Document a1JYzBxeQZQeVbJmvLVqEo89e

t ^vk>r. MANUFACTURING CHEMISTS ASSOCIATION 1825 CONNECTICUT AVENUE, N W. WASHINGTON, D C 20009 (202) 483-6126 April 10, 1973 t /U c<n To: AIR QUALITY COMMITTEE JOINT SUBCOMMITTEE ON ENVIRONMENTAL LAW / Subject: Emission Standards for Hazardous Air Pollutants__________________ Gentlemen: Distributed herewith are copies of the emission standards for beryllium, asbestos, and mercury issued by EPA pursuant to section 112 of the Clean Air Act, as amended. These are the first standards to be promulgated under this authority. Although other pollutants are under study for possible inclusion in an extension to the initial list, EPA has not announced any intention of, or schedule for, such additions. Sincerely, KDJ:mb Attachment Distribution "C" Kenneth D. Johnson, Ph.D. Assistant Technical Director Air Quality 010784 S'S'.'O RULES AND REGL'IAT.'O'IS Title 40--Protection of Environment CHAPTER 1--ENVIRONMENTAL PROTECTION AGENCY SUBCHAPTER C--AIR PROGRAMS btane* lining the chest ar.d abdomen <30-47). There are reports of mesotheli oma associated with nonoccupational exposures in the neighborhood of as bestos sources (33, 42, 47, 48 >. An out it is necessary to control emissions from major man-made sources of asbestos emissions into the atmosphere, but that it is not necessary to prohibit all emissions. ` PART 61--NATIONAL EMISSION STAND ARDS FOR HAZARDOUS AIR POLLUTANTS standing feature has been the long period, commonly over 30 years, between In this determination, the Administra tor has relied on the National Academy Asbestos, Beryllium, and Mercury On March 31, 1971 (36 FR 59311. pur suant to section 112 of the Clean Air Act. as amended, the Administrator published an initial list of three hazardous air pol lutants which, in his judgment may rause. or contribute to. an increase in mortality or an increase in serious ir reversible. or incapacitating reversible, the first exposure to asbestos and llie ap pearance of a tumor (49, S0>. Tnere is evidence which Indicates that mssoUtliomas occur after much less exposure to asbestos dust than the exposure associ ated with asbestos (51, 52). It is not practicable, at this time, to establish allowable numerical concentra tions or mass emission limits for asbestos. Satisfactory means of measuring ambient of Sciences' report on asbestos (5J i. which concludes; 'htsbestps is. too im portant in our technology and frtjppmY for its essential use to be stopped. But. because ol the known serious etfeccs of uncontrolled inha'lation~of asliestos min erals in industry and uncertainty' as to the shape and character of the doseresponse curve in man, it would be highly" imprudent to permit additional ranumi- illness. The pollutants were asbestos, asbestos concentrations have on!./ re nation of the public environment with ^ervlhum. and mercury. On December 7, cently been developed, and satisfactory asbestos. Continued use at minimal risk 71971 (36' FR 232391, the Administrator means of measuring asbestos emissions to the public requires that the major proposed standards for these pollutants. are still unavailable. Even li saasfactory sources of man-made asbestose emission Interested persons participated in the means of measuring asbestos emissions into the atmosphere be defined and con rulemaking by giving testimony at public did exist, the previous unavailability of a trolled." hearings and by sending comments to satisfactory means of measuring ambient The means of control used are limita EPA. Public hearings were held in New levels of asbestos makes it impossible to tions on visible emissions with an option York City on January lu. 1972. and in estimate even roughly the quantitative in some cases to use designated control Los Angeles on February 15 and 16, 1972. relationship between asbestos-caused ill equipment, requirements that certain A third hearing, scheduled to be held ness and the doses which caused those ill procedures be followed, and prohibitions in Kansas City, on February 1, 1972, was nesses. This is a major problem, since on the use of certain materials or of cer canceled because of a lack of requests to some asbestos caused illnesses have a 30- tain operations. These means of control participate. Sixty-eight persons gave year latency period. are required because of the impossibility testimony at the public hearings, and 56 EPA considered the possibility of ban at this time of prescribing and enforc persons sent comments to EPA. Repre ning production, processing, and use of ing allowable numerical concentrations sented were industries, universities, gov asbestos or banning all emissions of as or mass emission limitations known to ernmental agencies--Federal, State, and bestos into the atmosphere, but rejected provide an ample margin of safety. The local, and environmental groups. Copies these approaches. The problem of meas alternative of no control of the sources of the public hearing records ore avail- uring asbestos emissions would make the subject to this standard was rejected able at all EPA Regional Oifices and at latter approach impossible to enforce. because of the significant health hazard the Division of Stationary Source En Either approach would result In the pro of unregulated emissions of asbestos into forcement, room 3220. 401 M Street 6W,, hibition of many activities which are the atmosphere from the designated Washington, D.C. 20460, where copies of extremely important; moreover, the major sources. the comments received are also available. available evidence relating to the health It is the Administrator's Judgment The bases for the Administrator's de hazards of asbestos does not suggest that that the asbestos sources subject to this terminations that asbestos, beryllium, such prohibition is necessary to protect standard are the major sources of as and mercury are hazardous, the deriva public health. For example, demolition of bestos emissions. In the absence of quan tions of the standards now adopted, the any building containing asbestos fire titative emission data, the Administra Environmental Protection Agency's re proofing or insulating materials would tor's Judgment was based on an national sponses to the significant comments received, and the principal revisions to the proposed standards are summarized below. A more detailed statement is available on request from the Emission Standards and Enginering Division, En vironmental Protection Agency, Re have to be prohibited as would the use of materials containing even trace amounts of asbestos which could escape into the atmosphere. Finally, the available evidence suggests a gradient of effects from direct occupa tional, to indirect occupational exposure, Inventory of sources and emissions of asbestos (54) and other reports (53, 55). The asbestos emissions and emission factors presented in the national inven tory were based on information obtained from production and reprocessing com panies. This Information Included pro search Triangle Park, N.C. 27711, Atten tion: Ur. Don Goodwin. In addition, the Administrator Is Issuing information on control techniques for asbestos, beryl lium, and mercury as directed by section 112(b) (2) of the act. Copies of these documents may be obtained free of charge from EPA Regional Offices. to families of workers exposed to asbestos and persons in the neighborhood of as bestos tources--in all of which situa tions asbestos concentrations are un doubtedly high by comparison with most community air. This suggests that there are levels of asbestos exposure that will not be associated with any detectable risk, although these levels ere not duction figures, estimates of control . equipment efficiency and material bal ances: it did not include emission test results. The major sources of asbestos emissions were considered to fall into five categories: (1) Mining and milling; (2) manufacturing: (3) fabrication; (4> de molition; and (5) spraying. In deter mining which of these major sources Asbestos known (53). should be covered by the standard pro Asbestos is a hazardous air pollutant It is probable that the effects of as mulgated herein, the Administrator con within the meaning of section 112. Many bestos inhalation are cumulative; tha t Is. sidered the effect other Federal regula persons exposed to asbestos dust de low-level and,'or intermittent exposure tions will have on the emissions from veloped asbestosls when the dust concen to asbestos over a long time may oe such sources and the proximity of such tration was high or the duration of ex posure was long (1-71. A large number of studies hnve shown that there is an association between occupational ex equally as Important in the etloijgy of asbesiotir disease as high level and/or continuous exposure over e shorter pe riod. On the other hand, the available sources to the public. In addition, the Administrator considered comments on the proposed standard and additional technical data not available before pro posure to asbestos and a higher-tlian- evidence does not Indicate tha: levels posal. The following paragraphs explain expectcd incidence of bronchial cancer of asbestos in most community air cause these considerations and the changes (3-30). Asbestos also has teen identified asbestotic disease. Taking both these made to the standard between proposal as a causal factor In the development of considerations into account, the Admin and final promulgation. mesotheliomas, cancers of the mem- istrator has determined that, in order to The promulgated standard applies to provide an ample margin of safety asbestos mills, selected manufacturing Rc.'erences at end of article. protect the public health from a'bcstos. operations, the use of spray-on asbestos Fcc:c*.l fCG'.TC. vc. 33, ;io cc-- '.".m 6. 1C73 -010785 "I'lCS AND REGULATIONS Sn'JI n..i!er.a).s. demolition operations. av-i U'.e mr.-suns t.ikcn to comply with tiiv ii'i- Viio prop i.-ed s'andaij \ .luiU hate surfacing of roadways with asbestos laii- re.tu of Minos and Occupational Safety lirr.icri emissions Irom a '.unii.'tr of ir.,,s. The Administrator u si 1 continue to and Health Administration regulations to souices by stipulating tha; such emis investigate other existing and new protect the health of persons who v.ork sions could not exceed the amounts which seiirces of asbestos emission and if any in proximity to dumps and open storage would be emitted from the source .f the of them are found to be major sources, arcus will prevent the dumps and storage source were equipped with a fabric filter, the standard will be revised to coscr areas from being major sources o! asbes or, in some cases, a wet-collection air- them. tos emissions. c'caiung device. This would have required As applied to mines, the proposed The proposed standard would have ap a standardized emission-measuring tech standard would have limited the emis plied to buddings, structures, or facilities nique. which is not currently available. sions from drilling operations and pro wi'-lnu which anv fabricating or nianu- The promulgated standard prohibits visi filin'cd visible emissions of particulate Jhctnrmg operation is carried on which ble emissions which contain asbestos and matter from mine roads surfaced with invoices !he use of asbestos materials. provides the option of using specified asbestos tailings. The Bureau of Mines Comments received on the proposed air-cleaning methods. T.'ie existence of lias prescribed health and safety regula standard indicated that the requirements particulate asbestos material in a gas tions (30 CFR 55.5) for the purpose of for fabricating and manufacturing oper stream vented to the atmosphere can be protecting life, the promotion of health ations were confusing. Much of the con determined by collecting a sample on a and safety, and the prevention of acci fusion was created by the use of terms ulcer and analyzing it by microscopy dents in open pit metal and nonmetallic such as "any," "continuously," and techniques. The proposed standard stated mines. As related to asbestos mines, these "forced gas streams." The promulgated that the air-cleaning requirement would i emulations prohibit persons working in standard is more definitive as to applica nut be met If a number of listed faults, a mine from being exposed to asbestos bility of the provisions. The promulgated e g., broken bags, leaking gases, thread concentrations which exceed the thresh standard prohibits visible emissions from bare bags, existed and it required that old limit value adopted by the American the nine manufacturing operations collection hoppers on some ba&houses be Conference of Governmental Industrial which, in the judgment of the Adminis emptied without generating visible emis Hygienists. The regulations specify that trator, are major sources of asbestos. The sions. Comments received suggested that respirators shall not be used to prevent promulgated standard does not cover this negative approach tended to make persons from being exposed to asbestos fabrication operations. Of all fabrication the quality of air-cleaning operations de where environmental measures are avail operations, only those operations at new pendent upon the ability of EPA to an able. For drilling operations, the regula construction sites are considered to be ticipate and to Include in the standard tions require that the holes be collared major sources of asbestos emissions. The all the factors which would constitute and drilled wet. The regulations recom Occupational Safety and Health Admin improper methods. Since the Intent was. mend that haulage roads, rock transfer istration regulations specify that all and is. to require high quality air-clean points, crushers, and other points where hand- or power-operated tools (l.e. saws, ing operations, the promulgated standard dust (asbestos) is produced sufficient to scorers, abrasive wheels, and drills' requires proper installation, use. opera cause a health or safety hazard be wetted which produce asbestos dust be provided tion. and maintenance without precisely down as often as necessary unless the with dust collection systems. In the judg defining the means to be used. dust is controlled adequately by other ment of the Administrator, implementa The proposed standard would have means. In the judgment of the Admin tion of these regulations will prevent prohibited the spraying of any material istrator, Implementation of these regu fabrication operations from being a containing asbestos on any portion of lations will prevent asbestos mines from major source which must be covered by a building or structure, prohibited the being a major source which must be cov the standard promulgated herein. spraying of any material containing as ered by the standard promulgated here The proposed standard would have bestos In an area directly open to the in. Furthermore, the public is sufficiently prohibited visible emissions of asbestos atmosphere, and limited emissions from removed from the mine work environ particulate material from the repair or ail other spraying of any material con ment that their exposure should be sig demolition of any building or structure taining asbestos to the amount which nificantly less than that of the workers other than a single-family dwelling. would be emitted If specified air-cleaning in the work environment. Accordingly, Comments indicated that the no visible equipment were used. Comments re the promulgated standard does not apply emission requirement would prohibit re ceived pointed out that this standard to drilling operations or roadways at pair or demolition in many situations, would: (1) Prohibit the use of materials mine locations. since it would be Impracticable, if not containing only the trace amounts of For asbestos mills, the proposed stand impossible, to do such work without cre asbestos which occur in numerous nat ard would have applied to ore dumps, ating visible emissions. Accordingly, the ural substances. (2) prohibit the use of open storage areas for asbestos materials, promulgated standard specifies certain materials to which very small quantities tailings dumps, ore dryers, air for proc essing ore, air for exhausting particulate material from work areas, and any mill ing operation which continuously gen erates inplant visible emissions. The work practices which must be followed when demolishing certain buildings or structures. The standard covers institu tional, industrial, and commercial build ings or structures, including apartment of asbestos are added In order to enhance tliclr effectiveness, and (3) prohibit the use of materials In which the asbestos is strongly bound and which would not gen erate particulate asbestos emissions. The promulgated standard prohibits visible emissions from any part of the mill, but It does not apply to dumps of asbestos tailings or open storage of asbestos ores. The Bureau of Mines' regulations pre houses having more than four dwelling units, which contain friable asbestos ma terial. Tills coverage is based on the Na tional Academy of Sciences' report (5J> whien states, "In general, single-family promulgated standard applies to those uses of spray-on asbestos materials which could generate major emissions of paniculate asbestos material. For those spray-on materials used to Insulate or viously referenced and regulations issued residential structures contain only small fireproof buildings, structures, pipes, and by the Occupational Safety and Health amounts of asbestos insulation. Demoli conduits, the standard limits the asbestos Administration (20 CFR 1910.93a) pro tect workers from the hazards of air con taminants In the work environment. The Occupational Safety and Health Admin istration regulations were promulgated on June 7. 1972. The regulations are in tended to protect the health of empioj ecs from asbestos exposure by means oi en gineering controls (i.e. Isolation, enclo sures, and dust collection) rather than by personal protective equipment. It is the tion of industrial and commercial build ings that have been fireproofed with asbestos-containing materials will prove to be an emission source in the future, requiring control mea'.ures." Apartment houses with four dwelling units or ,ess are ccr-ulered to be equivalent to single- familv residential structures. The stand ard requires that the Administrator be notified at least 20 days prior to the com content to no more than 1 percent Ma terials currently used contain from 10to 30-percent asbestos. Thp intent of the 1-percent limit is to ban the use of ma terials wliich contain significant quanti ties of asbestos, but to allow the ti*e of materials which would: <1> Contain tra.-e amounts of asbestos which occur :u numerous natural substances, and (2 > include very small quantities of asbestos (less turn 1 percent) added to enhance judgment of the Administrator that mencement of demolition. the material's effectiveness Although a Front At etd'trra, vol 3S. no. 6t--frioay, Aren 6, 1973 0-T0786 rules and regulations ;-ljr'.d.ivclj'ed reference method lia.s not sumdard will not require disposal Where J?. F i;o?'ii.r p. e. And m a Kendrick been developed to quantitatively deter disposal is required, the Oicupain.ial at Various mine the content of asbestos in a ma Safety and Health Administration regu and Mortality. Arch. Envir. Heakh 15 3i- terial. there are acceptable methods lations <29 CFR 1910.93a*h)l require 1C' 1067. available, based on electron microscopy, which independent laboratories have de veloped. Determining the asbestos con tent of a material with these methods costs approximately $300, and the results that any asbestos wasle. consigned for disposal, be collected and disposed of in sealed impermeable bags or other closed, impermeable containers. The contamina tion of ground water supplies with asbes !. Oloyne. 5. R.: Pneumoconiosis: A Histouyirr.l Surrey of Necropsy Material in 1.205 Cases. Lancet, J, BI0-3U. 1951, JO Tsseloacher. N J., M Klaus, and H I- lkrdy: Asbestos's and Bronchogenic C^ronoinrv: Report of one autopsied case and rr- me accurate within plus or minus 50 tos from landfill disposal is not consid vio a* of the available literature. Am. J Med.. percent: these limits on accuracy were ered a potential problem. 15. 721-732. 1953. taken into account in establishing the The substitution of ceramic wool, min TO. Jacob. S., and M. Anspach: Pulmonary 1-percent limitation. The proposed standard would have prohibited the surfacing of any roadway with asbestos tailings. The promulgated standard applies to all roadways except eral wool, and fiberglass for asbestos is not now known to be a problem. There is no evidence that these materials cause health effects in the concentrations found in occupational or ambient environments. Neoplasia Among Dresden Asbestos Workers. Ann N V. Arad. 6cl,. 152, 536-540. 1965. 21. Klclnfeld. M., J Messit*. and O. Kooym.m: Mortality Experience In a Croup of As bestos Workers. Arch Envlr. Health, IS, 177ISO. 1007. those on ore deposits: these roadways aie Although the standard was not twsod 22. Knox. J. P.. R. S. Doll, and I. D. Hill temporary, and control measures taken on economic considerations, EPA is Cohart Analysis of Changes In Incidence of to comply with the Bureau of Mines reg ulations prevent them from being a major source which must be covered by the standard promulgated herein. At this time, the application of asbestos tailings to public roadways Is not widely prac ticed. but because of the close proximity of roads to the public, a ban on using asbestos tailings on roadways is included in the promulgated standard to avoid a future problem and stop the practice where it is followed. The term "surfac ing" is defined to include the deposit of aware of the impact (55) and consideis it to be reasonable. Costs among the various sources covered by the standard are quite variable. Although the standard may ad versely affect some individual plants or companies which arc marginal opera tions. it appears that such effects will be minimal and the impact to the asbestos industries as a whole will not be large. REmzHCTS 1. Cooke, W. E.: Fibrosis of the Lungs due to the Inhalation of Asbestos Dust. Brit Med. J . 2. 147. 1924. Bronchial Carcinoma In a Textile Asbestos Factory. Ann. N.Y. Acad. Scl., 132, 526-535. 19<!5. 23. Knox, J. P., S. Holmes. R. Doll, and I. D. Hill- Mortality from Lung Cancer rvnd Other Onuses Among Workers in an Asbestos TextUe Factory. Brit. J. Ind. Med.. 25, 293-303 1068. 24 Lleben. J.: Malignancies In Asbestos Workers. Arch. Envir. Health, 23, 619-621, 1066. 25. Lynch. K. M.. end W. A. Smith: Pul monary Asbestosls. in. Carcinoma of Lung in Asbestos-silicosis. Am. J. Cancer. 14. 66-64. J935. 26. Mancuso, T. P., and A. A. El-Attar: asbestos tailings on roadways covered 2. Cooke. W. E.: Pulmonary Asbestosir, Mortality Pattern In a Cohort of Asbestos with snow or ice; therefore, this practice Brit. Med. J., 2, 1024-1025. 1527. Workers. J. Occup. Med.. 9, 147-162, 1967. is prohibited. Consideration was given to including provisions in the standard requiring proper disposal of the asbestos material generated during demolition and col lected in control devices used to comply 3. Dreessen, W. C, J. M. Daiiavalle, T. I. Edwards, J. Vi. Miller, and R. R. Bayers: A Btudy of Asbestos In the Asbestos Textile In dustry rubllc Health Bull. 241. Washington. US. Government Printing Office, 1938. 126 pp. 4. McDonald. S.: History of Pulmonary As bestos's. Brit. Med. J.. 2. 1025-1026. 1927. 27. McDonald. J. C . A. D. McDonald. D. W. Gibbs. J. SiemlatyckJ, and C. E. Rossiter: Mortality In the Chrysotlle Asbestos Mines and Mills of Quebec. Arch. Envir. Health, 22, 677-666. 1971. 23. Merewether. E. R. A.: Asbestosls and CarcmomA of the Lung. In: Annual report of with the requirements of this standard. J. Merewether. E R A.: The Occurrence of the chief inspector of factories for the year It was decided that this was not neces sary because the Occupational Safety and Health Administration regulations <29 CFR 1910 93a(h)i Include house keeping and waste disposal requirements. These regulations require that any as Pulmonary Fibiosts and Other Pulmonary Aflecilons In Asbestos Workers, J. ind. Hyg, 12, 198-222. and 12. 239-257, 1930. 6. Milis, R. o.: Pulmonary AsbestosLs: Re port of a case. Minn. Med., 13, 495-499. 1930 7 Soper, W. B.: Pulmonary Asbehtosls. A report of a case and a review. Am. Rev. 1047. London: M. Y. Stationary Office, 1949, 79 pp. 23. Kcwhouse, M. I.: A Study of the Mor tality of Workers in an Asbestos Factory. Brit. J. Ind Med.. 26. 294-301.1969. 30. SelikofT I. J.. J. Churg. and E. C. Ham mond: Asbcjtoa Exposure and Neoplasia. bestos waste, consigned for disposal, be Tubers., 22. 571-584. 1930. TAMA. 18S, 22-36. 1064. collected and disposed of in sealed im 6. Bonser, O. M,, J B. Faulds, and M. J. 31. Berov. M,, A. Constoa, L. L. Llvornete. permeable bags or other closed, imperme able containers. The potential environmental impact or the promulgated standard was evalu ated. and it was concluded that the standard will not cause any adverse ef Stewart: Occupational Canver of the Urinary Bladder in Dyestuffs Operatives er.d of the Lung in Asbestos Textile Workers and Ironora Miners. Am. J. Clio. Path, 25. 126-m. JOSS. 9. Braun. D. C, and T. D Traan: An Enldcmlologlral Study of Lung Cance- in As and X. 8chalet: Mesothelioma and Its Associ ation with Asbestos. JAMA. 201, 567-501, Jfc67. 32 Etmes. P. C., W. T. E. McCaughey, ar.d O. U Wade: Diffuse Mesothelioma of the Pleura and Asbestos. Brit, Med. J., 1, 350653. 1965. fects. The potentially adverse environ bestos Miners. Arch. Ind. Uesltli. IT, 614- 31. Elmes, P. C.. and O. L. Wade: Relation mental effects of the standard are: G53. 1958 ship Bettreen Exposure to Asbestos and (1) The asbestos-materials which will be collected in control devices and gen erated during demolition will have to be disposed of or recycled. <2) Materials, such as mineral wool, ceramic wool, and fiberglass, will be sub stituted for asbestos presently contained in spray-applied fireproofing and insulat 10. Buchanan, W. D : Asbestosls and Pri mary Intrathoradc Neoplasms. Ann. N Y. Acad. Scl.. 132, 607-618.1965. It. Cordova. J. F, H. Teiluk, and R P. Kcudtson: Asbestosls sad Carcinomas of - he Lung. Cancer. IS, 1181-1187. 1962. 12. DoU.R.: Mortality from Lung Cancer lr. Asbestos Workers. Brit. J. Ind. Med 12, 81-66, 1955. Pleural Malignancy in Belfast. Ann. N.Y. Acad. Sri- 132. 549-657, 1965. 34. rnlicknap, J. B.. and W. N. Smlther: Peritoneal Tumor In Asbestosls. Brit. J. Ind. Med., 21,20-61.1964. 13. Fowler, R B. 8.. J. C. 6Je*per. and E. C. W.irr.er: Exposure to Asbestcs and MesothellonM of the Pleura. Brit. Med. J, 2, 211-213. mi. ing materials. 13. Dunn. J. E., Jr., and J. M. W-l-: A 25. Hammond. E. C.. I. J. SelikofT. e.rd J. In some manufacturing operations, a Prospective Study of Mortality of Several Oc Churg: Neoplasia Among Insulation Workers major portion of the asbestos-material collected by fabric filters is either re cycled to the process or is marketed for other uses. For example, one asbestos tex tile mill recycles large quantities of lor.gcr-fiber asbestos for process use and sells more than 90 percent of the remain ing collected materials to a brake .Inina manufacturer. Consequently, a. signifi cant portion of the increased quantities of "waste" asbestos materials which wll result from the implementation oi the cupational Groups--Special Emphatic on Lung Cancer. Arch. Envlr. Health. 17, 71-1 6 1968. If. Dunn J E., Jr., ar.d J. M Weir- Career Expericn.v or Several Otcupailoual G:n,I: , Followed Prospectively. Am, J. p-,b Heapn. 55. iau7-lj75. 1968. IS Eleryvi, p. c, and A. L Cochrane: A l'c.llo* tm study oi Workers from an As'f,n > Factory. Brp. J. Ind. Med.. 11, 304-3 7 :i>64. 16. rtperlioc. P. E.: Mortality Air.coc A;* beslos Product Workers in Ihr Co.ted St it. Ann. NY. Acad. Scl. 132, 150-165, ift The United States with Special Reference 1n<Ta^l>iominal Neoplasia. Ann. N.Y. Acad Scl.. 1J2. 519-625. 1905. .7. Hourlhjme. D O'B.: The Pathology or ?.. Nollieiiomd and nn Analysis of Tlieir As* -oct.v.iou '"tth Asbestos Erasure Tktr.u. IS, JW-na, 11/64. 25 Lichen J.. end H. PKtawkx: McscthcHoiarv aad Asbestos Exposure. Aich Favlr. Heelth. U. 559-563. 1967, Mnun. R. H.. J. L. Oros}-., and W M O'Donnell: Mesothelioma Associated wiii. Cancer. 10, 521-526, i960. FEDERAL RECISIE*. VOl. 35, NO. 66--FRIDAY. AT7IL 6, 197] 010787 : m i: \v2\-.vy. W. I r . C v: ::j i.: i-.. .ie mo.it l.kuly Out to ' ;>',-u; .ir.s i.n l I., iiul.i: ;h.` d.spe.xion es < Lime?; Z\posure to Lit.*. a:.d p-.-.j;- to ti-.e institution of controls, proper timates are river, in tne Background In L. r lie ;::eurM Me*otbehomas. Ur*.:. Med. J.. IDO7. 7! McDonald. A. D. A Harper. 0. A. El- AU.tr, at.d J. c. McDonald: Epidemiology of ;'ri:r.ary Malignant MesothelLal Tumors in ca;..Ua. Cancer. 26, 914-910. 1970. assessrn-.-nt of the period of exposure is not always possible if. 2); it is known, however, that chronic beryllium disease is associated not only with activities in volving extraction processes, but alto that formation Report lor Asbestos. Beryl lium. and Mercury 'APTD-075::/. pub lished at the time the standards were prOiXised. Rocket testing facilities are required Xewl-.oi.ie, M. L, ond H. Thompson: 64 registry .cases resulted from exposure to meet the limit of 75 microgram-mm- Lp.Je:niology of Mcsotheiial Tumors in tho dtinn? machining operations on nervl- utes per cubic meter, accumulated dur London Aren. Ann. N Y. Acad, fc:., 132, 579- lium materials <J>. There are at least 45 ing ar.y period of 2-consecutive weeks. 588 1-765. <7. Ouen. W. O : Mesotiiellai To r.ore oud i:\posure to Asbestos Dust. Ann. N.Y. Acad. 1>-1 . 333, 674-C79. 1905. 17- Sctikoff. I. J, J. Cliurg. and E C. Ham- mead: Relation Between E\posure to As cases of nonocciiputioiiallyincuri-d dis eases on file with the registry, of which approximately half have been fatal (3h and retrospective studies of tiie concen trations of beryllium that resulted in Tne limit for rocket testing facilities is the same as that developed in 1566 by the Committee on Toxicology of tiie Na tional Academy of Sciences for protec tion of off-site personnel from intermit he os and Mesothelioma. New Eng. J. Med, some cases of chronic beryllium disease tent exposures to soluble beryllium com 77.' 560-565. 1905 from nonoccupational exposure have pounds arising from the firing of rocket 1} Wright, O. W : Asbestos and Health In concluded that the lowest concentration motors ID. 1959 Am Rev. Resp. Dls.. 100, <07-179. 1969. 77. SeLkolI, I. J.. E. C. Hammond, and J. Chu:g: Asbestos Esposure, Smoking, and Neoplasia JAMA, 204, JC6-112, 1963. <7. Wagner, J. C, C. A Sleggs. and P. Marchand: Diffuse Pleural Mesothelioma and which produced disease was greater than 0 01 jig/m* and probably lees than 0.10 pg/ra1 ). In 1949, when it became apparent that beryllium was a toxic material, the Tiie proposed standard did not include a provision on open burning of berylliumcontaining waste. The promulgated standard includes a ban on open burning of beryllium-containing waste. Tins Asbestos Exposure In the North Western Atomic Energy Commission adopted a change was made because information Cape Province. Brit. J. Ind. Med.. 17, 260-271, limit for beryllium concentrations in received alter proposal indicated that I960. community air (l.e., 0.01 eg of beryllium such sources can cause ambient concen 46 Champion, P.: Two cases of Malignant Mesothelioma Alter Exposure to Asbestos. Am Rev. Resp D1S., 103, 821-829, 1971. 49. SelUcoff. I. J- and E. C. Hammond: En vironmental Epidemiology. III. Community Elects of Konoccupational Environmental Asbestos Exposure. Am. J. Pub. Health, 58, per cubic meter of air averaged over a 30day period) (2). Beryllium refining com panies holding contracts with the ABC to operate AEC-owned refinery facilities and expand their own refinery capacity to meet AEC's beryllium requirements, trations of beryllium in excess of 0.01 iig/in* and because it is not possible to control the emissions from open burning. The promulgated standard does allow disposal of beryllium-containing waste in incinerators which are controlled so 1653-1G66, 1968. were required to observe the community as not to exceed the 10-gram-per-day 50. Wagner, J.C.: Epidemiology of Diffuse Mesothelial Tumors- Evidence ol an Associa tion from Studies in South Africa and the United Kingdom. Ann. N.Y. Acad Set, 332, 575-578. 1965. S3. National Institute for Occupational Safety and Health: Occupational Exposures to Asbestos (Criteria for s Recommended Standard). Washington. US. Department of air limit. With the termination of these contracts in the 1961-63 period due to a reduction in AEC requirements for beryllium, the refineries were no longer subject to the AEC community air limit. The AEC's health and safety require ments. however, have continued to apply to all AEC-owned facilities, some of limit. The disposal of beryllium-contain ing ex-plosive waste is included in the standard covering rocket testing. The proposed standard would have covered all machining operations which iu,c alloys containing any amount of be ryllium. Comments were received which claimed that numerous machining opera Health. Education, and Welfare (PBS. HSMHA), 1972 (HSM 72-10267). 57. SelUcoff. I. J , W. J. Nicholson, and A. M. Danger: Asbestos Air Pollution. Arch. Envlr. Health, 25, 1-13, 1972. 52. National Academy of Sciences: Asbestos (Tbs Need for and Feasibility of Air Pollu tion Controls). Washington, National Acad emy of Sciences, 1971, <0 pp. which fabricate and assemble beryllium parts. In the period since the implementation of the AEC guideline, no reported cases of chronic beryllium disease have oc curred as a result of community exposure, and the Committee on Toxicology of the National Academy of Sciences concluded tions use alloys containing low concen trations of beryllium and do not exceed the 10-gram-per-day emission limita tion. An Investigation of these com ments revealed that alloys which Include beryllium either contain a large amount (greater than 60 percent) or a smell amount (less than 5 percent), and that 58. National Inventory of Sources and Emissions--Cadmium, Nickel, and Asbestos. Report by W. E. Davis A Associates under contract to the Department of Health. Edu cation, and Welfare (Contract No. CPA 2269-131). Feb. 1970. 55. Research Triangle Institute: Compre hensive Study of Specified Air Pollution Souroes to A i sees the Economic Impact of Air Quality Standard*--Asbestos, Beryllium. Mer cury. Report prepared under contract to the F.nvlronmental Protection Agency (Contract No. 68-02-0068). Aug. 1972. Bnnuiw Beryllium Is a hazardous air pollutant within the meaning of section 112. The proven effects of airborne beryllium ma terials on human health include both acute and chronic lethal inhalation elfects (I. 2), as well as skin and conjunc tival effects (2). Insufficient data are available to Incriminate beryllium as a human carcinogen II, 2). but the lack of of any mechanism for the total elimina tion of beryllium body burdens, and the that the AEC guideline limit represents a safe level of exposure 11). Accordingly, the Administrator has de termined that in order to provide an ample margin of safety to protect the public health from beryllium, sources of beryllium dust, fume, or mist emissions Into the atmosphere should be controlled to Insure that ambient concentrations of beryllium do not exceed 0.01 *g/m"-- 30-day average. Tiie beryllium standard covers extrac tion plants, foundries, ceramic manufac turing plants, machine shops (processing beryllium or beryllium alloys containing In excess of 6 percent beryllium) and disposal of beryllium-containing wastes. Most affected beryllium sources are lim ited to omissions of not more than 10 grams per day. This level was determined through dispersion estimates as the levei which would protect against the occur approximately 8,000 machining opera tions use the low beryllium content al loys. Tests were conducted by the Agency to determine the beryllium emissions from the operations which use the low beryllium content alloys (e.g. stamping, tube drawing, milling, and sawing). The results indicated that even If the emis sions were vented to the outside air, which they ordinarily are not, they would be significantly below the 10-gram-perday emission limitation. After consider ing these results and the administrative burden if the standard applied to such a large number ol sources, the proposed standard was changed to exempt the machining operations which use alloys containing less than 5-percent ber> 11mm. Tiie proposed standard would have al lowed ail sources of beryllium to choose between meeting the 10-gram-per-day c.nUsion limit and complying by use of ambient monitoring to Insure that the 0 01 ff'm' 20-day average is never cx- resulting possibly long residence time rence of 30-day average ambient concen (reded. After reconsidering the pro;'vied may enhance the opportunity fir cancer induction. The Beryllium Registry now contains over 820 proven cases of beryl lium-related disease <3>, but since many trations exceeding 0.01 ng'iir. The sources covered by the standard are the only known o.ies that could re..u'u in am bient beryllium concentrations in excess stunt1 i;-ci and the c'.iffieulty inherent in ving ambient air quality data, as oppo>-fl to emission data, as a regulatory t' .i:, ii. mis decided to limit the use of References at end of article. of 0.01 /.g 'ir.'. The rssunptions and cqui- nuibu'iit data os a means of compliance fEDESAl ntc HE, VOL 30. M3. .--fHiS'V, A."f t 4, I >73 -010788 nu.cj MHW KCUULAIIUli) to those sources which have demon Mercury L nations used to make the dispersion strated over a reasonable past period that they can meet and have met the ambient limitation. Therefore, the stand ard being promulgated herein allows the ambient option only to existing sources which have 3 years of current ambient air quality data which demonstrate to the Administrator's satisfaction that the 0 01 eg/m' level can be met in the vicinity of the source. A minimum of 3 years of data was judged to be necessary to dem onstrate that the ambient guideline of 0.01 .g/m` (30-day average) can be met because of the possibility of monthly, seasonal, and even annual variations in ambient levels caused by variations in meteorology and production. The exist ing sources which could quality or this option are four beryllium extraction plants and, possibly, a small number of machine shops. These sources were de signed or modified to facilitate compli ance with the 0.01 jig/m ambient limit. The potential environmental impact of this standard was evaluated and it was concluded that the standard will not cause any adverse effects. Beryllium is a very expensive material, and most gas streams emitting significant quantities of beryllium are controlled with high ef ficiency dry collectors, and the collected material is recycled or sold back to the primary producers. Wet collectors are rarely used strictly as an air pollution control device, but more often as an ex traction process control device allowing recycle of waste liquids to the process. Absolute filters are often used as final filters and collect small quantities of beryllium from very low concentration gas streams. These filters are usually burled In company owned or segregated dumps or stored in unused mines or buildings. Most of the solid wastes are prepackaged prior to burial to prevent escape of beryllium to the environment. Although the standard is not based on economic considerations, EPA Is aware of the economic Impact (5) of the stand ard. Since most of the sources of beryl lium emissions are already controlled and in compliance with the standard, the economic impact will be very small. Bmmcu 1. Committee on Toxicology. National Acad emy of Sciences: Air Quality Criteria for Beryllium and Its Compound* Report pre pared under contract to the OA. Public Health Service (Contract N7onr-291 (01)), Washington. Starch 1. IMS. 2. National Institute for Occupational Safety and Health: Occupational Exposure to Beryllium (Criteria for a Recommended Standard). Washington, TJ.S. Department of Mercury Is a hazardous air pollutant within the meaning of section 112. Ex posure to metallic mercury vapors may cause central nervous system injury, and renal damage (J. 3). Experience with mercury vapor comes almost exclusively from animal experiments and industrial exposures. Animal (rat) data indicate a risk of accumulation in critical systems upon prolonged exposure, with a poten tial, for example, for selective brain dam age (2. 3>. Prolonged exposure to about 1J0 micrograms mercury per cubic meter of air involves a definite risk of mercury intoxication (3). To determine the ambient air level of mercury that does not impair health, the airborne burden must be considered to gether with the water- and food-borne burdens. An expert group concluded, based on its analysis of several episodes of mercury poisoning in Japan, that 4 micrograms of methylmercury per kilo gram of bodyweight per day would result in the Intoxication of a sensitive adult: application of a safety factor of 10 yielded an acceptable exposure of about 30 micrograms per day for a 70-kllogram man, 8nd this level Is also believed to provide satisfactory protection against genetic lesions, and poisoning of the fetus and of children (<). It should be noted that methylmercury Is considered to be by far the most haz ardous mercury compound, particularly via the ingestion of fish In which It has been concentrated through the food chain. (3, S). The Environmental Protec tion Agency, in view of the piesent lim ited knowledge as to the effects of in haled mercury In the general population, and in order to best assure the requisite "ample margin of safety to protect the public health," has concluded that it Is prudent to consider exposures to methylmercury (diet) and mercury vapor (air) to be equivalent and additive. It has been estimated that from average diets, over a considerable period, mercury intakes of 10 microgram* per day may be expected (6), so that, in order to restrict total Intake to 30 micrograms per day. the average mercury intake from air would have to be limited to 20 mlcrograms per day. Assuming inhalation of 20 cubic meiers of air per day, the air could con tain an average daily concentration of no more than 1 mlcrogram of mercury per cubic meter. The standard promulgated herein reg ulates the only two sources, mercury ore processing facilities and mercury cell chtor-alkali plants, which have been estimates are given in the Background Information Report for Asbestos, Beryl lium, and Mercury (APTD-0753). pub lished at the time the standards were proposed. Many mercury cell chlor-alkaii plant cell rooms present severe source testing problems due to their design and con struction. Such sources may either recon struct the cell room so that accurate source tests can be made or employ housekeeping and maintenance practices that minimize mercury emissions from the cell room. Source test data and cal culations have Indicated that when such practices are used, 1.300 grams per day is a reasonable estimate of emissions from the cell room. Therefore, when this option is chosen, an emission of 1,300 grams per day will be assigned to the cell room. This permits emissions of not more than 1,000 grams per day from the hydro gen and end box ventilation streams com bined. Compliance with the standard will be determined by the EPA reference method or EPA-approved substitute methods. Where a chlor-alkall plant chooses the housekeeping and maintenance practices option, determination of compliance of the cell room emission will be based on the use of EPA-approved practices. A list of approved practices may be obtained from EPA on request to regional offices. The only major change In the mercury standard is the Introduction of the above option of assigning an emission number to the cell room provided certain house keeping and maintenance requirements are met. When this option is chosen, test ing is not required for emissions from the cell room. This option is offered because comments, testimony, and EPA source testing experience indicated that most existing cell rooms cannot be accurately tested for mercury emissions. Accurate emission tests are unduly complicated and costly because of the cell room configuration. Sonic of the changes suggested In writ ten comments and public hearing testi mony were considered by EPA but not made. The most significant one Involved the environmental chemistry of mercury, that Is. environmental mercury In the at mosphere is transformed to mercuric oxide by the action of ultraviolet radia tion, and since mercuric oxide is not as toxic as elemental mercury, the stand ard should be less stringent. This argu ment Is based on laboratory experiments under controlled conditions with generr.led radiation. The reaction cited In the Health, Education, and Welfare (PHS, found io emit mercury in a manner that testimony occurs when elemental mer HSMHA). 1972 (HSM 73-10268). could cause the ambient concentration tc cury is it radiated with ultraviolet lialit S. Massachusetts General Hospital, C.S. exceed the Inhalation effects limits of t Willi a wavelength of 2,537 angst 10m (A). Beryllium Case Registry, Boston, Mass. microEram per cubic meter. The stsnd- Naturally occurring ozone In the upper 4. Elsenbud. M. R. C. Wantc, C. Dust an. aid limits emissions from these facilities atmosphere absorbs light In the ultra L T. Steadman. tv. B. Hanls. and B. S. Wolf: to r.ot more than 2,300 grams per day. violet region below 3,000 A: (7) lienee the Nouoccup&uonai Berylliosis. J. Ond. Hyp. The emission limit of 2,300 grams per wavelength of ultraviolet necessary for Toxicol., 31. 282-294.1949. day was derived from dispersion esti the reaction Is absent In the ambient at 5 Research Triangle Institute: Compre hend"* Study of Specified Air Pollution Sources to Assess the Economic Impact oi Air Quality Standards--Asbestos. Beryllium Mer cury. Report prepared under contract to the mates as the level which would protect 15an1.1l Ihe violation of an average daily I'.mhient concentration of I microsmm per (Jbic meter. The assumptions and mosphere. and the reaction does not procied at ns high a rate as implied by the submitted testimony. Field measurements of both mercury vapors and particulate Environmental Protection Agency (Contract mercury In ambient air Indicate that as No. 68-02-0068). August 1972. Refrrppeei a- end of article. much ns 98 percent of the mercury de- FEDERAL RZCrS'ES, VOL 38. NO 66--MIOAY, APR:i 6, -010789 .. ,, --.-- .ijii,,, t-er,;.a:. i::a.!.T. co'lecUtl by IT'A ;vi. si; ,'deral Pklilloq ill Moundiv.iltf. \V. V3>. tiee.'.use tile sieves r. Ih- ri ': / in place without retorting ami can -e Mcrrury V.-oort pr-mr-ii under contract In li'e fuviroi'mcntai pmi'cnoii Agency (Con tract Nu. 68-Oe-C'MB. . .V. ;uit 1972. The Environmental Protection Agency reused many times. recognizes that mercury and its cunif.'Jiido constitute a multimedia contapounds constitute a tnuitimedia contamm.ilion problem, i.c.. strong evidence Ker Its natural distribution in the en vironment; that such uses may cause or hasten additional deposits into water or soil over and above those occurring naturally, thereby building up environ ment.'.1 concentrations; and the mercury levels accumulate in the biota, with the result that potentially dangerous residue levels are reached in foods consumed by man and animals. Current data on the environmental transport of mercury do not permit a clear assessment of the effect of mercury emissions into the atmosphere on the mercury content in the aquatic and ter restrial environments. Results of ongoing research will determine if there is a need for more comprehensive control of mer cury emissions Into the air. The stand ard promulgated herein is intended to protect the public health from the effects of Inhaled mercury. The environmental Impact of this standard was evaluated and it was con cluded that the standard will not cause any adverse effects since the control of mercury emissions to the atmosphere will have only minimal impact on other areas of environmental concern. The simplest control for mercury emissions to the atmosphere is cooling to condense the mercury. This cooling can be Indirect or direct. By Indirect cooling, the mer cury condenses and is retained for re cycle or sale. By direct cooling with a water scrubber, the water is usually re circulated after using centrifugal or gravitational separation to remove the mercury. The water cannot be reused Indefinitely and eventually requires addi Although the standard was not based on economic considerations. EPA is aware of the impact <S) and considers it to be reasonable. Because mercury is an international commodity, world prices determine the fortunes of the domestic mercury mining industry. Historically, mercury prices fluctuate greatly in re sponse to small changes in demand or supply. Domestic mercury mines are con sidered high-cost producers in relation to foreign producers. Eecause the average price has dropped from $404 per flask in 1969 to approximately $320 currently, the number of domestic mercury mines in operation has dropped sharply from 109 in 1969 to six or seven in March 1973. As long as the price of mercury remains below marginal costs of production (gen erally about $400), the remaining domes tic mines will be ill equipped to absorb any cost increases. The total chlor-alkali Industry com prises 60 plants. Approximately 28 are mercury cell plants and account for about 27 percent of the U. production of chlorine and caustic. The future of the chlorine-caustic in dustry appears healthy. Demand for chlorine is expected to grow at an annual rate of 6 percent projected from 1971. Demand for caustic soda will grow at least at the same rate as chlorine, and perhaps faster. Prices for chlorine and sodium hydroxide have been rising steadily through the sixties Into 1971. Based on these trends, the cost of control to comply with the mercury standard will be passed forward to the consumer. Use of these two basic commodities is so di verse that any price increases will be well dispersed through all manufacturing activities. fUnizHccs Gckexal Provisions The standards promulgated below are applicable to new. modified, and existing sources. Any new or modified source must comply with the standards upon begin ning operation. Any existing source mud comply with the standards within flu clays after promulgation, unless a waiver ol compliance is granted. After considering the proposed general provisions and the comments received on them, the Administrator made several changes which are included in the stand ards promulgated below. A new section was added to specifically require new sta tionary sources to notify the Administra tor before beglnnning operation. The requirements for source reporting and request for waiver of compliance were combined into one section. The time for submitting the source report was ex tended from 30 to 90 days to provide sources with more time to complete the information required. Appendix A was added to provide sources a description and format of the information required. The proposed standards required all sources of mercury and beryllium to test their emissions within 3 months of the effective date and at least once every 3 months thereafter; a provision was in cluded to allow the Administrator to waive the periodic tests for sources in compliance with a standard. The standards promulgated below require the ini tial test within 90 days of the effective date and include a provision to allow the Administrator to waive this requirement if the source is meeting the standard or has requested a waiver of compliance. Periodic tests are not required unless specifically requested by the Administra tor. The Administrator may cancel a waiver of emission tests and may require tional treatment to remove the mercury. In most cases, such treatment facilities are already being utilized to meet water quality standards. I Report of an International Committee: Maximum Allowable Concentrations ol mer cury Compounds. Arch. Envlr. Health. 19. 891- BOS. December 1B69. 2. Clarkson, T. W.: The Pharmacology of a test under the authority of section 114 of the Act at any time. Appendix A speci fies the information which a source must provide the Administrator when applying A widely used control device for par Mercury Compounds. Ann. Rev. Pharmacol lor a waiver of initial emission testing. ticulate mercury emissions is the mist eliminator. Residues in these devices are removed by gravity and washing with a recycled liquid. Another control method is chemical scrubbing. In this system, scrubbing liquids are continuously made up while waste materials are usually re cycled to the process feed solutions. Recycling of these liquids avoids significant contamination of water with mercury residues. The use of adsorption beds Is a highly efficient control method for removing mercury from gas streams. Two primary types are available: (l) Chemically treated activated carbon beds, and (2) molecular sieves. Most of the mercury collected by activated carbon can be re claimed by retorting the carbon but this usually destroys the carbon structure and necessitates disposal Some small amount of residual mercury will remain with the carbon, but it is tightly bound and is not easily transferred Into the air or water. Regenerative molecular sieves ogy. 22.375--408,1973. 3. Friberg. L-, and J. Voctal (Eds.): Mer cury In the Environment--A Toxicological and Epidemiological Appraisal. Prepared by the Karollnska Institute Department of En vironmental Hygiene (Stockholm) for the US. Environmental Protection Agency (Office of Air Programs). November 1971. 4 Methylmercury in Pish; a ToxicologicEpidemiologic Evaluation of Risks. Report from an expert group. Hord. Hyg. Tlsdkr. (Stockholm). Supplement 4. 1971 (English trsnslstlon). 3 Kelson. N.. T. C. Byeriy, A. C. Kolbyc, Jr.. L T. Kurland. R. E. Shapiro, S. I. ShlbLo. W H Stickle, J. E. Thompson. L. A Vau Den Berg, and A. Welssler: Hazard( of Mercury (.special report to the Secretary's F>'icldc Advisory Committee. Department of IPalth. Education, and Welfare. November 1970). Emir Res.. 4, 1-C9. 1971. 6. Westoo, O.: Mercury In Foodstu7s--Ts There a Great Risk of Poisoning? VAR I ODA. 4. 1-6, 1965. 7. Leighton. P. A.: Photochemistry of .Sir Pollution. Academic Press. 1961 J. Research Triangle Institute: Compre hensive Study of Specified Air romitlon Sources to Assess riie Economic Impact of The standards promulgated below do not require the owner or operator to request a waiver of compliance before a specific date. However, the owner or op erator should submit the request within 30 days after the effective date of the regulation to be assured that action will be taken pn the waiver application prior to the 90th day after the effective date. Continued operation in excess of a stand ard after the 90th day without a waiver is a violation of the act. The Administrator may grant an exist ing source a waiver, permitting a period of up to 2 years for compliance, provided that steps will be taken during the waiver period to assure that the health of per sons will be protected from imminent endangerment and provided that such period is necessary for ihe installation of controls. To be granted a waiver o! com pliance, a source must submit a written request to the Administiator and pro vide certain information to assist the Administrator in making a judgment. nCCZAl REGISTER, VOt. 38, NO. 68---ft PAY, APRIl 6, 1973 010790 >'2G RULES AND REGULATIONS WithHi SO days alter receiving a request, ferred methods of sampling and analyz Sec the Administrator will notify the owner ing used to determine compliance. The 61 22 Emission standard. or operator of approval or intention to deny the waiver. Any waiver of com reference methods for beryllium and mercury are included in appendix B to 61 23 Air cleaning. 61 24 Reporting. pliance granted by the Administrator will this part. An equivalent method is any be in writing and specify conditions the method of sampling and analyzing which Subpart C--National Emission Standard for Beryllium source must meet during the waiver period. If the Administrator intends to deny a request, the owner or operator will be given a specified time to provide additional information or arguments prior to final action on the request Pinal action on a request will be in writing by the Administrator, and if denied, will in clude reasons for denial. The President may exempt any new, modified, or existing stationary source has teen demonstrated to the Admin istrator's satisfaction to have a con sistent and quantitatively known rela tionship to the reference method under specified conditions. An alternative method is any method of sampling and analyzing which does not meet all the criteria for equivalency but which can be used in specific cases to determine com pliance. Alternative methods may be ap proved by the Administrator for source 61.30 6131 61 32 61 33 61.34 Applicability. Definitions. Emission standard.. Stock sampling. Air campling. Subpart E>--National Emission Standard for Beryllium Rocket Motor Firing 61 40 Applicability. 61.41 Definitions. 61 42 Emission standard. 6143 Emission testing-brocket firing or pro pellant disposal. from compliance with the standards for testing; however, in cases where deter 61.44 Stack sampling. a period of up to 2 years, provided the minations of compliance using an alter technology Is not available to implement native method are disputed, use of the Subpart E National Emission Standard for Mercury the standards and the operation of such reference method or Us equivalent will 61.50 Applicability. source is required for reasons of national be required by the Administrator. An ap 61 51 Definitions. security. Also, the President may grant proved alternative method for beryllium 61.52 Emission standard. exemptions for additional periods of 2 years or less. The construction of a new source or modification of an existing source cov ered by these standards cannot begin without approval of the Administrator. is included in appendix B hereto. All emission data provided to or ob tained by the Administrator in carrying out these regulations will be available to the public. Records, reports, or informa tion other than trade secrets will be 61 53 Stack sampling Appendix A---Compliance Status Information. Appendix B--`Test Methods. Method 101--Reference method for determi nation of particulate and gaseous mercury emissions from stationary sources (air streams). To obtain approval, the owner or opera tor of such sources must apply In writing to the Administrator. Within 60 days, the Administrator will notify the owner or operator of approval or intention to deny approval. If the Administrator in available to the public. Pursuant to section 112(d)(1) of the act, the Environmental Protection Agency intends to delegate the author ity to implement and enforce national emission standards (except with respect Method 102--Reference method for determi nation of particulate and gaseous mercury emissions from stationary sources (hydro gen streams). Method 103--Beryllium screening method. Method 104--Reference method for determi nation of beryllium emissions from sta tends to deny approval, a specified time to stationary sources owned or operated tionary sources. will be given to provide additional infor by the United States) for hazardous air mation or arguments prior to final action pollutants to any State which submits an on the application. The final action on adequate procedure to the Administrator. AuTHoarrr: 42 U.S.C. 1S57C-7. Subpart A--General Provisions any application will be in writing by the Administrator, and if denied, will in clude the reasons for denial. Although the demolition of buildings or structures containing asbestos ma terial and the spraying of asbestos ma The requisite procedure for requesting 61.01 Applicability. such delegation will be Issued in the future by the Environmental Protection Agency. The regulations for the national emisrsion standards for asbestos, beryllium, 1 I The provisions of this part apply to the owner or operator of any stationary source for which a standard is prescribed under this part. terial will In many cases be modifications and mercury are hereby promulgated ef- I 61.02 Definitions. of existing stationary sources, the Ad ministrator's approval Is not required be fore beginning such operations. Section 112(c)(1) of the act specifies that no person may construct any new source or modify any existing source"* * * unless the Administrator finds that such source if properly operated will not cause emis sions in violation of such standard." The demolition and spraying provisions are expressed In terms of procedures to be followed. Therefore, if the source is prop erly operated. It will be complying with the standard, and there is no need for the Administrator to make a finding with respect to each new source subject to these provisions. Each source covered by these stand ards is required to submit to the Admin fective 1973). upon promulgation (April 6. ------------------ ---------------------- / As fined used in this part, ail herein shall have the terms not de meaning given Dated; March 30. 1973. them in the act: RomstW. Fri. Acting Administrator. Environmental Protection Agency. (a) "Act" means the Clean Air Act (42 UB.C. 1857 et seq.). (b) "Administrator" means the Ad ministrator of the Environmental Pro A new Part 61 Is added to Chapter 1. tection Agency or his authorized repre Title 40, Code of Federal Regulations, as sentative. follows: (c) "Alternative method" means any ^ Subpart A ftnrl PreoMom method of sampling and analyzing for an Rlr pollutant which does not meet oil of 1.01 Applicability. the criteria for equivalency but which has 61.oa Definitions. been demonstrated to the Administra 61.03 Abbreviation*. tor's satisfaction to. In specific cases, pro 61.04 Address. 61.05 Prohibited activities. 6106 Determination of constructor! or duce results adequate for his determina tion of compliance. modification. (d> "Commenced" means that an own 61.07 Application for approval of construc er or operator has undertaken a con istrator within 90 days after promulga tion or modification. tinuous program of construction or tion certain information pertaining to its 61 06 Approval by Administrator. modification or that an owner or operator operation. Changes in the information must be submitted within 30 days after the change, except where the change Is considered a modification. Then the re quirements for a modified source are applicable. 61 09 6l 10 61 11 6112 61 13 61 li 61.15 Notification of startup. Source reporting and waiver request. Waiver of compliance. Emission tests and monitoring. Waiver of emlss;on tests. bource test and analytical methods. Availability of Information. has entered Into a contractual obligation to undertake and complete, within a rea sonable time, a continuous program of construction or modification. (e) "Compliance schedule" means the date or dates by which a source or cate Three terms are associated with deter 61.1G State authority. gory of sources Is required to comply with mining compliance by means of source Subpart B--National Emission Standard for tlie standards of this part and with any testing' (1) Reference method. <2> Asbsttos steps toward such compliance which are equivalent method, and (3) alternative 61.20 Appl IcabUlty. set forth in a waiver of compliance under method. Reference methods are the pre 61.21 Definitions. ? 61.11. fSOESM SECIITSS, VOl. 38, NO 46--F8IDAV. AMIt &, 147J 010791 f> T .nxlrurtun" < '.brii'.i.wn. yd --Irina:e yards. -..hich smmencftd ter :l>.e publtca- er-viiors. or installation o.' a ..taiionary v,.s --Water gage. t.'in date of tne '.anduras pi.mused (.v so'.:; ce. inHsr --Inches of merrury. be applicable to .-.uch source, are subject < rr' "Effective dote" Ls t'.ie date of inH O--Inches of water, to tins prohibition. nromiilgation in the Feoziivi. Recister g--Ci ams. <bi After the effective date of any of .mi applicable standard or other regu mg--Milligrams. standard prescribed under tills part, no lation under this part. N--Nc mal. owner or operator shall operate any new Mu 'Equivalent method" means any R--Degree Rankine. source :n violation of such standard ex me'hod of sampling and analyzing for mm--Minute cept under an exemption granted by the mi air pollutant which has been ciemon- sec--Second. President under section 112rcJ I2) of the raied to the Administrator's satisfac avg --Average. act. tion to have a consistent and qu.mtita- I D --Inside diameter. 'ci Ninety days after the effective date tnely known relationship to the reference O D --Outside diameter. of any standard prescribed under this method, under specified conditions. vS--Micrograms (10"gram). part, no owner or operator shall operate (l' "Existing source" means any sta T.--Percent. any existing stationary source in viola tionary source which is not a new source. Hg--Mercury. tion of such standard, except under a iji "Modification" means any physical Be--Beryllium. waiver granted by the Administrator in change in. or change in the method of operation of, a stationary source which increases the amount of any hazardous air pollutant emitted by such source or which results In the emission of any hazardous air pollutant not previously emitted, except that: (D Routine maintenance, repair, and replacement shall not be considered physical changes, and 61.01 Adilresa. All requests, reports, applications, sub mittals, and other communications to the Administrator pursuant to this part shall be submitted in duplicate and ad dressed to the appropriate regional office of the Environmental Protection Agency, to the attention of the Director, Enforce ment Division. The regional offices are as accordance with this subpart or under an exemption granted by the President under section 112(c) (2/ of the act. (d) No owner or operator subject to the provisions of this part shall fail to report, revise reports, or report source test results as required under this part. 61.06 Determination of construction or modification. (2) The following shall not be con sidered a change in the method of operation: (ii An increase in the production rate. If such increase does not exceed the op erating design capacity of the stationary source: (il) An Increase in hours of operation. (k > "New source" means any stationary source, the construction or modification of which is commenced after the publi cation in the Federal Register of pro posed national emission standards for hazardous air pollutants which will be applicable to such source. (1) "Owner or operator" means any person who owns, leases, operates, con trols. or supervises a stationary source. <m> "Reference method" means any method of sampling and analyzing for an air pollutant, as described in ap pendix B to this part. (n> "Startup" means the setting in operation of a stationary source for any purpose. (o> "Standard" means a national emission standard for a hazardous air pollutant proposed or promulgated under this part. follows: Region I (Connecticut, Maine, Massa chusetts. New Hampshire. Rhode Island. Vermont!. John F. Kennedy Federal Building. Boston. Mass. 02203. Region n (New York. New Jersey. Puerto Rico. Virgin Islands), Federal Office Building. 26 Federal Plaza (Foley Square'. New York. N.Y. 10007. Region m (Delaware, District of Co lumbia Pennsylvania, Maryland. Vir ginia. West Virginia). Curtis Building. Sixth and Walnut Streets, Philadelphia, Pa. 19106. Region IV (Alabama, Florida, Georgia. Mississippi, Kentucky, North Carolina, South Carolina, Tennessee). Suite 300, 1421 Peachtree Street, Atlanta, Ga. 30309. Region V (Illinois. Indiana. Minne sota, Michigan. Ohio, Wisconsin), 1 North Wacker Drive. Chicago, Hi. 60606. Region VI (Arkansas. Louisiana. New Mexico. Oklahoma, Texas), 1600 Pater son Street, Dallas, Tex. 75201. Region VH (Iowa. Kansas, Missouri. Nebraska), 1735 Baltimore Street, Kan sas City. Mo. 64108. Region vm (Colorado. Montana, Upon written application by an owner or operator, me Administrator will make a determination of whether actions taken or intended toToe taken by such owner or operator constitute construction or modification or the commencement thereof within the meaning ot this part. .Thf--Administrator will within 30 days of receipt of sufficient information to evaluate an application, notify the owner or operator ot his determination. 61.07 Application foe approval of coinlmclion or modification.___________ (a) The owner or operator of any new source to which a standard prescribed under this part is applicable shall, prior to the date on which construction or modification is planned to commence, or within 30 days after the effective date in the case of a new source that already has commenced construction or modifi cation and has not begun operation, sub mit to the Administrator an application for approval of such construction or modification. A separate application shall be submitted for each stationary source. (b) Each application shall include: (1) The name and address of the ap plicant. (p> "Stationary source" means any building, structure, facility, or installa tion which emits or may emit any air pollutant which has been designated as North Dakota. South Dakota, Utah. Wy oming). 916 Lincoln Towers, I860 Lin coln Street. Denver. Colo. 80203. Region DC (Arizona, California. (2i The location or proposed location of the source. (3) Technical information describing the proposed nature, size, design, operat hazardous by the Administrator.' Hawaii. Nevada, Guam, American ing design capacity, and method of oper 61,03 Abbreviations. The abbreviations used In this part have the following meanings: C--Degrees Centigrade, cfm--Cubic feet per minute, ft'--Square feet, ft'--Cubit feet. *F--Decrees Fahrenheit, Samoa), 100 California Street, San Francisco. Calif. 94111. Region X (Washington, Oregon. Idaho, Alaska). 1200 Sixth Avenue. Seattle. Wash. 98101. 61.03 Prohibited activities. ia) After the effective date of any standard prescribed under this part, no ation of the source, including a descrip tion of any equipment to be used for control of emissions. Such fechnical in formation shall include calculations of emission estimates in sufficient detail to permit assessment of the validity of such calculations. 61.68 Approval AilminiMnitor. in--Inch. 1--Liter, ml--Milliliter. M--Molar, m--Cubic meter, nm--Nanometer, oz--Ounces. v. v--Volume per volume. owner or operator shall construct or mod ify any stationary source subject to such standard v.r.aout r.rst ootamiiig written -nnr.e v.TtK thirTubpart. except unacr an exemption granted by the President under section li^(cWli) ol the act. Sources, the construction or modification ^ai Tne Administrator will, within 60 days of receipt of sufficient information to evaluate an application under 5 61.07, notify the owner or operator of .approval or intention to deny approval of con struction or modification. <b) If the Administrator determines that a stationary source for which ?.n No. 66--Pt. ii---- a FEDERAL REGISTER, VOL. 38, NO. 64--FRIDA/. APRIL 6. 1473 010792 SS2S RULES AND REGULATIONS a;;r'!::ut;un pursuant to 5 61 07 '.vis sub- (5) The average weight per month of s: under paragraph (i;i(3) of this m,`.lcd will. it properly operated, not the hazardous materials being processed tec'ai are not met. rim e emissions in violation of a stand by the source, over the last 12 months '3> Specity dates by which steps to ard he will approve the construction or preceding the date o1 the report. ri aid compliance are to be taken; and modulestion of such source. (6) A description of the existing con impose such additional conditions as the (c) Prior to denying any application trol equipment for each emission point. Administrator determines to be neces f'-r approval of construction or modifica (l)Primary control device(s) for each sary to assure installation of the neces tion pursuant to this section, the Admm- hazardous pollutant. sary controls within the waiver penod. iurator will notify the owner or operator (n) Secondary control device(s) for and to assure protection of the health making such application of the Admin- each hazardous pollutant. of persons during the waiver period. i 'tialor s intention to issue such denial, in) Estimated control efficiency 'per (cl Prior to denying any request for tr-e'her with: cent i for each control device. a waiver pursuant to this section, the ill Notice of the information and (7) A statement by the owner or oper Administrator will notify the owner or findings on which such intended denial ator ol tire source as to whether he can operator making such request of the Ad is based, and comply with the standards prescribed in ministrator's intention to issue such <21 Notice of opportunity for such this part within 00 days of the effective denial, together with: owner or operator to present, within such date. (11 Notice of the Information and time limit as the Administrator shall (b) The owner or operator of an exist findings on which such iutended denial specify, additional information or argu ing source unable to operate in compli is based, and ments to the Administrator prior to final ance with any standard prescribed under (2) Notice of opportunity for such action on such application. this pan may request a waiver of com owner or operator to present, within <d> A final determination to deny any pliance with such standard for a period such time limit as the Administrator application for approval will be in writ not exceeding 2 years from the effective specifies, additional information or argu ing and will set forth the specific grounds date. Any request shall be In writing and ments to the Administrator prior to final on which such denial Is based, ouch final shall Include the following information: action on such request. determination will be made within 60 days of presentation of additional infor mation or arguments, or 60 cays after the final date specified for presentation, if no presentation Is made. (e> Neither the submission of an ap plication for approval nor the Admin istrator's granting of approval to con struct or modify shall: (1) Relieve an owner or operator of legal responsibility for compliance with any applicable provision of this part or of any other applicable Federal. State, or local requirement, or (2) Prevent the Administrator from Implementing or enforcing this part or taking any other action under the act. ^L09Noiifiiioiio^iiBrtijj. <1> A description of the controls to be Installed to comply with the standard. (2) A compliance schedule, including the date each step toward compliance will be reached. Such list shall include as a minimum the following dates: (1) Date by which contracts for emis sion control systems or process modifica tions will be awarded, or date by which orders will be issued for the purchase of component parts to accomplish emis sion control or process modification: <ii> Date of Initiation of onsite con struction or Installation of emission con trol equipment or process change; <iii) Date by which onsite construc tion or installation of emission control equipment or process modification is to (d) A final determination to deny any request for a waiver will be In writing and will set forth the specific grounds on which such denial is based. Such final determination will be made within 60 days after presentation of additional in formation or arguments, or 60 days after the final date specified for such presen tation, if no presentation is made. (e) The granting of a waiver under this section shall not abrogate the Ad ministrator's authority under section 114 of the act. 61.12 Emission teats and monitoring. (a) Emission tests and monitoring shall be conducted and reported as set forth in this part and appendix B to this part. (a) Any owner or operator of a source be completed; and (b) The owner or operator of a new which has an initial startup after the (iv> Date by which final compliance is source subject to this part, and at the effective date of a standard prescribed under this part shall furnish the Admin istrator written notification as follows: (1) A notification of the anticipated date nf initial startup of the source not more than 60 davs nor less than 3>l days nrinrtnsnch date (2) A_notificationof the actual date rfif initial startup of the SOUTCC Within 15 Oav* After such date. 61.10 Soorct reporting and waiver re- to be achieved. (3) A description of interim emission control steps which will be taken during the waiver period. (c> Changes in the Information pro vided under paragraph (a) of this section shall be provided to the Administrator within 30 days after such change, except that if changes will result from modifica tion of the source, as defined In ( 61.02 (j), the provisions of I 61.07 and f 61.08 are applicable. request of the Administrator, the owner or operator of an existing source sub ject to this part, shall provide or cause to be provided, emission testing facili ties as follows: (1) Sampling ports adequate for test methods applicable to such source. (2) Safe sampling platform(s). (3) Safe access to. sampling platform(s). (4) Utilities for sampling and testing equipment. (a) The owner or operator of any existing source, or any new source to which a standard prescribed under this part is applicable which had an initial startup which preceded the effective date (d) Hie format for reporting under this section is Included as appendix A of this part. Advice on reporting the sta `-us of compliance may be obtained from the Administrator. 61.13 Waiver of emiuion lev(a. fa> Emission testa may be waived upon written application to the Admin istrator if. in his judgment, the source Is meeting the standard, or if the source of a standard prescribed under this part shell, within 90 days after the effective dale, provide me lonowmg imormation ui writing to the Administratori"-""""- 11 j Name and address of the owner or operator. i2) The location of the source. (3i The type of hazardous pollutants emitted by the stationary source. (4) A brief description of the nature, size, design, and method of operation of the stationary source including the op 61.11 \Tiiiver of compliance. (n) Eased on the information provided In cny request under f 61.10, or other in formation, the Administrator may gTant a w aiver of compliance with a standard for a period not exceeding 2 years from the effective date of such standard. (b)Such waiver will be in writing and will: <I Identify the stationary source covered. is operating under a waiver of compliance or has eequested a waiver of compliance. <b) If application for waiver of the emission test is made, such application shall accompany the information re quired by i 61.10. The appropriate form is contained in appendix A to this part. <ci Approval of any waiver granted pursuant to this section shall not abro gate the Administrator's authority under the ;.ct or in any way prohibit the Ad ministrator from later canceling such erating design capacity of such source. (2) Specify the termination date of wa.vcr. Such cancellation will be made Identify each point of emission for each the waiver. The waiver may be termi c::l/ after notice Is given to the owner hazardous pollutant. nated at an earlier date If the conditions or operator of the source. FCDEBAl BEGi :::r, vot. jo, mo. 6A--rS'OAV, APCIL S, 1073 010793 \ilES AND REGULATIONS Ss2'") x 61.1 V SuilfTf te-l uml ,'ii.iii !I |||- Subpan 3--National emission Standard i:\i tnll.it ion, or p.-dion liioreol .:i;. i i ior Asbestos contains any boiler, pipe, or load-sup iai Methods 101, 102 and 104 in ap pendix B to this part shall be used lor all source tests required under this part, unless an equivalent method or an al ternative method lias been approved by the Administrator. <b) Method 103 in appendix B to this part Is hereby approved by the Admin istrator as an alternative method (or sources subject to 5 6l.32<a' and 61 42 ib>. i c' The Administrator may. after no tice to the owner or operator, withdraw approval of an alternative method granted under paragraph (a' or (b) of this section Where the test results using mi alternative method do not adequately indicate whether a source is in compli ance with a standard, the Administrator may require the use of the" reference method or its equivalent. 61.13 Aiaiiahililjr of infsrniniitm. -- (a) Emission data provided to. or oth erwise obtained by. the Administrator in accordance with the provisions of this part shall be available to the public. (b) Any records, reports, or informa 61.20 Applicability. The provisions of tilts subpart are ap plicable to those sources .specified in ? Cl 22.' 61.21 Definitions. Terms used in this subpart are Defined in the act, in subpart A of this part, or in this section as follows' ia' "Asbestos" means actinolite amosite, anthophyllitc, chrysotile, crocidolite, trcinolite. <b> "Asbestos material'' means as bestos or any material containing as bestos (o' "Particulate asbestos material" means finely divided particles of asbestos material. idi "Asbestos tailings" means any solid waste product of asbestos mining or milling operations which contains as bestos. (e' "Outside air" means the air out side buildings and structures. ifi "Visible emissions" means any emissions which are visually detectable without the aid of instruments and which contain particulate asbestos material. porting structural member that is :nsulated or fireprooted with friaote asbestos material shall comply with the require ments set forth in this paragraph. (li Notice of intention to demolish shall be provided to the Administrator at least 20 days prior to commencement of such demolition or anytime prior to commencement of demolition subject to paragraph (d: < 4 > of this section. Such notice shall include the following information: ii) Name of owner or operator. (n) Address of owner or operator. <Hi) Description of the building, struc ture, facility, or installation to be de molished. (iv) Address or location of the build ing. structure, facility or installation. <v> Scheduled starting and completion dates of demolition. (vi) Method of demolition to be em ployed. -tvii) Procedures to be employed to meet the requirements of this paragraph. *_3> .The following procedures shall be used to prevent emissions of particulate asbestos material to outside air: (ti Friable asbestos materials, used to tion, other than emission data, provided 61.22 IvmiMion slanJird. insulate or fireproof any boiler, pipe, or to. or otherwise obtained by. the Admin istrator in accordance with the provisions of this part shall be available to the pub lic, except that upon a showing satisfac tory to the Administrator by any person that such records, reports, or informa tion, or particular part thereof (other than emission data), if made public, would divulge methods or processes en titled to protection as trade secrets of such person, the Administrator will con sider such records, reports, or informa tion, or particular part thereof, confi dential In accordance with the purposes of section 1905 of title 18 of the United States Code, except that such records, re ports, or information, or particular part thereof, may be disclosed to other officers, employees, or authorized representatives of the United States concerned with car rying out the provisions of the act or when relevant in any proceeding under the act. 61.16 State authority, (a) The provisions of this part shall not be construed in any manner to pre clude any State or political subdivision thereof from: (1) Adopting and enforcing any emis sion limiting regulation applicable to a stationary source, provided that such (a) Asbestos mills: There shall be no visible emissions to the outside air from any asbestos mill except as provided In paragraph (f) of this section. Outside storage of asbestos materials is not con sidered a part of an asbestos nulL ib> Roadways: The surfacing of road ways with asbestos tailings Is prohibited, except for temporary roadways on an area of asbestos ore deposits. The deposi tion of asbestos tailings on roadways cov ered with snow or ice is considered "sur facing." <ci Manufacturing: There shall be no visible emissions to the outside sir, ex cept as provided in paragraph <f) of this section, from any building or struc ture in which the following operations are conducted or directly from any of the following operations if they are con ducted outside of buildings or structures. (1) The manufacture of cloth, cord, wicks, tubing, tape, twine, rope, thread, yarn, roving, lap, or other textile ma terials. <2 The manufacture of cement prod ucts. (3) The manufacture of fireproofing and insulating materials. (4 The manufacture of friction products. (5) The manufacture of paper, mill board. and felt. load-supporting structural member, shall be wetted and removed from any build ing. structure, facility, or installation subject to this paragraph before wreck ing of load-supporting structural mem bers is commenced. The friable asbestos debris shall be wetted adequately to in sure that such debris remains wet during all stages of demolition and related han dling operations. cii) No pipe or load-supporting struc tural member that is covered with fri able asbestos insulating or fireproofing material shall be dropped or thrown to the ground from arijr' building, structure, facility, or Installation subject to this paragraph, but shall be carefully low ered or taken to ground level. (iii) No friable asbestos debris shall be dropped or thrown to the ground from any building, structure, facility, or in stallation subject to this paragraph or from any floor to any floor below. For buildings, structures, facilities, or in stallations, 50 feet or greater in height, friable asbestos debris shall be trans ported to the ground via dust-tight chutes or containers. (3) Sources subject to this paragraph are exempt from the requirements of 3! 61.05'a). 61.07, and 61.09. (4) Any owner or operator of a dernolttion opemtion who intends to demolish a emission limiting regulation is not less <61 The manufacture of floor tile. building, structure, facility, or installa stringent than the standards prescribed <7) The manufacture of paints, coat tion to which the provisions of this para under this part. 12) Requiring the owner or operator of a stationary source, other than a sta ings. caulks, adhesives, sealants. <8) The manufacture of plastics and rubber materials. <9> The manufacture of chlcrine. graph would be applicable but which has been declared by proper State or local authority to be structurally unsound and winch is-in danger of imminent collapse tionary source owned or operated by the <t< Demolition: Any owner or opera is exempt from the requirements of this United States, to obtain permits, licenses, tor of a demolition operation who intends, parapnph other than the reporting re or approvals prior to initiating construc tion, modification, or operation of such source. to demolish any institutional, commer cial, or industrial building (Including apartment buildings having more than four dwelling units), structure, facility. quirements specified by paragraph id1 <1' of this section and the wetting of friable asbestos debris as specified by pai.-i.raph (d/(3)<i> of this section. FEDERAL RIG STIR, VOl. 38, NO 64--FRIDAY, AFg:l 6, 1973 010794 SS: ;i> RULES AND REGULATIONS (e> Spraying: There shall be no v isible only for so long as it lakes to shut down Oi> "Incinerator" means any furnace emissions to the outside sir from the ih? operation generating the particulate used in the process of burning waste for sprsy-on application of materials con aibestos material. the primary purpose of reducing the taining move than 1 percent asbestos, on a dry weight basis, used to insulate or 61.21 Reporling. volume of the waste by removing com bustible matter. fireproof equipment and machinery, ex cept as provided in paragraph id of this The owner or operator oi any existing source to which tins subparc is applicable in "Propellant" means a fuel and oxi dizer physically or chemically combined section. Spray-on materials used to insu late or fireproof buildings, sirir.tuics. shall, within 90 days after the effective date, provide the following information which undergoes combustion to provide rocket propulsion. pipes, and conduits shall contain less than 1 percent asbestos on a dry weight basis. to the administrator: (a) A description of the emission con trol equipment used [or each process; (j) "Beryllium alloy" means any metal to which beryllium has been added in order to increase its beryllium content Mi Sources subject to this paragraph ib) It a fabric filter device is used to and which contains more than 0.1 per are exempt from the requirements of control emissions, the pressure drop cent beryllium by weight. 5 Gl.OSia). 5 61 07, and 5 61.09. (2) Any owner or operator who inlends to spray asbestos materials to insulate or acioss the fabric filter in inches water gage. (1> If the fabric filter device utilizes a (k) "Propellant plant" means any facility engaged in the mixing, casting, or machining of propellant. fireproof buildings, structures, pipes, con woven fabric, the airflow permeability duits, equipment, and machinery shall in ft:'min/ft1; and, if the fabric is syn 61.32 Emission standard. report such intention to the administra thetic, indicate whether the fill yarn is (a) Emissions to the atmosphere from tor at least 20 days prior ta tire com spun or not spun. stationary sources subject to the provi mencement of the spraying operation. (2) If the fabric filter device utilizes sions of this subpart shall not exceed 10 Such report shall Include the following a felted fabric, the density In oz/yd:, the grains of beryllium over a 24-hour period, information: minimum thickness in inches, and the except as provided in paragraph (b) of (i) Name of owner or operator. airflow permeability in ft7min/ft\ this section. (11 > Address of owner or operator. (iii) Location of spraying operation. (iv) Procedures to be followed to meet the requirements of this paragraph. (f) Rather than meet the no-vtsibleemisslon requirements of paragraphs (a), (ci Such information shall accompany the information required by ( 61.10. The appropriate form is contained in appen dix A to this part. Subpart C--National Emission Standard for Beryllium (b) Rather than meet the require ment of paragraph (a) of this section, an owner or operator may request ap proval from the Administrator to meet an ambient concentration limit on beryl lium in the vicinity of the stationary source of 0.01 /ig/m*, averaged over a (c), and (e) of this section, an owner or 61.30 Applicability, 30-day period. operator may elect to use the methods The provisions of this subpart arc ap (l) Approval of such requests may be specified by } 61.23 to clean emissions plicable to the following stationary granted by the Administrator provided containing particulate asbestos material sources: that: before such emissions escape to, or ore (a) Extraction plans, ceramic plants, (1) At least 3 years of data is avail vented to, the outside air. foundries, incinerators, and propellant able which in the Judgment of the Ad g 61.23 Air-cicaning. plants which process beryllium ore, beryl ministrator demonstrates that the fu If air-cleaning Is elected, as permit ted by { 61.22(f), the requirements of this section must be met. lium, beryllium oxide, beryllium alloys, or beryllium-containing waste. (bi Machine shops which process beryllium, beryllium oxides, or any alloy ture ambient concentrations of beryllium in the vicinity of the stationary source will not exceed 0.01 Ag/m*. averaged over a 30-day period. Such 3-year period shall (a> Fabric filter collection devices when such alloy contains more than 5 be the 3 years ending 30 days before the must be used, except as noted in para percent beryllium by weight. effective date of this standard. graphs (b) and (c) of this section. Such (ti) The owner or operator requests devices must be operated at a pressure 61.31 Definitions. such approval in writing within 30 days drop of no more than 4 inches water gage, Terms used in this subpart are de after the effective date of this standard. as measured across the filter fabric. The fined in the act. In subpart A of this Mil) The owner or operator submits a airflow permeability, as determined by part, or in this section as follows: report to the Administrator within 45 ASTM method D737-69, must not exceed (a) "Beryllium" means the element days after the effective date of this 30 ftyznin/ft* for woven fabrics or 35 beryllium. Where weights or concentra standard which report includes the fol ftymin/ft' for felted fabrics, except that tions are specified, such weights or con lowing Information: 40 ft'/mln/ft* for woven and 45 fty centrations apply to beryllium only, (n) Description of sampling method min/ft* for felted fabrics is allowed for excluding the weight or concentration of including the method and frequency of filtering air from asbestos ore dryers. any associated elements. calibration. Each square yard of felted fabric must weigh at least 14 ounces and be at least one-sixteenth inch thick throughout. Bynthetic fabrics must not contain fill yam other than that which is spun. <b> If the use of fabric filters creates a fire or explosion hazard, the adminis trator may authorize the use of wet col lectors designed to operate with a unit (b) "Extraction plant" means a fa cility chemically processing beryllium ore to beryllium metal, alloy, or oxide, or performing any of the intermediate steps in these processes. (ci ` Beryllium ore" means any natu rally occurring material mined or gathered for Its beryllium content. (d> "Machine shop" means a facility (b> Method of sample analysis. (ci Averaging technique for determin ing 30-day average concentrations. <d) Number, identity, and location (address, coordinates, or distance and heading from plant) of sampling sites. 'ci Ground elevations and height above ground of sampling inlets. contacting energy of at least 40 inches performing cutting, grinding, turning, </> Plant and sampling area plots water gage pressure. honing, milling, deburring. lapping, showing emission points and sampling (c) The administrator may authorize the use of filtering equipment other than that described in paragraphs (a) and (b> of tins section if the owner or operator electrochemical machining, etching, or other similar operations. (e) "Ceramic plant" means a manu facturing plant producing ceramic items. sites. Topographic features significantly affecting dispersion including plant building heights and locations shall be included. demonstrates to the satisfaction of the (fi "Foundry" means a facility en 'Oi Information necessary for esti administrator that the filtering of par gaged in the melting or casting of mating dispersion including stack height, ticulate asbestos material is equivalent beryllium metal or alloy. inside diameter, exit gas temperature, to that of the described equipment. (g> ` Beryllium-containing waste" exit velocity or flow rate, and beryllium (d) All air-cleaning equipment au- means material contaminated with concentration. thoi ized by this section must be properly beryllium and/or beryllium compounds 'h) A description of data and proce installed, used, operated, and maintained. used or generated during any process or dures (methods or models) used to de Bypass devices may be used only during operation performed bv a source subject sign the air sampling network (i c.. num upset or emergency conditions and then to this subpart. ber and location oTsampling sites). FEOE'Al H'CSTER, VOL 3S, NO. 66--FRIDAY, APRIL 6 - 010795 SUi.ES ANO REGULATIONS Ai samplm;.: data uiur-i.'inj; Ijei-y 1 - Jr. .'.'.oid'.r.ce w.'li a plan approved by Lefore the close of the r.ext b>Lsi::exs c ;. hum concentrations in me vicinity cf the to" AJmir.iotraior. Such sites shall be following determination cf such results. stationary souicc for ttie 3-yenr period lot .;i<d in such a manner -.is is calculated (ci Records of atr sampling test results specified in paragraph (bull of this to detect maximum concentrations of and other data needed to determine in section. Tins data shall tie presented bervlltum in the ambient air. tegrated intermittent concentrations chronologically and include the beryl <h> All monitoring sites shall be op- shall be retained at the source and made lium concentration and location of each eiuteri continuously except for a reason available, for inspection by the Adm.ii- individual sample taken by the network able time allowance for instalment main lwiator for a minimum of 2 years. and the corresponding 30-day average tenance and calibration, for changing (d) The Administrator shall be noti ben Ilium concentrations. filters, or for replaceniet of equipment fied at least 30 days prior to an air sam (2) Within CO days after receiving reeding major repair. pling test, so that he may at his epuon such report, the Administrator null notify <c> Filters shaii be analyzed and con observe the test. the owner or operator ip. wining whether approval is granted or denied Prior to centrations calculated within 30 days after filters are collected. Records of 61.4 4 Stark sampling. clen) ing approval to comply with the pro concentrations at all sampling sites and (a) Sources subject to 5 61.42(b) shall visions of paragraph (b) of this section, other data needed to determine such con be continuously sampled, during release the Administrator will consult with centrations shall be retained at the source of combustion products from the tank, in representatives of the stationary source and made available, for inspection by the .such a manner that compliance with the for which the demonstration report was Administrator, for a minimum of 2 years. standards can be determined. The pro submitted. id' Concentrations measured at all visions of j 61.14 shall apply. ic> The burning of beryllium and/or sampling sites shall be reported to the (b) All samples shall be analyzed, and bervllium-contaimng waste, except pro Administrator every 30 days by a regis beryllium emissions shall be determined pellants, is prohibited except in incinera tered letter. within 30 days after samples are taken tors, emissions from which must comply <e) The Administrator may at any time and before any subsequent rocket motor with the standard. require changes in, or expansion of, the firing or propellant disposal at the given 61.33 Snu-k sampling. (a) Unless a waiver of emission testing is obtained under { 61.13, each owner or operator required to comply with { 61.32(a) shall test emissions from his source. (1) Within 90 days of the effective date in the case of an existing source or a new source which has an initial startup date preceding the effective date; or (2) Within 90 days of startup in the case of a new source which did not have an initial startup date preceding the ef fective date. (b) The Administrator shall be noti fied at least 30 days prior to an emission test so that he may at his option observe the test. (c> Samples shall be taken over such a period or periods as are necessary to ac curately determine the maximum emis sions which will occur in any 24-hour period. Where emissions depend upon the relative frequency of operation of differ ent types of processes, operating hours, operating capacities, or other factors, the calculation of maximum 24-hourperiod emissions will be based on that combination of factors which is likely to occur during the subject period and which result In the maximum emissions. No changes In the operation shall be made, which would potentially increase emissions above that determined by the most recent source test, until a new emis sion level has been estimated by calcula tion and the results reported to the Ad ministrator. (d) All samples shall be analyzed and beryllium emissions shall be determined within 30 days after the source test. All determinations shall be reported to the Administrator by a registered letter dis patched before the close of the next busi ness day following such determination <e> Records of emission test results and other data needed to determine total emissions shall be retained at the source and made available, for inspection by the sampling network. Subpart D--National Emission Standard for Beryllium Rocket Motor Firing 61.40 Applicability. The provisions of this subpart are ap plicable to rocket motor test sites. 61.41 Definitions. Terms used In this subpart are defined In the Act, In Subpart A of this part, or in this section as follows: (a) "Rocket motor test site" means any building, structure, facility, or installa tion where the static test firing of a beryllium rocket motor and/or the dis posal of beryllium propellant is conducted. (b) "Beryllium propellant" means any propellant Incorporating beryllium. 61.42 Emiasion standard. (a) Emissions to the atmosphere from rocket-motor test sites shAll not cause time-weighted atmospheric concentra tions of beryllium to exceed 75 microgram minutes per cubic meter of air within the limits of 10 to 60 minutes, accumulated during any 2 consecutive weeks, In any area In which an effect adverse to public health could occur. <b) If combustion products from the firing of beryllium propellant are col lected In a closed tank, emissions from such tank shall not exceed 2 grams per hour and a maximum of 10 grams per day. 61.43 Emission tc-ling--rocket finite or propellant tli-posal. (R> Ambient air concentrations shall be measured during and after firing of a rocket motor or propellant disposal and tr. such a manner that the effect of these emissions can be compared with the standard. Such sampling techniques shall he approved by the Administrator. <b> All samples shall be analyzed and results shall be calculated within 30 day's site. All determinations shall be reported to the Administrator by a regnstered let ter dispatched before the close of the next business day following such deter minations. (o Records of emission test results and other data needed to determine total emissions shall be retained at the source and made available, for Inspection by the Admuiistrator, for a minimum of 2 years. (d) The Administrator shall be noti fied at least 30 days prior to an emission test, so that he may at his option observe the test. Subpart E--National Emission Standard for Mercury 61.50 Applicability. The provisions of this subpart are ap plicable to those stationary sources which process mercury ore to recover mercury, and to those which use mercury chloralkali cells to produce chlorine gas and alkali metal hydroxide. 61.51 Definitions. Terms used in this subpart are defined in the act. In subpart A of this part, or In this section as follows: (a) "Mercury" means the element mer cury, excluding any associated elements, and includes mercury In particulates, va pors. aerosols, and compounds. ib) "Mercury ore" means a mineral mined specifically for Its mercury con tent. (c) "Mercury ore processing facility" means a facility processing mercury ore to obtain mercury. id) "Condenser stack gases" mean the gaseous effluent evolved from the stack of processes utilizing heat to extract mer cury metal from mercury ore. (e> "Mercury chlor-alkuJi cell" means a device which is basically composed of an clectrofvzer section and ft rienuiier (decomposer) section and utilizes mer cury to produce chlorine gas, hydrogen gas. and alkali metal hydroxide. Administrator, for a minimum of 2 years. after samples axe taken and before any (f) "Mercury chlor-alkah elec trolyze; ' 61.31 Air sampling. subsequent rocket motor firing or pro means an electrolytic device v.-hhli is par: pellant disposal at the given site. All re of a mercury chlor-alkah cell and utilizes <a' Stationary sources subject to sults shall be reported to the Adminis a flowing mercury cathode to pro.u.e { 61.32(b) shall locate air sampling sites trator by a registered letter dispatched chlorine gas and alkali metal amahr.m FEEERAl REGISTER, VOl 3E, NO. 16--'RIOAV, AP.TII 6 IV7T -010796 ss:',2 P.ULES AND REGULATIONS <2' "Denuder" means a ho: izoi'tul or date in the case of an existing source or the Administrator, for a minimum of vertical container which is part of a mer a new source which has an initial startup 2 years. cury chlor-alkali ceh and in which water date preceding the effective date; or 'c> Mercury chlor-alkali plants__ and alkah metal amalgam are converted tiii Within 90 days of startup in the cell room ventilation system. to alkali metal hydroxide, mercury, and case of a new source which did not have (1) Stationary sources using mercurv hydrosen gas in a short-circuited, elec an initial'startup date preceding the ef chlor-alkali cells may test cell room trolytic reaction. fective date. emissions in accordance with paragraph <h> "Hydrogen gas stream" means a <21 The Administrator shall be noti <c)'2i of this section or demonstrate hydiogen stream formed in the chior- fied at least 30 days prior to an emission compliance with paragraph <c> (4) of this alkali cell denuder. test, so that he may at his option observe section and assume ventilation emissions in "End box" means a containers) the test. of 1.300 gms/day of mercury. located on one or both ends of a mercury * 31 Samples shall be taken over such '2i Unless a waiver of emission test chlor-alkali electrolyzer which serves a period or periods as are necessary to ing is obtained under 5 61.13, each owner as a connection between the electrolyzer accurately determine the maximum emis or operator shall pass all cell room air and denuder for rich and .stripped sions which will occur in a 24-hour in forced gas streams through stacks amalgam. period. No changes in the operation shall suitable for testing, iji "End box ventilation system" be made, which would potentially in 0) Within 90 days of the effective date means a ventilation system which col crease emissions above that determined In the case of an existing source or a new lects mercury emissions froin tne end- by the most recent source test, until the source which has an initial startup date boxes. the mercury pump sumps, and new emission has been estimated by cal preceding the effective date; or their water colection systems culation and the results reported to the ui) Within 90 days of startup In the iki "Cell room" means a structure's' Administrator. case of a new source which did not have housing one or more mercury electro (4) AU samples shall be analyzed and an initial startup date preceding the lytic chlor-alkali cells. mercury emisions shall be determined effective date. M.li2 Emirrion standard. within 30 days after the source test. All (3) The Administrator shall be noti the determinations will be reported to fied at least 30 days prior to an emission Emissions to the atmosphere from sta the Administrator by a registered letter test, so that he may at hrs option observe tionary sources subject to the provisions dispatched before the close of the next the test. of this subpart shall not exceed 2,300 business day following such determina (4) An owner or operator may carry grams of mercury per 24-hour period. tion. out approved design, maintenance, and 61.S3 Slack sampling. t5> Records of emission test results housekeeping practices. A list of ap ta> Mercury ore processing facility. (1) Unless a waiver of emission testing is obtained under f 61.13. each owmer and other data needed to determine total emissions shall be retained at the source and made available, for Inspection by proved design, maintenance, and house keeping practices may be obtained from the Administrator. or operator processing mercury ore shall test emissions from his source, APPENDIX A til Within 90 days of the effective date in the case of an existing source or National Emission Standards for Hazardous Air Pollutants a new source which has an initial start Con^liance Status Information up date preceding the effective date: or (ii) Within 90 days of startup in the I. SOURCE REPORT case of a new source which did not have an initial startup date preceding the ef fective date. t3) The Administrator shall be noti fied at least 30 days prior to an emission test, so that he may at his option observe the test. Instructions! Owners or operators of sources of hazardous pollutants subject to the National Emission Standards for Hazardous Air Pollutants are required to submit the informetlon contained in Section I to the appropriate EPA USE ONLY k "t * fc ` 13 'Tt -u_l 19 I 'AQC1k I lW>' I 28 . I "DC LJ <3> Samples shall be taken over such Environmental Protection Agency a period or periods as are necessary to Regional Office before (date which accurately determine the maximum emissions which will occur in a 24-hour is 90 days after the standards are promulgated). A listing Of regional offices Is provided in I 61.04. period. No chances in the operation shall be made, which would potentially In A. SOURCE INFORMATION. crease emissions above that determined by the most recent source test, until the new emission level has been estimated by 1 IdentlflcatlonAocatlon - Indicate the name and address of each source. calculation and the results reported to A29 the Administrator. (4) Ail samples shall be analyzed, and ccp(?wtV nXme mercury emissions shall be determined within 30 days after the source test. Each determination will be reported to the Ad A49 l--I--NJLUMBER ' A68. ...............1 ministrator by a registered letter dis- >Uched before the close of the next busi B19 833 838 ness day following such determination. <S) Records of emission test results I a- a- c'iW and other data needed to determine total emissions shall be retained at the source LzMrJ~ and made available, lor inspection by the Administrator, for a minimum of 2 years. < b Mercury chlor-alkali plant--hy 2. Contact - Indicate the name and telephone mmber of the owner or operator or other responsible official whom EPA say contact con drogen and end-box ventilation gas cerning this report. streams. D Unless a waiver of emission test ing is obtained under 1 61.13, each owner or operator employing mercury' chlor- 839 * ill... TtSJTE1- B53. alkali cell(s) shall test emissions from his source. to Within 90 days of the effective BS4 ``TELEPHONE' Jfj FEDERAL REGISTER, VOl 38, NO. 66--fRIDAY, APRIL 6, 1973 010797 S'JLES AND REGULATIONS Ss:t:T FEDERAL REGISTER, VOL 38. NO. 64-- FRIDAY, APRIL 6, 1973 M ** U u M * PC 4O-> C --cH +Mj El uT)j ECU*iTJ O a k I r O*" tl i_ 3*- C C O |lf- c- u So-Jg S S^Js * <B2|I P O SL ***5*6*K 5kTi cgVvVu- fr*X>EflCN<U<eu^ hkO 6 X v- ** .5 |fe1l&g 4 5 *- wee 3 * Sg e0> A* llgfcg* *> c e ^ e o ** M O > k VI c *- oo.^O v C | r- v* *- c a m S C?S--?E CJft-- MM Co > X4-* *O- X ^-1k->5r* 4* C > V-* z Ofc. 3 UC 3 VI U 1"XO*1iW>j>tow***0cW*--O4VmMV3tO- 010798 RUIE3 and regulations 35 < &" n12v uu a-. *e *- O. --C rQ". OtO*J 4Ow E* O.*-- O LL asCl *- A5* n 2s > a - k 73 co |S 2 a C- Ac > u W 7" c- c ***MOO L O M r-- II (LOI jSSE sS5 O *-- So VA 3A *rt O A 4 OL> fmMc- L i.S-2 O k* *-* 7*O3; lreAl --7Ir3Q3~ v> J3 O Cl M wMCc uaOL . -LuaVI. O r- ID La- -C> <u3. V<u* Jd) Mum -O 1 ** Cl `r- -C O > 2 U>a>-| omuw*&s*,<Ua-:ui -tsx----X JVaCtI J*1( 4L-l V-- <C A--- jz jz v ***** it Cm o> Ac = M O 4* *0 c ct V Cat |^f u MCl LV Ofc n FEDERAL REGISTER. V O L 3S, NO. 66-- FRIDAY. APRIL 6, 1973 010799 t'i'-J.'S d oo. o i v1 V- Ma> Io o>- - jV * c ua > f--oa&ou -kawua --cr c *E Ob ko O J3 I* *tset 5 O A O lit4SS 5i|j E e ^ o.**>*;** lb M-- Co? **S Wc O Cl 6c 5u --'Xv,-i* S v. -- oe C-- i ti-- |B^-s4-> I5 5 El. I.U OV kO.l C Cl oU Lo >p* uMl *k< sSc Oi a 44 OA <* -- J O > & esi CO VI 4Al jCl *> C k O a o d. 3<o CE*1- 1 4> cC- Cl OU 2S < c- MC o $ o V c 4-* C X) OuV--Ii o*0a-/ wOc ' -' x t- tt UJ O O' U. O of U> 4rt 3 C. - ca XO *- .+<cJ-ToJ k >VT} cc kOk01 > - ; -- "5 I I * O J> -- C C l *4 V 3 C i o a ee 4- V! v r* No 66--Pt n- rc < < o *1 M oI o 6 z o o > 010800 vvs:;o RUi.ES AND REGULATIONS <>f particulate matter The fil older i;ur; provide a positive against leakage frn outside or around the filter A healing capable of maintaining the tr^er at 0 minunum temperature o< 25U* F. should be used to prevent condensation from occur ring. 2.1 8 Baromeier. To measure atmospheric pressure to 0 1 in Hg. 2 2 Measurement of stack conditions (stack pressure, temperature, moisture and 1 clority)--2.2 1 Fifot tube. T) pe S. or equivalent. with a coefficient with i:i 3 percent over the working range. 2 2.2 Dxflerential pressure ga'iQc Inclined manometer, or equivalent, to measure veloc ity held to within 10 percent of the minimum value Wicromauometers should he used It warranted. 2 23 Temperature gauge Any tempera ture measuring device to measure i.t.vcW tem perature to within l* F. 2.2.4 Pressure gauge. Pitot lube and in clined manometer, or equlvAien., tc. measure stack pressure to within 0.1 m Kg. 2.2.5 Moisture dctermiv'itto* Wet and dry bulb thermometers, drying tubes, con densers, or equivalent, to de'r-mirte staci gas moisture content to aKh.n 1 percent. 2 3 Sample recovery--2J1 Lecfc-ferj glass sampfe bottles. 500 ml and ion n * a nh Teflon lined tops. 2.3.2 Graduated cylinder. 250 ml. 2u3 3 Plastic far, Approximate!? 30C ml. 2 4 Analysis--2.4.1 SpCLfrup.Hofometer. To measure absorbance at 253.7 nm Perkin Elmer Model 303. with a cylindrical gas cell (approximately 1.6 in. O.D. * 7 ir..j with quartz glass windows, and hollow cathode source, or equivalent. 2 42 Gas sampling bubbler. Tudor scien tific Glass Co , Smog Bubbler, Catalogue No. TP-1150, or equivalent. 2.4.3. Recorder. To match output of spec trophotometer. 3. Reagents--3.1 Stock reagents--3.1.1 Potassium iodide. Reagent grade. 3.1.2 Distilled water--3.1.3 Potassium iodide solution, 25 percent. Dissolve 250 g of potassium iodide (reagent 3.1.1) In dis tilled water and dilute to 1 to l. 3.1.4 Hydrochloric acid. Concentrated. 3 1.5. Potassium iodate. Reagent grade. 3.1.6 Iodine monochloride (ICl) 1.0M. To 600 ml. of 25% potassium Iodide solution (reageot 3.1.3), add 800 ml. of concentrated hydrochloric acid. Cool to room temperature. With vigorous stirring, slowly add 135 g. of potassium Iodate and continue stirring until aU free iodine has dissolved to give a clear orange-red solution. Cod to room tempera ture and dilute to 1800 ml. with distilled water. The solution should be kept in amber bottles to prevent degradation. 9.1.7 Sodium hydros*** pellets. Reagent grade. 3.13 AHtrie arid. Concentrated. 8 1.9 Hydrosyiamine rulfate. Reagent grade. 3.1.10 Sodium chloride. Reagent grade. 33 An<jtj/*w--3 3 l Splinti Imrlroj 10 N--Dissolve 400 g of indium hvlrntiue peliets in distilled water and dilute to 1 to 1. 3.12 Reducing agent, 12 percent hydroxy/amin* sulfate, 12 percent sodium chlo ride.--To 60 ml of distilled water, add 12 g of hydroxylamtne sulfate and 12 g of sodium chlonde. Dilute to 100 ml. This quantity is sufficient for 20 analyses and must be pre pared daily. 333 Aeration gas--Zero grade air. 3 3 4 Hydrochloric and. 0.3N --Dilute 2*> 5 mi of concentrated hydrochlouc acid to l to 1 with distilled water 3 4 Standard mercury solution<--34 1 Stock solution.--Add 0 1354 g of mercuric chlonde to 80 ml of 0.3N hydrochloric aud. After the mercuric chloride has dissolved, add 0 2N hydrochloric acid and adjust the volume to 100 ml. One ml of this solution Is equivalent to l mg of free mercury. 3 4.2 Standard solutions.--Prepare cali bration solutions by serially diluting the stock solution (3.4.1) with 0.3N hydrochlo ric arid. Prepare solutions at concentrations In the linear working range for the instru ment to be used. Soutions of 0.2 /ig/ral. 0 4 and 0.6 Mg/ml have been found ac ceptable for most Instruments. Store aii solutions In glass-stopperod. glass bottles. These solutions should be stable for at least 2 months; however, periodic checks should be performed to Insure quality. 4. Procedure.--4.1 Guidelines for source testing are detailed In. the following sections. These guidelines are generally applicable, however, most sample sites differ to some degree and temporary alterations such os stack extensions or expansions often are re quired to ensure tbe best possible sample site. Further, since mercury Is hazardous, care should be taken to minimize exposure. Finally, since tbe total quantity of mercury to be collected generally is small, the test must be carefully conducted to prevent con tamination or loss of sample. 4.2 Selection of a sampling site and mini mum number of traverse points: 42.) Select a suitable sampling site that Is as close as Is practicable to the point of atmospheric emission. If possible, stacks smaller than 1 foot in diameter should not be sampled. 4 2 2 The sampling site should be a* least t i*41it stack or duct diameters downstream and two diameters upstream from any fto* disturbance cucb aa a bend, expansion, or contraction. For a rectangular cross section, determine an equivalent diameter from the following equaliou: 2LW D- = rzw where D' = Equivalent diameter. L -z Length. W n Width. I01-' 4 2.3 When the above sampling site cri teria can be met, the minimum number of traverse points is four (4) for stacks l foot in diameter or less, eight (8) for staexs larger t han i foot but 2 feet in diameter or less, and twelve (12) for stacks larger than 2 feet. 4 2 4 Some sampling situations may ren der the above sampling site criteria Imprac tical. When thLs is the case, choose a con venient sampling location and use figure 101-3 to determine tbe minimum number of traverse points. However, use figure 101-3 only for stacks 1 foot in diameter or larger. 4 2.6 To use figure 101-3, first measure tho distance from the chosen sampling loca tion to the nearest upstream and downstream disturbances Divide this distance by the diameter or equivalent diameter to deter mine the distance in terms of pipe diameters Determine the corresponding number of traverse points for each distance from fig ure 101-3. Select the higher of the two num bers of traverse points, or a greater value, such that for circular stacks the number is a multiple of four, and for rectangular stacks the number follows the criteria of section 4.3.2, 4.2.6 If a selected sampling point Ls closer than 1 inch from the stack wall, adjust the location of that point to ensure that the sample is taken at least 1 inch away from tbe wall. 4.3 Cross sectional layout and location of traverse points: 4.3.1 For circular stacks locate the trav erse points on at least two diameters accord ing to figure 101-4 and table 101-1. Tbe traverse axes shall divide the stack cross section into equal parts. NUMBER OP OUCT DIAMETERS UPSTREAM (0I5TANCE AJ gj 2 **{ 2 3 l.U Mercuric chloride. Reagent grade. 32 Sampling--32.1 Absorbing volution, 0.1M let. Dilute 100 ml. of the I.OM ICl stock solution (reagent 3.1 6) to 1 to 1 with distilled water. The solution should be kept in glass bottles to prevent degradation. Tills reagent should be stable for at least 2 o gj g s g | months; however, periodic checks should be performed to Insure quality. 3 2.2 Wash acid. 1:1 V/V nitric arid-- water. sg 3 2-7 Distilled, defaulted icatrr, 3.2.4 Silica gel. Indicating type. 6 to 16 mesh dried at 350* F. for 2 hours. 32 5 Pilfer (optional). Glass fiber. Mine Safety Appliances 1106BH, or equivalent. A filter may be necessary to coses where tbe gaa stream to be sampled contains large quantities of particulate matter. Figure 102-3. M*nmum of traverse points, FfDEftAt ScGJSfflt, VOL 38, NO. 66--FRIDAY, Ami 6 1773 ^_ _010801 ftUkSJ HMW Tj,,:a 101-1. Lr'cjticn of traverse r^'n:-5 in c"`- r (Percent of stac1: diameter from inside wail to traverse point) Traverse point number fiur.ber of traverse points on i tfismete r on a diameter 2 4 6 8 10 12 14 16 ie 20 22 24 1 14.6 6.7 4.4 3.3 2.5 2.1 1.8 1.6 1.4 1.3 1.1 1.1 2 85.4 25.0 14.7 10.5 8.2 6.7 5.7 4.9 4,4 3.9 3.5 3.2 3 1 75.0 29.5 19.4 14.6 11.8 9.9 8.5 7.5 6.7 6.0 5.5 A 93.3 70.5 32.3 22.8 17.7 14.6 12.5 10.9 9.7 8.7 7.9 5 B5.3 67.7 34.2 25.0 20.1 16.9 14.6 12.9 11.6 10.5 6 95.6 80.6 65.8 35.5 26.9 22.0 18.8 16.5 14.6 13.2 7 89.5 77.4 64.5 36.6 28.3 23.6 20.4 18.0 16.1 8 96.7 85.4 75.0 63.4 37.5 29.6 25.0 21.8 19.4 9 91.8 82.3 73.1 62.5 38.2 30.6 26.1 23.0 10 97.5 88.2 79.9 71.7 61.6 38.8 31.5 27.2 n 93.3 05.4 78.0 7C.4 61.2 39.3 32.3 12 97.9 90.1 83.1 76.4 69.4 60.7 39.8 13 94.3 87.5 B1.2 75.0 68.5 60.2 14 98.2 91.5 85.4 79.6 73.9 67.7* 15 95.1 69.1 83.5 78.2 72.8 16 98.4 92.5 87.1 82.0 77.0 17 95.6 90.3 85.4 80.6 18 9a.6 93.3 88.4 83.9 19 96.1 91.3 86.8 20 98.7 94.0 89.5 21 96.5 92.1 22 98.9 94.5 23 96.8 24 98.9 Ftgur* 1&14. Cwi tl i*ftw^ar ttack J(tM M 12 aqtal *w, wtUi iravtrw p*Ai at wr.tfo.d *t Kh . 4.3.2 For rectangular stacks divide the cross section into as nuuv equal rectangular areas as traverse points, such that the ratio of the length to the width of the elemental areas Is between one and two. Locate the traverse points at the cemroKl of each equal area according to figure 101-5. 4.4 Measurement of stack conditions: 4.4.1 Bet up the apparatus as shown In figure 101-2. Make sure all connections are tight and leak-free. Measure the Telocity head and temperature at the tmverse point* specified by scctlou 4.2 and 43. 4.43 Measure the static pressure In the stack. 4.43 Determine the stack gas moisture. 4.4.4 Determine the stack gas molecular weight from the measured moisture content and knowledge of the expected gas stream composition. A standard Orsat analyser has been found valuable at combustion sources. In all cases, sound engineering judgment should be used. FEDERAL REGISTER, VOL 35, NO. 6A--FRlDAT, APRIL 6, 1973 RULES AND REGULATIONS 4.5 Preparation of sampling train4.5 1 Prior to assembly. clean all glassware (probe. Impingers, and connectors) by rinsing .with wash acid, tap water. 0.1M ICI, tap water, and finally distilled water Plai.e 100 ml of 0 1M ICI in each of the first three impingers. and place approximately 200 g of preweighed silica gel in tne fourth impinger. Save 60 ml of the D IM ICI as a blank in the sample analysis. Set up the train and the probe as in figure 101--1. 4 52 If the gas stream to be sampled is excessively dirty or moist, the first impinger may clog or become dilute too rapidly ior suifictent testing. A filter can be placed ahead of the impingers to collect the particulates. An initial empty impinger may also be used to remove excess moisture. If r. fifth impinger is required, the final impinger may have to be carefully taped to tac outside of the sample box 4.5 3 Leak check the sampiin? train at the sampling site. The leakage race should not be in excess of 1 percent of tbe desired sam pling rate. IX condensation in the probe or filter is a problem, probe awl fi't-fr beaters will be required. Adjust the hca.ers to pro vide a temperature of at least JS0* F Place crushed ice around the impingers Add more ice during the test to keep the temperature of the gases leaving the last Impinger at 70* F or less. 4 6 Mercury train operation: 46 1 For each run. record the data re quired on the example sheet shown in figure 101-6 Take readings at each sampling point at least every 5 minutes and when signifi cant changes in stack conditions necessitate additional adjustments In flow rate. 4 62 Sample at a rate of 0.5 to 1 0 cfm Samples shall be taken over such a period or periods as are necessary to accurately determine the maximum emissions whi-li would occur in a 24-hour period. In the case of cyclic operations, sufficient tests shall be made so as to allow accurate determination or calculation of the emissions which will occur over the duration of the cycle. A mini mum sample time of 2 hours is recommended. In some instances, high mercury concentra tions can prevent sampling In one run for the desired minimum time. This Is indicated by reddening in the first impinger as free Iodine is liberated. In this case, a run may be divided Into two or more subruns to en sure that tbe absorbing solutions are not depleted. #uuir_ LOCAtOi. OKAAin. aatc _ MrmaocNO., amnmi rtmaanav. lUMincanM. HLATR gTtWO MOKICNGM.*.. __ NCMiLf MMTIV * _ MM HtAici unmc_ f tAj-wrm K*>nc Of >TACt CTOW MCfCM iiiiim >1 lUVMKFQWf IUW> IMfUNC UMC TN* MSauK I*. --. Vjl *- i:ia wiocrr TUVTWIIUM IV U V MUMI ft1VOlhMK oai uMi nvmnet If 0*tGM**TW war IT* ourur *r rtwtwnM. runwix f th^iii 4 d.v.s, the initial and wash procedure must be followed. 4 8 Analysis: 4 8 I Apparatus preparation.---Clean all glassware according to the procedure of sec tion 4.5 1. Adjust the instrument settings ac cording to the instrument manual, using an absorption wavelength of 253 7 tun. 482 Analysis preparation--Adjust the air delivery pressure and the needle valve to obtain a constant airflow of about 1.3 to/ l /min. The analysis tube should be bypassed except during aeration. Purge the equipment for 2 minutes Prepare a sample of mercury standard solution (3.4 2) according to section 4 8 3. Place the analysis tube in the line, and aerate until a maximum peak height is reached on the recorder. Remove the analysis tube, flush the lines, and rinse the analysis tube with distilled water. Repeat with an other sample of the same standard solution. This purge and analysts cycle la to be re peated until peak heights are reproducible. 483 Sample preparation--Just prior to analysis, transfer a sample aliquot of up to 50 ml to the cleaned 100 ml analysis tube. Adjust the volume to 50 ml with 0.1M ICI if required. Add 5 ml of 10 N sodium hy droxide. cap tube with a clean glasa stopper and shake vigorously. Prolonged, vigorous shaking at this point is aecessary to obtain an accurate analysis. Add 5 ml of the re ducing agent (reagent 3.3.2). cap tube with a clean glass stopper and shake vigorously and immediately in sample line. 4 8 4 Mercury determination.--After the system has been stabilized, prepare samples from the sample bottle according to section 4 8 3. Aerate the sample until a maximum peak height la reached on the recorder. The mercury content Is determined by compar ing the peak heights of the samples to the peak heights of the calibration solutions. If collected samples are out of the linear range, the samples should be diluted. Prepare a blank from the 100 ml bottle according to section 4.84 and analyze to determine the reagent blank mercury level. 5. Calibration.--6.1 Sampling train -- 5 1.1 Use standard methods and equipment as detailed in AFTD-0576 to calibrate the rate meter, pitot tube, dry gas meter, and probe heater (If used). Recalibrate prior to each test series. ArtMCE Fte* 101-4* Field data *. 5.2 Analysis.--54.1 Prepare a calibra tion curve for the spectrophotometer using the standard mercury solutions. Plot the peak heights read on the recorder versus the concentrations of mercury In the standard solutions. Standards should be Interspersed with the samples since the calibration can change slightly with time. A new calibration curve should be prepared for each new set of samples run. 4.6.3 To begin sampling, position tbe nozzle at the Ant traverse point with the tip pointing directly into the gae stream. Im mediately start the pump and adjust the flow to lsokinstic conditions. 6ample for at least 5 minutes at each traverse point; samp ling time must be the same for each point. Maintain isokinetic sampling throughout the sampling period. Nomographs which aid in the rapid adjustment of the sampling rate without other computations are in APTD0576 and are available from commercial sup pliers. Note the standard nomographs are applicable only for type S pitot tubes and mr or a stack gas with an equivalent density. Contact EPA or the sampling train supplier for instructions when the standard nomo graph is not applicable. 4 6.4 Turn off the pump at the conclusion or each run and record the final readings. Immediately remove the probe and nozzle from the stack and handle in accordance with the sample recovery process described In section 4.7. 4.7 Sample recovery: 4.7.1 (All glass storage bottles and the grad uated cylinder must be precleaned as In sec tion 4.5.1). This operation should be per formed la an area free of possible mercury contamination. Industrial laboratories and ambient air around mercury-using facilities are not normally free of mercury contamina tion. When the sampling train Is moved, care must be exercised to prevent breakage and contamination. 4.7.2 Disconnect the probe from the Im pinger train. Place the contents (measured to 1 ml) of the first three Impingers into a 500 ml sample bottle. Rinse tbe probe and all glassware between it and the back half of the third impinger with two 50 ml portions of 0.1M ICI solution. Add these rinses to (he first sample bottle. For a blank, place 80 ml of the 0 1M ICI in a 100 ml sample bottle. If used, place the filter along with 100 rru of 0 1M ICI in another 100 ml sample bottle. Retain a filter blank. Place the silica gel in the plastic Jar. Seal and secure all containers for shipment. If an additional test is desired, the glassware can be carefully double nnsed with distilled water and reassembled. How ever, if the glassware is to be out of use more 6. CatcuXattoru.--6.1 Average dry gas meter temperature, stack temperature, stack pressure and average orlfloe pressure drop. See datasheet (fig. 101-6). 6.2 Dry gas volume.--Correct the sample volume measured by the dry gas meter to stack conditions by using equation 101-2. T {P'" r =] 1: i____ " T. i.T.G eq. 101 2 li> ro l ,, Vm'uiO-- <)( tus U;toiirii tl*- drv .* ft* l". \of satrpi* H-roueii the iliy fu* u.iri-r n>ittiitmii-i). fi T. A\>rnk'* IcinprriiMv rvf 't.v.k pa, *R. Tm r AriTji-p dry cai in*tw Uiu|*niurv. 'R. Pt... ~ Barometric pressure at the orifice meter, inHg. HI - Average pressure drop across the ori fice meter, lnK<0. 13 6 = Specific gravity of mercury. P, = Stack pressure. P.rrstatic pressure. inHg. ,FEDERAL REGISTER, VOL. 3>, NO. 66--FRIDAY. APRIL 6 197] "010803 C ?. Vo'.urr.e of traier repor. Vw.= K.VtlJf ct;. 101-3 vhtrs: tV,Vohimr *1 anfrf vapor tu the g is * irup'i* <>truk ' lonilKiniis), fi*. ft'u^d OU-CT wl^.i jn.f> .uc u l'i -Tot.il vo'uin# of liquid rolled.>0 in imj'iMpr'rs uni mIjl" gel fiyu'c Uil-7;, mi. T, A t< r um ?t.Lck pxs t*mp*r:\turf. r U. f`,i3i.u.k pri'iifi*. 1\,, *t stu'ic 1'nsS'ure, in. Jl^. * 4 Trial p u rnlmi.i r,,,.i-v.,+1'*, cq loi-i wlw'i rI .*i"T>fal volume of pis Mmplr i-t.n k iwnihtmuM, fi*. V. Volume of gx* tlirooyh g.\s ii'rti-r 'n.n U c<m<h. ItCMlO. Il* W.-Volumc of TT.ii*r fxi'or in pr.' sample (st nk condihunO, (iP VOLUME Of L'OU'O *it coutcrio FINAL Mill*. UOULO COUlCTtO 101*1 VOLUME COLLECTED nrinch volme. Mi SILICA CEL, KGHr. * * coNvttt mxtomthto volume vr dividing total wight MCiUll ll DiVUT? OF mil p ^-fl: wcw * ll l-l VOLUME ATI*. mi F<9Le 101-7. Analyhcil di;*. 6 5 Stack gas velocity. Use equation 101-5 to calculate tbe stack gas velocity. RULES ANO REGULATIONS PLAN T DATE________________________________________________ HUN NO._______________________________ ___ STACK DIAMETER, in. ___________________ BAROMETRIC PRESSURE, in. Hg,____________________ STATIC PRESSURE IN STACK (Pg 1. in. Hr). OPERATORS_______________________________________ SS.19 |----------------------------------- 1 ' SCHEMATIC OP STACK CROSS SECTION Traverse point number Velocity head, in. H20 v7 Stack Temperature (0*b. -- p~\j cq. 101-5 her*1 (').** Avornpe ff Juk pus rekyily, Pt scmn-J. K, M ,, ft / !).-m Me \lfi v^^(iu,noic>.;-.,,:7T7D) wbc,` C, (T.W <Va/w Ap/.. thev units arr osnl. Pitci lube eocfliclcnt, <liin*nioi1^. ATPr.ixt stack gns tcniperaliife, *it. 'Avw.ipe JC^ftre root f the wloeifv hvad <il pxa un. IljO)'f* (w ftp. 101-*) Stack prs5ure, /\-Hunr |H(4ire. m. ITp. MoUndur weight olvt.trk pas (wd la.*i>i, the eummaliAfl of the products of the molecular wHirht of wh i-oi:i|iM.i'nt multiplied hv its volumetric ]>ro|iortiou In the raitture, lb./lb. mole. Figure 101-6 shows a sample recording sheet for Telocity traverse data. Use the average* In the laat two oolumna of figure 101-8 to determine the average stack gas velocity from equation 101-6. 6 6 Mercury collected. Calculate the total weight of mercury collected by using equa tion 101-8. Wi = ViCi-V*C* (+VrCr)_.eq. 101-8 where: Wi = total weight of mercury collected, eg. AVERAGE: Figure 101-8. Velocity traverse data. FEDERAL REGISTER, VOL. 33, NO. 66--MIDAV. APRIL 6. 1973 010804 SS in RULES AND REGULATIONS Vi =;Total volume of condensed moisture and IC1 In sample bottle, ml. Ci = Concentration of mercury measured io sample bottle, sg/ml. V**=Total volume of ICl used In sampling (inipinger contents and ad wash amounts). ml C- Blank concentration of mercury in IC* solution. *g/mJ. V/ = Total volume of 1CI used In filter bottle (Lf used), ml. Cr = Concentration of mercury in Alter bottle (if used), .og/ml. 6 7 Total mercury emission. Calculate the total amount of mercury emitted from each stack per day by equation 101-7. This equa tion is applicable for continuous operations. Tor cyclic operations, use only the time per day each stack Is in operation. The total mercury emissions from a source will be the summation of results from all stacks. p TT((0*.^,.86,400 second*/day x iov&s. <q. 101-7 where: Rm Hate of emission, p/day. K, --TotiU wa;bt of mercury col'Kift! *<c. Vtaui-Total volume of ni tampio (mark condition/, ft . - ArMTiye stack p&i velocity, fcrl per srtond. /I,-Stack area, ft1. pling Measurements. Paper presented at the Animal Meeting of the Air Pollution Control Asioc:ation, St Louis. Mo . June 14-19. 1970 II. Smith, W. S.. et al.. Stack Gas Sampling Improved and Simplified with New Equip ment. APCA paper No. 67-119. 1967. 12 Smith, W. S . R. T. Shigehara. and W. F Todd. A Method of Interpreting Stack Sampling Data. PAper presented at the 63d Annual Meeting of the Air Pollution Control Association. St. Louis. Mo.. June 14-19, 1970. 13 Specifications for Incinerator Testing at Federal Facilities PHS. NCAPC. 1967. 14. Standard Method for Sampling Stacks for Particulate Matter. In: 1971 Book of ASTM Standards, part 23. Philadelphia, 1971, ASTM Designation D-2926-71. 15. Vennard, J. K., Elementary Fluid Me chanics. John Wiley and Sons, Lnc.. New York. 1947. a.CTKOO lot. REFERENCE HRROD FOR DfcTER- ormxnatton fasttcvuit* and caseous MER CURY EMISSIONS FROM STATIONARY SOURCES (HYDROGEN STREAMS) 1. Principle end applicability--1.1 Princi- --Particulate and gaseous mercurv emis sions are Isokinetically sampled from the source and collected in acidic iodine monochloride solution. The mercury collected (in the mercuric form) Is reduced to elemental mercury in basic solution by hydrorylamme sulfate Mercury is aerated from the solution and analyzed using spectrophotometry. 1.2 Applicability--ThtS method is appli cable for the determination of particulate and gaseous mercury emissions when the carrier gas stream is principally hydrogen. The method is for use in ducts or stacks at stationary sources. Unless otherwise specified, tins method is not intended to apply to gas streams other than those emitted directly to the atmosphere without further processing. 2. Apparatus--2 1 Sampling train --A sche matic of the sampling tram used by EPA is shown in figure 102-1. Commercial models of this train are available, although complete construction details are described in APTD0501 ,l and operating and maintenance pro* cedures are described in AFTD-0576. The components essential to this sampling train are the following: ACID TRAP 6.8 Isokinetic variation (comparison of velocity of gas In probe Up to stack velocity). r 100 7taltl eq. 101-8 where: Percent of isokinetic samphnp. Total volume of eajaa>u|iciiu^.-k ~omiitions), ft*. /I.-Probe tip area, fl*. -Sampbnp time, err. <*>*."Average steck pas velocity, />-< |tcr v-conJ. 7. evaluation of results--7.1 Determina tion of compliance.--*7.1.1 Each performance test shall consist of three repetitions of the applicable test method. For the purpose or determining compliance with an applicable national emission standard, the average of results of all repetitions shall apply. 7J Acceptable isokinetic results.--7J.1 The following range sets the limit on accept* able Isokinetic sampling results: If 90% ^1^110%, the results are accept able; otherwise, reject the test and repeat. 8. References.--1. Addendum to Specifica tions for Incinerator Testing at Federal Faculties, PHS. NCAPC, Dec. 6.1967. 2. Determining Dust Concentration in a Oas Stream. ASMS Performance Teat Code No. 37. New York. N.Y, 1987. 3. Devorkin. Howard, et aU Air Pollution Source Testing Manual, Air Pollution Con trol DUtrtct, Loe Angeles, Calif.. Nov. 1963. 4. Hatch, W. XL and W. L. Ott, ''Determina tion of Sub-Mlcrogram Quantities of Mercury bv Atomic Absorption Spectrophotometry." Anal. Chem., 40:3068-87,1968. 6. Mark. L. S- Mechanical Engineers' Hand book, McGraw-Hill Book Co.. Inc.. New York. N.Y,, 1951. 6. Martin. Robert M,, Construction Details of Isokinetic Source Sampling Equipment, Environmental Protection Agency, APTD- 0561. 7. Methods for Determination of velocity. Volume. Dust and Mist Content of Gases. Western Precipitation Division of Joy Mfg. Co.. Los Angeles. Calif. Bui. WP-50. 1968. 6 Perry, J. H . Chemical Englne-ra' Hand book. McGraw-Hill Book Co., Inc.. New York, N V.. 1960. 9. Rom, Jerome J,, Maintenance, Calibra tion. and Operation of Isokinetic Source Sam pling Equipment. Environmental Protection Agency. APTD-0S7. 10. Shlgeharm. R. T.. W. F. Todd, and W. S. Smith. Significance of Errors In Stack Sam PUMP Figure 102-1. Mercury sampling train a n Mottle. Stolnlaai ttttl or (lots with thorp, top*ltd leodlog td(t. 3.1 a Probe. Shtothtd Pjrex ' (lost. 3.1 a Pitot tube. Tfpe S (flfura 103-3). or equivalent, with a coefficient within 6 per cent over the working range, attached to probe to monitor stack gas velocity. 3.1.4 Impingert. Four Oreenburg-Smith impLngera connected In series with glass balljoint fittings. The first, third, and fourth implugors may be modified by replacing the tip with one-half loch ID gla*s tube extend ing to one-half inch from the bottom of the fiAftk. 2 15 Acid trap. Mine safety appliances atr line Alter, catalogue No. 81657, with acid ab sorbing cartridge and suitable connections, or equivalent. 2.t 6 Afcferinp syafem. Vacuum gage leak- leas pump, thermometers capable ot measur ing temperature to within 6*P, dry gae meter with 2 percent aocuracy, and related equip ment, described In AFTD-0581, to maintain an Isokinetic sampling rate and to determine sample volume. 2.1.7 Barometer. To measure atmospheric pressure to 0.1 In hg. These documents are available for a nomi nal cost from the National Technical In formation Service. U.S Department of Com merce, 5265 Port Royal Road. Springfield. Va. 22151. * Mention of trade names or commercial products does not constitute endorsement by the Environmental Protection Agency. FEDERAL REGISTER, VOL 36. NO. 68--ANDAY, APRIL 6, WJ ;<-JLSd Ml'tu ACVUIMHWII -'2 Mc-snrt'inrni 'v m`.j.k ron<lu:otu (shirk pressure, terr.fjtrji:ir-.\ moisture, and ic/cc :.*>> --2 21 Fisot Ji.be. Type i>. or equivalent, with a coefficient wilinr. 6 per* cent over thewcrklng ran^e. 222 Differential pressure gage. Inclined manometer, or equivalent, to measure veloc- 334 ft ydroWifunc o ;v D.i-iV *'* ml of concentrated hydrochloric ac-.d to 1 1 with dimmed water. 3 4 Standard mercury soluhon<--7 4 l Stock solution. Add 0 U54 g of mercuric chloride to 60 ml of 0-3N hydrochloric acid. After the mercuric chloride has dissolved, I 2 2 TV* MTHilim; .vce should he at least * v.'.ok or du.t diameter* downstream and two oiameters upstream from any flow disturbance such as a head. expanj;on or contraction. For rectangular cross section, determine an equivalent diameter from the lallowing equation: / head to within 10 percent of the mini n' .:m va' ue. Mjcromanometers should be uied if warranted. 2 ? 3 Temperature gage Any terv.perrv- ture-mexsuring device to measure stack tem perature to Within 1' F. 2 2 4 Pressure gage Pitot tube and in add 0 3N hydrochloric acid and adjust the volume to 100 ml. One rnl of this solution is equivalent to 1 mg of free mercury 3 4 2 Standard solutions. Prepare cali bration solutions by serially diluting the stock solution (3 4 l) with 0 3N hydrochloric acid. Prepare solutions at concentrations in a h e re D. = equivalent diameter L -- length. W = width. clined manometer, or equivalent, to measure stark pressure to within 0.1 in hg. 225 Afoisfiire determination. Drying times, condensers. or equivalent, to deter mine stack gas moisture content in hydrogen to within 2 percent. 23 Sam p/e rccoicry--23 1 Leakiest glass sample bottles 500 ml and 200 ml with Tef lon-lined tops. 2 3 2 Graduated cylinder. 250 ml. 233 Plastic jar. Approximately 300 ml. 2.4 Analysis--2 4.1 Spectrophotometer. To measure absorbAnce at 253.7 nm. Perkin Elmer model 303. with a cylindrical gas cell (approximately 1.5 In o d, x 7 in) with quartz the linear working range for the itistuimeni to be used Solutions of 0 2 *g/m 1. 0 4 *g ml and 0 6 ug ml have been found acceptable for most instruments Store all solutions m glas^-stoppered. glass bottles. These solutions should he stable for at least 2 months: how ever. periodic checks should be performed to insure quality. 4 Procedure. 4.1 Guidelines for source testing are detailed in the following sections. These guidelines are generally apphcabie. however, most sample sites differ to some de gree and temporary alterations such as stack extensions or expansions often are required to insure the best possible sample s.te Fur 4 2 3 When the above sampling site crite ria can be met, the minimum number of traverse points is four (4| for stacks 1 foot in diameter or less, eight (6) for stacks larger than f foot but 2 feet in diameter or less, and twelve (12) for stacks larger than 2 feet. 4 24 Some sampling situations may ren der the Above sampling site criteria Imprac tical. When this is the case, choose a con venient sampling location and use figure 102-3 to determine the irunimum number of traverse points. However, use figure 102-3 only for stacks 1 foot in diameter or larger. 4 2 5 To use figure 102-3, first measure the gloss windows, and hollow cathode source, or equivalent. 242 Gas sampling bubbler. Tudor Scien tific Co. Smog Bubbler, catalogue No. TP1150. or equivalent. ther. since mercury Is hazardous, care should be taken to minimize exposure. Fnally. s.nce the total quantity of mercury to be collected generally is small, the test must be care fully conducted to prevent contamination or distance from the chosen sampling location to the nearest upstream and downstream dis turbances. Dtvide this distance by the di ameter or equivalent diameter to determine the distance m terms of pipe diameters. De 2 4 3 Recorder. To match output of loss of sample. termine the corresponding number of trav spectrophotometer. 4.2 Selection of a sampling site and mini erse points for each distance from figure 3. RengentsSl Stock reagents.--3.1 1 Potassium Iodide. Reagent grade. 3.1.2 Distilled water, 3 1.3 Potassium Iodide solution, 25 per cent.--Dissolve 250 g of potassium Iodide (re mum number of traverse points. 4.2.1 Select a suitable sampling site that Is as close as Is practicable to the point of atmospheric emission. If possible, stacks smaller than 1 foot lu diameter should not 102-3. Select the higher of the two numbers of traverse points, or a greater value, such that for circular stacks the number is a mul tiple of four, and for rectangular stacks the agent 3 11) In distilled water and dilute to be sampled. number follows the criteria of section 4.3.2 I to 1. 3 1.4 Hydrochloric acid. Concentrated. NUUSER or DUCT DIAMETERS UPSTREAM* 3 1.5 Potassium lodate. Reagent grade. (DISTANCE A) 3.1.6 Iodine monochloride <ICl) 1.0M. To 600 ml of 25 percent potassium Iodide 05 1.0 15 2.0 2 5 solution (reagent 3.1.3), add 600 ml of con centrated hydrochloric acid. Cool to room temperature. With vigorous stirring, slowly add 135 g of potassium lodate and continue stirring until all free iodine has dissolved to give a clear Mange-red solution. Cool to room temperature and dilute to 2,600 ml with dis tilled water. The solution should be kept In ember bottles to prevent degradation. 3.1.7 Sodium hydroxide pellets. Reagent grade. 3.1-8 Nitric ectd. Concentrated. 3.18 Hydroxylamine sulfate. Reagent grade. 3.1.10 Sodium chloride. Reagent grade. 31.11 Mercuric chloride. Reagent grade. 3.2 Sampling. 3-2 1 Absorbing solution. 0JM ICl. Dilute 100 ml of the 10M ICl stock solution (reagent 3.1.6) to 1 1 with dietstlled water. The solution should be kept in glass bottles to prevent degradation. This reagent should be stable for at least 2 months; how ever, periodic checks should be performed to Insure quality. 3.2 2 Wash. acid. 1:1 V/V nitrtr acid-water. 3 2.3 Distilled, efeionired voter. 3 2 4 Silica gel Indicating type, 6 to 16 mesh, dried at 350'F for 2 hours 3 3. Analysts--3.3 1 Sodium hydroxide, ION. Dissolve 400 g of sodium hydroxide pel lets In distilled water and dilute to 1 1. 3 3 2 Reducing agent. 12 percent hydrox- ytamtne sulfate, 12 percent sodium chloride. To 60 ml of distilled water, add 12 g of hy- droxylamine sulfate and 12 g of sodium chlo ride. Dilute to 100 ml. This quantity is sufficient for 20 analyses and must be pre FIgurv 104-3. Minimum number of traverse points. pared dally. 4.2.6 If a selected sampling point is cloew tion of that point to Insure that the sample 3 3.3 Aeration gas Zero grp.de air. than 1 inch from stack wall, adjust the loca la taken at least l Inch away from the wMl. FEDERAL REGISTER, VOL 36, NO. 66--fRIOAY, APRIL 6. 1973 010806 SM2 SUIES AND REGULATIONS 4 3 Cross-oertlonal layout and l^n.ion of traverse points. *3 i For circular stacks locate the trn- ver< points on at least two diameters nctorrttng to figure 102-4 and table 102-1. The traverse axe* shall divide the stack-cross sec- tif.ii into equal parts. * 3 2 For rectangular stacks divtc/e the c-~-<-section into tvs many equal rectangular r 'ns. a* traverse points, such that the ratio of t!'c length to the width of the elemental ureas i.s between one and two. Locate the traverse p mts at the centroid of each equal area ac c-'r niig to figure 102-5. 4 4 Measurement of stack conditions. 4 4 1 Set up the apparatus as shown in figure 102-2 Make sure all connections arc ti^ht and leak free. Measure the velocity head and temperature at the traverse points speci fic:! by section 4 2 and 4 3. 4 4 2 Measure the static pressure In the stack. 4 4 3 Determine the stock gas moisture. 102-4. C'o** >'! c<rtvUr 9**cti Wtowinc locti.o" oi t'ive<s p(ot* on p#epe*d<<ui*r s<iwiis. f .<wrt it: S. C*0 itCliOft ol mt****1* tttcli 4ivt4*d IM '.2 iih fuh* 41 cm/o> W tacnM. Table 102-1. Location of traverse points In circular stacks (Percent of stack dtaneter from Inside vail to traverse point) Traverse point number Number of traverse points on a diameter on a diameter 2 4 6 10 | 12 14 16 18 20 22 24 1 14.6 6.7 4.4 3.3 | 2.5 2.1 1.8 1.6 1.4 1.3 1.1 1.1 a 85.4 25.0 14.7 10.5 8.2 6.7 5.7 4.9 4.4 3.9 3.5 3.2 3 75.0 29.5 19.4 14.6 11.8 9.9 8.5 7.5 6.7 6.0 5.5 4 93.3 70.5 32.3 22.6 17.7 14.6 12.5 10.9 9.7 8.7 7.9 5 85.3 67.7 34.2 25.0 20.1 16.9 14.6 12.9 11.6 10.5 6 95.6 80.6 65.8 35.5 26.9 22.0 18.8 16.5 14.6 13.2 7 89.5 77.4 64.5 36.6 28.3 23.6 20.4 18.0 16.1 & 96.7 85.4 75.0 63.4 37.5 29.6 25.0 21.8 19.4 9 91.8 82.3 73.1 62.5 38.2 30.6 26.1 23.0 10 97.5 88.2 79.9 71.7 61.8 38.8 31.5 27.2 n 93.3 85.4 78.0 70.4 61.2 39.3 32.3 12 97.9 90.1 83.1 76.4 69.4 60.7 39.8 T3 94.3 87.5 81.2 75.0 68.5 60.2 14 98.2 91.5 85.4 79.6 73.9 67.7* 15 95.1 89.1 83.S 78.2 72.8 16 98.4 92.5 87.1 82.0 77.0 17 95.6 90.3 85 .'4 80.6 18 98.6 93.3 88.4 83.9 19 96.1 91.3 86.8 20 98.7 94.0 89.5 21 96.5 92.1 22 98.9 94.5 23 96.8 24 98.9 4 4 4 determine the stack sas molecular weight from the measured moisture content nnd knowledge of the expected gas stream composition. Sound engineering Judgment should be used. 4 5 Preparation of sampling train. 4.5 l Prior to assembly, clean all glass ware (probe, imptngers, and connectors) by ringing v,;th wash acid, tap water. 0 1M IC1. tap water, and finally distilled water. Place 100 ml of 0 1M IC1 in each of the first three tmpingers. and place approximately 200 g. of preweighed silica gel in the fourth tmpinger Save SO ml of the 0 1M IC1 as a blank in the sample analysis Set up the train and ihe probe a-s in Figure 102-1. 4 52 Leak check the sampling train at the sampling site. The leakage rate should not be in excess of 1 percent of the desired sampling rate. Place crushed Ice around the imp.ngerv Add more Ice during the run to keep the temperature of the gases leaving the last Implnger at 70* F or less. 4 6 Mercury train operation. 4 6 1 Safety procedures It Is Imperative th^t the sampler conduct the source test under conditions of utmost safety, since hydrogen and air mixture* are explosive. The sample train essentially is leskJes*, so that attention to safe operation can be concen trated at the inlet and outlet. The following specific items are recommended: 4 6 1.1 Operate only the vacuum pump during the test. The other electrical equip ment, e g heaters, fans and timers, normally are not essential to the ruccess of a hydro gen stream test. 4 6.1.2 Seal the sample port to minimize leakage of hydrogen from the stack. 4 6 1.3 Vent sampled hydrogen at least 10 feet away from the train. This can be accomplished easily by attaching a Vj-lo I d Tygon tube to the exhaust from the orifice meter. 4 6 2 For each run, record the data re quired on the sample sheet shown In figure 102-6. Take readings at each sampling point at least every 5 minutes and when significant changes in stack oondttlons necessitate ad ditional adjustments In flow rate. 4.6.3 Sample at a rate of 0.5 to 1.0 cfm. Samples shall be taken over such a period or periods as are necessary to accurately determine the maximum emissions which would occur In a 24-hour period. In the case of cyclic operations, sufficient tests shall be made so as to allow accurate determination or calculation of the emissions which will occur over the duration of the cycle. A mini mum sample time of 2 hours is recommended. 2d some instances, high mercury concentra tions can prevent sampling In one run tor the desired minimum time. This is indicated by reddening in the first impinger as free iodine is liberated. In this ease, a run may be divided Into two or more subnxns to Insure that the absorbing solutions are not depleted. FEDERAL UGttTIR, VOL 39, HO. 64--FRIDAY, APRIL 6, 1973 04-0807 RStt -- PTf_________ W**C f-l*U KM Ml_ ItlMICrf NO _ Mllll.M. r ucio*____ i.. <x ic ;ov'. v A 4~\' -, ..tj- l'_ F.wo 40is".k.; N-w :<,'* Hom i -4 Fr*1W. field feU 4 6 4 To begin sampling, position the noz zle at the first traverse point with the tip pointing directly into the gas stream. Imme diately start the pump and adjust the flow to isokinetic conditions. Sample lor at least 5 minutes at each traverse point; sampling time must be the same for each point. Main tain isokinetic sampling throughout the sam pling period, using the following procedures 4 6.4.1 Nomographs which aid in the rapid adjustment of the sampling rate without other computations are in APTD-0S76 and are available from commercial suppliers. The available nomographs, however, are set up for use In air streams, and minor changes are required to provide applicability to hydrogen. 4 6.4.2 Calibrate the meter box orifice. Use the techniques as described In APTD-0676. 4 6 4.3 The correction factor nomograph discussed In APTD-0576 and shown on the reverse aide of commercial nomographs will not be used. In tts place, the correction factor will be calculated using equstion 102-2. C-0.01 P. Tm Ml cq. 102-2 where: C = Correction factor C, = Pitot tube coefficient. s Mole fraction dry gas. P, =8tack pressure. InHg. P. = Meter pressure, InHg. T- =Meter temperature. +R. Af#=5 Molecular weight of stack gas (from 4.4.4), lb/lb mole. iff & =: Meter box calibration factor, ob tained in step 4.6.4.S. 4.C 4.4 Set the calculated correction factor on the front of the operating nomograph. Select the proper nozzle and set the K-factor on the nomograph as detailed m APTD-0576. 4 6 4.5 Read the velocity head In the stack at each sample point from the manometer In the meter box. Convert the hydrogen AP to an equivalent value for air by multiplying by a ratio of the molecular weight of air to hy drogen at the stack moisture content. Insert this value of AP onto the nomograph and read off Art. Again, convert the Art. which M an air equivalent value, to the A// for hydro gen by dividing by 13 Tills factor includes the ratio of the dry molecular weights and a correction for the different orifice calibration factors for hydrogen and air. Th.s procedure is diagrammed below: OWrvc Al* -MtiHiply I'X ;t fnln'i-'jvo/ntfi'iiph- Kean off a//--Divide l*jr 13* M7f U>lH'Uv*(jeHi nw't-v iox. 4.64.6 Operate the aample train at the calculated &H at each sample point. 4.6.5 Turn off the pump at the conclusion of each run and record the final readings. Immediately remove the probe and nozzle from the stack and handle in accordance with the sample recovery process described in sec tion 4.7. 4 7 Sample recovery. 4 7.1 (All glass storage bottles aud the graduated cylinder must be precleaned as in aection 4.5.1). This operation should be per formed in an area free of possible mercury contamination. Industrial laboratories and ambient air around mercury-using facilities are not normally free of mercury contamina tion. When the sampling train is moved, care must be exercised to prevent breuksge and contamination. 4.7.2 Disconnect the probe from the Imptnger train. Place the contents (measured to zl ml) of the first three implngera into a 500 ml sample bottle. Rinse the probe and all glassware between ft and the back half of the third Impinger with two 60 ml por tions of 0 IM ICI solution. Add these rinses to the first bottle. For a blank, place BO ml of the 0.1M ICI in a 100 ml sample bottle. Pu*ce the siltca gel in the plastic Jar beat! and secure all containers for shipment. If an ad ditional test is desired, the glassware can be carefully double rinsed with distilled writer and reassembled However, if the glassware Is to be out of use more than 2 days, the imuai acid wajU procedure mun be followed 4.fl Analysts--4.6 1 Apparatus prrpuraf/on.--Clean all glassware according to the procedure of section 4.5 l. Adjust the instru ment settings according to the instrument u L'-j.iV nm vi .\V>orp; ,on vAVc-;?-\;*h of l :i`2 AeuJ/vij* pr.-parution--AUJu.*t i<e a>r delivery p. c.-sure and tne needle \aKe to obtain a constant air flow of about 1 3 1 mm The analysis lube snould be bypassed ex cept during aeration. Purge the equipment lor 2 minutes Prepare a simple of mercury standard solution (3 4 2) accord.ng to sre- i ion 4 8 3 Pia:e the analysis tube m the and aerate unto a maximum peak height is reached on the recorder. Remove the un.iiv- si* tube, flush the lines, and rinse the analysis tube with distilled water P.epeit with another sample of the same standard solution. This purge and analysis cycle K lo be repeated until peak heights are repro ducible. 4 3 3 Sample preparation--Just prior to analysis, transfer a sample aliquot of up to 50 ml to the cleaned 100 ml analysis tube. Adju-w the volume to 50 ml with 0.1M ICI if required. Add 5 ml of iO N sodium hydrox ide, cap tube with & clean glass stopper and shake vigorously. Prolonged, vigorous shak ing at this point is necessary to obtain an accurate analysis Add 5 ml of the reducing agent (reagent 3 3 2), cap tube with a eleun glass stopper and shake vigorously and im mediately place In sample Une. 4 84 JHercury determination--After the svstem has been stabilized, prepare samples from the sample bottle according to section 4 8.3 Aerate the sample until a maximum peak height Is reached on the recorder. The mercury content is determined by comparing the peak heights of the samples to the peak heights of the calibration solutions. If col lected samples are out of the linear range, the samples should be diluted. Prepare & blank from the 100 ml bottle according to section 4 8 3 and analyze to determine the reagent blank mercury level. 5. Calibration.--5.1 Sampling Train. 5 1.1 Use standard methods and equipment as de tailed In APTD-0576 to calibrate the rate meter, pitot tube and dry gas meter Recali brate prior to each test series. 52 Analysts.--5.2.1 Prepare a calibra tion curve for the spectrophotometer using the standard mercury solutions. Plot the peAk heights read on the recorder versus the concentration of mercury In the standard solutions. Standards should be interspersed with the samples since the calibration can change slightly with time. A new calibration curve should be prepared for each new set of samples run. 6. Calculations--6.1 Average dry gas meter temperature, ttack temperature, stack pres sure and average orifice pressure drop.--Sec data sheet (fig. 102-6). C 2 Dry gas volume,--Correct the sample volume measured by the dry gas meter to stack conditions by using equation 102-3. r.(F-+m) V- Tm P. cq. 102-3 h'l IK I mt- Volume of p-is through I he dry p t (>l wk condition'}, ft 1*-,=.Volume of gas sample through the dry gas meter (meter conditions). ftJ. T. r- Average temperature of stack gas. 'R T-Average drv gas meter temperature, R. /V. = Barometric pressure at the orifice meter, irvHe of/= Average pressure drop across the ori fice meter. lnH.-O. 13 r> -Specific gravity of mercury. P = Stack pressure. Pur static pressure, tnHg. No. 60--Pt IT FEDERAL REGISTER. VOl. 33. NO. 66--FRI0AY, APRIL 6, 1973 U10808 SSil RULES AND REGULATIONS 6 3 Volumf o/ uafcr vapor. V.^K.V,?-* eq.102-4 * aIn r<`- V'^ - V.iJnm** ot COtniiLluiisl, ( * nj'Pf in ifu* gri nmpla (sleek In T7? -- f11 ml - UK-0 OOXT------ ------- -- , * !m* ihe units art usM. l*i<T9tM Tolunir nf Iniind colWlM in Lmpingto mi'I *ilu*-'<*1 (siy fipHr*' l*iJ 7), ml. T. - Averopc Sl.bk ^.i.s tom prillin', H. /'.-Sl.wk prr*sui*, /'**, si-Uu- pr^urr. In. 1!*:. 0.4 7*ofaJ gas volune. 1 i4ki -- \ (., 4" V*,, cq. 102-5 whc re: Vi#(*i = total volume of gas sample (stack conditions), ft1. rM'*Voetuofn>.il*iHoomf pi..i(i*.fltrouvlt dry c-* nvu*r frf.tuk l'r#Yolunic ol vk.U'-r t.ia< In g_a mu.pie (slock condiiioiw), fl\ final vtxire or iiouio Af(R CUL^.I'JI saiNUs WS4C, tuu CA *c*or, e PLANT_______________ DATE __________________________________________ PUN NO--------------------------------------------------------------------- - STACK DIAMETER, in. ____________________ __ BAROMETRIC PRESSURE, in. Hg;____________________ STATIC PRESSURE IN STACK |Pg), in. Hg. OPERATORS_________________ _________________________ Traverse point number Velocity head, in, H20 va7 i------------------------------------ SCHEMATIC Of STACK CROSS SECTION Stack Temperature UOJlO COUJCTTO TOTAL VCAUMf CSLUCTtO rl 'C0*e/T*T moHT ov watt* re vouM it diyiiifrvj total weight MCRLASt if puam or Arw. u mcm.k<t 9 ti e**) VUUW1ATCI ml Flflurt 1027. Analytical dale. GA Stack gas velocity--Use equation 102-4 to calculate the stack gas Telocity. V^lfr(.)..." k.c.uap).., Wh^rr Kt ff\wCm (Vajjj P AC eq 102-6 iron** stack gas Telocity, feet per mend. . ^ it / Ift-niHg V/*, c\ )t> mota'-R-taUkr / Th* these units ere tned. *ltet tube eoeiftcfent, dimenstonleea, i Tense stack ns teinserelura *R. >ATenure aqunre root of the Hoily bred of stack pas UiiHiO)1/1 (see fijrare 14B-*). Stack pressure iVr^statlc irtrsure, ta Hr. Mokeular Treffht cl stack fw tmH buJ>, the summation of the products of Uw molecular mulU plied weijflit by its Toolfumeaectrhtc cotoponcMt proportiou Id Um mlstuiT, Ib/lb-moio. Figure 102-9 shows a nmpla recording sheet for Telocity traTerso data. Use the average* In the last two columns of figure 102-0 to de termine the arerage stack gas Telocity from equation 102-0. 0 Mercury collected. Calculate the total weight of mercury collected by using eq. 102-7. AVERAGE: Figure 102-8. Velocity traverse data. HDKAt MGI5TEI, VOL 38, NO 64--fRIOAV, Af>ll 6, 1973 -010809 wi -v ri-v.r-... 10 Sh i:*fhsr:i. T? T V* P Todd, and 'V 23? Temperature r:uge--Any impe-a- Smith, s,:;mficuKe of Errors m stach .urf* n:oa*.iri:ig device to incisure alack tem Wri r. i\>lal weight of mercury collected, *i>. Vi-ToLaI \olume of condensed moisture aud ICi tn sample bottle, ml. Ct = Concentration of mercury measured in sample bottle, *g/ml. Vr:Total volume oC ICI used in sampling (impinfcr contents aud ail wash amounts), ml C* =. Blank concentration of mercury in ICt solution, jig.'mi. 6.7 Total mercury emission.--Calculate the total amount of mercury emitted from each stack per day by equation 102-8. This piinv Measurement*. Piper presented at me Annual Meeting of the A:r Pollution Control Awuialion, St. Louis. Mo, June 14-19. I:>70. 11. Smith. W. S.. et al.. Stack Gas Sam pling Improved and Simplified with New Equipment, APCA paper No. 67-119. 19(7. 12. Smith. W. S.. R. T. Shigehara. and W. F. Todd. A Method of Interpreting Stack Sam pling Data. Paper presented at the 63d An nual Meeting of the Air Pollution Control Association, St. Louis. Mo.. June 14-9. 1970 1J Specifications for Incinerator Testing at Federal Facilities PHS. NCAPC. 1067 14. Standard Method for Sampling Stacks perature to vmh.n 5> F. 2 2 4 Pressure gauge--Any device to ni*-GSurc stack pressure to within 9 1 in. Hr. 2 2 5 Barometer.--To measure atmos pheric pressure to within 0.1 In. Hg. 226 AfoiAftxre determination.--Wet and dry bulb thermometers, drying tubes, condmsers. or equivalent, t j determine stack gas moisture content to within 1 percent. 2 3 Semple recovery--2 3.1 Probe clean ing equipment--Probe brush or cleaning rod at least as long as probe, or equivalent. Clean "otton balls, or equivalent, should be used u ith the rod. equation is applicable for continuous opera tions For cyclic operations, use only the time per day each stack is in operation. The total mercury emissions from a source will be the f.r Paniculate Matter, In: 1971 Book of ASTM Standards, part 23, Philadelphia. 1J71, ASTM Designation D-2928-71. 15 Vennard, J. K.. Elementary Fivud Me 2 3 2 Lenktess glass sample bottles. 2 4 Arwtlysir.--2 1.1 Equipment neces sary to perform an atomic absorption, spectrographlc. fiuorometrtc. chromato summation of results from all stacks. chanics. John Wiley and Sons, Inc . New graphic. or equivalent analysis. ir,(f,l... A. 80,400 srcondp.'cDiy l',.i 10* mfJi4 Yotk, 1947. METHOD 103. DERTLLIUM SCREENING .METHOD 3 Reagents.--3 1 Sample recovery--3.1.1 Acetone.--Reagent grade. 312 Wash acid.--1:1 V/V hydrochloric where: cc|. 102-S P m Rat of emission, g/day. H',Total wrlsht o.' mercury colloctod, oC l'iui*ToiaJ volume of gas sample conditions), ft*. Arorape stack cos velocity, feet pir second. A, -Stack area, it1. 1. Principle and applicability.-- l 1 Prin ciple.--Beryllium emissions are isokmetraiiy sampled from three points In a duct or stack The collected sample is analyzed for beryl lium using an appropriate technique. 1.2 Applicability.--This procedure details guidelines and requirements for methods acceptable for use in determining beryllium emissions In ducts or stacks at stationary acid-water. 3 2 Analysis.--3.2 1 Reagents as neces sary for the selected analytical procedure. 4. Procedure.--4.1 Guidelines for source testing are detailed in the following sections. These guidelines are generally applicable: however, most sample sites differ to some de gree and temporary alterations such as stack extensions or expansions often are required G 8 Isokinetic variation (comparison of velocity of gas tn probe tip to stack velocity). r I 00 V\o\*X sources, as specified under the provisions of I Cl.14 of the regulations. 2. Apparatus--2 l Sampling train,--A schematic of the required sampling tram to insure the best possible sample site. Fur ther, since beryllium is hazardous, care should be taken to minimize exposure Finally, since the total quantity of beryllium cq. 102-9 configuration la shown In figure 103-1. The to be collected Is quite small, the test must where: /Percent of Isokinetic sampling. U.ui-Total volume of gas sample (suck condition.*), ft*. /t.-Probe tip ores. ft1. Sampling time, fee. Artnfe stack gas velocity, fect tier second. 7. Evaluation of result*.--*7.1 Determina tion of compliance.--7.1.1 Each performance test shall consist of three repltltlons of the applicable test method. For the purpose of determining' compliance with an applicable national emission standard, the average of results of all repetitions shall apply. 12 Acceptable isokinetic results.--7 2.1 The following range sets the limit on ac ceptable isokinetic sampling results: If C9%^1^110%. the results are acceptable; otherwise, reject the test and repeat. essential component* of the train arc the following: 2.1.1 Hozzle.--Stainless steel, or equiva lent. with sharp, tapered leading edge. 2 1.2 Probe.--Sheathed Pyres1 glass. 2.1.3 Filler.--Mlllipore AA, or equivalent, with appropriate filter holder that provides a positive seal against leakage from outside or around the filter. It is suggested that a Whatman 41. or equivalent, be placed imme diately against the back side of the Miinpore filter as a guard against breakage of the Mlllipore. Include the Whatman 41 in the analysis. Equivalent filters must be at least 99 95 percent efficient (DOP Test) and amenable to the analytical procedure. be carefully conducted to prevent contami nation or loss of sample. 4.2 Selection of a sampling site and ntmber of runs.-^.2.l Select a suitable sam pling site that Is as close as practicable to the point of atmospheric emission. If possible, stacks smaller than l fool in diameter should not be sampled. 4 2.2 The sampling site should be at least eight stack or duct diameters downstream and two diameters upstream from any flow disturbance such as a bend, expansion or contraction. For rectangular cross-section, determine an equivalent diameter using the following equation: 2LW D L+W eq. 103-1 8. References.---1. Addendum to Specifi cations for Incinerator Testing at Federal Facilities, PHS, NCAPC, Dec. 6. 1967. 2. Determining Dust Concentration In a Gas Stream, ASME Performance Test Code where: Do=equivalent diameter L ~ length W = width No. 27, New York. N.Y.. 1987. 3. Devorkln, Howard, et *1., Air Pollution Source Testing Manual, Air Pollution Con trol District, Los Angeles, Calif., Noe. 1963. 4. Hatch, W. R. and W. L. Ott, ''Determina tion of Sub-Microgram Quantities of Mer cury by Atomic Absorption Spectrophotom etry." Anal. Cbem., 40 : 2085-87, 1968. 8. Mark. L. S., Mechanical Engineers* Handbook. McGraw-Hill Book Co . Inc., New York. N.Y.. 1951. 6. Martin. Robert M,, Construction Details of Isokinetic Source Sampling Equipment, Environmental Protection Agency. APTD0581. 7. Methods for Determination of Velocity, Volume. Dust and Mist Content of Gar.cs, Western Precipitation Division of Joy Manu facturing Co.. Los Angeles, Calif. Bull. WP-50. 19G8. 8. Perry. J. H., Chemical Engineers' Hand book. McGraw-Hill Book Co, Inc . New York, NY.. 1960. 9. Rom. Jerome J.. Maintenance. Calibra tion. and Operation of Isokinetic Source Sampling Equipment, Environmental Protec tion Agency. APTD-0576. Flfm MS-1. SvryniM mull iwOm*; --yfc Sale tthwuifc. 2 1.4 Meter-pump system.--Any system tliat will maintain Isokinetic sampling rate, determine sample volume, and. la capable of a sampling rate of greater than 0.6 cfm. 22 Measurement of afoeJr conditions (stack pressure, temperature, moisture cud ceJoctty) .--The following equipment shall lie u^ed in the manner specified in section 4 3 1. 2 2.1 Pilot tube.--Type 6, or equivalent, with a coefficient within 6 percenl over the working range. 2.22 Differential pressure gauge--In clined manometer, or equivalent, to measure veioc'ty head to within 10 percent of (lie minimum value. * Mention of trade names or specific prod ucts does not constitute endorsement hy the Environmental Protection Agency. 4.23 Some sampling situations may ren der the above sampling site criteria Imprac tical. When this is the case, an alternste site may be selected but must be no less than two diameters downstream and onehalf diameter upstream from any point of disturbance. Additional sample runs are rec ommended at any sample site not meeting the criteria of section 4.2.2. 4 2.4 Three runs shall constitute a test. The runs shall be conducted at three dif ferent points. The three poults shall pro portionately divide the diameter. !e. be In cited at 25. 50 and 75 percent of the diameter from the Inside wall. F^r horizontal duct.', the diameter shall be in the vertical direc tion. For rectangular ducts, sample on a line through the centroid and parallel to a sid:. If additional runs are required per section 4 2.3 proportionately divide the duct to ac commodate the total number of runs.' 4 J Measurement of sfack conditions. 4 3 i Measure the stack gas pressure, mohture, and tempemture, using the equipment described In I 2 2 Determine the molecular weight of the stack gas. Sound en'inerrinq estimate; may l*e made In lieu of direct FEDERAL REGISTER, VOL. 38, NO. 66--FRIDAY, APRIL 6, 1973 - 010810 measurements The bwli for *ucv 'sUmates shall b given ^ *h< test report. 4.1 Preparation of samphh^ tmin -- 4 4 1 Assemble the sampling tram as shown in figure 103-1. It is recommended that ell glassware be precleaned by soaking in wash acid for 2 hours. 4 4 2 Leak check the sampling train at the sampling she. The leakage rate should rot be m excess of 1 percent of the desired sample rale. 4 5 Beryllium train operation.--4 5 l For each rim, measure the velocity at the selected sampling point Determine the isokinetic sampling rate. Record the velocity head and tiie required sampling rate. 4 5.2 Place the nozzle at the sampling pouit with the tip pointing directly into the gas stream. Immediately start the pump and adjust the how to isokinetic conditions. At the conclusion of the test, record the sam pling rate. Again measure the velocity head at the sampling point. The required isokinetic rate at the end of the period should not have rtertated more than 20 percent from that originally calculated. 4 5 3 Sample at a minimum rate of 0.5 ftVmln. Samples shall be Lcken ovr such A period or periods as are necessary to deter mine the maximum emission* which would occur in a 24-hour period, in the case of cyclic operations, sufficient tests shall be made so as to allow determination or calcu lation of the emissions which would occur over the duration of the cycle. A minimum sampling time of 2 hours is recommended. 4 5.4 AU pertinent data should be in cluded In the test report. 4 0 Semple recovery.--4 6.1 It is recom mended that all glassware be prscleaned as in I 4.4.1. Sample recovery should also be performed in an area free of possible beryl lium contamination. When, the sampling train is moved, exercise care to prevent breakage and contamination. Set aside a por tion of the acetone used in the sample re covery as a blank for analysis. The total amount of acetone used should be measured for accurate blank correction. Blanks can be eliminated if prior analysis shows negligible amounts. 4 6J Remove the filter and any loose par ticulate matter from filter holder and place in a container. 4 6.3 Clean the probe with acetone and a brush or long rod and cotton balls. Wash into the container. Wash out the filter holder with acetone and add to the same container. 4.7 Analysis.--4.7.1 Make the necessary preparation of samples and analyze for beryl lium. Any currently acceptable method such as atomic absorption, spectrographic, fluoro- metric, chromatographic, or equivalent may be used. 5. Calibration and standards--6.1 Sam pling train.--6.1.1 As a procedural check, sampling rate regulation should be compared with a dry gas meter, spirometer, rotameter (calibrated lor prevailing atmospheric con ditions), or equivalent, attached to noszle Inlet of the complete sampling train. 5 12 Data from this test and calculations should be shown In test report. 5.2 Analyst*.--6.3.1 Standard ixation is made as suggested by the manufacturer of the instrument or the procedures for the analytical method.' 6. Calculations--6 1 Total beryllium emis sion. Calculate the total amount of beryl lium emitted from each stack per day by equation 103-2. This equation is applicable for continuous operations. For cyclic opera tions, use only the time per day each stark Is la operation. The total beryllium emis sions from a source will be the summation of results from all stacks. IT,h. Ml JHM wh r r. ` 1'.' I iihshj.i i. t' il.tv. H i To' il WHi'hl of l** i vUtim -Toi,\l vulum* l p.v tM, (.* 0.) sta*W fjs fotixiiy, l*i p-r 'uni. ,1.*Stack sum, fl?. 7. Test report. 7.1 A test report shall be prepared which shall include as a minimum: 7.1.1 A detailed description of the sam pling tram \ised and results of the proce dural check with all data and calculations made. 7.1.2 AJi pertinent data taken during test, the basis for any estimates made, cal culations. and results. 7.1 3 A description of the test site in cluding a block diagram with a brief de scription of the process, location of the sam ple points in the cross section, dimensions and distances from any point of disturbance. METHOD 104. RETTRENCE METHOD FOA DETER MINATION OF BERTlXrDM EMISSIONS FROM STATION*** SOURCES 1. Principle and opplirabiltfp-- 1 1 Prin ciple.--Beryllium emissions are isoktnetlcajly sampled from the source, and the collected -.imp e *-> digested In an acid solution nr.t m..Jived by atomic absorption spectropho tometry. 1.2 Applicability ---This method is appli cable for the determination of beryllium emissions m ducts or stocks at stationary sources Unless otherwise specified, this method is not intended to apply to {-ns streams other than those emitted directly to the atmosphere without further processing. 2 Apparatus--2 1 Sampling train A schematic of the sampling train used by EPA is shown in figure 104-1. Commercial models of this train are available, although construction details are described In APTD050],' And operating and maintenance pro cedures are described in APTD-0576. The components essential to this sampling train are the following: 2.1.1 Noale --Stainless steel or glass with sharp, tapered leading edge. 212 Probe.--Sheathed Pyrex glass. A heating system capable of maintaining a minimum gas temperature in the range of the stack temperature at the probe outlet during sampling may be used to prevent condensation from occurring. PUMP Figure 104-1. Beryllium sampling train 313 Pitot tttbe.--Type 8 (djurt. 104-3), or equivalent, with a coefficient within S per cent over the working range, attached to probe to monitor stack gas velocity. 2.1.4 Filter holder.--Pyrex glass. The filter holder must provide a positive seal against leakage from outside or around the filter. A heating system capable of maintaining the filter at a minimum temperature in the range of the stack temperature may be used to prevent condensation from occurring. 2.1.6 Jmpingers--Four Oreenburg-Smith implngers connected in series with glass hll Joint fittings. The first, third, and fourth implngers may be modified by replacing the tip with a Va-lnch. id. glass tube extending to one-half inch from the bottom of the AftfCc. 2 16 Afeferfnp system --Vacuum gauge, leakl^ss pump, thermometers capable of measunng temperature to within 6r F. dry ga.3 meter with 2 percent accuracy, ond re lated equipment, described In APTD-0581, to maintain an isokinetic sampling rate and to determine sample volume. 2.1.7 Barometer.--To measure atmos pheric pressure to 0.1 in Eg. 22 Measurement of stack conditions (stack pressure, temperature, moisture and rcfocity)--2.2.1 Pilot tube.--Type 6. or equivalent, with a coefficient within 5 percent over the working range. 2.2.2 Differential pressure gauge--In clined manometer, or equivalent, to measure velocity head to within 30 percent of the minimum value.1 1 These documents are available for a nom inal cost from the National Technical In formation Service. US. Department of Com merce, 5285 Port Royal Road, Springfield, Va. 22151. ; Mention of trade names on specific prod ucts does not constitute endorsement by the Environmental Protection Agency. FEOERAl REGtSTil, VOL 38, NO. 46--FRIDAY, APRIL 6, 1973 J310811 S'JLfci AND rttoOLAitUPo hhi7 however. most sample sites didcr to ik-crce and temporary alterations j.urh .. stack extensions or expansions often are re quired to insure the best possible sample site. Further, since beryllium Is hazardous, care should be taken to minimize exposure. Finally, since the total quantity of beryllium to be collected is quite small, the test must be carefully conducted to prevent contami nation or loss of sample. 4 2 Selection of a sampling site and mini mum number of traverse points. 4.2.1 Select a suitable sampling site that Is as close as practicable to the point of at mospheric emission. If possible, stacks -ni.tuvr thau l foot in diameter should not b * b.mpled. 4.2.2 The samphug site should be at least 8 stack or duct diameters downstream and 2 diameters upstream from any flow disturb ance such as a bend, expaas.on or contrac tion. For a rectangular cross-section, deter mine an equivalent diameter from the following equation: D, = 2LW L+W where: D = equivalent diameter L ---length iv = width eq l04-1 NUMBER OF DUCT DIAMETERS UPSTREAM* (DISTANCE A) 2.2 3 Temperature gage---Anv tempera ture measuring device to measure stack tem perature to within 5* P. 22 4 Pressure gage.--Pilot tube and in clined manometer, or equivalent, to measure stack pressure to within 0 1 in Hg. 2.2.5 Moisture determination.--Wet and dry bulb thermometers, drying tubes, con densers, or equivalent, to determine stack gas moisture content to within 1 percent, 22 Sample recovery--2.3.1 Probe clean ing rod.--At least as long as probe. 2.3.2 Leakless glass sample bottles.--500 ml. 2.3.3 Graduated cylinder.--250 ml. 2.3.4 Plastic iar.--Approximately 300 ml. 2.4 Analysis--2.4.1 Atomic absorption spectrophotometer.--To measure absorbance at 234.6 nm. Perkin Elmer Model 303, or equivalent, with N.O/acetyteoe burner. 2.42 Hotplate.' 2.4 3 Perchloric acid fume hood. 3. fleopents--3.1 Stock reagents.--3.1.1 Hydrochloric acid.--Concentrated. 3.1.2 Perchloric acid.--Concentrated, 70 percent. 3.1.3 Nitric acid --Concentrated. 3.1.4 Sulfuric acid.--Concentrated. 3.1 & Distilled and deionized water. 3.1.6 Beryllium powder.--08 percent mini mum purity. 3.2 Sampling--82.1 Filter. -- Milllpore AA. or equivalent. It Is suggested that a Whatman 41 filter be placed immediately against the back side of the Milllpore filter as a guard against breaking the Milllpore filter. In the analysis of the filter, the What man 41 filter should be included with the Milllpore filter. 3.22 Silica gel.--Indicating type, 6 to 16 mesh, dried at 360* F for 2 hours. 322 Distilled and deionized water. 32 Sample recovery--32.1 Distilled and deionized water. 322 Acetone.--Reagent grade. 322 Wash acid.---1.1 V/V hydrochloric acid-water. 3.4 Analysis.--34.1 Sulfuric add solu tion, J2 AT--Dilute 333 ml of concentrated sulfuric acid to 1 1 with distilled water. 342 25 percent V/V hydrochloric acidwater. 35 Standard bcrylitum solution--3.5.1 stock solution--l jig'ml beryllium. Dis solve 10 mg of beryllium In 80 ml of 12 N sulfuric acid solution aud dilute to a volume of 1000 ml with distilled water. Dilute a 10 ml aliquot to 100 ml with 25 percent V/V hydro chloric acid, giving a concentration of 1 *g/ml. This dilute stock solution should be prepared fresh dally. Equivalent strength (In beryllium! stock solutions may be prepared from beryllium salts as BeClr and Be(NO ), (88 percent minimum purity!*. 4. Procedure. 4.1 Guidelines for source testing are detailed In the following sections. These guidelines are generally applicable; NUMBER OF OUCTDIAMETERS OOttNSTftU* iDISTANCE 81 Figure iOi *3. Minimum numoer of traverse points. pViaqvmwwtMp-a4to.isCr*pumMfmelitotonni<srcVcvtr ttack rhow1*9'loc*trfl of Flfufi 194 e. Citn MCllait r*e:w9y! ttacfc . uvMtM pe*U tt V tu.'i vu. tolO 12 tv! 4 2 3 When the f.bove sampling site cri teria can be met, the minimum number of traverse point* l* four (4) for stacks 1 foot In diameter or less, eight (6) for stacks larger than 1 foot but 2 feet In diameter or less, aud twelve (12) for stacks larger than 2 leet. 4 2.4 8ome sampling situations may ren der the above sampling site criteria imprac tical. When this Is the case, choose a con venient sampling location and uso figure 104-2 to determine the minimum number of traverse points. However, use figure 104-2 only for stacks 1 foot in diameter or larger. 42.5 To use figure 104-3, first measure the distance from the chosen sampling lo cation to the nearest upstream and down stream disturbances. Divide this distance by the diameter or equivalent diameter to deter mine the distance In terms of pipe diameters. Determine the corresponding number of traverse points for each distance from fig ure 104-3. Select the higher of the two num bers of traverse points, or a greater value such that for circular stacks the number i-i a multiple of four, and for rectaugular stacks the number follows the criteria of section 4 3.2 4 2 6 If a selected sampling point Is cloxer thrm l inch from the stack wall, adjust the location of that point to ensure that the sample is taken at least 1 inch away from ihe wall. 4 3 Cross-sectional layout and location ,-.{ traverse points. FEDERAL REGISTER, VOL 31, NO. 66--FRI0AY, APRIL 6, 1923 -010812 8S IS RULES AND REGULATIONS M *- UO 3 " VI V u40 E 35 5 r- 9 OC4 r k *1 CM LfJ 91 in CM CM O Pm o CM m CO CM CO O 40 9l 00 in in co 04 r** C1*M4 hCM! o <n 40 40 r*. ppo*o 00 CO CO CO 04 CM m r> o r** CO 40 r 40 M1' CO CO rC-M* V* CM in r n 9r>4 N 40 in s 91 PP*I. CM S o CO CO s o 94 o 04 in 04 94 04 cn C7 r-* r* 04 in O 40 CO CM *9 o 40 in P) r> - r*. CM r- n 40 r* CM CM n s s 40 PM Pm CO NCO s 94 04 91 CO *r tn 04 40 CO to 40 CM a> CM p. in 40 40 r"r r-- n CM 0CM4 CnO pj ro** 4r0* pj CO CinO <*; CO CM in 40 04. to to Ot O n m in fs o c-- m IA r- a CM CM n 40 f** CrO CO CD 04 94 & q N 04 o 04 40 9t P) CM 04 CM CM n 40 p*. r*. car 04 S s04 M r- PM CD p- O `in in o n CM 94 CM 40 r-- pr-m* iCnM nin 3 in r>. CCMO 3 n04 P9m4 in CM 40 40 CM CO CM CO CM n 40 CO in CO 04 04 M in r> r* 40 in r* CO <n 04 nCM p4*0. oCO CO Cn ** r>. in in n 40 40 w *--r CM r CO 04 r* o -o n CmM in P** n C4 to r** CO J f- JQ _ J ; s.| 51 I? WN N N M IsSMI aikt ti " ot) e- 2 ;tOCi E 0u sz _T, "O --c T3 iHsSi al 5| S 6Ic s* * C| O. 1 Is!IS o ? elsa-f 5! iotB*-j%-c 3* 3c t? 6 slSsJM = Sso s Ee- ** j= ? 2So<. 2s ^2 Sg- J,,SB *.p-* <zb;E w o a 5 *a *E* -OEi-t ft J fe fcft < > O |= ej=fss *11" -Es JS *2 Ocftgjs-'wS g3s K~< 4* ftOfS-- C m * C >5a S-S * pi HAS.w^CC_ ^* SH i*. 5 _* fcl IaSc5^afc">i|*jfeefl afi 5e ES3!SE=," = EB1` SbS-3smSo"c.ES|xj:-:SSJ*e_;_Z*l_c!s*,2a.c ^ISiSIsU* S'cSaf.^gS -"ueact32^oifAcl2f<j-8'03 010813 RULES AND REGULATIONS Itnm '.it ii.itu i .J handle ia riconrili- wt the recovery piocess descr.Ued it i t . 1 *1 S-int'j.e recovery.--4.7 I (All bl.us Gtora^e l*ott!es and the graduated cylinder in*: ,t be pr?'lcati**d as in $ 4 3 1 ) This oneratiun should oe performed m an area free of po^ible beryllium contamination. When the s.xmpLuS tr.un is moved, care must be ever* ci^ed to prevent breakage and contamination. 4 7 2 disconnect the probe from the impm,er train Remove the filter and any loose particulate matter from the filter holder and place in a sample bottle Place the contents tmeasured to 2:1 ml) of the first three Impingeri into another sample bottle Rinse the probe and all glassware between It and the back half of the third Impinger with water and acetone, and add this to the latter sam ple bottle Clean the probe with a brush or a long slender rod and cotton balls. Use acetunc while cleaning. Add these to the sample bot tle Retain a sample of the water and acetone a) a blank. The total amount of wash water find acetone used 6hould be measured for ac curate blank correction. Place the silica gel in the plastic Jar. Seal and secure all sample containers for shipment. If an additional test is desired, the glassware can be carefully dou ble rinsed with dtstUied water and reassem bled. However, if the glassware is to be out of use more thou 2 days, the initial acid wash procedure must be followed. 48 Analysis. 4.8.1 Apparatus preparation.--C\tin all glassware according to the procedure of sec tion 45.1. Adjust the instrument settings according to the instrument manual, using an absorption wavelength of 234.8 nra. 4 8.2 Sample preparation.--The digestion of beryllium samples Is accomplished In part In concentrated perchloric acid. Caution: The analyst must Insure that the sample Is heated to light brown fumes after the initial nitric acid addition; otherwise, dangerous perchlorates may result from the subsequent perchloric acid digestion. Perchloric acid also should be used only under a perchloric acid hood. 4.8.2.1 Transfer the filter and any loose particulate matter from the sample container to a ISO ml beaker. Add 35 ml concentrated nitric acid. Heat on a hotplate until light brown fumes are evident to destroy all or ganic matter. Cool to room temperature and add S ml concentrated sulfuric acid and 5 ml concentrated perchloric acid. Then pro ceed with step 4 8.2.4. 4 8.2.2 Place a portion of the water and acetone sample into a 150 ml beaker and put on a hotplate. Add portions of the remainder as evaporation proceeds and evaporate to dry ness. Cool the residue and add 35 ml concen trated nitric acid. Heat on a hotplate until light brown fumes are evident to destroy any organic matter. Cool to room temperature and add 5 ml concentrated sulfuric acid, and 5 '\i\ c j. e;.`rated perclilnru satl Then pro- i `<J \.uns,.ej-8S4. 4 8 2 2 Weuh the spent silica arid re port to the nearest jiram 482 1 Samples Iron 4 82 1 and 4822 may be combined here for ease of a'ialvi>. Replace on a hotplate and evaporate to drv- ne*" m a perchloric acid hood Cool and dis solve the residue in 10 0 ml of 25 percent V/V hydrochloric acid. Samples are now rendy for the atomic absorption unit. The berviiium concentration of the sample must be within the calibration range of the unit.. 1* necessary further dilution of sample with 25 percent V/V hydrochloric acid must be performed to bring the sample within the calibration range. 4 82 beryllium determination.--Analyze the samples prepared in 4.8.2 at 234.8 nm using a nitrous oxide/acetyleue flame. Alumi num, silicon aud other elements can inter fere with this method If present In large quantities Standard methods are available, however, to effectively eliminate these inter ferences (see Reference 5). 5. Calibration--5.1 Sampling train.-- 5 11 Use standard methods and equipment as deta.ied in APTD-0576 to calibrate the rate meter, pitot tube, dry gas meter and probe heater (U used). Recalibrate prior to each, test series. 5.2 Analysis.--6.2.1 Standardization is made w ith the procedure as suggested by the manufacturer with standard beryllium solu tion. Standard solutions wilt be prepared from the stock solution by dilution with 25 percent V/V hydrochloric acid. The linearity of working range should be established with a aeries of standard solutions. If collected samples are out of the linear range, the samples should be diluted. Standards should be interspersed with the samples since the calibration can change slightly with time. 6. Calculations--8.1 Average dry gas meter temperature, stack temperature, stack pres sure and average orifice pressure drop.--See data sheet (figure 104-8). 6.2 Dry pas volume.--Correct the sample volume measured by the dry gas meter to stack conditions by using equation 104-2. wl*re: I .,Voiufvc of gas Mm pie through the dry gas meter ('tick condition*!, ft1. V.Volume of gag sample through the dry gas ni#*er (meter condition*), ft1. T, Average temperature o< fteek gas, * R. T*Awii dry gas meter temperature* *R. Pm,-* Barometric pressure at the orifice meter, is He. d// Arcr.ice pressure drop icrou the orifice raetir. IQ fi)0 * 13 a-Sfhsific gravity of mercury. Stack prewar*. /** static pressure. In llg. V 'i, "ic of -j atcr t apor. n li T- cq. 104- 1 IV = V ilume nl a.il'-f vapor in the gas ainipP- (<tirk ft*. 1(11 i u Jtl h\ 'i f\v,7 --ml* It when lliee units are used, --Toul volume of hqmd collected In (mplnpm r. i'l mJ,,-j (xo ficure W4-7j, ml. T. - XT. myr* si*fk -x* lomix-riUUA *K. = b' j-:k pressure, iV,static pevsjure, In Hg. G 4 Tofaf gas volume. V..,.i=r.,+ V,, cq. 104-4 ^ volume of gas sample (.tack conditions), fi>. 1 olutnc of pat through dry gas meter Odoi-k conditions), ft1. r,4Volunio of water vapor in gas sample (s(a k conditions), ft1. C 5 Stack gas velocity. Use equation 104-6 to calculate the stack gas velocity. eq. 104-5 wlv*rr: (rA.*,.Average stack gas velocity, feet por second. KV-85.53-^* sec (-- Vlb IWnHr yn mofe-*R-iuHjO/ * *b**n these units are used. C,- Pitot tube coefficient, dimenstonfesa. <r.) ,*. Average stack gas temperature, *R. (y/ap) ....Average square root of tbe velocity heed of stack gas (inHiO)1* (see figure 104-4), P*mStark pressure. P.d=staUc pressure, in Hg. A/, Molecular weight of stack gas (wet basi'). the summation of the products of lit* molecular weight of each component multiplied by it* volumetric proportiou in the mi it urs, Ib.lb-moie. VOL UNI Of OOUlO VATU COLUCriO mu. turmcn VOtUNfc, Ml taicAGa WIGHT. e UHTUL uoMocauidD tutu. wjuM eaueno *1 * cowwtratwKTor eATtsTOvounwer dfvIdfM total Mfaht WdUASt sr Dcnsrrv or vara. tt e/wj: "'viV.Su1 vouac mth. -e Fipwe 104*7. Analytical data. FEDERAL REGISTER, VOL 38. NO. 64--FRIDAY, APRIL 6r 1973 - J010814