Limits of detection in XRF spectroscopy

Kadachi, Ahmed N.; Al-Eshaikh, Mohammad A.

doi:10.1002/xrs.2412

Cited by 61 publications

(34 citation statements)

References 11 publications

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“…Red coloured results are the results obtained in the measurement of nitrides, whereas results coloured in blue are the ones obtained in the measurement of nitrates, and the ones coloured in green are the ones obtained in the measurement of the synthetic standards (C1–C8), prepared from the mixtures of reference materials and chemical reagents. It can be noted that nitrates and nitrides show a good correlation when treated separately, which can denote the existence of a matrix effect, which increases the intensity of the element, because of the fluorescence effect, or decreases it if the signal is absorbed …”

Section: Resultsmentioning

confidence: 99%

Nitrogen determination by SEM‐EDS and elemental analysis

et al. 2013

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This paper describes a methodology for the analysis of nitrogen by scanning electron microscope with an energy dispersive X‐ray spectrometer (SEM‐EDS). The methodology was developed to have a rapid and accurate alternative method to the elemental analysis by combustion and thermoconductivity detection that does not imply the decomposition of the sample. Two methods by SEM‐EDS were established: a quantitative method trying to construct a calibration curve with reference materials and another using the standardless method provided with the instrument software, and the results were compared with those obtained by elemental analysis using two instruments that work at different temperature. An important matrix effect was found when trying to construct a calibration curve for SEM‐EDS for any kind of material, being corrected when using the standardless method because this method corrects the matrix effect. The quantification of nitrogen by SEM‐EDS is a good alternative to elemental analysis by combustion and thermoconductivity detection in those cases where the sample has a very high decomposition temperature. Copyright © 2013 John Wiley & Sons, Ltd.

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Section: Resultsmentioning

confidence: 99%

Nitrogen determination by SEM‐EDS and elemental analysis

et al. 2013

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“…• Detection limit: ≤0.01 at.%, but element specific 136,137 • Spot size: 100 μm to 1 mm, but can be reduced in μXRF 134 • Accurate quantification can be limited by self-absorption effects in films with high concentrations of the element analyzed 112 • Inaccurate quantification can occur if the sample is insufficiently thick to attenuate the primary X-ray beam or if the sample is not homogeneous 135 • Typically limited to heavier elements for standard Be detector windows: Z ≥ 11 (Na) 137 • Escape peaks can be generated 138 Energy dispersive X-ray spectroscopy (EDX or EDS)…”

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confidence: 99%

Perovskite-Inspired Photovoltaic Materials: Toward Best Practices in Materials Characterization and Calculations

et al. 2017

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ABSTRACT:Recently, there has been an explosive growth in research based on hybrid lead-halide perovskites for photovoltaics owing to rapid improvements in efficiency. The advent of these materials for solar applications has led to widespread interest in understanding the key enabling properties of these materials. This has resulted in renewed interest in related compounds and a search for materials that may replicate the defect-tolerant properties and long lifetimes of the hybrid lead-halide perovskites. Given the rapid pace of development of the field, the rises in efficiencies of these systems have outpaced the more basic understanding of these materials. Measuring or calculating the basic properties, such as crystal/electronic structure and composition, can be challenging because some of these materials have anisotropic structures, and/or are composed of both heavy metal cations and volatile, mobile, light elements. Some consequences are beam damage during characterization, composition change under vacuum, or compound effects, such as the alteration of the electronic structure through the influence of the substrate. These effects make it challenging to understand the basic properties integral to optoelectronic operation. Compounding these difficulties is the rapid pace with which the field progresses. This has created an ongoing need to continually evaluate best practices with respect to characterization and calculations, as well as to identify inconsistencies in reported values to determine if those inconsistencies are rooted in characterization methodology or materials synthesis. This article describes the difficulties in characterizing hybrid lead-halide perovskites and new materials, and how these challenges may be overcome. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 2 challenges discussed. The focus in this article is on crystallography, composition measurements, photoemission spectroscopy and calculations on perovskites and new, related absorbers. We suggest how some of the important artifacts could be avoided and how the reporting for each technique could be streamlined between groups to ensure reproducibility as the field progresses.

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“…The lower limit of detection (LLD) of an analytical method is the smallest amount of the analyte, which can be detected, corresponding to the minimum net signal, which exceeds the background signal with a certain level of confidence . It can be estimated on the basis of the statistical error σ B of the mean background signal

{\overset{true¯}{x}}_{B}

.…”

Section: Performance Of the Analytical Methodsmentioning

confidence: 99%

“…It can be estimated on the basis of the statistical error σ B of the mean background signal

{\overset{true¯}{x}}_{B}

. In the case of the LLD, commonly, a value of 3 ⋅ σ B is estimated for the minimum net signal corresponding to a confidence level of 0.05 for false background signal . So as to quantify the amount of the analyte, however, the limit of determination is estimated with 6 ⋅ σ B or, in the case that an acceptable experimental error should be achieved, the limit of quantification (LOQ) with 10 ⋅ σ B , respectively.…”

Section: Performance Of the Analytical Methodsmentioning

confidence: 99%

Development and calibration of a WDXRF routine applied to provenance studies on archaeological ceramics

et al. 2017

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Elemental analysis of ancient ceramics is primarily used in provenance research, where defined compositional groups are attributed to particular raw materials sources or production locations. Requirements in data quality and analytical performance are high, as is the need for clear and reproducible methodologies, and the availability of information on the above to ensure interlaboratory comparability and long-term data validity. This paper outlines the measurement parameters of a dedicated calibration set-up for the analysis of ancient ceramics using wavelength-dispersive X-ray fluorescence spectrometry (WDXRF). The specimens are prepared as concentrated glass beads, allowing the measurement of 26 elements from a single sample, thus minimising sample size requirements. Certified and non-commercial standards are used to evaluate the performance of the method in terms of detection limits, precision, repeatability, and accuracy. The materials used cover a range of compositions in line with the matrix variability encountered in archaeological ceramics. The data confirm the high standard of the method and highlight specific limitations. An initial assessment of comparability with other set-ups used in ceramic analyses, primarily Neutron Activation Analysis, is given through a discussion of performance on commonly analysed materials. The advantages of the proposed method include excellent analytical performance, analysis of a large suite of elements including all major, minor and a good range of traces, relatively small sample sizes, and preparation of samples that can be stored and re-analysed.

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Limits of detection in XRF spectroscopy

Cited by 61 publications

References 11 publications

Nitrogen determination by SEM‐EDS and elemental analysis

Nitrogen determination by SEM‐EDS and elemental analysis

Perovskite-Inspired Photovoltaic Materials: Toward Best Practices in Materials Characterization and Calculations

Development and calibration of a WDXRF routine applied to provenance studies on archaeological ceramics

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