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Title: Sulfur Limits of Detection and Spectral Interference Corrections for DWPF Sludge Matrices by Inductively Coupled Plasma Emission Spectrometry

Abstract

The Savannah River Technology Center (SRTC) has been requested to perform sulfur (S) analysis on digested radioactive sludge and supernatant samples by Inductively Coupled Plasma Emission Spectrometry (ICP-ES). The amount of sulfur is a concern because there are sulfur limits for the incoming feed, due to glass melter, process vessel, and off-gas line corrosion concerns and limited sulfur solubility in the glass wasteform. Recent changes in the washing strategy and stream additions change the amount of sulfur in the sludge. Increasing the sulfur concentration in the sludge challenges the current limits, so accurately determining the amount of sulfur present in a sludge batch is paramount. There are two important figures of merit that need to be evaluated for this analysis. The first is the detection limit (LOD), the smallest concentration of an element that can be detected with a defined certainty. This issue is important since the sulfur concentration in these process streams is l ow. Another critical analytical parameter is the effect on the S quantitation from potential spectral interferences. Spectral interferences are caused by background emission from plasma recombination events, scattered and stray light from the line emission of high concentration elements, or molecular band emission and frommore » direct or tailing spectral line overlap from a matrix element. Any existing spectral overlaps could give false positives or increase the measured S concentrations in these matrices.« less

Authors:
Publication Date:
Research Org.:
Savannah River Site (US)
Sponsoring Org.:
US Department of Energy (US)
OSTI Identifier:
823120
Report Number(s):
WSRC-TR-2004-00090
TRN: US0401512
DOE Contract Number:  
AC09-96SR18500
Resource Type:
Technical Report
Resource Relation:
Other Information: PBD: 20 Apr 2004
Country of Publication:
United States
Language:
English
Subject:
12 MANAGEMENT OF RADIOACTIVE WASTES, AND NON-RADIOACTIVE WASTES FROM NUCLEAR FACILITIES; 37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; CERAMIC MELTERS; CORROSION; DETECTION; GLASS; SENSITIVITY; SLUDGES; SOLUBILITY; EMISSION SPECTROSCOPY; SULFUR; WASTE FORMS; RADIOACTIVE WASTE PROCESSING

Citation Formats

JURGENSEN, AR. Sulfur Limits of Detection and Spectral Interference Corrections for DWPF Sludge Matrices by Inductively Coupled Plasma Emission Spectrometry. United States: N. p., 2004. Web. doi:10.2172/823120.
JURGENSEN, AR. Sulfur Limits of Detection and Spectral Interference Corrections for DWPF Sludge Matrices by Inductively Coupled Plasma Emission Spectrometry. United States. https://doi.org/10.2172/823120
JURGENSEN, AR. Tue . "Sulfur Limits of Detection and Spectral Interference Corrections for DWPF Sludge Matrices by Inductively Coupled Plasma Emission Spectrometry". United States. https://doi.org/10.2172/823120. https://www.osti.gov/servlets/purl/823120.
@article{osti_823120,
title = {Sulfur Limits of Detection and Spectral Interference Corrections for DWPF Sludge Matrices by Inductively Coupled Plasma Emission Spectrometry},
author = {JURGENSEN, AR},
abstractNote = {The Savannah River Technology Center (SRTC) has been requested to perform sulfur (S) analysis on digested radioactive sludge and supernatant samples by Inductively Coupled Plasma Emission Spectrometry (ICP-ES). The amount of sulfur is a concern because there are sulfur limits for the incoming feed, due to glass melter, process vessel, and off-gas line corrosion concerns and limited sulfur solubility in the glass wasteform. Recent changes in the washing strategy and stream additions change the amount of sulfur in the sludge. Increasing the sulfur concentration in the sludge challenges the current limits, so accurately determining the amount of sulfur present in a sludge batch is paramount. There are two important figures of merit that need to be evaluated for this analysis. The first is the detection limit (LOD), the smallest concentration of an element that can be detected with a defined certainty. This issue is important since the sulfur concentration in these process streams is l ow. Another critical analytical parameter is the effect on the S quantitation from potential spectral interferences. Spectral interferences are caused by background emission from plasma recombination events, scattered and stray light from the line emission of high concentration elements, or molecular band emission and from direct or tailing spectral line overlap from a matrix element. Any existing spectral overlaps could give false positives or increase the measured S concentrations in these matrices.},
doi = {10.2172/823120},
url = {https://www.osti.gov/biblio/823120}, journal = {},
number = ,
volume = ,
place = {United States},
year = {2004},
month = {4}
}