Monte Carlo simulation is used to determine the effects of selfabsorption for the low energy X-rays of light elements in the size range front 1 to 20 μm. Calculations are performed for a wide angle Fe-55 radioisotope-excited energy dispersive XRF system. Results are obtained for sulfur attenuation in thin layers, long cylinders, and spheres composed of various matrix materials. The enhancement effect is also treated for the transition region between thin and thick layer samples as well as in spheres of various sizes. Results are also comrpared to fixed angle analytical models.

Residual stress values in a material are governed by the measurements of the atomic spacings in a specific crystallographic plane and the elastic constant for that plane. It has been reported that the value of the elastic constant depends on microstructure, preferred orientation, plastic deformation and morphology [1], Thus, the theoretical calculation of the elastic constant may deviate from the intrinsic value for a real alloy.

Oscillations jn "d" vs. sin2ψ plots are due to the inhomogeneous partitioning of strains within the diffracting volume. In polycrystalline specimens, such inhomogeneity can be caused by the elastic incompatibility of neighboring grains or by the inhoniogeneous partitioning of plastic deformation within the diffracting volume. There is, however, little work on the degree of inhomogeneity required to cause a given oscillation, and the relative contribution from the elastic and plastic deformation components to a given oscillation.

In view of the amount of data per time unit the scanning electron probe is capable of producing, time economy in data presentation is of great practical importance. In this paper, the characteristics and advantages of various previously known techniques of data presentation are described, and some novel procedures are proposed.

A critical discussion of the equivalent wavelength representation of polychromatic primary radiation as applied to the fundamental parameters method is given. This representation raises problems with appropriate selection of equivalent wavelengths and with accurate calculation of secondary fluorescence. Methods for reducing these difficulties are discussed and have been incorporated into a mini-computer program which achieves reasonable accuracy for alloy test cases.

The authors have developed two independent software packages that store x-ray peak locations, integrated intensities and full-width half-maximum intensity data as a function of diffractometer tilt and orientation angle; this information is used to compute residual stress tensor values. Each program retrieves the fitted x-ray peak locations from a dBASE-compatible data set that is independent of both x-ray diffractometer and acquisition software. Machine-specific routines have been coded to transfer peak data and general diffraction setup information from several different x-ray acquisition platforms into this common format. The two database management programs provide stand-alone storage, retrieval, analysis and graphic output of data, and thus have become practical laboratory vehicles toward establishing a standard database format for storing x-ray strain measurements and the residual stress values calculated therefrom.

The results of the third year of observations on the effects of self-irradiation on the lattice of 238(80%)PuO2 indicate a small but definite trend toward a reduction in the lattice parameter of this material. The lattice parameter increased from 5.41408±6 Å at 5 weeks to 5.41636±38 at 114 weeks and then decreased to 5.41364±23 at 157 weeks after the start of the experiment. A similar trend is noted in the half-widths of the diffraction lines. For the 622 reflection the half-width increased from 0.283±14°20 at 5 weeks to 0.711±90 at 114 weeks and then decreased to 0.660±89 at 157 weeks.

A refined x-ray line profile analysis was used to determine the lattice strain distribution and crystallite domain size in nickel and a series of alloys, Ni-Cr, Ni-ThO2 and Ni-Cr-ThO2 in a wide range of thermo-mechanical conditions. Corrections were made for instrumental broadening and doublet broadening according to Stokes and Rachinger respectively, for errors due to the “hook effect”, for terminal errors in the series arising from Instability of the components, and for the presence of stacking faults and twins on the basis of peak shift and asymmetry. The internal consistency of the x-ray data was reviewed critically and good agreement was found. The values of lattice strain and domain size were used to evaluate the presence of a dislocation substructure and the degree of polygonization of the subgraln boundaries.

It was concluded that the thoria-free materials developed much higher lattice strains during cold rolling than did the Ni-ThO2, due it is thought to the operation of multiple slip in the latter. The Ni-Cr-ThO2 also developed high lattice strains during cold rolling, similar to those of the thoria-free lattices, and this was explained by the influence of chromium on cross-slip. It was postulated that the regions of high lattice strain act as driving forces in the process of recrystallization and promote grain growth during heat treatment following cold rolling.

The x-ray results were correlated with transmission electron microscopy and tensile data in a parallel study in which models for room temperature and high temperature strengthening were proposed.

There are currently no plans for the commercial reprocessing of nuclear fuel in the U.S. This is not the case in Japan, England, France, Germany, or the USSR. The U.S. does, however, include the reprocessing of spent nuclear fuel as a part of its defense programs. The Office of Safeguards and Security of DOE's Defense Programs has funded the development and optimization of numerous nondestructive analysis techniques including K-edge x-ray fluorescence analysis. This paper reviews some of the implementation efforts resulting from R&D supported by that office.

In 1979, the concept of using K-edge x-ray fluorescence analysis (K XRFA) for the analysis of actinide solution concentrations was first presented. K XRFA using small radioactive Co-57 sources has been shown to be a practical way to measure actinide solution concentrations in offline, at-line, or on-line configurations. The experimental methodology is elegant and the hardware is simple.

Phosphorite is a sedimentary rock with a high enough content of phosphate minerals to bo of economic Interest. Most phosphorites are composed predominantly of m1crocrystall1no to cryptocrystalline carbonate fluorapatlte thenceforth In this report referred to simply by the mineral group name apatite). Florida produces roughly 1/3 of the world's supply of phosphate rock, most of which is used 1n the fe rtiliz e r Industry.

Long term continuation of phosphorite mining In Florida will require exploitation of the extensive hlgh-magneslum phosphorite deposits south of the present mining d istrict 1n central Florida, and this will require new technology In order to produce beneficlated concentrates with less than 1% MgO, a limit Imposed by fe r tiliz e r processing technology. In order to develop benefication methods applicable to these ores, it is essential to know how Mg occurs in phosphorites. Dolomite, CaMg(C03)2, is the chief host of Mg In phosphorites from Florida. Magnesium may also be present, however, as a substituent In apatite (the chief phosphate.mineral in these deposits), as a minor substituent 1n calcite (CaCO3), in certain clay minerals (particularly palygorskite and to a lesser extent in some smectites), and/or in organic matter within the apatite particles.

Several examples of time-resolved X-ray powder diffraction studies with linear position-sensitive proportional counters (PSPC) are described. The changing patterns are recorded by spectrum multiplexing in a multichannel counter device. The time resolution for single processes is limited to seconds or tenths of seconds mainly because of the counting statistics of the observed peaks. Repetitive processes, however, where the interesting peaks can be accumulated over a large number of periods, permit much higher time resolution. It is finally determined by the timing of a detected X-ray quantum. Using a continuous beam source like a conventional X-ray tube the incidence of a photon into the PSPC can be timed with an accuracy of 20 ns (fwhm). A pulsed synchrotron radiation source, like a storage ring, will be able to define this resolution to its pulse duration, which is less than 200 ps.

Before approaching those limits this paper presents the high temperature phase transformations in iron for different steel specimens as an example of single processes. It also discusses domain-wall effects and electrostriction in ferroelectric perovskites as a function of polarization at frequencies of up to 10 Hz, and elastic lattice distortions of a steel sheet vibrating at about 200 Hz. The timing limit of 20 ns for the PSPC detection system was measured at the storage ring DORIS at DESY, Hamburg.

In nuclear power plants the fast neutron fluence on the pressure vessel (PV) inner wall is measured by the scraping sampling method (1). As the inner plating of the pressure vessel contains 0.5 - 0.6 % of niobium, 93mNb (tt/2 = 16a) isomer is produced by the reaction 93Nb (n, n’). The activity of 93mNb is related to the fast neutron fluence.

Scraping samples (few hundred of mg) were taken from the PV inner wall. The niobium was chemically extracted from steel by using a HAP column. This extraction was needed to reduce matrix effects and to avoid interferences of other activities with 93mNb

The introduction of various atoms into crystal surfaces by ion implantation has become common practice in the research laboratory and in many industrial processes. The deceleration of the introduced foreign ions during implantation results in extensive lattice damage. Atom displacement from equilibrium crystal sites and pile-up of the new atoms take place. The use of the pulsed laser for annealing these atomic defects in a single crystal is well documented . The absorption of the total energy in the laser pulse can be rapidly transferred to the lattice, approximately 10-9s, for an elevated temperature anneal of the damaged crystal. The photon energy of the monochromatic laser beam can be tailored so that the absorption of the radiation by a specific crystal can “be matched for its penetration into the crystal to that of the depth of the implanted atoms. A highly efficient mechanism is thus utilized to anneal just that portion of the crystal which is damaged by the impinging atoms of the implant.

The residual stress produced by surface and cylindrical grinding was measured by a position sensitive proportional counter. In medium carbon steels the residual stress depends largely on the grinding conditions. For a gentle cylindrical grinding compressive stress was observed, but for a rough grinding tensile stress was present in the workpiece.

X-ray diffraction topography is the name given to several x-ray diffraction techniques where large area x-ray beams diffracted from a crystal provide detailed information about the surface structure and internal perfection of crystal microstructures. Since x-ray topographic techniques are based on Bragg (reflection) or Laue (transmission) diffraction from a crystal lattice, they are extremely sensitive to any atomic lattice imperfections and strains. Alterations of the interplanar spacing as small as one part in ten thousand extending over a reasonable number of atomic ce11 lengths can be recorded as a corresponding change in the diffracted beam intensity. Line Modified-Asymmetric Crystal Topography (LM-ACT) is one such reflection technique that shows particular promise in Che field of microelectronics. The LM-ACT system is designed with low angular divergence in the x-ray beam probe. Low probe beam divergence allows details of device geometries on the order of microns to be resolved in the recorded x-ray intensity variation of the diffracted beam.

The LM-ACT system was applied here to the study of integrated circuits (IC) after specific processing steps were accomplished during IC fabrication and in the final product condition. Topographs obtained from specular crystal surfaces that were implanted through a patterned mask showed contrast variations between the implanted and non-implanted regions; details of the mask patterns have been resolved on the order of a few microns. LMACT topographs from annealed, and unannealed, Implanted specimens showed marked differences and as a result it is suggested that LM-ACT would be beneficial in optimizing the processing schedule for a particular wafer/electronic system. A significant feature of the LM-ACT technique is the capability for producing high resolution stereo-pair topographs that provide quantitative information through the depth of individual process layers in an integrated circuit.

Synchrotron X-radiation provides unique opportunities for diffraction experiments and, therefore, for extending our understanding of the structure - property interplay in catalyst systems. The present status of opportunities and applications of synchrotron X-ray diffraction techniques in the structural chemistry and catalysis science areas is overviewed, and illustrated by selected recent results.

Different procedures used in precision measurements of lattice parameters are, strictly, only valid if they can be shown to give results that are mutually reproducible. For this purpose reproducibility is defined in terms of the parameters a. and standard deviations a. obtained for X-ray specimens of one or more reference materials. The requirement is that all systematic errors should be minimized to a level below that of the random measurement errors. Where these have a Gaussian distribution the significance of the difference, Δa°, between two , measurements can then be Let;Led by evaluating . Thus, if K < 2 the difference, Δa°, cannot be distinguished from the effects of random measurement errors. This condition should be met for specimens of the same sample if reproducibility is good. For K ≥ 3 the value of Δa° is then taken to reflect real differences in the crystalline Jattice of two X-ray specimens of a given compound. A basis is thus created for the study of solid solubility and for the precise characterization of crystalline compounds.

Solid state equilibria in iron-nickel alloys containing 0-65 at % nickel were studied by X-ray diffraction techniques, and the gamma/gamma + alpha boundary has been relocated.

Alloys were prepared by thermal decomposition and hydrogen reduction of mixed-crystal iron—nickel formates and by distilling off mercury from mixed ironnickel “amalgams,” both methods of preparation yielding equilibrium alloys in relatively short time at temperatures below 500°C, Alloys were studied at various temperatures by use of a high-temperature diffraction camera, or at room temperature as quenched from the temperature of preparation.

The study showed that the gamma/gamma + alpha boundary lies at generally higher temperatures than in previous diagrams and is concave downwards instead of upwards. The boundary shows three discontinuities which have been located to lie at approximately (a) 3 at % nickel and 760°C, (b) 35–43 at % nickel and S25°C, and (c) 50 at % nickel and 330°C. These discontinuities indicate the possible existence of three isobaric invariant three-phase equilibria, heretofore, undetected in the iron-nickel system. Further studies covering the entire range of iron—nickel alloy compositions are in progress.

The present paper describes an energy-dispersive x-ray fluorescence method for measuring tin in bis(tri-n-butyl)tin-oxide impregnated wood. The proposed method is of the backscatter/fundamental parameter type. Its versatility, precision, and accuracy is demonstrated by analyses of eleven samples of sapwood of Baltic Redwood. The results obtained are compared with those from neutron activation analysis.

A special measurement technique has been developed to measure very low level iodine concentrations. The gas and water samples to be analysed are taken from the POSEIDON facility at PSI where retention of iodine in water pools in conjunction with light water reactor safety analysis is under investigation. The amount of iodine was measured by means of a Total Reflectance X-Ray Spectrometer (TXRF).