Methylmercury and Ethylmercury Analytical Performance in SRR Samples Measured by SRNL and Eurofins Frontier Global Sciences
- Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)
Existing models and simulants of tank disposition media at the Savannah River Site (SRS) have presumed the presence of high concentrations of inorganic mercury. However, quarterly Tank 50 analyses have shown that mercury is present as organomercurial species at concentrations that may present challenges to its remediation and disposition and may challenge the Waste Acceptance Criteria (WAC) for Saltstone. Todate, methylmercury analyses for Savannah River Remediation (SRR) have been performed at an off-site laboratory by Eurofins Frontier Global Sciences (FGS) in Bothell, WA. Savannah River Remediation requested the development of methylmercury and ethylmercury determination capabilities at the Savannah River National Laboratory (SRNL) to support the Liquid Waste Operations at SRS. As part of that method development, SRR requested that SRNL Analytical Development (AD) compare their results with those obtained from their outside contract laboratory, Eurofins FGS. This document reports on this method development work as well as the comparative analyses conducted between the two laboratories. A series of optimization and validation experiments has been performed at SRNL, which has resulted in the development of on-site methylmercury and ethylmercury speciation capabilities using purge and trap (P&T) gas chromatography (GC) coupled with thermal desorption (TD) cold vapor – atomic fluorescence spectroscopy (CVAFS). Speciation has been achieved for both species, with a methylmercury method reporting limit (MRL) value of 1.13 pg and an overall uncertainty (1σ) of 5.1%. An ethylmercury MRL of 11.5 pg and an overall uncertainty (1σ) of 4.8% were obtained. These analytical parameters compare favorably with Eurofins FGS, which demonstrates uncertainties (1σ) for methylmercury and ethylmercury of 13% and 9.1%, respectively. Results obtained by SRNL from the routine analysis of Tanks 21, 40, 50, and 51 samples have provided statistically indistinguishable results compared with Eurofins FGS. Based upon the work performed by SRNL-AD and the data currently available, the following recommendations can be made: Further work should be performed to determine a “best practices” for sample holding time prior to analysis (both preserved and non-preserved samples), as well as any detrimental effects sample age may have on data quality. Analysis of ethylmercury is only recommended for tank samples that are reasonably expected to have significant quantities of ethylmercury, such as from the DWPF SMECT. Trace levels of ethylmercury in the presence of large quantities of methylmercury can be difficult or impossible to quantify. SRNL-AD development of methods for total mercury, purgeable mercury (which includes Hg(0) and dimethylmercury), inorganic mercury (Hg(I) and Hg(II)), dissolved mercury, and particulate mercury are underway and will be reported upon separately.
- Research Organization:
- Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)
- Sponsoring Organization:
- USDOE Office of Environmental Management (EM)
- DOE Contract Number:
- AC09-08SR22470
- OSTI ID:
- 1557972
- Report Number(s):
- SRNL-STI-2018-00250; TRN: US2100451
- Country of Publication:
- United States
- Language:
- English
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