M K Tiwari
Articles written in Bulletin of Materials Science
Volume 24 Issue 6 December 2001 pp 633-638 Alloys and Steels
A simple method for the analysis of stainless steel samples is presented which is based on radioisotope excited energy dispersive X-ray fluorescence (EDXRF) spectrometry and does not require any type-standards. Both absorption and enhancement effects have been taken into account in the fundamental parameter method for quantitative analysis and an iterative approach is followed for calculation of concentrations in steel samples. Non-linear least square fitting (NL-LSF) procedures have been used to determine accurately the fluorescent peak intensities. The method has been tested by analysing several CRM standard reference samples and 304 and 316 steel samples assuming as unknown. The EDXRF results have also been compared with the results of analysis of same samples by vacuum emission spark spectrometry (VES). Obtained values for concentration in steel samples match quite well with their certified values.
Volume 25 Issue 5 October 2002 pp 435-441 Instrumentation
A simple and fairly inexpensive total reflection X-ray fluorescence (TXRF) spectrometer has been designed, constructed and realized. The spectrometer is capable of ultra-trace multielement analysis as well as performs surface characterization of thin films. The TXRF setup comprises of an X-ray generator, a slitcollimator arrangement, a monochromator/cutoff-stage, a sample reflector stage and an X-ray detection system. The glancing angle of incidence on the two reflectors is implemented using a sine-bar mechanism that enables precise angle adjustments. An energy dispersive detector and a GM counter are employed for measuring respectively the fluorescence intensities and the direct X-ray beam intensity. A Cu-target X-ray generator with its line focus window is used as an excitation source. The spectrometer is quite portable with its compact design and use of a peltier cooled solid state detector for energy dispersive detection. Alignment and characterization of the TXRF system has been performed and the minimum detection limits for various elements have been determined to be in the range of 100 pg to 5 ng even at low X-ray generator powers of 30 kV, 5 mA. The capability of the TXRF system developed for thin film characterization is also demonstrated.
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