HCL Dynamic Spiking Protocol

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1 ELI LILLY AND COMPANY TIPPECANOE LABORATORIES LAFAYETTE, IN Revisio 2.0

2 TABLE OF CONTENTS REVISION HISTORY REVISION REVISION OVERVIEW DEFINITIONS EQUIPMENT EQUIPMENT CALIBRATION AND STANDARDS HCL CEMS ELEMENT OF OPPORTUNITY CEMS FLOW MEASUREMENT SYSTEM Lamiar flow elemet Flow by dilutio GAS MANIFOLD HCL CALIBRATION GAS FOR DYNAMIC SPIKING DYNAMIC SPIKING RANGE TYPICAL DYNAMIC SPIKING SET-UP DYNAMIC SPIKING PROCEDURE COLLECTION OF BASELINE DATA COLLECTION OF TEST DATA DATA CALCULATIONS Baselie data Dyamic Spikig Test ru data Referece HCL cocetratio calculatios Liear Regressio CRITERIA FOR ACCEPTANCE BIAS CORRECTION TABLES REFERENCES APPENDIXES...2

3 REVISION HISTORY. REVISION.0 Revisio.0, Tippecaoe Laboratories NON-GMP Stadard Operatig Procedure, Eli Lilly ad Compay, December 8, REVISION 2.0 This revisio is a update of the origial Dyamic Spikig protocol, December The followig are key updates i revisio 2.0:. Recommedatio that all HCL QA gases be certified with a miimum tolerace of 5% 2. Discussio for the use of quatitative itroductio of the HCL calibratio gas ad subsequet total flow measuremet as method for determiig the referece HCL cocetratio durig each test ru. 3. Updated the dyamic spikig procedure descriptio for easier flow of iformatio 4. Updated the equatios to iclude percet relative stadard deviatio ad the calculatio for the referece HCL cocetratio whe usig quatitative itroductio of the HCL calibratio gas with subsequet total flow measuremet. 2

4 2 OVERVIEW Dyamic Spikig is procedure to establish the accuracy, precisio, ad bias of a moitorig system. Durig the dyamic spikig procedure, a certified calibratio gas (+/- 5%) is spiked ito the moitorig system while the system is samplig flue gas. It is importat that the spiked calibratio gas flow through the etire samplig system. The target ratio of flue gas to HCL calibratio gas is 9:, with a miimum requiremet of :. The HCL calibratio gas is spiked i three rages (low, mid, high) through the rage of HCL detector. A miimum of 30, oe miute averaged data poits should be collected for each of the three test rus. It is recommeded that the percet relative stadard deviatio of the data set, for each test level, be less tha or equal to 20%. If the flue gas has sigificat amouts of HCL preset, the data may be corrected for the baselie HCL cocetratio. This is performed by collectig at least 0, oe miute average HCL data poits prior to each test ru. The average of the te baselie HCL values will be used to compesate the subsequet test ru data for backgroud HCL cocetratios. It is importat that the cotrol device be ruig at steady state; alleviatig large fluctuatios i the backgroud HCL cocetratios. The HCL CEMS will provide the measured HCL values. These values are compared, usig liear regressio, to the kow or spiked HCL cocetratios. There are two methods for calculatig the kow HCL cocetratios: () Use of a elemet of opportuity ad (2) Quatitative itroductio of the HCL calibratio gas with total flow through the system. A elemet of opportuity ca be ay elemet ormally preset, i steady cocetratios, i the flue gas stream. Examples are O2, CO, NOx, SO2, CO2, ad moisture. Total flow through the system is also a example of a elemet of opportuity. The elemet of opportuity is measured durig the baselie data collectio, prior to the test ru. The average value durig this baselie collectio period is used to establish the baselie cocetratio, or flow value, without ay spikig of the calibratio gas. The elemet of opportuity is measured durig each test ru while the HCL calibratio gas is beig spiked. The elemets of opportuity values, collected durig each test ru are averaged. Kowig the cocetratio of the HCL calibratio gas, ad the dilutio of the elemet of opportuity due to the spikig, the kow value of the HCL calibratio gas i the measuremet stream ca be calculated. The kow value of the spiked HCL calibratio gas i the measuremet stream ca also be calculated by quatitatively itroducig the HCL calibratio gas, ad, measurig the total flow through the system. I this case, the HCL calibratio gas cocetratio, the flow rate of spiked HCL calibratio gas ito the measuremet stream, ad the total flow through the system are used to calculate the kow value of the spiked calibratio gas. As with the HCL CEMS data sets, it is recommeded that the percet relative stadard deviatio for the elemet of opportuity data sets be less tha or equal to 20%. Oce the data is collected, liear regressio is performed usig the kow HCL spike values ad the correlatig HCL CEMS measured values. Criteria for the HCL dyamic spikig are:. The correlatio coefficiet must be greater tha or equal to the slope of the regressio lie must be.0 +/

5 3. The itercept, of the regressio lie, must be less tha or equal to 5% of the istrumet spa. The HCL CEMS must meet the correlatio criteria. If either the slope ad/or itercept criteria are ot met, a bias may be applied to the HCL CEMS oe miute value. Performace Specificatio Z: Specificatios ad Test Procedures for the HCL Cotiuous Emissio Moitorig Systems at Statioary Sources should be as a referece documet for dyamic spikig requiremets ad calculatios. 4

6 3 DEFINITIONS Bias: The differece betwee the referece value ad the measured value. Calibratio Drift: The differece i the CEMS output readigs from the established referece value after a stated period of operatio durig which o uscheduled maiteace or adjustmet took place. Cotiuous Emissio Moitorig System: meas the total equipmet required for the determiatio of a gas cocetratio or emissio rate. The sample iterface, pollutat aalyzer, diluet aalyzer, ad data recorder are the major subsystems of the CEMS. Correlatio Coefficiet: determies the extet of a liear relatioship betwee two fields over a give period of time. Data Recorder: The portio of the CEMS that provides a record of aalyzer output, flags which idicate ormal operatio, ad flags idicatig abormal operatio. The data recorder may record other pertiet data such as effluet flow rates, ad various istrumet temperatures. Dyamic Spikig: a procedure used to documet the accuracy, precisio, ad bias of the moitorig system by quatitatively spikig a certified gas ito the pollutat gas stream. Elemet of Opportuity: Ay elemet, preset i the flue gas matrix (or total flow) that has little fluctuatio ad ca be used to determie the referece HCL cocetratio durig the dyamic spikig test rus. Gas Chromatograph: A aalytical istrumet which uses a carrier gas to trasport gas/vapor phase samples to a solid matrix for separatio, ad subsequet detectio by a aalyte specific detector. Gas maifold: Idividual, or series of flow cotrollers that allow cotrolled flow of a gas. Calibrated flow cotrollers ca be used to quatitatively cotrol the flow of gases. 5

7 Istrumet Measuremet Rage: The rage of HCl cocetratios the istrumet ca reliably measure from the lowest cocetratio to the highest. Itercept: value of the Y variable whe the X variable is equal to zero. Lamiar Flow Elemet: A device used to measure the flow gas through a system by measurig the pressure drop of the gas over a restrictio (forces parallel, or lamiar flow). Liear Regressio: a methodology used to fid a formula that ca be used to relate two variables that are liearly related. Respose Time: The time iterval betwee the start of a step chage i the system iput ad whe the pollutat aalyzer output reached 95% of the fial value. Sample Iterface: The portio of the CEMS used for oe or more of the followig: sample acquisitio, sample trasport, sample coditioig, or protectio of the moitor from the effects of stack gas. Slope: The rate of chage of Y relative to the chage i X. Upscale drift: meas the absolute differece betwee a high-level calibratio gas ad the moitor respose, i uits of the applicable stadard. Zero drift: meas the absolute differece betwee a high-level calibratio gas ad the moitor respose, i uits of the applicable stadard. 6

8 4 EQUIPMENT The followig list cotais typical equipmet required to perform the HCL dyamic spikig.. HCL CEMS 2. Referece Aalyzer(s) for the elemet of opportuity (examples are NOx, SO2, CO, CO2, O2) 3. Flow Measuremet Systems a. Lamiar flow elemet b. Gas chromatograph (for dilutio flow with a hydrocarbo) 4. Calibratio Equipmet a. Bubble Flow meter, maometer, or equivalet for primary flow calibratio b. Certified HCL Calibratio gas for spikig c. HCL calibratio gases for zero ad upscale drift check of the HCL CEMS d. Calibratio gas for the elemet(s) of opportuity CEMS calibratio e. Hydrocarbo gas for flow measuremet via dilutio samplig 5. Quatitative gas maifold, or equivalet, for itroductio of the HCL calibratio gas 6. Quatitative gas maifold, or equivalet, for the itroductio of the hydrocarbo for dilutio flow (if used) 7. Various fittigs ad tubig 7

9 5 EQUIPMENT CALIBRATION AND STANDARDS Prior to performig the HCL dyamic spikig, it is importat that all equipmet ad/or aalyzers are calibrated. This sectio provides guidace o the calibratio requiremets for all equipmet used durig the HCL dyamic spikig procedure. 5. HCL CEMS Prior to performig the dyamic spikig procedure, the HCL CEMS must pass the QA requiremets specified i performace specificatio Z: Specificatios ad Test Procedures For HCL Cotiuous Emissio Moitorig Systems at Statioary Sources. Typically, this would iclude passig the daily zero ad upscale calibratio drift check, ad for aual audits passig both the zero ad upscale drift check as well as a seve day drift test. All calibratio gases must be certified gases, with a recommeded tolerace ot to exceed +/- 5%. 5.2 ELEMENT OF OPPORTUNITY CEMS The moitorig system used to measure the elemet(s) of opportuity, other tha total flow, must pass a calibratio directly prior to use. After dyamic spikig ru, the zero ad upscale calibratio drift are checked. The drift requiremet, for both zero ad upscale, is 3% of the referece value, uless stated otherwise i the applicable referece method. If either the zero or upscale calibratio check fails the drift limit after a dyamic spikig ru, the ru must be repeated. 5.3 FLOW MEASUREMENT SYSTEM Total flow may be used as a elemet of opportuity, or, as part of measurig the quatitative itroductio of the HCL calibratio gas for the dyamic spikig tests. There are several methods that ca be used to provide a total flow measuremet. This protocol outlies two approaches, lamiar flow elemet ad flow by dilutio. Other total flow measuremet systems ca be used; however, specific protocol describig the methodology must be used Lamiar flow elemet Prior to the dyamic spikig procedure, the lamiar flow elemet is calibrated agaist a primary flow stadard, such as a bubble flow meter. The calibratio must iclude at least three poits throughout the expected measuremet rage. After each dyamic spikig test ru, the calibratio drift is checked at each of the three poits. The lamiar flow elemet must be re-calibrated if ay of the drift check poits exceed 0% of the expected value (established durig the pre-test calibratio). 8

10 5.3.2 Flow by dilutio Flow by dilutio is a method where a kow cocetratio of gas is quatitatively itroduced to the flue gas stream ad measured dowstream by a calibrated istrumet. For example, a kow cocetratio of propae ca be quatitatively itroduced to the flue gas stream ad the diluted propae measured dowstream. Prior to the dyamic spikig procedure, the gas chromatograph is calibrated, usig at least four poits through the expected measuremet rage. After the dyamic spikig procedure is complete, the gas chromatograph is checked for bias at each of the four calibratio levels. The bias should be less tha 5% of the expected value for each poit. Method 8 provides guidace for the calibratio procedure ad requiremets. Prior to the dyamic spikig procedure, the gas maifold (used to quatitatively itroduce propae, or similar hydrocarbo), which is typically a mass flow cotroller, is calibrated to a primary stadard. After each test ru, the gas maifold is checked for drift, ad adjusted if the drift exceeds 0% of the expected value (calibrated value prior to dyamic spikig procedure). Method 205 provides guidace for this procedure. 5.4 GAS MANIFOLD HCL may be quatitatively itroduced ito the flue gas stream, ad whe used i cojuctio with a total flow measuremet, ca provide the referece HCL spikig cocetratios for each dyamic spikig ru. Prior to the dyamic spikig procedure, the gas maifold (used to quatitatively itroduce HCL), which is typically a mass flow cotroller, is calibrated to a primary stadard. After each test ru, the gas maifold is checked for drift, ad adjusted if the drift exceeds 0% of the expected value (calibrated value prior to dyamic spikig procedure). Method 205 provides guidace for this procedure. 5.5 HCL CALIBRATION GAS FOR DYNAMIC SPIKING The HCL calibratio gas used for dyamic spikig must be a certified gas with a tolerace less tha or equal to 5%. 9

11 6 DYNAMIC SPIKING RANGE The flue gas stream must be spiked at a miimum of three separate levels (low, mid, high) throughout the rage of the HCL CEMS. The low level should be betwee 0 50%, the mid rage should be betwee 25 75%, ad the high rage should be betwee 50 00% of the spa of the istrumet. The dyamic spiked HCL cocetratios ca oly be used for oe rage (Table ). 7 TYPICAL DYNAMIC SPIKING SET-UP Figure. Typical Dyamic Spikig Apparatus Dyamic Spikig Apparatus Sample Probe Heated lie iside sample umbillical Flue Gas Heated sample lie Heated Filter Pressure Cotrol Lamiar Flow Elemet Calibratio Maifold (Mass flow meters) ppm HCL i N2 HCL CEMS Gas Coditioer Referece Measuremet(s) 0

12 8 DYNAMIC SPIKING PROCEDURE This sectio describes the procedure used to perform HCL dyamic spikig. Prior to testig, it is importat that all aalyzers are calibrated accordig to sectio 6 of this documet. I additio, the cotrol device should be at a steady state (small fluctuatios of HCL or elemets of opportuity). 8. COLLECTION OF BASELINE DATA The baselie data will be used to compesate the measured HCl, durig the dyamic spikig ru, for backgroud cocetratios of HCL which may be preset durig ormal operatios. It is importat to collect all elemet of opportuity data as well as HCL backgroud data durig the baselie collectio period.. Collect a miimum of te, miute averaged HCL data poits prior to each dyamic spikig test ru. 2. Collect te, miute averaged data poits for the elemet(s) of opportuity to be used for calculatig the referece HCL cocetratio. The elemet of opportuity data set is collected simultaeous to the HCL baselie data, ad must be collected prior to each dyamic spikig test ru. 3. If usig total flow, collect a miimum of oe flow readig durig the baselie data collectio. 4. Prior to begiig the dyamic spike, esure that all baselie data (HCL, elemet of opportuity, flow) does ot exhibit large fluctuatios i cocetratio (steady state). If large fluctuatios exist, the baselie data collectio procedure must be repeated. 8.2 COLLECTION OF TEST DATA The HCL CEMS must be tested at a miimum of three levels through the measuremet rage of the istrumet (low, mid, high), Table. Prior to each dyamic spikig test ru, it is importat that the appropriate baselie data is collected (sectio 7.) ad that all equipmet is calibrated ad appropriate bias checks are performed (sectio 6).. Itroduce the HCL calibratio gas to the measuremet system ad allow the HCL CEMS values to reach a steady state. This may take up to 5 miutes.

13 2. Collect a miimum of 30, oe miute average HCL data poits. 3. Collect a miimum of 30, oe miute average elemet(s) of opportuity data poits. 4. If usig total flow through the system, collect at least five data poits durig the dyamic spikig test ru. 5. If usig quatitative itroductio of the HCL calibratio gas, collect at least five data poits for the calibratio gas flow rate ito the system durig the dyamic spikig test ru. 6. Before stoppig the dyamic spikig test ru, esure that the data sets are complete. It is recommeded that the percet stadard deviatio, for all data sets, be less tha or equal to 20%. 7. Stop the HCL calibratio gas dyamic spikig ad allow the system to retur to baselie coditios. 8. Perform a bias check for the elemet of opportuity referece CEMS, the flow measuremet system, ad the gas maifold for the HCL calibratio gas ad hydrocarbo (if dilutio flow is used to calculate the referece HCL cocetratio). Sectio 6 provides guidace for the bias checks. 9. Repeat the baselie data collectio, ad the dyamic spikig data collectio, for subsequet HCL test levels. 0. If dilutio flow is used to calculate the HCl referece values, after the HCL dyamic spikig test rus are complete, perform a bias check of the dilutio aalyzer. 8.3 DATA CALCULATIONS This sectio provides the calculatios required to determie the accuracy, precisio, ad bias of the HCL CEMS Baselie data HCL CEMS data The baselie HCL cocetratio is measured prior to each dyamic spikig ru. For each baselie HCL data set, calculate the average, i ppm, usig equatio. 2

14 Calculate the arithmetic mea of a data set as follows: x = xi (Equatio ) where : x = Arithmetic mea = Number of data poits x i = Value of each data poit Elemet of Opportuity Data The elemet of opportuity data set is acquired prior to each dyamic spikig test ru, simultaeous to the baselie HCL cocetratio data set. For each elemet of opportuity, calculate the average value usig equatio Flow via dilutio Whe usig dilutio of a measured aalyte (such as a hydrocarbo with subsequet GC measuremet) as a idicator of total flow, calculate the total flow, i liters per miute usig equatio 2. Calculate the total flow as follows: Tflow = ( Aaltye spike ) * Tflow ( Aalyte measured) (Equatio 2) Tflow = Total flow through the system i lpm Aalyte-Spike = Cocetratio of Spiked Aalyte (ppm) Aalyte-measured = Measuremet, dowstream, of spiked Aalyte (ppm) Calculate the average flow value, for the data set, usig equatio. 3

15 8.3.2 Dyamic Spikig Test ru data HCL CEMS data For each dyamic spikig test ru, calculate the average ad percet relative stadard deviatio of the data set usig equatios ad 3, respectively. Calculate the percet stadard deviatio as follows: PRS d = i = / d i = i d i (Equatio 3) x Where: PRS = Percet Relative Stadard Deviatio of the data set d x = Arithmetic mea Elemet of Opportuity data For each dyamic spikig test ru, calculate the average ad percet relative stadard deviatio of the data set usig equatios ad 3, respectively. If usig total flow as a meas to determie the referece HCL calibratio gas cocetratio, use equatio 2 to calculate the total flow prior to determiig the average ad percet relative stadard deviatio of the data set. 4

16 8.3.3 Referece HCL cocetratio calculatios Elemet of opportuity to calculate referece HCL cocetratio Equatio 4 is used to calculate the referece HCL cocetratio for a give dyamic spikig test ru. Opp post HCl ref = * CalGas + BaselieHCl (Equatio 4) Opp pre avg avg where: Opp-post avg = average referece elemet of opportuity value durig dyamic spikig test ru Opp-pre avg = average referece elemet of opportuity value durig baselie test ru CalGas = HCl calibratio gas cocetratio Baselie HCl = CEMS HCl average baselie value Quatitative HCL calibratio gas itroductio ad total flow to calculate referece HCL cocetratio Whe usig the quatitative itroductio of calibratio gas ad total system flow to calculatio the referece HCL cocetratio for a give dyamic spikig test ru, use equatio 5. Equatio 2 is used to calculate the total system flow. HCl ref = Cflow Tflow avg avg * CalGas + BaselieHCl (Equatio 5) Where: HCl ref = Referece HCl value for ru X Cflow = Average calibratio HCL gas flow rate ito system (lpm) 5

17 Tflow = Average Total System Flow durig ru (lpm) CalGas = HCl calibratio gas cocetratio Baselie HCl = CEMS HCl average baselie value Liear Regressio Liear regressio is used to calculate the accuracy, precisio, ad bias of the HCL CEMS. For each dyamic spikig test ru, plot the HCL CEMS referece value, Xaxis, versus the HCL measured value, Y axis. Determie the correlatio coefficiet (r ), the slope, ad the itercept usig equatios 6-9. ˆ = b + b x (Equatio 6) y o where: b o = The y itercept b = The slope The itercept is calculated accordig to the followig equatio: b o = y b x (Equatio 7) where: x = y = x i i= y i i= The slope of the lie is calculated accordig to equatio below: 6

18 ( xi x )( yi y ) i= b = (Equatio 8) 2 ( x x ) i= i The liear correlatio coefficiet is calculated accordig to the followig equatio. r 2 ( x x)( y i i i= = 2 ( xi x) ( i= i= y) y y) i 2 2 (Equatio 9) 8.4 CRITERIA FOR ACCEPTANCE The criteria for the HCl dyamic spikig is: The correlatio coefficiet, r, must be greater tha or equal to 0.90 The slope must be.0, +/- 0.5 The Itercept must be equal to or less tha 5% of the istrumet spa. At a miimum, the data set must meet the correlatio coefficiet. If this is ot met, the dyamic spikig procedure must be repeated util the correlatio coefficiet criteria are met. If the HCl CEMS has met the correlatio coefficiet requiremet, but does ot meet either the slope, or itercept criteria, a bias exists ad a correctio factor must be applied to the HCl CEMS for data collectio. The equatios to determie the corrected value are provided i Sectio 8.5. The correctio factor must be applied to the HCl CEMS oe-miute average data util a ew dyamic spikig procedure idicates the specific bias o loger exists, or, a differet correctio factor (bias) is idicated. 7

19 8.5 BIAS CORRECTION If the HCl CEMS fails to meet both the slope ad itercept criteria, the followig correctio factor must be applied to the oe-miute average HCl data: C C y b i 0 = (Equatio 0) b Where: C C = corrected CEMS HCL cocetratio y i = CEMS reported HCL cocetratio b 0 = the itercept of the least squares liear regressio lie b = the slope of the least squares liear regressio lie b). If the HCl CEMS fails to meet the slope criteria, but meets the itercept criteria, the followig correctio factor must be applied to the oe-miute average HCl data: yi C C = (Equatio ) b c). If the HCl CEMS fails to meet the itercept criteria, but meets the slope criteria, the followig correctio factor must be applied to the oe-miute average HCl data: C C = y (Equatio 2) i b 0 8

20 9 TABLES Table. Ogoig Quality Assurace/Quality Cotrol Calibratio Gas Rages HCl Calibratio Gas Cocetratios a Test Uits Zero-level Mid-Level High-Level Daily Calibratio Drift % of Spa 0-30 NA Absolute Audit Calibratio % of Spa Dyamic Spikig % of Spa a A copy of the supplier s certificate of aalysis must be provided for each gas cylider. Calibratio gases do ot eed to be Protocol gases. It is recommeded that the calibratio gases, for all QA, have a miimum tolerace of 5%. 9

21 0 REFERENCES. Uited States Evirometal Protectio Agecy (EPA). Techology Trasfer Network, Emissio Measuremet Ceter, Promulgated Methods, Test Method 205: Verificatio of Gas Dilutio Systems for Field Istrumet Calibratios. Available: 205.pdf via the iteret. 2. Uited States Evirometal Protectio Agecy (EPA). Techology Trasfer Network, Emissio Measuremet Ceter, Promulgated Methods, Test Method 8: Measuremet of Gaseous Orgaic Compoud Emissios by Gas Chromatography. Available: via the iteret. 3. Performace Specificatio Z: Specificatios ad Test Procedures for Hydrochloric Acid Cotiuous Emissio Moitorig Systems at Statioary Sources. Eli Lilly ad Compay, Procedure DD: Quality Cotrol ad Quality Assurace Requiremets for Hydrochloric Acid Cotiuous Emissio Moitorig Systems at Statioary Sources. Eli Lilly ad Compay, Dilutio Flow Measuremet Protocol: Measuremet of Total flow usig a tracer gas with subsequet dow stream quatitatio. Eli Lilly ad Compay,

22 APPENDICES 2

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