X-ray fluorescence determination of Ni, Ti and Nb in memory alloys using solution and thin film samples with an internal standard

2019 ◽  
Vol 11 (28) ◽  
pp. 3619-3622
Author(s):  
L. F. Tian ◽  
Y. C. Dai ◽  
D. S. Zou ◽  
T. C. Lei ◽  
S. K. Huang
Keyword(s):  
Thin Film ◽  
Filter Paper ◽  
Internal Standard ◽  
X Ray ◽  
Xrf Analysis ◽  
Fluorescence Determination ◽  
Paper Disk ◽  
Filter Paper Disk

Specimen for XRF analysis of high content of Ni, Ti and Nb in memory alloys, prepared by solution (a) and a filter paper disk (b).

X-ray Spectrographic Microanalysis of Human Urine for Arsenic

1974 ◽  
Vol 28 (2) ◽  
pp. 165-170 ◽  
Author(s):  
James C. Mathies
Keyword(s):  
Standard Deviation ◽  
Human Body ◽  
Human Urine ◽  
Test Paper ◽  
X Ray ◽  
Paper Disk ◽  
Filter Paper Disk ◽  
Relative Standard ◽  
Digestion Mixture

A rapid, precise, and interference-free x-ray spectrographic procedure for the determination of arsenic in human body fluids and tissues has been devised. The organic material in the sample is oxidized, and the arsenic is released by a simplified rapid wet-washing technique using nitric-sulfuric-perchloric acids. The arsenic in the digestion mixture is converted to arsine and collected quantitatively on a silver nitrate-impregnated filter paper disk using a new and convenient sub-micro modification of the Gutzeit arsine generator. The arsenic in the test paper is rapidly and nondestructively quantitated to the nearest 0.1 µg in the x-ray spectrograph. The method is relatively free of the interferences usually associated with Gutzeit and colorimetric techniques for arsenic. The precision of the method is indicated by the fact that 5 µg of arsenic can be quantitated with a relative standard deviation of 2.5% or less. Normal levels of arsenic in human urine have been redetermined.

X-Ray Spectrometric Determination of Composition and Distribution of Sublimates in Receiving-Type Electron Tubes*

1963 ◽  
Vol 7 ◽  
pp. 566-583 ◽  
Author(s):  
Eugene P. Bertin ◽  
Rita J. Longobucco
Keyword(s):  
Film Studies ◽  
Normal Operation ◽  
Point Mapping ◽  
X Ray ◽  
Electron Tube ◽  
Barium Strontium ◽  
Paper Disk ◽  
Filter Paper Disk ◽  
Small Parts

AbstractDuring the normal operation of conventional receiving-type electron tubes, certain metallic elements, such as barium, strontium, nickel, and manganese, sublime from the hot cathode and deposit on cooler parts of the tube. This process gradually impairs the performance of the tube and may eventually limit its useful life. This paper describes some applications of a variety of X-ray spectrometric techniques to the qualitative and quantitative analysis of these sublimates and to the mapping of their distribution on various surfaces in the tubes.All work was done on a standard commercial X-ray spectrometer, but specially designed accessories are described for mounting and rotating small parts in the primary X-ray beam and for confining the beam to these parts. Procedures are given for analysis of microgram deposits on electron-tube cathodes, grids, plates, micas, and bulbs by both nondestructive and filter-paper-disk techniques. Procedures are given for point-by-point mapping of the distribution of sublimates over the surfaces of these parts by use of a commercial “X-ray probe” selectedarea accessory in conjunction with a curved crystal to give increased intensity. Procedures are given for various techniques for calibrating all the analytical methods, including preparation of thin films of known composition.The results of some typical electron tube studies are described and illustrated. The approximate sensitivity of the methods for determination of total sublimate is, in micrograms per part, 0.1 for barium, strontium, and manganese and 0.05 for nickel. The approximate sensitivity for mapping sublimate distribution with a 1-mm aperture is, in micrograms per square centimeter, 1 for barium, strontium, and manganese and 0.5 for nickel. Although the techniques described are applied specifically to sublimates in electron tubes, they are also readily applicable to analysis of specks and films on other small parts and to thin-film studies in general

Determination of Stoichiometry of GaAs Component in (Gaas)Ge Epitaxially Grown Thin Films by Electron Microprobe X-Ray Analysis

1990 ◽  
Vol 48 (2) ◽  
pp. 264-265
Author(s):  
D. R. Liu ◽  
S. S. Shinozaki ◽  
R. J. Baird
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Monte Carlo Simulation ◽  
Monte Carlo ◽  
Compound Semiconductors ◽  
Energy Dispersive Analysis ◽  
X Ray ◽  
Metastable Alloys ◽  
Lower Voltage

The epitaxially grown (GaAs)Ge thin film has been arousing much interest because it is one of metastable alloys of III-V compound semiconductors with germanium and a possible candidate in optoelectronic applications. It is important to be able to accurately determine the composition of the film, particularly whether or not the GaAs component is in stoichiometry, but x-ray energy dispersive analysis (EDS) cannot meet this need. The thickness of the film is usually about 0.5-1.5 μm. If Kα peaks are used for quantification, the accelerating voltage must be more than 10 kV in order for these peaks to be excited. Under this voltage, the generation depth of x-ray photons approaches 1 μm, as evidenced by a Monte Carlo simulation and actual x-ray intensity measurement as discussed below. If a lower voltage is used to reduce the generation depth, their L peaks have to be used. But these L peaks actually are merged as one big hump simply because the atomic numbers of these three elements are relatively small and close together, and the EDS energy resolution is limited.

Problems in Thin-Film X-ray Quantification

1990 ◽  
Vol 48 (2) ◽  
pp. 458-459
Author(s):  
J N Chapman ◽  
W A P Nicholson
Keyword(s):  
Thin Film ◽  
Specimen Thickness ◽  
X Rays ◽  
Characteristic Peak ◽  
Local Composition ◽  
X Ray ◽  
Measured Ratio ◽  
Path Lengths ◽  
Composition Changes

Energy dispersive x-ray microanalysis (EDX) is widely used for the quantitative determination of local composition in thin film specimens. Extraction of quantitative data is usually accomplished by relating the ratio of the number of atoms of two species A and B in the volume excited by the electron beam (nA/nB) to the corresponding ratio of detected characteristic photons (NA/NB) through the use of a k-factor. This leads to an expression of the form nA/nB = kAB NA/NB where kAB is a measure of the relative efficiency with which x-rays are generated and detected from the two species.Errors in thin film x-ray quantification can arise from uncertainties in both NA/NB and kAB. In addition to the inevitable statistical errors, particularly severe problems arise in accurately determining the former if (i) mass loss occurs during spectrum acquisition so that the composition changes as irradiation proceeds, (ii) the characteristic peak from one of the minority components of interest is overlapped by the much larger peak from a majority component, (iii) the measured ratio varies significantly with specimen thickness as a result of electron channeling, or (iv) varying absorption corrections are required due to photons generated at different points having to traverse different path lengths through specimens of irregular and unknown topography on their way to the detector.

X-ray fluorescence determination of zinc sulfate in acidic zinc plating electrolyte

2020 ◽  
Vol 86 (10) ◽  
pp. 18-22
Author(s):  
K. N. Vdovin ◽  
K. G. Pivovarova ◽  
N. A. Feoktistov ◽  
T. B. Ponamareva
Keyword(s):  
Zinc Sulfate ◽  
Zinc Coating ◽  
Electrolyte Composition ◽  
Complexometric Titration ◽  
X Ray ◽  
Fluorescence Determination ◽  
Zinc Plating ◽  
Zinc Determination

Zinc sulfate is the main component in the composition of the acidic zinc plating electrolyte. Deviation in the electrolyte composition from the optimum content leads to destabilization of the electrolysis process and deteriorate the quality of the resulting zinc coating. The proper quality of a zinc coating obtained by galvanic deposition can be ensured only with timely monitoring and adjustment of the electrolyte composition. A technique of X-ray fluorescence determination of zinc (in terms of zinc sulfate) in an acidic zinc plating electrolyte is proposed. The study was carried out using an ARL Quant’X energy dispersive spectrometer (Thermo Fisher Scientific, USA) with a semiconductor silicon-lithium detector. The features of the spectrometer design are presented. The optimal parameters of excitation and detection of zinc radiation were specified when the electrolyte sample was diluted 1:1000. The ZnKα1 line was used as an analytical line. The plotted calibration graph is linear, the correlation coefficient being 0.999234. The results of zinc determination according to the developed method were compared with the data of the reference method of complexometric titration to prove the reliability of the procedure. The results are characterized by good convergence and accuracy. The proposed method of X-ray fluorescence zinc determination in a zinc plating electrolyte equals complexometric titration in the limiting capabilities and even exceeds the latter in terms of the simplicity of sample preparation and rapidity. The developed method of X-ray fluorescence determination of zinc is implemented in analysis of the electrolyte used in the continuous galvanizing unit at «METSERVIS LLC».

X-Ray Fluorescence Determination of Ore Elements in Ferromanganese Formations

2020 ◽  
Vol 56 (14) ◽  
pp. 1423-1430
Author(s):  
V. M. Chubarov ◽  
A. A. Amosova ◽  
A. L. Finkelshtein
Keyword(s):  
X Ray ◽  
Fluorescence Determination

Quantitative Determination of some Carbonate Minerals in Greenschist Facies Meta-volcanic Rocks

1972 ◽  
Vol 9 (1) ◽  
pp. 36-42 ◽  
Author(s):  
Calvert C. Bristol
Keyword(s):  
Standard Deviation ◽  
Quantitative Determination ◽  
Volcanic Rocks ◽  
Internal Standard ◽  
Greenschist Facies ◽  
Carbonate Mineral ◽  
Mineral Contents ◽  
X Ray ◽  
Fine Grained

X-ray powder diffraction methods, successful in quantitative determination of silicate minerals in fine-grained rocks, have been applied to the determination of calcite, dolomite, and magnesite in greenschist facies meta-volcanic rocks. Internal standard graphs employing two standards (NaCl and Mo) have been determined.Carbonate mineral modes (calcite and dolomite) for 6 greenschist facies meta-volcanic rocks obtained by the X-ray powder method have been compared to normative carbonate mineral contents calculated for the same rocks. This comparison showed a maximum variation of 7.7 wt.% between the X-ray modes and the normative carbonate mineral contents of the rocks. Maximum standard deviation for the X-ray modes of these rocks was equivalent to 4.4 wt.%.

Total reflection X-ray Fluorescence determination of interfering elements rubidium and uranium by profile fitting

2018 ◽  
Vol 144 ◽  
pp. 87-91 ◽  
Author(s):  
Sangita Dhara ◽  
Ajay Khooha ◽  
Ajit Kumar Singh ◽  
M.K. Tiwari ◽  
N.L. Misra
Keyword(s):  
Total Reflection ◽  
X Ray ◽  
Fluorescence Determination ◽  
Profile Fitting

Rapid X-Ray Fluorescence Determination of Sulfur in Mineralized Rocks from the Bingham Mining District, Utah

1970 ◽  
Vol 24 (4) ◽  
pp. 426-428 ◽  
Author(s):  
Brent P. Fabbi ◽  
William J. Moore
Keyword(s):  
Mining District ◽  
Total Sulfur ◽  
Ground Sample ◽  
X Ray ◽  
Incomplete Oxidation ◽  
Fluorescence Determination

Determination of total sulfur by x-ray fluorescence eliminates problems of incomplete oxidation of sulfur or coprecipitation often encountered in gravimetric analyses. Durable pellets are prepared from finely ground sample powders mixed with chromatographic cellulose. X-ray fluorescence total sulfur values compare well with gravimetric sulfur values.

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