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Enhancing the analytical performance of laser-induced breakdown spectroscopy

Description: This is the final report of a one-year, Laboratory Directed Research and Development (LDRD) project at Los Alamos National Laboratory (LANL). The objective of this work is to enhance the analytical capabilities of laser-induced breakdown spectroscopy (LIBS). LIBS is a method of elemental analysis in which powerful laser pulses are focused on a sample to form a microplasma. LIBS is perhaps the most versatile elemental analysis method, applicable to a variety of different real-world analysis problems. Therefore, it is important to enhance the capabilities of the method as much as possible. Accomplishments include: (1) demonstration of signal enhancements of 5--30 times from soils and metals using a double pulse method; (2) development of a model of the observed enhancement obtained using double pulses; (3) demonstration that the analytical performance achievable using low laser-pulse energies (10 and 25 mJ) can match that achievable using an energy of 100 mJ; and (4) demonstration that time-gated detection is not necessary with LIBS.
Date: December 31, 1998
Creator: Cremers, D.A.; Chinni, R.C.; Pichahchy, A.E. & Thornquist, H.K.
Partner: UNT Libraries Government Documents Department

In Situ Causticizing for Black Liquor Gasification

Description: Black liquor gasification offers a number of attractive incentives to replace Tomlinson boilers but it also leads to an increase in the causticizing load. Reasons for this have been described in previous reports (FY04 ERC, et.al.). The chemistries have also been covered but will be reviewed here briefly. Experimental results of the causticizing reactions with black liquor are presented here. Results of the modeling work were presented in detail in the Phase 1 report. They are included in Table 2 for comparison but will not be discussed in detail. The causticizing agents were added to black liquor in the ratios shown in Table 1, mixed, and then spray-dried. The mixture ratios (doping levels) reflect amount calculated from the stoichiometry above to achieve specified conversions shown in the table. The solids were sieved to 63-90 microns for use in the entrained flow reactors. The firing conditions are shown in Table 2. Pictures and descriptions of the reactors can be found in the Phase 1 annual report. Following gasification, the solids (char) was collected and analyzed by coulometric titration (for carbonate and total carbon), and by inductively coupled plasma emission spectroscopy (ICP) for a wide array of metals.
Date: October 1, 2005
Creator: Sinquefield, Scott Alan
Partner: UNT Libraries Government Documents Department

Chemical and isotopic variations of precipitation in the Los Alamos Region, New Mexico

Description: Precipitation collectors were installed at 14 locations on the Pajarito Plateau and surrounding areas to study variations in chemistry, stable isotopes and tritium for the years 1990 to 1993. The volume of precipitation was measured and samples were collected and analyzed every three to four months. All precipitation samples contain <2.50 mg/kg Cl and have pH values ranging from 5.4 to 6.7. The stable isotope ({delta}D/{delta}{sup 18}O) results record seasonal variations in precipitation as the weather patterns shift from sources in the Pacific Ocean to sources in the Gulf of Mexico. The stable isotope results also show isotopic variations due to elevation differences among the collection points. The tritium contents ({sup 3}H) in rain samples vary from 6.54 T.U. to 141 T.U. Contouring of high tritium values (e.g. >20 T.U.) from each collection period clearly shows that Laboratory activities release some tritium to the atmosphere. The effect of these releases are well below the limits set by the Environmental Protection Agency for drinking water (about 6200 T.U.). The magnitude of the releases is apparently greatest during the summer months. However, anomalous tritium values are detected as far north as Espahola, New Mexico for many collection periods. Tritium releases by the Laboratory are not constant; thus, the actual amount of tritium in each release has been diluted in the composite samples of our three to four month collection periods.
Date: February 1, 1995
Creator: Adams, A.I.; Goff, F. & Counce, D.
Partner: UNT Libraries Government Documents Department

TRACE ELEMENT ANALYSES OF URANIUM MATERIALS

Description: The Savannah River National Laboratory (SRNL) has developed an analytical method to measure many trace elements in a variety of uranium materials at the high part-per-billion (ppb) to low part-per-million (ppm) levels using matrix removal and analysis by quadrapole ICP-MS. Over 35 elements were measured in uranium oxides, acetate, ore and metal. Replicate analyses of samples did provide precise results however none of the materials was certified for trace element content thus no measure of the accuracy could be made. The DOE New Brunswick Laboratory (NBL) does provide a Certified Reference Material (CRM) that has provisional values for a series of trace elements. The NBL CRM were purchased and analyzed to determine the accuracy of the method for the analysis of trace elements in uranium oxide. These results are presented and discussed in the following paper.
Date: June 9, 2008
Creator: Beals, D & Charles Shick, C
Partner: UNT Libraries Government Documents Department

LDRD final report on high power broadly tunable Mid-IR quantum cascade lasers for improved chemical species detection.

Description: The goal of our project was to examine a novel quantum cascade laser design that should inherently increase the output power of the laser while simultaneously providing a broad tuning range. Such a laser source enables multiple chemical species identification with a single laser and/or very broad frequency coverage with a small number of different lasers, thus reducing the size and cost of laser based chemical detection systems. In our design concept, the discrete states in quantum cascade lasers are replaced by minibands made of multiple closely spaced electron levels. To facilitate the arduous task of designing miniband-to-miniband quantum cascade lasers, we developed a program that works in conjunction with our existing modeling software to completely automate the design process. Laser designs were grown, characterized, and iterated. The details of the automated design program and the measurement results are summarized in this report.
Date: January 1, 2006
Creator: Wanke, Michael Clement; Hudgens, James J.; Fuller, Charles T.; Samora, Sally; Klem, John Frederick & Young, Erik W.
Partner: UNT Libraries Government Documents Department

Multi-parameter on-line coal bulk analysis. Quarterly report, March 16--June 15, 1997

Description: An on-line coal analyzer is being developed as a joint venture between the French company SODERN which specializes in the manufacturing of neutron generators and associated electronics and the John B. Long Company which specializes in coal sampling equipment. Progress this quarter is summarized under the following topical headings: Measurement layout; Detector temperature stabilization; Raw coal library; and Determination of Btu content from elemental concentrations.
Date: December 31, 1997
Creator: Vourvopoulos, G.
Partner: UNT Libraries Government Documents Department

Metal Mesh Smear Sampling for Glow Discharge Analytical Spectroscopy

Description: Metal mesh smear sampling is being developed and evaluated for use in a number of glow discharge and other optical and mass spectrometric techniques. Sensitive elemental and isotopic analyses thus will be coupled with a convenient sampling scheme similar to one that is common for radiological surveys.
Date: June 1, 2000
Creator: Shaw, R.W.; Barshick, C.M.; Ramsey, J.M. & Smith, D.H.
Partner: UNT Libraries Government Documents Department

STATISTICAL REVIEW OF CESIUM CARBONATE FUSION MEASUREMENTS OF ARCHIVED GLASS SAMPLES FROM THE DWPF PROCESS

Description: This technical report provides a statistical review of measurements that the Defense Waste Processing Facility (DWPF) Laboratory (Lab) generated by Inductively-Coupled Plasma--Atomic Emission Spectroscopy (ICP-AES) for samples of archived Slurry Mix Evaporator (SME) glass that were prepared using a cesium carbonate (Cs{sub 2}CO{sub 3}) fusion dissolution method. Measurements were generated by both of the Lab's ICPs, which are designated as M-13 and M-14. Comparisons between the two ICPs suggest that for the ARG-1 measurements the M-14 provided lower (on average) concentration measurements for about 13 of the 16 elements reported by DWPF with Cr, Mn, Ni, and Zr being statistically lower (at a 5% significance level) for the ARG-1 samples. One of the three exceptions is Li, for which the M-14 yielded (on average) higher concentration measurements than the M-13. For the SME samples, the M-14 and M-13 measurements had statistically different (at the 5% significance level) means for B, Ca, Cr, Cu, Fe, Li, Mg, Mn, Na, Ni, Si, Ti, U, and Zr with the M-14 being lower than the M-13 for all of these elements except for Li. For the screened SME samples, statistically significant (at the 5% level) differences between the means of the Cs{sub 2}CO{sub 3} and prototypic preparations are seen for Ca (Cs{sub 2}CO{sub 3} higher for both ICPs), Cr (Cs{sub 2}CO{sub 3} higher for both ICPs), Cu (Cs{sub 2}CO{sub 3} higher for M-13), K (Cs{sub 2}CO{sub 3} higher for M-13), Mn (Cs{sub 2}CO{sub 3} lower for M-14), Ni (Cs{sub 2}CO{sub 3} lower for M-14), Si (Cs{sub 2}CO{sub 3} lower for M-14), Ti (Cs{sub 2}CO{sub 3} higher for M-13), U (Cs{sub 2}CO{sub 3} higher for both ICPs), and Zr (Cs{sub 2}CO{sub 3} lower for M-14). The Cs{sub 2}CO{sub 3} fusion method provided elemental of glass samples made from SME batches that were statistically comparable to ...
Date: July 31, 2006
Creator: Edwards, T
Partner: UNT Libraries Government Documents Department

RHEOLOGICAL AND ELEMENTAL ANALYSES OF SIMULANT SB5 SLURRY MIX EVAPORATOR-MELTER FEED TANK SLURRIES

Description: The Defense Waste Processing Facility (DWPF) will complete Sludge Batch 5 (SB5) processing in fiscal year 2010. DWPF has experienced multiple feed stoppages for the SB5 Melter Feed Tank (MFT) due to clogs. Melter throughput is decreased not only due to the feed stoppage, but also because dilution of the feed by addition of prime water (about 60 gallons), which is required to restart the MFT pump. SB5 conditions are different from previous batches in one respect: pH of the Slurry Mix Evaporator (SME) product (9 for SB5 vs. 7 for SB4). Since a higher pH could cause gel formation, due in part to greater leaching from the glass frit into the supernate, SRNL studies were undertaken to check this hypothesis. The clogging issue is addressed by this simulant work, requested via a technical task request from DWPF. The experiments were conducted at Aiken County Technology Laboratory (ACTL) wherein a non-radioactive simulant consisting of SB5 Sludge Receipt and Adjustment Tank (SRAT) product simulant and frit was subjected to a 30 hour SME cycle at two different pH levels, 7.5 and 10; the boiling was completed over a period of six days. Rheology and supernate elemental composition measurements were conducted. The caustic run exhibited foaming once, after 30 minutes of boiling. It was expected that caustic boiling would exhibit a greater leaching rate, which could cause formation of sodium aluminosilicate and would allow gel formation to increase the thickness of the simulant. Xray Diffraction (XRD) measurements of the simulant did not detect crystalline sodium aluminosilicate, a possible gel formation species. Instead, it was observed that caustic conditions, but not necessarily boiling time, induced greater thickness, but lowered the leach rate. Leaching consists of the formation of metal hydroxides from the oxides, formation of boric acid from the boron oxide, and dissolution ...
Date: February 8, 2010
Creator: Fernandez, A.
Partner: UNT Libraries Government Documents Department

TANK 40 FINAL SB4 CHEMICAL CHARACTERIZATION RESULTS

Description: A sample of Sludge Batch 4 (SB4) was pulled from Tank 40 in order to obtain radionuclide inventory analyses necessary for compliance with the Waste Acceptance Product Specifications (WAPS). This sample was also analyzed for elemental and chemical composition including noble metals. These analyses along with the WAPS analyses will help define the composition of the sludge currently in Tank 40 which is currently being fed to DWPF and will become part of Sludge Batch 5 (SB5). At SRNL the 3-L Tank 40 SB4 sample was transferred from the shipping container into a 4-L vessel and solids allowed to settle overnight. Supernate was then siphoned off and circulated through the shipping container to complete the transfer of the sample. Following thorough mixing of the 3-L sample, a 280 g sub-sample was removed. This sub-sample was then utilized for all subsequent analytical samples. Eight separate aliquots of the slurry were digested, four with HNO{sub 3}/HCl in sealed Teflon{reg_sign} vessels and four in Na{sub 2}O{sub 2} using Zr crucibles. Due to the use of Zr crucibles and Na in the peroxide fusions, Na and Zr cannot be determined from this preparation. Three glass standards were digested along with a blank for each preparation. Each aqua regia digestion and blank was diluted and submitted to Analytical Development (AD) for inductively coupled plasma-atomic emission spectroscopy (ICP-AES) analysis, inductively coupled plasma-mass spectrometry (ICP-MS) analysis, and cold vapor atomic absorption (CV-AA) analysis. Equivalent dilutions of the peroxide fusion digestions and blank were submitted to AD for ICP-AES analysis. Tank 40 SB4 supernate was collected from a mixed slurry sample in the SRNL Shielded Cells and submitted to AD for ICP-AES and ICP-MS. Weighted dilutions of slurry were submitted for ion chromatography (IC), total inorganic carbon/total organic carbon (TIC/TOC), and total base analyses. A sample of Tank ...
Date: January 30, 2008
Creator: Best, J
Partner: UNT Libraries Government Documents Department

TANK 40 FINAL SB5 CHEMICAL CHARACTERIZATION RESULTS PRIOR TO NP ADDITION

Description: A sample of Sludge Batch 5 (SB5) was pulled from Tank 40 in order to obtain radionuclide inventory analyses necessary for compliance with the Waste Acceptance Product Specifications (WAPS). This sample was also analyzed for chemical composition including noble metals. Prior to radionuclide inventory analyses, a final sample of the H-canyon Np stream will be added to bound the Np addition anticipated for Tank 40. These analyses along with the WAPS radionuclide analyses will help define the composition of the sludge in Tank 40 that is currently being fed to DWPF as SB5. At the Savannah River National Laboratory (SRNL) the 3-L Tank 40 SB5 sample was transferred from the shipping container into a 4-L high density polyethylene vessel and solids allowed to settle overnight. Supernate was then siphoned off and circulated through the shipping container to complete the transfer of the sample. Following thorough mixing of the 3-L sample, a 239 g sub-sample was removed. This sub-sample was then utilized for all subsequent analytical samples. Eight separate aliquots of the slurry were digested, four with HNO{sub 3}/HCl (aqua regia) in sealed Teflon{reg_sign} vessels and four in Na{sub 2}O{sub 2} (alkali or peroxide fusion) using Zr crucibles. Due to the use of Zr crucibles and Na in the peroxide fusions, Na and Zr cannot be determined from this preparation. Additionally, other alkali metals, such as Li and K that may be contaminants in the Na{sub 2}O{sub 2} are not determined from this preparation. Three Analytical Reference Glass-1 (ARG-1) standards were digested along with a blank for each preparation. The ARG-1 glass allows for an assessment of the completeness of each digestion. Each aqua regia digestion and blank was diluted to 1:100 mL with deionized water and submitted to Analytical Development (AD) for inductively coupled plasma--atomic emission spectroscopy (ICPAES) analysis, inductively ...
Date: February 26, 2009
Creator: Bannochie, C & Damon Click, D
Partner: UNT Libraries Government Documents Department

Evaluation of Wet Chemical ICP-AES Elemental Analysis Methods usingSimulated Hanford Waste Samples-Phase I Interim Report

Description: The wet chemistry digestion method development for providing process control elemental analyses of the Hanford Tank Waste Treatment and Immobilization Plant (WTP) Melter Feed Preparation Vessel (MFPV) samples is divided into two phases: Phase I consists of: (1) optimizing digestion methods as a precursor to elemental analyses by ICP-AES techniques; (2) selecting methods with the desired analytical reliability and speed to support the nine-hour or less turnaround time requirement of the WTP; and (3) providing baseline comparison to the laser ablation (LA) sample introduction technique for ICP-AES elemental analyses that is being developed at the Savannah River National Laboratory (SRNL). Phase II consists of: (1) Time-and-Motion study of the selected methods from Phase I with actual Hanford waste or waste simulants in shielded cell facilities to ensure that the methods can be performed remotely and maintain the desired characteristics; and (2) digestion of glass samples prepared from actual Hanford Waste tank sludge for providing comparative results to the LA Phase II study. Based on the Phase I testing discussed in this report, a tandem digestion approach consisting of sodium peroxide fusion digestions carried out in nickel crucibles and warm mixed-acid digestions carried out in plastic bottles has been selected for Time-and-Motion study in Phase II. SRNL experience with performing this analytical approach in laboratory hoods indicates that well-trained cell operator teams will be able to perform the tandem digestions in five hours or less. The selected approach will produce two sets of solutions for analysis by ICP-AES techniques. Four hours would then be allocated for performing the ICP-AES analyses and reporting results to meet the nine-hour or less turnaround time requirement. The tandem digestion approach will need to be performed in two separate shielded analytical cells by two separate cell operator teams in order to achieve the nine-hour or less ...
Date: April 30, 2005
Creator: Coleman, Charles J. & Edwards, Thomas B.
Partner: UNT Libraries Government Documents Department

DEFENSE WASTE PROCESSING FACILITY ANALYTICAL METHOD VERIFICATION FOR THE SLUDGE BATCH 5 QUALIFICATION SAMPLE

Description: For each sludge batch that is processed in the Defense Waste Processing Facility (DWPF), the Savannah River National Laboratory (SRNL) performs confirmation of the applicability of the digestion method to be used by the DWPF lab for elemental analysis of Sludge Receipt and Adjustment Tank (SRAT) receipt samples and SRAT product process control samples. DWPF SRAT samples are typically dissolved using a room temperature HF-HNO3 acid dissolution (i.e., DWPF Cold Chem Method, see Procedure SW4-15.201) and then analyzed by inductively coupled plasma - atomic emission spectroscopy (ICP-AES). This report contains the results and comparison of data generated from performing the Aqua Regia (AR), Sodium Peroxide/Hydroxide Fusion (PF) and DWPF Cold Chem (CC) method digestion of Sludge Batch 5 (SB5) SRAT Receipt and SB5 SRAT Product samples. The SB5 SRAT Receipt and SB5 SRAT Product samples were prepared in the SRNL Shielded Cells, and the SRAT Receipt material is representative of the sludge that constitutes the SB5 Batch composition. This is the sludge in Tank 51 that is to be transferred into Tank 40, which will contain the heel of Sludge Batch 4 (SB4), to form the SB5 Blend composition. The results for any one particular element should not be used in any way to identify the form or speciation of a particular element in the sludge or used to estimate ratios of compounds in the sludge. A statistical comparison of the data validates the use of the DWPF CC method for SB5 Batch composition. However, the difficulty that was encountered in using the CC method for SB4 brings into question the adequacy of CC for the SB5 Blend. Also, it should be noted that visible solids remained in the final diluted solutions of all samples digested by this method at SRNL (8 samples total), which is typical for the DWPF ...
Date: July 25, 2008
Creator: Click, D; Tommy Edwards, T & Henry Ajo, H
Partner: UNT Libraries Government Documents Department

Active voltammetric microsensors with neural signal processing.

Description: Many industrial and environmental processes, including bioremediation, would benefit from the feedback and control information provided by a local multi-analyte chemical sensor. For most processes, such a sensor would need to be rugged enough to be placed in situ for long-term remote monitoring, and inexpensive enough to be fielded in useful numbers. The multi-analyte capability is difficult to obtain from common passive sensors, but can be provided by an active device that produces a spectrum-type response. Such new active gas microsensor technology has been developed at Argonne National Laboratory. The technology couples an electrocatalytic ceramic-metallic (cermet) microsensor with a voltammetric measurement technique and advanced neural signal processing. It has been demonstrated to be flexible, rugged, and very economical to produce and deploy. Both narrow interest detectors and wide spectrum instruments have been developed around this technology. Much of this technology's strength lies in the active measurement technique employed. The technique involves applying voltammetry to a miniature electrocatalytic cell to produce unique chemical ''signatures'' from the analytes. These signatures are processed with neural pattern recognition algorithms to identify and quantify the components in the analyte. The neural signal processing allows for innovative sampling and analysis strategies to be employed with the microsensor. In most situations, the whole response signature from the voltammogram can be used to identify, classify, and quantify an analyte, without dissecting it into component parts. This allows an instrument to be calibrated once for a specific gas or mixture of gases by simple exposure to a multi-component standard rather than by a series of individual gases. The sampled unknown analytes can vary in composition or in concentration, the calibration, sensing, and processing methods of these active voltammetric microsensors can detect, recognize, and quantify different signatures and support subsequent analyses. The instrument can be trained to recognize and report ...
Date: December 11, 1998
Creator: Vogt, M. C.
Partner: UNT Libraries Government Documents Department

Depth profiling of oxidized a-C:D Layers on Be -- A comparison of {sup 4}He RBS and {sup 28}Si ERD analysis

Description: In applications dealing with the deposition of amorphous hydrogenated carbon layers or in the determination of the composition of deposited layers on the walls of nuclear fusion plasma experiments, the analysis of mixtures of light elements on heavy substrates is necessary. Depth profiling by means of RBS is often difficult due to the overlap of the backscattering intensities of different constituents from different depths. The erosion and reaction of deposited amorphous deuterated carbon (a-C:D) films with a Be substrate due to annealing in air poses an analytical challenge especially if simultaneously the exchange of hydrogen isotopes should be monitored. The analysis of the different recoiling atoms from collisions with heavy ions in Elastic Recoil Detection (ERD) can provide a tool which resolves all constituents in a single analysis. In the present study the composition of intermixed layers on Be containing H, D, Be, C and O has been analyzed using conventional {sup 4}He RBS at 2.2 MeV together with 2.5 MeV {sup 4}He ERD for hydrogen isotope analysis. At these energies, an overlap of signals from different constituents could be avoided in most cases. As alternative method heavy ion ERD using Si{sup 7+} ions extracted from a 5 MeV Tandem Van de Graff accelerator was investigated. At a scattering angle of 30{degree} Si ions could not be scattered into the detector and a solid state detector without protecting foil could be used. Even in the intermixed layers at terminal energies of 5 MeV the heavy constituents could be separated while signals from recoiling hydrogen and deuterium atoms could be resolved on top of the signal from the Be substrate. For the analysis of the RBS and ERD data the newly developed spectra simulation program SIMNRA has been used which includes a large data bank for scattering and nuclear reaction cross ...
Date: June 1, 1997
Creator: Roth, J.; Mayer, M.; Walsh, D. & Wampler, W.R.
Partner: UNT Libraries Government Documents Department

Inorganic, radioisotopic and organic analysis of 241-AP-101 tank waste

Description: Battelle received five samples from Hanford waste tank 241-AP-101, taken at five different depths within the tank. No visible solids or organic layer were observed in the individual samples. Individual sample densities were measured, then the five samples were mixed together to provide a single composite. The composite was homogenized and representative sub-samples taken for inorganic, radioisotopic, and organic analysis. All analyses were performed on triplicate sub-samples of the composite material. The sample composite did not contain visible solids or an organic layer. A subsample held at 10 C for seven days formed no visible solids. The characterization of the 241-AP-101 composite samples included: (1) Inductively-coupled plasma spectrometry for Ag, Al, Ba, Bi, Ca, Cd, Cr, Cu, Fe, K, La, Mg, Mn, Na, Nd, Ni, P, Pb, Pd, Ru, Rh, Si, Sr, Ti, U, Zn, and Zr (Note: Although not specified in the test plan, As, B, Be, Co, Li, Mo, Sb, Se, Sn, Tl, V, W, and Y were also measured and reported for information only) (2) Radioisotopic analyses for total alpha and total beta activities, {sup 3}H, {sup 14}C, {sup 60}Co, {sup 79}Se, {sup 90}Sr, {sup 99}Tc as pertechnetate, {sup 106}Ru/Rh, {sup 125}Sb, {sup 134}Cs, {sup 137}Cs, {sup 152}Eu, {sup 154}Eu, {sup 155}Eu, {sup 238}Pu, {sup 239+240}Pu, {sup 241}Am, {sup 242}Cm, and {sup 243+244}Cm; (3) Inductively-coupled plasma mass spectrometry for {sup 237}Np, {sup 239}Pu, {sup 240}Pu, {sup 99}Tc, {sup 126}Sn, {sup 129}I, {sup 231}Pa, {sup 233}U, {sup 234}U, {sup 235}U, {sup 236}U, {sup 238}U, {sup 241}AMU, {sup 242}AMU, {sup 243}AMU, As, B, Be, Ce, Co, Cs, Eu, I, Li, Mo, Pr, Rb, Sb, Se, Ta, Te, Th, Tl, V, and W; (4) total U by kinetic phosphorescence analysis; (5) Ion chromatography for Cl, F, NO{sub 2}, NO{sub 3}, PO{sub 4}, SO{sub 4}, acetate, formate, oxalate, and citrate; (6) ...
Date: June 28, 2000
Creator: Fiskum, SK; Bredt, PR; Campbell, JA; Greenwood, LR; Farmer, OT; Lumetta, GJ et al.
Partner: UNT Libraries Government Documents Department

Characterization and leaching study of sludge from Melton Valley Storage Tank W-25

Description: One of the greatest challenges facing the Department of Energy (DOE) is the remediation of the 100 million gallons of high-level and low-level radioactive waste in the underground storage tanks at its Hanford, Savannah River, Oak Ridge, Idaho, and Fernald sites. Bench-scale batch tests have been conducted with sludge from the Melton Valley Storage Tank (MVST) Facility at Oak Ridge National Laboratory (ORNL) to evaluate separation processes for use in a comprehensive sludge-processing flow sheet for concentrating the radionuclides and reducing the volumes of storage tanks wastes for final disposal. This report discusses the hot cell apparatus, the characterization of the sludge, and the results obtained from a variety of basic and acidic leaching tests of samples of sludge. Approximately 5 L of sludge/supernate from MVST W-25 was retrieved and transferred to a stainless steel tank for mixing and storage in a hot cell. Samples were centrifuged to separate the sludge liquid and the sludge solids. Air-dried samples of sludge were analyzed to determine the concentrations of radionuclides, other metals, and anions. Based upon the air-dried weight, about 41% of the centrifuged, wet sludge solids was water. The major alpha-, gamma-, and beta-emitting radionuclides in the centrifuged, wet sludge solids were {sup 137}Cs, {sup 60}Co, {sup 154}Eu, {sup 241}Am, {sup 244}Cm, {sup 90}Sr, Pu, U, and Th. The other major metals (in addition to the U and Th) and the anions were Na, Ca, Al, K, Mg, NO{sub 3}{sup {minus}}, CO{sub 3}{sup 2{minus}}, OH{sup {minus}}, and O{sub 2{minus}}. The organic carbon content was 3.0 {+-} 1.0%. The pH was 13.
Date: August 1, 1997
Creator: Collins, J.L.; Egan, B.Z.; Beahm, E.C.; Chase, C.W. & Anderson, K.K.
Partner: UNT Libraries Government Documents Department

Toxic substances from coal combustion -- Forms of occurrence analyses. Technical progress report, April 30--November 1, 1996

Description: The overall objective of this project is to provide analytical support for the Physical Sciences, Inc. (PSI) effort being performed under a DOE Contract. The Pittsburgh, Elkhorn/Hazard, and Illinois No. 6 program coals have been examined to determine the mode of occurrence of selected trace elements using scanning electron microscopy, microprobe analysis, and experimental leaching procedures. Preliminary microprobe data indicates that the arsenic content of pyrite grains in the Illinois No. 6 (0.0--0.027 ppm As) and Pittsburgh (0.0--0.080 ppm As) coals is similar. Pyrite grains observed in the Elkhorn/Hazard coal generally have arsenic concentrations (0.0--0.272 wt.% As) that are slightly higher than those of the Pittsburgh or Illinois No. 6 coals. One pyrite grain observed in the Elkhorn/Hazard coal contained much higher levels of arsenic (approximately 2 wt.% As). Preliminary microprobe analyses and data from leaching experiments indicate the association of arsenic with pyrite in the Pittsburgh and Illinois No. 6 coals. Leaching data for arsenic in the Elkhorn/Hazard coal, in contrast, is inconclusive and additional data are needed before a definite determination can be made.
Date: December 6, 1996
Creator: Crowley, S.S.; Palmer, C.A.; Kolker, A.; Finkelman, R.B.; Kolb, K.C. & Belkin, H.E.
Partner: UNT Libraries Government Documents Department