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The Ion-Exchange Separation of Zirconium and Hafnium

Description: In the course of a rather cursory examination of the elution of tetra-positive ions from the cation exchange resin Dowex 50 with hydrochloric acid solutions, the authors have discovered a very effective method of separating zirconium from hafnimu. In view of the great labor involved in preparing even reasonably pure hafnium compounds by existing methods, they feel that this procedure will prove very valuable to those interested in obtaining hafnium compounds free of zirconium. Although the conditions which give satisfactory separation were first worked out using microgram amounts of material and the radioactive tracer technique, the run described here, involving milligrams of material, illustrates the applicability of the method to the production of significant amounts of pure hafnium and zirconium.
Date: October 11, 1948
Creator: Street, Kenneth, Jr. & Seaborg, Glenn T.
Partner: UNT Libraries Government Documents Department

LAB STUDY ON REGENERATION OF SPENT DOWEX 21K 16-20 MESH ION EXCHANGE RESIN

Description: Currently the effort to remove chromate from groundwater in the 100K and 100H Areas uses DOWEX 21K 16-20. This report addresses the procedure and results of a laboratory study for regeneration of the spent resin by sodium hydroxide, sulfuric acid, or sodium sulfate to determine if onsite regeneration by the Effluent Treatment Facility is a feasible option.
Date: January 24, 2007
Creator: DUNCAN, J.B.
Partner: UNT Libraries Government Documents Department

Organic ion exchange resin separation methods evaluation

Description: This document describes testing to find effective methods to separate Organic Ion Exchange Resin (OIER) from a sludge simulant. This task supports a comprehensive strategy for treatment and processing of K-Basin sludge. The simulant to be used resembles sludge that has accumulated in the 105KE and 105KW Basins in the 1OOK area of the Hanford Site. The sludge is an accumulation of fuel element corrosion products, organic and inorganic ion exchange materials, canister gasket materials, iron and aluminum corrosion products, sand, dirt, and other minor amounts of organic matter.
Date: May 27, 1998
Creator: Witwer, K.S.
Partner: UNT Libraries Government Documents Department

New bifunctional anion-exchange resins for nuclear waste treatment: Part 2

Description: Additional bifunctional anion-exchange resins have been designed, synthesized and evaluated for their ability to take up Pu(IV) from nitric acid solutions. Bifunctionality is achieved by adding a second anion-exchange site to the pyridine nitrogen (also an anion-exchange site) of the base poly(4-vinylpyridine) resin. Previous work focused on the effect of varying the chemical properties of the added site along with the length of an alkylene spacer between the two sites. Here the authors examine four new 3- and 4-picolyl derivatives which maintain more rigidly defined geometries between the two nitrogen cationic sites. These materials, which have the two anion-exchange sites separated by three and four carbons, respectively, exhibit lower overall Pu(IV) distribution coefficients than the corresponding N-alkylenepyridium derivatives with more flexible spacers. Methylation of the second pyridium site results in a ca. 20% increase in the Pu(IV) distribution coefficients.
Date: June 1, 1997
Creator: Marsh, S.F.; Jarvinen, G.D.; Barr, M.E. & Bartsch, R.A.
Partner: UNT Libraries Government Documents Department

Cementation of residue ion exchange resins at Rocky Flats

Description: Ion exchange resins have been used to purify nitric acid solutions of plutonium at Rocky Flats since the 1950s. Spent ion exchange resins were retained for eventual recovery of residual plutonium, typically by incineration followed by the aqueous extraction of plutonium from the resultant ash. The elimination of incineration as a recovery process in the late 1980s and the absence of a suitable alternative process for plutonium recovery from resins led to a situation where spent ion exchange resins were simply placed into temporary storage. This report describes the method that Rocky Flats is currently using to stabilize residue ion exchange resins. The objective of the resin stabilization program is: (1) to ensure their safety during interim storage at the site, and (2) to prepare them for ultimate shipment to the Waste Isolation Pilot Plant (WIPP) in New Mexico. Included in the discussion is a description of the safety concerns associated with ion exchange resins, alternatives considered for their stabilization, the selection of the preferred treatment method, the means of implementing the preferred option, and the progress to date.
Date: March 3, 1998
Creator: Dustin, D.F.; Beckman, T.D. & Madore, C.M.
Partner: UNT Libraries Government Documents Department

Use of Cation Exchange Resins for Production of U{sub 3}O{sub 8} Suitable for the Al-U{sub 3}O{sub 8} Powder Metallurgy Process

Description: This report describes the production of U{sub 3}O{sub 8} powders from three types of cation exchange resins: Dowex 50W, a strong acid, sulfonate resin; AG MP-50, a macroporous form of sulfonate resin; and Bio-Rex 70, a weak acid, carboxylic resin.
Date: September 17, 2001
Creator: Mosley, W.C.
Partner: UNT Libraries Government Documents Department

Radionuclide Leaching from Organic Ion Exchange Resin

Description: Laboratory tests were performed to examine the efficacy of leach treatments for decontaminating organic ion exchange resins (OIER), which have been found in a number of samples retrieved from K East Basin sludge. Based on process records, the OIER found in the K Basins is a mixed-bet strong acid/strong base material marketed as Purolite{trademark} NRW-037. Radionuclides sorbed or associated with the OIER can restrict its disposal to the Environmental Restoration Disposal Facility (ERDF). The need for testing to support development of a treatment process for K Basin sludge has been described in Section 4.2 of ''Testing Strategy to Support the Development of K Basins Sludge Treatment Process'' (Flament 1998). To help understand the effects of anticipated OIER elutriation and washing, tests were performed with well-rinsed OIER material from K East Basin floor sludge (sample H-08 BEAD G) and with well-rinsed OIER having approximately 5% added K East canister composite sludge (sample KECOMP). The rinsed resin-bearing material also contained the inorganic ion exchanger Zeolon-900{trademark}, a zeolite primarily composed of the mineral mordenite. The zeolite was estimated to comprise 27 weight percent of the dry H-08 BEAD G material.
Date: April 2, 1999
Creator: Delegard, C.H. & Rinehart, D.E.
Partner: UNT Libraries Government Documents Department

Loading and unloading resin from MPPF rapid ion-exchange columns

Description: A process was developed which permits changing the resin in the Multipurpose Processing Facility Rapid Ion Exchange columns, without replacing the entire column assembly. The columns remain on the rack during the resin removal and replacement. The resin displacement process consists of a resin unloading and a resin loading step. During resin removal, the spent resin is hydraulically displaced from the columns to a resin collection tank, and then transferred to the evaporator for dissolution. Fresh resin is loaded into the empty column by hydraulic displacement or a combination of vacuum loading followed by hydraulic displacement. In the hydraulic displacement loading process, the amount of fresh resin needed to load the columns is transferred to a resin displacement tank where the resin is hydraulically displaced to the appropriate column. In the vacuum loading process, part of the resin feed is loaded directly into the column by applying a negative pressure to the column.
Date: October 1, 1981
Creator: Ng, W.C.
Partner: UNT Libraries Government Documents Department

Synthesis, structural characterization, and performance evaluation of resorcinol-formaldehyde (R-F) ion-exchange resin

Description: The 177 underground storage tanks at the DOE`s Hanford Site contain an estimated 180 million tons of high-level radioactive wastes. It is desirable to remove and concentrate the highly radioactive fraction of the tank wastes for vitrification. Resorcinol-formaldehyde (R-F) resin, an organic ion-exchange resin with high selectivity and capacity for the cesium ion, which is a candidate ion-exchange material for use in remediation of tank wastes. The report includes information on the structure/function analysis of R-F resin and the synthetic factors that affect performance of the resin. CS-100, a commercially available phenol-formaldehyde (P-F) resin, and currently the baseline ion-exchanger for removal of cesium ion at Hanford, is compared with the R-F resin. The primary structural unit of the R-F resin was determined to consist of a 1,2,3,4-tetrasubstituted resorcinol ring unit while CS-100, was composed mainly of a 1,2,4-trisubstituted ring. CS-100 shows the presence of phenoxy-ether groups, and this may account for the much lower decontamination factor of CS-100 for cesium ion. Curing temperatures for the R-F resin were found to be optimal at 105--130C. At lower temperatures, insufficient curing, hence crosslinking, of the polymer resin occurs and selectivity for cesium drops. Curing at elevated temperatures leads to chemical degradation. Optimal particle size for R-F resin is in the range of 20--50 mesh-sized particles. R-F resin undergoes chemical degradation or oxidation which destroys ion-exchange sites. The ion-exchange sites (hydroxyl groups) are converted to quinones and ketones. CS-100, though it has much lower performance for cesium ion-exchange, is significantly more chemically stable than R-F resin. To gamma radiation, CS-100 is more radiolytically stable than R-F resin.
Date: August 1, 1995
Creator: Hubler, T.L.; Franz, J.A.; Shaw, W.J.; Bryan, S.A.; Hallen, R.T.; Brown, G.N. et al.
Partner: UNT Libraries Government Documents Department

CORROSION STUDY FOR THE EFFLUENT TREATMENT FACILITY (ETF) CHROME (VI) REDUCTANT SOLUTION USING 304 & 316L STAINLESS STEEL

Description: The Effluent Treatment Facility has developed a method to regenerate spent resin from the groundwater pump and treat intercepting chrome(VI) plumes (RPP-RPT-32207, Laboratory Study on Regeneration of Spent DOWEX 21K 16-20 Mesh Ion Exchange Resin). Subsequent laboratory studies have shown that the chrome(VI) may be reduced to chrome(III) by titrating with sodium metabisulfite to an oxidation reduction potential (ORP) of +280 mV at a pH of 2. This test plan describes the use of cyclic potentiodynamic polarization and linear polarization techniques to ascertain the electrochemical corrosion and pitting propensity of the 304 and 316L stainless steel in the acidified reducing the solution that will be contained in either the secondary waste receiver tank or concentrate tank.
Date: June 27, 2007
Creator: DUNCAN, J.B.
Partner: UNT Libraries Government Documents Department

Uranium Adsorption on Ion-Exchange Resins - Batch Testing

Description: The uranium adsorption performance of five resins (Dowex 1, Dowex 21K 16-30 [fresh], Dowex 21K 16-30 [regenerated], Purofine PFA600/4740, and ResinTech SIR-1200) were tested using unspiked, nitrate-spiked, and nitrate-spiked/pH adjusted source water from well 299-W19-36. These batch tests were conducted in support of a resin selection process in which the best resin to use for uranium treatment in the 200-West Area groundwater pump-and-treat system will be identified. The results from these tests are as follows: • The data from the high-nitrate (1331 mg/L) tests indicated that Dowex 1, Dowex 21K 16-30 (fresh), Purofine PFA600/4740, and ResinTech SIR-1200 all adsorbed uranium similarly well with Kd values ranging from ~15,000 to 95,000 ml/g. All four resins would be considered suitable for use in the treatment system based on uranium adsorption characteristics. • Lowering the pH of the high nitrate test conditions from 8.2 to 7.5 did not significantly change the uranium adsorption isotherms for the four tested resins. The Kd values for these four resins under high nitrate (1338 mg/L), lower pH (7.5) ranged from ~15,000 to 80,000 ml/g. • Higher nitrate concentrations greatly reduced the uranium adsorption on all four resins. Tests conducted with unspiked (no amendments; nitrate at 337 mg/L and pH at 8.2) source water yielded Kd values for Dowex 1, Dowex 21K 16-30 (fresh), Purofine PFA600/4740, and ResinTech SIR-1200 resins ranging from ~800,000 to >3,000,000 ml/g. These values are about two orders of magnitude higher than the Kd values noted from tests conducted using amended source water. • Compared to the fresh resin, the regenerated Dowex 21K 16-30 resin exhibited significantly lower uranium-adsorption performance under all test conditions. The calculated Kd values for the regenerated resin were typically an order of magnitude lower than the values calculated for the fresh resin. • Additional testing using laboratory columns is ...
Date: December 1, 2010
Creator: Mattigod, Shas V.; Golovich, Elizabeth C.; Wellman, Dawn M.; Cordova, Elsa A. & Smith, Ronald M.
Partner: UNT Libraries Government Documents Department

Processing of $sup 238$Pu and $sup 237$Np with macroporous anion exchange resin

Description: ' Dowex'' MSA-1 macroporous anion exchange was found to be superior to Dowex'' 1 gel-type resin for separation and purification of /sup 238/Pu and /sup 237/Np. Higher actinide loading per unit of resin is attained, and elution is accomplished in smaller volume. Crosscontamination of the products is lower with macroporous resin, and higher processing rates can be attained. Process performance with different lots of macroporous resin is more consistent than generally obtained with different lots of Dowex'' 1 resin because the high porosity of the macroporous resin facilitates ionic diffusion. The chemical, thermal, and radiolytic stabilities of macroporous and gel-type resins are similar. (auth)
Date: November 1, 1973
Creator: Thompson, G.H. & Burney, G.A.
Partner: UNT Libraries Government Documents Department

Field lysimeter investigations: Low-level waste data base development program for fiscal year 1996. Annual report; Volume 9

Description: A data base development program, funded by the US Nuclear Regulatory Commission, is (a) studying the degradation effects in organic ion-exchange resins caused by radiation, (b) examining the adequacy of test procedures recommended in the Branch Technical Position on Waste Form to meet the requirements of 10 CFR 61 using solidified ion-exchange resins, (c) obtaining performance information on solidified ion-exchange resins in a disposal environment, and (d) determining the condition of liners used to dispose the ion-exchange resins. During the field testing experiments, both portland type 1--2 cement and Dow vinyl ester-styrene waste form samples were tested in lysimeter arrays located at Argonne National Laboratory-East (ANL-E) in Illinois and at Oak Ridge National Laboratory (ORNL). The study was designed to provide continuous data on nuclide release and movement, as well as environmental conditions, over an extended period. Those experiments have been shut down and are to be exhumed. This report discusses the plans for removal, sampling, and analysis of waste form and soil cores from the lysimeters. Results of partition coefficient determinations are presented, as well as application of a source term computer code using those coefficients to predict the lysimeter results. A study of radionuclide-containing colloids associated with the leachate waters removed from these lysimeters is described. An update of upward migration of radionuclides in the sand-filled lysimeter at ORNL is included.
Date: August 1997
Creator: McConnell, J. W., Jr.; Rogers, R. D.; Larsen, I. L.; Jastrow, J. D.; Sanford, W. E.; Sullivan, T. M. et al.
Partner: UNT Libraries Government Documents Department

Decontamination of Dissolved Salt Solution from Tank 19F Using Duolite CS-100 and Amberlite IRC-718 Resins

Description: In this study actual Savannah River Plant liquid supernate solutions were processed to refine and verify these synthetic solution studies. The main objectives were: (1) confirm high decontamination factors (DFs) for cesium-137 and strontium-90 using Duolite CS-100 and Amberlite IRC-718 ion exchange resins, (2) obtain DFs for other minor radioactive isotopes such as plutonium, technetium and ruthenium, (3) provide ion exchange elutriant containing cesium-137, strontium-90 and other radioactive isotopes for ''hot'' melter studies, (4) determine the quality of the decontaminated salt solution, and (5) provide actual decontaminated salt solution for saltcrete development programs.
Date: October 17, 2001
Creator: Lee, L.M.
Partner: UNT Libraries Government Documents Department

Initial evaluation of two organic resins and their ion exchange column performance for the recovery of cesium from Hanford alkaline wastes

Description: The contents of Hanford`s 177 underground storage tanks include a mixture of sludge, salt cake and alkaline supernatant liquids. Most of the cesium is expected to be in the aqueous liquids and it is these solutions that are the focus of the cesium ion exchange removal process. This process is being designed with the goal of removing enough cesium so that the resulting low-level waste (LLW) will meet the NRC 10CFR61 class A limits for {sup 137}Cs (1 Ci/m{sup 3}). The overall objective of the WHC program is (1) to evaluate ion exchange materials for the recovery of cesium from alkaline wastes, (2) to determine their loading and elution capacities, (3) to determine the physical life cycle (including radiation and chemical stability) for selected ion exchangers, (4) to determine if basic ion exchange data can be applied to a broad range of tank wastes, and (5) to provide credible laboratory data for engineering-scale evaluation and ion exchange media selection. The goal will be to provide the technology to produce a Class A waste. The results presented in this document provide initial test cesium loading and elution results for ion exchange column operations for two selected ion exchange resins under a limited range of conditions. Data in this report can be found in PNL laboratory record books BNW 54705 and BNW 55026.
Date: April 1, 1996
Creator: Bray, L.A.; Carson, K.J.; Elovich, R.J.; Carlson, C.D.; DesChane, J.R. & Kurath, D.E.
Partner: UNT Libraries Government Documents Department

Radionuclide Sensors for Water Monitoring

Description: Completed off-line measurements of 99Tc with solid-state semiconductor detectors - Began evaluation of the above detection system for on-line measurements - Discontinued development of macroporous scintillating YSO - Conducted light collection efficiency of heterogeneous scintillators experiments and Monte Carlo simulations Batch sorption of 99TcO4- onto anion exchange resin and measurement with solid-state semiconductor detectors is completed. Solid-state semiconductor detection using a passive ion implanted planar silicon (PIPS) detector of beta radiation from 99Tc is being investigated as an alternative to scintillation detection. There are advantages and disadvantages to each approach, which are being quantified. To utilize the CAM PIPS detector, 99TcO4- is being concentrated on DOWEX 1 resin. The batch procedure involves the aqueous solution and the resin coming in direct contact with the PIPS detector. The PIPS is spray coated with Teflon AF polymer to offer an additional thin (4-14 micrometers) barrier to the already rugged design. During equilibration time, the solution and resin are mechanically stirred. After sufficient contact time, the resin gravimetrically settles to the surface of the PIPS detector, at which point the detection commences. We are in the process of modifying this method for a continuous flow regime. With this new configuration the spent resin can be removed as a slurry from the detector and replaced with virgin resin. Using the batch arrangement we are able to obtain a detection efficiency of 14% with 0.01 g of resin. The background count rate 0.32 cps. The background count rate is significantly higher than one normally associates with a PIPS detector, this is the result of having to increase the amplifier gain to be able to observe the low energy deposition from the beta interaction. Reduction of the background may be accomplished by one of two methods: (1) digital signal processing or (2) cooling the detector to ...
Date: June 1, 2003
Creator: Devol, Timothy A.
Partner: UNT Libraries Government Documents Department

Separation of $sup 238$Pu from $sup 237$Np by pressurized anion exchange

Description: Pressurized anion exchange with small particle ( ~2OO mesh) Dowex MSA-1 macroporous ion resin gave excellent separation of /sup 238/Pu from /sup 237/Np. Separation was satisfactory with ~9O mesh Dowex 1-X4 gel-type resin at 3 to 4 times the fiow rates normally used in the Savannah River Plant with 40 to 60 mesh Dowex 1 resin. Results wth small-particle Dowex 1-X2 in the pressurized system were not satisfactory because the resin beads deformed due to low structural stabiliiy, with resulting excessive pressure drop and poor separation. Small- particle Dowex 1-X6 was very ineffective because of slow ionic diffusion in the resin matrix. The excellent performance of the macroporous resin is attributed to rapid ionic diffusion resulting from high resin porosity. The pressurized system was Operated safely at temperatures up to 55 deg C and pressures up to 350 psig. (auth)
Date: January 1, 1974
Creator: Burney, G.A. & Thompson, G.H.
Partner: UNT Libraries Government Documents Department

Simplified method for the preparation of micro samples for the simultaneous isotopic analysis of uranium and plutonium

Description: A basic anion resin is employed to selectively adsorb plutonium and uranium from 8 M HNO$sub 3$ solutions containing dissolved spent reactor fuels. After a few beads of the resin are equilibrated with the solution, a single bead is used for establishing the isotopic composition of plutonium and uranium. The resin bead separation essentially removes all possible isobaric interference from such elements as americium and curium and at the same time eliminates most fission product contamination in the mass spectrometer. Small aliquots of dissolver solution that contain 10$sup -6$g of U and 10$sup -8$ g of Pu are adequate for preparing about ten resin beads. By employing a single-focusing, tandem-magnet-type mass spectrometer, equipped with pulse counting for ion detection, simultaneous plutonium and uranium assays are obtained. The quantity of each element per bead may be as low as 10$sup -9$ to 10$sup -10$g. The technique of isotope dilution can be coupled with the ion exchange bead separation and used effectively for measuring the total quantity of U and Pu. The technique possesses advantages such as: reduced radiation hazards from the infinitely smaller samples, thus less shielding and transport cost for sample handling; greatly simplified chemical preparations that eliminate fission products and actinide isobaric interferences; and the minor isotopes are more precisely established. (auth)
Date: January 1, 1974
Creator: Carter, J.A.; Walker, R.L.; Eby, R.E. & Pritchard, C.A.
Partner: UNT Libraries Government Documents Department

TECHNETIUM SORPTION MEDIA REVIEW

Description: This report presents information and references to aid in the selection of 99Tc sorption media for feasibility studies regarding the removal of 99Tc from Hanford's low activity waste. The report contains literature search material for sorption media (including ion exchange media) for the most tested media to date, including SuperLig 639, Reillex HPQ, TAM (Kruion), Purolite A520E and A530E, and Dowex 1X8. The U.S. Department of Energy (DOE), Office of River Protection (ORP) is responsible for management and completion of the River Protection Project (RPP) mission, which comprises both the Hanford Site tank farms and the Waste Treatment and Immobilization Plant (WTP). The RPP mission is to store, retrieve and treat Hanford's tank waste; store and dispose of treated wastes; and close the tank farm waste management areas and treatment facilities in a safe, environmentally compliant, cost-effective and energy-effective manner.
Date: August 25, 2011
Creator: JB, DUNCAN; SE, KELLY; RA, ROBBINS; RD, ADAMS; MA, THORSON & CC, HAASS
Partner: UNT Libraries Government Documents Department

ADVANCES IN HEXAVALENT CHROMIUM REMOVAL AT HANFORD

Description: At the Hanford Site, chromium was used as a corrosion inhibitor in the reactor cooling water and was introduced into the groundwater as a result of planned and unplanned discharges from reactors during plutonium production since 1944. Beginning in 1995, groundwater treatment methods were evaluated leading to the use of pump and treat facilities with ion exchange using Dowex 21 K, a regenerable strong base anion exchange resin. This required regeneration of the resin, which is currently performed offsite. Resin was installed in a 4 vessel train, with resin removal required from the lead vessel approximately once a month. In 2007, there were 8 trains (32 vessels) in operation. In 2008, DOE recognized that regulatory agreements would require significant expansion in the groundwater chromium treatment capacity. Previous experience from one of the DOE project managers led to identification of a possible alternative resin, and the contractor was requested to evaluate alternative resins for both cost and programmatic risk reductions. Testing was performed onsite in 2009 and 2010, using a variety of potential resins in two separate facilities with groundwater from specific remediation sites to demonstrate resin performance in the specific groundwater chemistry at each site. The testing demonstrated that a weak base anion single-use resin, ResinTech SIR-700, was effective at removing chromium, had a significantly higher capacity, could be disposed of efficiently on site, and would eliminate the complexities and programmatic risks from sampling, packaging, transportation and return of resin for regeneration. This resin was installed in Hanford's newest groundwater treatment facility, called 100-DX, which began operations in November, 2010, and used in a sister facility, 100-HX, which started up in September of 2011. This increased chromium treatment capacity to 25 trains (100 vessels). The resin is also being tested in existing facilities that utilize Dowex 21 K for conversion ...
Date: January 30, 2012
Creator: Neshem, D. O. & Riddelle, J.
Partner: UNT Libraries Government Documents Department