A specific XRF method, developed at the Soreq Nuclear Research Centre, was applied to the determination of bromine in blood. The method is based on excitation with a Mo X-ray tube and detection of the fluorescent Br K X-rays by a Si (Li) detector. Serum microsamples (300 μL) are counted directly, without drying, for 100 sec, The detection limit obtained under these conditions is 0.6 ppm Br, The overall precision of the method was found to be ±3.1%. The different parameters which contribute to the total error of the method were studied, A survey of the bromine concentration in the blood serum of industrial workers exposed to bromine compounds was carried out.

The number of products that have to be inspected in pre-service and/or in service is increasing. Not only inspection for flaws are required increasingly, using the ordinary non-destructive testing, but also inspection of material characteristics, such as material strength evaluation and/or damage detection. For such inspection, X-ray diffraction has great possibilities as one of the most promising techniques, because it is (a) noncontact, (b) very sensitive to changes in parameters of the crystalline structure, and (c) suitable for surface observation.

In this paper, three topics are introduced which will be useful in the field of material strength evaluation and damage detection using X-ray diffraction.

In order to determine the polluting atmospheric sources in urban and background areas source apportionment of the air particulate matter is necessary. Hitherto these studies were mostly based on bulk composition measurements of the aerosol. Source profiles, i.e. the concentrations of several elements for air particulate matter originating from one source, can be deduced from the receptor data using a number of multivariate techniques among which the chemical mass balance. The application is limited by the large number of observations that must be made for each of the variables. Often an elaborated sample preparation is necessary for fractionating the sample into several sub samples, according to the density, particle diameter or other relevant properties . Often this may results in poorly resolved source profiles.

Austempered ductile cast iron (ADI) lias microstructures that consist of martensite and of retained austenite. ADI has very toughness compared with cast iron heat-treated differently. The retained austenite near fracture surfaces transforms to martensite when fracture occurs.

In the present study, X-ray fraetography is applied to fatigue fracture surfaces of ADI. The fatigue tests were carried out on compact tension (CT) specimens. The volume fraction of retained austenite was measured quantitatively and the line broadening of X-ray diffraction profiles was measured on and beneath fatigue fracture surfaces. The depth of the plastic zone left on fracture surfaces was evaluated from line broadening. The results are discussed on the basis of fracture mechanics.

Two sample preparation procedures for XRF determination of critical elements in process control samples of a lead smelter have been compared. The two methods, pressed powder(PP) and borate fusion(BF) were used in the analysis of (in order of importance) lead, zinc, copper, sulphur, arsenic and the flux elements (FeO, MnO, Al2O3, CaO, MgO and SiO2). The techniques were applied to three points in the overall lead-zinc-copper production process.

The three sample types have been selected to allow comparison between the BF and PP methods, where the PP method suffers from difficulties with particle size, moisture absorption or composition variation.

The BF technique was found to give better precision (typically 0.2 to 1% RSD) than the PP approach (typically 0.8 to 9% RSD), and to give better accuracy as found using reference materials. The stability of the BF bead over time is also of advantage in quality control. The flexibility and reliability of the BF technique has lead to its acceptance, and in part, to changes in the overall smelter analysis structure.

X-ray diffraction observation of metal fractures provides fracture analysis with useful information on the mechanisms and mechanical conditions of fracturing. This method is called “X-ray fractography” and has been developed especially in Japan as a new engineering tool for fracture analysis.

Chromium glycerate solutions are exposed to X-ray absorption fine structure analysis to clarify the local structure around the chromium atom by the use of a laboratory XAFS system. The chromium solution is stabilized by addition of water soluble polyvinyl alcohol so that after excess water, the solution is a kind of homogenized “sol” without any apparent charge to the solution state. The new technique has been developed, because chromium is an element which has relatively small X-Ray absorption.

The comformations of two novel chromium glycerate compounds, which are prepared under both NH4OH and NaOH basic conditions, are examined with XANES and EXAFS techniques. From these experiments, it is suggested that these two chromium glycerates may have Cr-O-Cr bridge bonds consisting of chromium dimer complexes in common.

The residual stress measurement of quenched and tempered steels is of practical importance because the quenching can sometimes induce the high residual stress which affects the strength of materials. The stress constants of carbon steels quenched and tempered at various temperatures were measured in order to determine the residual stress of steels by x-ray diffraction. The stress constant increased slowly with increasing tempering temperatures below 500°C; it increased rapidly with tempering temperatures above about 500°C, This rapid increase in the stress constant is closely related to the change in microstructure of the steels in tempering; above the tempering temperature of around 500°C, the tempered martensite recrystallized and transformed to ferritic iron and fine cementite particles dispersed in the matrix; these coalesced and grew to be speroidized cementites and finally laminar cementite plates.

In multielement EDXRF analysis of very complex unknowns, some problems in data evaluation may be simplified if one can take into account a priori information on the properties of the incident and detected radiations, and also available data on the matrix of the sample. The number of variables can be drastically shortened in the LSM procedures in this case. One of the best examples of complex unknowns is the determination of the rare earth element content of ores, and most recently in samples of high temperature superconductors (HiTc).

The electroplating of Cr has been an important industrial process for cutting tools, press machines and molds for casting. In spite of these, quite a few problems remain unsolved regarding the basic property. It is important to know the mechanical characteristics of Cr electroplated layers.

In the present paper, the first part deals with the measurement of mechanical Young's modulus of Cr electroplated layers. The X-ray method was successfully applied to measure the X-ray Young's modulus and the residual stress on the Cr electroplated surface layer.

A new method, for the on-line determination of the composition and the coating weight of galvannealed (Zn-Fe-alloy-coated) steel sheets using monochromatic incident x-rays with two optical systems, is described. In the case of galvannealed steel sheets, it is difficult to determine the composition and the coating weight precisely by simple XRF, because fluorescent x-rays of Iron are emitted not only from the coating layer but also from the underlying steel sheets. We have developed an on-line analyzer with two optical systems which are different in incident angles, take-off angles and wavelengths of monochromatic incident x-rays. We determine the composition and the coating weight by solving simultaneous equations of the data which we derive using two optical systems. Using monochromatic x-rays enabled us to obtain high precision with high speed. We considered en-or factors in on-line measurement such as statistical error or fluctuation of the distance between the sensor head and steel sheets. This on-line analyzer has been applied to the continuous galvanizing line in our Fukuyama works successfully. As a result, we have been able to significantly improve product quality.

For determination of stress in a localized area, we combined a modified single exposure technique and the imaging plate, which is an x-ray digital area detector. With the, single exposure method, stress value is obtained from lattice strains in two directions with a single incident x-ray beam directed at an oblique angle. However, since diffraction data around a whole Debye-Scherrer ring was used in this study, a stress value can be accurately determined in comparison with the single exposure method. We observed the DS ring by use of the imaging plate with requiring only a short exposure time. Lattice strains in many directions on a DS ring were measured by an image analyzer connected to a computer; we verified the effectiveness of this method.

Three-dimensional tomographic reconstruction is capable of producing arrays of cubic voxels with resolution adequate to reveal important microstructural properties in materials. Visualization and measurement of these structures extends the types of information available from conventional 2D microscopy.

Elastic modulus EI of crystalline regions of various high polymers in the direction parallel to the chain axis were measured using an X-ray diffraction method. The crystal deformation can be detected directly by the diffraction peak shift as a function of applied constant stress. The stress in the crystalline regions is assumed to be equal to that applied to the specimen. The validity of this assumption has been proven experimentally for polyethylene, poly(p-phenylene terephthalamide) and so on. The EI values were discussed in relation to molecular conformation and deformation mechanism of the chains.

Scanning x-ray fluorescence microscopy is analogous to scanning electron microscopy. Maps of the distribution of chemical elements are produced by scanning the specimen with a very small x-ray beam while collecting the XRF spectrum. Our goal is to perform such scanning microscopy with resolution in the range of <1 to 10 μm, using standard laboratory x-ray tubes. In order to increase the radiation flux on the specimen, we are investigating mirror optics in the Kirkpatrick-Baez (K-B) configuration, K-B optics uses two curved mirrors mounted orthogonally along the optical axis. The first mirror provides vertical focus, the second mirror provides horizontal focus. We have used two types of mirrors: synthetic multilayers and crystals. Multilayer mirrors are used with lower energy radiation such as Cu Kμ. At higher energies such as Ag Kct, silicon wafers are used in order to increase the incidence angles and thereby the photon collection efficiency. In order to increase the surface area of multilayers which reflects x-rays at the Bragg angle, we have designed mirrors with the spacing between layers graded along the optic axis in order to compensate for the changing angle of incidence. Likewise, to achieve a large reflecting surface with silicon, the wafers are placed on a specially designed lever arm which is bent into a log spiral by applying force at one end. In this way, the same diffracting angle is maintained over the entire surface of the wafer, providing a large solid angle for photon collection.

The dependence of a peak diffraction angle on the positioning of the diffracted-beam Soller-slit pack was observed and studied by discussing the determining factors. In particular, the misalignment angle between the Soller pack and the counter axis is recognized as a key factor and experiments were performed for giving a quantitative basis to this statement. An important consequence of the results of these experiments and related profile analysis is the suggestion of designing parallel-beam diffractometers with the possibility of checking and changing the position of the diffracted-beam Soller-slit packs in order to optimize the performance of the instrument.

The analysis of linear dϕψ vs sin2ψ x-ray diffraction data in isotropic single phase materials was investigated for the evaluation of x-ray elastic constants. This study developed an experimental model for estimating x-ray elastic constants based on the analysis of biaxial residual stress states, A ball bearing steel and a 1018 steel weldment were evaluated.

In a second study, the measurement of residual stress gradients was evaluated for those depth ranges mat can not be evaluated with a single radiation. This requires various planes and radiation energies to obtain the simultaneous conditions of high diffraction angle and large x-ray penetration depth. The evaluation of the overlapped stress gradient region is illustrated in terms of x-ray energy and diffraction angle for the ease of iron. This analysis is specifically developed for the purpose of stress gradient measurement using synchrotron radiation.

Composition imaging of industrial samples has been reported using dual energy and multiple energy transmission computed tomography [1,2]. The simplest approach utilizes monoenergetic sources to obtain tomographs of a sample at two different energies. Each tomograph represents the linear attenuation coefficient distribution of the sample at the given source energy.

The physical basis for x-ray induced secondary electron emission in the range of the absorption edges is described. Applications of this principle for nondestructive composition determination and for nanometer resolved quantitative composition depth profiling are illustrated. A new commercial type of scientific instrument is presented which can be used for this new technique, and for almost all methods that require x-ray photon beam probing.

All the methods described in this paper are based on the same phenomenon, chat is, the phenomenon of the jump-like increase of x-ray photoabsorption in the vicinity of the x-ray absorption edges of the chemical elements of the sample.

HFIT is a program for the analysis of diffraction diagrams containing overlapping peak clusters. Profile functions have been implemented to analyze synchrotron diffraction data. It is written un Turbo C++ for PC operations. The analysis is done by operator interaction. The analysis is done on sections of the diffractogram containing a maximum of 2048 data points or 100 diffraction maxima. Special care is taken for smoothing the data and for the subtraction of background.