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Air' Igiararle-... ' EORGIA INSTITUTE OF TECHNOLOGY OFFICE OF CONTRACT ADMINISTRATION ORIGINAL PROJECT ADMINISTRATION DATA SHEET REVISION NO. roject No. 6-\-*5 3 -(.o -5 DATE: -oject Director: Schoo1/4,a4tr ponsor: A 1P.14 ' 61 ria• r /2 ; A_ 1 ype Agreement: e-^2th.A loo C— A- e, 1- gr M6/65-37 ward Period: From g- g To i4trlYmance) 0— i — 5 (Reports) ponsor Amount: r ip 5-.3 ) 1,) f Po Contracted through: ost Sharing: GTRI/111X- 1' 3 5 3 it 7, 2- .0 .,,L ..' -Lt4 i 1 1 itle: MEIMM ITIIR • ' Age, 4 AkA Air' IgiaraRLE-.../401111011111PIA ' i .:44.ao TIMPIEIP• J4kgra--..__..-1 , , IWO"Mallw . 1_6A Agaswaiftroira ct o.stt•Tn....tis: - ,••-• , • DMINISTRATIVE DATA OCA CONTACT ) Sponsor Technical Contact: L. 0 CUL • A. Al AL 4 I .60 11° g g / a,uro_tu-x 1/( SO S. ) Sponsor Admin./Contractual Contact: a-44 eports: See Deliverable Schedule Security Classification: efense Priority Rating: Mut, — 7 • ESTRICTIONS ee Attached _boc Supplemental Information Sheet for Additional Requirements ravel: Foreign travel must have prior approval - Contact OCA in each case. Domestic travel requires sponsor approval where total will exceed greater of $500 or 125% of approved proposal budget category. auipment: Title vests with /74 .01 A . (120 4,0 . aa „Lan. ■ A.•••.t..MA4. • I11- W4...se i f I• I A Mi 41.,- 0:41.1ENTS: A .(1,1 nAd 0/A-11.. J . Jo . ►,M41111 API A Grp .A, c' ,,,17 / i MOMMILUMMZUMIPMEK OPIES TO: RECEIVED A, Research Reports dministrative Coordinator Research Security Services EES Resear PulC4c Relit or.s ce research Property Management 130-4=11r-oar-dj-w■ake‘wre—€0CA) Project Fil 4c9FC97,(A 7counting Office Legal Services COCA) Other: )curement/FES Supply Services Library, Technical Reports GEORGIA INSTITUTE OF TECHNOLOGY OFFICE OF CONTRACT ADMINISTRATION SPONSORED PROJECT TERMINATION/CLOSEOUT SHEET Date 10/30/86 Project No. G - 33 - 603 School/KW Chem Includes Subproject No.(s) N/ A Project Director(s) Jim Gole GTRC / Sponsor U.S. Dept., of Energy, Morgantown, W.VA Title The Characterization of High-Temperature Vapor Phase Species and Vapor - solid Interactions of Import to Combustion and Gasification Processed in the Energy Technologies Effective Completion Date: 4/30/84 (Performance) (Reports) Grant/Contract Closeout Actions Remaining: El None Final Invoice or Final Fiscal Report Closing Documents n Final Report of Inventions n Govt. Property Inventory & Related Certificate Classified Material Certificate n Other ;ontinues Project No. Continued by Project No. :OPIES TO: 'roject Director Library iesearch Administrative Network GTRC lesearch Property Management Research Communications (2) kccounting Project File 'rocurement/GTRI Supply Services Other I. Newton tesearch Security Services A. Jones teports-CoOTZIrt , R. Embr y .egal Services 'ORM OCA 69.285 Progress August 14, 1981-November 14, 1981 Title of Contract: The Characterization of High Temperature Vapor Phase Species and Vapor-Solid Interactions of Import to Combustion and Gasification Processes in the Energy Techniques Place of Work: Georgia Institute of Technology Department of Chemistry Atlanta, Georgia 30332 Principal James L. Gole Investigator: Scope of Current Efforts: We have been concerned with the application of chemiluminescent and laser fluorescent techniques to the determination of bond energies and spectroscopic constants for the monohydroxides, monoxides, and monosulfides of sodium and potassium. We have investigated and are continuing to investigate non- equilibrium routes for the formation of these compounds and have carried out some kinetic parameterization. The sodium systems have been extended to the region in which sodium cluster, Mn (n›?), oxidation is now under study using optical techniques. This effort is soon to be supplemented with product analysis using a newly constructed mass spectrometric system. Efforts have been initiated toward the construction of a device for sodium surface oxidation. Our research effort has been divided into five areas: 1. The production and characterization of single and multiple collision KOH emission spectra. 2. The investigation of alkali-oxide production in hydroxide environ- ments. 3. The study of sodium atom and dimer oxidation to produce the metal oxides. 2 4. The initiation of sodium cluster, M n (n>3) ) oxidation studies. 5. The construction of a mass spectrometric system to allow simultaneous optical and mass spectrometric probing of the products of sodium oxidation. We summarize in more detail the current status of research efforts 1-4. Under tasks land 2: Both "single and multiple" collision chemiluminescent spectra have been observed and further characterized. Sample spectra are indicated in Figures (1) and (2). Note that the multiple collision diffusion flame spectrum onsets 0 0 at -3200A whereas the single collision spectrum onsets at -3900A. As the enclosed reprint indicates, this difference in onset is of fundamental impor- tance to the evaluation of the K-OH dissociation energy. One should also compare the significantly increased quality of the diffusion flame spectrum in Figure 2 with that depicted in Figure 4 of the enclosed reprint. As should be appa- rent from Figures 1 and 2, both the "single and multiple" collision KOH emis- sion spectra are characterized by significant structure'which we believe is attributable to emission to vibronic levels in the ground electronic state of potassium hydroxide, more specifically to primarily a progression in the K-OH stretch. There appears to be a reasonable if not one-to-one correlation 0 between the "multiple" and "single" collision spectra for X>3900A; however, there are some differences which may be attributable to (1) significant rota- tional relaxation in the multiple collision "diffusion flame" environment versus the high rotational excitation expected under single collision condi- tions or (2) the onset of rapid energy transfer and hence collisional depopu- lation of KOH excited state levels from which emission is observed under single collision conditions. The latter phenomena, collisional depopulation, should include collision induced dissociation of KOH molecules formed in the very weakly bound excited state from which emission is observed in the present study. 3 Unfortunately, the further investigation of the phenomena we have des- cribed here has been hampered by considerable experimental difficulties pri- marily associated with the difficulty entailed in handling 90+% hydrogen peroxide. Thus, a great deal of our recent research effort has entailed the replacement and reconstruction of both the single and multiple collision chemiluminescent systems. While this effort has slowed the continuation and completion of our work on KOH, it has led to significant discoveries concerning the formation of the alkali oxides in reactive hydroxide environments. In Figures (3) and (4) we depict chemiluminescent spectra which dominate emission observed in the Na-H 202 and K-H202 systems under conditions where we have partial decomposition of the hydrogen peroxide either through heating to temperatures in excess of 320K or reaction with the container walls, both of which create a hydroxide rich environment. The observed spectra are believed to result from emission from either MO or MO 2 excited states. Based on a comparison with spectra observed -in the Na-N 20 system, we favor formation of the latter MO 2 compounds. Under task 3: We have studied the single collision oxidation of equilibrium sodium (atom + 2% dimer) vapors with SO2 and N 20. The SO2 system yields a weak, if nonexistent, chemiluminescent emission. The weak nature of the emission is such as to preclude an unequivocal correlation with SO 2 oxidation. The sodium oxidation with N 20 is characterized by an intense red flame, the spectrum of which is shown in Figure 5. Although the structure associated with this emission is, as yet, unresolved, it must be associated with Na0*. It should 0 also be noted that the onset of the emission in Figure 5 is some 900A to the red of that in Figure 3. If both spectra resulted from Na0 or Na0 2 emission, it would be difficult to explain this difference in onset. Therefore, we suspect that the spectrum which results from sodium oxidation in a hydroxide environment does not result from the same emitter as that characterizing the sodium-N 20 system. Based upon the available literature which deals with the alkali monoxides (see enclosed reprint) and the bonding characteristics of the series of molecules A0 2 where A=F,C1,H,Na, and K, we tentatively correlate the emission, associated with sodium and potassium oxidation in a hydroxide environment, with Na0 2 and K02 . Under task 4: We have constructed an apparatus for the study of sodium cluster oxidation. The ultimate goal for this apparatus will be the study of sodium cluster oxidation with SO2 viz. Nax + SO 2 products; however, the initial experi- ments now being conducted involve sodium cluster oxidation with halogens. These experiments not only allow us to test the metal cluster oxidation system but also facilitate the characterization of a potentially important factor in .energy generating systems. It has currently been suggested that chlorine interacts with the alkali impurities in a combustion stream, resulting in the formation of alkali chloride complexes which then repartition with O,S,H,C,A1, or Si ash particulates. Thus, the influence of chlorine on the formation of alkali clusters and the subsequent reaction of these clusters with SO 2 must be evaluated in the intermediate region between the gas and surface phases. A schematic of the cluster oxidation device is shown in Figure (6) and a sample of the chemiluminescent spectra observed thusfar is shown in Figure (7). This cluster oxidation device will soon be coupled with our newly acquired mass spectrometric capability so as to provide simultaneous optical and mass spec- trometric probing of the system. 5 Associated Periferal Devices and Preliminary Studies We should note that the mass spectrometric system which we will use in conjunction with our optical studies is in the final stages of construction.
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