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CRADA Final Report For CRADA NO. CR-12-006 [Operation and Testing of an SO{sub 2}-depolarized Electrolyzer (SDE) for the Purpose of Hydrogen and Sulfuric Acid Production]

Description: Over the past several years, Savannah River National Laboratory (SRNL) has led a team of collaborators under the Department of Energy’s (DOE) nuclear hydrogen production program to develop the Hybrid Sulfur (HyS) Process. HyS is a 2-step water-splitting process consisting of high temperature decomposition of sulfuric acid to generate SO{sub 2}, followed by the electrolysis of aqueous SO{sub 2} to generate hydrogen and sulfuric acid. The latter is fed back into the high temperature reactor. SRNL designed and built an SO{sub 2}-depolarized electrolyzer (SDE) and a test facility. Over 40 SDE’s were tested using different catalysts, membranes and other components. SRNL demonstrated that an SDE could be operated continuously for approximately 200 hours under certain conditions without buildup of sulfur at the SDE’s cathode, thus solving a key technical problem with SDE technology. Air Products and Chemicals, Inc. (APCI) is a major supplier of hydrogen production systems, and they have proprietary technology that could benefit from the SDE developed by SRNS, or some improved version thereof. However, to demonstrate that SRNL’s SDE is a truly viable approach to the electrolyzer design, continuous operation for far greater periods of time than 200 hours must be demonstrated, and the electrolyzer must be scaled up to greater hydrogen production capacities. SRNL and Air Products entered into a Cooperative Research and Development Agreement with the objective of demonstrating the effectiveness of the SDE for hydrogen and sulfuric acid production and to demonstrate long-term continuous operation so as to dramatically increase the confidence in the SDE design for commercial operation. SRNL prepared a detailed technical report documenting previous SDE development, including the current SDE design and operating conditions that led to the 200-hour sulfurfree testing. SRNL refurbished its single cell SDE test facility and qualified the equipment for continuous operation. A new membrane electrode assembly ...
Date: February 24, 2014
Creator: Summers, W. A.; Colon-Mercado, H. R.; Steimke, J. L. & Zahn, Steffen
Partner: UNT Libraries Government Documents Department

Report of the Selby Smelter Commission

Description: From Preface: "This bulletin presents the report of the commission and the papers, prepared by the various experts, which give the results of investigations undertaken by the commission and form the basis of its findings."
Date: 1915
Creator: Holmes, J. A.; Franklin, Edward C.; Gould, Ralph A. & Gould, Ralph A.
Partner: UNT Libraries Government Documents Department

SOOT-CATALYZED OXIDATION OF SULFUR DIOXIDE

Description: Experimental results are reviewed which demonstrate that combustion-generated soot particles can oxidize SO{sub 2} in both the absence ('dry' mechanism) and the presence ('wet' mechanism) of liquid water. The 'wet' mechanism is much more efficient than the 'dry' one, and is applicable to situations where the aerosol particles are covered with a liquid water layer. Calculations are presented which suggest that the soot-catalyzed oxidation of SO{sub 2} can be the dominant mechanism under realistic atmospheric conditions.
Date: May 1, 1978
Creator: Chang, S.G. & Novakov, T.
Partner: UNT Libraries Government Documents Department

Removal of H2S and SO2 by CaCO3-Based Sorbents at High Pressure

Description: The theoretical and experimental investigation of the mechanism of SO2 and H2S removal by CaCO3 -based sorbents (limestones and dolomites) in pressurized uidized-bed coal combustors (PFBC) and high pressure gasi#12;ers, respectively, is the main objective of this study. It is planned to carry out reactivity evolution experiments under simulated high pressure conditions or in high pressure thermogravimetric and, if needed, uidized- bed reactor (high pressure) arrangements. The pore structure of fresh, heat-treated, and half-calcined solids (dolomites) will be analyzed using a variety of methods. Our work will focus on limestones and dolomites whose reaction with SO2 or H2S under atmospheric conditions has been studied by us or other research groups in past studies. Several theoret- ical tools will be employed to analyze the obtained experimental data including a variable di#11;usivity shrinking-core model and models for di#11;usion, reaction, and structure evolution in chemically reacting porous solids. During the six months of this reporting period, work was primarily done on the study of the behavior of the sul#12;dation of limestones under sequential calcination conditions in the presence of small amounts of oxygen and the development of a stochastic simulation code for determining the extent of pore volume trapping (formation of inaccessible pore space) in gas-solid reactions accompanied by pore volume reduction such as the sulfation and sul#12;dation of calcined limestones and dolomites. The incentive for carrying out sul#12;dation experiments in the presence of oxygen was provided by the observation that some sul#12;dation experiments that were conducted as oxygen was accidentally leaking into the feed mixture of the reactor showed completely di#11;erent behavior from that obtained in the absence of oxygen. Experiments were carried out in the thermogravimetric analysis system that we developed for studying gas-solid reactions at atmospheric or subambient pressures. The two CaCO3 solids (Greer limestone and Iceland spar) that we ...
Date: February 1, 1998
Creator: Sotirchos, Stratis V.
Partner: UNT Libraries Government Documents Department

High SO2 Removal Efficiency Testing

Description: This document provides a discussion of the technical progress on DOE/PETC project number DE-AC22-92PC91338, "High Efficiency SO2 Removal Testing", for the time period 1 January through 31 March 1997. The project involves testing at six full-scale utility flue gas desulfurization (FGD) systems, to evaluate low capital cost upgrades that may allow these systems to achieve up to 98% SO2 removal efficiency. The upgrades being evaluated mostly involve using performance additives in the FGD systems. The "base" project involved testing at the Tampa Electric Company�s Big Bend Station. All five potential options to the base program have been exercised by DOE, involving testing at Hoosier Energy�s Merom Station (Option I), Southwestern Electric Power Company�s Pirkey Station (Option II), PSI Energy�s Gibson Station (Option III), Duquesne Light�s Elrama Station (Option IV), and New York State Electric and Gas Corporation�s (NYSEG) Kintigh Station (Option V). The originally planned testing has been completed for all six sites. However, additional testing is planned at the Big Bend Station. The remainder of this document is divided into four sections. Section 2, Project Summary, provides a brief overview of the status of technical efforts on this project. Section 3, Results, summarizes the outcome from technical efforts during the quarter, or results from prior quarters that have not been previously reported. In Section 4, Plans for the Next Reporting Period, an overview is provided of the technical efforts that are anticipated for the second quarter of calendar year 1997. Section 5 contains a brief acknowledgement.
Date: April 23, 1997
Creator: Blythe, Gary
Partner: UNT Libraries Government Documents Department

Theoretical studies of collisional relaxation of highly excited SO{sub 2} in an Ar bath

Description: This paper describes molecular dynamics studies of collisional relaxation of highly excited SO{sub 2} in an Ar bath. Most of the calculations use a newly developed global ab initio potential surface for SO{sub 2} that correctly describes the superoxide (SOO) and ring isomers of SO{sub 2} that occur as secondary minima on the ground state potential surface at high energies (about 75% of the dissociation energy) above the C{sub 2v} minimum. Rate constants for the S + O{sub 2} and O + SO reactions are calculated to test this surface, and to examine the importance of electronically excited states in the O + SO recombination. The Ar + SO{sub 2} collisions are described by summing the ab initio potential with empirical intermolecular potentials. The resulting average vibrational energy transfer <{Delta}E> per collision is in good agreement with direct measurements (done at energies where the secondary minima are not populated) at 1000K, but the agreement is poorer at 300K. The agreement is significantly better than was obtained in a previous theoretical study, and our results indicate that the use of improved intramolecular and intermolecular potentials is crucial to obtaining the better results. The energy dependence of <{Delta}E> is found to be much stronger at energies where the secondary minima on the potential surface are accessible, however much of this effect is reproduced using a potential that has the same dissociation energy but not the secondary minima.
Date: December 31, 1995
Creator: Lendvay, G.; Schatz, G.C. & Harding, L.B.
Partner: UNT Libraries Government Documents Department

High SO2 Removal Efficiency Testing

Description: This document provides a discussion of the technical progress on DOE/PETC project number DE-AC22-92PC91338, "High Efficiency SO2 Removal Testing", for the time period 1 April through 30 June 1997. The project involves testing at six full-scale utility flue gas desulfurization (FGD) systems to evaluate low capital cost upgrades that may allow these systems to achieve up to 98% SO2 removal efficiency. The upgrades being evaluated mostly involve using performance additives in the FGD systems. The "base" project involved testing at the Tampa Electric Company�s Big Bend Station. All five potential options to the base program have been exercised by DOE, involving testing at Hoosier Energy�s Merom Station (Option I), Southwestern Electric Power Company�s Pirkey Station (Option II), PSI Energy�s Gibson Station (Option III), Duquesne Light�s Elrama Station (Option IV), and New York State Electric and Gas Corporation�s Kintigh Station (Option V). The originally planned testing has been completed for all six sites. However, additional testing is being conducted at the Big Bend Station. The remainder of this document is divided into four sections. Section 2, Project Summary, provides a brief overview of the status of technical efforts on this project. Section 3, Results, summarizes the outcome from technical efforts during the quarter, or results from prior quarters that have not been previously reported. In Section 4, Plans for the Next Reporting Period, an overview is provided of the technical efforts that are anticipated for the third quarter of calendar year 1997. Section 5 contains a brief acknowledgment.
Date: July 29, 1997
Creator: Blythe, Gary
Partner: UNT Libraries Government Documents Department

High SO2 Removal Efficiency Testing

Description: This document provides a discussion of the technical progress on DOE/PETC project number DE-AC22-92PC91338, "High Efficiency SO Removal Testing," for 2 the time period 1 October through 31 December 1996. The project involves testing at six full-scale utility flue gas desulfurization (FGD) systems, to evaluate low capital cost upgrades that may allow these systems to achieve up to 98% SO removal efficiency. The upgrades being 2 evaluated mostly involve using performance additives in the FGD systems. The "base" project involved testing at the Tampa Electric Company�s Big Bend Station. All five potential options to the base program have been exercised by DOE, involving testing at Hoosier Energy�s Merom Station (Option I), Southwestern Electric Power Company�s Pirkey Station (Option II), PSI Energy�s Gibson Station (Option III), Duquesne Light�s Elrama Station (Option IV), and New York State Electric and Gas Corporation�s Kintigh Station (Option V). The originally planned testing has been completed for all six sites. However, additional testing has been planned at the Big Bend Station, and that testing commenced during the current quarter. The remainder of this document is divided into four sections. Section 2, Project Summary, provides a brief overview of the status of technical efforts on this project. Section 3, Results, summarizes the outcome from technical efforts during the quarter, or results from prior quarters that have not been previously reported. In Section 4, Plans for the Next Reporting Period, an overview is provided of the technical efforts that are anticipated for the first quarter of calendar year 1996. Section 5 contains a brief acknowledgment.
Date: February 12, 1997
Creator: Blythe, Gary
Partner: UNT Libraries Government Documents Department

Determination of the Optimum Concentration of Sulfur Dioxide to be Used in Sweet Potato Dehydration

Description: The object of this paper is to determine the optimum concentration of sulfur dioxide to be used in the commercial dehydration of the sweet potato by this process. Attention has been given to two aspects of the problem, (1) the effect of sulfur dioxide upon the extraction of water from the sweet potato by mechanical means, and (2) the effect of sulfur dioxide upon the stability of the carotene in the sweet potato over a period of several months.
Date: 1941
Creator: Kearby, Howard Raymond
Partner: UNT Libraries

DESIGN AND PERFORMANCE OBJECTIVES OF THE SINGLE CELL TEST SYSTEM FOR SO2 DEPOLARIZED ELECTROLYZER DEVELOPMENT

Description: The single cell test system development for the SRNL sulfur dioxide-depolarized electrolyzer has been completed. Operating experience and improved operating procedures were developed during test operations in FY06 and the first quarter of FY07. Eight different cell configurations, using various MEA designs, have been tested. The single cell test electrolyzer has been modified to overcome difficulties experienced during testing, including modifications to the inlet connection to eliminate minute acid leaks that caused short circuits. The test facility was modified by adding a water bath for cell heating, thus permitting operation over a wider range of flowrates and cell temperatures. Modifications were also identified to permit continuous water flushing of the cathode to remove sulfur, thus extending operating time between required shutdowns. This is also expected to permit a means of independently measuring the rate of sulfur formation, and the corresponding SO{sub 2} flux through the membrane. This report contains a discussion of the design issues being addressed by the single cell test program, a test matrix being conducted to address these issues, and a summary of the performance objectives for the single cell test system. The current primary objective of single cell test system is to characterize and qualify electrolyzer configurations for the following 100-hour longevity tests. Although the single cell test system development is considered complete, SRNL will continue to utilize the test facility and the single cell electrolyzer to measure the operability and performance of various cell design configurations, including new MEA's produced by the component development tasks.
Date: January 15, 2007
Creator: Steimke, J
Partner: UNT Libraries Government Documents Department

Design and Evaluation of Ionic Liquids as Novel CO2 Absorbents

Description: Progress from the fourth quarter 2005 activity on the project ''Design and Evaluation of Ionic Liquids as Novel CO{sub 2} Absorbents'' is provided. Major activities in three areas are reported: compound synthesis, property measurement and molecular modeling. Last quarter we reported the first ever experimental measurement of SO{sub 2} solubility in an ionic liquid. We showed that SO{sub 2} was very soluble in the ionic liquid 1-hexyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide ([hmim][Tf{sub 2}N]). This quarter, we have measured SO{sub 2} solubility in two more ionic liquids: 1-hexyl-3-methylpyridinium bis(trifluoromethanesulfonyl)imide ([hmpy][Tf{sub 2}N]) and 1-hexyl-3-methylimidazolium lactate ([hmim][lactate]). As with [hmim][Tf{sub 2}N], we find very high solubility of SO{sub 2} in these ionic liquids, but the lactate compounds shows the highest affinity for SO{sub 2} at low pressure. CO{sub 2} solubility was measured in three new compounds: [boronium][Tf{sub 2}N], 1-hexyl-3-methylimidazolium acesulfumate ([hmim][ace]), and 1-hexyl-3-methylimidazolium saccharinate ([hmim][sac]). We find relatively poor solubility of CO{sub 2} in the latter two compounds, and solubility comparable to [hmim][Tf{sub 2}N] in the boronium compound. We also synthesized four new ionic liquids this quarter and continued refinement of our molecular simulation technique for measuring gas solubility.
Date: January 12, 2006
Creator: Maginn, Edward J.
Partner: UNT Libraries Government Documents Department

Test Plan for Characterization Testing of SO2-depolarized Electrolyzer Cell Designs

Description: SRNL received funding in FY 2005 to test the Hybrid Sulfur (HyS) Process for generating hydrogen. This technology employs an electrolyzer that uses a sulfur dioxide depolarized anode to greatly reduce the electrical energy requirement. The required current is the same as for conventional electrolysis of water, but the required cell voltage is reduced. The electrolyzer is a key part of HyS technology. Completing the material loop for HyS requires a high temperature decomposition of sulfuric acid to regenerate the sulfur dioxide gas needed for the anode reaction. Oxygen is also produced and could be sold. The decomposition of sulfuric acid is being studied by others in a separately funded task. It is not included in this SRNL task.
Date: February 15, 2006
Creator: Steimke, J. L.
Partner: UNT Libraries Government Documents Department

INFRARED and PHOTOELECTRON SPECTROSCOPIC STUDY OF S02 OXIDATION ON SOOT PARTICLES

Description: Results obtained by means of x-ray photoelectron spectroscopy and internal reflection infrared spectroscopy demonstrate the feasibility of heterogeneous oxidation of sulfur dioxide on soot particles in air. Sulfuric acid formed in this process can be neutralized on basic surface sites of soot particles, resulting in the formation of carbonium and/or oxonium sulfate. Hydrolysis of these salts into cyclic hemiacetals and sulfuric acid is expected.
Date: December 1, 1975
Creator: Chang, S.G. & Novakov, T.
Partner: UNT Libraries Government Documents Department

Fundamentals of Mercury Oxidation in Flue Gas

Description: The objective of this project is to understand the importance of and the contribution of gas-phase and solid-phase coal constituents in the mercury oxidation reactions. The project involves both experimental and modeling efforts. The team is comprised of the University of Utah, Reaction Engineering International, and the University of Connecticut. The objective is to determine the experimental parameters of importance in the homogeneous and heterogeneous oxidation reactions; validate models; and, improve existing models. Parameters to be studied include HCl, NO{sub x}, and SO{sub 2} concentrations, ash constituents, and temperature. This report summarizes Year 3 results for the experimental and modeling tasks. Experiments have been completed on the effects of chlorine. However, the experiments with sulfur dioxide and NO, in the presence of water, suggest that the wet-chemistry analysis system, namely the impingers, is possibly giving erroneous results. Future work will investigate this further and determine the role of reactions in the impingers on the oxidation results. The solid-phase experiments have not been completed and it is anticipated that only preliminary work will be accomplished during this study.
Date: July 31, 2006
Creator: Lighty, JoAnn S.; Silcox, Geoffrey; Fry, Andrew; Helble, Joseph & Krishnakumar, Balaji
Partner: UNT Libraries Government Documents Department

Designing a scrubber for maintenance

Description: Under Round 4 of the U.S. Department of Energy`s (DOE) Clean Coal Technology program, New York State Electric & Gas Corporation (NYSEG), in partnership with Saarberg-Holter-Umwelttechnik (SHU), Consolidation Coal Company and Stebbins Engineering and Manufacturing Company, has retrofitted a formic acid enhanced forced oxidation wet limestone scrubber on Units I and 2 at the Milliken Steam Electric Station. Units I and 2 are 1950s vintage Combustion Engineering tangentially fired pulverized coal units, which are rated at nominal 150 MW each and operate in balanced draft mode. The Flue Gas Desulfurization (FGD) system for Unit 2 was placed into operation in January 1995 and the Unit I system in June 1995. The project incorporates several unique aspects: low pH operation; a ceramic tile-lined cocurrent/countercurrent, split module absorber; a wet stack supported on the roof of the FGD building; and closed loop, zero liquid discharge operation that produces commercial grade gypsum and calcium chloride brine. The project objectives include 98% SO{sub 2} removal efficiency while burning high sulfur coal, the production of marketable byproducts to minimize solid waste disposal, zero wastewater discharge, space-saving design, and minimization of maintenance requirements of a wet scrubber. The paper provides a brief overview of the project scrubber design relating to maintenance considerations. A discussion of the early results of the maintenance history is also provided. Repair techniques that have been developed and tested for ceramic tile lined modules are included. 1 fig.
Date: December 1, 1996
Creator: Mahlmeister, M.E.; Baron, E.S. & Watts, J.
Partner: UNT Libraries Government Documents Department

A Summary of Experiments in Converting Copper Oxide Process Regenerator Off-Gases to Elemental Sulfur, CRADA 97-F006, Final Report

Description: Sorbent Technologies Corporation (Sorbtech) of Twinsburg, Ohio has developed a new technology for converting SO{sub 2}-rich gas streams directly to elemental sulfur. Key to the technology is a special catalyst that promotes the reaction of SO{sub 2} with reformed natural gas. The technology evolved from earlier flue-gas desulfurization (FGD) work that Sorbtech engineers performed in the late 1980's. In 1995, with U.S. Department of Energy (DOE) support, Sorbtech designed and constructed a larger, skid-mounted pilot-test unit suitable for demonstrating the new technology in field tests. This Report summarizes months of preparation work and eight days of testing that were performed at FETC'S facilities during late September and early October, 1997. On the basis of the results of this phase of the project, the following conclusions were made: (1) The chemistry of the new technology was well proven and demonstrated at FETC. The overall S0{sub 2}-to-elemental sulfur yields were typically in the range of 93 to 98 percent. (The project goal was 95 percent, so the goal was exceeded). (2) Sulfur selectivity values, indicating the tendency of S0{sub 2} to be converted to elemental sulfur in preference to H{sub 2}S or COS, were typically in the range of 98 to 100 percent. (3) Bright yellow sulfur of high quality was produced at FETC. (4) The FETC regenerator exhaust gas presented no processing difficulties. Swings in the level of methane in the exhaust gas were handled with relative ease. (5) With the exception of the water condenser, all system components performed well. (6) Condensing of the sulfur after its production was a serious problem at FETC. Solid sulfur deposits built up in the process-gas lines at several locations in the system. Clogging of the lines necessitated terminating runs typically after 2 to 4 hours of operation. Clogging problems were most severe in ...
Date: January 22, 1999
Creator: Cianciolo, Brian C.; Oehlberg, Richard J. & Nelson, Sidney G.
Partner: UNT Libraries Government Documents Department

Remote sensing of the atmosphere by resonance Raman LIDAR

Description: When in resonance, Raman scattering exhibits strong enhancement ranging from four to six orders of magnitude. This physical phenomenon has been applied to remote sensing of the Earth`s atmosphere. With a 16 inch Cassegrain telescope and spectrometer/ CCD-detector system, 70-150 ppm-m of SO{sub 2} in the atmosphere has been detected at a distance of 0.5 kilometer. This system can be used to detect/monitor chemical effluence in the atmosphere by their unique Raman fingerprints. Experimental result together with detailed resonance Raman and atmospheric laser propagation effects will be discussed.
Date: December 1, 1994
Creator: Sedlacek, A.J.; Harder, D.; Leung, K.P.; Zuhoski, P.B. Jr.; Burr, D. & Chen, C.L.
Partner: UNT Libraries Government Documents Department

Assessing historical global sulfur emission patterns for the period 1850--1990

Description: Anthropogenic sulfur dioxide emissions from energy-producing and metal production activities have become an important factor in better understanding the relationship between humans and the environment. Concerns about (1) acid rain effects on the environment and (2) anthropogenic aerosols affecting possible global change have prompted interest in the transformation and fate of sulfur in the environment. One step in assessing the importance of sulfur emissions is the development of a reliable regional emission inventory of sulfur as a function of time. The objective of this research effort was to create a homogeneous database for historical sulfur emission estimates for the world. The time from 1850--1990 was selected to include the period of industrialization form the time the main production of fuels and minerals began until the most recent year for which complete production data exist. This research effort attempts to correct some of the deficiencies associated with previous global sulfur emission estimates by (1) identifying those production activities that resulted in sulfur emissions by country and (2) calculating historical emission trends by country across years. An important component of this study was the comparison of the sulfur emission results with those of previous studies.
Date: July 19, 1996
Creator: Lefohn, A.S.; Husar, J.D.; Husar, R.B. & Brimblecombe, P.
Partner: UNT Libraries Government Documents Department