Author(s):  
D. A. Carpenter ◽  
M. A. Taylor

The development of intense sources of x rays has led to renewed interest in the use of microbeams of x rays in x-ray fluorescence analysis. Sparks pointed out that the use of x rays as a probe offered the advantages of high sensitivity, low detection limits, low beam damage, and large penetration depths with minimal specimen preparation or perturbation. In addition, the option of air operation provided special advantages for examination of hydrated systems or for nondestructive microanalysis of large specimens.The disadvantages of synchrotron sources prompted the development of laboratory-based instrumentation with various schemes to maximize the beam flux while maintaining small point-to-point resolution. Nichols and Ryon developed a microprobe using a rotating anode source and a modified microdiffractometer. Cross and Wherry showed that by close-coupling the x-ray source, specimen, and detector, good intensities could be obtained for beam sizes between 30 and 100μm. More importantly, both groups combined specimen scanning with modern imaging techniques for rapid element mapping.


Author(s):  
D. A. Carpenter ◽  
Ning Gao ◽  
G. J. Havrilla

A monolithic, polycapillary, x-ray optic was adapted to a laboratory-based x-ray microprobe to evaluate the potential of the optic for x-ray micro fluorescence analysis. The polycapillary was capable of collecting x-rays over a 6 degree angle from a point source and focusing them to a spot approximately 40 µm diameter. The high intensities expected from this capillary should be useful for determining and mapping minor to trace elements in materials. Fig. 1 shows a sketch of the capillary with important dimensions.The microprobe had previously been used with straight and with tapered monocapillaries. Alignment of the monocapillaries with the focal spot was accomplished by electromagnetically scanning the focal spot over the beveled anode. With the polycapillary it was also necessary to manually adjust the distance between the focal spot and the polycapillary.The focal distance and focal spot diameter of the polycapillary were determined from a series of edge scans.


2020 ◽  
Vol 86 (10) ◽  
pp. 5-9
Author(s):  
D. G. Filatova ◽  
A. A. Arkhipenko ◽  
M. A. Statkus ◽  
V. V. Es’kina ◽  
V. B. Baranovskaya ◽  
...  

An approach to sorptive separation of Se (IV) from solutions on a novel S,N-containing sorbent with subsequent determination of the analyte in the sorbent phase by micro-x-ray fluorescence method is presented. The sorbent copolymethylenesulfide-N-alkyl-methylenamine (CMA) was synthesized using «snake in the cage» procedure and proven to be stable in acid solutions. Conditions for quantitative extraction of Se (IV) were determined: sorption in 5 M HCl or 0.05 M HNO3 solutions when heated to 60°C, phase contact time being 1 h. The residual selenium content in the solution was determined by inductively coupled plasma mass spectrometry (ICP-MS) using 82Se isotope. The absence of selenium losses is proved and the mechanism of sorption interaction under specified conditions is proposed. The method of micro-x-ray fluorescence analysis (micro-RFA) with mapping revealed a uniform distribution of selenium on the sorbent surface. The possibility of determining selenium in the sorbent phase by micro-RFA is shown. When comparing the obtained results with the results of calculations by the method of fundamental parameters, it is shown the necessity of using standard samples of sorbates to obtain correct results of RFA determination of selenium in the sorbent phase.


1983 ◽  
Vol 19 (2) ◽  
pp. 201-211 ◽  
Author(s):  
A. B. Cormie ◽  
D. E. Nelson

AbstractThe use of energy-dispersive X-ray fluorescence analysis (XES) for the routine identification of three tephras (Mazama, Bridge River, Mount St. Helens Yn) commonly found in archeological sites in British Columbia has been investigated. Researchers have often assumed that chemical analysis of bulk samples of glass separates would be hampered by contamination and weathering effects. Our results indicate that XES of bulk glass separates provides a very reliable method for rapidly identifying the three tephras in question, even with a very simple sample preparation. This should enable persons not skilled in geology or in tephrochronology to collect and to identify samples of these tephras. Finally, as a part of the study, similar measurements were made on the separated glass portions of these three tephras and of three others (Glacier Peak B and G, White River) from northwest North America. The results suggest that this method may provide tephrochronologists with a useful additional tool for studying tephras in other regions.


2020 ◽  
Author(s):  
E. V. Kochergina ◽  
A. O. Vagina ◽  
A. O. Taukin ◽  
A. V. Abramov ◽  
G. M. Bunkov ◽  
...  

2021 ◽  
Vol 13 (5) ◽  
Author(s):  
Viktória Mozgai ◽  
Bernadett Bajnóczi ◽  
Zoltán May ◽  
Zsolt Mráv

AbstractThis study details the non-destructive chemical analysis of composite silver objects (ewers, situlas, amphora and casket) from one of the most significant late Roman finds, the Seuso Treasure. The Seuso Treasure consists of fourteen large silver vessels that were made in the fourth–early fifth centuries AD and used for dining during festive banquets and for washing and beautification. The measurements were systematically performed along a pre-designed grid at several points using handheld X-ray fluorescence analysis. The results demonstrate that all the objects were made from high-quality silver (above 90 wt% Ag), with the exception of the base of the Geometric Ewer B. Copper was added intentionally to improve the mechanical properties of soft silver. The gold and lead content of the objects shows constant values (less than 1 wt% Au and Pb). The chemical composition as well as the Bi/Pb ratio suggests that the parts of the composite objects were manufactured from different silver ingots. The ewers were constructed in two ways: (i) the base and the body were made separately, or (ii) the ewer was raised from a single silver sheet. The composite objects were assembled using three methods: (i) mechanical attachment; (ii) low-temperature, lead-tin soft solders; or (iii) high-temperature, copper-silver hard solders. Additionally, two types of gilding were revealed by the XRF analysis, one with remnants of mercury, i.e. fire-gilding, and another type without remnants of mercury, presumably diffusion bonding.


Author(s):  
Claudia Zech ◽  
Marco Evertz ◽  
Markus Börner ◽  
Yves Kayser ◽  
Philipp Hönicke ◽  
...  

The manganese deposition of an aged anode has been investigated with K-edge and L-edge NEXAFS to determine the manganese species. In addition, the absolute amount of manganese could be revealed with reference-free X-ray fluorescence analysis.


Minerals ◽  
2019 ◽  
Vol 9 (9) ◽  
pp. 507 ◽  
Author(s):  
Maxim Rudmin ◽  
Elshan Abdullayev ◽  
Alexey Ruban ◽  
Ales Buyakov ◽  
Bulat Soktoev

We investigated the mechanochemical synthesis of complex slow release fertilizers (SRF) derived from glauconite. We studied the effectiveness of the mechanical intercalation of urea into glauconite using planetary and ring mills. The potassium-nitric complex SRFs were synthesized via a mechanochemical method mixing glauconite with urea in a 3:1 ratio. The obtained composites were analyzed using X-ray diffraction analysis, scanning electron microscopy, X-ray fluorescence analysis, and infrared spectroscopy. The results show that as duration of mechanochemical activation increases, the mineralogical, chemical, and structural characteristics of composites change. Essential modifications associated with a decrease in absorbed urea and the formation of microcrystallites were observed when the planetary milling time increased from 5 to 10 min and the ring milling from 15 to 30 min. Complete intercalation of urea into glauconite was achieved by 20 min grinding in a planetary mill or 60 min in a ring mill. Urea intercalation in glauconite occurs much faster when using a planetary mill compared to a ring mill.


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