Development and Comparison of Purgeable Mercury Values in SRR Samples Measured by SRNL and Eurofins FGS
- Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)
Savannah River Remediation (SRR) requested the development of mercury speciation 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 Frontier Global Sciences (FGS). This document reports on this method development work as well as the comparative analyses conducted between the two laboratories. Development, optimization, and validation were undertaken at SRNL to produce a method for the species-specific analysis of dissolved gaseous mercury (DGM) in samples from SRR. It was determined that DGM present in SRR samples represented a combination of various soluble and volatile mercury species- and is thus referred to in this document as purgeable mercury. A method has been developed and analytically validated for the analysis of purgeable mercury in caustic nuclear waste. Using multivariate optimization method, purge flow rate was determined to be highly correlated with increased response (p=0.023). Total recovery of spiked purgeable mercury from deionized water was 99.4 ±10.6% and 91.6 ±14.9% from spiked high-activity tank waste samples. Calibration, by external calibration and standard addition calibration, maintained a mean accuracy of 101 ±5% and 99.9 ±1.7%, respectively. This method represents a decrease in sample handling and processing over currently standard methods and represents a more amenable method for purgeable mercury analysis in liquid nuclear waste.1 An interlaboratory comparison was performed between SRNL and Eurofins FGS in the co-analysis of three quarterly Tank 50 samples. Two samples demonstrated no statistically significant difference (p=0.271, p=0.0811), with one sample biased 30% low to a statistically significant degree (p=0.0432). Large mean uncertainty was present in the results reported by both laboratories (±15% and 40% from SRNL and Eurofins), with no significant difference observed in uncertainty (p=0.934). Across all co-analyzed samples, no significantly difference was observed in precision (p=0.205) or reported values (p=0.352) between SRNL and Eurofins. These results indicate that SRNL-AD may provide data to the customer of statistically similar quality.
- Research Organization:
- Savannah River Site (SRS), Aiken, SC (United States)
- Sponsoring Organization:
- USDOE
- DOE Contract Number:
- AC09-08SR22470
- OSTI ID:
- 1495081
- Report Number(s):
- SRNL--L4100-2019-00004
- Country of Publication:
- United States
- Language:
- English
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