Atomic energy levels, which represent the energy necessary to remove an electron in a given level from the atom, are used for a variety of purposes-from predicting possible interfering x-ray lines in analysis to serving as experimental values with which to compare the results of complicated computer calculations. X-ray wavelength data is essential to determine energy level differences but cannot be used to place the resulting level scheme on an absolute energy basis , X-ray absorption data can be so used but the results of photoelectron energy measurements are superior. Since there are a very large number of possible x-ray lines from a typical element, one can readily obtain many more energy differences than there are energy levels ; hence, to make the best use of the data available, a least squares fitting procedure is used to obtain the most probable value for each energy level,

The residual stress left on the fracture surface is one of the important parameters in X-ray fractographic study. It has been used to analyze fracture mechanisms in fracture toughness and fatigue tests especially of high strength steels.

In this paper, X-ray fractography was applied to brittle fracture of alumina (Al2O3) and zirconia (ZΓO2) ceramics.

Using a multiple regression procedure, X-ray fluorescence analysis has been applied to a 15-element system associated with ceramic supported automobile emissions catalysts. An equation taking inter-element effects into account was used to relate the concentrations and X-ray intensities of the active elements and contaminants deposited on the ceramic substrate. The major elements present in the substrate were intentionally excluded from the regression. The regression coefficients were determined from a set of 240 calibration standards using a multiple linear least-square regression. Elemental concentrations in the standards ranged from 0.05 to ten weight percent. The ceramic matrix was the same in both the standards and the unknowns to be analyzed and constituted at least 85 percent of the total weight of each sample. The regression coefficients were then used to solve for the contents of the elements in unknown samples. Limits of accuracy were determined by using the set of available standards. The performance of the regression was improved in certain cases by imposing constraints on the regression.

When an x-ray diffraction profile Is measured for stress analysis or profile analysis by the use of a linear (straight line) position sensitive proportional counter (PSPC) , a convex-type background line is obtained because of the geometrical problem and the absorption of x-rays. Such phenomenon is remarkable when a wide angular range is set on a linear PSPC and it is, in particular, necessary to correct with a straight background for accurate measurement of diffraction angle or half-value breadth of the broadened diffraction profile.

External X-ray total reflection occurs when collimated X-ray beams impinge on a smooth, flat surface of matter at a small glancing angle, typically a few mrad. With respect to the X-ray fluorescence technique, total reflection experiments have allowed the trace determination of solution samples using an X-ray mirror as a sample support. The grazing incidence X-ray fluorescence technique (GIF) is also suitable for near-surface element analysis of the material, because the penetration depth of X-rays is 10-1000 Å around the critical angle.

A model is under development at this laboratory to predict the mobilization of Th from an estimated 20,000 metric ton deposit, in place and weathering as long as 80 million years on the Morro do Ferro, a hill on the Pacos de Caldas plateau in Minas Gerais, Brazil. The significance of this deposit lies in the marked similarities, chemically, between Th and Pu with reference to the problem of Pu waste management from the nuclear fuel cycle. One of the objectives of this program is to determine the elemental composition of the Morro do Ferro soil and its relationship to the mobilization of Th from the deposit. X-ray fluorescence is used for the analysis of Th, U, Ba, La, Ce, Pr, Nd, Sm, Dy, Eu, Gd, Yb, Hf , Fe, Zr, N b , Mo and Pb. This paper describes the XRF system and methodology used for the determinations and presents the results of 72 core, soil and sediment sample analyses for the above 18 elements. Analyses of three United States Geological Survey (USGS) rock standards are also presented.

This paper reports and discusses the results of a computer modeling study on powder diffraction profile analysis for crystallite size and strain of polycrystalline materials. The results of this computer modeling show that if the spans of diffraction profiles in reciprocal space (1/d) are not carefully chosen, an overestimation on size and an underestimation on strain may result in analysis by both the Warren-Averbach and the Hall-Williamson methods. A general way to eliminate such errors based on profile fitting and regeneration is presented and discussed in this paper.

Escape peaks occur when the incident X-ray quantum, energy exceeds the absorption edge energy of the detector element and the resulting X-ray fluorescence is lost from the detector. The most common escape peaks result from 1 K-fluorescence in NaI-scintillation counters and Xe K-, Xe L-, and Kr K-fluorescence in proportional counters. The average pulse amplitude of the escape peak is proportional to the difference of the Energies of the incident and fluorescent X-rays. If the intensity of the escape peak is high as in the case of Mo Kα and a kryptoopreportional counter, and the lower level of the pulse height analyzer is raised to reject the escape peak, the quantum counting efficiency may be reduced by a factor of two. When the pulse height analyzer is set for characteristic incident radiation, escape peaks appear in powder patterns at small diffraction angles. These broad low-intensity peaks are often mistakenly identified as resulting from misalignment, scattering, etc. Each powder reflection can produce its own escape peak which occurs at an angle slightly smaller than the absorption edge of the detector element. In a silicon powder pattern the three strongest reflections produce three resolved escape peaks whose peak intensities are about 4% of their corresponding Cu Kα peaks when the X-ray tube is operated at 50 kV. The escape peak intensities decrease with decreasing X-ray tube voltage and disappear when the voltage is lower than the absorption edge energy of the detector element. Absorption edge peaks observed without the upper level of the pulse height analyzer are similar in appearance, intensity, and diffraction angle to the escape peaks. In complex powder patterns the escape peak pattern is unresolved and may produce a number of very broad peaks.

A comparison of the relative merits of the energy dispersive derector-pulse height analyzer, scintillation detector-graphite monochromator, and proportional detector-pulse height analyzer combinations.

Typical energy dispersive detectors are not configured for maximum efficiency on the diffractometer. Being only on the order of 3 mm diameter, a good deal of the available information is not collected by the detector. This is especially true with the Wide optics found in modern diffractometers. The energy dispersive detector incorporated into this system is optimized for the x-ray diffractometer. Its detection area is a 1.25 X 0.25 inch rectangle. The resolution is only sufficient to remove the Kβ portion of the spectrum.

Conventional diffractometer techniques incorporate either a scintillation detector-crystal monochromator, or a proportional detector-pulse height analyser combination. The question posed is “what are the advantages in signal to noise ratio and pulse height distribution of the energy dispersive-pulse height analyzer over the more conventional arrangements.”

Equipment is described whereby comparative measurements were made on the relative absorption of air.helium, and vacuum for the softer radiations which are of interest in furthering the range of sensitivities of the X-ray spectrograph. Data on magnesium, aluminum, and silicon and shorter wavelengths are presented.

A modified version of the Rietveld method has been developed for quantitative phase analysis in conjunction with crystallite size and microstrain determination.

Besides the information on the microstructural disorder in the different phases present in the sample, accurate phase analysis can be performed, even in presence of anisotropic crystallites, taking into account the non-instrumental peak broadening effect in a better way compared to conventional methods.

The method has been tested on binary mixtures of corundum, ceria stabilized zirconia and on a polyphase stabilized zirconia sample.

It is well-known that in EDXRF, using high-resolution semiconductor detectors, evaluation of x-ray fluorescence radiation line intensities from multiplex spectrometric information represents definite difficulties, especially in automation of measurement-calculation procedures.

A common spectrum decomposition problem is to get the following parameters: a number of spectral lines and their centroids, intensities from measured experimental data and their errors.

We have developed special software for solving this problem using personal computers and high-level programming language C. It uses profiles of real-form lines of pure chemical elements produced by semiconductor detector spectrometers and these techniques: digital filters with parameters for suppression of background, multiplex structure analysis, and stable linear least-squares fit to get peak intensities. Also it established special criteria for reliability of the results.

We compared our investigation with software “EDXRF” (ver.1.32) arid spectrum decomposition with Gaussian peaks.

Improving the detection limits in TXRF by optimizing the excitation conditions is the goal of this work. The properties of the exciting radiation due to spectral distribution, polarisation, intensity and energy are investigated and compared to find best conditions. Results are given from experiments performed with synchrotron radiation, Bragg polarized monoenergetic x-rays, high energy cut-off reflector in the primary beam path of a high power x-ray tube and several geometries for the sample reflector.

X-ray camera methods of stress measurement are inherently flexible and easy to apply in different situations because of the low weight, portability and maneuverability of the equipment. However, the digital intensity recording with the resulting objectivity and better statistical accuracy has given the diffractometer methods a distinct advantage over the conventional camera methods.

A minicomputer program system for phase Identifications in x-ray powder diffraction is described. The routines written in FORTRAN comprise the users’ special purpose standard-file management (creation of microfiles from the complete JCPDS-data base or own standards, as well as utility routines for corrections, supplements and bookkeeping) and the measured data processing, including raw data acceptance, data reduction by two selectable peak-search routines (trendoriented or 2nd derivative) and an exhaustive search/match procedure through selected microfiles. The data reduction and analysis programs have manifold graphical displays allowing manual interference. In one run up to five phases can be matched. The weight portion of every phase is estimated, using I/I (corundum)- values, Hie whole analysis (in automatic operation) consumes about 1 or 2 minutes of the processor time on a pdp 11/34 minicomputer. This matches well to the data collection times accessible for fast powder diffraction systems /I/.

Synchrotron radiation was used to obtain a high-resolution powder diffraction pattern of the high-density form of BeH2, a material whose unit-cell dimensions have not previously been determined. The observed d-spacing values were presented to three different computer indexing programs. All three programs returned as best solution a body-centered orthorhombic unit cell with a = 9.082, b = 4.160, c = 7.707 Å and V = 292 Å3. Interpretation of the three-dimensional Patterson led to 12 BeH2 molecules per unit cell; thus, the theoretical density is 0.755 g/cm3. The molecular structure is based on a network of corner-sharing BeH4 tetrahedra rather than flat, infinite chains with hydrogen bridges previously assumed.