21 Jun 2023

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%).

1 Jul 2020

PUBLICATION NOTICE: Laboratory spiking process of soil with various uranium and other heavy metals

Abstract: Laboratory studies using metal spiked soils are challenging due to soil heterogeneity. This work provides an easy, quick, precise, and accurate technique for the preparation of spiked soils for laboratory research. The process described spiking soil with various uranium species and other heavy metals for laboratory scale pilot experiments under various biogeochemical conditions. The procedure involves grinding both dry soil and metal chemicals into the fine powder. The spiked soil mixture was further homogenized through a modified splitting and combining of the sample by diagonal flipping using plastic sheeting. Comparison of measured concentrations with theoretical values were obtained with <20% precision and accuracy. However, tradition spiking method with metal solution of-ten yielded high heterogeneous spiked soils due to strong metal adsorption in soils. Re-drying and re-grinding of soils were required following the spiking in order to homogenize treated soils, generating inhalable particulates. Thus appropriate personal protective equipment and practices are required for the safety concern. The present method with metal salt powder proved a safe, useful, quick, accurate and precise, and homogenized soil spiking method.