United States Environmental Protection Agency Office of Air Quality Planning and Standards Research Triangle Park NC 27711 EMB Report 80-DRY-9 October 1980 Air Petroleum Dry Cleaners Centrifugal Separator Emission Test Report Cadet Cleaners Toronto, Canada ------- SOLVENT RECOVERY AND EMISSION CONTROL PETROLEUM DRY CLEANING INDUSTRY CADET CLEANERS PLANT Toronto, Ontario, Canada Prepared for the U.S. Environmental Protection Agency Emission Measurement Branch Research Triangle Park, N. C. 27711 Prepared by Clayton Environmental Consultants, Inc 25711 Southfield Road Southfield, Michigan 48075 EMB Report No. 80-DRY-9 Work Assignment 38 Contract No. 68-02-2817 ------- TABLE OF CONTENTS Page List of Tables i List of Figures ii 1.0 Introduction 1 2.0 Summary and Discussion of Results 2 3.0 Process Description 11 4.0 Location of Sampling Points 12 5.0 Sampling and Analytical Procedures 14 APPENDICES A. Esso Chemical Sheet B. ASTM Methods B-l. D 322 - 67 B-2. D 240 - 76 B-3. D 96 - 73 and Modifications C. Laboratory Analysis ------- LIST OF TABLES Table Page 2.1 Results of Filter and Dried Muck 3 Analyses 2.2 Petroleum Solvent Decanted Before 6 Distillation 2.3 Results of Liquid Sample Analyses 8 ------- LIST OF FIGURES Figure Page 4.1 Plan view of filtration equipment 13 and location of sampling points 11 ------- 1.0 INTRODUCTION The United States Environmental Protection Agency (EPA) retained Clayton Environmental Consultants, Inc. to evaluate the performance of a centrifugal separator at the Cadet Cleaners plant in Toronto, Ontario, Canada. The objective of this study was to determine the total uncon- trolled solvent loss from this plant (provided by TRW, Inc.) and to evaluate the performance of the centrifugal separator as an emission control technique. The results of this study will be used in research and development efforts for supporting New Source Performance Standards in the petroleum dry cleaning industry. This study was commis- sioned as Project No. 80-DRY-9, Contract No. 68-02-2817, Work Assignment 38. The field sampling program, conducted July 9 through 11, 1980, was slightly modified after inception and in- cluded the following: (1) Multiple soap and rinse filter muck samples acquired from diatomaceous earth filters for petroleum solvent loss determinations; (2) Multiple dried muck samples acquired from a centrifugal separator after extraction for petroleum solvent loss determinations; and, (3) Duplicate samples from the vacuum petroleum still bottom wastes, reclaimed distilled solvents, and a single sample of virgin petroleum solvent acquired for determina- tion of Btu content and inerts. - 1 - ------- 2.0 SUMMARY AND DISCUSSION OF RESULTS The results of the sample solvent recovery and heat of combustion analyses are presented in Tables 2.1 and 2.3, respectively. Table 2.1 presents the quantity of solvent (as a percent by weight) retained by the filter muck samples. These samples were collected from the East and West domes- tic soap and rinse filtered mucks, an industrial filtered muck, both before centrifuqation (after 24 hours of settling), and from the combined soap and rinse filter mucks after centrifugation. The efficiency of the centrifugal separation system also appears. The solvent retained, as percent by weight, was calculated using the following equation: Solvent Retained = (milliliters of diluent) (SpGr) (D) 1QQ weight of aliquot where:SpGr = specific gravity of solvent (60/60F) = 0.7857 (Appendix A) D = density of water, g/ml = 1.0 The efficiency of the centrifugal separation system (quantity of solvent removed, as percent by weight, during the solvent recovery process) was calculated using the following equation: Efficiency = SSF - SDM x 1QO SSF where: SSF = % solvent by weight retained by soap filter. SDM = % solvent by weight retained by dried muck. - 2 - ------- TABLE 2.1. RESULTS OF FILTER AND DRIED MUCK ANALYSES Sampling Date and Sam Time 7/09/80 West PM West 7/10/80 East AM East 7/10/80 West PM West 7/11/80 East AM 7/11/80 West PM West (% by Weight) p e Before Centrifugation (After 24 hr settling) soap 47 . 1 rinse 47.6 soap 54.9 rinse 52.3 soap 48.7 rinse 41.3 soap 52.3 soap 51.3 rinse 47.1 Average 49.2 7/11/80 Industrial 52.3 AM After Centrifugation 34.0 34.0 34.5 34.5 31.4 31.4 38.2 30.9 30.9 33.3 38.2 Extraction Efficiency (% by Weight) 27.8 28.6 37.1 34.0 35.5 24.0 27.0 39.8 34.4 32.0 27.0 Facility: Cadet Cleaners, Toronto, Ontario, Canada. - 3 - ------- The solvent retained by the filter muck samples collected from the domestic soap and rinse filters of the East and West filtering systems (before centrifugation) ranged from 41.3 to 54.9-percent, averaging 49.2-percent. The single industrial filter retained 52.3-percent solvent by weight. The solvent retained by the dried muck samples, after centrifugation, ranged from 30.9 to 38.2-percent, averaging 33.3-percent. Laboratory data appears in Appen- dix C. The relative difference in solvent content between the domestic soap and rinse filter muck samples seems to generally be a decreasing function. In theory, it is plausible that the industrial and soap diatomaceous earth filters separate a coarser dirt particle or a more sponge- like particle than do the rinse filters and thus, retain more solvent. However, there are not sufficient data sets to refute or corroborate this theory. The centrifugal separator reclaimed an average of 32.0-percent of the solvent in the filters. Therefore, the solvent loss from the plant is reduced by using the cen- trifugal separator. The efficiency of the centrifugal separator seems to depend on the particle size of the dirt concentration, solvent retention of the filter mucks to be extracted, and average rotational speed which the separator ultimately achieves during extraction. The efficiency of the sep- arator does not seem to depend on the condition of the - 4 - ------- cloth bag used to retain the dried muck for disposal. This was evidenced by the fact that the cloth bag was washed and cleaned prior to the last extraction sampled, yet no sig- nificant improvement in efficiency was displayed. Table 2.2 displays the amounts of petroleum solvent decanted from each filter muck sample (before centrifuga- tion). Each sample was decanted twice before the lab- oratory distillation procedure began. The first decanting occurred in the field after 24 hours or less of settling. Due to the hazardous/flammable nature of the solvent, field decanting was necessary to reduce the overall volume of solvent so the samples could be shipped by land carrier through customs. The field decanting removed most of the solvent above the settled filter muck leaving only a thin layer to keep the filter muck immersed and fluidized for later laboratory analysis. This layer of solvent was used by the laboratory to mix the samples to simulate the 24-hour settling period prior to distillation analysis which could not be achieved in the field. This thin layer of solvent was to be de- canted off by the laboratory after the 24-hour settling period. Although five filter muck samples had no excess solvent to be decanted after the settling period, the solvent retained by the filter muck dovetailed with those which did have decantable volumes to within 10.8 and 12.5- percent of the mean and average values, respectively. - 5 - ------- TABLE 2.2. PETROLEUM SOLVENT DECANTED BEFORE ANALYSES Sampling Date and Time 7/9 PM 7/10 AM 7/10 PM 7/11 AM 7/11 PM 7/11 AM Sample West soap West rinse East soap East rinse West soap West rinse East soap West soap West rinse Industrial Field Decantation ml 76 168 120 189 150 120 145 93 98 158 Laboratory Decantation ml 28 0 0 0 0 0 27 92 32 65 Total Volume ml 104 168 120 189 150 120 172 185 130 223 Facility: Cadet Cleaners, Toronto, Ontario, Canada. - 6 - ------- Table 2.3 presents the heat of combustion of the liquid samples, expressed as British Thermal Units per gallon of solvent (Btu/gal), and the percent inerts. The analyzed heat of combustion of the liquid samples ranged from 124,900 to 130,400 Btu/gal, with a mean of 128,900 Btu/gal. The still bottom waste samples averaged 130,400 Btu/gal and the reclaimed solvent averaged 127,000 Btu/gal. The still bottom waste has a higher heat value possibly due to fiber resins and organic constituents contained therein. It may be feasible to use the still bottom wastes, now being dumped into the city sewer system, as a supplemental fuel and/or boiler fuel additive. The liquid samples were analyzed for percent inerts. Due to sample contamination of the redistilled and virgin solvent samples, only the still bottom waste samples were analyzed and averaged 1.5-percent. No presurvey was conducted prior to the start of the project and the scope of the project was expanded in the field from an original total of six samples to 20 samples. Due to the brevity of the field sampling schedule (3 days) and the increase in the number of samples to be collected, it was necessary to purchase mason jars as extra sample containers, so as not to further delay the project. The mason jar lids were fitted with latex rubber gaskets to insure against leakage. The rubber gaskets on those sample containers that contained large quantities of petroleum solvent reacted with the solvent which softened _ -i _ ------- TABLE 2.3. RESULTS OF LIQUID SAMPLE ANALYSES 1980 Sample Date 7/11 7/10 7/11 7/10 7/11 Sample Virgin solvent Still bottom waste - 1 Still bottom waste - 2 Average Dry cleaning solvent - 1 Dry cleaning solvent - 2 Average Mean Btu/gal 129,700 130,400 130,400 130,400 129,100 124,900 127,000 128,900 % Inerts b 1.4 1.7 1.5 b b — Facility: Cadet Cleaners, Toronto, Ontario, Canada. ^Performed by Detroit Testing Laboratories, Inc., Oak Park, Michigan. DSamples could not be analyzed due to contamination. ------- the seal. The rubber seal did not soften in any of the dried filter muck sample containers because of the lack of solvent. The rubber seals on the containers of the filter muck samples collected before centrifugation, remained sandwiched between the lid and jar rim even after being stored for a month prior to analysis. Analysis was delayed because the glass receiver/traps needed to measure the diluent during distillationwere on back order by our laboratory suppliers. The rubber seals of the precentrifuged sample con- tainers were not appreciably altered due to the decanting of solvent in the field; therefore any contamination would be minimal in lieu of the mass weight of the filters in comparison to the mass weight of the gasket. Also, the receiver/trap used in the analysis was only capable of measuring to the nearest 0.1 milliliter; therefore, the small amount of rubber seal which might be contained in any of the mixed 15-grams of the filter muck aliquot would be negligible. The rubber seals on the virgin and recalimed solvent sample containers were also softened, causing portions of the gasket to separate from the main body and fall into the sample. The virgin solvent developed a very slight orange hue even after the pieces of the rubber gasket had been removed from the samples. These samples were filtered before the heat content analysis (Btu) was conducted. The contamination from the latex rubber seal, - 9 - ------- which would tend to increase the heat content, would be very small due to the minimal solubility of latex rubber in the solvent. The percent inerts were not obtained for these samples since contamination is a major contributor to inerts. - 10 - ------- 3.0 PROCESS DESCRIPTION AND OPERATIONS To be supplied by TRW, Inc. - 11 - ------- 4.0 LOCATION OF SAMPLING POINTS All filter muck from the diatomaceous earth filters is pumped to the centrifugal separator in varied combina- tions for extraction. The filter muck is delivered to the top of the centrifugal separator through two radial spout arms. The samples were collected at the discharge of these spouts as the muck dropped into the separator. All dried muck samples were obtained directly from the centrifugal separator following a 20-25 minute extrac- tion . The petroleum still bottom waste samples were col- lected from the bottom spigot of one 500-gallon per hour Washex vacuum still. Distilled petroleum solvent samples were acquired from the distillation collection vessel next to the still. The virgin solvent was obtained directly from the original shipping container. Figure 4.1 presents a plan view of the equipment and location of sampling points, as specified. - 12 - ------- J- Radial spout arms r Sewer trough 11 Diatomaceous Earth Filters No. 1-10 Domestic Nos. 11 - 13 Industrial Leading to City Sewer System N Figure 4.1. Plan view of filtration equipment and location of sampling points, ------- 5.0 SAMPLING AND ANALYTICAL PROCEDURES SAMPLING PROCEDURES Characteristic samples of muck were collected from the soap and rinse filters of the East and West filter systems. Only one industrial filter sample was collected, due to equipment malfunctions. The samples were collected by diverting a portion of each filter muck discharge into a glass collection container which was washed clean in petro- leum solvent and dried between each sample collection. Up to three equal amounts of each sample were proportionately composited in glass sample bottles. A representative sample of dried muck was obtained directly from the centrifugal separator after the comple- tion of a 20-25 minute extraction. Each extracted muck sample was composed of up to four filter muck discharges. A 1-inch (inside diameter) copper pipe was inserted into the dried muck at random points within the separator to ensure collection of all layers. A 1-inch (outside dia- meter) wooden dowel was inserted through the pipe to deposit the sample in a glass sample bottle. The pipe and dowel were washed clean in petroleum solvent and dried between each sample collection. Two still bottom samples were obtained from one 500- gallon per hour vacuum still. Because of high temperatures, the samples were initially collected in a galvanized pail, and later poured into glass sample bottles. - 14 - ------- Two distilled petroleum solvent samples were obtained from the vacuum still by directly collecting the solvent in qlass sample containers. One virgin petroleum solvent sample was obtained in a glass sample bottle directly from the original shipping container. Therefore, at the end of the study, the following samples were collected: 3 - West wash filter muck; 3 - West rinse filter muck; 2 - East wash filter muck; 1 - East rinse filter muck; 1 - industrial filter muck; 5 - dried muck; 2 - still bottom waste solvent; 2 - redistilled solvent; and, 1 - virgin petroleum solvent. For the July 9 and 10 samples, the muck levels were marked on the sample containers after 24 hours of settling, and the excess solvent had been decanted off leaving only a thin layer of solvent covering the muck. The decanting of the solvent was conducted in-field to comply with the hazardous/flammable shipping regulations. The settling times for the July llth morning and afternoon samples were 6-hours and 2-hours, respectively. The volume of solvents decanted in the field were recorded. The containers were sealed and taped to prevent leakage while being shipped to the laboratory for analyses. - 15 - ------- LABORATORY ANALYSIS All samples were checked for leakage and/or breakage upon receipt in the laboratory and none was detected. Each filter muck sample was thoroughly mixed with the remaining petroleum solvent in its container using a stain- less steel stirring rod. The samples were allowed to settle for 24 hours and any excess solvent was decanted off and the volume recorded. To determine the solvent content in the muck (percent by weight), representative portions (approximately 15- grams) were taken from both the filter muck and dried muck samples with a clean glass tube. The withdrawn portion was weighed to the nearest 0.01-gram, transferred with dis- tilled water to a distillation flask which was heated with an electric heater, and analyzed by following the refluxing procedure as described by the American Society for Testing and Materials (ASTM) Method D 322-67 (Appendix B-l). When heating/condensation began, the system was rechecked to ensure proper functioning. Refluxing was allowed to pro- ceed for 2 hours, after which, the volume of diluent was measured at one-half hour intervals. The analysis was considered complete when volume changes no longer occurred at the set refluxing temperature. - 16 - ------- The still bottom wastes, the redistilled solvent, and the virgin solvent were analyzed for Btu content and inerts by Detroit Testing Laboratory, Inc. Btu content was deter- mined according to the procedures outlined in ASTM Method D 240-76 (Appendix B-2). Prefiltering of the virgin and redistilled solvent samples removed any residue from the samples before Btu analyses. The procedures in ASTM Method D 96-73 were modified in the analysis for inerts. Both the method and modifications are presented in Appendix B-3. - 17 - ------- |