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Tag: X-ray spectroscopy
  • 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 plasma–optical 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%).
  • A Comparison of Handheld Field Chemical Sensors for Soil Characterization with a Focus on LIBS

    Abstract: Commercially available handheld chemical analyzers for forensic applications have been available for over a decade. Portable systems from multiple vendors can perform X-ray fluorescence (XRF) spectroscopy, Raman spectroscopy, Fourier transform infrared (FTIR) spectroscopy, and recently laser-induced breakdown spectroscopy (LIBS). Together, we have been exploring the development and potential applications of a multisensor system consisting of XRF, Raman, and LIBS for environmental characterization with a focus on soils from military ranges. Handheld sensors offer the potential to substantially increase sample throughput through the elimination of transport of samples back to the laboratory and labor-intensive sample preparation procedures. Further, these technologies have the capability for extremely rapid analysis, on the order of tens of seconds or less. We have compared and evaluated results from the analysis of several hundred soil samples using conventional laboratory bench top inductively coupled plasma atomic emission spectroscopy (ICP-AES) for metals evaluation and high-performance liquid chromatography (HPLC) and Raman spectroscopy for detection and characterization of energetic materials against handheld XRF, LIBS, and Raman analyzers. The soil samples contained antimony, copper, lead, tungsten, and zinc as well as energetic compounds such as 2,4,6-trinitrotoluene (TNT), hexahydro-1,3,5-triazine (RDX), nitroglycerine (NG), and dinitrotoluene isomers (DNT). Precision, accuracy, and sensitivity of the handheld field sensor technologies were compared against conventional laboratory instrumentation to determine their suitability for field characterization leading to decisional outcomes.
  • Fusion of Spectral Data from Multiple Handheld Analyzers (LIBS, XRF and Raman) for Chemical Analysis and Classification of Soil

     Abstract:  An 18-month multidisciplinary project was undertaken by JRPlumer & Associates, LLC and four subcontractors that had three technical objectives: (i) to upgrade current handheld technology for chemical analysis by X-ray fluorescence spectroscopy (XRFS), Raman spectroscopy (RS), and laser-induced breakdown spectroscopy (LIBS); (ii) to design a multisensor system based on these technologies for the rapid, in-situ chemical analysis of soils and other materials of military interest; and (iii) to investigate the classification/discrimination performance benefit that might be achieved through advanced signal pre-processing and data fusion with XRFS, RS, and LIBS analyses acquired for four suites of natural soils. Accomplishments of the program in the latter area are described in this report.