Determination of bromine in selected polymer materials by a wavelength-dispersive X-ray fluorescence spectrometric method — Critical thickness problem and solutions

Gorewoda, Tadeusz; Mzyk, Zofia; Anyszkiewicz, Jacek; Charasińska, Jadwiga

doi:10.1016/j.sab.2015.01.007

Cited by 10 publications

(7 citation statements)

References 9 publications

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“…The impurities present at low concentrations have a negligible impact on the d I values of the alloying elements. The elemental information depth values were estimated using the method described in our previous paper using the relation:

d_{I} = \log_{e} ((), 0.001) \frac{1}{- ({}, {(\frac{μ}{ρ})}_{λ italicprim} italiccscφ + {(\frac{μ}{ρ})}_{λ italicline} italiccscψ) ρ}

…”

Section: Methodsmentioning

confidence: 99%

Novel sample treatment procedures for the determination of phosphorus in Cu‐based alloys using X‐ray fluorescence spectrometry to solve the microstructural effect issue

et al. 2017

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The accurate analysis of hard CuP and CuPAg‐type solders using X‐ray fluorescence spectrometry is a difficult task. Surface milling, the most common sample preparation method for calibration materials, results in poor accuracy for the phosphorus analysis, as evidenced by the unacceptable values of the root mean square error. Meanwhile, the analysis of real samples provides incorrect results, and microstructural effects are the main source of error. Thus, this effect was negated by considering the information depth of the phosphorus Kα line and the microstructure size of the alloys. Phosphorus was measured using a thin layer of the sample (a thickness of several micrometers). As a result, the analyzed layer was a poor representative of the sample. Two different approaches for solving the microstructural effect issue were proposed. In the first method, the alloy was remelted under controlled conditions to obtain fine‐grain samples, which successfully limited the microstructural effects. The second solution used specially prepared thin layer samples, and the sample dissolution eliminated the microstructural effect. Using the developed sample treatment methods resulted in an improvement in the accuracy of the phosphorus calibration curves. This allowed for the correct determination of phosphorus and other alloying elements in the Cu‐based alloys with low uncertainties.

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d_{I} = \log_{e} ((), 0.001) \frac{1}{- ({}, {(\frac{μ}{ρ})}_{λ italicprim} italiccscφ + {(\frac{μ}{ρ})}_{λ italicline} italiccscψ) ρ}

…”

Section: Methodsmentioning

confidence: 99%

Novel sample treatment procedures for the determination of phosphorus in Cu‐based alloys using X‐ray fluorescence spectrometry to solve the microstructural effect issue

et al. 2017

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“…Low concentrations of impurities result in a negligible impact on t c values for alloying elements. The t c values were estimated as described in our previous papers [10,11] using the following equation:…”

Section: Critical Thickness Calculationmentioning

confidence: 99%

“…The critical thickness is the limit of the thickness of the sample above which all of the produced fluorescent radiation does not emerge. The volume of a sample analyzed by XRF spectrometry depends on the t c value [11], so it is an important characteristic for the selected element line and sample composition. With regard to the critical thickness which is on the order of several dozens to two hundred μm for analyzed solders, it is assumed that the volume needs to be disk-shaped with a diameter equal to the mask diameter and thickness as large as the t c value.…”

mentioning

confidence: 99%

Microstructural Effect Limitations in the Analysis of SnAg, SnBi and SnIn Lead-free Solders by Wavelength Dispersion X-Ray Spectrometry

et al. 2020

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This article describes the effects of microstructures in an analysis of lead-free solders, namely SnAg, SnBi and SnIn, using X-ray fluorescence spectrometry (XRF). The size of the microstructures in the samples and calibration materials has a strong impact on the calibration accuracy and results. A comparison of the microstructure size and critical thickness values demonstrated the importance of the former parameter in terms of the analyzed volume of the specimen. The re-melting and casting in an induction furnace at developed conditions were determined to be a way to obtain samples with fine-grained microstructures. Calibration with re-melted reference materials yielded more accurate calibration curves than calibration using the materials in their original state. Re-melting of the samples resulted in improvements in the XRF results in comparison to the reference values. This improvement is especially important in case of alloying elements with concentrations that determine the recognition of a specific solder grade.

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“…The pellets were analysed using LA-ICP-MS to determine the Br homogeneity. The other paper to determine Br in polymers was reported by Gorewoda et al, 272 who used WDXRF for the determination, even though the polymer samples were thinner than the critical thickness required for Br. This was especially true for cellulose and polyethylene samples that have a high Br critical thickness and yet come as thin sheets.…”

Section: Polymers and Compositesmentioning

confidence: 99%

Atomic spectrometry update. Review of advances in the analysis of metals, chemicals and functional materials

Carter

Fisher

García³

et al. 2015

J. Anal. At. Spectrom.

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Determination of bromine in selected polymer materials by a wavelength-dispersive X-ray fluorescence spectrometric method — Critical thickness problem and solutions

Cited by 10 publications

References 9 publications

Novel sample treatment procedures for the determination of phosphorus in Cu‐based alloys using X‐ray fluorescence spectrometry to solve the microstructural effect issue

Novel sample treatment procedures for the determination of phosphorus in Cu‐based alloys using X‐ray fluorescence spectrometry to solve the microstructural effect issue

Microstructural Effect Limitations in the Analysis of SnAg, SnBi and SnIn Lead-free Solders by Wavelength Dispersion X-Ray Spectrometry

Atomic spectrometry update. Review of advances in the analysis of metals, chemicals and functional materials

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