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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

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 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

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 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

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 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

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 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

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Cooper Environmental Services 12

~700 lpm

QAG Spike

CES Xact MM CEMS
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 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% O2

 Semi-Volatile (Pb + Cd)

 120 ug/dscm @7% O2

 Low Volatile (Be + As + Cr)

 97 ug/dscm @7% O2

 Be has a default value of 2 ug/dscm for each sample added to the LVM category

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 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

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Cooper Environmental Services 19

Drying Chamber

Bubblers

Pump

Reservoir

Balance Nebulizer

Droplet Size 

Control

Focused 

Transport
Cooper Environmental Services 20
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Cooper 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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Plotted Linear Regression for Hg: 0-1500

y = 0.7491x + 6.7424

R2 = 0.9986

0

500

1000

1500

0 500 1000 1500 2000

Reference ug/dscm (QAG)

Xact ug/dscm

Plotted Linear Regression for Pb: 0-2300

y = 0.7588x + 13.157

R2 = 0.9949

0

500

1000

1500

2000

2500

0 1000 2000 3000

Reference ug/dscm (QAG)

X

a

ct ug/d

s

c

m

Plotted Linear Regression for As:

 0-2300

y = 0.769x + 13.482

R2 = 0.9965

0

500

1000

1500

2000

0 400 800 1200 1600 2000 2400 2800

Reference ug/dscm (QAG)

Xact ug/dscm

Plotted Linear Regression for Cd:

 0-2300

y = 0.8139x + 5.1694

R2 = 0.9966

0

500

1000

1500

2000

0 500 1000 1500 2000 2500

Reference ug/dscm (QAG)

Xact ug/dscm

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Plotted Linear Regression for Cr: 0-850

y = 0.8277x - 1.1648

R2 = 0.9977

0

200

400

600

800

0 200 400 600 800 1000

Reference ug/dscm (QAG)

X

a

ct u

g/d

s

c

m

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Metal: Cr

Date(s) Data Collected: 8/05/10 - 8-06-10

Number of Runs Collected: 36

Regression 

Criteria

Regression 

Criteria Limits Regression Results Pass/Fail

Slope 0.85 - 1.15 0.9747 Pass

Intercept <19.4 3.7603 Pass

R

2 NA 0.996 NA

Correlation 

Coefficient (r) >0.90 1.00 Pass

Metal: As

Date(s) Data Collected: 8/05/10 - 8-06-10

Number of Runs Collected: 36

Regression 

Criteria

Regression 

Criteria Limits Regression Results Pass/Fail

Slope 0.85 - 1.15 1.061 Pass

Intercept <19.4 1.62 Pass

R

2 NA 0.995 NA

Correlation 

Coefficient (r) >0.90 1.00 Pass

Click for Chromium Regression

Click for Arsenic Regression

y = 0.9747x + 3.7603

R2 = 0.996

0

50

100

150

200

0.00 50.00 100.00 150.00 200.00 X

a

ct C

o

n

c

e

ntratio

n

(μ

g/d

s

c

m)

Reference Concentration (μg/dscm)

Plotted Linear Regression for Chromium

y = 1.0611x + 1.6166

R2 = 0.995

0

50

100

150

200

250

0 50 100 150 200 X

a

ct C

o

n

c

e

ntratio

n

(μ

g/d

s

c

m)

Reference Concentration (μg/dscm)

Plotted Linear Regression for Arsenic
 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 

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 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

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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

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 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

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 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 

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 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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