A straightforward method for the systematic peak‐shift correction using the standard reference material is proposed for the least‐squares determination of unit‐cell parameters. It requires no pre‐determined angle‐calibration curve, and the peak‐shift correction can be applied simultaneously during the least squares. The procedure, programmed with Fortran 77 statements, has been tested with powder diffractometer data of an α‐SiO2 + Si mixture. Advantages of the procedure are: (i) all reflection data from both sample and standard reference material contribute to determining the angle‐dependent calibration curve, and (ii) one reflection from the standard reference material suffices for the correction of systematic errors.
The authors present and discuss a method for simultaneous quantitative analysis of total loss on ignition (LOI) (CO2 + H2O) and CO2 content separate from the LOI, in an industrial environment of quicklime production. Total LOI is determined by the Compton scattered RhKα tube radiation which is used directly in the calibration equation. The resulting calibration curve for LOI, including matrix correction shows an accuracy of 0.15 mass%. The carbon content (CO2) is distinguished from total LOI by measuring CKα radiation, which is possible with the required accuracy by employing a new multilayer analyzer with greatly improved background characteristics. The method aims at high reliability and sample throughput and at becoming a less time-consuming alternative to the conventional method of LOI determination by weighing sequences before and after “ignition” at 1050 °C.
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