Comparison of the Quantitation of Heavy Metals in Soil Using Handheld LIBS, XRFS, and ICP-OES

Abstract

Handheld laser-induced breakdown spectroscopy (LIBS) is an emerging analytical technique that shows the potential to replace X-ray fluorescence spectroscopy (XRFS) in the field characterization of soils containing heavy metals. This study explored the accuracy and precision of handheld LIBS for analyzing soils containing copper and zinc to support LIBS as a re-placement for XRFS technology in situ. Success was defined by handheld LIBS results that could be replicated across field analyzers and verified by inductively coupled plasmaoptical emission spectrometry (ICP-OES). A total of 108 soil samples from eight military installations were pressed into 13 mm pellets and then analyzed by XRFS and LIBS. Handheld LIBS has a spot-size area 100-fold smaller than that of XRFS, and though it provided accurate measurements for NIST-certified reference materials, it was not able to measure unknown soils of varying soil texture with high particle size variability, regardless of sample size. Thus, soil sample particle size heterogeneity hindered the ability to provide accurate results and replicate quantitation results across LIBS and XRFS. Increasing the number of particles encountered by each shot through particle size reduction improved both field-analyzer correlation and the correlation between handheld LIBS and ICP-OES from weak (<15%) to strong (>80%).

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Document Details

Document Type
Technical Report
Publication Date
Jun 01, 2023
Accession Number
AD1203958

Entities

People

  • Jay Clausen
  • Megan I. Bishop
  • Patrick Sims
  • Samuel Beal

Organizations

  • Engineer Research and Development Center

Tags

Communities of Interest

  • Energy and Power Technologies
  • Weapons Technologies

DTIC Thesaurus Topics

  • Accuracy
  • Ball Mills
  • Chemical Analysis
  • Chemistry
  • Cold Regions
  • Detection
  • Detectors
  • Engineering
  • Engineers
  • Heavy Metals
  • Information Warfare
  • Instrumentation
  • Mass Spectrometry
  • Measurement
  • Particle Size
  • Particles
  • Spectra
  • Spectrometry
  • Spectroscopy
  • X Rays

Readers

  • Analytical Chemistry
  • Geotechnical Engineering.
  • Pulsed Power and Plasma Physics.

Technology Areas

  • Directed Energy