Search USGSSearch

USGS · 70147015

Characterisation of a natural quartz crystal as a reference material for microanalytical determination of Ti, Al, Li, Fe, Mn, Ga and Ge

Abstract

A natural smoky quartz crystal from Shandong province, China, was characterised by laser ablation ICP-MS, electron probe microanalysis (EPMA) and solution ICP-MS to determine the concentration of twenty-four trace and ultra trace elements. Our main focus was on Ti quantification because of the increased use of this element for titanium-in-quartz (TitaniQ) thermobarometry. Pieces of a uniform growth zone of 9 mm thickness within the quartz crystal were analysed in four different LA-ICP-MS laboratories, three EPMA laboratories and one solution-ICP-MS laboratory. The results reveal reproducible concentrations of Ti (57 ± 4 μg g -1 ), Al (154 ± 15 μg g -1 ), Li (30 ± 2 μg g -1 ), Fe (2.2 ± 0.3 μg g -1 ), Mn (0.34 ± 0.04 μg g -1 ), Ge (1.7 ± 0.2 μg g -1 ) and Ga (0.020 ± 0.002 μg g -1 ) and detectable, but less reproducible, concentrations of Be, B, Na, Cu, Zr, Sn and Pb. Concentrations of K, Ca, Sr, Mo, Ag, Sb, Ba and Au were below the limits of detection of all three techniques. The uncertainties on the average concentration determinations by multiple techniques and laboratories for Ti, Al, Li, Fe, Mn, Ga and Ge are low; hence, this quartz can serve as a reference material or a secondary reference material for microanalytical applications involving the quantification of trace elements in quartz.

Explore related subjects

Keep this discovery

Explore connections, maps & timelines

BibTeXRIS

Andreas Audetat, Dieter Garbe-Schonberg, Andreas Kronz, Thomas Pettke, Brian G. Rusk, John J. Donovan, Heather Lowers. 2014-10-23. Characterisation of a natural quartz crystal as a reference material for microanalytical determination of Ti, Al, Li, Fe, Mn, Ga and Ge. https://doi.org/10.1111/j.1751-908x.2014.00309.x

Cite the original work for its findings. Save a collection to share your selection of sources.

KEEP EXPLORING

Related USGS reports

Triple oxygen isotope compositions of isotopic reference waters: Implications for VSMOW-Scale and VSMOW-SLAP-Scale Δ′¹⁷O calibration

Triple oxygen isotope ratios of waters are commonly reported on the VSMOW–SLAP scale, whereas comparison with theoretical calculations and assessment of instrumental scale distortion require accurate constraints on the measured isotopic compositions of the primary isotopic reference materials (iRMs) themselves. In particular, the measured δ 17 O VSMOW and Δ ′ 17 O VSMOW values for SLAP and its substitute, SLAP2, remain insufficiently constrained and reported values differ among laboratories. Here, we measured triple oxygen isotope ratios for two primary iRMs (VSMOW and SLAP) and twelve secondary iRMs (VSMOW2, SLAP2, GISP, GRESP, USGS45, USGS46, USGS46a, USGS47, USGS48, USGS49, USGS50 and USGS53) using BrF 5 fluorination and dual-inlet isotope-ratio mass spectrometry. For SLAP, we obtained δ 18 O VSMOW = -55.50 ± 0.15‰ and δ 17 O VSMOW = -29.66 ± 0.08‰, giving Δ ′ 17 O VSMOW = 34 ± 6 per meg (all expanded uncertainties, k = 2). The corresponding values for SLAP2 agree within uncertainty. When expressed on the conventional VSMOW–SLAP scale, our Δ ′ 17 O VSMOW–SLAP values for all secondary iRMs with available literature values agree with previously published values within uncertainty, confirming interlaboratory comparability on that scale. In contrast, waters with low δ 18 O values, Δ ′ 17 O VSMOW values are systematically higher than the corresponding Δ ′ 17 O VSMOW–SLAP values. These results further suggest that accurate determination of the VSMOW-scale isotopic composition of SLAP and/or SLAP2 across laboratories is essential, particularly for low- δ 18 O samples, for which the difference between VSMOW-scale and VSMOW–SLAP-scale Δ ′ 17 O values becomes large, and for meaningful comparison between measured data and theoretical calculations.

Geostandards and Geoanalytical Research

RioM-1: A new calcite reference material for U-Pb LA-ICP-MS geochronology

Determining absolute ages of carbonate diagenesis, faulting, fossil formation, speleothem growth, carbonate-hosted hydrocarbon deposits, vein mineralisation and hydrothermal alteration has become increasingly accessible through LA-ICP-MS U-Pb dating of calcite, complementing traditional isotope dilution methods still applicable to certain materials (e.g., speleothems via micro-drilling). However, well-calibrated reference materials for LA-ICP-MS calcite geochronology remain scarce. Here, we characterise the Rio Maior calcite, designated ‘RioM-1’, as a potential reference material for U-Pb dating by LA-ICP-MS. Fragments (0.1 to 1 cm 3 ) from a single scalenohedral crystal were analysed by ID-TIMS (U-Pb), LA-ICP-MS (U-Pb and 87 Sr/ 86 Sr), and SIMS (O isotopes). RioM-1 displays high U mass fraction and low, though variable, proportions of common Pb. Combined ID-TIMS analyses from two independent laboratories yielded a Tera-Wasserburg lower intercept date of 63.93 ± 0.11 Ma (2 s , MSWD = 1.3, n = 16). LA-ICP-MS U-Pb data from three independent laboratories are concordant with the TIMS age, producing a pooled date of 64.10 ± 0.12/1.2 Ma (2 s , MSWD = 7.7, n = 708) and an initial 207 Pb/ 206 Pb ratio of 0.85 ± 0.01. Other calcite reference materials, when normalised to RioM-1, yielded dates within uncertainty of their published values. SIMS measurements returned a mean 18 O/ 16 O of 0.002044450 ± 181 (1 s ) and δ 18 O SMOW of 19.57 ± 0.92‰ (1 s ), while LA-ICP-MS strontium isotope measurement yielded a mean 87 Sr/ 86 Sr of 0.708177 ± 9 (2 s ).

Geostandards and Geoanalytical Research

Using peak geometry and shifts in the x-ray spectrum of carbon from electron probe microanalysis to determine thermal maturity of organic matter

During the burial of mudstones, the associated organic matter undergoes gradual thermal maturation, a key process that can influence the reactivity of organic matter during catagenesis, the formation of hydrocarbon deposits and the chemical weathering of mudstones. Conventional methods for assessing the thermal maturity of organic matter often fail to reflect the geochemical heterogeneity between individual organic phases in mudstone samples. Here, we report an alternative, non-destructive, surficial and micro-scale (analytical spot size of ~ 300 nm with about 4 μm diffusion depth for micrometre-size organic grains) method to evaluate the thermal maturity of organic matter in mudstones using the carbon K α X-ray spectrum measured by field emission-electron probe microanalyser (FE-EPMA). Using this method, we observed correlations between parameter values derived from FE-EPMA spectra, including the peak position, the peak area and the intra-sample heterogeneity of these measurements, and independently measured vitrinite/solid bitumen reflectance for a suite of mudstones, representing different age, geological context and burial depth. With the increased values in peak area and position, we identified an increase in the carbon mass fraction of organic matter and the mean nominal oxidation state of carbon approaching zero. These trends, which are consistent with aromatisation and graphitisation, provide the rationale for using FE-EPMA to estimate the thermal maturity of organic matter. To explore some of these trends in more detail, we employed time-of-flight secondary ionisation mass spectrometry, X-ray photoelectron spectroscopy and optical reflectance measurements on a subset of samples.

Geostandards and Geoanalytical Research