Quantitative analysis with a two-detector measuring system in in-air PIXE-design to improve detection sensitivity at low energies

2013 ◽  
Vol 23 (01n02) ◽  
pp. 55-67 ◽  
Author(s):  
K. Sera ◽  
S. Goto ◽  
C. Takahashi ◽  
Y. Saitoh

In this paper, a two-detector measuring system in in-air PIXE system composed of two Si(Li) detectors has been developed for simultaneous measurement of low- and high-Z elements. In order to improve detection sensitivity of the detector for low energy region, a new device which is attached at the tip of the detector has been designed. It is made of acryl and has a thin end on which a 1.5 μm-thick Mylar film is stuck. As a result, it exhibited a miraculous effect in improving detection sensitivity at low energies and it became possible to detect K X-rays of aluminium. In order to perform quantitative analysis in in-air system, we have measured detection efficiencies for the two Si(Li) detectors including the effect of X-ray absorption in air on the basis of the method that we developed. Concerning the beam energy at the target and corresponding X-ray production cross-sections, the same values as were reported in the previous paper were applicable since conditions of irradiating system were unchanged. It was confirmed that the new method allows us to quantitatively analyze all the elements heavier than aluminum and to obtain mostly the same results as those by in-vacuum PIXE for various kinds of samples. Accuracy of analysis was also confirmed by using a standard material.

2007 ◽  
Vol 17 (01n02) ◽  
pp. 1-10 ◽  
Author(s):  
K. SERA ◽  
K. TERASAKI ◽  
J. ITOH ◽  
Y. SAITOH ◽  
S. FUTATSUGAWA

A physical method of quantitative analysis for in-air PIXE has been established. Among the three parameters required for performing physical analysis, X-ray production cross sections were recalculated by using the effective energy of the proton beam after losing its energy through a Kapton foil and in air. Detection efficiencies of the Si ( Li ) detector have been determined according to our method established for in vacuum system, where effects of absorption of X-rays in air are incorporated into the detection efficiencies. As a result, it is confirmed that the present method gives us accurate results in the analyses of standard samples as well as actual samples such as soil and ash. It becomes possible to perform quantitative analysis of various samples by optimizing the measuring conditions depending on the samples.


Author(s):  
Y. Sato ◽  
T. Hashimoto ◽  
M. Ichihashi ◽  
Y. Ueki ◽  
K. Hirose ◽  
...  

Analytical TEMs have two variations in x-ray detector geometry, high and low angle take off. The high take off angle is advantageous for accuracy of quantitative analysis, because the x rays are less absorbed when they go through the sample. The low take off angle geometry enables better sensitivity because of larger detector solid angle.Hitachi HF-2000 cold field emission TEM has two versions; high angle take off and low angle take off. The former allows an energy dispersive x-ray detector above the objective lens. The latter allows the detector beside the objective lens. The x-ray take off angle is 68° for the high take off angle with the specimen held at right angles to the beam, and 22° for the low angle take off. The solid angle is 0.037 sr for the high angle take off, and 0.12 sr for the low angle take off, using a 30 mm2 detector.


2001 ◽  
Vol 7 (S2) ◽  
pp. 340-341
Author(s):  
Peter Miller

Quantitative analysis in the TEM by EELS or EDXS depends on the K-factor method in which uniform ionization, independent of specimen orientation and thickness, is assumed. This assumption is of limited validity for crystals, where channeling of the electron wave ψ affects the ionization rate as observed in both energy loss and X-ray signals. Both EELS and EDXS are sensitive to changes in ψψ*near the atomic sites, and this variation as a function of crystal orientation forms the basis for ALCHEMI. Simultaneously recorded EELS and EDXS spectra were used to monitor changes in Cu/Ba ratio from YBaCu-oxides using L2,3/M4,5 ionization edges or K/L X-rays respectively. Although the acceptance aperture for EELS (11 mrad at 300 keV) may not be sufficiently large to mask double-channeling effects, it is small enough that momentum transfer is sufficiently limited to enhance derealization. Thus it is expected that the EELS signal should be less sensitive to crystal orientation than EDXS (an estimate of impact parameters yields 0.73 and 0.61 Å for the Ba and Cu energy loss signals, reducing to 0.06 and 0.04 Å respectively for X-ray emissions).


2001 ◽  
Vol 7 (S2) ◽  
pp. 700-701
Author(s):  
Ning Gao ◽  
David Rohdeb

An inevitable consequence of the presence of the gas in the sample chamber of a low-vacuum scanning electron microscope (LV-SEM) and environmental SEM (ESEM) is the electron beam broadening due to the scattering in the gas. The electron broadening has a large impact on x-ray analysis because the fluorescent characteristic x rays generated far from the center of the electron probe form a high background, which reduces the detection sensitivity of x-ray analysis and degrades the x-ray image contrast. We report in this paper of using a polycapillary focusing x-ray optic between the sample and the energy-dispersive spectrometer as a spatial filter to filter out unwanted x-rays generated far from the specimen. As a result, the x-ray image contrast and the detection sensitivity of the system were notably improved.A polycapillary focusing optic collects a large solid angle of x rays from an x-ray source of small area at its input focus, guide them through the curved channels by multiple external total reflections, and focus them to the output focus.


1987 ◽  
Vol 93 ◽  
pp. 281-292
Author(s):  
W. Pietsch ◽  
W. Voges ◽  
E. Kendziorra ◽  
M. Pakull

AbstractThe 805 sec pulsing X-ray source H2252−035 has been observed for 7 h on September 14/15 and on September 17, 1983 in X-rays with the low energy telescope and the medium energy detectors of EXOSAT. While below 2 keV the semiamplitude of the 805 s pulses is ~ 100% in the 2.3–7.9 keV band it is only ~ 40%. X-ray dips that are more pronounced in low energies occur simultaneously with the orbital minimum of the optical light curve. The medium energy spectra during dips with respect to the non dip spectrum can be explained by just enhanced cold gas absorption of an additional absorbing column of 2 1022 cm−2. Model spectra for the 805 s minimum have to include a strong iron emission line at 6.55 keV with an equivalent width of 3 keV in addition to a reduced continuum intensity (radiating area) and enhanced low energy absorption.


2020 ◽  
Vol 108 (5) ◽  
pp. 415-423
Author(s):  
Esra Cinan ◽  
Bünyamin Aygün ◽  
M. I. Sayyed ◽  
Yüksel Özdemir

AbstractL X-ray intensity ratios for CeO2, Sm2(SO4)3, Ho2O3, and Yb2O3 compounds were experimentally investigated. The measurements were gauged following excitation by 59.54 keV γ-rays from a 100 mCi 241Am radioactive annular source at different temperatures in situ. Temperature change occurred between 50 °C and 400 °C. L X-ray emission spectra were obtained by using a solid-state Si(Li) X-ray detector. L X-ray production cross sections, intensity ratios, and full-width half maximum (FWHM) values for the compounds were determined by evaluating the emission spectra varying with the temperature. According to the results obtained, it was observed that Lβ1 X-rays were less influenced in comparison with Lα X-rays while Lα X-rays were also less influenced in comparison with Lβ2 X-rays.


1995 ◽  
Vol 10 (3) ◽  
pp. 170-172
Author(s):  
Stefano Battaglia

A technique is presented utilizing an unmodified commercial X-ray diffractometer, equipped with a Bragg–Brentano geometry, for reducing preferred orientation effects in measured intensities during quantitative diffraction analysis. The diffractometer setup examined makes possible data acquisition with Θ fixed at 1° and 2Θ scanning the Bragg line. The results obtained with this technique are shown in the quantitative X-ray diffraction analysis of three international standards of carbonate rocks (401,402,403).


2017 ◽  
Vol 890 ◽  
pp. 223-226 ◽  
Author(s):  
Rıdvan Durak ◽  
Ferdi Akman ◽  
Abdulhalik Karabulut

The Ll, Lα and Lβ X-ray production cross sections for Pr, Nd, Sm, Eu, Gd and Tb elements were determined using a reflection geometry. The excitation was performed with a 241Am radioactive annular source and the L X-rays emitted from targets were counted with a high-resolution Si (Li) detector. The experimental values were compared with other available experimental results and theoretical data. An agreement is observed between the measured and other experimental results or theoretical data.


2004 ◽  
Vol 14 (01n02) ◽  
pp. 9-18 ◽  
Author(s):  
K. SERA ◽  
K. TERASAKI ◽  
Y. SAITOH ◽  
J. ITOH ◽  
S. FUTATSUGAWA ◽  
...  

We recently developed and reported a three-detector measuring system making use of a pure-Ge detector combined with two Si ( Li ) detectors. The efficiency curve of the pure-Ge detector was determined as relative efficiencies to those of the existing Si ( Li ) detectors and accuracy of it was confirmed by analyzing a few samples whose elemental concentrations were known. It was found that detection of fluorine becomes possible by analyzing prompt γ-rays and the detection limit was found to be less than 0.1 ppm for water samples. In this work, a method of quantitative analysis of fluorine has been established in order to investigate environmental contamination by fluorine. This method is based on the fact that both characteristic x-rays from many elements and 110 keV prompt γ-rays from fluorine can be detected in the same spectrum. The present method is applied to analyses of a few environmental samples such as tealeaves, feed for domestic animals and human bone. The results are consistent with those obtained by other methods and it is found that the present method is quite useful and convenient for investigation studies on regional pollution by fluorine.


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