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Atomic Absorption Spectroscopy: Lab01:21

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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.
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Atomic fluorescence spectroscopy (AFS) is an analytical technique that involves the electronic transitions of atoms in a flame, furnace, or plasma being excited by electromagnetic (EM) radiation. When these atoms absorb energy, they become excited and subsequently release energy as they return to their original state. This emitted light, or "fluorescence," is observed at a right angle to the incident beam. Both absorption and emission processes transpire at distinct wavelengths, which...
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Atomic Absorption Spectroscopy: Atomization Methods01:25

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Atomic Absorption Spectroscopy (AAS) atomizes samples through flame atomization or electrothermal atomization. Flame atomization typically involves a nebulizer and spray chamber assembly to combine the sample with a fuel–oxidant mixture, creating a fine aerosol mist that enters a burner. Typically, the fuel and oxidant are combined in an approximately stoichiometric ratio. However, for atoms that are easily oxidized, a fuel-rich mixture may be more advantageous. Only about 5% of the...
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High-accuracy total reflection X-ray fluorescence analysis for determining trace elements using substrate cleaned by

Tsugufumi Matsuyama1, Yudai Tanaka1, Yoshihiro Mori2

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Researchers improved trace element analysis using total reflection X-ray fluorescence (TXRF) by creating superhydrophilic substrates. This method enhances sensitivity and accuracy for low-Z elements, overcoming matrix absorption issues in dried residues.

Keywords:
Ammonia-hydrogen peroxide mixtureDried residueSubstrate cleaning/ hydrophilizationTotal reflection X-ray fluorescence analysis

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Area of Science:

  • Analytical Chemistry
  • Materials Science
  • Spectroscopy

Background:

  • Total reflection X-ray fluorescence (TXRF) is valuable for trace element determination.
  • Hydrophobic substrates are typically used, forming dot-type residues.
  • Challenges exist in measuring low-Z elements due to matrix absorption in thicker residues.

Purpose of the Study:

  • To develop a thin film-type residue method to mitigate matrix absorption effects in TXRF.
  • To enhance analytical sensitivity and accuracy for low-Z elements.
  • To investigate the use of superhydrophilic substrates for TXRF sample preparation.

Main Methods:

  • Glass substrates were treated with an ammonia-hydrogen peroxide mixture (APM) to create superhydrophilic surfaces (contact angle ~5°).
  • A polytetrafluoroethylene mask defined the APM-treated region to a 6 mm diameter.
  • Dried residues were prepared on both APM-treated (superhydrophilic) and untreated (hydrophobic) substrates for comparison.

Main Results:

  • APM-treated superhydrophilic substrates significantly improved net intensities for low-Z elements.
  • The ratio of Al Kα intensity (net) on APM-treated vs. hydrophobic substrates was 2.29.
  • Elemental recovery was near 100% on APM-treated substrates, while hydrophobic substrates showed significant deviations (e.g., ~32% for Al).

Conclusions:

  • Using APM-treated superhydrophilic substrates successfully enhances analytical sensitivity in TXRF.
  • The proposed method improves the accuracy of trace element quantification, particularly for low-Z elements.
  • This approach effectively overcomes the limitations of matrix absorption in TXRF analysis.