Escape Peaks in X-Ray Diffractometry*

1964 ◽  
Vol 8 ◽  
pp. 118-133 ◽  
Author(s):  
William Parrish

AbstractEscape peaks occur when the incident X-ray quantum, energy exceeds the absorption edge energy of the detector element and the resulting X-ray fluorescence is lost from the detector. The most common escape peaks result from 1 K-fluorescence in NaI-scintillation counters and Xe K-, Xe L-, and Kr K-fluorescence in proportional counters. The average pulse amplitude of the escape peak is proportional to the difference of the Energies of the incident and fluorescent X-rays. If the intensity of the escape peak is high as in the case of Mo Kα and a kryptoopreportional counter, and the lower level of the pulse height analyzer is raised to reject the escape peak, the quantum counting efficiency may be reduced by a factor of two. When the pulse height analyzer is set for characteristic incident radiation, escape peaks appear in powder patterns at small diffraction angles. These broad low-intensity peaks are often mistakenly identified as resulting from misalignment, scattering, etc. Each powder reflection can produce its own escape peak which occurs at an angle slightly smaller than the absorption edge of the detector element. In a silicon powder pattern the three strongest reflections produce three resolved escape peaks whose peak intensities are about 4% of their corresponding Cu Kα peaks when the X-ray tube is operated at 50 kV. The escape peak intensities decrease with decreasing X-ray tube voltage and disappear when the voltage is lower than the absorption edge energy of the detector element. Absorption edge peaks observed without the upper level of the pulse height analyzer are similar in appearance, intensity, and diffraction angle to the escape peaks. In complex powder patterns the escape peak pattern is unresolved and may produce a number of very broad peaks.

1959 ◽  
Vol 3 ◽  
pp. 11-39
Author(s):  
Charles G. Dodd

AbstractThe applications of X-ray emission or fluorescent spectrography to chemical analysis have increased spectacularly in recent years, but little attention has been paid to the potentialities of X-ray absorption techniques. Monochromatic X-ray absorption-edge spectrometry, in particular, is most promising. The ultimate sensitivity of absorption-edge spectrometry probably will be less than that of fluorescent analysis, but this disadvantage may be outweighed by the convenience, economy, and absence of matrix effects with the former method. Both methods appear limited in application only to certain elements.A pulse height analyzer coupled with scintillation and proportional counter detection has been found to permit an increase in sensitivity of absorption-edge spectrometry, primarily because controlled window widths may be utilized in determining transmitted X-ray intensities with a sealer. Further work has led to the development of a new rapid, convenient technique known as “differential pulse amplitude distribution (PAD) peak height analysis.” Work carried out during the development of the new method is described.


1968 ◽  
Vol 46 (10) ◽  
pp. S437-S443 ◽  
Author(s):  
Laurence E. Peterson ◽  
Allan S. Jacobson ◽  
R. M. Pelling ◽  
Daniel A. Schwartz

Observations of cosmic X-ray sources have been made from high-altitude balloons over Palestine, Texas, using actively collimated detectors. In this technique, a thin NaI central counter 10 to 50 cm2 in area is surrounded by a CsI well crystal shield several centimeters thick. The aperture, about 8° to 20° FWHM, is determined by either the well opening or an active honeycomb collimator. The background is determined mainly by diffuse cosmic and atmospheric X-rays entering the forward aperture. The detector is usually either servo-controlled to track the source or operated as a meridian device. Data are telemetered over the 20–250 keV range in a digital format from a 128-channel pulse-height analyzer. Several strong sources in the northern hemispheric sky have been observed. The Crab nebula has a power-law differential number spectrum with an index of –1.9 ± 0.1 and an intensity of about 10−2 photons/cm2-s-keV at 20 keV. Two observations in September 1965 and September 1966 on this object give the same flux and spectral index within about 5% over the 20–100 keV range. The source Cygnus XR-1 also has a power-law shape, very similar in slope and intensity to the Crab, which extends above background to at least 180 keV. These measurements are in general agreement with those of other workers. The power-law spectrum of the Crab and Cygnus XR-1 may be contrasted with that of SCO XR-1, which has an exponential spectrum, typical of a hot gas at 50 × 106 °K.


Author(s):  
R. L. Stears

Because of the nature of the bacterial endospore, little work has been done on analyzing their elemental distribution and composition in the intact, living, hydrated state. The majority of the qualitative analysis entailed intensive disruption and processing of the endospores, which effects their cellular integrity and composition.Absorption edge imaging permits elemental analysis of hydrated, unstained specimens at high resolution. By taking advantage of differential absorption of x-ray photons in regions of varying elemental composition, and using a high brightness, tuneable synchrotron source to obtain monochromatic x-rays, contact x-ray micrographs can be made of unfixed, intact endospores that reveal sites of elemental localization. This study presents new data demonstrating the application of x-ray absorption edge imaging to produce elemental information about nitrogen (N) and calcium (Ca) localization using Bacillus thuringiensis as the test specimen.


1967 ◽  
Vol 11 ◽  
pp. 249-274 ◽  
Author(s):  
J. R. Rhodes ◽  
T. Furuta

AbstractA portable, battery-operated X-ray fluorescence analyzer weighing 15 lb is described, consisting of a Nal(Tl) scintillation-counter probe and an electronic unit with a single-channel pulse-height analyzer and reversible scaler. Radioisotope X-ray sources are used for excitation of the sample and, where necessary, balanced filters for resolution of neighboring characteristic X-rays. Emphasis has been placed on designing and producing an instrument that is easy and convenient to operate in laboratory, factory, or field conditions and that can equally well be used to measure extended surfaces, such as rock faces, or finite samples in the form of powders, briquettes, or liquids. The feasibility of the following analyses has been studied by using for each determination the appropriate radioisotope source and filters: sulfur in coal; calcium and iron in cement raw mix; copper in copper ores; and vanadium, chromium, molybdenum, and tungsten in steels. Detection limits, based on counting statistics obtained in count times of 10 to 100 sec, range from 0.03% for copper in ores to 0.2% for sulfur in coal. Both matrix absorption and enhancement effects were encountered and were eliminated or reduced substantially by suitable choice of source energy, by the use of nomograms, or by semiempirical correction factors based on attenuation or scattering coefficients.


1960 ◽  
Vol 4 ◽  
pp. 370-381
Author(s):  
Kurt F.J. Heinrich

AbstractPulse-height analysis is a valuable tool in X-ray fluorescence analysis, both for qualitative and quantitative purposes. The elimination of higher order interferences permits determinations that would otherwise be very difficult or impossible, The systematic application of pulse-height analysis in qualitative work greatly simplifies the interpretation of complex spectra. In certain cases one can apply nondispersive analysis, relying on the pulse-height analyzer alone for separating energy levels of X-ray photons. Technique and limitations of pulse-height analysis will be discussed.


1971 ◽  
Vol 15 ◽  
pp. 388-406 ◽  
Author(s):  
Ernest J. Franzgrote

The analysis of alpha-excited X-rays has been studied as a possible addition to the alpha-scattering technique used on the Surveyor spacecraft for the first in situ chemical analyses of the lunar surface.Targets of pure elements, simple compounds, and silicate rocks have been exposed to alpha particles and other radiation from a curium-214 source and the resulting X-ray spectra measured by means of a cooled lithium-drifted silicon detector and pulse-height analysis.Alpha-particle bombardment is a simple and efficient means of X-ray excitation for light elements. Useful spectra of silicate rocks may be obtained in a few minutes with a source activity of 50 millicuries, a detector area of 0.1 cm2 and a sample distance of 3 cm. An advantage over electron excitation is the higher characteristic response relative to the bremsstrahlung continuum. Peak-to- background ratios of greater than 100 to 1 have been obtained for elemental targets. Relative efficiencies of X-ray excitation by alpha particles and by X-rays from the curium source have been determined.Resolution of the detector system used is approximately 150 eV for the lighter elements. This is sufficient to resolve the Kα X-rays of the geochemically important elements, Na, Mg, Al, and Si in silicate rocks. Although these and lighter elements are analyzed as well or better by the alpha-scattering and alpha-proton technique, the X-ray mode enables results to be obtained more quickly.The study shows that the addition of an X-ray mode to the alpha-scattering analysis technique would result in a significant improvement in analytical capability for the heavier elements. In particular, important indicators of geochemical differentiation such as K and Ca (which are only marginally separated in an alpha-scattering and alpha-proton analysis) may be determined quantitatively by measuring the alpha-excited X-rays. An X-ray detector is under consideration as an addition to an alpha-scattering instrument now under development for possible use on a Mars-lander mission.


1971 ◽  
Vol 15 ◽  
pp. 285-294 ◽  
Author(s):  
J. H. McCrary ◽  
Ted Van Vorous

Recently developed, miniature, steady state, field emission tubes are finding application in several areas of x-ray analysis. These tubes require only a high voltage, low current power supply to produce relatively intense beams of x-rays. Since anodes can be fabricated from almost any element, and since the tubes can be operated at potentials up to about 70 kV, many different output x-ray spectra are available. Miniaturized battery operated x-ray sources of this type, occupying a volume of about one liter, have several advantages over radioisotope sources. These include cost, safety, and controllable output spectra and intensity. X-ray sources for energy dispersive fluorescence analyzers are designed so that no scattered characteristic radiations will interfer with the analysis of the sample fluorescence. Sources which are essentially monoenergetic can be fabricated for use in non-dispersive x-ray fluorescence analyzers. Because of the intensity and safety of the field emission tubes, such analyzers can be made which are sensitive while compact, portable, and inexpensive. In x-ray absorption analysis the measurement of absorption edge jump ratios provides a quantitative measure of sample impurities. Field emission tubes whose output spectra consist primarily of bremsstrahlung are particularly well suited to such measurements. The techniques involved in using these tubes in x-ray analysis are described.


1972 ◽  
Vol 16 ◽  
pp. 322-335 ◽  
Author(s):  
Davis Carpenter ◽  
John Thatcher

AbstractA comparison of the relative merits of the energy dispersive derector-pulse height analyzer, scintillation detector-graphite monochromator, and proportional detector-pulse height analyzer combinations.Typical energy dispersive detectors are not configured for maximum efficiency on the diffractometer. Being only on the order of 3 mm diameter, a good deal of the available information is not collected by the detector. This is especially true with the Wide optics found in modern diffractometers. The energy dispersive detector incorporated into this system is optimized for the x-ray diffractometer. Its detection area is a 1.25 X 0.25 inch rectangle. The resolution is only sufficient to remove the Kβ portion of the spectrum.Conventional diffractometer techniques incorporate either a scintillation detector-crystal monochromator, or a proportional detector-pulse height analyser combination. The question posed is “what are the advantages in signal to noise ratio and pulse height distribution of the energy dispersive-pulse height analyzer over the more conventional arrangements.”


1960 ◽  
Vol 4 ◽  
pp. 117-129
Author(s):  
W. L. Kehl

AbstractA diffractometer equipped with a gas proportional counter and pulse-height analyzer provides a very satisfactory means of recording the X-ray diffraction patterns of chromium-containing materials with Cu Kα radiation. The fluorescent chromium K radiation can be rejected along with much of the white background radiation without appreciable loss of Cu Kα intensity, and the advantages of copper over chromium or molybdenum radiation can be fully utilized. This is illustrated by an X-ray diffraction study of coprecipitated chromia-alumina catalysts, in which the chromium concentration varies between 0 and 37 w, %. At each chromium concentration the precipitate was studied in the washed and dried state, as well as after calcination at 500, 750, and 1400°C. X-ray diffraction patterns are presented to show the phase transformations and sample inhomogenelties that were observed.


2007 ◽  
Vol 2 ◽  
pp. S1069-S1069 ◽  
Author(s):  
Sadatsugu MUTO ◽  
Shigeru MORITA ◽  
LHD Experimental Group

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