Incorporation of U, Pb and rare earth elements in calcite through crystallisation from amorphous calcium carbonate; Simple preparation of reference materials for microanalysis

Miyajima, Yusuke*; Saito, Ayaka*; Kagi, Hiroyuki*; Yokoyama, Tatsunori; Takahashi, Yoshio*; Hirata, Takafumi*

Geostandards and Geoanalytical Research, 45(1), p.189 - 205, 2021/03

https://doi.org/10.1111/ggr.12367

Uncertainty for elemental and isotopic analyses of calcite by LA-ICP-MS is largely controlled by the homogeneity of the reference materials (RMs) used for normalization and validation. In order to produce calcite RMs with homogeneous elemental and isotopic compositions, we incorporated elements including U, Pb, and rare earth elements into calcite through heat- and pressure-induced crystallization from amorphous calcium carbonate that was precipitated from element-doped reagent solution. X-ray absorption spectra showed that U was present as U(VI) in the synthesized calcite, probably with a different local structure from that of aqueous uranyl ions. The uptake rate of U by our calcite was higher in comparison to synthetic calcite of previous studies. Variations of element mass fractions in the calcite were better than 12% 2RSD, mostly within 7%. The Pb/Pb ratio in the calcite showed 1% variations, while the U/Pb ratio showed 3-24% variations depending on element mass fractions. Using the synthetic calcite as primary RMs, we could date a natural calcite RM, WC-1, with analytical uncertainty as low as 3%. The method presented can be useful to produce calcite with controlled and homogeneous element mass fractions, and is a promising alternative to natural calcite RMs for U-Pb geochronology.

Multi-element determination in soil and sediment reference materials by neutron-induced prompt -ray analysis using -standardization

Matsue, Hideaki; Yonezawa, Chushiro

Bunseki Kagaku, 53(7), p.749 - 751, 2004/07

https://doi.org/10.2116/bunsekikagaku.53.749

Multi-element determination in reference materials of soils (JASC401, JASC411) and sediments (NMIJ CRM 7302-a, NMIJ CRM 7303-a), which were prepared at the Japan Society for Analytical Chemistry and the National Institute of Advanced Industrial Science and Technology of the National Metrology Institute of Japan, respectively, has been carried out by neutron-induced prompt -ray analysis (PGA) using standard addition and -standardization methods. Firstly, absolute Ti concentrations in the samples were determined accurately by the standard addition method. Secondly, relative multi-element concentrations were determined by the -standardization method. Finally, absolute multi-element concentrations were obtained by normalizing the relative multi-element concentrations with the absolute Ti concentration in the samples. The 15 elements such as H, B, Na, Si, S, Cl, K, Ca, Ti Cr, Mn, Fe, Cd, Sm and Gd were determined by the -PGA. Analytical results of these reference materials agreed with the certified or reference values within about 10%.

Preparation and Certification of a Uranium Isotope Certified Reference Material JAERI-U5

;

JAERI-M 82-053, 33 Pages, 1982/06

JAERI-M-82-053.pdf:0.97MB

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