Total reflection X-ray fluorescence spectrometry (TXRF) was used to analyze residual surface contamination on Genesis solar wind samples and to evaluate different cleaning methods. To gauge the suitability of a cleaning method, two samples were analyzed following cleaning by lab-based TXRF. The analysis comprised an overview and a crude manual mapping of the samples by orienting them with respect to the incident X-ray beam in such a way that different regions were covered. The results show that cleaning with concentrated hydrochloric acid and a combination of hydrochloric acid and hydrofluoric acid decreased persistent inorganic contaminants substantially on one sample. The application of CO2 snow for surface cleaning tested on the other sample appears to be effective in removing one persistent Genesis contaminant, namely germanium. Unfortunately, the TXRF analysis results of the second sample were impacted by relatively high background contamination. This was mostly due to the relatively small sample size and that the solar wind collector was already mounted with silver glue for resonance ion mass spectrometry (RIMS) on an aluminium stub. Further studies are planned to eliminate this problem. In an effort to identify the location of very persistent contaminants, selected samples were also subjected to environmental scanning electron microscopy. The results showed excellent agreement with TXRF analysis.

The instrumentation developed for poly crystalline diffractometry using the storage ring at the Stanford Synchrotron Radiation Laboratory is described. A pair of automated vertical scan diffractometers was used for a Si (111) channel monochromator and the powder specimens. The parallel beam powder diffraction was defined by horizontal parallel slits which had several times higher intensity than a receiving slit at the same resolution. The patterns were obtained with 2:1 scanning with’ a selected monochromatic beam, and an energy dispersive diffraction method in which the monochromator is step-scanned, and the specimen and scintillation counter are fixed. Both methods use the same instrumentation.

Analytical polarized energy-dispersive X-ray fluorescence (PEDXRF) spectrometry (PEDXRFS) represents a substantial advancement over conventional XRF. The higher signal-to-noise commensurate with background lowering and better energy resolution, permits trace analysis for elements with Z ≥ 11. Concomitantly, improvements in analytical software based on the fundamental parameters (FP) approach have improved accuracies and precisions for standard-less analysis (SLA). Two ceramic and soil standard reference materials (SRMs), 98a-Plastic Clay and GSS-1 powders, differed in their intrinsic matrix properties of grain size, bulk, and surface monolayer densities as well as the elemental concentrations. The SRMs were analyzed as powder and as pellets compacted under the same pressure conditions to double the bulk density. Different geometries represented by the sample cup (10, 15, and 24 mm) and pellet (10, 15, and 25 mm) diameters with the same sample thickness (with differing masses and aspect ratios), as well as (for powder samples only) identical low masses (0.5 g) but with varying thicknesses, were analyzed. PEDXRFS combined with TURBOQUANT® (TQ) as SLA-FP enables good quantitative analysis for powders (Z ≥ 13) even for masses significantly lower than recommended, for soil–ceramic samples. Pellets (Z ≥ 12) yielded the best accuracy factor (AF) at high aspect ratio and thicknesses of the matrix analytical depth. Binder in pellets depreciates the AF. TQ needs to adequately quantitate matrix interferences effects, to improve accuracy in the analysis of low atomic numbers, e.g. Na and Mg.

The pharmacy (spezieria) Santa Maria della Scala was founded in Rome by the Discalced Carmelites Order in the 17th century, and during the 18th and 19th centuries it became the official supplier of medicines for Vatican Popes. The laboratory and the cases of this spezieria still preserve glass jars with organic and inorganic materials, which were presumably used for medicine and artistic material preparation, whose composition is unknown to date. A research project was initiated with the aim to study the stored materials and the role that the pharmacy played in regional, national and international contexts. In this manuscript, the compounds were analysed through X-ray powder diffraction with the scope to derive the quantitative mineralogical composition of the inorganic fraction, their possible use in pharmacopoeias and as mineral pigments. Most of the analysed samples are salts (sulphates, chlorides, carbonates, phosphates, borates, sulphides), sulphates being the predominant class; oxides were also detected.

The performances of Seeman-Bohlin (S-B) and Bragg-Brentano (B-B) diffractometers with flat thin film samples were compared on the basis of equal instrumental aberrations. It was found that the S-B arrangement has only a marginal advantage as regards diffracted intensity, and that both types of diffractometer may be successfully employed for characterization of thin films. Diffraction data obtained with very thin metallic films (down to 30 Å) are included for illustration. In order to eliminate reflections from the singlecrystal substrate in the B-B diffractometer, sample tilting was employed. Provided the tilting angle remains within 0.5°, sample tilting causes only moderate additional broadening of the thin film peaks.

High quality powder diffraction data were obtained from a specimen containing inseparable impurities, by using single crystal precession photographs to explore all possible reflections for the mineral being studied. In this manner it is acceptable to ignore weak reflections that do not index on the unit cell and that are not observed on the single crystal photographs. Triphylite is given as an example.

Indexed experimental powder diffraction patterns of Tl,Pb-1223 and Tl-1223 are presented with a method of determining good cell parameters for the former awkward case where c/a almost exactly equals 4. For Tl,Pb-1223, a = 3.814±0.001 Å, c = 15.267±0.005 Å, for Tl-1223, a = 3.814±0.001 Å, c = 15.302±0.005 Å, both tetragonal, space group P4/mmm.

After heat treating, finish machining of the hardened steel represents the last manufacturing step of machine elements. The practically most important operation of grinding is applied to achieve edge zone compressive residual stresses, best surface quality, and dimensional accuracy. Metal removal involves high plastic deformation work. Glide and intersection processes raise the density and produce lower energy substructures of dislocations. The temperature and time behavior of postmachining thermal treatment is analyzed on ground and honed martensitic SAE 52100 rolling bearing steel. Microstructure stabilization is reflected in a large XRD peak width decrease in the surface. The kinetics are modeled by rate-controlling carbide dissolution as the carbon source for Cottrell-type segregation at dislocations. This thermal static strain aging is verified by the formation of a slight white etching surface layer. The model is also extended to consider superimposed thermal dislocation recovery. Both effects are separable. In rolling contact fatigue tests under mixed friction conditions, air reheating below the tempering temperature, which avoids hardness loss, leads to a significant lifetime increase. The effect also occurs after cold working.

X-ray powder diffraction data, unit cell parameters, and space group for alaptide are presented (a=21.136(4) Å, b=7.212(4) Å, c=6.126(3) Å, space group P212121, cell volume=933.8(8) Å3, and Z=4). All measured lines were indexed and are consistent with the P212121 space group. No detectable impurities were observed.

The X-ray powder diffraction pattern of hydrated lithium monoborate LiB(OH)4, sometimes formulated LiBO2·2H2O, has been obtained. Refinements of indexed reflections yielded the following parameters: a = 9.1732(7)Å, b = 7.9622(6)Å, c = 8.5354(8)Å, space group Pbca, Z = 8, Dx = 1.827, Dm = 1.83 g/cm3. The Smith–Snyder figure-of-merit is F30 = 101(0.007,44).

Use of the overlap integral in X-ray diffraction (XRD) powder pattern recognition of crystalline materials is presented. The mathematical expression, derived specifically for diffraction data, provides a measure of similarity between two patterns. Each pattern is represented by a normalized mathematical function. The index of similarity, or overlap integral, indicates how faithfully the two functions overlap and ranges from zero to unity, reaching the latter limit when the two patterns become identical.

A state-of-art semiconductor technology-based position sensitive area detector, namely D/teX-25, has recently been developed for high-speed and high-sensitivity X-ray diffraction (XRD) analysis of materials. X-ray powder diffraction intensities obtained by a D/teX-25 detector were found to over 50 times higher than those by a conventional scintillation counter. A D/teX-25 detector mounted on a conventional 2 kW XRD system has been used to collect ultrafast XRD data with scanning speeds up to 160°2θ per minute. Ultrahigh-speed XRD is particularly useful for time-resolved dynamical and in-situ studies. A D/teX-25 detector was successfully used on a Rigaku XRD differential scanning calorimetry (DSC) system for simultaneous measurements of XRD and DSC data under controlled temperature and humidity conditions. This has made possible the study of complex and rapid phase transformations of pharmaceutical terfenadine. The D/teX-25 area detector has also been used for recording two-dimensional XRD patterns showing the particle-size effects on α-quartz powder intensities and to obtain digital X-ray topographic images of a complex dislocation network in a Si wafer.

A Siemens D500 powder diffractometer has been modified to accommodate data collection and storage by an IBM microcomputer. The interface mechanism, described in detail, is simple, versatile and relatively low cost. The system performance is evaluated and further enhancements suggested.

Phase transformation temperatures of a polycrystalline Ni-rich Ti49.86Ni50.14 shape memory alloy were investigated using a differential scanning calorimeter. In situ structural and texture analyses of the monoclinic Ti49.86Ni50.14 were investigated using neutron powder diffractometer technique. Differential scanning calorimeter results showed that this Ni-rich alloy has a one-step cubic to monoclinic martensitic phase transformation on cooling and a one-step monoclinic to cubic transformation on heating. In situ high-resolution neutron powder diffraction data of the monoclinic phase from low temperatures to room temperature on heating are consistent with the differential scanning calorimeter’s heating results. In addition, the refined monoclinic crystal structure parameters for all neutron diffraction data sets agree satisfactorily with single-crystal X-ray diffraction results. The multiple-data-set capabilities of the GSAS Rietveld refinement program, with a generalized spherical-harmonics description was used successfully to extract the texture description directly from a simultaneous refinement using 52 time-of-flight monoclinic neutron diffraction patterns, taken from a polycrystalline sample held in 13 orientations inside the diffractometer.

The intense interest in production of heteroepitaxial quaternary structures of Gax In1-x Asy p1-y on InP for electro-optical telecommunications systems has Stimulated development of non-destructive techniques for their analysis. One of the most important is double axis X-ray diffractometry, a technique originally developed in the 1920s but only now coming into widespread use as a routine assessment tool. The basic theory is well treated by James and discussion of alignment errors are found in references cited by Fewster in a paper describing alignment procedures for the automated diffractometer manufactured by Bede Scientific Instruments of Durham, The application to III-V systems has been discussed by Tanner, Barnett and Bill.

While conventional X-ray signal readout systems can be used in connection with the electron probe analyzer, new readout techniques can be applied with advantage, particularly for scanning procedures. Several novel techniques involving photographic recordings of oscilloscope tracings will be described. These techniques are applicable to area scanning (enhanced concentration method, concentration mapping with use of X-ray signals, and target current concentration mapping procedures) as well as line scanning. Combinations of area-scanning images with line-scan registration ate used for representing line-scan results.

By using operational amplifiers as signal adders, wavelength scans can be efficiently registered on a Polaroid photogram, with baseline indication and wavelength markers, in a single exposure. Another wavelength scanning technique registers the pulse height of the lines observed during the scanning operation, so that the order of reflection of the lines can be established. The use of an x-y recorder also offers advantages in the registration of line scans. Techniques for registration of multiple scans and for concentration mapping with the x-y recorder will be described.

Diffraction data of calcite were collected using a conventional Bragg–Brentano diffractometer, which is a convenient, low-cost, and highly popular in-house instrument, and its crystal structure was refined by the Rietveld method. This paper shows how one treats preferred orientation and how different refinement strategies affect the accuracy of the result.

X-ray fluorescence (XRF) is a well-established method for quantitative elemental analysis. For accurate quantification, secondary excitation has to be taken into account. In this paper, the secondary excitation process was discussed for analysis by confocal micro-XRF. Experimental depth profiles were shown for a layered sample of Co and Cu. An additional peak was observed in the depth profile of Co, and it was explained by secondary excitation process. Additionally, a Mosaic model was proposed for quantification of confocal micro- XRF analysis.

To interpret highly superimposed diffraction patterns, the Rietveld method together with conventional X-ray powder diffraction techniques were carried out on a series of heat-treated weldments of cast super duplex stainless steel. High temperature processing of this type of alloys causes embrittlement and loss of corrosion resistance owing to precipitation of intermediate phases, principally sigma-phase. The annealing processing of the samples proceeded at temperatures in the range of 800–950 °C for periods of time from 1 to 96 h. This procedure permitted an accurate quantification of the microstructural components such as austenite, ferrite and sigma-phase in all studied samples. The contents of sigma-phase in the heat-affected zones of all weldments reached asymptotical values of 30–38 wt% after 96 h of heat treatment.