Determination of the REE in Geological Reference Materials DTS-1 (Dunite) and PCC-1 (Peridotite) by Ultrasonic and Microconcentric Desolvating Nebulisation ICP-MS

Inductively coupled plasma-mass spectrometry is well suited for the precise, accurate and rapid determination of rare earth elements in most geological samples. However, determination of rare earth elements in certain mantle-derived materials, without applying preconcentration techniques, remains problematical due to low natural concentrations (generally < 1 ng g⁻¹). Consequently, USGS reference materials DTS-1 (a dunite) and PCC-1 (a partially serpentinized harzburgite) have only suggested rather than recommended values for the rare earth elements in reference material compilations. We compared results obtained using two ICP-MS instruments: a U-5000AT ultrasonic nebuliser coupled to a PQ2+ quadrupole ICP-MS and an ELEMENT sector field ICP-MS equipped with a MCN-6000 microconcentric desolvating nebuliser, with the suggested literature values for these two reference materials. Precision and accuracy of analytical methods employed by both instruments were demonstrated by excellent relative standard deviations (< 2%) and inter-laboratory agreement (< 5%) for numerous analyses of BHVO-1 and BIR-1, which are well established with rare earth elements contents at the μg g⁻¹ level. Repeat analyses of DTS-1 and PCC-1 at each laboratory indicate that each method is generally precise to better than 5% at sub-g g⁻¹ levels. Furthermore, values from both instruments generally agree to within 10%. Our DTS-1 and PCC-1 values agree reasonably well with selected data reported in the literature (except for Ce and Sm in DTS-1) but exhibit poorer agreement with reported compilation values. With the demonstrated level of precision and accuracy, we contend that these new values for DTS-1 and PCC-1, generated by two different instruments, are the best estimates of the true whole-rock composition of these samples reported to date.     

SiO2 precipitation in olivine: ATEM investigation of two dunites annealed at 300 MPa in hydrous conditions

Two natural dunites were annealed at pressure P=300 MPa, temperature T=1373, 1473 and 1573 K, and fO₂ within the stability field of olivine. The starting materials contained small amounts of hydroxyls in the form of minor phases of hydrated minerals, which released an aqueous phase during the experiments. A detailed analytical transmission electron microscopy (ATEM) investigation of these materials revealed that small quantities of two types of silica-rich glass formed during heat treatment. The first type of glass, found at triple junctions as rare partially crystallized glass pockets, results from melting dehydration reactions involving the hydrous phases. The second type of glass is found as pure silica precipitates (0.1–0.5 μm in size, for a total of a few 0.1 vol%) within the olivine grains of specimens heated to ≥1473 K. From considerations of the kinetics of the precipitation at 1473 K, we interpret this silica precipitation as resulting from the condensation of olivine metallic vacancies promoted by increasing fluid fugacities during the runs. Our observations, thus, demonstrate that metastable silica can precipitate in olivine from dunites experiencing rapid changes in their thermodynamical environment.     

Controlled sources for shear-wave surveys in mines

The ability to analyse shear-wave anisotropy in a mine environment is greatly aided by using multiple source orientations of a reproducible, impulsive shear-wave source. The analysis of what is probably the first controlled source shear-wave experiment in a mine environment demonstrates clearly that shear-wave polarizations and time delays between split shear-wave arrivals are reliably measured because of the use of multiple source orientations rather than a single shear-wave source. Reliability is further aided by modelling the shear-wave source radiation pattern, which allows for the unequivocal discrimination between seismic raypaths where shear-wave splitting did and did not occur. The analysis also demonstrates the great importance of high reproducibility of the seismic source for the use of shear waves in time-lapse surveys to monitor changes in a rockmass.     

A Study of Chloride Aerosol, Total Aerosol and Ice Nuclei in the Indian Regions

--Atmospheric aerosols were sampled from aircraft at various levels over Rihand in northern India during the monsoon season of 1974 and at surface levels at Calcutta, Delhi, Varanasi and Jodhpur during different seasons of 1970 and 1971. Millipore filter assembly was used for this purpose. Chloride nuclei, total aerosol and ice nuclei concentrations were evaluated from millipore filters. At Rihand/Varanasi, during the monsoon, the chloride size spectrum was broader and the distribution bimodal at cloud base level while the spectra were narrower and the distributions unimodal at other levels. At Rihand, chloride mass and larger giant chloride number were considerably higher, total aerosol higher while ice nuclei concentrations were lower on the days with moderate rain as compared to those with light rain. Calcutta (maritime) showed maximum while Varanasi (well-inland) showed minimum chloride number concentrations. As compared with Calcutta, Delhi (continental) had lower chloride and total aerosol, and markedly higher ice nuclei concentrations. Varanasi (high rainfall region) showed all the values, except for small-sized chlorides, notably higher with respect to Jodhpur (low rainfall region). Ice nuclei concentration was lowest in winter and highest in summer at Delhi. Variations of the aerosols during different parts of the day/night are also discussed.     

Terrestrial age measurements using natural thermoluminescence of a drained zone under the fusion crust of Antarctic ordinary chondrites

Abstract— Miono et al. (1990) and Miono and Nakanishi (1994) have proposed that the build‐up of natural thermoluminescence (TL) in a drained layer directly below the meteorite fusion crust can be used to determine terrestrial ages of meteorites in the 40 to 200 ka range. We have measured the natural TL of the drained layer of 15 meteorites. The data indicate that this technique could be used to determine terrestrial ages of meteorites with ages <200 ka, after which TL equilibrium is reached. Comparison of TL build‐up with terrestrial ages for a suite of Antarctic meteorites suggests that the meteorites have been exposed to temperatures of 0 to 5 °C. The close correspondence between natural TL levels and surface exposure TL growth curves suggest that Allan Hills meteorites with ages <200 ka have spent a significant portion of their terrestrial history exposed on the ice surface, rather than being buried in the ice sheet. The technique is, however, sensitive to thermal history; and, for Antarctic meteorites with terrestrial ages <200 ka, natural TL of the drained zone largely reflects exposure on the ice surface.