The electron probe is an extremely valuable tool for chemical analysis on a microscopic scale. There are many situations, however, that require analyses in the millimeter rather than micron range, where in fact, the use of the electron probe causes concern about sample homogeneity. The X-ray probe consisting of a small X-ray beam and focusing monochromator is very useful for this intermediate region. This X-ray probe is equally useful for electrically non-conducting as well as conducting specimens. Analysis need not be performed in vacuum and can be done with great rapidity.

For example by traversing a polished section of a combination of opaque minerals, it was possible to determine the distribution of copper, silver, arsenic, iron, and mercury and to show that an unidentified mineral was a copper arsenic mineral rather than an arsenoargentite as had been supposed.

A review of the crystal structures of the elements shows some prevailing tendencies of atomic arrangement. These are discussed as space, symmetry, and connection principles. Counteracting temperature and bond factors can be recognized.

The same principles and factors are responsible for the formation of alloy structures, taking into account additional factors due to the component's similarities and dissimilarities in size and electronegativity.

Similarity favors solid solution and dissimilarity favors compound formation. A q compound is here defined as a phase in a q-component system not connected with any other phase of the system by continuous solid solution. Similarly a q structure is defined as a structure type which needs only q components to be formed (considering present-day knowledge). For example, the binary compound Mg17Al12 has the elementary (1 ™) structure of α-manganese. As a rule, q compounds tend to form p structures with q > p.

A discussion of q structures with q = 1, 2, and 3 is given in some detail on the basis of known representatives to show: (1) the competition of geometrical principles and physicochemical factors in determining atomic arrangements of alloys; and (2) the value of rules for making guesses on the probable occurrence of compounds and their chemical composition in polycomponent systems yet unknown.

An attachment to a commercial flat-crystal X-ray fluorescent goniometer permits analysis of small areas. The selection of the sample area is achieved by collimating the secondary beam. The geometry of the probe, its stage, and counting statistics applied to the probe are discussed. Experimental data are shown referring to determination of spot size, counting rates obtained, and both qualitative and quantitative applications.

This method describes the addition of cerium (IV) oxide to a lithium borate flux. CeO2 provides a non-analytic glass former to the melt production. CeO2 also acts as an interelemental buffer replacing the use of lanthanum oxide for long wavelength absorption. With cerium oxide addition, excellent results are produced, resulting in part from the elimination of recrystallization problems encountered with lanthanum oxide use. Analytical results easily meet the ASTM C-114 qualification requirements for rapid method analysis of hydraulic cements.

The diffraction elastic constants have been measured for the 211 and 310 peaks of a high-strength, low-alloy ferritic steel using X-rays and neutrons. The X-ray measurements were performed using both a uniaxial tension and a bending device. The neutron measurements were performed using a uniaxial tensile device. Ten X-ray and four neutron measurements were made for each case. Statistical errors were calculated and compared with the standard deviations of the average values. In addition, neutron measurements were made for the 310 peak utilizing an interior probe volume.

The results indicate that the calculated statistical errors and the observed standard deviations were almost the same for each radiation. The X-ray and neutron tensile device measurements yielded similar results within experimental error. Furthermore, the X-ray tensile and bending results were similar as were the neutron internal volume measurements. These results suggest that near-surface X-ray measurements adequately sample the bulk material in the case of steel, and that different measurement techniques can be used to obtain reliable diffraction elastic constants.

In the 100 years since the landmark work of Wilhelm Conrad Röntgen, much progress has been made in X-ray science and applications. X-ray Fluorescence Analysis (XRF) essentially had its beginning not long after that development, when, in 1913, Moseley demonstrated the relationship between the atomic number of an element and the wavelength of its X-ray spectra. As early as the 1930's, workers were analyzing materials for trace elements. By the time of the 1940's, X-ray spectroscopic instruments were becoming commercially available, and analysts were beginning to appreciate the simplicity of the X-ray spectra, and thus the potential for a significant impact on elemental analysis.

Objects of art and archaeology are relicts of the past, and art historians, archaeologists and conservators are constantly concerned with the questions of where, when or by whom such artifacts were made. Usually stylistic considerations can provide answers to these questions, but as styles were sometimes copied at locations and times quite different from those for which they were most characteristic, material analysis is often essential when one is attempting to infer how and of what materials an object was made. The use of several compounds e.g. as pigments in paintings, or the deliberate alloying of Cu with Sn, As, Sb and Pb, has varied greatly from region to region and from time to time and can be used to infer the geographic origin of an object or at least the origin of the materials, out of which it was made.

A novel method using Fourier transform algorithm is proposed to determine each layer thickness of multi-layered thin films from interference oscillation observed in X-ray specular reflection. The peak position in Fourier space gives each layer thickness of the film. The principle of the present technique as well as its applications are described.

A fast X-ray diffraction powder method of quantitative analysis has been developed and demonstrated using mixtures of alpha and beta silicon nitride and silicon.

An analytical procedure, assuming both Gaussian and Cauchy diffracted characteristic line distributions, was used to synthesize CuKα X-ray peaks in the 2θ range 20° to 50° with peak widths from 0.1° to 0.4° 2θ. The relationship of peak height to integrated intensity was established as a function of peak width and tested using pure silicon powder with variable receiving slit widths from 0.01° to 0.40° 2θ.

Concentration calibration curves for silicon nitride and silicon were corrected for extinction and preferred orientation with statistical figures of merit to indicate the extent of preferred orientation.

Preliminary results indicate that this procedure may be used for cold-worked materials.

The relevance of X-ray diffraction techniques to the investigation of the chemical, physical, and crystallographic changes occurring during sliding wear is discussed in relation to existing theories of wear. By-way of illustration, the application of the powder X-ray cylindrical film technique to the unlubricated wear of a low-alloy, medium carbon steel is treated in some detail. The variation of the relative proportions of iron and its oxides in the wear debris with changes in sliding speed is described. It is shown that the results lend partial support to the oxidational hypothesis of the unlubricated wear of steel.

A new proportional counter x-ray detector with application for powder diffractometry has been developed. The new detector collects virtually the entire diffraction spectrum simultaneously with good efficiency and angular resolution. Thus, the powder spectrum of a small sample can be obtained much faster than with film or a conventional powder diffractometer. The detector read-out is digital and is interfaced to a dedicated minicomputer. A description of the detector system is discussed and preliminary results are presented.

The Fuji Imaging Plate (IP) is a 2-dimensional detector in which a latent X-ray image is stored as a distribution of color centers on a photostimulable phosphor (BaFBr:Eu2+) screen. It has a large effective area, wide dynamic range and high sensitivity. Thus it has been widely used not only in medical but also in scientific and industrial fields. Particularly in X-ray structure analysis, mainly of proteins, it has been used extensively and achieved good results.

On the other hand, few applications have been reported in the field except for structure analysis, in spite of the superior performance of the IP which will give significant advantages in various measurements which have been done using an X-ray film such as electric device and fiber specimen.

Therefore we report here the basic performance of R-AXIS II(Rigaku Automated X-Ray Imaging System II), an IP reader made by Rigaku, and some applications of X-ray diffraction measurements using IP.

Trace element analyses by energy dispersive X-ray fluorescence measurements were made using synchrotron radiation from a dedicated electron storage ring at the Photon Factory in Japan. The continuum or the monochromatic beam was used for excitation. A crystal monochromator or two types of mirror systems were used for monochromatic excitation. A high signal to background ratio was attained with the crystal monochromator, while the highest absolute detectability was achieved with the mirror system. The minimum detection limita obtained from thin samples are of the order of 0.1 ppm or less than 0.1 pg. Furthermore the signal to background ratio was significantly improved by using an X-ray mirror as a sample support in which, external total reflection of exciting X-rays occured.

Production efficiencies for the excitation of characteristic soft X-ray emission spectra by proton bombardment were investigated. Results were obtained for K-, L-, and M-shell lines of various elements as a function of proton energies ranging up to 100 keV.

For comparison putposes, helium, nitrogen, and argon ions also were accelerated and used as bombarding particles to yield efficiency data for some of the same spectral lines.

The data demonstrate that:

• 1. The production efficiencies of spectral lines excited by protons are, in the first approximation, dependent on wavelength only and are independent of the atomic shell with which they are associated.

• 2. Production efficiencies increase with the atomic weight of the bombarding ions for some of the spectral lines investigated.

X-ray generation by proton bombardment is a powerful method for producing high-intensity monochromatic radiation for wavelengths above approximately 10 Å, The same technique can be used for analytical purposes to determine the concentration of low atomic number elements.

This paper describes the principles, methods, instrumentation and results of EDXKD and a computer method of profile fitting to obtain corrected intensities and peak energies from isolated and overlapping reflections. The profile, P, of a diffraction peak is a convolution of the incident X-ray spectrum, X, the geometrical aberrations, T, the contribution from the specimen, S, and the detector resolution function, D.

A new analysis principle for energy-dispersive X–ray fluorescence has been identified and investigated as to feasibility. It consists of: (1) generating the complete spectral response for a sample of known (assumed) composition by Monte Carlo simulation,(2) keeping track of the individual elemental responses within the Monte Carlo simulation for use as library spectra, (3) use of the library least–squares (linear) analysis method to obtain the elemental amounts for any unknown sample spectrum, and (4) iterating these steps if the unknown amounts are too fax from the assumed composition originally used.

This principle has been investigated for a radioisotope source excited EDXRF system consisting of a 109Cd source and a Si(Li) detector for a Cu-Ni alloy sample (CDA Alloy 715) and a stainless steel sample (304 Stainless Steel) and found to give excellent results. This analysis principle makes unique use of the Monte Carlo “forward” simulation method to provide the elemental library spectra for use in the library least-squares method of analysis.

A numerical procedure is described and demonstrated for determining z-profiles from measured τ-profiles of diffraction data such as may be obtained by grazing incidence x-ray diffraction (GIXD). The z-profile was approximated by a piece wise linear function and the problem of solving the integral equation for the z-profile was thus converted to one of solving a set of linear equations. With a sufficient number of the linear pieces, the z-pTofile could be accurately determined. The procedure and its sensitivity to data errors was tested with several arbitrarily chosen known functions. It was found that when errors were introduced into either the τ-profile or the sample thickness D the resulting z-profiles become oscillatory.

Ceramics are sometimes bonded to ductile metals in order to make up for their brittle behavior for industrial use. The residual stress will be induced in ceramics bonded to metals at high temeprature, and it has a strong influence on the strength of ceramic-metal joints. A silicon nitride plate was bonded to a carbon steel plate by brazing to a copper sheet sandwiched between the two materials. The residual stress distribution of the joint specimen was determined by x-ray diffraction using the Gaussian curve method. The measured residual stress distribution almost agreed with that calculated by the three-dimensional thermoelastoplastic stress analysis using FEM, but differed remarkably from that calculated by the two-dimensional stress analysis. This is because a stress concentration occurs at the ceramic-metal interface and the stress distributes three - dimensionally. The stress σx in the axial direction on the surface of the specimen takes maximum values at the center and the edge of the interface.

Non-destructive analysis of Venezuelan pottery samples of different sizes and shapes from various archeological sites along the Orinoco River in the middle of Venezuela was performed by radioisotope X-ray fluorescence. The method employed a low intensity 109Cd source. The precision of the measurements for Fe, Rb, Sr and Zr from three different areas on each side of one of the artifacts was about 5%. A comparison of the data analysis using gross peak intensities and net peak intensities employing a digital filter technique to eliminate the background is presented. Finally an attempt to discriminate the samples of one location from another one or ones, assuming that the potter's clays were from different sources, is described.

Compressive residual stress is one of the essential elements which contributes to the exceptional fracture resistance of case-hardened components. The sign and magnitude of residual stress are determined by transformation characteristics, thermal and mechanical histories of the steel. Accurate determination of residual stresses is essential in research on case-hardened steels.