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Quality of electron probe X-ray microanalysis determinations obtained from laboratory reference materials of the coppery alloys and basaltic glasses
Authors:Liudmila A Pavlova  
Institution:aVinogradov Institute of Geochemistry, Siberian Branch, Russian Academy of Sciences, 1А Favorsky Street, 664033 Irkutsk, Russia
Abstract:Nine coppery alloys and five basaltic glasses have been quantitatively evaluated as the reference materials to employ in electron probe X-ray microanalysis. The optimum conditions for measurements were selected considering the dependence of intensity and detection limit on the conditions of the X-ray radiation excitation and analytical signal recording. The homogeneity of basaltic glasses and coppery alloys has been examined. The dependence of electron probe X-ray microanalysis accuracy on the homogeneity of reference materials was studied in the reference materials of coppery alloys.Six data sets comprising the average concentrations, standard deviations, relative standard deviations, confidence interval and the z-score of data quality were calculated for 50 control samples: 10 alloys, 14 glasses, 2 metals, 24 minerals and oxides. The average compositions of every control sample were derived in 8–16 analyses. The measured values were corrected for matrix effects applying the original program. These series of concentrations have been compared with each other and with the certified/recommended values using 2-pair selective Student's t-test.The results gained from both laboratory reference materials and certified glass reference materials show comparable accuracy. The quality of all available results complies with the “applied geochemistry” category of performance (2nd category). The laboratory reference materials give comparable accuracy to certified reference materials and can be used for calibrating microprobe techniques, as well as data quality control. The application of laboratory reference materials in microanalysis of silicate minerals and coppery alloys allows reliable analytical data to be acquired. The applications in mineralogy and metallurgy can be extended successfully to the targets when certified reference materials are not available.
Keywords:Electron probe X-ray microanalysis  Reference material  Coppery alloy  Basaltic glass
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