Total Mercury Analysis Comparison: Deployment of Analytical Method for the Savannah River Site Liquid Waste System

A direct mercury analyzer (DMA; EPA 7473) and Cold Vapor Atomic Absorption Spectroscopy (CVAAS; EPA 245.2) have been used to analyze samples high in methylmercury and other forms of mercury with oxidation states of Hg^o (elemental), Hg¹⁺ (mercurous), and/or Hg²⁺ (mercuric) to determine analytical data equivalency for total mercury. The DMA instrument has been determined to be the preferred method based on both simulated and radioactive sample testing due to analytical results and ease of use in a radiological hood. SRNL made a number of modifications to the DMA instrument and analysis method to limit the amount of time personnel are required to work in a radiological environment. Equivalency is based on comparative statistical evaluation of the results from: spike solutions/simulants, Tank 50 samples, Mixed Analyte Performance Evaluation Program (MAPEP) samples, and Modular Caustic-Side Solvent Extraction Unit (MCU) solvent samples. SRNL performed a cross-comparison of results using CVAAS, DMA, and Inductively Coupled Plasma Mass Spectrometer (ICP-MS), as well as independent analysis from an offsite laboratory (using cold vapor sample processing with atomic fluorescence detection, EPA 1631). All data were within the combined uncertainty (2σ ± 20%) of the CVAAS and DMA methods