Document zQykKp75bmr6adkzLGp4KVG23

FROM P. R. ATKINS T. B. BONNEY V. W. RIEKE TO SEE DISTRIBUTION LIST July 20, 1973 . RE: AIR SAMPLING REQUIREMENTS ------------------------------------------------------- The recent activities of EPA and OSHA and their State counterparts have resulted in increased demands for in-plant, source and ambient air sampling. Extensive testing is necessary to provide a basis for choosing the proper air pollution control techniques and designing the necessary equipment. Compliance testing is required after each control project is completed. Source testing is, or soon will be, required semi-annually or more often for all "significant" emission points. These results will have to be reported to the state agencies. Ambient monitoring, in addition to our existing fluoride sampling program, may be required in some states. Similarly, OSHA will increase its demands for in-plant sampling. At the present time only one comprehensive OSHA standard exists for which there are sampling requirements. This is the asbestos standard. On the other hand, on the present priority list there are about 450 chemical and physical agents for which comprehensive standards will be written. A look at those standards whose promulgation is imminent assures us that environmental monitoring will be a requirement in most of them. It is obvious that these sampling requirements are extensive and necessitate the formulation of a detailed manpower and resource allocation plan. Some plants may be capable of performing all the required sampling work on schedule, but many will need to make some changes. In order that we can better determine the company-wide needs, and coordinate the company's efforts in this area, please provide me with the following information by August 17, 1973: 1. A list of all routine sampling activities that occur at your plant and the schedule for these tests. Note the pollutants that are tested and briefly describe the sampling methods used. 2. A list of all emission sources that presently are not sampled routinely but in your opinion need to be sampled. Note the pollutants which should be measured. If any major problems exist which might make sampling difficult at any emission point, note this. ALCOA 409673 0054 ** >.i VDOM n Page 2 July 26, 1973 3. A list of all the remaining emission sources that you feel don't necessarily need to be sampled. 4. A description of the ambient sampling program presently maintained at your plant and your comments on how it should be improved. 5. The names, background and experience of all personnel that conduct sampling tests at your plant. Estimate the manhours required from these individuals and from super visory personnel. 6. A list of "problem areas" which you feel will require sampling equipment or expertise beyond the capabilities of your staff. The information that you submit will be used in conjunction with input from Environmental Engineering, Health and Environment and operating departments to develop a detailed plan that will insure that the company will be able to meet all the sampling requirements at every operating location. Beginning in late summer, a series of four-day short courses in air sampling technology will be offered for sampling personnel. Information from this survey will aid in the development of this short course. Your cooperation in providing as much information as possible will be appreciated. PATRICK R. ATKINS 409673 0055 THIS COPY FOR: MR. T. B. BONNEY - 7J- DISTRIBUTION LIST To: CO. / J.L. Laudenberg, Arkansas Operations R. C. Hinkle, Badin Works J. J. Thimons, Chillicothe Works E. A. Higginson, Cleveland Works B. W. Hilton, Corona Works. E. J. Schafer, Cressona Works R. J. Reitz, Davenport Works A. F. Tassaro, Lafayette Works R. C. Coleman, Lancaster Works R. Andrew, Lebanon Works J. Hicks, Logans Ferry J. W. Warnock, Marshall Works R. W. Knapp, Massena Operations R. V. Newsome, Mobile Works C. L. Green, Pt. Comfort Operations M. H-^-No-l'be-, Richmond Works B. M. Starner, Rockdale Works B. R. Hood, Tennessee Operations H. E. Chandler, Tifton Works P. F. Woodward, Vancouver Works J. R. Jones, Vernon Works R. J. Knox, Warrick Operations J. A. Thompson, Wenatchee Operations W. W. Williams, Fort Meade E. S. Howarth, Aloca Laboratories G. T. Haymaker, Rea Magnet cc: J. W. Wells, Arkansas Operations L. J. O'Connell, Cleveland Works R. H. Allen, Corona Works N. 0. Kraft, Cressona Works J. B. Dolan, Lafayette Works R. S. Howell, Lancaster Works L. E. Norris, Marshall Works J. C. Vergho, Tennessee Operations F. D. Koran, Tifton Works R, L. Parsons, Warrick Operations Info cc: Dr. M. 0. Colwell, Pghi. - 29 Mr. S. A. Jones, Pgh. - 23 Mr. A. B. Kaltwasser, Pgh. Mr. F. J. Resch, Pgh. - 18 Mr. R. W. Wrenn, Pgh. - 23 Mr. J. E. Yates, Pgh. - 24 1 409673 0056 I t FROM . R. E. PODHORA/A. A. RAMBIKUR ENVIRONMENTAL CONTROL POINT COMFORT OPERATIONS \ February 27, 1974 j TO DR. P. R. ATKINS PITTSBURGH OFFICE ^Mlr. T. B. Bonney - Pittsburgh Mr. V. W. Rieke - Pittsburgh ... Mr. A. A. Rambikur-Point Comfort Mr. C. L. Green - Point Comfort Dr. L. F. Brennecke- Point Comfort RE: AIR SAMPLING REQUIREMENTS ! In response to your letter of July 26, 1973, the following are data and comments you requested. 1. Table I shows the Point Comfort plant routine sampling activities, in cluding the pollutant, frequency of sampling and sampling method used. Included in this table are the source numbers for reference to our TACB emissions inventory for further details. 2. Table II shows emission sources that presently are not sampled, but in our opinion need to be sampled. The following emission sources do not necessarily need to be sampled at this time. a. Five stacks (POC of natural gas)- Oil & Gas Plant b. One Elevated Flare - Oil & Gas Plant Source Number 111 112 c. Smelting power individual engine exhaust stacks d. Alumina reactivator - Power Department e. Cryolite mist eliminator f. H2 emergency vent stack 114 115 169 177 g- Chlor-Alkali boilers *h. R-110 low pressure boiler 181 182 *i. R-110 boilers 1-5 193 - 197 *-Provided we remain on natural gas fuel. 4. The ambient air sampling program presently maintained is described below. ,A s r--r--t 409673 0059 arises (ftiv. n-e) 1 v- ^P"a6ge^ *2a. High volume air samples arc obtained at three locations: (1) Witco pumps (Smielting dock area). (2) Witco gate, next to the company fence along Highway 35. (3) Mr. A. A. Rambikur property. Point Comfort City. These are 24-hour samples, 4 days per week. b. One Leigh Instrument monitors ambient F- 24 hours/day (located at A. A. Rambikur property (City of Point Comfort). c. One MSA Lira Instrument monitors ambient carbon monoxide 24 hours/ day. Located at A. A. Rambikur property. .. The ambient air sampling program could be improved to include the up wind data and expanded to include ambient air monitoring around the Chlor-Alkali plant for chlorine and mercury and F around 'the A1 F3 Plant. We may need to monitor for CO in the potrooms and total oxidants to confirm State's data in Point Comfort. An estimate of manhours is shown below. See Table III for personnel data. Type of Test ______ Man Hours/Test _______ Technicians Supervisory a. Compliance dust tests Tests requiring 2 men 6-10 MH 0;5 - 1 Tests requiring 3 men 9-12 MH 0.5 - 1 b. Engineering tests, i.e., flov;s and/or particle size determination. 2 Men 6-10 0.5 - 1 3 Men c. Hg Sampling 9-12 0.5 - 1 Ambient - Cell House 6 0.5 Hg Fume Stack and H Line 7 0.5 d. Asbestos e. Smoke Opacity f. Detector Tubes 2-4 0.25 - 0.5 1-2 0.25 - 0.5 1 0.25 - 0.5 409673 0060 Page 3 g. Ind. hygiene \ h. Potroom Scrubber Towers Technicians 1-8 Supervisory 0.5 - 1 Inlet Outlet i. Potroom monitor (24 hour) 8 8 1 (set up) 0.5 0.5 0.5 j. Lab analyses (for #8 and #9) Elapsed time - 17 hours 1-2 (periodic inspection and adjustment) 4-7 0.5 - 1 ~ Compliance sampling, ambient monitoring, mercury sampling, asbestos monitoring, and engineering tests occupy the time of two Chemical Engineer ing Technicians, one-half ihe time of n Laboratory Assistant and one- half the time of three Day Analysts. 6. The Point Comfort air sampling team-has ample expertise to handle most problems with occasional advise or recommendations from environmental health lab personnel. REPrvh R. E. PODHORA P.S. I must apologize for the lateness of this response. Due to the press of other matters, your request for information was put aside and neglected. A. A. RAMBIKUR 409673 0061 TABLE I Area: Smelting Location 1. Power Department ROUTINE SAMPLING ACTIVITIES Source No. Frequency Pollutant Sampling Method Exhaust heat boilers (24) 2. Potroom Scrubbers a. Inlet 113 116 b. Outlet 3. . Monitors 117 4. Flotation Cyclone 118 5. Flotation Bag Col. 122 6. Flotation Drum Drier 190 7. Paste Plant EP 123 8. Paste Plant Bag Col. 125 9. Paste Plant #1 Air Classifier 191 10. Paste Plant #2 Air Classifier 192 11. Alumina Unloading, Building 40 126 12. Alumina Unloading Building 41 127 13. Ingot Casting a. Furnace Stacks 130 b. Skim Shed 131 14. Potlining--Shot blast collector - 54E 132 15. Marinite Collector 134 2/Year .Smoke Visual opacity, LearSiegler Transmissometer 1 2 sets towers/ quarter F & Part. Thimbles ASME 2 towers/ month F" & Part. Petrey filters & irapingers/ NaOH Soln. \ 2/Qtr. F- & Part. Petrey filters & impingers/ NaOH Soln. 2/Year Particulate Thimbles--ASME 2/Year Particulate Thimbles--ASME 2/Year Particulate Thimbles--ASME 2/Year 2/Year Particulate Thimb1e s --ASME j Particulate 2/Year Particulate Thimbles--ASME 2/Year 2/Year 2/Year 2/Year 2/Year Particulate Thimbles--ASME Alumina Dust Alumina Dust i i J j Thimbles--ASME t JIi ||Thimbles--ASME ! !I Particulate, Cl", Cl2 1'Thimbles--ASME, Impingers Particulate: 2/Year 2/Year Particulate: Asbestos 1iMSA Personal Sampler and jFilter. 409673 0062 TABLE I - continued Area; Refining Location \ \ Source No. Frequency Pollutant Page 2 Sampling Method 1. Lime Kiln Cold end (Venturi) 141 2/year Lime dust Thimbles--AS ME 2. Lime Storage 3. Bauxite Crushing (bags bad 10-24-73) 144 2/year 148 2/year Lime dust :Bauxite dust Thimbles --ASMS Thimbles--Asme > 4. Calcination a. R-50 - EP-1 b. R-50 - EP-2 *c. R-55 - EP-2 *d. R-55 - EP-3 5. Bulk Loading 151 2/year 185 2/year 186 Often 187 Often Alumina Dust Thimbles--ASME Alumina dust Thimb1e s --ASME Alumina dust Thimbles--ASME Alumina dust Thimbles--ASME ^ a. R-52 b. R-53 159 2/year 158 2/year AloOo Briquette Thimbles--ASME Dust Briquette Dust Thimbles--ASME 6. Spar Grinding Col. R81 160 2/year Spar Dust Thimbles--ASME 7. Spar Drying R81-- *Aerodyne-air tumbler 161 Often Spar Dust Brinks and Anderson Impactor--Thimbles--ASME 8. a. Spar storage R-82 top 163 2/year Spar Dust Thimbles--ASME b. Spar storage R82 grd .. 168 2/year 9. AIF^ wet scrubbers (converters) 10. #2 Hydrate drier air tumbler. i 165 I i1 2/year 166 2/year 11. #2 Nuisance air tumbler. 12. AIF3 Storage R86A a. #1 Hydrate drier air tumbler 167 ' 2/year i 183 : 2/year 1 188 ; Often b. irl Nuisance air tumbler 189 Often j Spar Dust Thimbles--ASME i ! -jParticulate, HE Thimble--ASME, Impingers i j Hydrate Dust Thimbles--ASME i Hydrate Dust i or AIF3 1 AIF3 dust l i j Hydrate 1 I Hydrate or AIF3 Thimb1e s --ASME Thimble--ASME Thimble--ASME Thimble--ASME ^-Numerous Engineering Tests 409673 0063 TABLE I - continued Page 3 Area: Refining Location 13. Cryolite Source No.; Frequency Pollutant Sampling Method a. Fluid drier venturi 170 b. Fine collector 171 c. Pelletizer Col. 172 d. Pelletizer drier venturi 173 14. Chlor-Alkali 2/Year 2/Year 2/Year 2/Year Cryolite dust Thimble - ASME Cryolite dust Thimble - ASME Cryolite Dust Thimble - ASME Cryolite Dust Thimble - ASME > a. Hg vapor stack 178 1-2/Week Hg EPA with Alcoa impinger train. | H2 line to R-110 powerhouse - 1-2/Week Hg - c. Cell house ambient air. - 1-2/Week-- Hg EPA with Alcoa impinger train. Cell house traverse with mini-impingers. 409673 0064 Area: Refining; TABLE II EMISSION StlURCES THAT NEED TO BE SAMPLED J Location Raw Materials Source No. Pollutant Remarks a. Bauxite unloading (fugitive) b. Bauxite transfer (fugitive) c. Bauxite storage (fugitive) d. Bauxite Storage R-25N R-25S Chlor-Alkali Diamond Snift vent stack Chlor Alkali Hypo Unit Paste Plant Fume Stack 145 Bauxite Dust Sometime in future, dust collection must be provided. 146 Bauxite dust Sometime in future, dust collection must be provided. 147 Bauxite dust Sometime in future, dust collection must be provided. 149 Bauxite dust Revise existing collector. 145 Bauxite dust Revise existing collector. 179 cci4 & ci2 3" diameter vent line off the absorber and normally runs at 80 - 90 psi. 180 NaOH Mist, Cl2 Intermittently used for Cl2 NaOH Mist continually. 124 Carbon dust Thimbles - ASME,'Alcoa 4070 and Hydro carbons 409673 0065 TABLE III PERSONNEL: BACKGROUND. EXPERIENCE Name & Statistics Tom Flores Age: 38 Co. Sen. 18-1/2 years College: 2 years Reports to A. A. Rambikur E. A. Brogger Age: 37 Co. Sen. 15 years College: No Assigned to Lab Background Environmental Experience Potrooms, Casting Since February, 1968, Chem. Engr. Lab, Quantometer Technician. Development of dust Lead Analyst, 10 Years, testing, air sampling, industrial hygiene sampling. Qualified smoke reader. Qualified asbestos analyst. ^ Lab - Process Control Bath Lab, Oil Lab, Quantometer Since mid-1968, water analyses, Hg sampling, ambient and stack Bay solids/Hg, urine analyses, vege tation samples, industrial hygiene hi-volume air, Leigh instrument. Lira CO-monitor. R. L. Nolen Age: 39 Co. Sen. 15 years College: 4 Hours Chem Assigned to Lab Paste Plant lab. Power Maint. Lab Process Control, Chlor-Alkali Lab, vac. relief and Lead Analyst. Since June, 1969, water analyses, Hg sampling - ambient and stack Bay solids/Hg, urine analyses, industrial hygiene, hi-vol. air, .Leigh instrument. Lira C0-Monitor. L. F. Wagner Age: 41 Co. Sen. 17 years College: No Assigned to Lab L. W. Onken Age: 31 Co. Sen. 8-1/2 years College: 1 + years Reports to A. A. Rambikur Texas Hiway Dept. Sur veyor, Supply School, U. S. Army. Surveyor Alcoa Const. 7th pot line, Refining Plant, Warrick Operations. Lab 1959, Jr. Analyst, Bath Lab. Since June, 1969, water analyses, Hg sampling, ambient and stack Bay solids/Hg, urine analyses, indus trial hygiene, Hi-vol air., Leigh Instrument, Lira Co-Monitor. Lab - Process Control Chlor-Alkali Lab, Quantometer, AlFg task force. Ft. Meade Plant, Florida. Since October, 1973, Chem. Engr. Technician. Dust testing. Quali fied smoke reader. Qualified asbestos analyst. E. A. Kozelskv Age: 27 Co. Sen. 6 Years College: 1 + years Assigned to Lab U. S. Marines, Supply. Lab--Process Control sampler. Storeroom. Lab--Process Control Since January 15, 1974, effluent sampler. Dust test sampling assistant. R. J, Putnam Age: 26 Co. Sen. 5 + Years College: 2 Years Assigned to Smelting Roughneck--oil fields. Computer - bank Office - Invoice. Lab Assistant. Cathodic Protection. November, 1969, Process Engr. Tech. (Smelting). Potroom scrubber tower testing. Potroom monitor testing. See H. E. Bonds' letter 1-9-74. Re: Environmental Tests & Inspection (not included) 409673 0066 *1 4 FROM j. D. BREAZEAL ENGINEERING & MAINTENANCE DIVISION DAVENPORT WORKS September 13, 1973 TO P. R. ATKINS HEALTH & ENVIRONMENT DEPARTMENT PITTSBURGH OFFICE - 7 C. C. to; V. W. Rieke - Pittsburgh Office 7 UT..B. Bonney -Pittsburgh Office 7 R. J. Reitz - Davenport Works K. Williams - Davenport WWoorks RE: AIR SAMPLING REQUIREMENTS In response to your July 26, 1973 memo to R. J. Reitz, Safety and Environ ment Steering Committee Chairman, on the captioned subject we are forwarding the attached "Information" sheets. These attachments contain information on the six subjects requested, numbered to correspond to the questions in your July 26 letter. Our in-plant and stack sampling program is progressing at a slow rate, due primarily to a lack of trained manpower. We hope to take full advantage of any short courses in sampling technology offered by the company as mentioned in your letter. JDB/11 Attachments (4) J. D. BREAZEAL 409673 0074 F*49e (rv. i *-co) TO: P. R. ATKINS September 7, 1973 Information - Sampling Requirements \ I. List of all routine sampling activities: No in-plant or stack sampling is done on a routine basis. Sources and areas are only checked when there is a specific need or request. Operations or areas that have been sampled at least once are as follows: Stack Sampling Ingot Melting & Holding Furnaces - Particulate, Beryllium, Solid Waste Incinerator Hcl & Cl2 Gas - Particulate Foil Rolling Mill Exhausts - Particulate Hill Acme Polisher Scrubber Exhaust - Particulate Skim House Rotary Barrel Stacks - Particulate, Beryllium Skim House Dust Collector Stack - Particulate, Beryllium In-plant Sampling: Ingot Plant - Beryllium, Cadmium, Chlorine, Hcl, SO Hot Line - Oil Mist Vapors Cold Mills - Oil Mist Vapors Foil Mills - Oil Mist Vapors Preheat & Reheat Furnaces - Fluoride Fume, Carbon Monoxide 1A. Sampling Procedures - Stack Samples a. Pitot tube measurements taken to determine velocity profile, CFM, and sampling position. b. Sample collected using glass probe, Petrey filter holder and glass fiber filter, impingers (where required), gas meter, and vacuum pump. c. Analysis of samples. c-1. Beryllium samples are forwarded to Industrial 409673 0075 Hygiene Laboratory--A'lcoa Technical Center, TO: P. R. ATKINS September 7, 1973 -3 - for analysis. c-2. Samples Ifrom Ingot Plant operations are analyzed according' to "Method for Sampling and Analyzing Stack Effluents from Chlorine - Fluxing Opera' tions" received from T. B. Bonney (copy attached). c-3. Particulate emissions from other sources deter mined from weight gain of dry glass fiber filters. II. List of sources that have not been sampled but that need to be checked Stack Samples Paint Line Foil. Rolling Mills Cold Rolling Mills - Hydrocarbons - Hydrocarbons - Hydrocarbons Laminator Bay Stacks - Hydrocarbons 60" Process Line (Solvent Cleaning) - Hydrocarbons 84" Process Line (Solvent Cleaning) #4 Tension Level Line - Hydrocarbons (Solvent Cleaning) - Hydrocarbons Melting & Holding Furnaces - Opacity or Ringleman number In-plant Sampling - first (or additional samples required) Ingot Plant - Check for asbestos, beryllium, nuisance ducts, Cl2 & I'.cl gas, metallic chloride fumes, fluo ride fumes (from fluxes, skim pots, & proces sing) sulfur dioxide, carbon dioxide, cadmium (2021 alloy) copper oxide dusts, phosphate ester fumes. 409673 0076 'TO: P. R. ATKINS September 7, 1973 4 Hot Rolling Area - Soluble oil mist and fumes, phosphate \ ester fumes. j Plate Mill Area - Oil fumes from sawing operation, 1,1,1,- trichloroethane vapors, ozone. Furnace Department - Carbon monoxide, smoke. Sheet Finishing - Solvent vapors. Paint Line - Fluoride mists, chromate mists, solvent fumes. Cold Mills - Oil mists & fumes, nuisance dusts in filter houses. I. P. S. - Solvent vapors, vapors from TEC chemical stripable coating-799. Foil Mill - Solvent fumes, oil mists, paper dusts, carbon monox ide, nuisance dusts in filter house. Machine Shop - Ozone in welding area. III. List of remaining sources that don't need sampling: Foil Annealing Furnaces - 8 Preheat Furnaces - 9 Reheat Furnaces - 19 Soaking Pit Exhausts - 26 Ageing Furnaces - 2 IV. Description of ambient sampling program: --none, with present regu lations, there is no apparent need for an ambient sampling program. V. Names, background, and experience of sampling personnel: Actual stack samples are collected and analyzed by one or more chemical analyst from Chemical Laboratory. These are hourly employees with no specific training other than that obtained by experience in the laboratory. Supervision: K. W. Williams, Laboratory Supervisor, B.A. Degree, major in biology, no formal training in stack sampling, 15+ years experience in Davenport Chemical Laboratory. 409673 0077 TO: P. R. ATKINS September 7, 1973 5- M. K. Sqnksen, B.S.M.E., no formal training in stack sampling.procedures. Man-hours required vary depending on the testing required. Example: 3 sets of Ingot stack samples require 16 man-hours for sampling, 8 hours for analytical work, 2-4 hours laboratory supervision, and 1-2 hours engineering time. In the last half of 1972 a total of 640 hours were spent in collecting and analyzing stack samples, not including supervisory or engineering time. VI. "Problem Areas" that will require expertise or equipment beyond Davenport's capabilities: 1. Collection and analysis of hydrocarbon samples. 2. Determination of quantity and identification of solvent vapor fumes. 3. Beryllium analysis - currently done by Technical Center, Merwin. 4. Determination of fluoride fumes. 5. Need for a trained technician to arrange and supervise sampling and write up reports on results. MKS;11 M. K. SONKSEN 409673 0078 METHOD FOH SAMPLING AND ANALYZING STACK EFFLUENTS 1, Scope FROM, CHLORINE-FLUXING OPERATIONS ' 2 * Tile method covets sampling and analysis of particulate and gaseous effluents from stacks exhausting chlorino-fluxing operations. The components are principally HC1, CI2. AI2O3 and AICI3 (or AI2O3 with adsorbed 11C1), ns gases, aerosols and particulate.' Some of theso are not specifically identified but all arc accounted for. There is a separation of particulate from gaseous components and these are analyzed separately. For convenience, the particulates are reported ns AI2O3 nnd IIC1. . ' ..' . - .. Summary of Method .A - - . .. * J ." 2.1 A measured volume of the effluent stream is sampled through a filter paper to separate particulates, then through n solution of 6odium . hydroxide to absorb chlorlno and hydrogen chloride gases. " 2.2 The filter retaining particulates is nnalyzod for aluminum oxide gravimetrically, and for total chloride as HC1 by titration after leaching from the filter into, solution. 2.3 The liquid irapingcr sample is analyzed for chlorine by titration . of an aliquot portion. Another aliquot is nnnlyzed for chlorides, and the titration obtained includes the chlorine present in the sample. . Subtraction of the UC1 equivalent of CI2 present from the chloride ' titration gives the chlorides prosent as HC1. NOTE: The Mohr titration is presented in this method for chloride ' determination. The Yolhnrd titration is also acceptable and may be used at the chemist's discretion. The chloride specific ion electrode is also recommended and its use is briefly described in an appendix. - 3. Sampling Apparatus ' .3.1 Sampling Probe. Use a borosiliente glass tube (Vycor is required for temperatures above 500C) of 10-12 mm I.D. and long enough to reach the appropriate sampling point with about one foot outside the stack to cool the gases enough to prevent charring tho filter. This tube should have a 90 bond of ca.2-inch radius on tho inlet end. 3.2 ' Potrey Filter Holder. Holds 12.5 cm din. filter paper. Whatmon #42 is used. V* 3.3 Grccnburg-Smlth Standard Impingcrs. 500 ml capacity. Two required. 3.4 Metering Povlco. Sprnguo dry gas meter or oquivnlont. Must bo calibrated and include a dinl thormomotor and vacuum gauge for correcting volumes to otandnrd conditions. 3.5 Vacuum Source. Willson or Cast pump, air ejector, or equivalent, capablo of pulling 1/2-1 CFM thr.ough tho sample train. 409673 0079 I 3.6 Pilot Tulio nnd Draft Gnugo for determining stack velocity 2 3.7 Thermometer or Thermocouple (range to 1500*F) for determining duct -or stack tcinperapuroa. ., ' 3.8 v.'nlkio-Tnlkics for communicating with sampling coordinator at the furnace. .. ' . . ... . .... .. x ;. 3.D Stop-Watch 3.10 Data Sheets . '. - *' -V . ' ' ' 4, Analytical Hengents 4.1 Sodium Hydroxide (NaOH), IN; diusolvo 40 g of NaOH pellets in H2O nnd dilute to 1000 ml. . it ' 4.2 Sulfuric Acid (II2SO4), 0.01H; add 3 ml of II2SO4 (sp.gr. 1.84) to 1120 nnd dilute to 1000 ml. 4.3 Sulfuric Acid (H2SO4), 2N; add 60 ml of H2SO4 to H2O end dilute to 1000 ml. .. v .. . ., 4.4 Potassium Chromate indicator (K2Cr04).dissolve 10 g K2Cr04 in 100 ml II20. 4.5 Potassium Iodide (KI), crystals 4.6 Hydrochloric Acid (IIC1), 4K; add 50 ml HC1 (sp.gr. 1.1B) to 100 ml Vr: h2* . .. ` .. 4.7 Sodium Thiosulfate (Na2s23-5Il2J 0.1N; dissolve 24,819 g Na2S203.51120 in II2O and dilute to ono liter. 4.8 Silver Nitrate (AgN03), 0.1N; dissolve 16.989 g AgN03 in H2O and diluto to 1 liter. Standardize with Sodium Chloride. 4.9 Starch Indicator (Soluble Starch); mix 1 g soluble starch into a paste in 5 ml H2O with a mortar nnd pestle. Rinse into 100 ml hot JI20 au(* hoil 3 min. (Substitutes may also bo used for indicators in iodinctry. Thyodenc is recommended.) 4.10 Ammonium Hydroxide (NU4OH); sp.gr. 0.899. 4.11 Methyl Red Indicator Solution, 0.04%; dissolve .1 g of Methyl Red in 10.6 ml 0.02N NaOH, diluto with H2O to 250 ml. 4.12 Phcnolphthalein Indicator, 0.1%; dissolve 0.1 g in 60 ml alcohol and Slluto with H2O to 100 ml, ' . .m.';:,.- .-.-- '. 4.13 Nitric Acid (HN(>3> ; 'sp.gr, 1.41.' : 409673 0080 4*14 Ar.nnoulinn NUrnto Wash Solution; dilute 20 ml Nib; OH, up.nr. 0.800, with HoO, neutralize using Methyl Hctl with 1:1 IIHO3, add 1 ml excess NlI.jOH (sp.gr, 0,800) and diluto to 1000 ml. \ 4.15 Sodium Chloride (NnCl) 0.1N; diusolvo 5.845 g KaCl in H20 and diluto to 1000 ml. .j Sampling Procedure 5,1 Determine velocity and volumetric flow rato of stack gases (Ref. Mothod 4070.5.2) . 5.2 Choose sampling loention. The ideal location is 5 to 10 diameters downstream from any bend, branch, or blower, and 3 to 5 diameters upstream from similar causes of turbulence. Since this is usually non-existent, an optimum location is determined .by surveying several profiles at available locations. The most uniform profile marks the best location. From the profile obtained'and the average velocity calculated choose for sampling that point which is nearest the average velocity. \ 5.3 Collecting the Sample. - 5.3.1 Determine the sampling rate by roforring the average velocity .-.above to the chart. (Fig. 9.2) '5.3.2' Duration of the test is dotormined by the operation. Sampling .. should continue through a coraploto cycle, including fluxing ' nnd skimming. 5.3.3 Assemble tho equipment (See Fig. 9.1) ' Load the filter holder with 12.5 cm diameter Whatman U42 filter paper and connect to two standard impingers, each containing ; 100 ml IN NaOH and protected from dust by .covering the ground `.'.. joint with masking tape. Plnco the gas meter neat between the sample train and the suction source, and control the flow rato with a screw clamp on tho meter outlet hose. 5.3.desampling procedure. . ^.a.4.1 Check system for leaks before sampling by blocking the nozzle and applying about 10 in. mercury vacuum. Close the clamp K nnd, if the vacuum holds, relense .tho nozzle slowly nnd proceed with sampling. A drop in vncuum indicates a leak, which must be corrected. y-5.3,4.2 Insert campling probo at tho proper location (5.2), '.j; directing the nozzle into the gas stream with the clamp 'K closed. Start tho vacuum source and open the clamp to tho desired flow rate (5.3.1). This rate should bo observed and adjusted as frequently as necessary 'X1 throughout the entire sampling period, noting time, . . tempornturo, and pressure for each change. At tha 'end of tho sampling period, tho filter holder and ': iraplngoro arc scaled to avoid contamination or loss `' whilo transporting to tho laboratory. ? i . V.- S ;T` . . i-i\ 409673 oosi 6. Analysis of Samples G.l Filter sample ' 6.1.1 Transfer paper to a beaker, brushing or washing any ^ residues from inside the holder (3.2) nnd sampling .* probe (3.1), adding enough water to cover the paper. Add 3 drops Methyl lied indicator nnd NH4OII (4.10) until just alkaline, bring to n boil and filter through Whatman #40 paper, or equivlcnt, into a 250 ml volumetric flask. Wash with hot NU4NO3 wash solution (4.14). Cool, diluto to 250 ml, mix, and set aside for determination of ' : 11C1. : 6.1.2 Place the paper containing washed precipitate in a tnred crucible and ignite at 1000C for ono hour. Cool and- '.weigh. Record the increase in weight as AI2O3 (retain tho residue for analysis of minor constituents, if needed).. .6.1.3, Calculation of AI2O3 concentration AI2O3, mg/m3 = where: v Wn c Hct weight of AI2O3 in mg V = Volume of gas sample in cubic meters S.T.P. : (25<'C, 760 Torr.) _6.1.4 Transfer, a 50 ml portion of filtrate (6.1.1) into a .' 'casserole, add 3 drops phenolphthalein indicator (4.12) and H2SO4 (4.2) until just acid. Add a few drops of l^CrO^ indicator (4.4) and titrate with 0.1N AgNC>3 (4.8) , y; to the first color change from pure yellow. Deduct a .;. determined blank. . 6.1.5 Calculation of 1IC1 concentration vv.-. V Total wt. 1IC1, mg = Tn x N x 36.5 x A.F. * ' Cone. HC1, mg/m3 = wt. IIC1, mg/V . .' Cone. 1IC1, ppm mg liCl/a? x 0.670 Tn H ,36.5 A.F. V 0.670 net ml AgR03 titer normality AgNC>3 m.e.w^ci aliquot factor ml total volume] \50 ml aliquot sampled vol. in m3 S.T.P. conversion factor mg RCl/m3 to ppm 1-v 6.2 ' Impingcr Samples o ,' 6.2.1 Transfer contents and washings of both impingers into -2&0 -' '. ml volumetric flasks and make up volume with water. - . 6.2.2 Chlorine. Pipet n -H>- ml aliqviot (the aliquot amount depends '.V.-. -,on concentration in tho sample) in a 250 ml Erlenncycr V .; o 7^ V ' flask and add 5 g KI crystals (4.5) and 5 ml 4.N 11C1 (4,6). Titrate with 0.1M KaoS203 solution (4.7), using starch , indicator (4.9) ns tho end point approaches. Deduct a determined blank. 6.2.3 Calculation of Chlorine concentration ; wt. Clj, mg Tn x N x 35.5 x A.F. cone. Cl2 mg/m3 CIt# mg/V,m3 ppm CI2 *> Cl2> mg/in3 x 0.689 'V: whore: Tn " not ml Na2S203 titer N * normnlity Kn2S203 .. 35.5 " m.o.w CI2 A.F. " aliquot factor (250/ samplod vol. S.T.P. 0.609- conversion Cl2. mg/; to ' 409673 0082 6 6,2,4. l'oul' Clilor iilo. J'lpet n -16-ml aliquot (nll(|iioL nnount depends on concent ration in the sample) into a 250 ErnlcJimeyer flask and add 23 ml NII^OIl (4.10) to reduce chlorine to chloride. Add 5 gl'nss bends and boll vigorously to remove excess ammonia. Add 3 drops phenolphthalein indicator (4.12) and l^SO^ (4.2) until Just acid. Add a few drops of K^Cr&i indicator (4.4) and titrate with O.lJf AgNCP} (4.8) to the first color change from yellow. Deduct a determined blank. 6.2.5 Cftlculfttion of Total Chloride ns HC1. The samo calculation procedure as in G.1,5; is used with tho possible exception of tlic aliquot factor. In the cxamplo used a 5 ml aliquot- 'of the total 250 ml sample solution is used. The factor therefore would be 250/5 or 50. 6.2.6 Calculation of Hydrogen Chloride. Convort the wt. of. chlorine found in 6.2.3 to its JiCl equivalent nnd subtract , -from the total chloride weight found in 6.2.5. conversion CI2 to 11C1: Cl2i mg x 1.03 HC1, mg whore; m.c.w. JIC1 (36.5) m.o.w. CI2 (35.5) , \ )1C1 in sample, mg = Total Chloride as HC1, mg - HC1 equiv. of chlorine,m ' Concentration lid, mg/m3= HC1, mg/V,m3 Concentration HC1, ppm = HC1, mg/m3 x 0.670 ' whore: V * sampled volume (m3 S.T.P. 0.670 m conversion mg HCl/m3 to ppm HC1 . 6.3 See appendix 8.1 for use of specific ion electrode Report of Data Date of test, sample number, sampling location Operation, alloy processed, duration of fluxing Average stack temperature, C Stack gas volume, m3/min. at S.T.P. (25C nnd 760 torr.) Results:. Aerosols - total AI2O3 mg/m3 . - IIC1 mg/m3 Gas . - Chlorino . . mg/m3 and ppm ' ' ' ' : HCl Hass Emission;- total .Vy v; mg/m3.;'-. 409673 0083