Lateral resolution of the electron microbeam analysis

Author(s):  
H.J. Dudek

The chemical inhomogenities in modern materials such as fibers, phases and inclusions, often have diameters in the region of one micrometer. Using electron microbeam analysis for the determination of the element concentrations one has to know the smallest possible diameter of such regions for a given accuracy of the quantitative analysis.In th is paper the correction procedure for the quantitative electron microbeam analysis is extended to a spacial problem to determine the smallest possible measurements of a cylindrical particle P of high D (depth resolution) and diameter L (lateral resolution) embeded in a matrix M and which has to be analysed quantitative with the accuracy q. The mathematical accounts lead to the following form of the characteristic x-ray intens ity of the element i of a particle P embeded in the matrix M in relation to the intensity of a standard S

2003 ◽  
Vol 321 (2-3) ◽  
pp. 221-232 ◽  
Author(s):  
A Yilmazbayhan ◽  
O Delaire ◽  
A.T Motta ◽  
R.C Birtcher ◽  
J.M Maser ◽  
...  

2021 ◽  
pp. 124-131
Author(s):  
A.V. Alekseev ◽  
◽  
G.V. Orlov ◽  
P.S. Petrov ◽  
A.V. Slavin ◽  
...  

The determination of the elements Cu, Ni, Sb, Bi, Pb, Zn and Fe in the tin-based solder VPr35, as well as the elements Sn, Ni, Sb, Bi and In in the lead-based VPr40 solder by the method of х-ray fluorescence spectroscopy has been carried out. The calibration dependences are corrected taking into account the superposition of signals from interfering elements on the analytical signal and changes in intensity caused by inter-element influences in the matrix. The analysis was carried out by the method of fundamental parameters without using standard samples. The correctness of the results obtained was confirmed by their comparative analysis by atomic emission spectroscopy and high-resolution mass spectrometry with a glow discharge.


2001 ◽  
Vol 56 (2) ◽  
pp. 187-201 ◽  
Author(s):  
F Bosch-Reig ◽  
J.V Gimeno-Adelantado ◽  
S Sánchez-Ramos ◽  
D.J Yusá-Marco ◽  
F Bosch-Mossi

1991 ◽  
Vol 35 (B) ◽  
pp. 1205-1209
Author(s):  
I. A. Kondurov ◽  
P. A. Sushkov ◽  
T. M. Tjukavina ◽  
G. I. Shulyak

In multielement EDXRF analysis of very complex unknowns, some problems in data evaluation may be simplified if one can take into account a priori information on the properties of the incident and detected radiations, and also available data on the matrix of the sample. The number of variables can be drastically shortened in the LSM procedures in this case. One of the best examples of complex unknowns is the determination of the rare earth element content of ores, and most recently in samples of high temperature superconductors (HiTc).


1968 ◽  
Vol 12 ◽  
pp. 546-562
Author(s):  
R. Tertian

AbstractThe double dilution method has many important advantages. For any element to be determined, let us say A, It enables us to control or calculate the matrix factor (sum of the absorption end enhancement effects) for the sample being Investigated towards A radiation, and it furnishes corrected Intensities which are strictly proportional to A concentration. Thus the results are exact, whatever the general composition of the sample, their accuracy depending only on the quality of measurement and preparation. Another major practical advantage is that the method does not require systematic calibration but only a few permanent standards consisting of a pure compound or of an accurately known sample.The procedure has been tested successfully for accurate determination of rare earth elements using, for solid materials such as ores and oxide mixtures, the borax fusion technique. It also can be readily applied to liquids. All the rare earth elements can be titrated by that method, as well as yttrium, thorium and, if necessary, all the elements relevant to X-ray fluorescence analysis. The concentration range considered for solids is of one comprised between 0.5 and 100 % and, with a lesser accuracy, between 0.1 and 0-5 % Examples are given relative to the analysis of various ores. Finally it rcust be pointed out that the method is universal and applies to the analysis of every solid, especially ores, provided that they can be converted to solid or liquid solutions. It appears that most industrial analyses can be worked on In this way.


1963 ◽  
Vol 7 ◽  
pp. 542-554
Author(s):  
Frank L. Chan

AbstractRecently, interest in the determination of selenium in trace amounts has been greatly intensified because of the nutritional aspects of this element. It has been reported that selenium in the amount of 13 μg in the form of sodium selenite in 100 g of feed has an effect similar to that of vitamin E. In the field of semiconductors, the detection and determination of trace amounts of selenium in arsenic, antimony, and small single crystals of solid solution of cadmium selenide and sulfide are of considerable importance in semiconductor performance.In the Aerospace Research Laboratories, 4,5 diamino-6-tbiopyi-imidine has been successfully adopted as a reagent for the spectrophotometric determination of selenium. The reaction of 4,5 diamino-6-thiopyrimidine and tetxavalent selenium produces a yellow color with the formation of elemental selenium. It is possible to determine elemental selenium by collecting it in a thin layer. The selenium deposited in this layer may then be determined by an X-ray fluorescence method. A procedure of this nature has the advantage of eliminating the matrix effects commonly encountered in X-ray fluorescence. Furthermore, the slow generation of selenium affords a convenient means of detection and confirmation of this element by the use of X-ray diffraction procedures. By this technique selenium is first converted to its tetravalent state and is then reacted with 4,5 diamino-6-thiopyrimidine. On standing, the selenium is reduced to a red precipitate of elemental selenium which can be dissolved in carbon disulfide. Finally, the selenium can be converted into its hexagonal structure by annealing at 205-207°C.


1964 ◽  
Vol 8 ◽  
pp. 456-461
Author(s):  
Donald Mitcham ◽  
Biagio Piccolo ◽  
Verne W. Tripp ◽  
Robert T. O’Connor

AbstractThe application of X-ray fluorescence to the qualitative and quantitative analysis of chemically modified cotton textile materials is described. The scope and flexibility of the technique have permitted the determination of more than 20 elements with, greatly reduced elapsed time compared with the corresponding spectroscopic or wet methods. Precautions to be observed in preparing standards are discussed. Results of the analysis of typical modifications and their significance in the development of cottons for specific uses are described.


1985 ◽  
Vol 29 ◽  
pp. 587-592
Author(s):  
K.K. Nielson ◽  
V.C. Rogers

Particle-size effects can cause significant errors in x-ray fluorescence (XRF) analysis of particulate materials. The effects are usually removed when samples are fused or dissolved to standardize the matrix for quantitative analysis. Recent improvements in numerical matrix corrections reduce the need to standardize the sample matrix via fusion or dissolution, particularly when the CEMAS method is used to estimate unmeasured light-element components of undefined materials for matrix calculations. A new method to correct for particle-size effects has therefore been examined to potentially avoid the need for destructive preparation of homogeneous samples.


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