Director Standard Reference Materials : Homogeneity Characterization of NBS Spectrometric Standards IV : Preparation and Microprobe Characterization of W-20 % Mo Alloy Fabricated by Powder Metallurgical Methods
A significant problem of the National Bureau of Standards Standard Reference Materials program is the provision of standards suitable in homogeneity for use with microanalytical techniques such as the spark source mass spectrograph and the electron probe microanalyzer. An interim approach to the problem has been the extended homogeneity characterization of selected existing standards. This paper describes the preparation and evaluation of the first NBS standard tested specifically from the beginning for application to electron probe microanalyzers. The standard designated SRM 480 is a tungsten-20 weight percent molybdenum alloy prepared by a powder metallurgy process. Based on the results of about 1500 determinations for both tungsten and molybdenum by electron probe microanalysis, the material was found to be of high homogeneity at about the micrometer level of spatial resolution. The coefficient of variation for molybdenum was 2.5% and that for tungsten 1.5%. Correction of relative intensity ratios to obtain concentrations is discussed in terms of input parameter uncertainties such as mass absorption coefficients, and electron backscatter factors. The result of studies for atomic number correction and effects on operating voltage on the microprobe absorption correction., will be given. It is concluded that SRM 480 should be a valuable addition to any microprobe laboratory doing quantitative analysts.
Correction for Non-Linearity of Proportional Counter Systems in Electron Probe X-Ray Microanalysis
While the theoretical basis for the correction of non-linearity of detector systems is well known, methods for the determination of dead-time effects must be adapted to electron probe microanalyzer systems. Two such methods, one employing both X-ray and current measurements and the other employing simultaneous X-ray measurements on two spectrometers, are described. The effect of pulse-height shrinkage at high counting rates on the linearity of the detector system is discussed. When the proposed corrections for the dead-time of X-ray detector systems employing proportional counters are applied to the X-ray intensity measurements obtained with the electron probe microanalyzer, count rates as high as 50,000 counts/sec can be used.
Magnetic properties of Lu2Fe17 crystals
Abstract We present the results of crystal structure and magnetization studies of three single crystals grown from melts of different nominal compositions in the vicinity of the Lu2Fe17 stoichiometry. The ferromagnetic state of the crystals is strongly dependent on the real sample composition and the local atomic ordering. A drastic difference is observed in the behaviour of the ferro–antiferromagnetic transition, even in crystals for which almost identical composition and crystal parameters were determined by microprobe and X-ray analysis.