X-RAY FLUORESCENCE ANALYSIS OF HANFORD LOW ACTIVITY WASTE SIMULANTS

Jurgensen, A ; David Missimer, D ; Ronny Rutherford, R

Savannah River Site (S.C.)

关键词: Waste Processing;    Sodium;    Fluorescence;    Compliance;    Glass;   

DOI  :  10.2172/891691
RP-ID  :  WSRC-TR-2006-00137
RP-ID  :  DE-AC09-96SR18500
RP-ID  :  891691

美国|英语

来源: UNT Digital Library

【 摘 要 】

Savannah River National Laboratory (SRNL) was requested to develop an x-ray fluorescence (XRF) spectrometry method for elemental characterization of the Hanford Tank Waste Treatment and Immobilization Plant (WTP) pretreated low activity waste (LAW) stream to the LAW Vitrification Plant. The WTP is evaluating the potential for using XRF as a rapid turnaround technique to support LAW product compliance and glass former batching. The overall objective of this task was to develop XRF analytical methods that provide the rapid turnaround time (<8 hours) requested by the WTP, while providing sufficient accuracy and precision to determine waste composition variations. For Phase 1a, SRNL (1) evaluated, selected, and procured an XRF instrument for WTP installation, (2) investigated three XRF sample methods for preparing the LAW sub-sample for XRF analysis, and (3) initiated scoping studies on AN-105 (Envelope A) simulant to determine the instrument's capability, limitations, and optimum operating parameters. After preliminary method development on simulants and the completion of Phase 1a activities, SRNL received approval from WTP to begin Phase 1b activities with the objective of optimizing the XRF methodology. Three XRF sample methods used for preparing the LAW sub-sample for XRF analysis were studied: direct liquid analysis, dried spot, and fused glass. The direct liquid method was selected because its major advantage is that the LAW can be analyzed directly without any sample alteration that could bias the method accuracy. It also is the fastest preparation technique--a typical XRF measurement could be completed in < 1hr after sample delivery. Except for sodium, the method detection limits (MDLs) for the most important analytes in solution, the hold point elements, were achieved by this method. The XRF detection limits are generally adequate for glass former batching and product composition reporting, but may be inadequate for some species (Hg, Cd, and Ba) important to land disposal restrictions. The long term precision (24-hr) also was good with percent relative standard deviations (%RSDs) < 10 % for most elements in filtered solution. There were some issues with a few elements precipitating out of solution over time affecting the long term precision of the method. Additional research will need to be performed to resolve this sample stability problem. Activities related to methodology optimization in the Phase 1b portion of the study were eliminated as a result of WTP request to discontinue remaining activities due to funding reduction. These preliminary studies demonstrate that developing an XRF method to support the LAW vitrification plant is feasible. When funding is restored for the WTP, it is recommended that optimization of this technology should be pursued.