A series of FORTRAN IV programs have been written to aid in qualitative x-ray fluorescence (XRF) analysis. These programs have been implemented on a DEC PDP 11/34 computer with an RSX-11M operating system and access the NIH elemental data base (1). The programs and their application to XRF analysis in our laboratory will be described.

Instrumentation has been developed which employs standard x-ray diffraction equipment and an energy dispersive analyzer for elemental and phase analysis. A General Electric XRD-6 diffractometer, a sample chamber, a Nuclear Semiconductor energy dispersive analyzer (EDA) with 155 eV resolution, and a Tracor Northern multichannel analyzer are its main components.

Ferroelectric polycrystalline thin films are being pursued as materials for use in the next generation of radiation hardened nonvolatile semiconductor memories, optical switches and optical computers. Of particular interest are PZT films with a composition near the morphotropic phase boundary. In order to fully understand the the difference in electrical properties as a function of processing parameters it is necessary to fully characterize phase composition and crystallographic properties of these films. Since some films are produced by either spinning or dipping successive layers to obtain the desired thickness it was necessary to compare the properties of each layer.

X-ray diffraction techniques employing parallel beam optics with grazing incidence angle geometry were used to characterize the films. Experimental procedures using sealed tube xray diffraction systems to determine differences in crystallite size and microstrain as a function of depth into the films are a rather unique application of this technique. Discerning the contribution to line broadening due to phase changes, grazing incident angle geometry, crystallite size and microstrain are key to the success of this technique.

This paper discusses the experimental techniques employed and will demonstrate how we were able to successfully determine microstrain as a function of depth into the film. We use transmission electron microscopy (TEM) to aid in the characterization of the films. A brief description of the processing procedures used to produce the films is also provided.

The physical properties of polymer blends consisting of one or more crystallizable components are affected by the microstructure of these materials. In particular, the degree of crystallinity can be influenced by processing parameters, and the crystallinity, as well as the phase distribution, may vary as a function of depth through an injection molded part. Conventional x-ray diffraction techniques can provide information regarding both phase composition and degree of crystallinity, but, because of the relative transparency of these materials to wavelengths generally available in the laboratory, these techniques provide information representative of only the bulk. By employing parallel beam optics at varying grazing incidence angles, the x-ray sampling depth can be varied without loss of resolution, This technique can be used to vary the effective analysis depth from the top several hundred angstroms for low grazing incidence to centimeters for transmission diffraction patterns, Grazing incidence techniques have found initial application in the characterization of thin metallic and ceramic films. This paper demonstrates the feasibility of using parallel beam optics to depth profile low atomic number materials. The specific application of this technique to the characterization of injection molded polymers, including a blend of bisphenol-A polycarbonate (PC) and polybutylene terephthalate (PBT), will be presented.

The automation of analytical equipment is proceeding at a rapid pace, particularly since the introduction of inexpensive microcomputer systems. Most of this equipment has one characteristic in common, that is, they produce digital spectral data. The usual method of recording spectral data has been the strip chart recorder. Strip charts require the hand encoding of position and intensities of the spectral lines. This requires that all of the lines be on scale or that the sample be run several times in order to amplify weaker lines. This problem is eliminated by recording the data digitally. Digital data can then be rapidly plotted on a cathode ray terminal to any desired scale. The user of digital data has access to a great variety of automatic data reduction programs.

A simple gradient heating apparatus was developed and used successfully in growing oriented single crystals of high-purity aluminum suitable for X-ray dinfraction analysis.

Grazing incidence x-ray diffraction (GIXRD) using long soller slit assemblies and a flat crystal monochromator, sometimes referred to as thin film optics, are used to study poly crystal line thin films, polymers, metals, etc. The unique ability of GIXRD to characterize crystalline materials as function of depth and provide accurate strain measurements has lead to the growing popularity of this technique. This non-focusing pseudo-parallel beam geometry can produce various effects on diffraction data which can make interpretation difficult Artifacts such as peak splitting, kα2 distortion, and peaks which shift dramatically as a function of grazing incidence angle are observed when using GIXRD. These artifacts can be related to grazing incidence angle, the divergence of the soller plates, the thickness of the soller plates, the substrate material, and the type of monochromator used. This paper briefly describes some of the topics discussed at the 1992 & 1993 Denver Conferences workshops on parallel beam optics.

Diffraction peaks can occur as unidentifiable peaks in the energy spectrum of an x-ray spectrometric analysis. Recently, there has been increased interest in oriented thin polycrystalline films and epitaxial films on single crystal substrates for electronic applications. Since these materials diffract x-rays more efficiently than randomly oriented polycrystalline materials, diffraction peaks are being observed more frequently in x-ray fluorescent spectra In addition, micro x-ray spectrometric analysis utilizes a small, intense, collimated x-ray beam that can yield well defined diffraction peaks. In some cases these diffraction peaks can occur at the same position as elemental peaks. These diffraction peaks, although a possible problem in qualitative and quantitative elemental analysis, can give very useful information about the crystallographic structure and orientation of the material being analyzed. The observed diffraction peaks are dependent on the geometry of the x-ray spectrometer, the degree of collimation and the distribution of wavelengths (energies) originating from the x-ray tube and striking the sample.

This paper describes the procedures used to retrieve JCPDS powder diffraction data by certain characteristics. These characteristics may include chemistry, mineral name, highest intensity dspacing, largest dspacing, PDF number, etc. The storage scheme used for the powder data and the procedures used to enhance the retrieval speed are described.

Values of the Debye temperature 0 for iron-manganese solid-solution alloys have been determined from X-ray diffracted intensity measurements of powder specimens at ambient temperatures of 310, 239, and 98°K. Corrections to 0 were made with respect to the temperature-dependence of Θ, temperature diffuse scattering, dispersion, volume expansion of the alloy, and the temperature gradient through the specimen. The variation of Θ with temperature has been found to be approximately linear, the value of Θ decreasing 3 % between 98 and SICTK. for a nominal Fe–4%Mn alloy.

Increasing the concentration of manganese in an iron-manganese solid-solution alloy decreases Θ in qualitative agreement with Lindemann's equation. The values of Θ for other s olid-solution alloys computed using Lindemann's equation also agree with reported experimental values of Θ. The Debye temperature of a nominal Fe-3%Mn alloy annealed for 2 hr at 300, 600, and 700°C has not been found to maximize at 600°C as has been reported by Il'ina et al. On the contrary, Θ decreases with increasing annealing temperature until, in the range 600 to 700°C, it reaches its true value; and at these temperatures the powder was found to be fully annealed.

The use of quantitative x-ray diffraction (XRD) as an analytical technique has recently become increasingly popular. There ate primarily two reasons for this increasing interest in a relatively old discipline. The first is simply the need for quantitative phase analysis. This need arises from several sources such as government regulations on respiratory quartz, industrial quality control, and material research. X-ray diffraction provides a readily available technique for bulk phase analysis on chemically similiar phases. For phases which are elementally distinct, our sister science, x-ray fluorescence, can more easily provide the quantitation needed. The second reason for the increasing interest in quantitative XRD is the ready availability of automated powder diffractometers. These instruments remove much of the tedium involved in the collection and reduction of the data.

This paper describes a set of interactive computer programs written in FORTRAN IV and implemented on a POP 11/34 equipped with RLO-2 ten Mbyte discs and an RSX-11M operating system to assist in x-ray diffraction phase analysis. The packing of the data base will be described along with the various interactive programs that access it. The search/match package is designed more as a set of aids for the diffractionist rather than as a single totally automated search/match program, the procedure adapted by many of the xray diffraction (XRD) equipment manufacturers. The approach taken allows the analyst to direct the analysis procedure by utilizing different search/match programs or specifying various options within a given program.

The use of grazing incidence parallel beam x-ray diffraction (GIXRD) in the characterization of lead zirconate titanate (PZT) films is described. This tool has enabled us to depth profile the films. The transmission electron microscopy (TEM) results obtained from a cross section of one film are shown to compliment the GIXRD results. The variation in crystallographic structure versus depth in the film was the primary focus of this study.

The insults from three PZT films having Zr/Ti ratios of 25/75, 48/52, and 75/25 are given. TEM results are reported from the sample with a Zr/Ti ratio of 48/52.

Medical issues facing the aging population are of growing concern with consequences for patients and their caregivers. This study determined the indirect and out-of-pocket costs incurred by the caregivers of elderly patients in Canadian Intensive Care Units (ICUs). Primary family caregivers were surveyed capturing out-of-pocket costs, hours of work, and hours of leisure forgone in providing patient care while the patient was in the ICU. Total costs of care per month were reported across caregiver sex, age, and geographic region. Average out-of-pocket costs were $791 (2016 Canadian dollars) in the first month of ICU care. The mean total cost to family caregivers per patient was $162 per day. Male primary caregivers had higher mean out-of-pocket costs than female caregivers. Subsidization programs covering expenses such as travel, meals, accommodation, and parking are needed to support family caregivers of elderly ICU patients who are incurring considerable out-of-pocket costs.

We examine whether speed is an important characteristic of traders who anticipate local price trends. These anticipatory participants correctly trade prior to the overall market and systematically act before other participants. They use manual and algorithmic order entry methods, but most are not fast enough to be high frequency traders (HFTs). Those anticipating price trends have impacts as if they are informed traders, while the case for anticipatory participants affecting the volume of other traders is rejected. A follow-up sample shows significant attrition in accounts and difficulty maintaining the anticipatory strategies. To identify anticipatory traders, we devise novel methods to isolate local price trends using order book data from the West Texas Intermediate (WTI) crude oil futures market.

Case Description: A 64 year-old male presented with left-sided weakness and altered level of consciousness after a suspected seizure. MR Brain demonstrated right mesial temporal lobe diffusion restriction. Empiric antiviral and antibiotic treatments were initiated despite CSF negative for HSV/VZV and enteroviruses. Lumbar puncture on admission day five was unchanged and empiric treatments were discontinued. On day 13 he deteriorated into status epilepticus necessitating ICU transfer. A third lumbar puncture demonstrated elevated protein and HSV-1 positive PCR. Acyclovir was restarted with guarded prognosis. Discussion: Detection of HSV-1 in CSF is considered the diagnostic gold standard for HSV-1 encephalitis. The validated multiplex assay used in Alberta, Canada has a 95% level of detection significantly better than the recommended threshold for HSV laboratory diagnosis. Previous reports have indicated that CSF PCR may be negative early in the disease course. Others have suggested that initially negative/follow up positive HSV PCR cases may represent secondary reactivation or release from underlying tissue damage. Consideration of the full clinical picture is crucial in patients with HSV negative PCR. Continuation of antiviral therapy may be appropriate in select HSV PCR negative patients.