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## Richard Lambert, Eli Lilly Michael Foster, Eli Lilly 

## The Emission Monitoring System in this paper was installed at the Eli Lilly Tippecanoe Laboratory Facility from 2005 until 2010  

## Evonic DeGussa purchased the Tippecanoe Laboratory site in 2010  

## This paper will focus ONLY on the operation 

## from 2005 to 2010 while under the ownership of Eli Lilly 6/8/2011 RH Lambert 3 

## Key Points to Remember  

## Background  

## Regulatory  

## Multi-Metals CEMS Technology  

### X- Ray Fluorescence Technology  

### “Doped Tape” for elemental and ionic metals (Hg)  

### Quantitative Aerosol Generator

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## Quality Assurance  

## Accuracy Test using a Quantitative Aerosol Generator  

## Experience using Multi-Metals CEMS  

### Used in lieu of M29 for most recent Performance Test  

### Used to gather information on specific waste lots  

### Used at Coal Fire Boiler for Hg study  

## The Good, the bad, and ugly

6/8/2011 RH Lambert 5 Lilly successfully installed, certified, and operated a Multi -Metals

Emission Monitoring System on a Rotary Kiln Incinerator  The benefit of using a multi- metals CEMS was in conjunction to using a total particulate and HCL CEMS  The Regulatory piece was significant and required negotiation with EPA technical branch and the Sate of Indiana  The Quantitative Aerosol Generator was essential for development, certification and on- going QA  The choice of X-Ray Fluorescence as the analytical technique was not an accident  The sample interface design was integral to success  Development of compliance software and interfacing the instrument to a site control system takes time and patience 6/8/2011 RH Lambert 6 

## Requires a proven analytical technique

 

### Use of solutions become problematic  

## Requires a proven sample interface  

## Providing a representative sample to the analyzer is experience based  

## Requires a proven standard generator for comparison of analytical results  

### Real time information is necessary to fully understand the system

6/8/2011 RH Lambert 7 

## Tippecanoe Labs Rotary Kiln hazardous waste incinerator (T149 Kiln)  

## T149 kiln capacity is 50 mm BTU/hour  

### T149 Kiln was permitted as a NEW incinerator under the interim HWC MACT Standards  

## There is a site Title V permit

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## The T149 Kiln used 3 continuous emission monitoring systems (CEMS) to demonstrate compliance with specific HWC MACT emission standards  

## EcochemTM 

## multi-component CEMS  

### SigristTM 

### total particulate CEMS  

### XactTM 

### multi- metals CEMS 

## These three CEMS allow compliance with respective HWC MACT emission limits in lieu



## of specific operating limits

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## Alternative Monitoring Petition required

 

### Approved by OAQPS (EPA) in 2006  

## Title V permit approved in early 2007  

## Major modification  

### Required prior to using the metals CEMS for compliance with the HWC MACT metals emission 

## standards  

## This was a three year exercise with EPA and the State of Indiana

6/8/2011 RH Lambert 106/8/2011 RH Lambert 11Cooper Environmental Services 12 

### ~700 lpm QAG Spike

CES Xact MM CEMS6/8/2011 RH Lambert 13 

## Quantitated 26 metals every 15 minutes  

## Averaging time was 12 hour rolling average updated every hour  

## Compliance was based upon the HWC MACT Metals  High Volatile (Hg)  45 ug/dscm @7% O 2  Semi-Volatile (Pb + Cd)  120 ug/dscm @7% O 2  Low Volatile (Be + As + Cr)  97 ug/dscm @7% O 2  Be has a default value of 2 ug/dscm for each sample added to the LVM category 6/8/2011 RH Lambert 14 

## Precision: Stability check with each sample

 

### Pd rod  

## Accuracy: Zero and upscale drift check daily for MACT metal classes  

### High volatile (Hg)  

### Semi volatile (Cd, Pb)  

### Low volatile (Cr)  

## Sample Flow Check daily

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## Quarterly Audits

 

### Thin film calibration audit (MACT Metals)  

### Sample Volume Audit  

## Annual Audit  

### Thin film calibration audit (MACT Metals)  

## Sample Volume Audit  

### Linearity Test with QAG  

### Four levels for each MACT metal

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## QAG provides quantitative metal aerosols at selected concentrations over the expected measurement range  

### 0 to 10,000 ug theoretical range  

### Method 301 validated as NIST traceable for Heavy Metals

6/8/2011 RH Lambert 18Cooper Environmental Services 19 

### Drying Chamber Bubblers Pump Reservoir 

### Balance Nebulizer Droplet Size 

### Control Focused TransportCooper Environmental Services 206/8/2011 RH Lambert 21Cooper Environmental Services 22 

## Provide metal aerosols at a minimum of three levels and zero for MACT metals  

### Use QAG to quantitatively spike metals  

## 5 MACT metals simultaneously spiked  

### Minimum of nine data points per spiking level  

### Spike through the emission limit for all metals  

## Establish Quantitative Range of “system”  

### Regression analysis

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## Regression Analysis  

## Plot Xact CEMS response versus quantitatively spiked metal concentration  

### Slope represents accuracy  

### 0.85 – 1.15  

### Correlation Coefficient represents precision  

### < 0.90  

### Intercept must be < 20% of applicable emission standard for each metal

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## Used as reference method during performance test of the T149 incinerator  

### Total particulate and HCL  

## Used to profile coal fired boiler for:  

### Hg emissions during different firing rates  

### Profiling different lots of coal  

### Understanding impact of carbon injection on Hg removal  

### Efficiency 6/8/2011 RH Lambert 30 

## Development of “WSIS” sheets for various lots of solid waste  

### Characterizes solid waste drums into categories 

## based upon contents and emissions profiled by CEMS (metals, PM, HCL)  

## Used to understand best operating conditions 

## for efficiency (energy reduction)  

### PM and HCL as well  

### No parametric limits when in CEMS mode for those 

## correlating to PM, HCL, and metals

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## Metals CEMS installed and operated on-line since 2005  

## Clean Air Act Technology Award Winner  

## Largest hurdle to reach steady operation was the interfacing to the site control system as well as the compliance software in the site control system  

## Required deconvolution work for some 

## overlapping energy lines  

### Lab development brought analysis to the 90% level 6/8/2011 RH Lambert 32 

## The paper (doped) used to collect the aerosol and particulate costs approximately $20,000 annually  

## The detector tube life is 12 – 18 months  

## Very few issues with mechanical parts of system  

### Things do wear out and part of our experience was documenting this for a preventative maintenance plan Maintenance support agreement with Cooper Environmental Services was necessary and prudent 6/8/2011 RH Lambert 33 

## The unit does not enjoy lightening strikes  

## The unit is not hydrophobic  

## The Xact multi-metals CEMS has evolved since 

## the 2004 unit was build  

### Better detection limits  

### Component upgrades from Lilly experience  

## Flows now mostly reducing orifice  

### Controller for unit now PLC based  

### XRF components and software different with better 

## control and flexible software  

## Unit operates well but requires attention from trained personel 6/8/2011 RH Lambert 34 

## Dr. John Cooper and staff, Cooper Environmental Services LLC  

### Mike Foster, Corporate Environmental Affairs, Eli Lilly  

### Sherman Wright, Tippecanoe Laboratory Incineration Operations, Evonik Degussa  

### Jason Marlin, Operations, Eli Lilly

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