4Dw was measured under conditions in which the analyte is strongly retained by the resin and weakly retained by the resin.What do these types of measurements tell you?Did you use the correct extractant?Did you use the correct quantity of extractant?
5What Dw does not tell you. How completely will an analyte be retained by the column? In other words, how much breakthrough will occur?When exactly will an analyte elute from the column?How efficiently will an analyte elute from the column? (% recovery)How much cross contamination will occur between two or more analytes?
6New QC ProtocolsExtractants (Solvent extraction test)-helps to determine purity of extractant2) Every batch of resin (Dw Test)-ensures correct extractant used3) Resin with new lot of at least one starting material (New column QC)a) 1 chromatogramb) 4 vacuum box tests-ensures good performance of resin in most commonly used application
7Chromatogram Simplified version of common Eichrom method performed Aliquots taken for gamma, LSC or ICP-AES analysiscpm or ppm plotted vs Bed Volumes
8Chromatogram Important Parameters Recovery of analytes (>95%) Cross-contamination (<1-3%)Reproducibility (4-5 replicates)
9Vacuum Box TestEssentially the same as the chromatogram test, however, fewer fractions are collectedProvides reproducibility data
10General Time Line1) Determine separation schemes to test each Eichrom resin.2) Perform liquid-liquid extraction (extractants) and chromatogram and vacuum box tests on quality control retains (10-12 resin lots) to determine reasonable recovery/separation metrics for future lots.3) Implement new QC procedure and provide improved certificates of analysis for each lot of Eichrom resin.TRUTEVAUTEVASr ResinDGA, nDGA, brBerylliumPb ResinLn (a+s)TritiumNickleMnO2AnionCation1)2)3)Progress as ofGoal: Complete 4 main resins by summer 2005
11Proposed QC Protocols TRU: Load: Am and Pu from 3 M HNO3 Rinse: 3 M HNO M NaNO2Strip Am with 4 M HClStrip Pu with 0.03 M ammonium oxalateTEVA: Load: Th and Pu from 3 M HNO M NaNO2Rinse: 3 M HNO M NaNO2Strip Th with 6 M HClStrip Pu with 0.02 M HCl M HF
12Proposed QC Protocols UTEVA: Load: Th and U from 4 M HNO3 Rinse: 4 M HNO3Strip Th with 6 M HClStrip U with 0.1 HClSr: Load: Sr and Ba from 8 M HNO3Rinse: 8 M HNO3Strip Sr with 0.05 M HNO3
14Results (TRU) >95% yields for Pu and Am Good separation of Pu and Am<1% Pu in Am<1.5% Am in PuVery reproducibledifferent lotssame lotOnly significant variability observed was the amount of Pu remaining on column
16Results (TEVA) >95% yields for Pu and Th Good separation of Pu and Th<1% Pu in Th<2% Th in PuVery reproducibledifferent lotssame lotOnly significant variability observed was the amount of Pu remaining on column
18ConclusionsEichrom is implementing a new QC program.The new QC program will include liquid-liquid extraction tests (extractants), Dw tests (every resin lot) and column elution tests (resin lots with new raw materials).So far, TRU and TEVA from 2004 have been tested to generate data from which metrics to evaluate new resin lots will be determined.UTEVA and Sr Resin tests are next, followed by DGA and the remaining Eichrom products.