Standard less analysis

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Information about Standard less analysis

Published on January 11, 2008

Author: Quintilliano


Quantitative Standard-less XRF Analysis AXAA Conference Newcastle 2002 :  Quantitative Standard-less XRF Analysis AXAA Conference Newcastle 2002 Stanislav Ulitzka Twotheta Pty Ltd Sydney Quantitative Standard-less XRF Analysis:  Quantitative Standard-less XRF Analysis Quantitative vs. Semi-quantitative Standard-less Round robin test Standard-less … WHY?:  Standard-less … WHY? Varying sample types Solid, liquid, loose powders, scales, drillings … Sample shapes Flat, odd, small quantities or pieces, thin layers … “Unusual” elements (Be, B, C, N, O) - Fluorine to Uranium Methods:  Methods “Peak hopping” better counting statistics Scanning possibility of very fast scanning (3 to 5 min) Fine-tuning and sub-sets possible with own standards (steel, alloys etc.) “Peak hopping” vs. Scanning:  “Peak hopping” vs. Scanning Counting Statistics:  Counting Statistics th = sqrt ( R * t ) R = counts/s t = counting time CSE rel [%] = 100 / sqrt (R * t) Example: sqrt (1’000’000) = 1000  0.1 % relative error Calibration!!!:  Calibration!!! Standards single element/oxide or multi-element  intrinsic sensitivities Corrections Background Overlaps Matrix Drift, media, and film correction Background correction:  Background correction Background correction:  Background correction 66 kcps 23 kcps 12 kcps Analysis of unknowns - ASMQ:  Analysis of unknowns - ASMQ Tuned analytical recipe Select measurement Load analytical recipe Load sample parameters Automatic Search Match and Quantify Analysis of unknowns:  Analysis of unknowns Measurement - acquisition of intensities same method as for standards Manual check of BG correction & labelling of peaks (optional) Sample description – most important! Type – solid, liquid, bead, PP Flux/binder – chemistry, weights Normalisation Y/N?; balance compound? Unmeasured compounds – B2O3, LOI, CO2, organics … Sample description – IQ+:  Sample description – IQ+ Sample description - UQ:  Sample description - UQ Report – IQ+:  Report – IQ+ Report - UQ:  Report - UQ Major elements – SY-2:  Major elements – SY-2 Major elements – SY-3:  Major elements – SY-3 Trace elements – SY-2:  Trace elements – SY-2 Trace elements – SY-3:  Trace elements – SY-3 Conclusions:  Conclusions Any standardless method yields “numbers” Quality of analysis (accuracy) depends on Calibration Matrix correction (to a certain extent) Correct sample description/definition “Driver” training!!!

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