SEPA United States Environmental Protection Agency Environmental Sciences Researe Laboratory "/ _ -, Research Triangle Park NC 27711 /1v ! Research and Development EPA-600/S3-81-040 Dec. 1981 Project Summary Modeling of Oxidation in Smog David F. Miller Smog chamber experiments were conducted to investigate the kinetics of the free radical reactions of SOz in smog and the transformation of SO2 to sulfate under simulated urban and rural atmospheric conditions. Rate constants were derived for three re- actions: SO2 + HO + M - SULFATE (60); SOz + HO2 - SULFATE (61); and SO2 + CH3O2 - SULFATE (64); where keo = 1600, k6i < 0.2, and k64 < 0.8 ppm'1 min 1, respectively. Oxidation of SO2 by the unstable intermediate HO led exclusively to particulate sulfate. However, even under favorable NOX conditions, particulate nitrate was not a product. Hydrocarbon mixtures typical of urban environments promoted SO2 oxidation faster than hydrocarbons selected to represent rural conditions. Maximum SO2 oxida- tion rates occurred during periods of peak NO2 formation. Oxidation rates of SOz in aged smog were 25 to 35% of the maximum rates. Model calculations indicated that the SOz + HO + M - SULFATE reaction dominated sulfate production from SOz in polluted air. The model also indicated that SOz oxidation is heavily influenced by solar radiation intensity and pollutant conditions. For clear-sky and a variety of HC-NOX conditions, maximum SO2 conversion rates ranged from 3.7 to 7.4%/h. Models used to simulate free radical reactions in power plant plumes showed that SOz oxidation is strongly dependent on plume dispersion rates, as well as on the same parameters governing SOz oxidation in ambient air. Although exceptions do occur for certain HC-NO* conditions, SOz oxida- tion rates in plumes are generally bound by the ambient rates. This Project Summary was devel- oped by EPA's EnviornmentalSciences Research Laboratory, Research Tri- angle Park, NC, to announce key findings of the research project that is fully documented in a separate report of the same title (see Project Report ordering information at back). Introduction The widespread distribution of sulfate aerosols in the atmosphere and their associated effects on visibility and precipitation pH (acid rain) are serious environmental concerns in the United States. The Environmental Sciences Research Laboratory of the U.S. Envi- ronmental Protection Agency is working to formulate strategies for the effective control of sulfates. One step toward achieving such control is the develop- ment of models to predict regional production of sulfate by SOz sources. The study summarized here was con- ducted by Battelle Columbus Laborato- ries to broaden the information base available on SOz reactions and trans- formations and to provide the Environ- mental Sciences Research Laboratory with the predictive models necessary for sulfate control. Oxidation of SOz in the atmosphere is considered the primary source of sulfate particulates. The chemical and micro- physical processes involved in the gas- to-particulate transformations of oxida- tion, however, are highly complex. ------- Despite numerous research efforts to define these processes more clearly, many essential details pertaining to reaction rates and mechanisms are missing. To date, kinetic and mechanistic studies of the elementary gas phase reactions of SO2 in air have yielded only that all known reactions involving electronically excited states of S02 are insignificantly slow in the troposphere and that HO, H02, and R02 are the only tropospheric species capable of oxidizing S02 at substantial rates. Numerous studies have presented evidence that submicron-radii sulfates are predominantly (NH4)xH2-xSO« with associated water. However, although microphysical aspects of H2S04 particle formation are well understood, much uncertainty surrounds defining new particle nucleation. Some investigators have concluded that SO2 oxidation in the gas phase is the rate limiting step for the formulation and growth of secondary H2S04 particles in the atmosphere. One objective of this study was to examine these rate limiting reactions. Finally, based on the new findings and on additional smog chamber data obtained with rural and urban hydro- carbon systems, a photochemical smog model was applied to simulate gas phase S02 oxidation rates for various atmospheric conditions. Procedure Experiments to investigate the kinet- ics of the free radical reactions of SOz in smog and to obtain data on SO2 transformation to sulfate under various atmospheric conditions were conducted in Battelle's 17.4 m3 smog chamber. Rate constants were derived for the following reactions: S02 + HO + M — SULFATE (60); S02 + HO2 - SULFATE (61); and SO2 + CH3O2 - SULFATE (64). Pseudo second-order rate constants (ppnrf1 min'1) were keo=1600, k6i<0.2, and k64 < 0.8. The values for kei and k64 were only upper limit estimates; the rates pertained to the overall conversion of SOz to paniculate sulfate. Although the mechanisms of S02 conversion were not investigated, some work was done to determine if NO and/or N02 form stable aerosol products with the intermediates created after HO addition to SO2. Methods for Kinetic Studies The smog chamber facility has a surfacervolume ratio of 0.8 m"1; the surface is polished aluminum (—80%) and FEP Teflon™ (—20%). Irradiation was provided by a bank of 95 fluorescent blacklamps and 15 fluorescent sun- lamps. Combined intensity of the lamps yielded a N02 photodissociation rate of approximately 0.14 min"1. Background air for the chamber was passed through a purification system for dehumidification and filtering. S02 and N02 concentrations were usually below the detection levels of 1 ppb and 2 ppb, respectively. Background NO concen- trations ranged from 1 to 2 ppb. Background total hydrocarbon ranged between 1.9 and 2.5 ppmC (of which most was CH4). Gas chromatographic analyses of background air showed no detectable olefins or aromatics in the C2-C9 range when nonmethane hydro- carbon was 0.1 to 0.3 ppmC. When relatively small concentrations of nitrous acid (a source of HO radicals and NOX) were added to the background air under high molecular weight hydro- carbon contamination, irradiation re- sulted in peak 03 concentrations in the 8 to 12 ppb range. The reactivity of this amount of hydrocarbon contamination in terms of 03 production corresponds to the reactivity of about 4 to 6 ppm CO. Thus, intentional addition of 4.5 ppmC hydro- carbons and/or large quantities of CH4 and CO clearly overwhelmed any effects due to background HC contaminants. In addition, intentional introduction of nitrous acid into the air for most of the experiments was thought to overcome any spurious surface contaminant effects which might have led to the generation of free radicals at the outset of irradiation. Gas phase analyses included mea- surement of PAN, Ci-Ca hydrocarbons, CO, 03, H2O2, HNO2, N02, NOX, NO and SO2. Initial measurements of SO2 were taken with a Meloy 285 flame photo- meter. Upon irradiation, the instrument was used to monitor sulfate aerosol. The photometer was intermittently operated in the total sulfur mode (S02 plus sulfate) to check on the S02 concentration. Gas calibrations were performed routinely. The chemiluminescense analyzer used to monitor NO, HNO2, and N02 was spanned before almost every experiment. In situ 03 titrations were conducted in the chamber to check on the span of the 03 analyzer and the efficiency of the NOX converters. After an experiment (lamps off), excess NO was injected into the chamber to more than titrate the remaining 03. Condensed phase analysis conce trated on the measurement of sulf< aerosol. The primary method for mo toring sulfate was based on continue sampling by a flame photometric detc tor (FPD). Checks were made on tl method by taking simultaneous lar volume collections on quartz filters a comparing the results. Using tl tremendous difference in diffusiv between SO2 and H2S04 aerosols, diffusion-denuder tube was designed remove virtually all of the S02 in the i sample entering the FPD, while allowi: most of the paniculate sulfur to pass the detector. Optimization betwe< maximum S02 removal and minimu H2SO4 loss was determined expe mentally by generating independent known concentrations of S02 a: H2SO4 aerosol in the smog chambc The optimization work resulted in sample flow of 200 ml/min through 35 cm lead acetate diffusion tube, wi >99.5% removal of S02 and 35% loss H2S04 aerosol. Kinetic Data The objective of the first portion of thi project was to investigate the kinetic (and mechanisms where feasible) c S02 oxidation by free radicals; nameh HO, H02, and CH302. The approac taken to study these reactions was t generate a variety of distribution: between HO, H02, and CH3O2 in a smo chamber containing S02. This wor began with a series of smog chambe experiments using an inorganic smo system (HNO2/NOX/CO/SO2). By se lecting the initial concentrations c system components, it was possible t affect a range of HO:HO2 ratios ani thereby observe the relative rates of SO oxidation attributable to the respectivi radicals. To obtain estimates of the free radica concentrations, and hence to calculati absolute rate constants, the experi mental data were fitted with a chemica kinetics model. Throughout the study the S02 oxidation rates related to the subject radicals were determined solely in terms of sulfate aerosol product. Am sulfur products remaining in the gas phase were not determined. As such the rate constants obtained represen rate limiting kinetics for conversion o SO2 to sulfate and not the upper limi rates for S02 removal. In general, gooc material balances were observed be tween gas-phase and condensed-phase sulfur, but once the reactions began U ------- was not certain that the gas-phase sulfur was exclusively SO2. In the inorganic smog system, NO, (i.e., HNOZ, NO, and N02) governed the free radical concentrations because their reaction rates with the radicals were typically orders of magnitude larger than those of the corresponding reactions with S02. Thus, before attempting to interpret experimental data pertaining to S02 oxidation, the NOx chemistry as it occurred in the smog chamber had to be investigated. Substantial concentrations of HN02 were used as a radical source in many of the experiments. Three initial experiments were con- ducted to determine the reaction rates for HNOz under experimental conditions and to account for the large NO* losses observed in most experiments. The first experiment showed that the NO con- centration was largely a function of HNOz's photolysis rate and the HO + NO recombination rate. Material balances between the model and experimental data were reasonably good, although the model slightly underestimated NO, losses. The next experiment, conducted to investigate further the smog chamber reactions involving HNOz and the formation of HN03, investigated two routes for HNOs formation in the gas phase: HN02 + 03 — HNOa+Ozand N205 + H2O — 2HNOs. The results suggested that neither reaction produced appre- ciable amounts. The experiments also provided no conclusive data on the HNOa photolysis rate in the smog chamber. However the choice of k=0.28 x I0~1min~1 seemed to fit these and other experimental data as well as alternative values. The last of these three experiments attempted to measure the reactions involving N20s formation. Thermal decomposition of N2O5 apparently limited its concentrations in the tropo- sphere. The slow rate found for homo- genous conversion to HNO3 coupled to the strong temperature dependence for N20S decomposition suggested that Nz05 persists for substantial periods in the colder regions of the lower atmos- phere and that clouds and perhaps moist aerosols may be the dominant sink for N205. A series of experiments was also conducted in the inorganic smog system to study the conversion of SO2 to sulfate via hydroxyl radicals. SOz was added to air mixtures of HN02 and NO, in the chamber. Sulfate aerosol formation was observed immediately after the lamps were turned on, and the rate of sulfate formation was generally found to maximize early in the irradiation period and then gradually diminish. The eight experiments were simulated by kinetic modeling in order to estimate the HO profiles and assess the overall conversion rate for SO2, as initiated by HO radicals. Some investigators had suggested that NO, could have various roles in the transformation process and even be- come incorporated in the condensed phase as the reactions reached comple- tion. To investigate these hypotheses, various amounts of NO or NO2 were added to some of the mixtures, in addition to the amounts produced while charging HN02 to the chamber. The model gave satisfactory fits to the experimental data, with only one experiment in the series excepted. The model tended to underestimate NO2 conversion and sulfate aerosol concen- trations, particularly during the latter half of the experimental periods. The discrepancies rarely exceeded 20% of the experimental values, however. The data supported a rate constant of 1.6 x 103 ppm min~1 for the conversion of S02 to sulfate aerosol, as initiated by the HO radical. The last series of experiments in the inorganic smog system was conducted to determine the kinetics of SO2 oxidation by hydroperoxy radicals. To investigate the reactions in the smog chamber, relatively large concentrations of CO were added to mixtures of NO,/HN02/S02. CO was found to give a negative interference to the analyses of SO2 and sulfate aerosols with the FPD. This interference severely limited the range of useful CO concentration. Based on the data from this group of experiments, the selection of an upper limit for the S02 + H02 - SULFATE reaction was arbitrary. Thus for subse- quent modeling, 0.2 ppm"1min"1 was chosen as a certain upper limit, although the true rate is likely to be much lower. In the organic smog system, experi- menters investigated the methylperoxy- S02 reaction beginning with the same approach used for the H02-SO2 kinetics studies. The approach consisted of irradiating high concentrations of CH4 with controlled HNO2/NO,/S02 mix- tures in the smog chamber. The reaction of principal concern was CH302 + S02 — CH30 + SULFATE. Two initial experiments were under- taken to determine the overall rate of the above reaction based on sulfate aerosol formation in an atmosphere of moderate humidity. Methane was used as the methylperoxy source in the experiments. Although results were inconclusive, an upper limit estimate of 0.8 pprrT1min~1 was obtained for the conversion of S02 to sulfate via the methylperoxy radical. The mechanism of the conversion was not investigated. Because of the inconclusive results obtained with the CH4/HN02/NO,/SO2 smog system, additional experiments were conducted using azomethane as the methylperoxy source. However, these experiments too were quite limited. Role of /VOx in SOz Oxidation Via HO Radicals Experiments conducted with the HN02/NO,/SOZ smog system served to investigate the possibility for paniculate nitrate formation. At the conclusion of an experiment, sample air was drawn through acid washed and neutralized quartz filters and analyzed for N03~, S04*, and NH4+. To avoid HNOz or HNO3 volatilization losses, filter samples were immediately halved; one-half was stored in a desiccatory containing NH3, and the other was refrigerated without treatment. The analytical results from nine experiments showed no substantial differences in either S04= or N03" for the NH3 treated samples versus the untreated samples. Although ammoni- ated samples contained somewhat higher NH4+ concentrations, nearly all samples were deficient in NH3 when compared to the expected stoichiometry for (NH4)aS04 and NH4NO3. In every case, the paniculate nitrate concentrations were very low compared to the sulfate concentrations. The highest paniculate nitrate concentra- tions were recorded for the two experi- ments without SO2. Thus a substantial amount of nitrate was not incorporated in the particulate phase under the conditions of these experiments. While the results do not rule out the possibility that HOS02O interacts with N02 to produce H2S04 and HMOs, they do indicate that nitrate (if formed via this route) is not maintained in the aerosol phase, even under the presumably stabilizing influence of NH3. Oxidation in Simulated Urban and Rural Atmospheres In the second portion of this study, a series of smog chamber experiments ------- was conducted to investigate some of the factors affecting S02 oxidation under simulated atmospheric conditions and to develop data needed to evaluate photochemical models of S02 oxidation in polluted air. Experiments were conducted using hydrocarbon mixtures selected to represent urban and rural conditions. For each experiment, the initial non- methane hydrocarbon concentration was about 4.5 ppmC, and the initial NOX concentration was 0.3 ppm. Apart from the control experiments where no S02 was introduced, 0.6 ppm S02 was injected into the chamber at either 1 or 5 h intervals after the irradiation began. Replicate experiments were also con- ducted in which 0.15 ppm NO was injected, together with 0.6 ppm SO2. This approach was designed to simulate conditions in which S02 is emitted into polluted air from point sources. The experimenters attempted to determine whether or not S02 oxidation rates depended substantially on the interval of the photochemical smog period, and to what extent the presence of NO (NO is generally emitted along with S02) affected the oxidation rates. Analytical methods for determining SO2 and sulfate aerosols were identical to those used in the kinetic experiments. For this experimental series, two Meloy sulfur analyzers were used to monitor S02 and particulate sulfate simulta- neously. During the period of these experiments, Battelle's large smog chamber was lined with 5 mil FEP Teflon™ filter. The light intensity corresponding to k was 0.17 min"1. Gas chromatographic anal- yses for hydrocarbons were obtained initially and at irradiation intervals of 1, 3, 5, and 7 h. PAN concentrations were obtained hourly. For both urban and rural hydrocarbon mixtures, the rates of SO2 oxidation were greatest near the periods of peak N02 formation, and gradually diminished thereafter. After 24 h of irradiation, the rate of S02 oxidation was about one- fourth as large as the maximum rate observed with the urban hydrocarbon mix: for the rural hydrocarbon mix, the rate of S02 oxidation at 24 h was about one-third the maximum rate. The addition of NO with S02 (at SO2:NO ratios of 4:1) at different intervals of the irradiation period had mixed results. When added at 5 h, NO had small positive effects on the rates of S02 oxidation, but when added at 1 h, NO reduced the rates of S02 oxidation. Kinetic Model Application One objective of this portion of the study was to determine if a relatively simple model of atmospheric chemistry could suffice to represent S02 oxidation in polluted air. The smog chamber data previously presented and some field data from the Midwest Interstate Sulfur Transformation and Transport (MISTT) project provided the basis for applying the model. In most cases, the predictions for S02 conversion to sulfate were reasonably good; within 20%forthe inorganicsmog systems and within 25% for the HC-NO* systems. The model tended to under- estimate S02 conversion, and the hydrocarbon systems when the model estimates were only one-half the actual rates. For the smog conditions that were modeled, it was estimated that at least 75% and sometimes greater than 90% of the S02 oxidation was initiated by reactions of S02 with HO radicals. Although several shortcomings of the lumped model were found during its application to these data, it was still of interest to adapt the model to estimate diurnal patterns of S02 oxidation in comparison with field data. The objective of this exercise was to estimate the rate of S02 oxidation for power plant plumes resident in polluted atmospheres, as a function of solar radiation, plume emission periods, and plume dispersion rates. According to the modeling results, the production of HO and the oxidation of SO2 depended strongly on solar radia- tion intensity. Reduced radiation resulted in disproportionately lower rates of S02 oxidation. For reduced radiation condi- tions, the maximum rates of SO2 oxidation were predicted to occur near mid-afternoon, while for clear sky conditions, the maximum oxidation rates occurred between 11:00 a.m. and noon. The rates of S02 oxidation were shown to depend on ambient HC and NO, conditions. For the range of conditions modeled, the maximum rate of SO2 oxidation (clear sky) varied from 3.7 to 7.4%/h. Plume dispersion rates affected the induction period of NO and S02 oxida- tion. Variations in solar radiation intensity and thus the diurnal period of the power plant emissions strongly affected S02 oxidation rates. For well- dispersed plumes and clear sky condi- tions, maximum S02 oxidation rate (ranging from 2.7 to 6.9%/h) wen estimated to occur during the noon t early afternoon periods. The patterns c S02 oxidation predicted by the mode agreed well with the data for thi Labadie plume as reported in the MIST project. For relatively low HC:NOX ratios fo ambient air, SO2 oxidation rates com puted for plumes were bound by thi ambient rates of S02 oxidation. At higl HC:NOX ratios, the rates of SO2oxidatioi in plumes were predicted to exceed thi rates in ambient air. Under sucl conditions, the model also predicted ai excess (or bulge) in the plume 0 concentrations. These features havi been observed in actual plume studies Conclusions and Recommendations Regarding reaction 60 (S02 + OH + M — SULFATE), it appears that all of the S02 oxidized by this route results in the formation of sulfate particles. According to the analyses for particulate nitrate they did not form stable aerosol products with the intermediates created after HO addition to SO2. In the course of the experiment with inorganic smog systems (HN02/NOX/ S02), additional kinetic information was obtained, particularly as it pertained to the experimental system. An upper limit rate of 3 x 10~7 ppm"1min"1 was derived for the homogeneous reaction between dinitrogen pentoxide and water vapor to yield nitric acid (N205 + H2O — HN03). It was also determined that ozone and nitrous acid do not react at a significant rate to produce nitric acid. No hetero- geneous reaction between S02 and nitrous acid in the presence of sulfuric acid aerosols could be detected. Although the average reactivity for the urban and rural hydrocarbon mix- tures, based on rate constants ol individual hydrocarbons with HO radicals, was nearly equal, there were marked differences in several important smog parameters. With the urban hydro- carbon mixture, the rates of NO oxidation and xylene disappearance and the maximum rates of SO2 oxidation were about twice as great as for the rural hydrocarbon mixture. The formation of PAN and other products of N02 oxidation were also greater for the experiments with urban hydrocarbon. Since SO2 oxidation is dominated by the reaction with hydroxyl radicals, and since this initial reaction is the rate-. 4 ------- limiting step in S02's conversion to sulfate, it follows that relatively simple kinetic models which adequately de- scribe the variations in atmospheric HO should suffice to estimate gas phase SO2 transformation rates. Experimental and theoretical simula- tions of urban and rural atmospheres showed that the rates of S02 oxidation are strongly coupled to solar radiation intensity and pollution conditions. Although high concentrations of NO generally suppressed or delayed HO production and S02 oxidation, N02 inhibited SOz oxidation by scavenging HO. Aldehydes, CO, and possibly some hydrocarbons tended to inhibit S02 oxidation by converting HO into products which were less efficient in oxidizing S02. In general, reactive hydrocarbons served to promote S02 oxidation, and the stoichiometry or net flux of HO affected by hydrocarbon degradation appeared to be key to the acceleration of SOz oxidation in polluted air. SOz oxidation rates in moderately polluted air or in well-aged air that was once polluted were found for the most part to be 60 to 80% lower than the rates in freshly polluted air. Modeling results indicated that S02 oxidation rates in power plant plumes are highly dependent on plume disper- sion rates and are coupled to the same parameters governing SO2 oxidation in the ambient air. For well-dispersed plumes, most rapid SOz conversion was predicted to occur from noon through early afternoon. The accompaniment of NO in plumes generally suppressed HO and the rate of SOz oxidation. However, under certain circumstances where high concentrations of reactive HC were mixed into a rapidly-dispersing plume, the rate of SO2 oxidation was expected to exceed the oxidation rate in ambient air. Under such circumstances, an excess of ozone was also predicted in the plume. This study pointed out the need for further study in the area of sulfate aerosol formation. In particular, since the overall conversion rate for the SOz •*• H02 — SULFATE reaction was consider- ably less in this study than the literature value, it is recommended that additional high-pressure measurements of the reaction be made. Any such effort should include the determination of reaction products. David F. Miller is with Battelle-Columbus Laboratories, Columbus, OH 43201. Joseph J. Bufalini is the EPA Project Officer (see below). The complete report, entitled "Modeling of SO2 Oxidation in Smog," (Order No. PB 82-101 932; Cost: $13.50, subject to change) will be available only from: National Technical Information Service 5285 Port Royal Road Springfield, VA 22161 Telelphone: 703-487-4650 The EPA Project Officer can be contacted at: Environmental Sciences Research Laboratory U.S. Environmental Protection Agency Research Triangle Park, NC 27711 •frU.S. GOVERNMENT PRINTING OFFICE:1982--559-092/3365 ------- United States Environmental Protection Agency Center for Environmental Research Information Cincinnati OH 45268 Postage and Fees Paid Environmental Protection Agency EPA 335 Official Business Penalty for Private Use S300 PS 00005?9 U S ENVIR PROTECTION AGENCY REGION 5 LIBRARY 230 S DEARBORN STREET CHICAGO IL 60604 ------- |