# ALTERNATIVE MONITORING PETITION FOR THE SOLI D-LIQUI D INCI NERATOR

Eli Lillyand Company Tippecano e Laboratories 1650 Lill yRoad Lafayette, IN 47909

October 20 05 Revision: 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

TA BLE OF CON T EN TS 1.0 INTROD UCTION

............................................................................................................... .... 1 2.0 ENGINEE R ING DES CRI PT ION

............................................................................................ 3 2.1 KEY COMP ONENTS

...................................................................................................... 3 2.2 SYSTEM O VERVIEW

..................................................................................................... 4 3.0 CANDIDATE S FOR ALTE RNATIVE MONITORING UNDE R §63. 8( f)

................................. 6 3.1 PARTICULATE MATTER CE MS

.................................................................................... 7 3.1.1 Indic a tor of Performanc e

................................................................................. 7 3.1.2 Measurement Tec hnique

................................................................................. 7 3.1.2.1 Operati ng Princ i ples

......................................................................... 7 3.1.2.2 Ins t alla tion Loc a tion

......................................................................... 9 3.1.2.3 Ins t allation

........................................................................................ 9 3.1.2.4 Ins t ru ment Span

............................................................................... 9 3.1.2.5 Sys t em Start Up (Initial Op eration)

.................................................. 9 3.1.2.6 PM CEMS Calibration Correlatio n Test (PM CEMS Certificat ion)

................................................................................... 12 3.1.2.7 Routine Operati on of the PM CEMS

.............................................. 16 3.1.2.8 ComponentReplac ement

.............................................................. 19 3.1.2.9 Out of Control

................................................................................. 19 3.1.3 Use of the PM CEMS for Co mpli an ce with the HW C MA CTPM Standard

........................................................................................................ 20 3.1.4 Monitori ng Frequency and Averaging Time

.................................................. 20 3.1.5 Rolling Block Average Cal c ulat ions during Routi ne Checks and Sys t em Audits

................................................................................................ 21 3.1.6 Bac k up to the Part ic ulate Matte r CEMS

........................................................ 22 3.1.7 Deviations from Performanc e Spec if ic ation 11

............................................. 23 3.2 MULTI

- META LS CEMS

................................................................................................ 25 3.2.1 Indic a tor of Performanc e

............................................................................... 25 3.2.2 Measurement Tec hni que

............................................................................... 26 3.2.2.1 Operati ng Princ i ples

....................................................................... 26 3.2.2.2 Ins t alla tion Loc a tion

....................................................................... 29 3.2.2.3 Ins t allati on

...................................................................................... 29 3.2.2.4 Ins t ru ment Span

............................................................................. 29 3.2.2.5 Sys t em Start-up (Initial Op eration)

................................................ 29 3.2.2.6 Sys t em Start-up (Field Ins t allati on)

................................................ 30 3.2.2.7 Performanc e S pec ificati on Tes t

..................................................... 31 3.2.2.8 Routine Operation of the Multi-Metals CEMS

................................ 34 3.2.2.9 ComponentReplac ement

.............................................................. 37
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3.2.2.10 Out of Control

................................................................................. 37 3.2.3 Use of the XACT Multi M e tals CEMS to Dem o n s trate Complia n c e with the HWC MACT Metal s St andards

........................................................ 37 3.2.4 Monitori ng Frequency and Averaging Time

.................................................. 37 3.2.5 Block Averag e Cal c ulation s duri ng Multi

- Metal s CEM S DailyChe c ks and Ongoing Quality A ssurance Ch ecks

....................................................... 39 3.2.6 Multi-Metals CEMS Back up

........................................................................... 39 3.3 HYDROGEN CHLORI DE (HCl) CEMS

......................................................................... 40 3.3.1 Indic a tor of Performanc e

............................................................................... 40 3.3.2 Measurement Tec hni que

............................................................................... 41 3.3.2.1 Operati ng Princ i ples

....................................................................... 41 3.3.2.2 Ins t alla tion Loc a tion

....................................................................... 43 3.3.2.3 Ins t allati on

...................................................................................... 43 3.3.2.4 Ins t ru ment Span

............................................................................. 43 3.3.2.5 Sys t em Start-up (Initial Op eration)

................................................ 43 3.3.2.6 Sys t em Start-up (Field Ins t allati on)

................................................ 44 3.3.2.7 Performanc e S pec ificati on Tes t

..................................................... 44 3.3.2.8 Routine Operat ion of HCl CEMS

................................................... 47 3.3.2.9 Out Of Control

................................................................................ 49 3.3.3 Use of HCl CEMS for Demon s tratin g Contin uou s Compli an ce with the HCl/ C l 2 HWC MA CT Emi s s i on Stan dard

................................................. 49 3.3.4 Monitori ng Frequency and Averaging Time

.................................................. 50 3.3.4.1 Rolling Average Cal c ulat ions du ring HCl CEMS Daily Calibration and Ongoing Qua lity As s u rance Audits

....................... 51 3.3.4.2 Rolling Average Cal c ul ati ons during System Autopurge

............... 51 3.3.4.3 PM and HWC MA CT M e tals Rolling Av erage Calculations durin g Ecochem CEMS Daily Calib ration and Ongoi n g Quality As s u rance Audi ts

............................................................... 52 3.3.5 Bac k up to the HCl CEMS

.............................................................................. 52 3.4 JUSTIFI C ATION FO R REQUESTFOR ALTE RNATIVE MONITO RIN G METHOD

....................................................................................................................... 53 4.0 ALTERNATIVE MONITORING CA NDI D ATES UNDER 63.1209( g)

................................... 54 4.1 STACK GAS FLOWMETE R DAIL Y CHECK AND AU TOPURGE

................................ 54 4.2 COMB USTION GAS FLOW RATE OP ERATING PA RAME TER LI MI T

....................... 54 4.3 CALCULATI O N OF ROLLING AVERAGES WHEN AL L ONE-MINUTE AVERAGE VALUES ARE NOT AVAIL ABLE

................................................................ 55 5.0 ALTERNATIVE MONITORI NG PETITI O N APPROV AL

..................................................... 56
6.0 RELEVANT RE FERE NCES

................................................................................................ 57

Rev. 7.0 iiEli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

FIGURES

Figure 1. Block Fl ow Diag ram of Solid-Li quid Inci nerator Figure 2. Sigrist Parti c ulat e Matter CE MS Figure 3. T149 CEMS Dat a Exchang e Figure 4. Multi-Metals CEMS (XACT) Figure 5. Ecoch e m CEM S (HCl ) Figure 6. Ecoch e m Dyna mic Spiki ng Overview

TABLES

Table 1. Rot a ry Kiln Incin e rato r HWC MACT Op era t ing and Emission Limits

APPENDI CIES

Appendix A: EPA Draft Guidance Document for PM CEMS Appendix B: XACT Multi-Metals CEMS Guidan ce Do cu me nts, Performan c e Sp ecification s , and Quality Assu ra nce Docum ents Appendix C: HCl CEMS Perform a n c e S pecifi c ati on, HCL CEMS Quality Assu rance Do cum ents Appendix D: Cited Perfo r mance Spe c ificat ion s an d Quality Assu rance Pro c ed ure s

Rev. 7.0 iiiEli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

1.0 INTRODUCT I ON
Eli Lilly and Company (Lil ly ) operates a rotary kiln i n cineration system located at th e Lilly Tippecanoe Labo rato rie s in Lafayette, Indian a. The rotary kil n is referred to as the solid -liqui d incine rato r. The solidliquid i n ci nerator i s used to b u rn ha zardo u s a nd non-ha za rdo u s soli d wa stes a n d ha zardo u s liqui d
wa stes. T h e soli d-liq uid incin e rato r i s subje ct to req u ire m ents of the ha zardo u s wa st e co mbu s tor maximum achievable cont rol technol ogy (HWC MA CT) rule under 40 CF R 63 Subpart EEE and the Gene ral Provi s ion s un der 4 0 CFR 63 Su bpart A.

The HWC M A CT pla c e s consi derable e m pha sis on cont inuo us m o nitoring fo r d e mon s tratin g compli an ce with appli c a b l e emissio n stand ard s a n d ope rating para m eter li mits. As such, facilities a re requi red t o install contin uou s emi ssi o n monito ring system s (CE M S) that co n t inuou sly mo nitor an d re cord e m ission data an d co ntinuou s pa rametri cmoni toring syste m s (CPMS) that contin uo usly monito r and record operating dat a. Sectio n 6 3 .1209 (a )(5 ) of the HWC MACT allo ws facilitie s to petition the Administrator unde r Se ctio n 63.8 ( f) of t he Ge ne ral P rovisio ns to u s e CEMS for com p lian c e monitori ng fo r pa rticul ate matter, mercury, semivolatile metals , l o w vol a tile metals, a nd hydro c hlo r i c acid/ c hlo r ine gas in lie u o f complyin g wi th corre s po n d ing op eratin g para m eters. Section 63 .8(f) of the G eneral Provisions all o ws facilities to request approv a l of an alternative monitoring petition t o use alternat ive CEMS to demonstrate compli an ce with the appl icabl e MACTreq u ire m ents. In a dditio n , Section 1 209(g) of the HWC MACT allows faciliti e s to submit an appli c atio n to the Admini strato r to re que st app roval of alternati v e monitorin g requi rem ents to docum ent compli an ce with operatin g limits monitored by para m e t ric inst rume n t s. As requi red by the HWC MACT, Lilly will i n stall a nd o perate a CO an d O 2 C E MS to de mo ns tra t e compli an ce with the CO emission limi t, corre cted to 7% oxygen. Lilly is also prop osi ng to install and operate CEM S for multi-m e tals, pa rticul ate matter, and HCl to de monst rate attainment with the semivolatile metal s , low-volat ile metals , mercury, partic u lat e matter, and HCl/ C l 2 emission limits. Pursuant to Section 63.1 2 09(a ) (5) of th e HWC MACT, Lilly will not be required to use CPMS s to contin uo usly monito r operating p a rameters id ent ified in Sectio n 120 9 of th e HWC MA CT whe n CEMS are u s e d to d e mon s trate
c o mplianc e with the metals, partic u late matter, and HCl/ C l 2 HW C MACTemi s sion sta nda rd s. Ho wev e r, whe n the CE MS are n o t in use, Lilly will operate CP MSs to monit o r an d dem o n strate co mpl i ance with th e
corre s p ondin g operating para m eter li mits (OPL s) to avoid shutting down ha zardou s wast e feed to the solid s-li quid s incin e rato r. Table 1 p rovi des a su mm ary of which HWC MA CT stand ard s wil l apply while operating th e altern ative CEMS (CEM S mode ), an d whi c h o p e rating pa ram e ter limits will ap ply whe n a CEMS are n o tin use (pa ra m etric m ode ).

1 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

Lilly submitted an earli er version of this Alternative Monitoring Petition to EPA in conj unction with the Comp re hen si ve Perfo r man c e Te st Plan i n Septem be r 2003 to a d d ress alte rnativ e reque sts u n der Sectio n 40 CF R 63.8 ( f) Use of an alternative m onitoring m e thod and 4 0 CFR 63.12 0 9 (g) Alternativ e m onitoring requi rem ents other tha n contin uou s e m ission s m onitoring system s (CEMS )

. EPA responded to the majority of th e pa ramet r ic monitori ng re que sts u nde r 40 CFR 63. 1209 (g ) in a letter date d F ebru a ry 2 7 , 2004 whi c h was sign ed by George T. Czernia k , Chief of the Air Enf o rceme n t an d Co mplian c e Assuran c e Bran ch, EPA Re gion 5. Therefore, th ose Se ction 1209 (g ) p a ra metric mo nitoring requ ests fo rme r ly in Sect ion 4.0 of this doc u ment add res s ed by EPA’s February27, 2004 letter hav e been removed from this revisio n of the Alternative Monitori ng Petition.

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2.0 ENGINEE R ING DES CRI PTION
The key co mpone nts of the solid -li quid in cine rator are de scribe d belo w . The Co mpre hen sive Perform a n c e Te st (CPT) Plan fo r th e solid-li quid in ci nerator provide s a more detail e d en gine erin g descri p tion of the incine rat o r.

2.1 KEY COMPONENTS
The followi ng are the key compon ents of the solid-li qui d incin e rato r:
Wa st e Fee d S y st em – Th e wa ste feed system is d e s ign ed to fe e d solid a nd li quid waste s to the rotary kiln, and liq uid wa stes to the se co nda ry combu s tion cham be r (SCC). Rotary Kiln – The rotary kiln is a refra ctory-line d cyli nder that rot a tes while in cine rating sol i d and liquid
was t es

. Wet Ash Ha n d ling System – Hot, dry a s h from the rot a ry kiln i s coo l ed and ha s moistu re ad d ed in the wet ash h andlin g system.

Vertical U p -F low SC C – T he com b u s tio n gase s from the rotary kiln enter the SCC which is desi gne d to compl e te the com b u s tion of the g a se s from the kiln, and t o bu rn prima ry liqui d (hig h BT U content) and
se con dary liq uid (lo wBTU conte n t) wa st es.
NO x Abatement System – The hot com bustio n g a se s e n ter the selective non -catalytic re du ction (SNCR) system which uses u rea injection to red u ce NO x emissi on s. Th e NO x Abatement System do es not m eet the re gulato r y definition of a lo w o r a hi gh-e n e rgy we t scrub b e r an d the o p e rati on of the NO x abatement system i s not regul ated by the HWC MA CT re gulatio n s

. Quen ch – T he combu s ti on ga se s from the NO x abatem ent system enter the que nch whe re th e comb ustio n g a se s are co ol ed to their ad iabatic satu ra tion temperature. The qu ench is not d e sig ned no r intende d to be an air p o llut i on co ntrol d e v ice. The qu ench doe s no t meet the re gulatory d e finition of a low
or a hig h e n e rgy wet scrubbe r a nd th e op eratio n of the q uen ch is not re gu lated by th e HWC MACT regul ation s

. Con den se r/ A b so rbe r – Th e co mbu s tion gases from the qu en ch e n ter the cond enser/ab s o r b e r whe re th e gases a re cooled to bel ow thei r adi abatic satu ra tion temperature. The co n den ser/a b sorber p rovide s

3 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

addition al co nditioning of the comb u s tion ga se s exiting the quen ch. T he co nde nser/ab s o r be r i s con s id ere d a low en ergy wet scrubb er a c cordi ng to the HWC MACT regul ation s
H y d ro- So n i cTM Scr u bb er – Th e comb u s tion ga se s from th e con d enser/ab s o r b e r enter the Hydro

- Soni c scrub b e r whe re p a rti c ulate and metal s are rem o ved from the co m bustio n ga s stream. Rem o val of a c id gases is al so provided. Steam inje ctio n can be used to enh an ce t he pa rticul ate removal. The HydroSonic scrub b e r is con s ide red a high e n e rgy wet scrub ber a c cording to the HWC MACT re gula t ions

A block flo wdiagram of the solid -liqui d inci n e ratio n system is provided in Figu re 1.

2.2 SYSTEM OVERVIEW
The i n ci neration system is de sign ed to comb ust soli d a s well a s prima ry a nd se con daryliq uid wa stes. Solid wa ste s are fed th rou gh the solid wa ste feed syste m on the rotary kil n . Liquid wa stes can b e fed to both the rotary kiln an d SCC. The comb ustion ga s fro m the t reatm ent of th e wa stes is tre a te d in a wet ai r pollution cont rol (APC) system con s istin g of a NO x abatement syst em, a full qu e n ch, co nde nser/ab s o r be r, Hydro

- Soni c scrub b e r , and stack. An induced draft fan is the co mb ustion g a s p r i m e mover.
The fun ction of the qu en ch is to adia b a tically cool t he comb ustio n ga s via sat u rating water sp rays. The quen ch con s i s ts of a vertical, cylind r ica l , brick-line d cham be r. Fre s h and re circulating wate r is sprayed throug h que n c h no zzle s to adiab atically satu rate and cool the inl e t comb ustio n g a s.
Saturated co mbustio n g a s fro m the quen ch ente rs th e lo we r portio n of the co nde nser/ab s o r be r. Comb ustio n gas flo w s up throug h the p a cked se ctio n. Reci rculat ed wate r is i n trodu ced to t he top of the packe d sectio n and flo w s count ercu rrent to the combu s tion g a s flo wfor ad ditional com b u s tion gas co olin g and conditio n i ng.
Comb ustio n gas from the co nde nser/a bso r be r flo w s to th e Hyd ro-So nic scru bber. Th e Hydro

- Soni c scrub b e r re m o ves fine part i culate m a tter by inertial im pactio n . Particulate remo val efficien cy is a fun ctio n of the p ressu re differential acro ssthe Hydro

- Soni c scrub b e r . Th e differe ntial pre s sure is d epen dent o n the flow of combu s tion g a s e s and wat e r through th e Hydro-So ni c scrubb er. The combu s ti on ga s flow cha nge s with chan ge s in the inci nerato r co ndition s. The water flo wto the Hyd ro-So nics scrubbe r is a combi nation of reci rculate d water a n d makeu p wa t e r. Steam injectio n ca n be used to enha nce the particulate re moval of the Hydro

- Soni cs scrubb er.

4 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

An indu ce d d raft (ID) fan dra w s the co mbustio n g a s throu gh th e comb ustio n chambe r and APC sy stem and discha rg es th e g a se s throu gh an FRP (or eq uivalent) stack co nstructe d with sampli n g po rts an d platform s.

5 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

3.0 CA N D ID ATE S FOR ALTE RN ATIVE MONITO RIN G UN DER § 63. 8(f)
Lilly intend s t o in stall and operate a p a rticulate ma tte r CEMS, a m u lti-metal s CEMS, and an HCl CEMS to demon strate com p lian c e with the p a rticul ate m a tter, metals, and HCl/Cl 2 HW C MA CT emi s sion standards. As previousl y stated, Section 1209(a)(5) of the HWC MA CT allows Lilly to petition the Administrator und er Sectio n 63.8 ( f) of th e Ge ne ral P rovision s to u s e CEMS for complian c e m onitorin g fo r particulate m a tter, mercury, semivola tile metals, low volatile metals, and hydro c hlo r ic a c id/ c horin e ga s in lieu of compl y ing with the corre s p ondin g HWC MACT ope rating p a ram e ter limits. As requi re d in Sectio n 63.8(f), thi s appli c ation m u st contain a description of the propo sed altern ative monito ring system an d address the four elem ents co ntaine d in the definition of monitoring in Se ct ion 63.2 of the Gen e ral Provisio ns. T hose four ele m ents a re a s follows: 1) Indicato r(s) of Performa nce: The p a ram e ter or paramete rs you measu re or ob se rve for demon stratin g prop er o p e ration of th e pollution control me asure s or com p lian c e with the appli c able e m issi on s limi t ation or sta ndard. Indicators of p e rf orma nce ma y include di rect or predi cted em issi on s me asurem ents an d may b e ex pre s sed as a singl e maxi mum o r mini mum value; 2) Measurement Techni que s: The mean s by which you gather an d re co rd info rm ation of or a bout the indi cators of p e rfo r m ance. The comp one nts of the mea s urem ent tech nique i n cl ud e the detecto r typ e , locatio n and in stallati on spe c ificat ions, in sp ect i on p ro c ed ures, a nd q u a lity
assuran c e an d quality cont rol mea s u re s ; 3) Monitori ng F requ en cy: Th e num ber of times yo u obtain a nd reco rd monito ring data over a spe c ified time interval. E x amples of monitori ng freque nci e s in clud e at l east four points e qually spa c e d for ea ch ho ur for CEMS; and 4) Averagin g Time: The peri od over whi c h you averag e and use da ta to verify proper o peratio n of the pollution control app ro ach o r co mpli ance with the emissi on s limitation or st anda rd.

Pursuant to Section 63.8 ( f)(4 )(ii), t he a pplication mu st also contai n a perform a n ce evalu a tio n test plan (PETP) if req ueste d. The detailed info rmation c ont ained in this petition m eets the req u ire m ents of 40 CFR6 3 .8(e )( 3)(i ) whi c h s p ecifie s the inf o rmatio n that mu st be cont ained in a CMS PETP. T herefo re, th e PET P re qu ireme n t s fo r the p a rtic u la te matter CEMS, the multi-metal CEMS, a nd the HCl CEM S are met throug h su bm issi on of the detailed alte rnative monito ring petition.

6 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

In additio n , S e ction 3.4 of t h is altern ative mo nitorin g petition in clu d e s i n form atio n ju stifying th e requ est fo r an alte rnative monitori ng m e thod, such a s the te chni cal or economi cunfe a si bility, or the im pra cticality, of the affected source u s ing t he req u ired method. This meets the re quire ments of Section 63.8 ( f)(4)(ii).

3.1 PARTI C U LAT E MATTER CEMS 3.1.1 Indicator o f Performan c e The parti cula te matter CEMS is desi gned to co nti nuou sly mo nitor the sta ck ga s pa rticulate matter
con c e n tration

. Compliance with the particulate HW C MACT emi ssi on stand ard is demo n st rat ed whe n the particulate m a tter mea s u red sta c k co nce n tration i s le ss tha n or eq ual to the appli c abl e stand ard. Currently, Lilly must compl ywith the int e rim PM st andard of 34 m g /dscm, correc ted to 7 percent oxygen, spe c ified und er Se ction 63 .1203(b) of t he HWC MA CT. Lilly will com p ly with the HWC MA CT final PM stand ard spe c ified in Secti on 63.12 19(a ) no later tha n the date re quire d by Sect ion 12 06(a)(1)(ii) of th e HWC MA CTFinal Repl a c eme n t Stan dard s . T he averagi ng ti me for both the interim a nd final PM stand ard i s a 6-ho ur rolling averag e, upd ated every ho ur. 3.1.2 Measure men t Techniq u e 3.1.2.1 Opera t ing Pr inciples The total pa rticulate ma ss contin uou s e m issi on moni tori ng sy stem is a Sig r ist Du st Emissio n Me asu r in g System CT NR (o r eq uival ent), man u fa cture d by Sig r ist Pro c e s s-Photometer, AG. The Sig r ist sy stem is intende d to measure pa rticle ma ss concentratio n from the i n cin e rato r stack. It will withdraw a rep re s entativ e sam p le of the exhau st from the st ack and tran spo rt it, via the Sigrist ri ng pipe, for measurement by the photometer. The sample tra n sp ort system m a intain s sam p le stre am te mperature at approximatel y 160 o C (3 20 o F). A po rtion of the sampl e strea m is sep a rat ed (red uci n g orifice) a n d measured by the p hotome t er, then me rged ba ck i n to the mai n sa mple stre am for tra n sport back i n to th e incin e rato r st ack. A d a ta acq u isitio n system colle cts p a rti c le m e asu rem ent d a ta from the photo m eter throug h the S i grist Controll er. Figu re s 2 and 3 illu stra t e the major compon ents of the Sigrist CEMS, which inclu de:

1. Sample Extra ction System

2. Photometer 3. System Cont roller

4. Data Acq u isiti on System (DAS) and Hi storian

7 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

3.1.2.1.1 Sample Extraction System The Sig r ist sample syste m co nsi s ts o f a sam p le p robe and rin g pipe. T h e sam p le p ro be si ze wa s sele cted by the manufa ctu rer to provide an inlet gas velo city that is app roximat e ly1.0 - 1.5 times g reate r than the no rmal sta ck g a s velocity wh en sa mpling at the pre s et (de s ign ) rate of approximately 1 acm/mi n. This su pe r-i sokin e tic ope rating con d ition is u s ed t o minimize pa rt iculate mea s urem ent e r ro r that can be signifi cant at su b-i s o k ineti c conditio n s. The su pe r- iso k ineti cco ndition i s a n altern ative to continuo us monitori ng of the stack ga s velocity an d adjustm ent of the sampl i ng rate in order to mainta in iso k inetic conditions.

Stack ga se s are tran sferre d thro ugh a ri ng pip e whe re the g a s i s condition ed byheating to a pproxim ately 160 o C (3 20 o F) to vapo ri ze a n y water and acid droplets th at m a y be p re s e n t in the g a s stre am. A slip strea m of the sampl e gas is extra cted for “cont i nuou s” an alysis by the p hotomete r , which is al so heated to 16 0°C and ke pt at a con s iste nt pre s sure. After analysi s , the slip stre am ga s p a sses th rou gh a flow mea s u rement venturi and retu rn s to the bypa ss sam p le g a s strea m , which i s forwa rded by the blower, to the sample return prob e in the stack.

3.1.2.1.2 Photome t ric Analys is

The PM anal ysis is pe rformed by the photomete r wh ic h mea s u re s the attenuation in forwa rd light caused by the PM prese n t in the sampl e ga s. The p hotom eter me asure s forwa rd lig h tscatte red at 15 ofrom an inca nde scent bulb emitting over the ran ge of 360 to 2800 n anom e t ers. Du al be am com pen sation is u s ed in whi c h the li ght path i s sp lit and the intensity of th e referen c e pat h is adju s ted by an atten u a t or to e qua l the inten s ity of the mea s u reme n t path. The sample and referen c e scattere d li ght are co mbi ned a head of
a ph otocell, whi c h gen era t es a ph otoel ectri csig nal t hatis p rop ort i onal to the concentratio n of PM in the sampl e strea m . The instrument re sp o n se time is a pproxim ately 5 se con d s. The photo e le ctri c sign al is amplified to 4 to 20 milliampere (mA) and output to the data acquisitio n syst em (DAS) on one of four available ch annel s a c cording to the increa sing l e ve ls of inten s ity asso ciat ed with increasi ng PM
con c e n tration

. An a u tomat i c swit chin g d e vice ope rate s relays to block a si gnal being sent fro m the othe r three cha n n e ls. The system ca n also ope rate in a sin g le or lo cked range. Th e nominal P M
con c e n tration s asso ciated with the four measurement levels are 0-5, 0-1, 0-0.2, and 0-0.05 PLA base d o n a polystyrene latex aerosol (PLA) used i n facto ry cali bration of the monitor. Th e monito r’s o u tput sig nal, however, is al ways a singl e current value in the 4 -20 mA range. 3.1.2.1.3 System Controller

The SIGAR 4000 cont roll er, or equival ent, is the co nne cting lin k betwe en the photomete r , the sam p le transpo rt syst em, and the DAS. It com m unicates wi th the photo m eter, and p roce s se s and displ a ys the

8 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

particl e ma ss rea d ing si gnal. The SIGAR cont rolle r op erate s the sam p l e transpo rt system valves, heaters, blo w ers, a nd tem peratu re se n s ors. Th e co ntrolle r outpu ts crit i c al system informati on in cludin g the real -time mass re adin g , sample tran spo rt syste m temperature s , and co ntroll er pa ram e ters. It stores all the th re sh old pa ram e te rs fo r th e Sig r ist p hotom et er. It provid es relay co ntact in put an d outputs to sign al photo m eter a nd sa mple tra n sp o rt system stat us . It provide s the u s e r int e rface for p h otometer and controlle r parameter setup and preservat i on.
3.1.2.1.4 Data Ac quisi ti on System and His t oria n The Sigri s t m i cro co ntrolle r provide s system ope rati o n , status, in st rume nt outpu t, and ran ge i dentificatio n to a com put erized DAS. The DAS p e rform s all d a ta cal c ulatio ns for com p li ance. All data, system operation, sta t us, and qu ali ty assu ran c e data are stored in a histo r i an. 3.1.2.2 Installation Loca t ion The Sig r ist P M CEMS will be lo cate d a ta point i n t he stack that allows a rep resentative sample to be extracted fo r sub s e que nt analysi s . This location will be at least two du ct diam eters from th e top of the stack, a nd at lea s t two d u ct di amete rs d o wnstrea m from th e l a st p o int of i n terferen ce. The fin a l P M CEMS location will be determine d duri n g the correlation test. 3.1.2.3 Installation
The PM CE MS will b e in stalled pe r m anufa cture r’ s re comm end ations. The CEMS will b e in stalled i n a locatio n su ch that the co rrelation between th e PM CEMS respo n se an d emi ssi on s d e termined by a referen c e me thod will me e tthe perform ance sp ecifi c ati ons stated in this do cum ent. Once th e system i s installe d, it wi ll be commi ssioned fo r u s e. This exe rcise will verify th e system i s i n stalle d prop erly pe r the manufa cturer’ s sp ecifi c atio n. 3.1.2.4 Instrumen t Span The operating range of the PM CEMS will be establi s hed during t he CEMS init ial startup and correlation test plan p e ri od. Lilly will verify that th e ope rati ng range (zero to span ) will e n c omp a ss the respon se of the PM CEMS for all expected waste stream s. 3.1.2.5 System Start Up (Initial O p eratio n) The Sig r ist wi ll be starte d a nd allo we d to run u s ing am bient ai r in th e sample line

. A valve, located at th e probe, allows Lilly to start the sy stem with ambient air as opposed to flue gas. The system will run on ambient ai r for app roxima tely four wee ks. Du ring t h is time, Lilly will che c k t he operation o f the system and corre ct any issu es that arise.

9 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

After this approximate four-week pe ri od, Lilly will sampl e the flue ga s under different feed conditions (su r rogate m a terial, liquid waste, so lid waste, natu ral ga s, fuel oil). Lilly will sam p le flue ga s fo r approximatel y 4-8 wee k s. The obje ctive is to corre ct any issu es th at ari s e, an d begin to com pare the type of waste burned to th e out put of the Si grist. Linearity checks w ill begin duri ng this phase of the PM CEMS operation.

The line a rity che c k is a proce dure which ch ecks the inst rument drift at five lev e ls . With an ins t rument respon se ra n ge of 4 to 20 milliamp s, the linearity te st ch e c ks th e in strum ent d r ift at app roxima tely 4, 5, 8, 12, and 16 mi lliamps. The percent d r ift will be calculated as:

Percent Drift = 

### 100 * Span R R REF

CEMS 

### −

whe re:
Percent Drift = Amount of drift (%)

R CE M S = The measured PM CEMS re spon se (mA )

R REF=The PM reference standard value (mA) Span =Sp an of the instrum ent (20 mA)

3.1.2.5.1 Preliminary Correla tion Test Plan Pe riod

The inte nt of the prelimina r y correlatio n t e st pl an p e ri od (P CTPP) durin g the PM CEMS startup is to: (1 ) unde rsta nd the affect of specifi cmateri als (su rro gat e material an d/or ha za rdo u s waste ) on the resp on se of the Sig r ist PM CEMS (2) e s tabli s h a prelimina ry co rrelation t o predi ct pa rticulate m a ss in terms of mg/scm, based on the out put of the PM CEMS. It is expected that the PC TPP will take up t o 16 weeks. Activities du ri ng the P C TP P will follo w g u idan ce i n 40 CF R 60 App endix B, Perf orma nce Spe c ificatio n 11 (PS11). The followin g acti vities will be condu cted d u ri ng the PCTP P: Seven-Day Drift : Prior to beginni ng the PCTPP, the PM CEMS wi ll have passe d a seven

- da y drift test. For seven consecutive days, the lineari ty check will be completed. T he percent drift at five l e vels will be recorded. Each value mu st be within 5 % of the reference value.

Referen c e M e thod: Duri ng the PCTPP , Lilly will use Method 5 or Method 5i as the reference method. Lilly will u s e dual train s (p erpe ndi cula r t rain s ) for t he referen c e m e thod (RM ) sa mpling. The targets a re 60-mi nute ru ns. Sh orte r o r lon ger run s may be ne ce ss ary. F o r e x ample, for hi gh p a rticulate loadin g , the

10 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

test runs ma y only be 45 minute s d u e to excessiv e pressu re d rop acro ss t he filter, a n d for ve ry lo w particulate loading, test runs may be 120 minutes. The averagi ng time for each run will be documented. Lilly will treat each sam p le train result in the data set as an individual data point. Data rang e: Duri ng the PCTPP, Lilly will colle ct at le ast 15 vali d d a ta sets con s isting of simul t aneou s PM CEMS and d ual RM me asurem ents. M o re may be collecte d so th at certain te st results may be reje cted. Lilly will attempt to coll ect data in three ranges [(Low) from zero to 50% of maximum m easured PM
con c e n tration ; (Mid) 2 5 – 75% of the maximum me asu red PM concentratio n ; and (high ) 5 0 to 100 % o f the maximum mea s u red PM co ncentration]. The go a l is to have at lea s t 20% of the total dat a in ea ch o f the three ran ges. A data set ca n only be used for one ra nge. Li lly will use zero poi nt data for the low values if a re spo n se at the low level ca n not be achiev ed.

Referen c e M e thod Data : Duri ng the P C TPP, Lilly will evaluate the preci s ion of the two sam p le trai ns by determi ning t he rel a tive standard devi a tion (RSD) fo r ea ch p a ired data set and comp ari ng it to the recommended maximum RSD. The RS D will be cal c ulated for each test run usi ng the followi ng equation:



### ) ( ) ( * 100 b a b a 

### C C C C RSD + − =

whe re:
RSD = relativ e stand ard d e v iation (%)

Ca = con c e n tration me asured usi ng Trai n A, units of concentratio n
Cb = con c e n tration me asured usi ng Trai n B, same uni ts as Ca.

Pursuant to Section Z.1.4 of EPA’s Draft Guidance Document on PM CEMS, the recommended maximum RSD will be determined as follows:

• For avera ge PM co ncentrations that a re at le ast 10 mg/dscm (o r at lea s t 10 m g /acm ), the recomme nded maxim u m RSD is 1 0 %

• For ave rag e PM con c ent rations that a re less than o r equ al to 1.0 mg/dscm (o r less than or eq ual to 1.0 mg/acm), the re co mmend ed ma ximum RSD i s 25%; and

• For ave rag e PM con c e n trations betwe en 1.0 an d 1 0 mg/dscm (or betwee n 1

. 0 and 10 mg/a cm ), the re comm ende d maxi mum RSD is dete r mine d usin g the foll owin g equatio n:

11 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition


### ) 67

. 1 67

. 26 ( ave r 

### C RSD

− =
whe re:
RSD r = re co mmend ed m a ximum RSD for avera g e PM con c ent ration betwe en 1. 0 and 10 mg/d scm, (%).

C av e= average PM con c ent ration for the Train s A and B, units of co nce n tration EPA’s draft guidance document on PM CEMS is provided in Appendix A.

If the RSD a nalysi s sh ows that the dat a for all te st runs are withi n the re com m ende d maxi mum RS D, n o further assessment of data preci s io n will be perform ed. If the RS D shows one or more outli ers, Lilly will use th e sta n dardi ze d resi dual meth od. Und e r th e standardized resid ual meth od, Lilly will plot data that comp ares Train 1 samplin g re sults to T rain 2 sam p ling results. T he lin ear rel a tionship m u st have a sl op e falling betwe en 0.93 an d 1.07. Data sets will be re moved until the refe ren c e method dat a meets thi s criterion.

Prelimina ry Correl ation Developme n t: Valid refere nce metho d data (Trai n 1 and Trai n 2 as i ndividu al points) will be plotted against the Sigrist output (mA or PLA ) averaged ov er the samp l e period. T h e averag e Sigri s t output will be on the X

- axis a nd RM re s u lt, in mg/sc m (to repres ent the c o nditions in sampl e train stand ardi ze d to stan da rd t e mpe rature a nd p re s sure) on the Y-axi s . Using the equatio ns i n PS11, Lilly wi ll cal c ulate up to five correl ations (1 ) lin e a r (2) polyn o m ial (3) l oga ri thmic (4) exp onential (5 ) power correl ation model s. Each attempted co rrel at ion will ha ve the correl ation co effici ent, toleran c e interval, and confidence i n terval cal c ul ated as described in PS11. Lilly will co mpare the correlation coeffici ent, confiden ce int e rval, an d tol e ran c e inte rval to the limits in PS 11. A succe s sfu l preli m ina ry correl ation wi ll be obtained , that uses re al-time CEM S va lues to predi ct PM co nce n tration s i n mg/scm, if all statistical che c ks in PS 11 are m e t.

Duri ng the correl a tion dev elopment, dri ft from the linear ity checks will be recorded daily. If the drift, for any of the values, exceeds 8%, the PM CEMS will be adjusted and a new dr ift test performed.

3.1.2.6 PM CEMS Calibration Co rrelati on Te s t(PM CEMS Certification)
The obje ctive of the calibration co rrel a tion te st p e rio d (CCTP) is to colle ct data , while bu rni n g ha za rdo u s waste, to est ablish a correlation wh ich will predict t o tal parti culat e ma ss emi s sions, in mg/s cm, based upon the out put of the Sig r ist PM CEM S . PS 11 will be used as guida nce to e s tabli s h a vali d calibration correl ation.

12 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

The followi ng activities will be conducted dur ing the CCTP: Seven day Drift : Prior to begin n ing th e CCTP, the PM CE MS will have pa ssed a seven day drift test pursuant to S e ction 8.5(3) of PS 11. F o r seven consecutive days, the linearity check will be com p leted. The percent drift at five le vels will be recored. Each value must be within 5% of the reference value.

Absolute Correlation Audit : The ab solut e correlatio n audit (ACA) e v aluates the PM CEMS re spo n se to a seri es of refe ren c e sta nda rds coverin g a full measu re m ent ran ge o f the instrume nt. To condu ct this audit the PM CEM S will be cha llenge d three times at ea ch of the five audit points. Lilly will follow Se ction 10.3(2 ) of 40 CFR 60 App endix F Pro c edure 2 (P ro ced u re 2) a s guida nce for con d u cting th e ACA. The average response will be used to calc ulate the accuracy at each audit point. T he ACA will be cal c ul ated usin g the eq u a tion in Pro c edure 2 liste d below. Th e erro r can not excee d 10% of the audit value, or 7.5% of the applica b le stan dard; whi c heve r is greate r

.

ACA Ac curacy = 

### 100 *
REF REF CEMS 

### R R R

−

whe re:
ACA Accura cy = The ACA accuracy at e a ch a udit poi nt, (%)

R CE M S =the measure d PM CEMS re spo n se to the referen c e stand ard (mA )

R REF=the PM refere nce sta ndard value (mA)

Stratific a tion Tes t : Lilly wil l test for PM stratification by followi ng the same g eneral step s spe c ified f o r gaseous pollutants , and following the guidanc e spec ified in S e ct ion V.5 of EPA’s Draf t Guidanc e Do cume nt on PM CEMS. To dete r min e wheth e r effluent stratificati on exists , a d ual p robe sy stem will b e use d to dete r mine the averag e effluen t concentrati on whil e me asu rem ents at each trave rse point a re being ma de. One probe, l o cate d at t he stack cent ro id, will be used as a stati onary refere n c e point to indicate cha n ge in the effluent con c ent ra tion over ti me. The second prob e will be use d for sam p ling at the traverse poi n t s spe c ified i n Method 1 (40 CFR par t 60 appe ndi x A). The monitorin g sy stem sam p le s simultan eou sl y at the reference and trav erse points th roug hout the testing pe riod for approximately fifteen minutes at each poi nt. A minimum of 12 sam p ling po ints will be used, with 6 sampling points along each of the two traverses. Lilly will us e M e thod 5 as the sampling method and sample at least 15 minutes at each sam p lin g point.

13 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

The PM co nce n tration s at each traverse poi nt are the n compa red to the avera g e of the P M
con c e n tration s for all samp ling points to determi ne th e percent stratification u s ing the followin g equatio n:


### % 100 * ave i 

### C C S

− =

whe re: S = percent stratification

C i = PM concentration at sampling p o int

C av e= average PM con c ent ration for all sampling p o ints

. If the percen tstratificatio n is le ss th an or e qual to 10 pe rcent f o r any traverse p o int, the duct i s not
con s id ere d st ratified at that location.

Referen c e M e thod: Lilly will use Metho d 5 o r M e tho d 5i a s th e referen c e metho d . Lilly will use dual trai n s (pe r pe ndi cula r trai ns) fo r th e refe re nce method (RM) sa m p ling. T he targets are 60 -minute runs. Short e r or lon ger run s may be n e cessary. For example, for high pa rticul a t e loading, th e test run s m a y only be 45 minutes du e to exce ssive pre s sure d ro p a c ro ss the filter, and fo r very lo w p a rticulate l oadi ng, test run s may be 120 minutes. The averagin g time for each r un will be wel l docum ented . Lilly will adhere to PS11 and treat ea ch sampl e trai n result in the data set as a n individual d a ta point.

Data ran ge: Lilly will adhere to PS11 for th e data collection. T h is requires at least 15 valid data sets
con s i s ting of simulta neou s PM CEMS and d ual RM mea s u rem ents. Mo re may be colle cted so tha t certai n te st results m a y b e reje cted as long a s at l east 15 valid data sets are u s ed to de termine the correl ation. All data will be reported. Lilly will attempt to collect data in three ranges [(Low) from zero to 50% of ma x PM concentration; (Mid) 25 – 75% of the max PM concentratio n ; and (hi g h ) 50 to 100 % of the max PM concentratio n ]. The goal is to have at least 2 0 % of the total data in ea ch of th e three ra nge s. A data set can only be u s ed fo r o n e range. Lilly will use zero point data for the low values i f a response at the low level cannot be achi eved.

While colle cti ng total parti culate ma ss data duri ng the CCTP, the intention is to c o llecttotal particulate data that is clo s e to, but not sig n ifica n tly greate r than the total parti culate mass emi s si on sta nda rd

. Ho wever, be cau s e th e p u rpo s e of CCTP i s to d e velop a n a c ceptabl e co rrel a tion that can verify compli an ce a tthe emissio n stan dard, it is impo ssibl e to en sure t hat the total particulate m a ss emi ssi on stand ard will not be ex cee ded d u rin g so me of the te st run s . Accordingly, emissi ons stan dard s from pa rts 60, 61, 63, 264, 265, a n d 266 of Titl e 40 of the Cod e of Fed e ral Reg u lati ons do not apply whil e

14 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

con d u cting a correl ation te sting prog ra m. Any permit or other em issi on s or op erating p a ra meter limits o r con d ition s , includi ng any li mitations o n work pl ace p r acti ce s, that are ap plicab le to ensu re compli an ce with the emission s stand ards of parts 6 0 , 61, 63, 2 6 4 , 265, a nd 266 of Title 4 0 of the Cod e of Fed e ral Reg u lation s a l so do n o t ap ply while con ductin g a co rrelation testin g prog ram.
Referen c e M e thod Dat a : Lilly will evaluate the precisi on of the two sampl e trains by determining the relative stan dard deviatio n (RSD) for each pai re d data set an d co mpa r ing it to the re comm end ed maximum RS D. Lilly will follow the gui dance provided in Section Z.1.4 of EPA’s Draft Guidance Document on PM CEMS . The RSD will be cal c ulat ed for ea ch te st run u s ing t he followi ng e quation:



### ) ( ) ( * 100 b a b a 

### C C C C RSD + − =

whe re:
RSD = relativ e stand ard d e v iation (%)

Ca = con c e n tration me asured usi ng Trai n A, units of concentratio n
Cb = con c e n tration me asured usi ng Trai n B, same uni ts as Ca

Pursuant to Section Z.1.4 of EPA’s Draft Guidance Document on PM CEMS, the recommended maximum RSD will be determined as follows:

• For avera ge PM co ncentrations that a re at le ast 10 mg/dscm (o r at lea s t 10 m g /acm ), the recomme nded maxim u m RSD is 1 0 %

• For ave rag e PM con c ent rations that a re less than o r equ al to 1.0 mg/dscm (o r less than or eq ual to 1.0 mg/acm), the re co mmend ed ma ximum RSD i s 25%; and

• For ave rag e PM con c e n trations betwe en 1.0 an d 1 0 mg/dscm (or betwee n 1

. 0 and 10 mg/a cm ), the re comm ende d maxi mum RSD is dete r mine d usin g the foll owin g equatio n: 

### ) 67

. 1 67

. 26 ( ave r 

### C RSD

− =
whe re:
RSD r = re co mmend ed m a ximum RSD for avera g e PM con c ent ration betwe en 1. 0 and 10 mg/d scm, (%).

C av e= average PM con c ent ration for the Train s A and B, units of co nce n tration

15 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

If the RSD a nalysi s sh ows that the dat a for all te st runs are withi n the re com m ende d maxi mum RS D, n o further assessment of data preci s io n will be perform ed. If the RS D shows one or more outli ers, Lilly will use th e sta n dardi ze d resi dual meth od. Und e r th e standardized resid ual meth od, Lilly will plot data that comp ares Train 1 samplin g re sults to T rain 2 sam p ling results. T he lin ear rel a tionship m u st have a sl op e falling betwe en 0.93 an d 1.07. Data sets will be re moved until the refe ren c e method dat a meets thi s criterion. All data will be saved and submitted. Regard less of whi c h method is used, any potential outliers will be investigated to determine possibl e causes for t he lackof precisi on.
Correl ation Developme n t: Valid referen c e metho d d a ta (Trai n 1 and Train 2 a s individual p o ints) will be plotted agai n s t the Sigrist output (mA or PLA) av e raged ove r the sampl e pe riod. The ave rage Sig r ist output will b e on the X-axis and RM result, in mg/scm (to re pre s ent the con d ition s in sampl e trai n standardi zed to standard temperature and pres sure) on the Y-axi s . Usi ng t he equations in PS 11, Lilly will cal c ulate u p to five correlation s (1 ) linear (2) p o l y nomial (3 ) logarith m ic (4 ) expone ntial (5) po we r correl ation m odel s. Ea ch attempted correlation will have the co rrel a tion co efficient, tole ra nce inte rval, and co nfiden ce interval calcul ated as descri bed in PS 11. Lilly will com pare the correlatio n coefficie n t, confid en ce i n terval, and toleran c e int e rval to the limits in PS 11. A successful co rrel ation will be establi s h ed t hat uses real -time CEMS value s to predi ct pa rticulate con c e n tration in mg/scm if all statisti cal che c ks in P S 11 are met

. If the PM CEMS does notpass th e statistical limits for any of the five correl ations, Lilly, with appropriate agency review, m a y develop an altern ative correl ation by providing an explanation o f how co mplia nce d e mon s tration wo uld b e assured.

The correlati on establi s hed during the CCTP for the PM CEMS will supersede any previous correl ations, whi c h may ha ve been e s ta blish ed.

Duri ng the CCTP, drift from the linearity checks will be recorded daily. If the dri ft, for any of the values, exceeds 8% once, the PM CEMS will be adjus ted and a new drift test perf o rmed.

3.1.2.7 Rou t ine Ope ration of the PM CEMS
3.1.2.7.1 On-G oing Q u alityAssura nce
This section descri b es the on-going quality assurance that will be perf orm ed on the PM CEMS to ensure that it continues to op era t e corre ctly and pro d u c e s valid data. These qualityassura nce a ctivities will
occur only when the PM CEMS is op e rational

. Lill y will follow Procedure 2 and EPA’s Draft Guidance Do cume nt on PM CEMS located in Appendix A of this docu m ent whe n perfo rming o n -goi ng qu ali ty assuran c e on the PM CEMS.

16 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

3.1.2.7.2 Rou t ine Syst em Chec ks Daily che c ks of the PM CE MS will b e do ne a c cordi ng the re com m e nded ch eckli s t provide d by Sigrist, a s modified by Lilly. Data status flags will be used to troubleshoot any problem s th at arise in the PM CEMS system. This meets the int ent of the daily system ch e c ks in PS11.

3.1.2.7.3 Wee k lyLinearity Drift Ch ecks Lilly will perf o rm a linea ri ty check on ce per wee k

. This will be perform ed manually a c cordin g to the pro c ed ure ou tlined in the Sigrist op eratio nal manu al.
The pe rcent drift is cal c ula t ed as:

% Drift = 

### 100 * Span R R REF

CEMS 

### −

whe re:
% Drift = Drift of the CEMS (% )

R CE M S = the measured PM CEMS re spon se (mA )

R REF=the PM refere nce sta ndard value (mA) Span =Sp an of the instrum ent (20 mA)

Five values between 0-20 mA will be checked. T he actual val ue( s) will be adjusted when the drift
excee d s 5% for any of the five values. (Refer to Sectio n 3.1.2.9 for out of control definition). The Sigri s t wi ll be off-line for up to on e hour duri ng the li nea rity check. All cali bration data collecte d alon g with the drift percenta ge will be recorde d . Durin g this time, the 6-hour rolling blo ck ave rag e wi ll be froze n

. 3.1.2.7.4 System Audi ts

3.1.2.7.4.1 Quar terly Absolute Corre lation Audi t (ACA)

The ab solute co rrelation audit (ACA) evaluate s th e PM CEM S re spo n se to a se rie s of refe ren c e stand ard s co vering a full measurement ra nge of the inst rume nt. To cond uct this audit, Lill y will p e rfo r m the linearity d r ift che ck. Th e PM CEMS will be challe nged th ree ti mes at ea ch of the five audit points. Th e

17 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

average response will be used to calc ulate the accuracy at each audit point. T he ACA will be cal c ul ated usin g the Equ a tion 2-1 in P rocedu re 2 a s follows:

ACA Ac curacy = 

### 100 *
REF REF CEMS 

### R R R

−

whe re:
ACA Acc u ra cy= Accu ra cyof the CEMS (% )

R CE M S = the measured PM CEMS re spon se (mA )

R REF=the PM refere nce sta ndard value (mA)

The erro r can not exceed 1 0 % of the audit value, or 7.5% of the ap plica b le stan d a rd; whi c h e ver is greate r

. The ACA will be performed each quarter.
3.1.2.7.4.2 Quar terly Rela tiv e Response Au dit ( R RA )

The relative respon se au dit (RRA) i s a b r ief seri es of tests con ducte d b e tween ann ual fu ll re sp on se correl ation a udits (RCA ) to assure the contin ued val i dity of the PM CEMS correlation. The RRA will be perfo rmed by colle cting, at curre n t sou rce conditi o n s, three refe re nce m e thod sampl e s and PM CEMS measurements at the as-fo und so urce o peratin g con d i tions. The d a ta poi nts will be plotted on the cu rre nt calib ration co rrel a tion fu nct i on. T o me et the RRA pe rforma nce crite r ia, the thre e points mu st b e le ss tha n or e qual to th e hig h e s t CE MS value s u s ed for the cali bration curve and tw o of th e thre e sets o f PM CEMS and RM m e asu rem ents must fall wit h in a sp ecifi ed are a on t he gra ph of the calib ratio n co rrel a tion function. Th e spe c ified are a is two line s parall e l with t he correlation reg re ssi on curve, offset at a dista n ce of ± 25% of the nume r i c al emission limit val ue from the correl ation regre s sion cu rve.
If the PM CEMS does n o t meet the RRA criteria, Lill y w ill take the nece s sary corrective a ction to eliminat e the probl em a nd rep eat the test. If the RRA crit e r ia ca nnot be a c hie v ed, Lilly will perfo rm an RCA.

3.1.2.7.4.3 Annu al Resp on se C o rrela tion Audi t (R CA ) Lilly will perfo rm a respon se co rrelation audit (RCA ) a nnually. The quarte rly RRA will not be perfo rmed i n the sam e qu arter th at the annu al RCA i s preform ed. The respon se co rrelation audit (RCA ) i s a seri es of tests conduct ed to assu re the continued validity of the PM CEMS correl ation. Lilly will conduct the RCA as prescribed in PS11 a nd Procedure 2. Lilly will collect a mi nimum of 12 data points attempting to disp erse the points th rou g h low, mi d, a nd high ran g e s o n the cali bration co rrel ation fun ction . The points

18 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

will be plotted on the current calibrati on correl ation function. T o m eet the RCA criteria, 75% of the points must fall within a spe c ifi ed are a on the co rrel a tio n regressio n curve. The spe c ified a re a is two line s parall e l with t he calibration co rrel a tion functio n , offse tat a distan ce of ± 2 5 % o f the nume r ical emissio n limit value from the correlat ion reg re s sio n curve.
As defined i n Section 10.6 of Proced ure 2, if Lilly d oes n o t meet t he perform ance criteria, then the two data sets (cu r rent co rrelatio n an d the current RCA ) w ill be co mbine d and the co rrelation statisti cs in PS1 1 applie d. If a correl ation fro m the combin ed data sets pas se s the st atistical li mits, this correlati on be co me s the new co rre lation cu rve. If the stat istical limits are n o t met with the com b ined d a ta, Lilly will use o n ly the RCA data an d run th e PS 11 statistics. If the statisti cal lim its a re met, this i s th e ne w co rrela t ion curve. If the statisti cal limits are not met for the RCA data, the correl ation te st will b e re d one with a mi nimum of 1 5 data points, applying the st atistics in PS11. If the new data do no t meet the statistical crite r i a for any of the five PS11 equations, and assumi ng no definabl e probl ems exist with t he PM CEM S , Lilly, with approp riate a gen cy revie w , may develop an alternati v e correlatio n by providin g an explan a t ion of how compli an ce d e mon s tratio n woul d be a s sured.

While colle cti ng total parti culate ma ss d a ta duri ng th e RCA , the in tention is to collect total pa rticulate data that is cl ose to, but not si g n ificant ly gre a ter than the total particula te mass emi s sion stan dard

. However, becau se the purp o se of RCA is to verif ythat the co rrelation i s sui t able for com p lying with th e emissio n stand ard, it i s impo ssi ble t o en su re th at the total p a rti c ulate ma ss emission sta n dard will not be ex ceed ed durin g some of the test ru ns. Acco rdin gly, emission s sta nda rd s from pa rts 6 0 , 61, 63, 26 4, 265, an d 26 6 of Title 40 of the Code of Federal Regulatio ns d o not apply while con d u cting a co rrel a tion testin g prog ram. A n y permit o r other e m issions or o p e rating pa ram e ter limits o r con d ition s , in cludi ng any limitations o n wo rk pl ace pra ctices, that are a p p licabl e to en sure complia nce with the emission s stand ard s of parts 60, 61, 63, 26 4, 265, and 266 of Title 40 of th e Code of Fe deral Regul ations also d o not apply whil e con d u cting a correl ation testing p rog ra m. 3.1.2.8 Compon ent Replac emen t Duri ng no rma l ope ration of the PM CEM S , spe c ific co mpone nts will nee d to be repla c ed. The PM CEMS stand ard op erating p ro c edures will address th e crite r ia to be met upo n re pla c eme n t of si gnificant comp one nts. 3.1.2.9 Out of Con t ro l Lilly will adjust the PM CEMS when t he drift is equal to or greater than 5%

. Lilly will consider the P M CEMS out of control if drift, for any of the five va lues, exceeds 8%. In additi on, the CEMS will be deemed out of control if the PM CEMS fails to meet the RCA criteria, RRA crit eria, or ACA criteria.

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The out of co ntrol pe riod will begi n im mediately after t he la st test run or che ck of an un succe ssful RCA, RRA, ACA, o r linea rity drif t che ck. T h e out of contro l perio d en ds immediately after the la st test ru n o r che c k of the sub s e que nt succe ssful au dit or drift ch eck, when th e metals CE MS is used a s a back-up, or whe n the i n ci nerato r enters p a ra metri c mode. Wh en the in cine rat o r i s o peratin g in parametric mo de, th e PM CEMS will not be deem ed out of cont rol. 3.1.3 Use o f the P M CEMS for Compliance w i th the HWC MACT PM Standa rd Lilly may begin usi ng the PM CEMS to demonstrate continuous compli ance with the HWC MACT PM emission stan dard o n ly after the followin g is achieved:

• A succe ssful PM CEMS Calib ration Correlation Te st as sp ecifi ed in Sectio n 3.1.2.6 followin g EPA’s approval of this Alternative Monitoring Petition.

• A modificatio n to the Title V pe rmit i s a pproved t hat in corpora t es the re qui reme nts of the approved Alternative Mo ni toring Petition

. Followi ng completion of t he above, on-going quality assurance will be performed on the PM CEMS as spe c ified in S e ction 3.1.2.7 of this docu m ent. 3.1.4 Monitoring F requen c y an d Av eraging Time

The PM CEM S will provide a six-hou r rol ling block av e rage in mg/d scm co rrecte d to 7% oxygen. The sixhour blo ck averag e was se lected as re p resentative of the time pe ri od to colle ct three man ual particulate measurement sampl e s. One-mi nute val ues will be used to develop 15-mi nute average values, which will be used to de velop one -ho u r blo ck ave rage value s a nd six-h o u r ro lling blo ck av erag e value s

. Usi ng the equation from t he cali bration correlation, the PM CEM S output values will be converted to mg/scm each minute. The Ecoch e m CEMS will sen d the DAS one-min u te average oxyge n and moi s ture values to u s e to correct the PM CEMS value s to mg/dscm at 7% oxygen.
The pa rticul ate stack con c e n tration will b e corre cted to 7% oxygen by the followin g equatio n:

2 

### 21 7

21 * O PM PM uncorr corr



### − − =

whe re: PM corr = PM concentratio n corre cted to 7 % oxygen (mg/dscm) PM uncorr = PM stack ga s co nce n tration (mg/dscm ) O 2 = Oxygen stack ga s pe rcent (vol % dry)

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The 15-minut e data i s the averag e of th e on e-mi nute data withi n t hat blo c k of time. Only o n e valid one minute value is req u ired to achi eve a valid 15-mi nute a v erage valu e. The hourly bl ock average will be calcul ated from the f our 15 minute averaged val ues during the hour as sho w n in the followin g equ ation:



### 4 4

1 

# ∑

= 

### = i 

### Ci HBA
whe re:

HBA = Ho urlyblock avera g e value (mg/d s cm co rrecte d to 7% O 2 ) Ci = a fifteen minute ob se rvation from the CEMS anal yzer (mg/d s cm corre cted t o 7% O 2 .)

In the event that four vali d 15 -m in ute averag ed values a re not available to cal c ulate an hourly blo ck averag e (i.e. the CEMS p rodu ced pro b l e matic d a ta), valid re sults must b e avail able for at le ast three 15

- minute cycl es of operation t o ca l c ulate a one-hou r blo c k avera ge.
The six-hou r rolling ave ra g e will be calculated ba se d on the avera ge of the six mo st re ce nt hourly blo c k averag es a s sho w n in the followin g equ ation:



### 6 6

1 

# ∑

= 

### = i 

### HBA SHRA
whe re: SHRA = Six h our rolling av erag e value (mg/dscm corrected to 7% O 2 )
HBA = Ho urlyblock avera g e value (mg/d s cm co rrecte d to 7% O 2 )

The six-h o u r rolling bl ock averag e will be update d e v ery hour wh en a new, val i d, hourly blo ck ave rag e is cal c ulate d

. 3.1.5 Rolling Bloc k Av erage Calculations d u ring Rou t in e Chec ks an d System Au dits Lilly will put t he PM CEMS in a no n-m e asu re m ode once pe r wee kfor up to o n e hou r in ord e r to p e rfo r m the we ekly lin earity che c ks while bu rnin g ha za rdou s wa st e. Durin g this time, bl ock ave rag e cal c ulatio n s will be frozen. Rolling block hour average calculations will resume once t he linearity check is successfully

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perfo rmed. T he six-ho ur rolling blo c k a v erage calcul ations will re sume byaddi n g the fi rst vali d ho ur blo c k averag e after the linearity che c k to the previou s five hour bl ock av erag e value s

. The rolling av erage cal c ulations will al so be frozen during the quarterly absol u te corr el ation audits. Block hour ave rag e cal c ul ation s will resume o n ce the audit is compl e te. The A C A au d i ting may ta ke mo re th an one ho ur to complete.

The PM CE MS DAS u s e s the oxygen con c e n tratio n and moi s tu re conte n t fro m the Ecoch e m CEMS to
corre ct the o ne minute averag e mg/s cm con c e n trati ons of PM to 7% oxygen, dry ba sis. O n ce per day , the Ecochem will be in cal i bration m o de for up to one hour. During this time t he PM block average will also be frozen. Incinera tor operations will attem p t to mai n tain st able operating param e ters during times of calibration.
3.1.6 Bac k up to th e Particula t e Matte r CEM S

In the event t he PM CEM S is not operating, Lilly wi l l have the option to use th e multi-metal s CEMS as a backu p to the PM CEMS under the follo wing con d itions:

1. Re sults obtai ned from p a rallel op eratio n of the tw o CEMS will b e u s ed to de velop a te ch nica l justificatio n of how the m e tals CEMS p rovides rea s o nable a s su ra nce of compli ance with the PM emission stan dard.

2. Whe n the PM CEMS is n o t operatin g and the mu lti

- metal s CEM S begins u s e as a ba ckup , Lilly will use its b e st efforts to avoid introd ucin g ne w waste st ream s (i.e. those that have not been histori c ally b u rne d whil e the two CE MS were in parallel o p e ration ) from the six “in-feed” conveyo rs to the final “merge” conveyo r that leads to the kiln fee d chute.

In ord e r to allow CEMS mode to e s tabli s h wa st e stre am s that are not “ne w ” du rin g its initial impleme n tation p e rio d , th e ab ove restriction s on u s e of the multi

- metal s CEM S se rving a s a ba ckup fo r the PM CEM S will apply only after a suf ficient time pe riod has elapsed ( not to exceed 6 months from the first CEMS m ode o peratio n) for Lilly to gain exp e rie n c e while pro c essing a vari ety of existing soli d waste strea m s. Fin a lly, Lilly will attempt to m a intain nomi n ally stable or histori c allylowe r feed rat e s of wa ste while th e ba ckup i s b e ing use d , and wil l limit the use of the multi-metals CEM S as a b a ck up for the P M CEMS to 14 con s e c utive d a ys per e p iso de. Lilly will use i t s best efforts to minimize t he time thatthe multi-m e tals CEMS acts as a backup to the PM CEMS. To facilitate its ef forts, Lilly will kee p sp are parts i n sto ck and will m a i n tain a servi c e relatio n ship with the PM CEMS ma nuf acturer, or other qualifie d con s ulta nts, t o minimi ze d o wntime. If both the PM CEMS and the multi-metal s CEMS are not i n use, L illy will m onit o r operating parameter li mits defined i n

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Section 1 209 of the HWC MACT (i.e. para m etri c o perat io n). De tails of the specifi cop erat ing limits a re provide d in the Notificatio n of Complia nce (NOC). Lilly will incorporate delay s when t ran siti oning from th e CEMS mod e of ope ratio n to the para m etric m ode of ope ratio n . Spe c ificall y , once the prim ary PM CEMS and the ba ckup multi-m e tals CEMS are unavailabl e, the control system will aut omatically switch to the p a ram e tric mo de of o p e rati on. Rolling averages, rel a ted to the Air Pollution Control Syst em (APCS ) , will not start un til the sy stem has been unde r the parametri c mode of operation for 10 minute s . This 10-minute time peri od will allo w Lilly time to make any adjustments to the APCS to brin g the sy st em to withi n the re spe ct i ve ope rating paramete r limits. In addition, up to four hou rs will be allowed b e fore re-starti ng co nstitue n tfeed rate rol ling avera ge operating p a rameter limits in ord e r to clea r the soli d feed conve y or syste m . (Note th at, in a simila r fashion to t h e “backup” sc enario descri bed above, Lill y will use its best effo rts to avoid introducing “new”
wa ste strea m s from the si x “in-fe ed” co nveyors to th e final “me rg e ” conveyo r t hat lea d s to t he kiln fe ed chute duri ng this four hou r perio d. Ho wever, d u rin g initial CEMS mode o peration pe riod s t here will be pra ctical limit ations to this criteri on be cause fe w wa ste stream s will have be e n burned.) F eed rates will be maintain e d nominally stable or hi sto r ically lo we r than when o p e rating in CE MS mode. If the CEMS mode of op eration is sti ll not availa ble after fou r ho urs, the tran sition to parametri c mode will b e compl e ted an d only wa ste with kno w n compo s ition wi ll be proce ssed in the i n ci nerato r so th at co nstitue n t feed rate op e rating pa ram e ter limits ca n be com pute d

. 3.1.7 Dev i ations from Perform a nce Speci fication 1 1

• The Sigr i s t PM CEMS sa mp les supe ri so kinetic a n d m a y n o t cont inuou sl y m e e t the requi re m e n t of plus o r m i nus 10% i s oki netic. The Sigrist system i s de sign ed to sample su pe riso kin e tic. This is normally about 1.2 to 1.5 times iso k in etic. Be cau s e of the Sigrist desi gn, Lilly cannot be sure that the system will always be with in ±10% of isoki n etics. Lillywill adhere to P S 11 and prov ide data in dicatin g that i s o k in e t ic sampli ng i s n o t n e ce ssary. Thi s data will consi s t o f parti culate size distrib u tion d a ta sho w ing the PM i s predomin ately small pa rticle s; thu s actin g a s a g a s. The particulate si ze distribution data will be collect ed duri n g the Comprehensi ve Performance Test.

• The calibration correl a tion function will plot Sigr ist values (m A or PLA) on the X-axi sand the referen c e m e thod a v e r

a g ein units of m g /scmo ntheY-ax is. PS1 1 indi cate s t h at the refe ren c e method value s for PM sh o u ld be in the same units a s the CEMS (the Sigrist uni ts are m g /Sigrist
m 3 ). Based upon th e exp e rien ce with t he Sigri s t at Lilly (PM CE MS demo n strations 1 an d 2), Lilly saw no affect upon the correlat ion by correcti ng the Method 5 units to units of the Si grist. The o p e ratin g pressu re i n sid e t he ph otometer is not well defi ned, ma kin g corre ction to this pre s sure a n unkno wn. B a se d u pon e x perien c e, Lil l y will sta nda rdize the RM data to mg/scm

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(68°F a nd 29. 92 in ch es). This i s also consi s tent with the way Lilly’ s Kin s ale, I rel and fa cility h a s establi s hed valid correl ations to the two Sigrist units operated at that facility.

• Lilly will use up to 20% of the co rrelation data (low range only) f o r zero point s if lo w PM dat a can not be p r odu ced. It is impo rtant to provid e PM emis sion data for the correl ation th at is spread a c ro ss the de sire d range of me asu rem ent. Often, data at the low end of the range is diffic u lt to obtain. Given this fact, us in g zero poi nts for the low data may be req u ired.

• Lilly will conduct a seven-day drift pri o r to the calibration correlati on. Thi s will be the li nea rity che c k proced ure d e scri bed in the Sigri s t operat ion m anual (che cks 5 value s b e tween 0

- 2 0 m A ), whi c h i s a m anual exerci se ea ch day f o r seven day s. T he crite r i a will defa u lt to the all o wa ble drift recomme nded by Sigri s t of 5% as oppo sed to 2% of the span indicated in PS11. Use of the Sigrist fo r co mplian c e to a PM stan da rd i s ne w in the US. In ou r exp e rie n ce, th e crit eri a spe c ified ab o v e are suffici ent to unde rstand the d r i ft of the unit a n d is a c ceptab le ba se d o n our PM CEMS de monst ration s

. Sigrist (the CEMS m anufa cture r) sup p o rts u s ing the above criteri a

.

• PS11 stipul ates im m ediate comp lia nce with Q A

/QC req uirem ents (Pro cedu re 2) u pon su cc es sf ull

y comp let i ng t h e co rr elation test outline d in PS11. Lill y will comply with Proposed Procedu re 2 after final correlation a n d statis tics h a ve been e s tablish ed an d the Sigrist PM CEMS is d e e m ed re ady fo r use a s a co mplian c e tool . Until then, Lilly will use anothe r mea n s (su r rogate op erating pa ra meters o r the multi-me tal s CEMS) to assure com p lia nce with th e PM stand ard if waste is b e ing burn ed in the solid -liqui d in cine rato r.

• Appendi x F, Procedure 2 doe s n o t di scu s s tim eto calib rate fo r t he Sigr ist. Lilly will put the Sigrist in a non-m e a s ure mode on ce per wee kfor up to one hour while co ntinuing to b u rn hazard o u s waste in orde r to perfo rm the calibration checks.

• Linearity drift will be checked once per week, not once per day. Lilly will follow PS11 on adjus ting the z e ro or upsc ale value when the dri ft, per the Procedure 2 equat ion, is greater than 5%. Sigrist recom m en ds che c king th e zero an d o r u p scale drift n o t more th an once pe r wee k

. Since th e ph otometer co mpen sate s fo r ele ctroni c d r ift duri ng ea ch sa mple, checkin g the zero and u p scal e drift daily is o f no value. NOTE: Th e weekly calib rati on d r ift che ck will che c k five values withi n the 0 – 100% range of the PM CE MS. This exceeds the zero and up scale drift rang e re quire ments.

• PS11 deem s the CEMS out of control if the dail y

, zero o r u

p scale d r ift exce eds 4% for five
con s e c utiv e days, or 8% once. Lilly w ill adhere to the 8% requi rement as de scrib ed in se ct ion 3.1.2.9.

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• While pe rform i ng the quarterl y ACA the PM CEMS m a y be off-line for greate r than one h our pe r day. The time off-line will not require use of ei ther the mul t i-metals CE MS or surrogate para m eters t o dem on strat e co mplia nce with the HWC MACT

. The qua rterl y audits will not requi re the u s e of param etric mode.

3.2 MULTI-METALS CEMS 3.2.1 Indicator o f Performan c e Lilly ha s volu ntarily cho s e n to use a m u lti-metal s CEMS to de m onstrate co ntinuou s co mpli ance with the HWC MACT metals emi ssion limits. Using a CEMS to monitor st ack ga s co ncentration s of metals i s a relatively ne w appli c ation a nd a s su ch, t he HWC MA CT d o e s n o t requi re fa ciliti e s to install a nd o perate a multi-metal s CEMS for HWC MA CT co mplian c e pu rposes.
The multi

- me tals CEMS is desi gne d to contin uou sly monitor the sta ck ga s concentratio n of mercu ry, arseni c, ch ro mium, cadmi u m, and lead to demonst rate compli an ce with the HWC MA CT m e tals emi ssi o n limits. Com p liance with HWC MACT metals em issi on standards will be demonstrated when the measured sta ck m e tals co nce n tration s are le ss than or eq ual to the appli c abl e stand ard s . Currently, Lilly must complywith the HWC MACT i n te rim sta nda rd s un der 40 CFR 63.12 03 (b). Compli a n ce with the interim HWC MACT mercu ry standa rd will be demo n stra te d wh e n the measu red sta ck con c entration s of mercuryis le ss than o r e qual to 45 u g /dscm co rre cted to 7% o xygen over a 12 -hou r rolli ng ave ragi ng perio d, upd ated ho urly. Complian c e wi th the lo w vo la tile metal s HW C MA CT interim e m is s i on sta nda rd will be de mo nstrate d whe n the mea s u red stack co nc e n tration s of arseni c a nd ch romi um and defa u lt levels of b e ry llium (see se ction 3.2.2.1 ) are le ss tha n or e qual to 97 ug/d s cm combine d , co rrecte d to 7% oxygen over a 12 -hou r rolli ng averagin g perio d, upd ated ho urly. Complian c e wit h the semi-vo l atile metals interim HWC MACT emi ssi on standard will be de monstrated when the measured stack concentrations o f lead an d cad m ium are le ss than o r e q u a l to 120 u g /d scm combi n ed, co rrecte d to 7% oxygen over a 12- hour rolling a v eragin g pe riod, update d h ourly. Lilly will com p ly with the HWC MA CT final re place m entmetal s emission sta ndards specified in Se ctio n 63.121 9(a ) n o late r tha n th e date requi red by Secti o n 120 6(a)(1)(ii) of the HW C MACT Final Repl acement Standards.

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3.2.2 Measure men t Techniq u e 3.2.2.1 Opera t ing Pr inciples
The m u lti-met a ls CEMS i s an X-ray based contin uou s e m ission m onitor (XACT) manufa ctu re d by Coo p e r Environme n tal Service s L L C (or eq uiva lent). The XACT extra cts a representa t iv e st ack ga s sa mple a n d
con c e n trate s the parti culat e and ga s p h a se m e tals o n a ch emicall y -rea ctive filter. The con c entration s of metals in the filter depo sits are mea s u red with a n e nergy -di s pe rsive X-ray fluo resce n ce (X RF) analyz e r

. Figures 3 a n d 4 sch ematically illustrate the majo r com pone nts of the XACT, whi c h inclu de:

1. A sample extraction system

2. A sample coll ection mo dul e
3. A metals anal ysis mod u le

4. A flow control module

5. A system co n t rol modul e
6. A PC interface

7. A Data Acqui sition System and Hi storia n
The XACT i s desi gne d to measure th e co ncentrati on of up to 20 elem ents, inclu d ing a n t imony (Sb), arseni c (As), ba rium (Ba ) , cad m ium (Cd), chro miu m (Cr), coba lt (Co), le ad (Pb ) , man g ane se (Mn ) , mercury (Hg), nickel (Ni ) , selenium (Se) silver (Ag), and thallium (T l).

Becau s e th e XACT is in capabl e of m easurin g be ry llium (Be), Lilly has develope d a def ault value for beryllium emi ssi on s. Fort unately, beryl lium is a sca rce eleme n t that is not u s ed in Lilly ph arma ce utical manufa cturi n g pro c e s se s. Lilly has examined a ll its manufa cturi ng processe s and a s so cia t ed pro c e ss
con s tru ction material s (e.g. alloy stee ls) a nd f oun d no indi cati on that beryl lium sh ould be present. Therefore, Li lly believes that a co nservatively calculated default value for beryllium i s techni cally defen sible.

Trace level s of beryllium are possibl e in raw materi als and ground water. Lil l y has sam p l ed its liquid
was t e and found only sporadic “hit s” of beryllium at levels c l ose to the detection limits

. Lilly h a s als o done
some limited sam p ling of plant tra s h, some of whi c h might b e p rocesse d in t he solid-li qui d inci nerator, and som e lo w-level s of b e ryllium we re rep o rte d . F o r the pu rpo s es of calcul ating a co nserv a tive default emission co n c entration, Lil l y has a s sum ed that all liq uid and soli d wa stes fe d to the solid -liqui d incin e rator

26 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

contai n Be at the maximu m levels dete cted: 1.0 ppm in the solid wa ste an d 0. 01ppm in the liquid wa stes. The d e fault e m issi on co ncentration was then cal c ulat ed u s ing the maximum wa ste fee d rate s fro m the CPT pla n , an d an LVM sy stem removal efficien cy (S RE ) of 98% (whi ch i s a fa ctor of two le ss th an th e desi gn SRE of 99% and a factor of 20 less th an th e SRE of 99. 9% obtaine d durin g the CPT of anothe r Lilly incin e rat o r with a virt ually identi c al scru bbe r sy st em). The re sulting val ue wa s ju st over 1 ug/d s cm. To be more conservative, Lilly has chosen 2 ug/dscm as a default value. Theref ore, a value of 2 ug/dscm will be added to the measured LVM emissi on before compari s on to t he emission standard limit. If the CPT data or any othe r eviden ce in di cate s the de fault value i s not app ro priate, it will be adj uste d accordingly. Copi es of the XACT Multi

- Metals CEM S Guida n ce Do cume nts, Perform a n c e Specification s , and Qu ality Assu ra nce Docum ents a re provided in A ppen dix B.

3.2.2.1.1 Sample Extraction System

The extractio n sy stem fo r the XACTis i dentical to th e extra ction system u s e d b ythe Sig r ist PM CEMS

. The sam p le system co nsi s ts of a sam p le p rob e a n d ri n g pi pe. The sam p le prob e size was sel e cte d b y the man u fact ure r to provide an inlet ga s velo city tha tis a p p roxim ately 1.0 to 1

. 5 times grea ter tha n the
norm a l sta c k gas velo city whe n sam p li ng at the pre s et(d esig n) rate of approximately 1 acm/min. This sup e r-isoki n e t ic ope rating conditio n is used to mi nimize parti culate mea s u rement erro r that can b e signifi cant at su b-i s o k ineti c conditio n s. The su pe r- iso k ineti cco ndition i s a n altern ative to continuo us monitori ng of the stack ga s velocity an d adjustm ent of the sampl i ng rate in order to mainta in iso k inetic conditions.

Stack ga se s are withd ra w n thro ugh a fi xed sa mple p robe, t ran sferred th rou gh a ring pipe wh ere th e ga s is
con d itioned b yheating to approxim ately 160 o C (3 20 o F) to vapori z e any water an d acid d roplets that may be pre s e n t in the gas strea m . A slipstre am of the sa mple ga s is e xtracted i s oki netically from the main ring pipe flow into a large di ame t er stilling cha m ber a nd through the flo wcontrol m odu le.

3.2.2.1.2 Sample Collection Mod u l e
About one liter pe r mi nute (lpm ) of the stack g a s i s i s o k ineti c ally dra w n from t he stillin g ch ambe r thro ug h
a sam p ling t ube, mixed with a redu ci ng ag ent, an d filtered th rough a filter t ape for a n a lysis. Afte r sampli ng fo r approximatel y 15 minute s , the dep osit spotis a d van c ed ab out two inch es wh ere the metal s con c e n tration s per sam p le depo sit are m easure d by XRF whil e the next sample i s bein g coll ected.

27 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

3.2.2.1.3 Metals Analys is Module

The m e tals a nalysi s m odu le of th e XA CT co nsi s ts of an ene rgy disp ersive m u lti-elem ent XRF a nalyze r. This multi

- ele m ent se nsor con s i s ts of a n X-ray t ube and a lithium -drifted silico n ene rgy dispersive X-ray detecto r, o r equivalent. The e nergy of the cha ra cteri stic X-ray s p rovide s th e qualitative i n formatio n to identify the el ements p re s ent in th e sa mple while th e inten s ity of ea ch analyt e line (X-ray) provid es the quantitative i n formatio n to determi ne th e mass of e a c h el ement p rese n t in the d epo sit. The mass of ea ch metal per sa mple dep osit spot is re p o rted to t he data acquisiti on system f o r su bsequ e n t stack gas
c o nc en tra t io n c a lcu l a t io ns

. 3.2.2.1.4 Flow Con t rol Module

The filtered g a s fro m the sampl e mod u l e is d rawn th rou gh the g a s conditio n i ng compo n e n t of the flow control mod u l e . These co mpone nts re move moistu re and corro s i v e gase s fro m the sta ck g a s allo win g for volume me asurem ents i n dry sta nda rd cubi c m e ters (dscm ) . Th e gas is then dra w n th rou g h a two-way sole noid valve, pressu re tran sdu c e r , and mass flo wco ntrolle r. Typically, the flowtravels dire ctly to a manual le ak che c k valve and vacuum pump but a fl owQA loo p is available for cross-che cki ng flows again s t a second ma ss flow meter. After flowi ng th rough the va cuum pum p, the sa mple g a s is returned to the stack.

3.2.2.1.5 System Control Module

The system control m odu le con s ists of programma b l e logi c co ntrol devi c e s , firmware, po wer su pplie s, relays, fuses, etc. to contro l the temperat ure s , flows a nd mechani cal aspe cts of t he system. The statu s of these comp o nents i s moni tored by software and firm ware asso ciat ed with the PC modul e.
3.2.2.1.6 PC Inter face Module

The PC mo dule contain s the overall system con t rol, XRF an alysis, an d calcul ation software. Thi s softwa re mon i tors the syst em o perating pa ramete rs and presents a va riety of st atus an d fl ags when a comp one nt is op eratin g outsid e of d e fined contro l rang es. It also perfo rm s qu antitative XRF metal s con c e n tration calcul ation s and co mbin e s the metals con c e n tration s per sampl e deposit with the volume sampl ed pe r sampl e dep o s it data to cal c ulate d ry sta ck g a s con c e n tration s in m i cro g rams p e r dscm.

3.2.2.1.7 Data Ac quisi ti on System and His t oria n
Metals con c e n tration s , in microgram s per d s cm, da ta status, q u a lity assura n c e d a ta, stat us flag s, an d system op era t ional status/a larm s are p a ssed to a d a t a acqui sition sy stem (DA S ). T he DAS pe rform s th e data cal c ul ations for com p l i ance. All data are saved i n a histori an.

28 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

3.2.2.2 Installation Loca t ion The XACT sample interface inlet will be installed at an accessible l o cati on downstream of the air pollution control equi p m ent wh ere t he metal s co nce n tration of the XACT-extracted sam p l e of stack ae rosol will be rep re s entativ e of the metals co ncentration (u g/m 3 ) in the effluent emitted from the sta ck. Sp ecifically, the monitor locati on will be at l east:

y 2 eq uivalent duct diamete rs do wn stre a m from the nearest co ntrol devi c e, p o i nt of pollution ge n e ration o r oth e r point at wh ich a cha nge in the polluta nt co ncentration o r emission rate may occur.

y 2 equivalent duct diam eters up st rea m from the effluent exhaust.
The equival e nt duct diame t er is calcul ated as p e r 40 CFR Pa rt 60, Appendix A, Method 1, Se ction 2.1.
A repre s e n tative sample of stack ga s wi ll be dra w n from the sta c k at an appro x imate rate o f one cubi c meter per m i nute, imme d i ately heate d to a tem p e rat ure a bove the d e w po int for m o st acid s, a nd maintaine d at that temp era t ure d u ri ng transport th ro u gh h eat-trace d an d in sulat ed stainle s s steel tu bing to an instru m ent she d hou sing the CE M S and other monitori ng in strum ents. 3.2.2.3 Installation The XACT CEMS will be i n stalle d pe r manufa cturer’ s re co mmen d a tions. O n ce the syste m i s in stalled, it will be com m issi oned for use. T h is exercise wi ll verify the syst em i s installed properly per the manufa cturer’ s sp ecifi c atio n. 3.2.2.4 Instrumen t Span The operating range of the XACT CEM S will be established during the CEMS certification period. Lilly wi ll verify that th e ope rating range (zero t o spa n ) will encompa ss the re sp on se of the XACT CEMS for all expected waste streams. T he HWC M A CT emi s sion limits, for the thre e metal classes, will fall within thi s measurement range. 3.2.2.5 System Start-up (Initial O p eratio n)
The initial sta rt-up of the X A CT CEMS will be at Co oper Environ m ental Services. The XACT CEMS wil l be op erated, sampli ng roo m air, to sha k edo wn the sy st em. O n ce the sy stem i s operating wit hout e rro rs, the XACTCE MS will un dergo a Fa cto ry Acce ptan ce Test to verifythat the s y s t em meets or excee d s the function al crit eria.

29 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

3.2.2.5.1 Factory Accepta nce Te st

The Fa ctory Acce ptan ce Test will b e e x ecuted at Coope r Enviro nmental Se rv ice s . The ob jective of this testing i s t o ensure the XACT CEMS meets or ex ceed s the fun ctional op erat ing crite r ia. Re sults of th e Facto ry Acce ptance Test will be do cum ented an d include the follo wing maj o r compon ents:

1. Manual Che c k List

2. Nation al Institute of Standa rds a nd Te ch nol ogy (NIST) Tra c e able T h in Film Cali b ration

3. XRF Energy Alignment Ch eck 4. Stability Check

5. Blank Bia s Check (ze ro dri ft check)

6. XRF Ins t rument Drift Ch e c k (up s cale d r i f tchec k)

7. Flow Rate Drift Check

8. MACT Metal Linea rity Che ck

9. MACT Metal Relative Acc u racyChec k 3.2.2.6 System Start-up (Field In stallation ) Once the XACT CEMS i s i n stalle d, the system will u ndergo an i n stallation q uali fication (IQ) to en su re th e system i s i n stalle d to manufa cturer’ s recomme n dation s an d that the system me ets all safety requi rem ents. Following succe ssful IQ, the system wi ll operate, sa mpling am bie n t air, for sev e ral wee ks. Once the XACT CEMS ha s ope rated fo r seve ral we e ks wi thout si gnifica nt issu es, Lilly will (1) Cali brat e (or che c k cali bration ) the X R F (2 ) Begin routine dailyQA/QC (3 ) B egin daily sy stem che c k for appropri a te operation. T he XACT CE MS will ope rate continu o u sly in this mode (at lea s t fou r wee k s) pri o r to th e perfo rman ce spe c ification test.

3.2.2.6.1 NIST Trace a b le Thin Film Calibratio n
Duri ng the ini t ial start-up of the XACT CEMS, the XR F will be calibrated using NI ST traceable thin fil m standards. T h is calibration will est abli s h calibration factors for each of the m e tals to be analyzed. The calib ration fa ctors are used to provid e ug/sp ot qu antitation for eac h metal analyzed. After the XACT CEMS is installed at Lilly, the calibration factors will be checked by using thin fi lm standards for up to five

30 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

different m e tals (at l e ast one m e tal for each of the t h ree metal s classes). The XACT CEM S XRF will be re-cali b rate d if the relative percent difference is great er than 10% by using the f o llowin g equ a t ion:

CA Acc u ra cy = 

### 100 *
REF REF CEMS 

### R R R

−

whe re:
C A = X- ray fluoresc e nc e calibra tion accura cy
R CE M S = the value of the st anda rd repo rted by the CEMS

R REF= the known valu e of the stand ard

3.2.2.6.2 Rou t ine Dail y QualityAssuranc e and QualityCon t rol

The XACTCEMS con d u cts auto m atic pre c isi on che c ks with eve r y sampl e run as well as d a ily upscal e and bla n k m easure m ents (ze ro a nd u p scale d r ift checks ). Th ese ch ecks en sure that the XRF data i s pre c ise; mini mal blan k bia s is o c curring , and significantinst rume n tdrift has not taken pla c e. Specifi c ally, the XACT CE MS will automatically (1) check energy alignm ent (2) check X R F stability (3) check zero drif t (4) c h eckupsc ale drift (5) checksample flow drift.

3.2.2.6.3 DailyS yste m Check Operation s wi ll manually pe rform a d a ily che c k of t he XACT CEMS. The daily ch eck will be d o cume nted. 3.2.2.7 Performanc e Specifica tion Test Once the XA CT CEMS installation and initial fiel d o peratio n hav e bee n a c hie v ed, a valida t ion of the XACT CEMS will be performed with ha zardous waste. Data collected during these tests wi ll provide an initial validati on of the XA CT CEMS. T h is validation will allow the use of the XA CT CEMS to demonstrate contin uou s complian c e with the HWC M A CT metal s e m issi on limits.

The performance specificat ion test w ill be performed to determine t he ac curacy, bias, prec i s ion, stability, and cy cle tim e of the XACT CEMS. The followin g che cks will be performed a s pa rt of the perfo rman ce specification test: Cy cle Time: The XACT CEMS will adhere to Performa nce Spe c ificatio n YY (Spe cificatio n s and Te st Procedu re s f o r X-ray Flu o re scen ce B a se d Multi-M e ta ls Contin u ous Emi s sio n Monito ring Systems at Stationary So urces prepa red by Coope r Environme n tal Services, L L C). Pe rform ance Spe c ification YY is

31 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

provide d in A ppen dix B. Pursuant to Section 1.2. 1 of Perform a nce Sp ecifi c a t ion YY, the CEMS mu st have a cy cle time that is l e ss tha n on e - third the per i od of th e ap p licabl e sta n d a rd. For this appli c ation, the cycle time will not exce ed fifteen minutes.

Stratific a tion Tes t : The s t ratific a tion tes t, des c ribed in s e ct ion 3. 1.2.6, for PM CEMS, will be a pplied to meet this re q u irem ent for the XACT CE MS. X-ray Flu o re scen ce Calib ration Ch eck: The XA CT CEMS will a dhere to Pe rforma nce Spe c ificatio n YY whe n cond ucting the X-rayFluoresce nce Cali bratio n Che c k. Usin g NIST tra c e able stand ard s , the XACT

XRF is ch alle nged three times for ea ch metal measured. The error is cal c ulate d according to the followin g equatio n:

CA = 

### 100 *
REF REF CEMS 

### R R R

−

whe re:
C A = X- ray fluoresc e nc e calibra tion accura cy
R CE M S = the value of the st anda rd repo rted by the CEMS (ug)

R REF= the known valu e of the stand ard (ug ) The average error of the three m e a s urements fo r e a ch metal m u st be le ss t han 10% of the cali bratio n stand ard’ s va lue for ea ch metal. Stability: The 7-Day Cali bration Drift Te st: The XACTCEMS will a dhere to Perf orma nce Spe c ificatio n YY when conducting the 7-day Calibration Drift Test. The stability test will be performed prior t o the accuracy testing. The CEMS must meet the following sp eci fication s for each of the seven con s e c utive days, without any a djustme nts o r calibration s made to the CEMS:

• z e ro drift: ≤ 2 0 % (of the emissi on limit value) dete r m i ned by the following equati on:



## 100 * Ci Ri Ri ZDi REF CEMS 

## − =

where: ZDi = the zero drift of the i th element (%)

32 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

Ri CE M S = the measured CE MS respon se to the zero standa rd for th e i th element
Ri REF= the referen c e value of the i th ele m ent on the zero sta nda rd Ci = the emi s sion limit of the i th element. Lilly will con s i der the emi ssion limit of the individual m e tals (Ci) to b e equal to the HWC MACT limit for the metal cl ass. For exampl e, the emi s si on limit fo r l ead will b e consi dered to be 1 20 u g /d scm fo r the purp o ses of d e termini ng ze ro drift for the XACT.

• upsc a le drift: ≤ 15% (of the refere nce value) dete r min ed by the followin g equati on:



### 100 *
REF REF CEMS 

### Ri Ri Ri UDi − =

where:
UDi = the up scale d r ift of the i th element (%)
Ri CE M S = the mea s ured CEMS re sp o n se to th e u p scale stan d a rd fo r the i th element.
Ri REF= the referen c e value of the i th ele m ent on the u p scale stand ard

• volume of flow drift: ≤ 20% (of i n strum ent spa n ) d e termi n e d by the foll owin g equatio n:



### 100 * F

S V V VD m CEMSR 

### − =

where:
VD = Volume drift (%)
V CE M S R= Sample ga s volume or flo wmeasured bythe CEMS volume che c k measurement device.
V m = Sample gas volum e o r flow re porte d by the multi-metal s CEM S FS = Full scal e value of the CEMS volume or flow me a s ureme n t

33 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

CEMS Acc u ra cy : The XACT CEMS wi ll adhere to Perform a n c e Specification YY when det ermini ng the C E M S a c c u ra cy

. T h e a c c u ra cyo f t h e XA C TC E M S i s d e termi n e d u s ing one o f the followi n g four optio ns and pe rform a nce crite r ia:

• Option A: Linearity test of the entire CE MS

− slop e: 0.85-1

. 15

− r ≥ 0.90

− intercept < 20 % of emissio n limit for each metal

• Option B: L i nearity te st of the XRF and sam p lin g mod u le s separately fro m the sampl e interf ace. Thi s opt ion will al so include a Transport Efficiency Test.

− slop e: 0.85-1

. 15

− r ≥ 0.90

− intercept < 20 % of emissio n limit for each metal

− Percent tran sport ≥ 90 % o r ≤ 110%

• Option C: Re lative bias of the entire CE MS

− Relative % Bias ≤ 1 5 % for each metal

− % RSD ≤ 10 % for each m e tal

− r ≥ 0.90 for th e metal use d to demon strat e the 3-fold chang e

• Option D: Relative bia s of the XRF and sa mpli ng modul es sep a rately from the sampl e interf ace. Thi s opt ion will al so include a Transport E fficiency Test.

− Relative % Bias ≤ 1 5 % for each metal

− % RSD ≤ 10 % for each m e tal

− r ≥ 0.90 for th e metal use d to demon strat e the 3-fold chang e

− Percent tran sport ≥ 90 % o r ≤ 110%

3.2.2.8 Rou t ine Ope ration of the Multi-Me tals CEMS The q uality a s sura nce req u irem ents will adhe re to Proce dure Z: Q uality Assura nce Re quire ments fo r Xray Fluo re scence Based Multi-Metal s Contin uou s Em issi on Mo nitoring Sy stems at Stati onary So urce s prep ared by Coo per Environmental Se rvices, LL C. Procedu re Z i s located in Appen dix B.

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3.2.2.8.1 DailyQualityAssura nce Chec ks

Each d a y, operatio ns will manually p e rform a dai ly check of the XACT CEMS. Resu lts will be documente d . The XACT CEMS cond u cts automati cpre c i s ion ch ecks with every sample run a s well as daily upscale and blank measurem ents (zero drift, upscale drift, and volume (flow) checks). These chec ks ensure th at the XRF data is preci s e; mi nimal bla n k b i as i s occu rri ng, and signifi cant in stru m ent drift ha s not taken pl ace. Specifi c ally, the XACT CEMS will automatically (1) check en ergy alignment (2) check XRF stability (3) check zero drift (4) check upscale drift (5) check sample flow drift. For ea ch daily check, the percent d r ift cannot ex cee d :

• z e ro drift: 20% in terms of the emiss i on limit

• upsc a le drift: 15% in terms of the bas eline value for eac h metal

• volume flow: 20% in terms of ins t rument s p an 3.2.2.8.2 Quar terly Audit

3.2.2.8.2.1 First Qua rte r l yAudit a fter Performanc e Specifica tion Test The first qu a rterly audit af ter the perfo rmance sp ecificat ion te st will con s ist of the CEMS accuracy test descri bed in Section 3.2.2. 7.

XRF calib rati on fa ctors wil l also b e che c ked by pe rf o r ming an X-ray Fluo re sce n ce Calibration Audit. Fo r each el ement mea s u red, t he p e rcent di fference m u st not ex cee d 10%. Ea ch quarte r, a sa mple volu me (flow) audit will be pe rformed. T he average of three volume s, taken at diffe rent mea s u re m ent cycle s , must n o t exceed 1 0 % of the refe ren c e value. T h e entire XA CTCEMS an d transpo rt sy stem will b e examined f o r pro b lem s , such as pa rticulate build up. App rop riate preventa t ive mainten ance will be perfo rmed o n the CEMS. 3.2.2.8.2.2 Subsequ e nt Quar terly Audits
Each quarter the XRF cali bration factors will be chec ked by performing an X-ray Fluorescence Calibration Audit. For e a ch elem ent measured, th e pe rcent dif f eren ce must not exceed 10%. Ea ch qua rter, a sampl e volu me (flo w) a udit will be perfo rmed. The ave ra g e of three vo lumes, ta ke n at different measurement cycle s , must not exce e d 1 0 % of the referen c e valu e.
The entire XA CT CEMS an d transport sy stem will be e x am ined for p roble m s, su ch as parti cula te build up. Appro p riate p reventative m a intena nce wi ll be perfo rme d on the CEM S

.

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3.2.2.8.3 Annu al Audi t Annually, in a ddition to the quarte rly che c ks, the XAC T CEMS will be che c ked f o r a c curacy (Perform an ce Specification YY). The accuracy will be determined usi ng one of t he four options and respectiv e perfo rman ce crite r ia:

• Option A: Linearity test of the entire CE MS

− slop e: 0.85-1

. 15

− r ≥ 0.90

− intercept < 20 % of emissio n limit for each metal

• Option B: L i nearity te st of the XRF and sam p lin g mod u le s separately fro m the sampl e interf ace. Thi s opt ion will al so include a Transport Efficiency Test.

− slop e: 0.85-1

. 15

− r ≥ 0.90

− intercept < 20 % of emissio n limit for each metal

− Percent tran sport ≥ 90 % o r ≤ 110%

• Option C: Re lative bias of the entire CE MS

− Relative % Bias ≤ 1 5 % for each metal

− % RSD ≤ 10 % for each m e tal

− r ≥ 0.90 for th e metal use d to demon strat e the 3-fold chang e

• Option D: Relative bia s of the XRF and sa mpli ng modul es sep a rately from the sampl e interf ace. Thi s opt ion will al so include a Transport E fficiency Test.

− Relative % Bias ≤ 1 5 % for each metal

− % RSD ≤ 10 % for each m e tal

− r ≥ 0.90 for th e metal use d to demon strat e the 3-fold chang e

− Percent tran sport ≥ 90 % o r ≤ 110%

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3.2.2.9 Compon ent Replac emen t Duri ng normal operation of the XACT CEMS, specific components w ill need to be replaced. The XACT CEMS standard operating procedures will address t he criteria to be me t upon replacement of significant comp one nts. 3.2.2.10 Out of Control The out of co ntrol pe riod will begi n immediately after t he la st test run o r che ck of an un succe ssful ze ro drift, upsc a le drift, s a mple flow drift, or uns ucc e s s f ul ac curacyaudit. The out of c ontrol period end s immediately after the l a st test ru n o r check of t he subsequ ent su ccessful audi t or d r ift check, when t h e PM CEMS is use d as a ba ck-up o r wh e n the incine ra tor enters pa rametri cmode . When the incin e rato r is operating in p a ram e tric m o de, the XACTCE MS will not be deeme d out of control

.

3.2.3 Use of th e XACT Multi Metals CEM S to Demon s tra t e Comp liance w i th the HWC M ACT Metals Stan dards Lilly may begin usi ng the XACT CEM S to demonstra te continuous com p liance with the HWC MA CT metals emi s si on stan dards only after the followin g is a c hieve d :

• A successful Perform a nce Specifi c ati on Test is perform ed fo ll owing EPA’s approval of this Alternative Monitorin g Petition.

• A modificatio n to the Title V pe rmit i s a pproved t hat in corpora t es the re qui reme nts of the approved Alternative Mo ni toring Petition

. Followi ng co mpletion of th e above, o n -going quality as suran c e wil l be pe rforme d on the XA CT CEMS a s spe c ified in S e ction 3.2.2.8 of this docu m ent.

3.2.4 Monitoring F requen c y an d Av eraging Time

The m u lti-me tals CEMS wi ll monito r an d record con c ent ration val ues (μ g/dscm ) of mercu ry, low volatile metals (arsenic and chromi um; a default value will be incorporated for beryllium ) , and semivol a tile metal s (lead a nd cad m ium) at lea s t once every 15 minute s

.

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The metal s concentratio n s will be co rrected to 7% oxygen by the followin g equati on:

2 

### 21 7

21 * O M M uncorr corr



### − − =

whe re: M corr = Mercury, semivolatile metals, or l o w volatile m e tals con c ent ration corre cted to 7% oxygen (μg/dscm ) M uncorr = Mercury, semivolatile metals, or low volat ile metals stack gas con c e n tration (μg/d s cm) O 2 = Oxygen stack ga s pe rcent (vol % dry) An hourly blo ck ave ra ge will be calcul ated from th e four 15 mi nute mea s u rements duri n g the hou r a s sho w n in the followin g equ ation:



### 4 4

1 

# ∑

= 

### = i 

### Ci HBA whe re:

HBA = Ho urly block avera g e value (ug/d s cm) Ci = a fifteen minute ob se rvation from the CEMS anal yzer (ug/d s cm)

The e s tabli s h ed be ryllium default value will be ad ded to the fifteen-minute ch ro mium and a rseni c CEMS observation s to calculate t he LVM hou rl y block ave ra ge.
Valid results must be avail able fo r at le ast th ree of t he 1 5 -mi nute cycl es of op eration to cal c ulate a one hour bl ock av erag e.
Twelve -ho u r rolling avera g e s will be cal c ulate d ba se d on the ave rage of the twelve mo st rece nt hou rly block averag es a s sh own in the followin g equatio n:



## 12 12

1 

# ∑

= 

## = i 

## HBA THRA

Whe re: THRA = Twel ve hour rollin g averag e value (ug/d s cm)
HBA = Ho urly block avera g e value (ug/d s cm)

38 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

The twelve-hour rolling av erage will be updated every hour when a new hou rly block average i s cal c ulate d

. 3.2.5 Block Av erage Calculati ons du ring Multi-Me tals CEMS Daily Chec ks and Ongoing Qu ality Assu ranc e Checks

The XA CT CEMS will be off line u p to one hou r ea ch dayt o p e rf orm th e daily quality a s su rance che c ks. Block average calcul ations will be frozen during the daily upscal e and zero checks. Lilly will continue to burn hazardous waste duri ng the daily quality assurance checks. Block average cal c ulatio ns will resume once the che c ks a re pe rformed. The twelve-ho u r ro lli ng blo ck average calculatio ns will re sum e by addin g the first valid hour bl ock av erag e after th e drift ch e c k to the previou s 11-hou r blo ck ave rag e value s

. In additio n , bl ock ave ra ge cal c ulatio ns will b e frozen du ring the q uarte rly an d annu al a udits. Rolling blo c k averag e cal c ulation s will resum e on ce t hese quality assuran c e ch ecks a re com p leted. 3.2.6 Multi-Metals CEMS Backup

In the event t he m u lti-metals CEMS i s not operating, Lilly will have the option to use the PM CEMS as a backu p to the multi-metals CEMS unde r the followin g con d ition s :
1. Re sults obtai ned from p a rallel op eratio n of the tw o CEMS will b e u s ed to de velop a te ch nica l justificatio n o f how the PM CEMS pro v ides re ason able a s sura n c e of co mplia nce with the HWC MACT metal s emissi on sta ndard.

2. Whe n the mu lti-metals CEMS is not op erati ng a nd the PM CEM S begins u s e as a ba ckup , Lilly will use its b e st efforts to avoid introd ucin g ne w waste st ream s (i.e. those that have not been histori c ally b u rne d whil e the two CE MS were in parallel o p e ration ) from the six “in-feed” conveyo rs to the final “merge” conveyo r that leads to the kiln fee d chute.

In ord e r to allow CEMS mode to e s tabli s h wa st e stre am s that are not “ne w ” du rin g its initial impleme n tation pe riod, th e above re striction s on use of the PM CEMS se rvin g as a ba cku p for the m u ltimetals CEM S will apply o n ly after a su fficient time p e riod ha s ela p se d (n ot to excee d 6 mo nths fro m the first CEMS m ode o peratio n) for Lilly to gain exp e rie n c e while pro c essing a vari ety of existing soli d waste strea m s. Fin a lly, Lilly will attempt to m a intain nomi n ally stable or histori c allylowe r feed rat e s of wa ste while th e ba ckup i s b e ing use d , and wil l limit the use of the PM CEMS as a b a ck up for th e multi-metal s CEMS to 14 con s e c utive d a ys per e p iso de. Lilly will use its best efforts to minimize the time t hat t he PM CEMS acts as a backup to the X A CT CEMS. To facilitate its efforts, Lillywill ke ep sp are p a rts in stock and will maintain a se rvice relation ship with the XACT CEMS manufa cture r, or othe r q ualified con s ul tants. If bot h the PM CEMS and th e multi-metal s

39 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

CEMS are n o t in use, Lill y will monito r ope rating p a ramete r limits defined i n S e ction 120 9 of the HWC MACT (i.e. p a ram e tric ope ration ). Detail s of the spe c i fic ope rating l i mits are provided in the Notification o f Compli an ce ( N O C ). Lilly will incorporate delay s when t ran siti oning from th e CEMS mod e of ope ratio n to the para m etric m ode of ope ratio n . Spe c ificall y , once the prim ary mu lti-metals CE MS and the ba ckup PM CEMS are unavailabl e, the control system will aut omatically switch to the p a ram e tric mo de of o p e rati on. Rolling averages, rel a ted to the Air Pollution Control Syst em (APCS ) , will not start un til the sy stem has been unde r the parametri c mode of operation for 10 minute s . This 10-minute time peri od will allo w Lilly time to make any adjustments to the APCS to brin g the sy st em to withi n the re spe ct i ve ope rating paramete r limits. In addition, up to four hou rs will be allowed b e fore re-starti ng co nstitue n tfeed rate rol ling avera ge operating p a rameter limits in ord e r to clea r the soli d feed conve y or syste m . (Note th at, in a simila r fashion to t h e “backup” sc enario descri bed above, Lill y will use its best effo rts to avoid introducing “new”
wa ste strea m s from the si x “in-fe ed” co nveyors to th e final “me rg e ” conveyo r t hat lea d s to t he kiln fe ed chute duri ng this four hou r perio d. Ho wever, d u rin g initial CEMS mode o peration pe riod s t here will be pra ctical limit ations to this criteri on be cause fe w wa ste stream s will have be e n burned.) F eed rates will be maintain e d nominally stable or hi sto r ically lo we r than when o p e rating in CE MS mode. If the CEMS mode of op eration is sti ll not availa ble after fou r ho urs, the tran sition to parametri c mode will b e compl e ted an d only wa ste with kno w n compo s ition wi ll be proce ssed in the i n ci nerato r so th at co nstitue n t feed rate op e rating pa ram e ter limits ca n be com pute d

.

3.3 HYD R O G EN CHL ORI D E ( HCl) CEMS 3.3.1 Indicator o f Performan c e
The HCl CEMS is de sign ed to continu ously monito r t he sta c k ga s HCl con c en tration. Comp liance with th e HCl/ C l 2 HWC MACT emission standard will be dem onstrate d when the measured st ack concentration of H C l co mb ined w i th th e de fa u l t ch lo r i ne con c ent rati on i s le ss th an o r e qual to the appli c a b le stand ard. Cur re n tly , Lillymust compl ywith the HCl/Cl 2 HWC MACT interi m standa rd o f 21 ppmvd, corre cted to 7 percent oxygen, spe c ified unde r Se ct io n 63.1 203 (b ) of the HWC MACT. Lilly will comply with the HWC MACT final HCl/ C l 2 standard spe c ified in Section 6 3 .1219 (a ) no later than th e date re quired by Sectio n 1206 (a )(1 )(ii ) of the HWC MACT final repla c em ent st and ard s

. The ave ragin g time is ov er a 1 2 -h ou r perio d, updat ed every min u te.

40 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

3.3.2 Measure men t Techniq u e 3.3.2.1 Opera t ing Pr inciples The HCl CE MS is an Eco c hem M u lti-Compon ent Infrared Analyzer (M C3 ), or equivalent, m anufa cture d b y Ecochem An alytics. The MC3 mo nitors the sta c k g a s sample fo r HCl co ncen trations. Th e MC3 al so measures sta c k ga s con c e n tration s of carbo n m onoxi de (CO ) , oxy gen (O 2 ), ca rbon dioxide (CO 2 ), sulfu r dioxide (SO 2 ) and nitro g e n oxide s (NO x ). In addit i on, the M C 3 mea s u re s th e moi s ture content of th e stack ga s. Figure s 3 an d 5 sch ematicall yillustrate the major comp onents of the MC3, whi c h i n clu de:

1. Sample Extra ction System

2. Pressu re Reg u lation Mod u l e
3. Ecochem Mul t i-Com pon ent Infrared Anal yzer 4. System Cont roller

5. Data Acq u isiti on System an d Histo r ian

3.3.2.1.1 Sample Extraction System

The sa mple e xtraction syst em con s i s ts o f two elements; a sam p le p robe a nd a h eated umbili cal line.

The he ated sampl e prob e is M&C P rodu cts Samp le Drift Pro b e , or eq uivalent, manufa ctured by M& C Produ cts. To provide accurate m e a s urement of HCl , the sampl e extraction system, sam p l e line an d prob e, p rovid es a hot, we t sampl e to t he M C 3; eli m inating th e scrub b ing of water-solu b le com pou nd s su ch as HCl and S O 2 . The M&C Products S a mple Drift Probe provides the ca pability of sam p ling a water saturated ga s stre am, redu cing th e affe ct of wate r dro p le ts at th e sample point (first step in eli m inating th e water sol uble aero s ol ). Op eration of the sampl e p ro b e (tempe ratu re , sample, purge, cali bratio n mode s) i s controlled by a Programma ble Logi c Con t roller (P LC); locate d in the MC3 sample cabin e t.

The sam p le umbilical line has the function of (1) prov id ing cali brati on gas to the probe for dai ly zero and upscal e span che c ks (2 ) p roviding cali b ration gas to the probe fo r linearity au dits (3) p rovidi n g a hot, wet sampl e to t he M C 3 an alyzer. Th e sam p le um bilical is de signed to o p e rate at tem peratu re s of approximatel y 180 °C; whi c h is imp e rative for hot, we t sampling of HCl, moi s ture , and SO 2 .

41 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

3.3.2.1.2 Pressure Re gulation Mo dule
The pressu re regulatio n m odule i s de si gned to remo ve both free particulate s a nd wate r-sol u ble aerosols from the ga s strea m p r io r t o an alysi s bythe M C 3 an al yzers. Th e syste m al so provide s a sa mple gas to the MC3 at a con s tant pressure. Contro l of this syste m resi de s wit h the PLC in the MC3 cabi net. The pressu re regulatio n module is d e si gned to maint a in a temperature of at least 180 Celsi u s, minimi zin g scrub b ing of HCl, moi s ture , and SO 2 . 3.3.2.1.3 Ecochem M u lti-Comp on ent Infrared Analyz er
The sa mple extraction system delive rs a hot, wet sampl e to the Ecochem Multi-Compo nent infra re d Analyze r . Th e MC3 qua ntitates sta c k g a s con c e n trat ions of CO, O 2 , CO 2 , SO 2, NO x , H 2 O a nd HCl. HCl analysi s o c cu rs by u s ing si ngle be am du al wavele ngt h nondi sp ersi ve infrare d sp ectro s copy. T he HCl ga s absorb s infra red radi ation at a sp ecifi cwavelen g th , which de pe nds on its m o lecular stru cture. T h e degree of ab sorption i s p roportio nal to the con c entra tion of the ta rget ga s. Fin a l value s a re rep o rted by the PLC in pp mv, dry units.

Be c a us e the H C l /C l 2 HWC MACT emi ssi on limit is based on co mbine d sta ck emissio n s of hydrog en chlo ride and chlo rine g a s and th e MC3 o n ly meas ure s hyd rogen chlo rid e , Lilly has develop ed a
con s e rvative default value for the chl o ri ne con c ent ra tion. Fortu n a t ely the amo unt of chlo rin e present in st ac k ga s fro m inci nerat ors simila r t o t he solid -liqui d in cine rator is typica lly very low, parti cularly if they burn aqueous wastes an d have wet air poll u tion control sy stems. Lilly has tested its i n cinerator in Mayague z, Puerto Ri co th at is equip p e d with the sa me air poll u tion co ntrol sy stem and b u r ns simila r liquid waste s as the soli d-liquid in cine rator. The re sults sho w ed chlo rine l e vel s mu ch le ss than 1 p p m (NOTE: Duri ng this te stin g, the bromi n e/chlo rine an d sulfu r /chl ori ne wa ste co mpositio n rati os were belo w levels that E PA believes coul d resulti n a negative measurement bias. ) To be conservati ve, Lilly will use 1 ppm as the default value for chlorine. Therefore, a value of 1 ppm will be add ed to the measured value of HCl b e fore comp ari s on t o the HWC MACT emi s si on sta nda rd. If the CPT data or a n y other evid en ce indicates the default value is not appropr iate, it will be adjusted accordingly. 3.3.2.1.4 System Controller A PLC provid es control of t he MC3, sa m p le probe, p ressure regul a t ion modul e, and the sam p le interfa c e. The PLC pro v ides on e mi nute average d data, and v a lidity status, for each an a l yte measu re d as well a s flow. T h e calibration an d li nearity pro c e dure s are al so controlled b ythe PL C. A ll data, and st atus fla g s, are sent to a data acqui sition syste m for data formatting and compl i ance determi nation.

42 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

3.3.2.1.5 Data Ac quisi ti on System and His t oria n
HCl concentrations i n part per milli on corrected for moisture, dat a status , qual ity assuranc e data, status flags, and sy stem op erati onal statu s /al a rm s are pa ssed to a d a ta acqui sition system (DAS ) via modbu s comm uni cati on from the MC3 PL C. T he DAS perf o rm s the dat a cal c ul ation s for co mplia nce. All data , both syste m status a nd HCl co ncent rati ons, are save d in an histo r i an. 3.3.2.2 Installation Loca t ion
The HCl CE MS extracts its sample from the flue gas s t re am in the stack. S e ction 3.1.1 o f Perform a n c e Specification 2 p rovide s g u idan ce re ga rding ap propriate monito r l o catio n . T h is mea s u reme n t location i s at least:

y 2 eq uivalent duct diamete rs do wn stre a m from the nearest co ntrol devi c e, p o i nt of pollution ge n e ration o r oth e r point at wh ich a cha nge in the polluta nt co ncentration o r emission rate may occur.

y 0.5 equivale n tduct diamet ers u p st ream from the effluent exhau st. 3.3.2.3 Installation
The M C 3 sy stem will be in stalled p e r m anufa cture r’ s re comme ndat ions. On ce t he sy stem is installe d, it will be com m issi oned for use. T h is exercise wi ll verify the syst em i s installed properly per the manufa cturer’ s sp ecifi c atio n. 3.3.2.4 Instrumen t Span
The spa n for the HCl CEM S is 1 00 p p m v . An instru ment span which covers t he expe cted pea k level s will help to en su re that the 12 -hou r rollin g averag e valu e corre ctly accounts for the sho rt pe ri ods of mo re
con c e n trated emissio n s. Additionally, 100 ppmv HCl calib ration ga s i s a n HCl bl endin g concentratio n much prefe r red by vendo rs. Du e to the high rea ctivi ty of HCl, it is difficult to ensu re the co ntinuin g accuracy of the cali bratio n gas at lower con c e n tration s

. 3.3.2.5 System Start-up (Initial O p eratio n)
3.3.2.5.1 Factory Accepta nce Te st The Factory Acceptan ce Test will be executed at Ecochem Anal ytics. The objective of this testing is to ensure th e Eco c hem CEM S meets o r e x ceed s the functi o nal op e rating crite r ia . Results of the Facto ry Acce ptan ce T e st will be d o c ume n ted an d inclu de the followin g maj o r co mpo nents:
1. Sample Extra ction System

43 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

2. Pressu re Reg u lation Mod u l e 3. System Confi guratio n
4. Ecochem Mul t i-Com pon ent Infrared Anal yzer 5. System Cont roller
3.3.2.6 System Start-up (Field In stallation ) Once the E c och e m CEM S is in stalled, the syste m w ill un dergo an in stallatio n qualifi c atio n (IQ) to en sure the syste m is installe d pe r the m anufa ct u re r re co mm endatio ns. F o llowin g successful IQ of t he MC3, the system will operate sam p li ng ambient ai r for several week s. Duri ng this time, MC 3 operational issues will be a ddresse d

. On ce the M C 3 syste m h a s o perated fo r several wee k s with out sig n ificant i s sue s , daily QA pro c ed ures will begin (zero and u p scal e drift ch ecks, al arm m onito ring, an d co mpletion of a daily syste m check sheet). The MC3 sy stem will operate in this mode unt il the incinerator is re ady to treat waste. 3.3.2.7 Performan c e Specificatio n Test
The ce rtificati on of the Ecoch e m CEM S for HCl wi l l follow th e HCl CEMS Perform a n c e Specifi c atio n (attach ed a s appe ndix C). Spe c ifically, t he follo win g w ill b e eith er tested or do cu mented: 1) data re corder
s c ale, 2) daily c a libration drift, 3) ins t allation and measurement loc a tion, 4) c a libration drift tes t, 5) calib ration error te st, 6) system re spo n se time, 7) st rati fication te st, and, 8) a c curacy dete r min a tion. Up on
su ccessful completion/ve rification of the a bove te sts, the Eco c hem CEMS ca n b e used to sh o w contin uou s complian c e th e HWC MACT HCl/Cl 2 emissi on sta nda rd. Each test is de scribe d b e low:

3.3.2.7.1 Data Re cord er Scale The range of the data recorder a nd the measurement range of the HCl CEMS will be docum e nted. T he daily zero and upsc ale calibration checks will fall within th is range. The HCl CEM S will have a measurement range of 0

- 1 00 ppm HCl.

3.3.2.7.2 DailyCalibration Drift

The zero and upscal e drift will be checked once dail y. Zero gas (0 ppm HCl ) will be used f o r the zero, and a pproximately 50 -1 00 ppmv HCl for the up scale. Th e calibratio n drif t limit will be 5% of the instru ment span, or ± 5 ppmv. Zero and high -lev el calib ration drifts shall b e adjuste d, at a minimum, whe never the 24 -hou r ze ro drift ex cee d s the limits of the calibratio n d r ift sp ecifi c ation of ±5 ppmv. Th e amount of exce ss ze ro an d high-l e vel d r ift measu red atthe 24-ho u r interval che c ks will b e re corded.

3.3.2.7.3 Installation a nd Measu re ment Loc ati on

44 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

The HCl CE MS extracts its sample from the flue gas s t re am in the stack. S e ction 8.1.2 o f Perform a n c e Specification 2 p rovide s g u idan ce re ga rding ap propriate monito r l o catio n . T h is mea s u reme n t location i s at least:

y 2 eq uivalent duct diamete rs do wn stre a m from the nearest co ntrol devi c e, p o i nt of pollution ge n e ration o r oth e r point at wh ich a cha nge in the polluta nt co ncentration o r emission rate may occur.

y 0.5 equivale n tduct diamet ers u p st ream from the effluent exhau st.

3.3.2.7.4 Se v e n Da y C a libration Dr ift Tes t The procedure outlined in the HCl CE MS Performance Specification (attached as appendi x C) will be
use d for this spe c ification. The specifi c ation p rop osed for the calibration drift is 5 ppmv, which is 5% of the ins t rument s p an. This is c o ns is tent with the ex pe cted drift for HCl monito rin g u s ing Fou r i e r T ran sfo r m Infrare d Spe ctro s copy (F TIR) fou nd i n Performan c e Spe c ification 15 (PS15 ) , Section 1 0

. 1. It is also consi s tent with Lilly’s expe rience with a similar monito ring sy stem in Ireland, an d with others ’ experience in the U.S. T he highe r cali bration d r ift fo r HCl monit o ring a s co m pare d to that for NO xor SO 2 monitorin g appe ars to be a re sult of the rea ctivity of HCl. The chem i c al’ s hi gh rea ctivity cau s e s it to “stick” to the calib ration cy linder wall s, and to be ext racte d un eve n ly from the cylinde r du rin g t he cali brati on process. Thus, it i s th e calibration gas itself th a tis cau s in g varian ce i n t he calib ration drift results, as well a s whateve r dri ft the an alyzer exp e rie n c e s . It is a l so wo rth n o ting that some other perfo rman ce spe c ification s , such a s PS 4 (for CO) d o allow a calib ration drift of up to 5% of span.

3.3.2.7.5 Calibra tion Error Test

The Calibrati on Error test will fo llow the procedures i n the HCl CE MS P e rform a nce Specification (attach ed a s appe ndix C). The Ecoch e m CEMS wi ll be challe n ged thre e no n-con s e c utive times with zero, mid

- lev e l, and hi gh -l evel ce rtified gases. T he cylinder g a ses will not be E PA Protocol 1 ga se s. The calib ration g a s e s will be inj e cted into the sample syste m as clo s e to the samplin g probe o u tlet as practi cal and will pa ss throug h all CEMS comp on ents u s e d d u ring no rmal m onitorin g . Th e differe nce b e twee n the instrument response and t he reference value (certified gas) will be cal c ulated af ter each i njection and the resulting thre e differen c e s will be averaged to dete r mine the CE at each measurement point. The calib ration e r ror for ea ch of the three levels will n o t excee d 5% of span.

3.3.2.7.6 System Res ponse Time

45 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

Usi ng the Resp on se Tim e Test p ro c e dure in th e HCl CEMS Perform a n c e S pecificatio n (attached as appe ndix C), Lilly will det ermin e a me an u p scale a nd me an do wn scale syst em respon se time for the Ecochem (ba s ed u pon CO). The sl ower of the upsca le an d do wn scale mea n respon se ti mes will b e considered the system res ponse time. The system resp onse time will meet the requirem ents specified in perfo rman ce spe c ification (i.e. 2 minutes).

3.3.2.7.7 Interfe renc e Respo n se Determina t ion The affect of other analyt es up on the measurement of HCl will be do cume nted (Ecochem calibratio n table).

3.3.2.7.8 Stratifi cation Test

The stratifica tion of the g a s stream wil l be determi n ed u s in g g u i dan ce i n the HCl CEMS Perform a n c e Specification (attach ed as appe ndix C). Du e to the lo w con c e n trati on of HCl ex pecte d in th e gas stream, stratification will be docum ented i n term s of velocity

. A minim u m of 12 sampling points will be used, wit h 6 sampli ng p o ints alo ng e a ch of the two traverse s.
The value at each t raverse poi nt is t hen comp are d to the ave rage val ue for all sampli ng points to determi ne the percent stratification u s ing the followin g equatio n:


### % 100 * ave i 

### C C S

− =

whe re: S = percent stratification

C i = velocity at sampling point i

C av e= average velocity at all samplin g po ints. If the percen tstratificatio n is le ss th an or e qual to 10 pe rcent f o r any traverse p o int, the duct i s not
con s id ere d st ratified at that location

3.3.2.7.9 Accu racy Determinatio n
The a c cura cy of the HCl CEMS will be determined by p e rformi ng eit her a Relati ve Accu ra cy determi nation , or by dynamic spi k in g.
3.3.2.7.9.1 Relativ e Acc u rac y Deter m ination

46 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

The procedure outlined in the HCl CE MS Performance Specification (attached as appendi x C) will be
use d as a gu ide for this specifi c ation. The RA of th e CEMS mu st not be gre a ter than 2 0 % of the mean value of the referen c e met hod (RM ) test data, or not greate r tha n 10% in term s of the emissi on sta nda rd (ppmv, d ry), or h a ve a n a b sol u te difference of le ss t han 5 pp mv betwe en th e mean refe ren c e val ue a n d the mean CE MS value.

3.3.2.7.9.2 D y namic Spiking Dynami c ally spi k ing may be used in lieu of a Rela ti ve Accuracy Test as a mean s to do cume nt the accuracy, pre c isi on, and bi as of the HCl CEMS. The dyn a mi c spi k ing will follow th e HCl Pe rform a n c e Sp ecifi c ati on (attach ed in App endix C). Lin ear reg re ssi on i s use d to e s ta blish th e a ccura cy, preci s i on, an d bia s of the HCl CEMS. The criteria fo r the HCl dynami cspi k ing i s (1 ) The correla t ion co efficie n t, r, must b e greater tha n or equ al to 0.90 (2) The slop e mu st b e 1.0, +/- 0.1 5 (3 ) The Int e rcept mu st be equ al to o r less tha n 1 5 % of the instrument spa n

. See Figure 6 for the Eco c h e m dynami cspi k ing ove rview. 3.3.2.8 Rou t ine Ope ration of HCl CEMS Ongoi ng q u a lity assura nce will foll ow the CMS op eration an d maintena nce req u ire m ents in 40 CF R 63.8(c) a nd the quality co ntrol program requi reme nts under 4 0 CF R 63.8(d). In addition, Lilly will perform daily calib rati on drift tests, quarte rly calibratio n error au dits (ab s olute calib ration audit ) , and an nual accuracy test audits a s part of on-going quality assurance.

3.3.2.8.1 DailyCalibration Drift

The zero and upscal e drift will be checked once dail y. Zero gas (0 ppm HCl ) will be used f o r the zero, and a pproximately 50 -1 00 ppmv HCl for the up scale. Th e calibratio n drif t limit will be 5% of the instru ment span, or ± 5 ppmv. Zero and high -lev el calib ration drifts shall b e adjuste d, at a minimum, whe never the 24 -hou r ze ro drift ex cee d s the limits of the calibratio n d r ift sp ecifi c ation of ±5 ppmv. Th e amount of exce ss ze ro an d high-l e vel d r ift measu red atthe 24-ho u r interval che c ks will b e re corded.

The HCl CE MS will be deemed out of control when ei ther the zero or upscale drift exceeds 2x the perfo rman ce spe c ification. See Section 3.3.2.9. 3.3.2.8.2 Quar terly Absolute Calibra tion Au dit (Calibra tion Error Test)

The Calibrati on Error test will fo llow the procedures i n the HCl CE MS P e rform a nce Specification (attach ed a s appe ndix C). The Ecoch e m CEMS wi ll be challe n ged thre e no n-con s e c utive times with zero, mid-lev e l, and high-l evel certified gases. The cylinder gases will be certif ied gases (EPA Protocol 1

47 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

gases are not available for HCl ). The cal i bration gase s will be inj e cted into the sample sy stem as cl ose to the samplin g probe outlet as p ra ctical and will pa ss thro ugh all CEMS comp onents u s e d durin g n o rm a l monitori ng. The difference between the inst rument re sponse and the re ference value (certi fied gas) will be calculated after ea ch inj e ction and th e re sulting th ree differe nce s will be ave raged to determine the CE at each me asurem ent point . The calib rati on error fo r e a ch of the th ree levels will not excee d 5 % of span.

An absol ute calibration audit will be perf o rmed quarterly , except during the quart e r the annual accuracy is perfo rmed.

3.3.2.8.3 Annu al Accu rac y Test Au dit

The a c cura cy of the HCl CEMS will be determined by p e rformi ng eit her a Relati ve Accu ra cy determi nation , or by dynamic spi k in g. The lo catio n of the sam p le p robe will b e verified.

3.3.2.8.3.1 Se v e n Da y D r ift Tes t

Prior to th e st art of the a ccura cy test (eit her th e Re lati ve Accura cy Determinatio n or Dynami cSpiking ) you must pe rform a calibration drift test for a perio d of at least seve n da ys. The seve n-day calib rat i on drift test must b e cond ucted wh en t he facility i s u nder no rmal operation s . During the cali bration drift te st pe riod yo u must dete r mi ne the magni tude of the zero calib ratio n dr ift and the upscal e cal i bration d r ift at least on ce each day. During the stability tests no adjustments or cali brations may be m ade to the CEMS . If periodic automatic o r manual a dju stments are made to the CE MS zero a n d calib ration setting s, con duct the CD test imme diat ely befo re th ese adj ustm e n ts, o r con d u ct it in such a way that th e CD ca n be dete r mine d. The zero a n d up scale dri ft each m u st be le ss tha n 5% of the instrument spa n ea ch d a y for seven
c o ns ec u t ive da ys

.

3.3.2.8.3.2 Relativ e Acc u rac y Deter m ination The procedure outlined in the HCl CE MS Performance Specification (attached as appendi x C) will be
use d as a gu ide for this specifi c ation. The RA of th e CEMS mu st not be gre a ter than 2 0 % of the mean value of the referen c e met hod (RM ) test data, or not greate r tha n 10% in term s of the emissi on sta nda rd (ppmv, d ry), or h a ve a n a b sol u te difference of le ss t han 5 pp mv betwe en th e mean refe ren c e val ue a n d the mean CE MS value.

3.3.2.8.3.3 D y namic Spiking

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Dynami c ally spi k ing may be used in lieu of a Rela ti ve Accuracy Test as a mean s to do cume nt the accuracy, pre c isi on, and bi as of the HCl CEMS. The dynami cspiki ng will follow the HCl CEMS Perf orma nce Specifi c ation (attache d in Appendix C). Linea r regression i s u s e d t o esta blis h th e accu ra cy, p reci s io n, and bias of the HCl CEMS. T he criteri a for the HCl dyna mic spiki ng a re: (1 ) The correlation coe ffi cient (r) mu st be g reate r t han or equ al to 0.90, (2 ) The slop e m u st b e 1.0, +/- 0.15, (3 ) Th e Intercept m u st b e eq ual to or l e ss tha n 15% of th e instrumen t spa n . See Figure 6 fo r the Ecoch e m dy namic spi k ing overview. 3.3.2.9 Out O f Con t ro l Out of control determinations will follow 40 CF R 63.8(c) (7). Specifically, the HCl CEMS will be considered out of cont ro l if the zero (low-l evel ) or hig h level calib ration drift excee d s two times t he appli c a b l e calib ration d r i ft specifi c atio n (i.e. the ca libration dr ift is greater th an ± 10 ppm v.) In addition, the HCl CEMS will al so b e con s id ered out of control if the CEMS fail s the a c cura cy test audit or a b solute
c a libration audit.

When the HCl CEMS is out of control , Lilly will take the necessary corrective action and shall repeat all
necessa ry tests which in d i cate that the system is o u t of control. Lilly will take co rrective action and
con d u ct rete sting until the perfo rman ce requi rem ents are b e low th e appli c abl e l i mits. The b eginni ng of the out of co ntrol pe riod i s the hour Lill y condu cts a perfo rman ce che c k that in dicate s an excee dan ce of the performance requirem ents. T he end of the out of control perio d will be the hour following the compl e tion o f corre ctive action and succe ssful de mons t ration t hat the sy ste m is within t he allo wa ble limits. When the incine rat o r is o peratin g in para m etric mode, the HCl CEMS will not be dee med out of control. 3.3.3 Use o f HCl CEMS for Demonstratin g Continu o u s Complianc e w i th the HCl/Cl 2 HW C MAC T Emission Standard Lilly may begin using the Ecochem CE MS to demonstrate continuous com p liance with the HWC MA CT HCl/ C l 2 emission stan dard only after the followin g is a c hieve d :

• A successful Perform a nce Specifi c ati on Test is perform ed fo ll owing EPA’s approval of this Alternative Monitorin g Petition.

• A modificatio n to the Title V permit i s a pprove d whi c h e s tablishe s monito ring requireme nts based on the re sults of the approv ed AMP.

Followi ng co mpletion of th e ab ove, on -going qu ality assuran c e wil l be pe rform e d on the Eco c hem CEMS as spe c ified i n Section 3.3. 2.8 of this do cume nt.

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3.3.4 Monitoring F requen c y an d Av eraging Time

The Ecochem CEMS will monitor and record an HCl co ncentrat i on at least once every 15 seconds. A one minute averag e will be cal c ul ated from the f our 15 se con d mea s urem ents du ring t he minute a s sho w n in the followin g equ ation:

2 4

1

### 4 Cl Ci OMA i 

### + = 

# ∑

=

whe re: OMA = HCl/ Cl 2 one-minut e averag e value (pp m vd) Ci = HCl fifteen se co nd ob servatio n fro m the CEMS analyzer (pp m vd)

Cl 2 = Chlorin e gas d e fault value (1 pp m v d),

The twelve h our rolling av erag e will be cal c ulate d ba sed o n the averag e of the 720 mo st re cent valid oneminute avera ges a s sho w n in the followi ng equ ation:



### 720 720

1 

# ∑

= 

### = i 

### OMA THRA

Whe re: THRA = Twel ve hour rollin g averag e value (pp m vd) OMA = One minute avera ge value (p p m vd)

The twelve hour rolling averag e will be u pdate d ev ery min u te wh en a ne w o ne mi nut e average is cal c ulate d

. The HCl/Cl 2 stack con c e n tration will be correcte d to 7% oxygen by the followin g equatio n:

2 

### 21 7 21 * O HCl HCl uncorr corr



### − − =

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whe re: HCl corr = HCl/ C l 2 conce n tra t ion, expressed as HCl correcte d to 7% oxygen (pp m vd) HCl uncorr = HC l/Cl 2 stack ga s co ncentrati on, expre s se d as HCl (p p m vd) O 2 = Oxygen stack ga s pe rcent (vol % dry)

3.3.4.1 Rolling Av erage Calc ulations during HCl CEMS DailyCalibration and O ngoing Qual ity Assu ranc e Audits

The Ecoche m CEMS will be off-line f o r up to a n hour , d a ily, to perfo rm th e daily quality assura nce. Ha zardou s waste will cont inue to be bu rned while p e rf ormi ng the zero a nd up scale drift ch ecks for th e Ecochem CE MS (CO, O 2 , HCl ). Thi s i s in lieu of the 20 min u tes per day p rovi ded fo r in th e appe ndix to subpart EEE of part 63 (section 6.2 of the appendix).
Rolling average cal c ulations will be frozen while Lill y performs the dailyspan drift check and zero drift che c k while contin uing to burn ha zardou s waste, unle ss a re dund ant HCl measureme n t system i s available. T he rolli ng av erage calcul ations will be frozen for a period not t o exceed one hour while burni ng ha za rdou s wa ste for the daily calibratio n test . This hour in clud es the time need ed to calib rate th e Ecochem system for all me asu red para m eters (HCl, CO, O 2 , SO 2 , and NO x ). R o lling ave rag e cal c ulatio ns will resume o n ce th e spa n drift ch eck a n d ze ro drift check h a ve b e en pe rformed

. The twelve-hour rolli ng averag e cal c ulation s will resum e by ad ding the first valid one-mi n u te averag e after the drift che c k to the previou s 71 9 one minute a v erage valu e s

. In addition, ro lling average cal c ulatio ns will also be froz e n while th e qua rterly a b sol u te calibration audit i s con d u cted. Rolling ave rag e cal c ulatio ns will re sum e once the tests have b een compl e ted. T he one -h ou r rolling average calculations will resu me by adding the firs t valid one-mi nute averag e to the previous 59 one minute a v erage valu e s . The twelve-ho u r rolling average cal c ulation s will resum e by ad ding the first valid one-min u te averag e to the previou s 719 o ne mi nute avera ge values.
3.3.4.2 Rolling Av erage Calc ulat ions during System Auto purge The Eco c he m CEMS may be purged automatically once pe r da y while hazardou s wa ste is being burne d. Purgin g invol v es directin g comp re ssed air thro ugh th e pro be into t he sta ck fo r a sho rt pe rio d of time to prevent b u ild up of soli ds i n the probe. The pu rge p e riod will la st approximatel y 5 minutes. Purgin g the stack probe is necessa ry for preventi v e maintena nce rea s on s and is re co mmend ed by the CEMS manufa cturer due to the types of waste s burne d in the solid liquid in cine ration system.

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Duri ng the a u topurge pe ri od, rolling av erag e cal c ul a t i ons for the pollutants mo nitored by the Ecochem sy st em (H Cl, CO, O 2 , SO 2 , and NO x ) will be frozen (similar to when the system is in cali bration mode). Once the autopurge pe rio d is compl e te and data is av ailable (a p p roximately 5 minutes), rolling avera g e cal c ulatio ns will be unfro zen. The app roximate 5-mi nut e time peri od whe n the Ecochem is o ffline due the autopu rge sh ould be con s i dere d excu se d downtime. 3.3.4.3 PM and HWC MACT Me tals Rolling Av erage Cal c ulations d u r ing Ecoche m CEMS Da il y Calibra tion a nd Ongoing Quality Assurance Audits The sta c k m o isture co nte n t mea s u red by the E c o c h e m i s u s e d t o calculate th e d ry sta c k fl owrate. The dry stack flowrate i s used to det ermine the rolling average val ue of t he P M emi ssi on rate in term s of mg/dscm. In addition, the PM CEMS and the Multi

- Metal s CEM S use the st ack O 2 concentration to
corre ct me asured sta c k d a ta to 7% o xygen. Si nce both th e stack moi s ture content a n d sta c k O 2 con c e n tration will be unav ailable when the Ecochem is being cali brated, when performi ng an ACA, or whe n the pro be is bein g p u rge d whil e burni ng ha za rdou s waste, the rolling a v erage cal c ul ations of the HWC MACT metals an d PM emissi on rates will be frozen du ring these pe rio d s . This is in addition to freezi ng the rolling averag e values of the co nsti tue n t s mea s ured by the Ecoch e m CEMS (HCl, CO, O 2 , SO 2 , and NO x (See Section 3.3.4.1). Specifica lly, the rolling ave rag es for the Mul t i-Metals and PM CEMS will be fro z e n on ce th re e co nsecutive 15-minute a v erage value s a re unavail able in a on e ho ur blo c k averag e pe ri od du e to calibration or A C A of the Eco c hem , or auto purg e of the Ecochem sta ck pro be. In addition, Lilly will co nsi der t he time peri o d the rolling a v erage s a re frozen a s excuse d do wnti me. 3.3.5 Bac k up to th e HCl CEMS Lilly will monitor ope ratin g param eter limits defined in Section 1209 of the HWC MACT wh en the incin e rato r is in para m etri c mode. Detail s of the spe c i fic operating l i mits are p rov ided in the NOC. Lilly will incorporate delay s when t ran siti oning from th e CEMS mod e of ope ratio n to the para m etric m ode of operation. Specifically , once the HCl CEMS is u n a v ailable, the control sy ste m will autom atically switch to the pa ram e tric mode o f operation. Rollin g ave rage s, rel a ted to the Air Pollution Co ntrol System (APCS), will not start until the system has b een u n der the pa ra metric m ode of operatio n for 10 min u te s. This 10-minute time period will allow Lilly time to m a ke anyadj ust m ents to the APCS to bring the sy stem to within the resp ective op erating p a ra meter limits. In addition, up to four hours will be allo wed befo re restarting co nst i tuent feed ra te rolling ave rage ope ratin g paramete r limits in orde r to cle a r the solid fee d conveyor sy stem. (Lilly wil l use its best efforts to avoi d introduci ng “new” waste streams from the six “infeed” co nveyors to the fin a l “me rge ” co n v eyor that le a d s to th e kiln feed c hute du ring thi s fo ur hour pe riod. Ho wever, during initial CE MS mode op eration pe rio d s th e re will be p ra ctical li mitations to t h is crite r io n becau se fe w wa ste strea m s will h a ve b een burned. ) Fe ed rate s will b e mai n tained nomi n a lly stable or histori c ally lo wer th an wh en ope rating in CEMS m ode. If the CEMS mode of operatio n is still not

52 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

available afte r four hou rs, the tran sition to param et ri c mode will be compl e ted an d only waste with kno w n comp ositio n will be proce s sed in the i n cin e rato r so that co nstitu ent feed rate ope rating pa ramete r limits can b e com p uted.

3.4 JUSTIFIC ATI O N FO R RE QUEST FO R ALTE RN ATI VE MONITO RING MET H OD
The HWC M A CT final rul e (4 0 CF R 6 3 Subp art EE E) did not m andate the u s e of CEMS f o r p a ramete rs other than CO, hydrocarb on, oxygen, and pa rticul a t e matter. (Use of a particulate matter CEMS is deferred until EPA prom ulgates PM CEMS per formance spec ifications and operational requirements )

. Ho wever, a s stated in the Septembe r 3 0 , 1999 p rea mble to the HWC MACT, 64 Fed. Re g

. 52925, the EPA has a s t rong preference for the use of CE MS for demons tration of c o mplianc e with emiss i on stand ard s . The reg u latory preferen ce for CEMS ove r the use of p rocess op erat ing limits is based on the CEMS dire ct measure of HAPs or surro gate HAP s in the stack g a s , a high deg ree of certai n ty regarding compli an ce with the emi ssi on standa rds, an d provisi on of better compli an ce informatio n to the publi c

. The EPA therefore encourages units like Lilly’s to use CEMS in th e manner proposed in thi s petition as an alte rnativ e to the HWC MACT mandate d p roce s s p a ra m e ter contin uo us monito rin g of 4 0 CF R 63.120 9. This Alternative Monitori ng P e tition inclu d e s p e rfo r ma nce sp ecifi c at ions and q ual ity assu ran c e requi rem ents for each CE MS.

The u s e of t he PM, multi-metal s and HCl CEMS i s a significa nt investmen tthat Lilly has volunta r ily unde rtaken i n orde r to receive certai n regul atory ince ntives. Such regulat ory ince ntives allowed to facilities usi n g altern ative CEMS are o u tlined in the prea mble to the Septem ber 3 0 , 199 9 final HWC MACT rule. The in ce ntives in clud e reli ef from the o peratin g p a ra meter limits p rescribe d in Section 120 9 of the HWC MACT and re lief from sam p ling and a n a l yzi ng the wa ste feed strea m s for a s h, mercury, SVM, LVM, and HCl/Cl 2 . See Table 1 for t he ope rating and emi ssi o n limits that apply whil e the altern ative CEMS are o peratin g. Providing in ce n t ives is a ke y factor for f a cilit ie s volun t arily operating alternative CEMS and e n co ura g e s the developm e n t and im ple m entation of new a nd eme rging CEMS.

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4.0 ALTE RN ATI VE MONITO RING CA N D IDATES UN D E R 63.120 9( g)
Lilly has prep ared this se ct ion of the alte rnative mo nitoring petiti on unde r Se ctio n 63.12 09 (g) of the HWC MACT to req uest reli ef fro m certai n ope rating pa ram e ter re quirem ents.

4.1 STAC K G A S FLOWMETE RD A ILY CH ECK A N D A U TOP U R G E
Section 6.2 o f the Appendi x to the HWC MACT allo ws facilitie s to burn ha zardo u s waste fo r a maximum of 20 minute s whil e cali brating the CO and oxygen CE MS. No compa rabl e provis ion exi s ts in the HWC MACT rul e for ro utine ch ecks of pa ra meter CMS t hat monitor operating dat a. Howeve r, the General Provisions all o w such routi ne chec ks to occur during norma l operation (40CF Rpart 63.8 (c)). Lilly will perfo rm daily routine che cks of the stack gas flow met e r whil e bu rni ng ha zardou s waste.

In additio n , the probe tip on the flo w mete r mo ni toring th e stack g a s flo wrate m a y be purged approximatel y once per day while h a za rdo u s wa ste i s being bu rne d . P u rgin g involv es directin g comp re ssed air throu gh th e prob e into the stack for a sh o rt perio d of time to p revent build u p of solids in the pro be. Th e purge pe rio d will last a p p roximately 5 minutes. Pu rging th e sta c k probe i s ne ce ssary for preventive m a intena nce reason s and i s re co mmen ded by the m anufa cture r d ue to the types of waste s burn ed in the solid liq uid in cine ration system.

Duri ng the daily checks an d auto purge periods, the st ack gas flowrate rolli ng av erage calculations will be froze n . On ce data i s av ailable, rollin g average calc ul ation s will be unfro zen. Spe c ifically, the first available on e - minute ave rage val ue foll owin g the au topurg e peri o d will be a d d ed to the mo st recent 5 9 one-minute a v erage valu e s prio r to free zing the rollin g averag e cal c ulatio ns.

4.2 COM BUSTI ON G A S FL OW RATE O PERATI N G PARAMETE R LIMIT
The sta c k mo isture co ntent measured by the Eco c he m is u s ed to cal c ulate th e dry sta ck flo w rate in te rm s of dscf/min. The dry sta c k flowrate ho urly ro lling a v erage i s co mpared to the HWC MACT maximum comb ustio n g a s flo w rate li mit. The sta c k m o istu re co ntent will be unavailabl e when th e E c o c hem i s being calib rated, pe rformin g a n ACA, or the Ecochem pro be is bein g p u rge d . Th erefore, the roll ing ave rage cal c ulations of the combus tion gas fl owrate will be frozen during th ese events. In addition, Lilly wil l
con s id er the time peri od th e rolling ave rage is fro z e n as excused d o wntime.

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4.3 CAL C U LATI ON OF ROL L ING AVE RAGES W H E N ALL O N E- MINUTE AVERAGE V A L U ES ARE N O T AV AILA BLE Lilly requests that the cal c ulation of the one hour roll ing average v a lu es be allowed to continue provided that 95% of t he o n e - minut e data value s , in terms of t he a ppli c abl e limit, are ava ilable (i.e. 5 7 minutes for an h ourly roll ing ave rag e and 684 min u tes fo r a 12 -hou r rollin g averag e). Correspon dingl y, histori c al stora ge of th e data will b e co nsid ered compl e te prov iding that 95% of the value s have b een captu red

. Purge a nd ca libration time s are ex clud e d from the 95 % calcul ation

. This req u e s t is ba se d on re spo n se to a co mment on the Ap ril 20, 200 4 p ro posed HWC MACT rule. Although, EPA was unabl e to make the change in the final HWC M A CT rul e si gned September 14, 2005, the age ncy stated that it understan ds t he ne ed fo r su ch la ngu ag e and ha s re comm end ed that sou rce s use the p rovi s ion s of 63.1 209(g) to re q ues t this alte rnative monito ring ap proa ch

.

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5.0 ALTE RN ATI VE MONITO RING PETITI O N APP R OV AL

Pursuant to Section 6 3 .8(f)(5 ) of t he G eneral Provisi ons, the Adm i nistra to r will provide n o tification of the approval o r i n tention to di sap p rove req uests m ade u nder Se ction 63.8(f) of th e Gene ral Prov ision s withi n 30 day s of re ceipt of the a pplication, an d within 3 0 d a ys after re ceipt of any supplem enta ry informatio n that is submi tted. Section 63.12 09(g)(1)(iii)(C) states t hat the ti ming for approva l of requests under §63.12 09(g) i s that the Administrator wil l provide notification of the approv al or in tention to disapprove the appli c ation within 90 da ys of recei p t of the application, and within 60 da ys after receipt of any sup p leme ntary information that is sub m itted.

Ho wever, Lill y would wel c ome co mm ents at the agen cy’s earliest conveni ence si nce the alternativ e monitori ng issue s identifie d in this appli c ation affe ct system de sig n and inst rum ent pro c u rem ent activities, test planni n g , control system con figuration, a nd com p leti on of MACT complia nce pl an s.

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6.0 RELEVA NT REFERE NC ES

1. Perform a n c e Spe c ificatio n 11 – Spe c ificatio ns a nd T e st P ro c ed ure s for Particul ate Matter Contin uou s E m issi on Moni toring Syste m s at Stat ion a ry Sou rce s, 40 CF R Pa rt 60, Ap pen di x B, Jan uary 12, 2 004.

2. EPA Draft Guidance Documents on PM CEMS, provided to Eli Lilly and Com p any by EPA Office of Air Quality Planning a nd Standards M a rch 3, 2005.

3. Procedu re 2

- Quality Assuran c e Req u irem ent s fo r Particulate Matter Con t inuou s Emission Monitori ng System s at Stationary Sou rce s, 40 CF R Pa rt 60, Append ix F, January 12, 2004.

4. Draft Metho d 301 Evaluatio n of Candi dat e Con d it ional Method s, Co oper Environ m ental Services, LLC., Volume I, June 10, 2005

• X-ray Based Filter Method s (XFM )

• Multi-Metals Ins t rumental A nalyze r Pro c ed ure (XACT-IAP)

• Quantitative Referen c e Ae rosol Gen e rator (QA G )

5. Draft Standa rd Ope ratin g Proce dure for Gene rati ng a Qua n titative Multi-metals Reference Aero sol with the CES QAG , Coo p e r Env i ronm ental S e rvice s , LL C., Draft Metho d 30 1 Evalu a t ion of Candi date Conditional M e thods Volum e II, Appendix C, June 9, 2005

6. Draft Pe rform ance Sp ecifi c ation YY: Sp ecificat ion s a nd T e st P ro c edures for X-ray Flu o resce n ce Based Multi-metals Co ntinuou s Emi s sion Mo nitori n g System s a tStationary Source s, Co op e r Environme n tal Services, LLC., Draft Method 301 Ev aluation of Can d idate Condition al Me thods, Volume II, Appendix F, June 8, 2005

7. Draft Pro c ed ure Z: Quality Assuran c e Req u ir e m ents for X-ray Fluore s cen c e B a se d Multi-m e tals Contin uou s Emissi on Mo nitoring System s at Stati onary Source s, Coope r Enviro nmental Servi c e s , LLC., Draft Method 301 Evaluation of Candidate Conditional Methods, Volum e II, Appendix F, Jun e 9, 2005

8. Draft Dete rmi nation of Metal Emissi ons from St ationa ry Sources Using Filte rs a nd Solid Sorb ents with X-ray Fl uore s cen c e Analysis, Co oper Envi ro n m ental Se rvice s , LL C., Draft Metho d 301 Evaluation of Can d idate Co nditional Met hod s, Volume II, Appendix B, June 10, 2 005.

57 Rev. 7.0Eli Lillyand Company Lafay e tte, Indiana Altern ativ e Monitoring P e tition

9. Standard Op erating Proce dure fo r Gen e rating a Qua n titative Multi-Metal s Refe rence Aero sol with the CES QAG, Coop er En vironme n tal Service s , LL C., June, 20 05.

10. Perform a n c e Specification 2- Specifi c ati ons an d Test Proced ures for SO2 and NOx Contin u ous Emissi on Mo nitoring Syste m s in Station a ry S ource s, 40 CF R 60 A ppen dix B, F ebru a ry 20 00

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11. Perform a n c e Specificatio n 4A - Specificatio ns a nd Test Pro c ed ure s for Carbon Mo n o xide Contin uou s Emissi on Mo nitoring Syst ems in Stationary Sou rces, 40 CF R 60 Appendi x B, February 20 0 0

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12. Perform a n c e Specificatio n 4B - Specifi c ation s an d Test Pro c e d u res fo r Ca rb on Monoxid e and Oxygen Conti nuou s Emi ssi on Mo nitorin g Systems i n Stationary So urces, 40 CF R 60 Appe ndi x B, Septembe r 3 0 , 1999.

13. Appendix to Subpart EEE of Part 63 – Quality Assurance Procedures fo r Cont inuous Emissions Monitors Us ed for Haz a rdous Was t e Combus tors , 40 CFR 63 Subpart EEE, Sept ember 30, 1999.

14. Perform a n c e Specification Z: Specifications an d Test Proced ures For Hyd rog e n Chlo ride (HCL) Contin uou s Emissi on Mo nitoring System s At Stat ionary Source s, Eli Lilly, November 20 05.

15. Procedu re DD: Quality Control and Quality Assu ran c e Requi rements fo r Hydro gen Ch lorid e (HCL ) Co ntin uou s Emissio n Monito ri ng Systems At Stationary Sou rce s, Eli Lilly, Novemb er 2 0 05.

58 Rev. 7.0