73-FRT-7 (REPORT NUMBER) AIR POLLUTION EMISSION TEST U.S.S. AGRI-CHEMICALS (PLANT NAME; NASHVILLE, TENNESSEE (PLANT ADDRESS) U. S. ENVIRONMENTAL PROTECTION AGENCY Office of Air and Water Programs Office of Air Quality Planning and Standards Emission Standards and Engineering Division Emission Measurement Branch Research Triangle Park, N. C. 27711 ------- EPA REPORT NUMBER 73-FRT-7 U.S.S. Agri-Chemicals NASHVILLE, TENNESSEE Submitted to Environmental Protection Agency Office of Air Programs Contract No. 68-02-0225 Task No. 15 Submitted by Engineering-Science, Inc. 7903 Westpark Drive McLean, Virginia 22101 November 1974 ------- I TABLE OF CONTENTS Section Title Page II INTRODUCTION 1 III SUMMARY AND DISCUSSION OF RESULTS 2 IV PROCESS OPERATION 12 V LOCATION OF SAMPLING PORTS 15 VI SAMPLING AND ANALYTICAL PROCEDURES 22 ------- LIST OF TABLES Table Title Page III-l Corresponding Changes of Ammonia Concentrations in Exhaust Gas and Scrubber Liquor 7 III-2 Kiln Dryer/Cooler Baghouse Emission Summary 8 III-3 Ammoniator Scrubber Emission Summary 9 III-4 Kiln Dryer/Cooler Baghouse Flow Data 10 III-5 Ammoniator Scrubber Flow Data 11 LIST OF FIGURES Number Title Page IV-1 Schematic Diagram of Process, U.S.S. Agrichemicals, Nashville, Tennessee 14 V-l Kiln Inlet to Baghouse 16 V-2 Kiln Baghouse Stack 17 V-3 Location of Sampling Ports: Ammoniator Scrubber Inlet and Outlet 20 V-4 Traverse Point Locations 21 ------- II INTRODUCTION Source emission tests were conducted at the U.S.S. Agri-Chemical phosphate fertilizer plant, Nashville, Tennessee, during the week of May 21, 1973. The purpose of the tests was to gather data upon which the U. S. Environmental Pro- tection Agency can establish emission standards for new sources in the phosphate fertilizer industry under Section 111 of the Clean Air Act of 1970. This report describes the methods used and results obtained in the test series. In total,twelve (12) samples were obtained for each of the following emissions; particulates, ammonia and total fluorides. Samples were obtained from two process operations, the dryer kiln/cooler baghouse and the ammoniator scrubber. Simultaneous sampling of both the inlet and outlet gas streams of each control device was conducted. Thus three samples were collected for each of the pollutants at each of the following locations: kiln baghouse inlet, kiln baghouse exit, ammoniator scrubber inlet and ammoniator scrubber exit. The sampling locations are shown in Figure IV-1. In addition to these gas stream samples, grab samples of scrubber liquid, phosphate rock and granu- lated fertilizer product were periodically taken for analysis by EPA. Analyses of the fluoride and ammonia samples were done by EPA chemists. An analysis of the particulate samples was done by ES. Section III of this report contains a discussion and summary of the results of the tests. Subsequent sections describe the location of the sampling ports and the sampling and analytical procedures. The Appendices contain all the raw data collected on-site as well as the complete analysis of this data. Mr. Robert M. Martin and Mr. J.E. McCarley, of the Office of Air Quality Planning and Standards, Environmental Protection Agency, coordinated the tests and arranged for the test facilities. 1 ------- Ill SUMMARY AND DISCUSSION OF RESULTS The data obtained during the test was reduced to computer format for analysis. The concentrations of particulate, fluoride, and ammonia in the exhaust gases along with their respective emission rates were calculated. Complete particulate results, along with a sample calculation, appear in Appendix A, and complete results for fluoride and ammonia appear in Appendix B. All results are expressed both in English and metric units. In accordance with EPA's letter of June 20, 1973, included in Appendix J, emission rates are reported in Ib/hr and Ib/ton feed. Summaries of the data appear in Table III-l through III-5, and are discussed in more detail later in this section. When the fertilizer plant changes production to a different type of fertilizer, input feed rates must also change. While ES was testing, two types of fertilizers were produced: 10-10-10 and 6-12-12, the numbers standing for proportionate amounts of constituents. Feed rates for each type of product, as reported by EPA in their letter of December 10, 1973, are as follows: NH- Feed Rates 10-10-10 1.20 tons/hr 6-12-12 2.45 tons/hr P-0 Feed Rates 10-10-10 0.465 tons/hr 6-12-12 2.90 tons/hr TOTAL FEED RATE 25 tons/hr ------- Fertilizer 10-10-10 was produced from tests number 1 through 6 and 6-12-12 was produced during the remainder of the tests. As described in Section V, the scrubber inlet (horizontal stack, see Figure V-3) had three inches of water flowing in the lower quarter. For flow rate calculations, an effective cross-sectional area was derived by sub- tracting the area occupied by the water. An effective stack diameter was then calculated from this derived area. The real diameter, 18 inches, was reduced to 15.4 inches. When reviewing the values for flow rate at the kiln and ammoniator, discrepancies on the order of 25-35% between inlet and outlet were noticed. EPA methods and standards were stringently adhered to and all calculations were carried out properly. No evidence is available to formulate an explanation for these discrepancies at the kiln. However, at the scrubber, system leakage could have allowed dilution air to enter the gas stream. When reviewing isokinetic values, a few are noted that are greater than 10% from isokinetic. For most cases where the isokinetic value was greater than 110%, the average orifice pressure drop is approximately 0.40 in. H_0. At this rate, the meter AH0 is about 1.7 instead of the value of 1.85 which was used to set up the nomograph. A. Particulate Analysis Test No. 11-1, at the scrubber inlet, must be disregarded because a quantity of mud and water, which was later found to be flowing in the stack, had been inadvertently sampled. Test No. 11-0, at the scrubber stack must be disregarded due to upset conditions at the scrubber which occurred suddenly during the test allowing a large amount of particulate matter to be caught by the sample train before the train could be shut down. ------- The particulate emissions do not appear to be influenced by the type of fertilizer being produced. Controlled filterable particulate emissions at the baghouse stack range from .65 to 1.38 Ibs/hr. Controlled total emissions range from 3 to 14 Ibs/hr. Controlled emissions as a function of feed rate range from 0.13 to 0.56 Ibs/ton feed. Comparing inlet and outlet emission data at the baghouse it is noted that filterable particulates are reduced greater than 99.9% in the baghouse; total particulates are reduced 99.7%. At the inlet to the baghouse only 0.43% of the total particulate catch is found in the impingers. At the outlet 86% of the total catch passes through the filter and is caught by the impingers. At the scrubber stack controlled filterable particulate emissions range from 2.73 to 3.24 Ibs./hr. Controlled total emissions range from 4.25 to 7.73 Ibs/hr. Controlled emissions from the baghouse as a function of feed rate range from 0.17 to 0.31 Ibs/ton feed. The scrubber is 97% efficient in re- moving filterable particulates and 95% efficient in removing the total particu- late load. At the scrubber inlet only 2% of the particulate catch is found in the impingers, but at the outlet 47% of the catch passes through the filters and is caught by the impingers. B. Fluoride Analysis Test No. 4-1 at the kiln baghouse inlet was voided because the sample was spilled during analysis. Controlled emission rates at the baghouse stack show a relationship to the type of fertilizer being produced. Production of 10-10-10 fertilizer with a P90_ feed rate of 0.465 ton/hr yields a controlled fluoride emission rate of about 2.7 Ib/hr, while 6-12-12 production, with a larger P^ feed rate of 2.90 tons/hr yields smaller controlled fluoride emissions of 0.57 to 0.78 Ibs/hr. Controlled emission'rates as a function of feed show this same rela- tionship with 5.8 Ibs/ton P205 feed being emitted during 10-10-10 production 4 ------- and 0.20 to 0.27 Ibs/ton ?205 feed being emitted during 6-12-12 production. Controlled fluoride emission rates from the scrubber stack during 6-12-12 production range from 0.02 to 0.25 Ibs/hr, or 0.006 to 0.087 Ibs/ton P20_ feed. No tests were conducted at the scrubber stack during 10-10-10 production, therefore, no comparison can be made. Checking inlet and outlet data, it is observed that the baghouse is 96% efficient in removing fluoride; at the scrubber, 46% of the fluoride load is removed. C. Ammonia Analysis Ammonia samples were drawn non-isokinetically and no attempt was made to measure stack velocity or flow rate. To calculate ammonia concentrations and emission rates, the flow rates calculated from parallel tests were used. If no parallel tests were made at the same time, then figures from tests conducted on the same day were used. If no tests were conducted on the same day at that particular test location, then an average value for flow rate was used. During 6-12-12 production, controlled ammonia emission rates are higher than during 10-10-10 production. At the baghouse stack, controlled ammonia emissions are about 2.1 Ib/hr or 1.8 Ib/ton NH_ feed with an NH^ feed rate of 1.20 tons/hr during 10-10-10 production, and 10 to 19 Ibs/hr or 4 to 8 Ibs/ton NH- feed with a higher feed rate of 2.45 tons/hr during 6-12-12 production. At the scrubber stack, controlled ammonia emissions during 10-10-10 production are 116 to 142 Ibs/hr or 97 to 118 Ibs/ton NH3 feed, while during 6-12-12 production, controlled emissions are about 177 Ibs/hr or 72 Ibs/ton NH3 feed. Comparing the inlet and outlet data, it is noted that the baghouse reduces ammonia emission by 88%. Negative efficiencies were noted at the scrubber. ------- Engineering-Science, Inc. had followed the EPA test methodology for sampling ammonia in exhaust gas streams. The results presented in this study indicate that more gaseous ammonia was liberated from the ammoniator scrubber than was measured in the inlet gas stream. In other words, by our calculations the ammoniator scrubber seemed to add ammonia to the gas stream instead of re- ducing or minimizing these emissions. ES has reviewed the data thoroughly and are convinced that errors in transcribing, calculations, laboratory reporting, and final writing did not result in the negative efficiencies projected. The most probable cause for the results obtained for ammonia emissions is the scrubber operation since gaseous ammonia can be absorbed in water or some acidic solution. Changes in the inlet concentration may change the equilibrium of the scrubber solution and thus may cause ammonia to be liber- ated. The net effect of this situation the liberation of ammonia from the scrubber water under certain conditions could have occurred during the three tests for ammonia made on the ammoniator scrubber. As shown in Table III-l, the change in ammonia concentration in the exhaust gas corres- ponded to the change in ammonia concentration of the scrubber liquor. When the concentration of ammonia in the exhaust gas decreased from inlet to outlet, the ammonia concentration in the scrubber liquor increased. When the concentration in the exhaust gas increased, the concentration in the scrubber liquor decreased. The scrubber was probably operating at near NH_ saturation level. It must be noted that the scrubber was primarily designed to remove particulates, not ammonia. ------- TABLE III-l CORRESPONDING CHANGES OF AMMONIA CONCENTRATIONS IN EXHAUST GAS AND SCRUBBER LIQUOR Test No. 2 6 9 Liquor HN3 Gas NH3 Concentration Concentration (mg/1) (gr/scfd) In Out In Out 48.7 49.4 2.14 1.99 39.9 52.1 3.22 2.57 116.8 108.7 1.71 3.22 ------- TABLE III-2 KILN DRYER/COOLER BAGHOUSE EMISSION SUMMARY Run No. 1 5 AVGa 7 4 8 10 AVGa 3 12 13 AVG Pollutant PT PT PT PT FL FL FL FL NH3 NH3 KH3 Product 10-10-10 10-10-10 10-10-10 6-12-12 10-10-10 6-12-12 6-12-12 6-12-12 10-1 10 6-12-12 6-12-12 6-12-12 FRONT HALF In gr/scfd 19.85 9.59 14.72 11.76 Out gr/scfd .008 .005 .007 .004 In Ib/hr 4532 2096 3314 2817 Out Ib/hr 1.376 .814 1.095 .649 In Ib/ton 181.3 83.8 132.6 112.7 Out Ib/ton .055 .033 .044 .026 Eff 99.9 99.9 99.9 99.9 TOTAL In gr/scfd 19.91 9.65 14.78 11.79 * .122 .045 .084 .052 .426 .697 .562 Out gr/scfd .079 .021 .050 .050 .015 .004 .003 .004 . .011 .112 .060 .086 In Ib/hr 4547 2109 3328 2825 * 27.7 10.3 19.0 12.17 101.3 164.2 132.8 Out Ib/hr 13.95 3.36 8.66 8.92 2.71 .778 .572 .675 2.11 18.86 10.45 14.66 In Ib/ton 181.9 84.4 133.2 113.0 * 9.54 3.57 6.56 10.14 41.36 67.02 54.19 Oat Ib/tor. .558 .134 .346 .357 5.83 .268 .197 .233 1.76 7.70 4.27 5.99 Eff 99.7 99.8 99.8 99.7 * 97.2 94.4 95.8 82.7 81.4 93.6 87.5 do *Sadple spilled during analysis. - Average for specified product. ------- TABLE III-3 AMMONIATOR SCRUBBER EMISSION SUMMARY Run No. 11 14 15 AVG 16 17 18 AVG 2 6 AVG 9 Pollutant PT PT PT PT FL FL FL FL NH3 NH3 NH3 Product 6-12-12 6-12-12 6-12-12 6-12-12 6-12-12 6-12-12 6^12-12 6-12-12 10-10-10 10-10-10 10-10-10 6-12-12 FRONT HALF In gr/scfd __«._.. 2.95 3.18 3.07 Out gr/scfd .__-»___ .068 .053 .061 In Ib/hr _«___ 95.0 133.4 114.2 Out Ib/hr _____.. 3%.24 2.73 2.99 In Ib/ton TEST 3.80 5.34 4.57 Out Ib/ton VOIDED .130 .109 .120 Eff .«.»_... 96.6 98.0 97.3 TOTAL In gr/scfd r. . -.- 3.07 3.20 3.14 .005 .005 .005 .005 2.15 3.23 2.69 1.72 Out gr/scfd _.._««-*».. .162 .083 .123 .001 .004 .001 .002 2.04 2.65 2.35 3.2? In Ib/hr -. 98.9 134.2 116.6 .21: .18; .19! .19? 84.0 113.0 98.5 66.0 Out Ib/hr 7.73 4.25 5.99 .03! .25' .01; .10: 115.9 142.0 129.0 177.5 In Ib/ton 3.96 5.37 4.67 .073 .064 .069 .069 70.0 102,5 86.3 26.9 Out Ib/ton .31 .17 .24 .013 .087 .006 .035 96.6 118.3 107.5 72.4 Eff X 92.2 96.8 94.5 82.0 -36. 8b" 91.5 45.6 -38.0 -25.7 -31.9 -169. Although negative efficiency, the value was included in average. ------- TABLE III-4 KILN DRYER/COOLER BAGHOUSE FLOW DATA Test No. 1-1 1-0 4-1 4-0 5-1 5-0 7-1 7-0 8-1 8-0 10-1 10-0 AVG-I AVG-0 Flow Rate (acfm) 38,949 29,576 38,931 29,628 37,949 27,334 40,002 29,094 39,629 28,915 38,193 28,752 38,942 28,883 Flow Rate (scfm) 26,650 20,604 26,822 21,040 25,510 18,834 27,961 20,646 26,417 20,518 26,641 20,353 26,667 20,333 Moisture C%) 8.71 9.85 8.95 8.85 10.63 10.43 7.47 8.44 11.68 9.16 7.36 10.31 Stack Temp.(°F) 224 210 214 202 218 210 216 205 219 203 221 196 Isokinetic (%) 105.7 101.1 116.4 96.7 114.2 102.5 110.4 101.0 118.0 101.6 111.3 99.2 Impinger Catch (%) .33 90.13 .65 75.76 .30 92.70 0.43 86.2 10 ------- TABLE 111-5 AMMQNIATOR SCRUBBER FLOW DATA Test No. 11-1 11-0 14-1 14-0 15-1 15-0 16-1 16-0 17-1 17-0 18-1 18-0 AVG-I AVG-0 Flow Rate (acfm) 5,066 7,579 5,348 7,753 6,148 8,115 6,056 7,965 6,003 8,795 5,577 8,073 5,700 8,046 Flow Rate Cscfm) 4,036 5,567 3,755 5,558 4,899 6,004 4,687 5,744 4,785 6,808 4,391 6,132 4,426 5,969 Moisture C%) 12.21 13.34 22.64 16.02 12.21 12.94 12.85 15.02 9.54 10.91 10.53 13.16 Stack Temp. (°F) 110 143 110 138 110 141 123 142 129 130 130 126 Isokinetic (%) | 99.8 113.5 104.7 107.0 105.1 105.9 107.7 102.8 107.8 95.7 Impinger Catch (%) ^«i 3.90 58.1 0.55 35.8 2.22 47.0 11 ------- IV PROCESS OPERATION This plant produces different grades of fertilizer with ammonium sulfate as the source of ammonia. The sulfate is shipped from Gary, Indiana, where it is produced as a by-product of coke oven operation. Anhydrous ammonia and nitro- gen solutions are also used as nitrogen sources to react with the phosphoric acid. Since the phosphoric acid might not react with all the ammonia, sulfuric acid is added to pick up excess ammonia. The mixing of these materials (plus some others) is carried out in the ammoniator which is basically a reaction vessel. Ammonia not absorbed in the mixture escapes into the air causing air pollution. Other emissions from the ammoniator are flourides and particulates. The granules produced in the ammoniator are dried in a rotary dryer. Cooling air is introduced into the rotary cooler to cool the hot material. The cooler gases charged with particulates are drawn by a fan located downstream of a cyclone which serves to remove the coarse material. The gases drawn by this fan are discharged into the plenum of the dryer. The dryer is operated by natural gas and has its own blower for supplying air to the burner. Gases and particulates are withdrawn by an induced fan via a baghouse and discharged into the atmosphere. The fan is centrifugal, driven by a 100 HP, 1725 RPM Reliance Motor. The pulley ratio is 1:2, resulting in about 3000 RPM on the fan shaft. The ID of the stack is 32.5 inches. The granules are sized in two closed (not hooded) screens. The first, called the hot screen, classifies the granules leaving the dryer. The fine material is introduced into the cooler and coarse material into a crusher for reduction in size and returned for screening to the same hot screen. 12 ------- From the cooler, the granules are discharged over a fine screen. Those not passing through this screen represent the product. The fines going through are recycled to the ammoniator. Raw material is fed to the ammoniator at 25 TPH. The recycle-to-feed ratio varies between 0.5:1 to 1.5:1. That means that total material handled in the ammoniator, recycle plus feed, ranges between 40 and 60 TPH for a production rate of 25 TPH. A schematic diagram of the process appears in Figure IV-1. This and the process description were provided by EPA. 13 ------- SCHEMATIC DIAGRAM OF PROCESS, USS AGRICHEMICALS NASHVILLE, TENNESSEE Test Locations Test Locations Phosphoric Acid Ammonia Ammonium Sulfate H2S04 tr> c/i C5 Product Ai r i ___ product Screen Hot Screen^ Fines Recycle CD 73 ------- V LOCATION OF SAMPLING PORTS Four different sampling locations were used during the tests; therefore, each will be discussed individually. A. Granulating Kiln Baghouse Inlet Two 2-1/2 inch diameter sampling ports were located in the granulating kiln effluent duct. The ports were located 90° apart and approximately 16 feet downstream from the kiln discharge point. Figure V-l is a line sketch showing the location and configuration of the sampling ports. The kiln effluent duct to the baghouse is constructed of 1/8 inch steel plate, 37 inches inside diameter. A small access platform was erected to support the sample train during the horizontal traverse. The vertical port was traversed by suspending the sample box on ropes and pulleys from the overhead roof supports. During the vertical traverse, the sample box was modified so that the probe extended downward vertically. Referring to Method 1 (Federal Register; Vol. 36; n. 247; December 23, 1971), a total of 12 sampling points (6 on each axis) were selected. B. Granulating Kiln Baghouse Exit Two 2-1/2 inch diameter sampling ports were located in the baghouse effluent stack, 90° apart approximately 30 feet above ground. Figure V-2 is a line sketch of the baghouse, showing the location and configuration of the sampling ports. The baghouse effluent stack is constructed of 1/8 inch steel plate, 32-1/2 inches inside diameter. A3' x 8' platform extension from the upper baghouse platform was constructed specifically for the project. Access to the platform was provided by a vertical ladder to the ground. 15 ------- FIGURE V-l. KILN INLET TO BAGHOUSE Sampli ng Port 2 1/2" Dia. 16 ENGINEERING-SCIENCE, INC. ------- FIGURE V-2 KILN BAGHOUSE STACK 09 Motor in CM 32-1/2 r Sampl1ng Port 2 1/2" Dia. Baghouse 17 ENGINEERING-SCIENCE, INC. ------- The ports were located approximately 25 feet downstream from the baghouse induced draft fan and 8 feet upstream from the effluent exit point. According to Method 1, a total of 12 sampling points (6 on each axis) were selected. C. Ammpniator Scrubber Inlet Two 2-1/2 inch diameter sampling ports were located in the horizontal section of the scrubber inlet duct about 25 feet above ground. Figure V-3 is a line sketch of the venturi scrubber, separation tank, fan and stack showing the location and configuration of the sampling ports. The horizontal orientation of the duct necessitated vertical sampling in one of the ports. A system of ropes and pulleys was used to support a standard EPA sample train box which had been modified for this purpose. The scrubber inlet duct is constructed of 1/4 inch fiberglass, 18 inches inside diameter. A 4' x 4' working platform was constructed specifically for the project. Platform access was provided by a vertical ladder down to a previously existing platform on the kiln baghouse structure. Access to this platform was by a vertical ladder to ground level. The ports were located 4 feet upstream from a 90° elbow and 10 feet I downstream from the nearest turn. According to Method 1, a total of 12 sampling points (6 on each axis) were selected, Later, this was reduced to only the 6 points on the horizontal access due to the extremely large quantity of water found to be flowing down the lower quarter diameter of the duct. The water was found upon inspection to be at least three inches deep in the bottom of the duct, thus negating the possibility of sampling the lower 3 points on the vertical axis. Testing continued after the EPA project officer approved the plan to utilize only the six horizontal axis points. Figure V-4 shows all traverse point locations for all stack ports. In all cases, the points are numbered consecutively, from 1 to 6 with the first point nearest the sampling port. 18 ------- D. Ammoniator Scrubber Outlet Two 2-1/2 inch diameter sampling ports were located in the ammoniator scrubber stack, 90° apart and approximately 30 feet above ground. The loca- tion and configuration of the sampling ports are also shown in the line sketch, Figure V-3. The ammoniator scrubber stack is constructed of 1/4 inch fiber- glass, 24 inches inside diameter. A 61 x 61 working platform at the building roof line already existed before the test and no modifications or additions were required to the structure. Access to the platform was provided by vertical ladders to a lower roof top and then to the ground. The ports were located 27 feet downstream from a forced draft fan and 15 feet upstream from the effluent exit point. According to Method 1, a total of 12 sampling points (6 on each axis) were selected. 19 ------- FIGURE V-3 LOCATION OF SAMPLING PORTS AHHONIATOR SCRUBBER INLET AND OUTLET 1/2" Dia Induced Draft Fan 20 ENGINEERING-SCIENCE, INC. ------- FIGURE V-4 TRAVERSE POINT LOCATIONS KILN OUTLET to Baghouse KILN STApK from Baghouse SCRUBBER INLET SCRUBBER STACK 21 ENGINEERING-SCIENCE, INC. ------- VI SAMPLING AND ANALYTICAL PROCEDURES The sample and velocity traverse points were selected as described in Section V. All participate and fluoride tests, with the exception of the ammoniator scrubber inlet, included a traverse of both axes in the stack with ten-minute sampling times at each point. Sampling data, however, was reported every five minutes, twice for each sample point. As described in Section V, the excessive quantity of water flowing down the ammoniator scrubber inlet duct necessitated sampling on only the horizontal axis. Sampling times and sequences were suggested or approved by the EPA field officer. Heavy particulate loading was experienced at times, expecially on the scrubber inlet and scrubber stack, necessitating a test shutdown, change of filter, and a test restart. This is noted in the test log in Appendix G. A. Particulate Sampling The isokinetic sampling of particulate matter was performed using an EPA approved sampling train. The probe tip in test 11-1 was changed to a smaller size in the middle of the test to keep the test isokinetic. The probe size used in calculations was a weighted average. Water was used instead of acetone for the front half wash after each particulate test. Since fertilizer is more soluble in water than acetone, a water wash would lead to a more efficient recovery of particulate from the sample train. Particulate sample catch was determined by Method 5, Standards of Performance for New Stationary Sources. B. Fluoride Sampling The sampling of fluorides was conducted isokinetically with a modified sampling train. An unheated filter holder was placed between the third and fourth impingers and contained'a Whatman No. 1 paper filter. The rest of the 22 ------- train remained the same as a standard particulate train. Sampling times were two hours with data points recorded every 5 minutes. AH fluoride catch was emptied into one bottle. Analysis consisted first of fusing insoluble fluoride with sodium hydroxide and distilling the samples from sulfuric acid to remove interferences, then a portion of the distillate was reacted with SPADNS reagent. The fluoride was determined spectrophotometrically by its bleaching effect upon the reagent dye. This procedure is described further in Appendix E. C. Ammonia Sampling Ammonia sampling was carried out non-isokinetically with the probe in- serted halfway into the stack port. Sampling times were 60 minutes with data recorded every 15 minutes. A modified sampling train was used in which the ammonia was absorbed with dilute sulfuric acid in the first two sample train impingers. The rest of the train remained the same as a standard particulate train. A modified Kjeldahl distillation procedure recovers the ammonia as ammonium borate, and subsequent titration with standard sulfuric acid solution yields the acid equivalent to isolated ammonia. This procedure is described further in Appendix E. 23 ------- |