Determination of impurities in graphite using synchrotron radiation based X-ray fluorescence spectrometry.
Determination of impurities namely Ca, Mn, Fe, Ni, Zn, Sr and Pb in graphite by energy dispersive X-ray fluorescence spectrometry is described using microfocused synchrotron radiation. The internal standard and standard addition methodologies were adopted for quantification and the results were compared with tube-based X-ray fluorescence spectrometry. Analysis of the results by the F and t-tests revealed their statistical equivalence. Synchrotron measurements improved the detection limits by an order of magnitude compared to the tube based technique. Cr and Zr, which were below the quantification limit in tube based technique, were also quantified by synchrotron based technique.
Evaluation of uncertainty in the energy dispersive X-ray fluorescence determination of platinum in alumina
Evaluation of uncertainty in the Energy Dispersive X-ray Fluorescence (EDXRF) spectrometric determination of platinum in alumina catalysts is discussed. Pressed pellets of the platinum standard and a catalyst sample were prepared by using microcrystalline cellulose powder as the base material. A linear calibration of the X-ray fluorescence spectrometer was obtained in the range of 0.1–3 mg g−1 of platinum using pellets of matrix matched synthetic standards. The calibration function was obtained through bivariate least squares fitting, in conjunction with weighted regression of the residuals. The EDXRF results were compared with those obtained by instrumental neutron activation analysis and inductively coupled plasma optical emission spectrometry. Analysis of variance established the statistical parity of the results obtained by all the three techniques. A comprehensive evaluation of the various sources of uncertainty in the complete measurement process was carried out using a bottom-up approach. The main source of uncertainty was identified as the calibration of the EDXRF spectrometer, in which the major share was attributed to the intercept of the calibration function.
A remote controlled XRF system for field analysis of cultural heritage objects
X-ray fluorescence (XRF) is a nondestructive, multielemental, fast and cost-effective analysis technique. It can be applied in a nonvacuum environment directly on the samples without any preparation. As archaeological and historical objects are often unique and may not be easily movable, a mobile XRF detector system allowing in situ analysis is ideally suited for archaeometric applications. A mobile system was designed and built at the IPNAS laboratory to provide such analyses. The system includes an industrial grade x-ray generator which supplies the primary x-ray beam, an air-cooled silicon rift Detector detector (SDD) with a 5-mm2 active area. The data acquisition system measures the energy and the intensity of the secondary fluorescence x-rays. The detector signal is amplified and analyzed by a multichannel recorder coupled to a microcomputer running JavaSpectre which visualizes and analyzes spectra obtained from the detector. The detection head, containing the detector, the x-ray tube and its power supply, are fixed on a movable platform allowing independent vertical and horizontal movement. All displacements are controlled by a hand-held personal digital assistant (PDA) (Palm) which exchanges data with microcontrollers embedded in the system providing a very precise positioning of the detector over a surface of many square meters. This system control, as well as a typical application of this XRF spectrometer for analyzing pigment composition of a wall painting, will be described. Copyright © 2008 John Wiley & Sons, Ltd.