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Title: Solvent hold tank sample results for MCU-16-1488-1493 (December 2016), MCU-17-86-88 (January 2017), and MCU-17-119-121 (February 2017): Quarterly Report

Abstract

A trend summary of three Solvent Hold Tank (SHT) monthly samples; MCU-16-1488-1493 (December 2016), MCU-17-86-88 (January 2017), and MCU-17-119-121 (February 2017) are reported. Analyses indicate that the modifier (CS-7SB) and the extractant (MaxCalix) concentrations are at their nominal recommended levels (169,000 mg/L and 46,300 mg/L respectively). The suppressor (TiDG) level has decreased to a steady state level of 673 mg/L well above the minimum recommended level (479 mg/L). This analysis confirms the Isopar™ addition to the solvent in January 18, 2017. This analysis also indicates the solvent did not require further additions. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended. No impurities above the 1000 ppm level were found in this solvent by the Semi-Volatile Organic Analysis (SVOA). No impurities were observed in the Hydrogen Nuclear Magnetic Resonance (HNMR). Another impurity observed in the samples was mercury. Up to 38 ± 8 micrograms of mercury per mL of solvent was detected in these samples (the average of the CV-AA and XRF methods). The higher mercury concentration in the solvent (as determined inmore » the last three monthly samples) is possibly due to the higher mercury concentration in Salt Batches 8 and 9 (Tank 49H) or mixing of previously undisturbed areas of high mercury concentration in Tank 49H. The gamma level (0.21E5 dpm/mL) measured in the February SHT sample was one order of magnitude lower than the gamma levels observed in the December and January SHT samples. The February gamma level is consistent with the solvent being idle (since January 10, 2017). The gamma levels observed in the December and January SHT samples were consistent with previous monthly measurements where the process operated normally. The laboratory will continue to monitor the quality of the solvent in particular for any new impurities or degradation of the solvent components.« less

Authors:
 [1];  [1]
  1. Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)
Publication Date:
Research Org.:
Savannah River Site (SRS), Aiken, SC (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1371695
Report Number(s):
SRNL-STI-2017-00367
DOE Contract Number:
AC09-08SR22470
Resource Type:
Technical Report
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats

Fondeur, F. F., and Jones, D. H.. Solvent hold tank sample results for MCU-16-1488-1493 (December 2016), MCU-17-86-88 (January 2017), and MCU-17-119-121 (February 2017): Quarterly Report. United States: N. p., 2017. Web. doi:10.2172/1371695.
Fondeur, F. F., & Jones, D. H.. Solvent hold tank sample results for MCU-16-1488-1493 (December 2016), MCU-17-86-88 (January 2017), and MCU-17-119-121 (February 2017): Quarterly Report. United States. doi:10.2172/1371695.
Fondeur, F. F., and Jones, D. H.. 2017. "Solvent hold tank sample results for MCU-16-1488-1493 (December 2016), MCU-17-86-88 (January 2017), and MCU-17-119-121 (February 2017): Quarterly Report". United States. doi:10.2172/1371695. https://www.osti.gov/servlets/purl/1371695.
@article{osti_1371695,
title = {Solvent hold tank sample results for MCU-16-1488-1493 (December 2016), MCU-17-86-88 (January 2017), and MCU-17-119-121 (February 2017): Quarterly Report},
author = {Fondeur, F. F. and Jones, D. H.},
abstractNote = {A trend summary of three Solvent Hold Tank (SHT) monthly samples; MCU-16-1488-1493 (December 2016), MCU-17-86-88 (January 2017), and MCU-17-119-121 (February 2017) are reported. Analyses indicate that the modifier (CS-7SB) and the extractant (MaxCalix) concentrations are at their nominal recommended levels (169,000 mg/L and 46,300 mg/L respectively). The suppressor (TiDG) level has decreased to a steady state level of 673 mg/L well above the minimum recommended level (479 mg/L). This analysis confirms the Isopar™ addition to the solvent in January 18, 2017. This analysis also indicates the solvent did not require further additions. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended. No impurities above the 1000 ppm level were found in this solvent by the Semi-Volatile Organic Analysis (SVOA). No impurities were observed in the Hydrogen Nuclear Magnetic Resonance (HNMR). Another impurity observed in the samples was mercury. Up to 38 ± 8 micrograms of mercury per mL of solvent was detected in these samples (the average of the CV-AA and XRF methods). The higher mercury concentration in the solvent (as determined in the last three monthly samples) is possibly due to the higher mercury concentration in Salt Batches 8 and 9 (Tank 49H) or mixing of previously undisturbed areas of high mercury concentration in Tank 49H. The gamma level (0.21E5 dpm/mL) measured in the February SHT sample was one order of magnitude lower than the gamma levels observed in the December and January SHT samples. The February gamma level is consistent with the solvent being idle (since January 10, 2017). The gamma levels observed in the December and January SHT samples were consistent with previous monthly measurements where the process operated normally. The laboratory will continue to monitor the quality of the solvent in particular for any new impurities or degradation of the solvent components.},
doi = {10.2172/1371695},
journal = {},
number = ,
volume = ,
place = {United States},
year = 2017,
month = 6
}

Technical Report:

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  • A trend summary of four Solvent Hold Tank (SHT) monthly samples; MCU-16-122-124 (March 2017), MCU-17-130-132 (April 2017), MCU-17-133-135 (May 2017), and MCU-17-141-149 (June 2017) are reported. Analyses of the June SHT sample (MCU-17-141-149) indicated that the modifier (CS-7SB) and the extractant (MaxCalix) concentrations were slightly below (4% each) their nominal recommended levels (169,000 mg/L and 46,400 mg/L respectively). The suppressor (TiDG) level has decreased since the January 2017 measurement but has remained steady in the range of 666 to 705 mg/L, well above the minimum recommended level (479 mg/L), but below the nominal level. The “flat” trends observed in themore » TiDG, MaxCalix, modifier, and Gamma measurement are consistent with the solvent being idle since January 10, 2017.« less
  • A trend summary that includes the last two Solvent Hold Tank (SHT) monthly samples is shown; MCU- 17-150-152 (July SHT) and MCU-17-153-155 (August SHT). Since the last SHT sample sent for analysis was the August sample the chemical state of the solvent is best approximated by the chemical analysis of the August SHT sample (MCU-17-153-155). This report mainly focused on the chemical analysis of the August SHT sample. The analysis data from the July SHT sample are presented in the “trend” plots of this report. Analysis of the August SHT sample (MCU-17-153-155) indicated that the modifier (CS-7SB) was 2% belowmore » but the extractant (MaxCalix) concentration was at its nominal recommended level (169,000 mg/L and 46,400 mg/L respectively). The suppressor (TiDG) level has decreased since the last measurement taken while the Modular Caustic-Side Solvent Extraction unit (MCU) was operating in January 2017, but has remained steady in the range of 666 (observed in April) to 715 mg/L (observed in the August 2017 sample) since February 2017, well above the minimum recommended level (479 mg/L), but below the nominal level. The “flat” trends observed in the TiDG, MaxCalix, modifier, and Gamma measurement are consistent with the solvent being idle since January 10, 2017. A strong correlation between density and modifier concentration in the solvent continues to be observed in the SHT samples. This analysis confirms the Isopar™L addition to the solvent in January 2017. This analysis also indicates the solvent did not require further additions. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time if the Modular Caustic-Side Solvent Extraction Unit (MCU) returns to processing radioactive liquid waste. Otherwise, the levels of these components will remain steady. A future Isopar™L trimming addition to the solvent is recommended when MCU resumes processing waste. Two unknown impurities related to the modifier (but not sec-butyl phenol: a modifier degradation product observed before) at the 290 and 110 mg/L levels were observed in the August SHT sample by the Gas - Chromatography-Mass Spectrometry (GC-MS) method. They were observed in a second GC-MS re-run with a new column. Their identification can’t be ascertained at this time. No impurities were observed in the Hydrogen Nuclear Magnetic Resonance (HNMR). Another impurity observed in the samples was mercury. Based on the August SHT sample, up to 23 ± 5 micrograms of mercury per mL of solvent was detected (the average of the Cold Vapor-Atomic Adsorption [CV-AA] and X-Ray Fluorescence [XRF] methods). The higher mercury concentration in the solvent (as determined in the last three-monthly samples) is possibly due to either a higher mercury concentration in Salt Batches 8 and 9 (Tank 49H) . The gamma level (~ 2.0E4 dpm/mL) measured in the August SHT samples was one order of magnitude lower than the gamma levels observed in the December 2016 and January 2017 SHT samples. A similar level was observed in the July SHT sample (MCU-SHT-150-152). The gamma level has remained consistently steady since January 10, 2017 when MCU stopped processing radioactive liquid waste. The laboratory will continue to monitor the quality of the solvent in particularly for any new impurities or degradation of the solvent components.« less
  • Savannah River National Lab (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-270-271-272), pulled on 02/21/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-270-271-272 indicated the Isopar TML concentration is above its nominal level (101%). The modifier (CS-7SB), the extractant (MaxCalix), and the TiDG concentrations are 7%, 6%, and 40% below their nominal concentrations. This analysis confirms the addition of TiDG, MaxCalix, and modifier to the solvent in November 2015. Based on the current monthly sample, the levels of TiDG, Isopar TML, MaxCalix, and modifier are sufficient for continuing operationmore » but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended.« less
  • Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-53-54-55), pulled on 01/25/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-53-54-55 indicated the Isopar™L, and MaxCalix are at nominal levels. The modifier and TiDG concentrations are 3% and 23 % below their nominal concentrations. This analysis confirms the addition of TiDG, MaxCalix, and modifier to the solvent on November 28, 2015. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time.more » Periodic characterization and trimming additions to the solvent are recommended. No impurities above the 1000 ppm level were found in this solvent by the Semi-Volatile Organic Analysis (SVOA). No impurities were observed in the Hydrogen Nuclear Magnetic Resonance (HNMR). However, the Fourier transform infra-red spectroscopy (FTIR) method detected trace levels (a few ppm) of amides (a possible degradation product of TiDG). In addition, up to 21 ± 4 micrograms of mercury per gram of solvent (or 17.5 μg/mL) was detected in this sample. There appears to be a possible correlation between the mercury level and the TiDG concentration in the solvent. The current gamma level (9.16 E4 dpm/mL) confirmed that the gamma concentration has returned to previous level where the process operated normally and as expected. The laboratory will continue to monitor the quality of the solvent in particular for any new impurities or degradation of the solvent components.« less
  • The Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-701, MCU-16-702 and MCU-16-703), pulled on 05/23/2016, and another set of SHT samples (MCU-16-710, MCU-16-711, and MCU-16-712) were pulled on 05/28/2016 after the solvent was superwashed with 300 mM sodium hydroxide for analysis. Samples MCU-16-701, MCU-16-702, and MCU-16-703 were combined into one sample (MCU-16-701-702-703) and samples MCU-16-710, MCU- 16-711, and MCU-16-712 were combined into one sample (MCU-16-710-711-712). Of the two composite samples MCU-16-710-711-712 represents the current chemical state of the solvent at MCU. All analytical conclusions are based on the chemical analysis of MCU-16-710-711-712. Theremore » were no chemical differences between MCU-16-701-702-703 and superwashed MCU-16-710-711-712. Analysis of the composited sample MCU-16-710-712-713 indicated the Isopar™L concentration is above its nominal level (102%). The modifier (CS-7SB) is 16% below its nominal concentration, while the TiDG and MaxCalix concentrations are at and above their nominal concentrations, respectively. The TiDG level has begun to decrease, and it is 7% below its nominal level as of May 28, 2016. Based on this current analysis, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended.« less