to deposition. Femtosecond laser ablation provides a means to identify the underlying processes involved in the formation of phytoliths using silicon isotope ratios.  相似文献   

9.
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   

10.
Zircon megacrysts from the Mud Tank carbonatite, Australia, are being used in many laboratories as a reference material for LA‐ICP‐MS U‐Pb dating and trace element measurement, and LA‐MC‐ICP‐MS determination of Hf isotopes. We summarise a database of > 10000 analyses of Mud Tank zircon (MTZ), collected from 2000 to 2018 during its use as a secondary reference material for simultaneous U‐Pb and trace element analysis, and for Hf‐isotope analysis. Trace element mass fractions are highest in dark red‐brown stones and lowest in colourless and gem‐quality ones. Individual unzoned grains can be chemically homogeneous, while significant variations in trace element mass fraction are associated with oscillatory zoning. Chondrite‐normalised trace element patterns are essentially parallel over large mass fraction ranges. A Concordia age of 731.0 ± 0.2 Ma (2s, n = 2272) is taken as the age of crystallisation. Some grains show lower concordant to mildly discordant ages, probably reflecting minor Pb loss associated with cooling and the Alice Springs Orogeny (450–300 Ma). Our weighted mean 176Hf/177Hf is 0.282523 ± 10 (2s, n = 9350); the uncertainties on this ratio reflect some heterogeneity, mainly between grains. A few analyses suggest that colourless grains have generally lower 176Hf/177Hf. MTZ is a useful secondary reference material for U‐Pb and Hf‐isotope analysis, but individual grains need to be carefully selected using CL imaging and tested for homogeneity, and ideally should be standardised by solution analysis.  相似文献   

11.
Partition coefficients between olivine and melt at upper mantle conditions, 3 to 14 GPa, have been determined for 27 trace elements (Li, Be, B, Na, Mg, Al, Si, P, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Rb, Sr, Y, Zr, Cs, Ba, La and Ce) using secondary-ion mass-spectrometry (SIMS) and electron-probe microanalysis (EPMA). The general pattern of olivine/melt partitioning on Onuma diagrams resembles those reported previously for natural systems. This agreement strongly supports the argument that partitioning is under structural control of olivine even at high pressure. The partition coefficients for mono- and tri-valent cations show significant pressure dependence, both becoming larger with pressure, and are strongly correlated with coupled substitution into cation sites in the olivine structure. The dominant type of trace element substitution for mono- and tri-valent cations into olivine changes gradually from (Si, Mg)↔(Al, Cr) at low pressure to (Si, Mg)↔(Al, Al) and (Mg, Mg)↔(Na, Al) at high pressure. The change in substitution type results in an increase in partition coefficients of Al and Na with pressure. An inverse correlation between the partition coefficients for divalent cations and pressure has been observed, especially for Ni, Co and Fe. The order of decreasing rate of partition coefficient with pressure correlates to strength of crystal field effect of the cation. The pressure dependence of olivine/melt partitioning can be attributed to the compression of cation polyhedra induced by pressure and the compensation of electrostatic valence by cation substitution. Received: March 6, 1997 / Revised, accepted: March 12, 1998  相似文献   

12.
The influence of non‐spectral matrix effects on the determination of twenty‐two trace elements (Rb, Sr, Y, Cs, Ba, lanthanides, Pb, Th and U) in rock samples using ICP‐MS was investigated. Three types of multi‐element solutions were synthesised containing the twenty‐two trace elements, In, Tl and ten major rock‐forming elements with varying mass fractions mimicking the compositions of basalt, peridotite and dolomite. The synthetic solutions were conditioned to have dilution factors (DF) of 1000–10000. The extent of sensitivity suppression relative to the DF = 10000 solution became more significant for smaller DF solutions, which was not constant across different elements in a single solution but displayed general dependence on m/z. This indicates that at least two internal standards (e.g., In and Tl) are required for the correction of sensitivity variation. On the basis of the results, a new isotope dilution‐internal standardisation method for the determination of twenty‐two trace elements with ICP‐MS was developed, in which the sensitivity variation was corrected by monitoring two enriched isotopes, 113In and 203Tl. This method, coupled with the quantitative correction of interference from oxides and hydroxides, achieved precise determination of twenty‐two trace elements in some rock reference materials with reproducibilities of ±2% for basaltic to andesitic samples.  相似文献   

13.
东昆仑造山带蛇绿岩矿物学特征及其岩石成因讨论   总被引：3，自引：0，他引：3  
首次对东昆仑复合造山带不同时代蛇绿岩主要造岩矿物橄榄石、辉石、斜长石进行了系统的矿物化学研究 ,查明了不同蛇绿岩带在矿物成分上的差异 ,对清水泉蛇绿岩带和布青山蛇绿岩带单斜辉石、斜方辉石、斜长石进行了矿物稀土、微量元素的研究 ,阐明了矿物稀土、微量元素与全岩稀土、微量元素的关系 ,证明了在以辉石和橄榄石为主的橄辉岩中 ,单斜辉石的稀土元素基本上代表了全岩的稀土元素。根据地幔岩石中矿物成分特征 ,对不同蛇绿岩带地幔类型进行了讨论 ,并根据实测的辉石、斜长石分配系数 ,确定了清水泉蛇绿岩带玄武岩的部分熔融定量模拟  相似文献   

14.
Fused glass prepared without the addition of a flux is generally more homogeneous than a pressed powder pellet and thus ideal for analysis of bulk samples by LA‐ICP‐MS. In this work, a new glass‐making method using a boron nitride crucible was developed to prepare homogenous glass samples from silicate rock powder. The apparatus consisted of a small boron nitride vessel with net volume of about 34 mm3 and two molybdenum strips. Applying the summed metal oxide normalisation technique, both major and trace element contents in the fused glass were measured by LA‐ICP‐MS. Analyses of five geochemical reference materials (spanning the compositional range basalt–andesite–rhyolite) indicated that the measured SiO2, Al2O3 and P2O5 contents matched the preferred values to within 5%, and the other major elements generally matched the preferred values to within 8%. Except for the transition metals, the measured trace element contents generally matched the preferred values to within 10%. Compared with the iridium heater method developed by Stoll et al. (2008), element volatilisation during high‐temperature melting was effectively suppressed in our method, but metal segregation caused by reduction of BN may cause loss of Cr, Ni and Cu. Although analysis with a large spot size has the advantage of improving counting statistics, matrix effects induced by mass loading of the ICP may hamper the accurate determination of some elements.  相似文献   

15.
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   

16.
Electron probe microanalyser measurements of trace elements with high accuracy are challenging. Accurate Al measurements in olivine are required to calibrate SIMS implant reference materials for measurement of Al in the solar wind. We adopt a combined EPMA/SIMS approach that is useful for producing SIMS reference materials as well as for EPMA at the ~ 100 µg g?1 level. Even for mounts not polished with alumina photoelectron spectroscopy shows high levels of Al surface contamination. In order to minimise electron beam current density, a rastered 50 × 100 µm electron beam was adequate and minimised sensitivity to small Al‐rich contaminants. Reproducible analyses of eleven SIMS‐cleaned spots on San Carlos olivine agreed at 69.3 ± 1.0 µg g?1. The known Al mass fraction was used to calibrate an Al implant into San Carlos. Accurate measurements of Al were made for olivines in the pallasites: Imilac, Eagle Station and Springwater. Our focus was on Al in olivine, but our technique could be refined to give accurate electron probe measurements for other contamination‐sensitive trace elements. For solar wind, it is projected that the Al/Mg abundance ratio can be determined to 6%, a factor of 2 more precise than the solar spectroscopic ratio.  相似文献   

17.
In this study, a technique for high precision in situ Fe and Mg isotope determinations by femtosecond‐laser ablation‐multi collector‐ICP‐MS (fs‐LA‐MC‐ICP‐MS) was developed. This technique was employed to determine reference values for a series of common reference glasses that may be used for external standardisation of in situ Fe and Mg isotope determinations in silicates. The analysed glasses are part of the MPI‐DING and United States Geological Survey (USGS) reference glass series, consisting of basaltic (BIR‐1G, BCR‐2G, BHVO‐2G, KL2‐G, ML3B‐G) and komatiitic (GOR128‐G and GOR132‐G) compositions. Their Fe and Mg isotope compositions were determined by in situ fs‐LA‐MC‐ICP‐MS and by conventional solution nebulisation multi‐collector ICP‐MS. We determined δ56Fe values for these glasses ranging between ‐0.04‰ and 0.10‰ (relative to IRMM‐014) and δ26Mg values ranging between ‐0.40‰ and ‐0.15‰ (relative to DSM‐3). Our fs‐LA‐MC‐ICP‐MS results for both Fe and Mg isotope compositions agreed with solution nebulisation analyses within analytical uncertainties. Furthermore, the results of three USGS reference glasses (BIR‐1G, BHVO‐2G and BCR‐2G) agreed with previous results for powdered and dissolved aliquots of the same reference materials. Measurement reproducibilities of the in situ determinations of δ56Fe and δ26Mg values were usually better than 0.12‰ and 0.13‰ (2s), respectively. We further demonstrate that our technique is a suitable tool to resolve isotopic zoning in chemically‐zoned olivine crystals. It may be used for a variety of different applications on isotopically‐zoned minerals, e.g., in magmatic or metamorphic rocks or meteorites, to unravel their formation or cooling rates.  相似文献   

18.
We present the first data on the petrology of the mantle lithosphereof the Southeastern (SE) Slave craton, Canada. These are basedon petrographic, mineralogical and geochemical studies of mantlexenoliths in Pipe 5034 of the Cambrian Gahcho Kué kimberlitecluster. Major types of mantle xenoliths include altered eclogite,coarse garnet or spinel peridotite, and deformed garnet peridotite.The peridotites belong to the low-temperature suite and formedat T=600–1300°C and P= 25–80 kbar in a thick(at least 220–250 km), cool lithosphere. The SE Slavemantle is cooler than the mantle of other Archaean cratons andthat below other terranes of the Slave craton. The thick lithosphereand the relatively cool thermal regime provide favourable conditionsfor formation and preservation of diamonds beneath the SE Slaveterrane. Similar to average Archaean mantle worldwide, the SESlave peridotite is depleted in magmaphile major elements andcontains olivine with forsterite content of 91–93·5.With respect to olivine composition and mode, all terranes ofthe Slave mantle show broadly similar compositions and are relativelyorthopyroxene-poor compared with those of the Kaapvaal and Siberiancratons. The SE Slave spinel peridotite is poorer in Al, Caand Fe, and richer in Mg than deeper garnet peridotite. Thegreater chemical depletion of the shallow upper mantle is typicalof all terranes of the Slave craton and may be common for thesubcontinental lithospheric peridotitic mantle in general. Peridotiticxenoliths of the SE Slave craton were impregnated by kimberliticfluids that caused late-stage recrystallization of primary clinopyroxene,spinel, olivine and spinel-facies orthopyroxene, and formationof interstitial clinopyroxene. This kimberlite-related recrystallizationdepleted primary pyroxenes and spinel in Al. The kimberliticfluid was oxidizing, Ti-, Fe- and K-rich, and Na-poor, and introducedserpentine, chlorite, phlogopite and spinel into peridotitesat P < 35 kbar. KEY WORDS: kimberlite xenolith; lithosphere; mantle terrane; chemical zoning; thermobarometry; Slave craton  相似文献   

19.
A rapid sample preparation procedure is described to determine trace element compositions of peridotites using LA‐ICP‐MS. Peridotite powders were fused with albite in a molybdenum–graphite assembly to obtain homogeneous glasses. Best conditions for the fusion procedure (heating at 1500–1550 °C for 10–15 min with a sample‐to‐flux ratio of 1:2) were constrained with melting experiments on two USGS reference materials, PCC‐1 and DTS‐2B. Mass fractions of first series transition elements, Ba and Pb, in quenched glasses of PCC‐1 and DTS‐2B are consistent with published data within 10% RSD. Three spinel peridotite xenoliths from eastern China were analysed following both our method and conventional solution ICP‐MS. Compared with solution ICP‐MS, the relative deviations of our method for most elements were within 10%, while for the REE, Ta, Pb, Th and U, the relative deviations were within 20%. In particular, volatile elements (e.g., Pb and Zn) are retained in the glass. Compared with conventional wet chemistry digestion, our method is faster. Additional advantages are complete sample fusion, especially useful for samples with acid‐resistant minerals (spinel and rutile), and long‐term conservation of glasses allowing unlimited repeated measurements with microbeam techniques. The same approach can be used for analyses of other mantle rocks, such as eclogites and pyroxenites.  相似文献   

20.
The attractive physical and chemical properties of corundum lend to this material’s importance in both its natural and synthetic forms. However, much of the quantitative work performed on this material is plagued by unknown inaccuracy as non‐matrix‐matched reference materials are used. To conduct accurate quantitative analysis using SIMS, matrix‐specific relative sensitivity factors (RSFs) were determined for eighteen trace elements in corundum using dose‐verified ion implants. The RSF values ranged from 2.56 × 1022 to 3.29 × 1024 cm‐1 with total combined uncertainty values ranging from 7 to 10%. The RSF values, which are related to ionisation potentials, showed trends consistent with expectations for an insulating oxide. The developed values were applied to calibrate reference materials for LA‐ICP‐MS and to study other natural and synthetic corundum samples. A measurement reference material calibrated for Mg, Si, Ti, V, Fe and Ga produced consistent results over ten sessions in 4 years with relative standard deviations per trace element of 5% or less, confirming the repeatability of our process. A key finding was that calibrating LA‐ICP‐MS with NIST SRM 610 and 612 glasses to analyse corundum resulted in under‐reporting trace elements Be, Ti, V, Fe, Co, Ni and Ga compared with using matrix‐matched reference materials.  相似文献   

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