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<div class="csl-entry">Hampel, S., Mähler, F., Iro, M., Ingerle, D., Streli, C., Fox, O. J. L., Sawhney, K., & Fittschen, U. E. A. (2023, April 12). <i>3D printed metal containing polymer layers as reference samples in micro XRF analysis</i> [Poster Presentation]. ANacon 2023, Wien, Austria. http://hdl.handle.net/20.500.12708/176781</div>
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dc.identifier.uri
http://hdl.handle.net/20.500.12708/176781
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dc.description.abstract
Introduction
Micro X-ray fluorescence analysis (microXRF) is a quasi-non-destructive method for studying the elemental composition spatially resolved. In laboratory set ups commonly polycapillaries are used, which yield focal spot sizes between 10 – 50 µm, depending on the energy. Volume based scanning of the sample is possible with a second polycapillary right in front of the detector. One challenge of the confocal setup is the absorption of X-ray fluorescence due to the scanning depth. Using fundamental parameters matrix effects can only be treated, if all geometrical and compositional parameters are known. Some of those can be derived from measurements of well-defined 3D printed metal containing references.
Methods
The preparation of the metal containing layer systems was done by 3d-printing of metal complex added acrylate based resin (ca. 0.05 w% metal – Cr, Co, Fe, Zn) using an Anycubic Photons S (Anycubic, Shenzhen, China). The homogeneity of the sample was proven with a lab-based microXRF (see [1]). Confocal measurements at the Diamond Light Source (B16 Test Beamline, 10 keV) with the setup from [2] were performed at an observed volume of ca. 20x27x20 µm (FWHM). Total reflection X ray fluorescence analysis (TXRF) of microwave-assisted digested specimen and elemental analysis (CHNS) were performed.
Results
The samples were found to have a homogeneous elemental distribution of the added metals with lab-based microXRF. Confocal measurements at the Diamond Light Source confirmed the depth resolved homogeneity for multilayer systems (up to three layers, ca. 50 µm each). Matrix-adapted TXRF and elemental analysis resulted in a composition of 59.37 ± 0.11 w% C, 7.04 ± 0.04 w% H, 2.61 ± 0.02 w% N, and between 294 ± 2 and 542 ± 5 µg·g-1 added metal.
Acknowledgment
We thankfully acknowledge the Diamond Light Source for the provision of experimental facilities and the financial support of Michael Iro, Dieter Ingerle and Christina Streli. We thank Karin Bode1 for the elemental analysis (CHNS).
Innovative aspects
• 3d printing of resin-based polymer with up to 542 ± 5 µg·g-1 metal added
• Conformation of homogeneity with confocal microXRF (synchrotron- and lab-based)
• Determination of composition important for Monte Carlo based simulation approach
References
[1] Fittschen, U. et al., A new micro X‐ray fluorescence spectrometer for in vivo elemental analysis in plants. X-Ray Spectrometry 2017, 46 (5), 374–381
[2] Ingerle, D. et al., A monochromatic confocal micro-x-ray fluorescence (μXRF) spectrometer for the lab. Review of Scientific Instruments 2020, 91 (12), 123107.
en
dc.language.iso
en
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dc.subject
XRF confocal
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dc.subject
micro XRF
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dc.title
3D printed metal containing polymer layers as reference samples in micro XRF analysis
