Censoring approach to the detection limits in X-ray fluorescence analysis

2004 ◽  
Vol 59 (10-11) ◽  
pp. 1739-1745 ◽  
Author(s):  
M. Pajek ◽  
A. Kubala-Kukuś
Author(s):  
K. Janssens ◽  
F. Adams ◽  
M.L. Rivers ◽  
K.W. Jones

Micro-SXRF (Synchrotron X-ray Fluorescence) or micro-SRIXE (Synchrotron Radiation Induced X-ray Emission) is a microanalytical technique which combines the sensitivity of more conventional microchemical methods such as Secondary Ion Microscopy (SIMS) and μ-PIXE (Proton Induced X-ray Emission) with the non-destructive and quantitative character of X-ray fluorescence analysis. The detection limits attainable at current SXRF-facilities are situated in the ppm (and in favourable cases the sub-ppm) range. The sensitivity of SRIXE can be used advantageously in individual particle analysis. This type of analysis is used, e.g., for studying sources of athmospheric pollution. Analysis of standard NIST micro-spheres at the NSLS-SRIXE facility yielded minimum detection limits in the 1 to 100 ppm range for particle sizes of around 10 to 30 μm.An interesting approach to individual particle characterisation is by means of electron microprobe analysis (EPMA). By using the backscattered electron signals, in an automated fashion, particles can be easily located on a filter substrate and their size and shape determined.


1995 ◽  
Vol 39 ◽  
pp. 755-766
Author(s):  
P. Wobrauschek ◽  
P. Kregsamer ◽  
W. Ladisich ◽  
R. Riede ◽  
Christina Streli ◽  
...  

Total reflection x-ray fluorescence analysis (TXRF) has reached a mature state but still improvements are possible in selecting the proper components for TXRF and optimizing them in the best suitable way. Two approaches are presented, the extension of the number of detectable elements after K-shell excitation and the improvement of the detection limits. The results show, that the elements from B to U can be detected by their characteristic K-lines and that detection limits for medium Z elements e.g. Ni in the fg range are achievable. Most of the best results have been measured using synchrotron radiation with spectral modifying devices like multilayer monochromators. Other x-ray sources like a windowless tube with exchangeable anodes of either material Al, Si or Mo were successfully tested for the efficient excitation of light elements.


2004 ◽  
Vol 33 (4) ◽  
pp. 306-311 ◽  
Author(s):  
M. Pajek ◽  
A. Kubala-Kukuś ◽  
D. Banaś ◽  
J. Braziewicz ◽  
U. Majewska

2004 ◽  
Vol 19 (1) ◽  
pp. 81-86 ◽  
Author(s):  
S. Török ◽  
J. Osán ◽  
B. Beckhoff ◽  
G. Ulm

Total reflection X-ray fluorescence analysis (TXRF) using monochromatized undulator radiation in the PTB radiometry laboratory at the synchrotron radiation facility BESSY II has been employed to investigate the chemical state of nitrogen compounds in aerosols. The aerosol samples of different size fractions were deposited on silicon wafer surfaces in a May impactor. Using a thin window Si(Li) detector, TXRF detection limits for nitrogen are in the upper fg and lower pg range. Taking advantage of the tunability of monochromatized undulator radiation, the near edge X-ray absorption fine structure (NEXAFS) could be combined with TXRF analysis, allowing for the speciation of the aerosols at the nitrogen K absorption edge. Such low detection limits enable an analysis of aerosol samples taken in 10 min with acceptable accuracy. Applicability of the technique to real aerosol samples has been used to compare nitrogen oxidation state in suburban and rural aerosols


1985 ◽  
Vol 29 ◽  
pp. 423-426 ◽  
Author(s):  
M. C. Nichols ◽  
R. W. Ryon

AbstractA prototype X-ray fluorescence system for chemical and phase microanalysis of materials has been developed and tested. Preliminary work with this system has indicated X-ray fluorescence detection limits on the order of 40 picograms for heavier elements such as gold when using a 100 micron collimator, 400 second counting time and a silver anode operating at 12 Kw. Phase identification by X- ray diffraction can be obtained from the same spot. A proposed design for an improved system providing greater elemental sensitivities and capable of semi-automated operation has been completed.


2020 ◽  
Vol 115 (2) ◽  
pp. 443-453
Author(s):  
Brian A. McNulty ◽  
Nathan Fox ◽  
J. Bruce Gemmell

Abstract Current portable X-ray fluorescence (pXRF) technology can rapidly and inexpensively yield concentrations of geologically significant elements, typically with instrument detection limits below several tens of parts per million. Based on conventional XRF whole-rock geochemical data, both the Ishikawa alteration index and the chlorite-carbonate-pyrite index increase with proximity to sulfide mineralization at Myra Falls. However, available pXRF technology is typically unable to detect all the elements required to calculate these alteration indices. As a result, there is a need to utilize the elements that are readily detectable using pXRF and apply these to hydrothermal alteration assessment. We propose that Rb/Sr ratios provide a robust proxy for the Ishikawa alteration index and demonstrate that conventional whole-rock XRF analytical results for Rb and Sr can be reproduced using pXRF analysis from drill core surfaces. At Myra Falls, the Rb/Sr ratios vary from <0.1 for least altered rocks, 0.1 to 0.5 for weakly altered rocks, 0.5 to 1.0 for moderately altered rocks, 1.0 to 2.0 for strongly altered rocks, and >2.0 for intensely altered rocks. Downhole profiles of alteration intensity generated from systematic pXRF analysis of drill core surfaces can be used to inform drilling and targeting decisions. The application of the Rb/Sr ratio as a proxy for alteration intensity extends beyond this case study and can be applied to other hydrothermal systems that produce phyllosilicate minerals as alteration products of feldspar.


2015 ◽  
Vol 30 (2) ◽  
pp. 93-98 ◽  
Author(s):  
J. Prost ◽  
P. Wobrauschek ◽  
C. Streli

The aim of this work was to compare different excitation modes for the analysis of light elements from carbon (Z = 6) upwards using a total reflection X-ray fluorescence analysis (TXRF) vacuum chamber which allows the attachment of different X-ray tubes and detectors. In the first set of experiments, two water-cooled high-power X-ray tubes with Cr (Z = 25) and Cu (Z = 29) anodes, respectively, were compared with an air-cooled low-power tube with Mo anode (Z = 42) and a thin Be window for the transmission of Mo-L lines. In the first two cases, monochromatic Kα radiation was used for excitation, while in the case of the Mo tube the multilayer acted as a cut-off reflector and part of the Mo bremsstrahlung continuum together with the Mo-L series were used for excitation. Multi-element standards containing elements ranging from Na (Z = 11) to Ti (Z = 22) were analyzed by a silicon drift detector (SDD) with a 300 nm ultrathin polymer window (UTW). Detection limits were calculated and compared for the three excitation modes. The second set of experiments was performed using an air-cooled low-power X-ray tube with Rh anode (Z = 45) in order to show that a conventional SDD with a 25 μm beryllium window can be used for the detection of elements from Na upwards. The use of compact air-cooled low-power X-ray tubes together with Peltier-cooled SDDs with UTW should lead to the development of highly sensitive tabletop vacuum TXRF spectrometers with a design optimized for the analysis of light elements. Detection limits as achieved by vacuum chambers using conventional water-cooled high-power tubes (e.g. Streli et al., 2004) are realistically achievable with the new approach.


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