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Related Concept Videos

Atomic Absorption Spectroscopy: Interference01:25

Atomic Absorption Spectroscopy: Interference

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Interference leads to systematic error in atomic absorption (AA) measurements by enhancing or diminishing the analytical signal or the background. These interferences can be grouped into three main categories: spectral interference, chemical interference, and physical interference.
Spectral interference occurs when signals from other elements or molecules overlap with the analyte signal, falsely elevating or masking the analyte's absorbance. This interference can be corrected using Zeeman,...
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Atomic Absorption Spectroscopy: Lab01:21

Atomic Absorption Spectroscopy: Lab

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For AAS measurements, samples must be introduced as clear solutions, often requiring extensive preliminary treatment to dissolve materials like soils, animal tissues, and minerals. Common methods for sample preparation include treatment with hot mineral acids, wet ashing, combustion in closed containers, high-temperature ashing, or fusion with reagents.
 Solutions containing organic solvents, such as low-molecular-mass alcohols, esters, or ketones, enhance absorbances by increasing...
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NMR Spectrometers: Resolution and Error Correction01:14

NMR Spectrometers: Resolution and Error Correction

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When magnetic nuclei in a sample achieve resonance and undergo relaxation, the signal detected in NMR is an approximately exponential free induction decay. Fourier transform of an exponential decay yields a Lorentzian peak in the frequency domain. Lorentzian peaks in an NMR spectrum are defined by their amplitude, full width at half maximum, and position, where the peak width is governed by the spin-spin relaxation time alone. In real experiments, however, the applied magnetic field is rendered...
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X-ray Crystallography02:18

X-ray Crystallography

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The size of the unit cell and the arrangement of atoms in a crystal may be determined from measurements of the diffraction of X-rays by the crystal, termed X-ray crystallography.
Diffraction
Diffraction is the change in the direction of travel experienced by an electromagnetic wave when it encounters a physical barrier whose dimensions are comparable to those of the wavelength of the light. X-rays are electromagnetic radiation with wavelengths about as long as the distance between neighboring...
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Atomic Spectroscopy: Absorption, Emission, and Fluorescence01:23

Atomic Spectroscopy: Absorption, Emission, and Fluorescence

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Atomic spectroscopy is a vital tool in elemental analysis, both qualitatively and quantitatively. It can be broadly divided into optical spectroscopy, mass spectroscopy, and X-ray spectroscopy methods. The optical spectroscopic methods are atomic absorption spectroscopy (AAS), atomic emission spectroscopy (AES), and atomic fluorescence spectroscopy (AFS). The first step in all three methods is atomization, where the solid, liquid, or solution-phase samples are converted into gas-phase atoms and...
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Atomic Absorption Spectroscopy: Overview01:27

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Atomic absorption spectroscopy (AAS) is a technique used to analyze elements by measuring electromagnetic radiation (EMR) absorbed by atoms, which causes them to transition to a higher-energy orbit. The most crucial step in AAS is atomization, where the analyte is converted into gas-phase atoms, typically through a flame or furnace. Some of these atoms become thermally excited in the flame, while most remain in the ground state.
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Quantifying X-Ray Fluorescence Data Using MAPS
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Quantifying X-Ray Fluorescence Data Using MAPS

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Self-absorption correction on 2D X-ray fluorescence maps.

Mingyuan Ge1, Hanfei Yan1, Xiaojing Huang1

  • 1National Synchrotron Light Source II, Brookhaven National Laboratory, Upton, NY, USA.

Scientific Reports
|May 4, 2023
PubMed
Summary
This summary is machine-generated.

This study introduces a new semi-empirical method to correct self-absorption in 2D X-ray fluorescence mapping (XRF). The technique accurately quantifies material composition, revealing previously hidden details like chromium enrichment in corroded stainless steel.

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Area of Science:

  • Materials Science
  • Analytical Chemistry
  • Physics

Background:

  • X-ray fluorescence mapping (XRF) is a powerful, non-invasive technique for elemental analysis at micro/nanoscale.
  • Quantitative XRF analysis is hindered by self-absorption, a persistent challenge, especially in 2D mapping.
  • Correcting 2D XRF data is complex due to its nature as an ill-posed inverse problem.

Purpose of the Study:

  • To develop and validate a semi-empirical method for accurate correction of 2D XRF mapping data.
  • To address the long-standing self-absorption problem in quantitative XRF analysis.
  • To improve the accuracy of elemental composition quantification in complex samples.

Main Methods:

  • Development of a novel semi-empirical correction method for 2D XRF datasets.
  • Comprehensive evaluation of the method's accuracy across various experimental configurations.
  • Application of the corrected XRF data to analyze material composition in corroded stainless steel.

Main Results:

  • The proposed method effectively corrects 2D XRF mapping data with generally less than 10% error.
  • Accurate quantification of elemental distribution around grain boundaries in stainless steel.
  • Discovery of highly localized chromium enrichment near crack sites, previously undetectable.

Conclusions:

  • The semi-empirical method provides a significant advancement for accurate quantitative 2D XRF analysis.
  • The technique overcomes limitations imposed by self-absorption, enhancing material characterization.
  • Reveals critical microstructural compositional details, essential for understanding material degradation and performance.