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Qualification of the First ICS-3000 ION Chromatograph for use at the Defense Waste Processing Facility

Description: The ICS-3000 Ion Chromatography (IC) system installed in 221-S M-13 has been qualified for use. The qualification was a head to head comparison of the ICS-3000 with the currently used DX-500 IC system. The crosscheck work included standards for instrument calibration and calibration verifications and standards for individual anion analysis, where the standards were traceable back to the National Institute of Standards and Technology (NIST). In addition the crosscheck work included the analysis of simulated Sludge Receipt Adjustment Tank (SRAT) Receipt, SRAT Product, and Slurry Mix Evaporator (SME) samples, along with radioactive Sludge Batch 5 material from the SRAT and SME tanks. Based upon the successful qualification of the ICS-3000 in M-13, it is recommended that this task proceed in developing the data to qualify, by a head to head comparison of the two ICS-3000 instruments, a second ICS-3000 to be installed in M-14. The Defense Waste Processing Facility (DWPF) requires the analysis of specific anions at various stages of its processing of high level waste (HLW). The anions of interest to the DWPF are fluoride, formate, chloride, nitrite, nitrate, sulfate, oxalate, and phosphate. The anion analysis is used to evaluate process chemistry including formic acid/nitric acid additions to establish optimum conditions for mercury stripping, reduction-oxidation (REDOX) chemistry for the melter, nitrite destruction, organic acid constituents, etc. The DWPF Laboratory (Lab) has been using Dionex DX-500 ion chromatography (IC) systems since 1998. The vendor informed DWPF in 2006 that the instruments would no longer be supported by service contracts after 2008. DWPF purchased three new ICS-3000 systems in September of 2006. The ICS-3000 instruments are (a) designed to be more stable using an eluent generator to make eluent, (b) require virtually no daily chemical handling by the analysts, (c) require less line breaks in the hood, and (d) generally require ...
Date: July 5, 2011
Creator: Edwards, T & Mahannah, R.
Partner: UNT Libraries Government Documents Department

Evaluation Of A Turbidity Meter For Use At The Defense Waste Processing Facility

Description: Savannah River Remediation's (SRR's) Defense Waste Processing Facility (DWPF) Laboratory currently tests for sludge carry-over into the Recycle Collection Tank (RCT) by evaluating the iron concentration in the Slurry Mix Evaporator Condensate Tank (SMECT) and relating this iron concentration to the amount of sludge solids present. A new method was proposed for detecting the amount of sludge in the SMECT that involves the use of an Optek turbidity sensor. Waste Services Laboratory (WSL) personnel conducted testing on two of these units following a test plan developed by Waste Solidification Engineering (WSE). Both Optek units (SN64217 and SN65164) use sensor model AF16-N and signal converter model series C4000. The sensor body of each unit was modified to hold a standard DWPF 12 cc sample vial, also known as a ''peanut'' vial. The purpose of this testing was to evaluate the use of this model of turbidity sensor, or meter, to provide a measurement of the sludge solids present in the SMECT based upon samples from that tank. During discussions of the results from this study by WSE, WSL, and Savannah River National Laboratory (SRNL) personnel, an upper limit on the acceptable level of solids in SMECT samples was set at 0.14 wt%. A ''go/no-go'' decision criterion was to be developed for the critical turbidity response, which is expressed in concentration units (CUs), for each Optek unit based upon the 0.14 wt% solids value. An acceptable or a ''go'' decision for the SMECT should reflect the situation that there is an identified risk (e.g. 5%) for a CU response from the Optek unit to be less than the critical CU value when the solids content of the SMECT is actually 0.14 wt% or greater, while a ''no-go'' determination (i.e., an Optek CU response above the critical CU value, a conservative decision relative ...
Date: January 15, 2013
Creator: Mahannah, R. N. & Edwards, T. B.
Partner: UNT Libraries Government Documents Department

EVALUATION OF A TURBIDITY METER FOR USE AT THE DEFENSE WASTE PROCESSING FACILITY

Description: Savannah River Remediation’s (SRR’s) Defense Waste Processing Facility (DWPF) Laboratory currently tests for sludge carry-over into the Recycle Collection Tank (RCT) by evaluating the iron concentration in the Slurry Mix Evaporator Condensate Tank (SMECT) and relating this iron concentration to the amount of sludge solids present. A new method was proposed for detecting the amount of sludge in the SMECT that involves the use of an Optek turbidity sensor. Waste Services Laboratory (WSL) personnel conducted testing on two of these units following a test plan developed by Waste Solidification Engineering (WSE). Both Optek units (SN64217 and SN65164) use sensor model AF16-N and signal converter model series C4000. The sensor body of each unit was modified to hold a standard DWPF 12 cc sample vial, also known as a “peanut” vial. The purpose of this testing was to evaluate the use of this model of turbidity sensor, or meter, to provide a measurement of the sludge solids present in the SMECT based upon samples from that tank. During discussions of the results from this study by WSE, WSL, and Savannah River National Laboratory (SRNL) personnel, an upper limit on the acceptable level of solids in SMECT samples was set at 0.14 weight percent (wt%). A “go/no-go” decision criterion was to be developed for the critical turbidity response, which is expressed in concentration units (CUs), for each Optek unit based upon the 0.14 wt% solids value. An acceptable or a “go” decision for the SMECT should reflect the situation that there is an identified risk (e.g. 5%) for a CU response from the Optek unit to be less than the critical CU value when the solids content of the SMECT is actually 0.14 wt% or greater, while a “no-go” determination (i.e., an Optek CU response above the critical CU value, a conservative ...
Date: June 4, 2013
Creator: Mahannah, R. & Edwards, T.
Partner: UNT Libraries Government Documents Department

QUALIFICATION OF THE SECOND ICS-3000 ION CHROMATOGRAPH FOR USE AT THE DEFENSE WASTE PROCESSING FACILITY

Description: The ICS-3000 Ion Chromatography (IC) system installed in 221-S M-14 has been qualified for use. The qualification testing was a head to head comparison of the second ICS-3000 with the initial ICS-3000 system that was installed in 221-S M-13. The crosscheck work included standards for instrument calibration and calibration verifications and standards for individual anion analysis, where the standards were traceable back to the National Institute of Standards and Technology (NIST). In addition the crosscheck work included the analysis of simulated Sludge Receipt and Adjustment Tank (SRAT) Receipt, SRAT Product, and Slurry Mix Evaporator (SME) samples, along with radioactive Sludge Batch 5 material from the SRAT and SME tanks. The Defense Waste Processing Facility (DWPF) requires the analysis of specific anions at various stages of its processing of high level waste (HLW). The anions of interest to the DWPF are fluoride, formate, chloride, nitrite, nitrate, sulfate, oxalate, and phosphate. The anion analysis is used to evaluate process chemistry including formic acid/nitric acid additions to establish optimum conditions for mercury stripping, reduction-oxidation (REDOX) chemistry for the melter, nitrite destruction, etc. The DWPF Laboratory (Lab) has recently replaced the Dionex DX-500 ion chromatography (IC) systems that had been used since 1998 by the first of two new ICS-3000 systems. The replacement effort was necessary due to the vendor of the DX-500 systems no longer supporting service contracts after 2008. DWPF purchased three new ICS-3000 systems in September of 2006. The ICS-3000 instruments are (a) designed to be more stable using an eluent generator to make eluent, (b) require virtually no daily chemical handling by the analysts, (c) require less line breaks in the hood, and (d) generally require less maintenance due to the pump configuration only using water versus the current system where the pump uses various hydroxide concentrations. The ICS-3000 instruments ...
Date: December 3, 2009
Creator: Edwards, T. & Mahannah, R.
Partner: UNT Libraries Government Documents Department

Qualification of the Nippon Instrumentation for use in Measuring Mercury at the Defense Waste Processing Facility

Description: The Nippon Mercury/RA-3000 system installed in 221-S M-14 has been qualified for use. The qualification was a side-by-side comparison of the Nippon Mercury/RA-3000 system with the currently used Bacharach Mercury Analyzer. The side-by-side testing included standards for instrument calibration verifications, spiked samples and unspiked samples. The standards were traceable back to the National Institute of Standards and Technology (NIST). The side-by-side work included the analysis of Sludge Receipt and Adjustment Tank (SRAT) Receipt, SRAT Product, and Slurry Mix Evaporator (SME) samples. With the qualification of the Nippon Mercury/RA-3000 system in M-14, the DWPF lab will be able to perform a head to head comparison of a second Nippon Mercury/RA-3000 system once the system is installed. The Defense Waste Processing Facility (DWPF) analyzes receipt and product samples from the Sludge Receipt and Adjustment Tank (SRAT) to determine the mercury (Hg) concentration in the sludge slurry. The SRAT receipt is typically sampled and analyzed for the first ten SRAT batches of a new sludge batch to obtain an average Hg concentration. This average Hg concentration is then used to determine the amount of steam stripping required during the concentration/reflux step of the SRAT cycle to achieve a less than 0.6 wt% Hg in the SRAT product solids. After processing is complete, the SRAT product is sampled and analyzed for mercury to ensure that the mercury concentration does not exceed the 0.45 wt% limit in the Slurry Mix Evaporator (SME). The DWPF Laboratory utilizes Bacharach Analyzers to support these Hg analyses at this facility. These analyzers are more than 10 years old, and they are no longer supported by the manufacturer. Due to these difficulties, the Bacharach Analyzers are to be replaced by new Nippon Mercury/RA-3000 systems. DWPF issued a Technical Task Request (TTR) for the Savannah River National Laboratory (SRNL) to assist ...
Date: July 5, 2011
Creator: Edwards, T. & Mahannah, R.
Partner: UNT Libraries Government Documents Department

Development Of Ion Chromatography Methods To Support Testing Of The Glycolic Acid Reductant Flowsheet In The Defense Waste Processing Facility

Description: Ion Chromatography (IC) is the principal analytical method used to support studies of Sludge Reciept and Adjustment Tank (SRAT) chemistry at DWPF. A series of prior analytical ''Round Robin'' (RR) studies included both supernate and sludge samples from SRAT simulant, previously reported as memos, are tabulated in this report.2,3 From these studies it was determined to standardize IC column size to 4 mm diameter, eliminating the capillary column from use. As a follow on test, the DWPF laboratory, the PSAL laboratory, and the AD laboratory participated in the current analytical RR to determine a suite of anions in SRAT simulant by IC, results also are tabulated in this report. The particular goal was to confirm the laboratories ability to measure and quantitate glycolate ion. The target was + or - 20% inter-lab agreement of the analyte averages for the RR. Each of the three laboratories analyzed a batch of 12 samples. For each laboratory, the percent relative standard deviation (%RSD) of the averages on nitrate, glycolate, and oxalate, was 10% or less. The three laboratories all met the goal of 20% relative agreement for nitrate and glycolate. For oxalate, the PSAL laboratory reported an average value that was 20% higher than the average values reported by the DWPF laboratory and the AD laboratory. Because of this wider window of agreement, it was concluded to continue the practice of an additional acid digestion for total oxalate measurement. It should also be noted that large amounts of glycolate in the SRAT samples will have an impact on detection limits of near eluting peaks, namely Fluoride and Formate. A suite of scoping experiments are presented in the report to identify and isolate other potential interlaboratory disceprancies. Specific ion chromatography inter-laboratory method conditions and differences are tabulated. Most differences were minor but there are ...
Date: October 1, 2013
Creator: Wiedenman, B. J.; White, T. L.; Mahannah, R. N.; Best, D. R.; Stone, M. E.; Click, D. R. et al.
Partner: UNT Libraries Government Documents Department