Report ICR Testing June 30, 2010 

Kansas City Power & Light ii CEC Project 100-208 

Sibley Generating Station 

TABLE OF CONTENTS 

Page

1.0 Project Summary ................................................................................................................. 1

1.1 Testing Approach ........................................................................................................ 1

1.2 Project Participants ..................................................................................................... 3

1.3 Sibley Generating Station ........................................................................................... 4

2.0 Data Summary .................................................................................................................... 5

2.1 Sampling Results for USEPA Method 29 Metals and Filterable Particulate Matter .. 5

2.2 Sampling Data for USEPA Method OTM 27/28 Filterable Particulate Matter Less 

Than 2.5 Microns and Condensible Particulate Matter .............................................. 6

2.3 Sampling Data for Mercury ........................................................................................ 7

3.0 Test Approach and Sampling Methods ............................................................................... 9

3.1 Sampling Strategy ....................................................................................................... 9

3.2 Sampling and Analytical Procedures .......................................................................... 9

3.2.1 USEPA Method 1 ............................................................................................. 9

3.2.2 USEPA Method 2 ........................................................................................... 11

3.2.3 USEPA Method 3A......................................................................................... 12

3.2.4 USEPA Method 4 ........................................................................................... 15

3.2.5 USEPA Method 29 ......................................................................................... 15

3.2.6 USEPA Method 30B ....................................................................................... 17

3.2.7 USEPA Other Test Method (OTM) 27 ........................................................... 19

3.2.8 USEPA Other Test method (OTM) 28 ........................................................... 22

3.3 Fuel Sampling and Analysis ..................................................................................... 26

3.4 Process Monitoring and Operating Loads................................................................. 27

4.0 Quality Assurance and Quality Control ............................................................................ 28

4.1 Quality Assurance Criteria ........................................................................................ 28

4.2 Blank Sampling Trains ............................................................................................. 31

4.3 Quality Assurance Objectives ................................................................................... 32

APPENDICES 

Appendix A – Field Data Forms 

Appendix B – Electronic Spread Sheets 

Appendix C – Example Calculations 

Appendix D – Analytical Data Enthalpy Analytical, OTM 27/28 

Appendix E – Analytical Data Pace Labs, Method 29 

Appendix F – Analytical Data Standard labs (fuel) 

Appendix G – Calibration Sheets, Certifications 

Appendix H – Process Data
 

Report ICR Testing June 30, 2010 

Kansas City Power & Light 1 CEC Project 100-208 

Sibley Generating Station 

1.0 PROJECT SUMMARY 

The United States Environmental Protection Agency’s (USEPA) Office of Air and Radiation 

(OAR) distributed a new Maximum Achievable Control Technology (MACT) Information 

Collection Request (ICR) to variety of new and existing coal- and oil-fired electric utilities. 

Under Part III of the ICR specific units are required to conduct stack emissions tests and submit 

the test results to USEPA using EPA's Electronic Reporting Tool (ERT) (Version 3). Kansas 

City Power & Light (KCP&L) operates four units that were required to test and report under the 

ICR. The facilities and the tests required to be conducted were: 

• Hawthorn Unit 5A - Acid Gas HAP (Hazardous Air Pollutants); Mercury and 

non-Mercury Metallic HAPs; and Non-Dioxin/furan organic HAPs. 

• La Cygne Unit 2 - Acid Gas HAP; Mercury and non-Mercury Metallic HAPs; and 

Non-Dioxin/furan organic HAPs. 

• Sibley Units 1, 2 and 3 - Mercury and non-Mercury Metallic HAPs. The Sibley 

units exhaust through a common stack and EPA has clarified the emissions testing 

will be conducted with all three units operating. 

• Lake Road Unit 6 - Mercury and non-Mercury Metallic HAPs. 

Civil & Environmental Consultants, Inc (CEC) was retained by KCP&L to provide the emissions 

testing services for the facilities listed in the ICR. This report discusses the sampling results for 

Sibley Generating Station Units 1, 2 and 3 located in Sibley, Missouri. 

1.1 TESTING APPROACH 

The first series of testing involved sampling the common stack for Units 1, 2 and 3 at the Sibley 

Generating Station. The testing program incorporated standard USEPA sampling protocols 

based on USEPA’s requested protocols for collecting information on Mercury and Non-mercury 

Metal HAPs. As defined in the ICR request, sampling for Mercury and Non-mercury Metal 

HAP’s consisted of sampling for mercury (Hg), metals, total filterable particulate, and particulate 

matter less than 2.5 microns, condensible particulate, oxygen (O2) and carbon dioxide (CO2). 

The USEPA also specified minimum sampling times, minimum sampling volumes, and which 

test methods need to be performed simultaneously. Table 1 lists the sampling protocols, 

minimum sampling times, and the units that the emissions data was reported in for the Mercury 

and Non mercury HAPs. 
 

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Kansas City Power & Light 2 CEC Project 100-208 

Sibley Generating Station 

*Also report scrubber recirculation liquid flow rate in liters/min and fuel feed rate in MMBTU/hr. 

For this test program CEC and KCP&L used the recommended method for the parameters listed 

in Table 1. 

Table 1 

Summary of Coal Electric Utility Steam Generating Unit Test Methods for Mercury 

 and Non-mercury Metallic HAP 

KCP&L ICR Sampling 

Sibley Generating Station

Pollutant Proposed Sampling Method Target Reported Units of 

Measure 

Hg U.S. EPA Method 30B. Use a minimum 

sample time of 2 hours per run. 

lb/MMBtu 

Metals U.S. EPA Method 29. Collect a minimum 

volume of 3.4 cubic meters and have a 

minimum sample time of 4 hours per run. 

Determine total filterable PM emissions 

according to §8.3.1.1. Use ICAP/MS for 

the analytical finish. 

lb/MMBtu 

PM2.5 (filterable) from 

stacks without entrained 

water droplets (e.g., not 

from units with wet 

scrubbers) 

U.S. EPA Other Test Method 27 (OTM 

27). Include cyclone catch as filterable 

PM. Collect a minimum volume of 3.4 

cubic meters and have a minimum sample 

time of 4 hours per run. 

lb/MMBtu 

PM2.5 (condensable) U.S. EPA Other Test Method 28 (OTM 

28). Collect a minimum volume of 3.4 

cubic meters and have a minimum sample 

time of 4 hours per run. 

lb/MMBtu 

O2/CO2

* U.S. EPA Method 3A % 

Moisture U.S. EPA Method 4 % 
 

Report ICR Testing June 30, 2010 

Kansas City Power & Light 3 CEC Project 100-208 

Sibley Generating Station 

1.2 PROJECT PARTICIPANTS 

The following personnel were involved in the execution of this project. 

Table 2 

Project Participants 

KCP&L ICR Sampling 

Sibley Generating Station

Participant Title Affiliation Contact 

Steve Brooks Plant Engineer 

Sibley 

Kansas City Power & 

Light 

Telephone: 

Lake Road - 816-387-6266 and 

Sibley - 816-650-2931. 

Email: Steve.Brooks@kcpl.com 

Christopher Dawdy Principal Civil & Environmental 

Consultants, Inc. 

Telephone: (314) 656-4566 

Facsimile: (314) 656-4595 

Email: CDawdy@cecinc.com

Franklin Stevens Project 

Manager 

Civil & Environmental 

Consultants, Inc. 

Telephone: (314) 656-4566 

Cell Phone: (314) 540-4622 

Facsimile: (314) 656-4595 

Email: FStevens@cecinc.com

Dan Cusac Sr. Technician Civil & Environmental 

Consultants, Inc. 

Nick Pichee Technician Civil & Environmental 

Consultants, Inc. 

AJ Anderson Technician Civil & Environmental 

Consultants, Inc. 

Joe Heilweck Sr. Technician Civil & Environmental 

Consultants, Inc. 

Bryan Tyler 

 

 

 

Air Sample 

Analysis Enthalpy Analytical, Inc. 

Telephone: 919/850-4392 x 250 

Fax: 919/850-9012 

Email: 

bryan.tyler@enthalpy.com

Steve Wilshire Coal Analysis Standard Laboratories 

Telephone: (618) 539-5836 ext. 115 

Fax: (618) 539-5839 

Email: swilshire@standardlabs.com

Scott Postma Observer USEPA Region 7 

Telephone: 

Fax: 

Email: postma.scott@epa.gov
 

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Kansas City Power & Light 4 CEC Project 100-208 

Sibley Generating Station 

1.3 SIBLEY GENERATING STATION 

Sibley Generating Station consists of three (3) Babcock & Wilcox cyclone boilers which are 

ducted to a common stack. Boiler #1 is a 1,300 PSIG, 950 °F/ 609.6 mmbtu/hr rated unit which 

serves Turbine #1 which has a gross 55 MW capacity. The boiler and turbine was installed in 

1960. Boiler #2 is the same as Boiler #1, except it was designed for a steam heat input of 627.3 

mmbtu/hr and was installed in 1962. It serves Turbine #2 which has a gross capacity rating of 51 

MW. Boiler #3 is a supercritical, 3,653 psig/1005 oF boiler with a design heat input of 4,094.1 

mmbtu/hour. The boiler serves Turbine #3 which has a gross capacity of 419 MW. This boiler 

and turbine was installed in 1969. The boilers burn a blend of coal typically 85% Powder River 

Basin (PRB) (sub bituminous) and 15% bituminous coal. Sibley #3 also burns tire derived fuel 

however normally this is less than 1% of the fuel being burned. Boilers #1 and 2 have burned 

biofuel in the past as a test burn but are not currently permitted for burning biofuel. 

Sibley Units 1 & 2 utilize electrostatic precipitators (ESP) over fire air (OFA) and selective noncatalytic reduction/rich reagent injection (SNCR/RRI) as pollution control devices. Sibley #3 

has an ESP, OFA and SCR for pollution control devices. 
 

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Kansas City Power & Light 5 CEC Project 100-208 

Sibley Generating Station 

2.0 DATA SUMMARY 

This section provides a summary of the test results. 

2.1 SAMPLING RESULTS FOR USEPA METHOD 29 METALS AND FILTERABLE 

PARTICULATE MATTER 

Tables 3 and 4 present a summary of the total filterable particulate matter and the metals 

sampling for the Sibley Generating Station. Three test runs were performed utilizing USEPA 

Method 29. The Method 29 sampling procedures are discussed in Section 3 of this report and the 

results of the QA/QC associated with the method are discussed in Section 4 of this report. 

Run1 has a smaller metals and particulate catch than runs 2 or 3. During Run 1, when moving 

the sampling train to the fourth port, it was noticed that the bottom of the last impinger had been 

broken. The run was stopped immediately and terminated at that point. The damage was likely 

caused by the high moisture conditions, long sample times and the resulting expansion of the 

silica gel. The run was accepted as a valid run since there was visible particulate catch on the 

filter. The results are consistent with the other runs. The final weight of the last impinger was 

estimated based on the moisture determinations of Runs 2 and 3, and the water catch in the first 

three impingers. 

Table 3 

Filterable Particulate Matter Data 

Sibley Generating Station

Run 1 Run 2 Run 3 Average 

Total Filter Catch (mg) 35.6 77.0 68.0 60.20 

Total Wash Catch (mg) 30.2 18.5 30.9 26.53 

Total Catch (mg) 65.8 95.5 98.9 86.73

PM Emission Rate (lbs/mmbtu) 

Run 1 Run 2 Run 3 Average 

Filterable PM Emission Rate 0.0091 0.0093 0.0092 0.0092 

Condensible PM Emission Rate* 0.0168 0.0203 0.0213 0.0195

Total PM** 0.0259 0.0296 0.0305 0.0287

*Condensible PM emissions determined by OTM-28 train and not corrected for blank values per 

discussions with ICR personnel 

**Total PM emission rate determined by combining filterable PM from M5/29 train and condensable 

 PM from OTM-27/28 train 

The results are very consistent validating the decision to accept the run as a valid run. To 

prevent this from happening on subsequent runs a small quantity of glass wool was placed 

beneath the silica gel to provide space for expansion should it occur. 
 

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Kansas City Power & Light 6 CEC Project 100-208 

Sibley Generating Station 

Table 4 

USEPA Method 29 Metals Data 

Sibley Generating Station

Metal 

Total Catch (ug)* 

Run 1 Run 2 Run 3 Average 

Antimony (Sb) 1.48 2.81 2.70 2.33

Arsenic (As) 11.57 20.00 19.46 17.01

Beryllium (Be) 0.33 0.54 0.55 0.47

Cadmium (Cd) 0.49 1.15 0.93 0.86

Chromium (Cr) 14.29 23.03 20.85 19.39

Cobalt (Co) 3.56 7.38 7.84 6.26

Lead (Pb) 12.62 23.40 25.36 20.46

Manganese (Mn) 15.85 23.74 24.74 21.44

Nickel (Ni) 15.86 28.72 22.83 22.47

Selenium (Se) 33.97 70.63 79.04 61.21

Metal 

Metals Emission Rate (lbs/mmbtu) 

Run 1 Run 2 Run 3 Average 

Antimony (Sb) 2.05E-07 2.74E-07 2.51E-07 2.43E-07

Arsenic (As) 1.60E-06 1.95E-06 1.81E-06 1.79E-06

Beryllium (Be) 4.58E-08 5.27E-08 5.11E-08 4.99E-08

Cadmium (Cd) 6.80E-08 1.12E-07 8.64E-08 8.89E-08

Chromium (Cr) 1.98E-06 2.25E-06 1.94E-06 2.06E-06

Cobalt (Co) 4.94E-07 7.20E-07 7.29E-07 6.47E-07

Lead (Pb) 1.75E-06 2.28E-06 2.36E-06 2.13E-06

Manganese (Mn) 2.20E-06 2.32E-06 2.30E-06 2.27E-06

Nickel (Ni) 2.20E-06 2.80E-06 2.12E-06 2.37E-06

Selenium (Se) 4.71E-06 6.89E-06 7.35E-06 6.32E-06

*Individual front and back half catch values can be found in appendices. 

2.2 SAMPLING DATA FOR USEPA METHOD OTM 27/28 FILTERABLE 

PARTICULATE MATTER LESS THAN 2.5 MICRONS AND CONDENSIBLE 

PARTICULATE MATTER 

To determine the emission rates for Filterable Particulate Matter less than 2.5 Microns in 

diameter (PM2.5) and Condensible Particulate Matter, three runs using USEPA Other Test 

Method (OTM) 27 and 28 were run simultaneously with USEPA Method 29. OTM 28 was 

combined with the OTM 27 sampling train. The procedure for operating the sampling train is 

discussed in Section 3 of this report, and the results of the QA/QC associated with the method 

are discussed in Section 4 of this report. 
 

Report ICR Testing June 30, 2010 

Kansas City Power & Light 7 CEC Project 100-208 

Sibley Generating Station 

Table 5 

Filterable Particulate Matter Less Than 2.5 Microns in Diameter (PM2.5) 

and Condensible Particulate Matter Results 

Sibley Generating Station

Filterable PM 

Filterable PM Catch 

Run 1 Run 2 Run 3 Average 

PM 2.5 Filter Catch (mg) 11.0 13.6 12.2 12.27 

PM 2.5 Wash Catch (mg) 0.8 1.5 1.1 1.13 

Total PM 2.5 Catch (mg) 11.8 15.1 13.3 13.40 

Total PM Catch (mg) 21.5 25.1 22.6 23.07

Filterable PM Emission Rate 

PM 2.5 Emission Rate (lbs/mmbtu) 0.0033 0.0043 0.0037 0.0038 

PM Emission Rate (lbs/mmbtu) 0.0061 0.0072 0.0063 0.0065

Condensible PM 

Condensible PM Catch (mg) 

Net organic Catch (mg) 3.50 4.90 5.70 4.70

Corrected Inorganic Catch (mg) * 55.80 66.40 70.60 64.27

Condensible Particulate Matter** 59.30 71.30 76.30 68.97

Corrected Condensible Particulate 

Matter* 57.40 69.30 74.30 67.00

Emission Rate Condensible PM 

Condensible Particulate Matter Emission 

Rate (lbs/mmbtu)** 0.0168 0.0203 0.0213 0.0195

Corrected Condensible Particulate Matter 

Emission Rate (lbs/mmbtu)* 0.0163 0.0197 0.0207 0.0189

 Total PM Emission Rate (lbs/mmbtu)*** 

Total PM ** 0.0229 0.0275 0.0276 0.0260

Corrected Total PM* 0.0224 0.0269 0.0270 0.0254

*Corrected based on the method and the results from the blank sampling train 

**Condensible PM not corrected for blank values per discussions with ICR personnel 

***Total PM emission rate determined by OTM27/28 

2.3 SAMPLING DATA FOR MERCURY 

Mercury was collected on paired Ohio Lumex high moisture carbon traps with a 100 ng spike on 

one tube per USEPA Method 30B. Three runs were completed using an Apex Instruments Merc 

6000 system for extracting the sample through paired carbon traps. One trap was spiked with 

100 ng of elemental mercury and the second trap was unspiked. The samples were collected 

over a 2 hour period and then analyzed on an Ohio Lumex 915+ with a thermal desorption 

device for removing the mercury from the carbon traps. The sample was collected from 12 

sampling points, 3 per port, at a constant sampling rate of approximately 500 ml/minute. 
 

Report ICR Testing June 30, 2010 

Kansas City Power & Light 8 CEC Project 100-208 

Sibley Generating Station 

Table 6 lists the tube identifications and the nanogram (ng) catch on each sorbent trap pair. 

Table 7 lists the mass emission rate in ng/l and lb/mmBtu for each tube and the average for the 

pair of tubes. The results of the QA/QC associate with the traps (percent recovery, breakthrough, 

tube agreement etc) are listed in Section 4 of this report. The detail description of the sampling 

approach can be found in section 3 of this report. 

Table 6 

USEPA 30B Mercury Results (ng) 

Sibley Generating Station 

No Description Tube ID Tube A/B 

Catch 

 ng 

Spiked 

(100 ng) 

STD 

Volume (l)

1 Run 1 A 68707 FH 68707 A 117 no 58.278

2 Run 1 A 68707 BH 1.7

3 Run 1 B 68534 FH Spike 68534 B 216 yes 56.695

4 Run 1 B 68534 BH 1.4

5 Run 2 A 68739 FH 68739 A 100 no 58.315

6 Run 2 A 68739 BH 0.3 

7 Run 2 B 68542 FH Spike 68542 B 186 yes 56.707

8 Run 2 B 68542 BH 0.7 

9 Run 3 A 68709 FH 68709 A 102 no 57.739

10 Run 3 A 68709 BH 0 

11 Run 3 B 65430 FH Spike 65430 B 191 yes 56.489

12 Run 3 B 65430 BH 1.2 

 

Table 7 

USEPA 30B Concentrations and Mass Emission Rates 

Sibley Generating Station 

Run Concentration 

Tube A 

ng/l 

Concentration

Tube B 

ng/l 

Average 

Concentration 

(ng/l) 

Tube A 

Emission 

Rate 

(lbs/mmBtu)

Tube B 

Emission 

Rate 

(lbs/mmBtu) 

Average 

Emission 

Rate 

(lbs/mmBtu)

1 2.04 2.07 2.05 1.48E-06 1.51E-06 1.49E-06 

2 1.72 1.52 1.62 1.25E-06 1.11E-06 1.18E-06 

3 1.77 1.61 1.69 1.27E-06 1.19E-06 1.23E-06 

Average 1.84 1.73 1.79 1.34E-06 1.27E-06 1.30E-06 

 
 

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Kansas City Power & Light 9 CEC Project 100-208 

Sibley Generating Station 

3.0 TEST APPROACH AND SAMPLING METHODS 

This section describes the sampling strategy, sampling and analytical methods, and quality 

assurance/quality control procedures that were implemented during this project. The project 

involved performing three (3) test runs for the parameters listed in Table 1 of this document at 

Sibley Generating Station in Sibley, Missouri. Sampling occurred on March 16 and 17, 2010. 

3.1 SAMPLING STRATEGY 

The USEPA methods that were utilized in this sampling program are: 

• Method 1 for the location of sampling ports and points, and determination of cyclonic flow; 

• Method 2 for velocity and volumetric flow rate determination; 

• Method 3A for the determination of dry molecular weight of the stack gas; 

• Method 4 for the determination of moisture in the stack gas; 

• Method 29 was used to determine concentrations and emission rates of non-mercury metals 

(antimony (Sb), arsenic (As), beryllium (Be), cadmium (Cd), chromium (Cr), cobalt (Co), 

lead (Pb), manganese (Mn), nickel (Ni), and selenium (Se)) and filterable particulate matter; 

• Method 30B was used for the determination of mercury (Hg) emissions; 

• Other Test Methods (OTM) 27 and 28 was used to determine filterable particulate matter 

less than 2.5 microns in diameter and condensible particulate matter, respectively. 

All methods were performed simultaneously during each test run. These test methods are available 

in the Code of Federal Regulations Volume 40, Part 60, US EPA’s web site www.epa.gov/ttn/emc/

or by request from CEC. 

3.2 SAMPLING AND ANALYTICAL PROCEDURES 

A sampling and analysis synopsis for these methods is discussed briefly in the following sections. 

3.2.1 USEPA Method 1 

USEPA Method 1 was used for this test program to determine the appropriateness of the existing 

ports as sampling locations and to determine the number of sampling points to be used when 

sampling at these locations. 

The duct diameters upstream and downstream from the sampling ports were determined based on 

the sampling port location. For particulate and flow traverses, Method 1 specifies that a minimum 

number of 12 traverse points can be used for stacks greater than 24 inches in diameter if the ports 

are located >8 stack diameters downstream and >2 stack diameters upstream from any flow 

disturbances and 24 traverse points when located >2 diameters downstream and >0.5 diameters 

upstream. These exact distances up and downstream from disturbances were determined during the 

initial set-up day at the site and the ratio of the distances to the diameter of the stack were used in 

conjunction with Figure 1 to determine the number of sampling points to be used during the testing. 
 

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Kansas City Power & Light 10 CEC Project 100-208 

Sibley Generating Station 

At Sibley generating station both the upstream and downstream distances from the port location was 

greater than 8 stack diameters which meant that the minimum of 12 sampling points (3 per port) 

could be used at the sampling location. The coupling length was 7 inches and the sampling points 

were located at 14.1, 30.7 and 55 inches into the port from the outside edge of the port coupling. 

Figure 1: Sampling Point Determinations 

After determining the number of sampling points, a Type “S” pitot tube such as the one defined in 

USEPA Method 2 was used to determine if cyclonic flow conditions existed at the sampling 

location. If the flow conditions at a sampling location are parallel or near parallel to the stack walls 

(< ± 20o

) then the location can be used to determine pollutant concentrations using isokinetic 

sampling methods. 

CEC leveled and zeroed the manometer and connected a Type “S” pitot and leak-checked the 

system. The pitot tube was positioned at each traverse point, in succession, so that the planes of the 

face openings of the pitot tube were perpendicular to the stack cross-sectional plane. This position 

was referred to as the"0o reference point." The differential pressure (Δp) reading at each traverse 

point was recorded. If a zero reading was obtained the angle of flow was recorded as 0o

. If the pitot 

50

40

30

20

10

0.5 1.0 1.5 2.0 2.5

0

2 3 4 5 6 7 8 9 10

B

A

Disturbance

Measurement

Site

Disturbance

Duct Diameters Downstream from Flow Disturbance* (Distance B) 

Stack Diameter = 0.30 to 0.61 m (12 - 24 in.) 

Duct Diameters Upstream from Flow Disturbance (Distance A) 

a Higher Number is for

 Rectangular Stack or Ducts

16

12

8 or 9 a

* From Point of Any Type of Disturbance

 (Bend, Expansion, Contraction, etc.)

Stack Diameter > 0.61 m (24 in.) 

Minimum Number of Traverse Points

20

24
 

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reading was not zero, the pitot tube was rotated until a null reading was obtained. The value of the 

rotation angle was determined to the nearest degree using a digital angle finder. After this technique 

had been applied at each traverse point, the average of the absolute value of the angles was 

determined. The average angle was ≤ 20o and the overall flow condition in the stack was found to 

be acceptable. This procedure was conducted in conjunction with the preliminary flow 

determinations using USEPA Method 2 which is discussed in the next section. 

3.2.2 USEPA Method 2 

After determining the appropriate number of sampling points and conducting the cyclonic flow 

check, USEPA Method 2 was used to perform velocity measurements of the flue gas in the stack. 

Preliminary velocity measurements were made to determine the appropriate nozzle size to use to 

maintain isokinetic sampling rates during the sampling. Velocity measurements were performed 

concurrently, while collecting the samples, to ensure the samples were collected isokinetically and 

to determine the pollutant concentrations and mass emission rates. 

The stack gas velocity was determined from the measurement of the velocity head at each 

traverse point with a calibrated Type "S" pitot tube connected to an inclined manometer (Figure 

2). Measurement of the stack gas temperature was made with a calibrated Type "K" 

thermocouple, and determination of the stack gas composition was made using USEPA 

Method 3A (Section 3.2.3). 

CEC made measurements of the face opening alignments, external tubing diameter, and base-toopening plane distances of the pitot tubes prior to coming to site These measurements meet the 

design criteria in USEPA Method 2 for an Type “S” pitot tube, therefore a baseline coefficient 

value of 0.84 inches was assigned to the pitot tube. Verification of these measurements were 

recorded onto a pitot tube calibration worksheet and presented in Appendix G. Once the 

measurements of the pitot tube were completed, the method 2 train was assembled and leak 

checked prior to conducting velocity measurements. 
 

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Kansas City Power & Light 12 CEC Project 100-208 

Sibley Generating Station 

Figure 2: Velocity Measurements System 

In addition to the velocity head measurements, USEPA Method 3A (Section 3.2.3) was used to 

determine O2 and CO2 concentrations in the flue gas in order to calculate the flue gas molecular 

weight. The measurement was made in order to complete the preliminary velocity calculations 

necessary to establish the sampling conditions for the actual pollutant measurements. 

3.2.3 USEPA Method 3A 

Method 3A was used for determining O2 and CO2 concentrations and dry molecular weight of a 

sample from the outlet of the boiler system. CEC used a California Analytical Model 600P 

O2/CO2 paramagnetic and non-dispersive infrared analyzer with a range of 0-25 percent for O2

and CO2. 

Due to the magnetic properties of O2, the analyzer utilizes the phenomenon of Para-magnetism to 

measure O2 in the sample stream and generates a proportional electrical current. The sensor consists 

of two sealed spheres at each end of a bar forming a dumbbell. The dumbbell is suspended in a 

symmetrical non-uniform magnetic field. Being slightly diamagnetic, the spheres are pushed away 

from the most intense part of the magnetic field. When the gas surrounding the spheres contains O2, 

the spheres are pushed further out of the field by the relatively stronger paramagnetic O2. 

The transducer incorporates a strong metal band suspension mechanism mounted to the dumbbell. 

In the zero position (O2 free gas) light is reflected from an attached mirror to a photocell. In the 

feedback loop, when O2 is present, a current was sent through the suspension system creating an 

electromagnetic counter torque. This torque restores the mirror to a position so that the photocell 

7.62 cm (3 in.)* Temperature Sensor

1.90 - 2.54 cm*

(0.75 - 1.0 in.)

Type S Pitot Tube

Manometer Leak-Free Connections

* Suggested (Interference Free)

 Pitot tube/Thermocouple Spacing
 

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Kansas City Power & Light 13 CEC Project 100-208 

Sibley Generating Station 

again detects the light. The amount of restoration required is related to the O2 concentration. The 

current simultaneously generates an output signal of 0-10 volts (V) which corresponds to 0-25% O2

that was recorded by the data acquisition system. 

The CO2 concentration in the effluent was measured by a non-dispersive infrared (NDIR) micro 

flow detector to measure CO2 in the sample stream and generates a proportional electrical current. 

A single infrared light beam is modulated by a chopper and passed through a sample cell of 

predetermined length containing the gas sample to be analyzed. As the beam passes through the 

cell, the sample gas absorbs some of its energy. 

The attenuated beam emerges from the cell and is introduced to the front chamber of a two-chamber 

infrared detector. The detector was filled with the component of interest and consequently the beam 

experiences further energy absorption. The absorption process increases the pressure in both of the 

chambers. The differential pressure between the front and rear chambers of the detector causes a 

slight gas flow between the two chambers. The flow is detected by a mass-flow sensor and is 

converted into an AC electrical signal. This is amplified and rectified into a DC voltage signal 

which was recorded by the data acquisition system in a percent range of 0 to 10V. The electrical 

output signal was directly proportional to the concentration of the sample gas. 

The collected sample is split by the analyzer using critical orifices and passed through the 

appropriate analyzer. This configuration prevents the system from being pressurized and biasing 

the sample results. Figure 3 presents a diagram of the Method 3A sampling system. 

An analyzer calibration error test was run, prior to sampling using a high-, mid-, and low-level gases 

O2/CO2 certified gas mixture with a balance of nitrogen. After the system had been calibrated, the 

mid-level cal gas was delivered to the probe tip and transported to the analyzer to determine the 

response time for the analyzer system configuration and to determine if the system had any biases 

that would affect the sample results. 

The electrical output response signal from the analyzer was recorded with a STRATA Version 

2.01 data acquisition system. The gas sample was continuously extracted from the stack and 

transported to the analyzers via a heated Teflon® sample line. The effluent gas sample from the 

stack flowed through the Teflon® tubing to a condenser where the water vapor was removed. 

The gas sample was transported to the analyzer’s inlet at a constant flow rate and pressure. The 

system response time was determined and recorded. 

An analyzer calibration error test was performed on the O2 analyzer by introducing a zero, mid 

and high-range calibration gas to the gas analyzer inlet. No adjustments were made to the 

analyzer. A zero gas (nitrogen) concentration of less than 0.25% of span, a certified Protocol-1 

mid range gas (40-60% of span) and a certified Protocol-1 high-range gas (100% of span) was 

used for the O2 analyzer calibration error test. 
 

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A sample system bias check was also performed on the analyzer sampling system by introducing 

a zero and a mid-range calibration gas at the calibration valve that is installed on the end of the 

sampling probe. The sampling system was operated at the normal sampling rate and no 

adjustments were made to the measurement system. 

The acceptance criteria for the analyzer used in this test program was as follows: 

• Calibration Error - Less than +2% of Calibration Span for the zero, mid, and high cal 

gases. 

• System Bias - Less than +5% of Calibration Span for the zero, mid, and high cal gases. 

• Zero Drift - Less than +3% of Calibration Span over the period of each test run. 

• Calibration Drift - Less than +3% of Calibration Span over the period of each test run. 

Figure 3 presents a basic diagram of a method 3A sampling system. 

Figure 3: USEPA Method 3A Sampling System 

The CEM sampling was conducted concurrently with the other pollutant measurements for an 

equal amount of time at the point of average velocity during each test run from a single test port. 

Heated 

filter 

Sample manifold

Calibration Gases 

Sample 

Pump 

Bypass 

Heated 

Line 

Sample line 

Stack 

System Calibration / 

Bias Line 

O2 CO2

DAS 

Computer 

Heated probe 

Universal Sample 

Conditioner 

Atmospheric 

Dump 
 

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3.2.4 USEPA Method 4 

The Method 4 sampling train was incorporated into the Method 29 sampling train for this test 

program. The moisture content of the sample gas stream was determined by extracting the gas 

sample at a known and regulated rate through a glass condenser train consisting of four glass 

impingers connected in series with leak-free glass u-tube connectors. The gas sample was 

extracted through the impinger train maintained below 68 degrees Fahrenheit (°F) in an ice bath 

with a vacuum pump. The volume of gas sampled was measured with a calibrated dry gas meter. 

The volume of moisture collected was measured gravimetrically with an analytical balance with 

a tolerance of 0.1 gram (g) and the volume of gas drawn, was corrected to dry standard 

conditions (528 oR, 29.92 in. Hg). 

3.2.5 USEPA Method 29 

Emissions testing for antimony (Sb), arsenic (As), beryllium (Be), cadmium (Cd), chromium (Cr), 

cobalt (Co), lead (Pb), manganese (Mn), nickel (Ni), and selenium (Se) and filterable particulate 

matter were performed according to US EPA Method 29. Since mercury (Hg) was sampled and 

analyzed using a separate procedure (Method 30B), the impingers containing potassium 

permanganate, 5th and 6th impingers were not used for this test program, per Section 6.1.5 of 

USEPA Method 29. For the metal sampling per Method 29 the minimum sample volume was 3.4 

cubic meters and a minimum sampling time of four (4) hours was used for each sampling run. 

Method 29 was used to collect gaseous and particulate pollutants isokinetically from the emission 

source and collect them in a multi-component sampling train. Particulate matter was collected on a 

tared quartz fiber filter. The gaseous components were then aspirated through a measured volume 

of 5% nitric acid/10% hydrogen peroxide to determine the moisture and multiple metal content of 

the emission source. The principal components of the sampling system are: 

1. Pitot Tube Assembly

a. Nozzle--Borosilicate glass with a sharp, tapered leading edge. 

b. Probe--Stainless steel sheath with a 5/8-inch diameter quartz glass insert wrapped with 

nichrome wire; electronically controlled and capable of maintaining 248 ± 25 oF with 

calibrated Type "K" thermocouple. 

c. Pitot--Calibrated stainless steel Type "S" pitot tube constructed and attached to probe 

according to specifications outlined in USEPA Method 2, 40 CFR 60. 

d. Thermocouple--Calibrated Type "K" thermocouple attached to the sample probe such 

that the tip has no contact with metal and does not interfere with the pitot tube face 

openings and the sample nozzle. 

e. Glass filter housing--with a Teflon frit filter support with a quartz fiber filter. 

2. Impingers

Four impingers connected in series with glass ball/socket joint fittings and placed in an ice bath 

were used for these tests. The second impinger was a Greenburg-Smith design with a standard 
 

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orifice tip. The first, third and fourth impingers were the modified Greenburg-Smith design. 

Final gas exit temperature was measured with a calibrated Type "K" thermocouple immersed in 

the gas stream. 

3. Control Box

This control box is a module containing vacuum gauge, external leak-free pump, and 

thermocouple capable of measuring temperature within ±5 ° F, and dry gas meter with a 

minimum of 2 percent accuracy, valves and related equipment to determine sample gas volume. 

Figure 4 presents the standard Method 29 sampling train with the mercury impingers and an 

extra knockout impinger up front that were not used during the sampling at Sibley. 

Figure 4: USEPA Standard Method 29 Sampling Train 

The sampling train was assembled, as previously described, ice was added to the impinger portion 

of the train, and the probe and hot box was heated to 248 ± 25 oF. Once the train was heated, the 

system was leak checked. A leak rate less than 0.02 cubic feet per minute (cfm) was determined 

and considered acceptable as outlined in 40 CFR 60. Once the sampling train passed the leak 

check, it was placed in the stack for sampling. 

The train was run for the minimum of 4 hours. After each test run, the filter, which collected the 

particulate sample, was carefully removed from the Teflon filter support and sealed in a petri dish. 

The nozzle, probe liner, and front filter-half of the filter assembly were rinsed with 0.1N nitric acid 

into a 500 milliliter amber glass storage container. 
 

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The liquid in the first two impingers were measured to the nearest tenth of a milligram. The 

collected sample was stored in a one liter amber glass storage container along with three 0.1N nitric 

acid rinse of the impingers and connecting glassware. The container was sealed and the liquid level 

marked. The contents of the third impinger were measured to the nearest tenth of a gram. The 

collected sample along with a 100 milliliter 0.1N nitric acid rinse of the impinger was stored in a 

250 ml amber glass storage container. The container was sealed and the liquid level marked. The 

volume of the moisture collected by the silica gel in the fourth impinger was determined to the 

nearest 0.1 gram per Method 4. Collected condensate measurements were recorded on the Method 

29 moisture determination data analysis form. 

These samples and filters were shipped to the laboratory, along with the appropriate chain of 

custody documentation. Samples, method blanks and spiked samples were weighed, digested, 

prepared and analyzed according to EPA Method 29 protocol. Samples were analyzed for metals 

on a PerkinElmer ELAN 6100 inductively coupled argon plasma emission spectroscopy/mass 

spectrometry (ICP-MS) or similar instrument. The metals analysis was performed by Pace 

Analytical located in Minneapolis, MN. 

3.2.6 USEPA Method 30B 

Method 30B is a self validating sampling procedure for measuring total vapor phase mercury 

(Hg) emissions from coal-fired combustion sources using sorbent trap sampling and subsequent 

analysis using thermal desorption. This method is designed to measure the mass concentration of 

total vapor phase Hg in flue gas, including elemental Hg (Hgo

) and oxidized forms of Hg (Hg+2), 

in micrograms per dry standard cubic meter. Known volumes of flue gas are extracted from the 

stack through paired, in stack sorbent media traps at a constant flow rate. By collecting the 

mercury on the sorbent media in the stack, potential loss of mercury during transport through a 

probe/sample line is eliminated. 

For each test run, paired train sampling was performed to allow for the determination of 

measurement precision and verify acceptability of the measured emissions data. A field recovery 

test was performed with each run to determine measurement bias and to verify data acceptability. 

The Method 30B sampling tubes were 6mm, 2-section sorbent traps containing halogenated 

carbon. CEC used sorbet traps supplied by Ohio Lumex which contained an iodated carbon for 

the mercury sampling at Sibley. For quality-assurance purposes, the back section of one of the 

paired sorbent traps was spiked with Hgo by Ohio Lumex. This section was analyzed separately 

and a specified percentage of the spike must be recovered for the method to be valid. All three 

runs meet the spike recovery criteria in the method. 

As part of the Method 30B QA/QC, CEC performed a Bias Test on the mercury analyzer prior to 

sampling on site. The Method 30B Bias Test is required in order to show that the analytical 

instrument is able to measure both elemental and oxidized mercury without bias. During the bias 

test three sorbent traps are spiked with elemental mercury at each of two levels (three low levels 

and three high levels between which actual samples are expected to fall). The sampling tubes are 

analyzed to demonstrate instrument accuracy in quantifying elemental mercury. Then, two sets 
 

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of three standards are made with aqueous mercury solutions and analyzed at the same mercury 

levels as the sorbent traps. As the water evaporates during analysis, for a short instance, the 

mercury exists as a mercury salt (oxidized mercury) until it is then broken down thermally and 

measured. 

The USEPA has established minimum sample run times for the Method 30B sampling to be 

performed under the ICR. For the Hg sampling per Method 30B the minimum sample time of two 

(2) hours was used for each sampling run. The Method 30B sampling train consisted of: 

• A heated sampling probes capable of holding paired Method 30B sorbent traps; 

• A heated umbilical; 

• A moisture knockout; 

• An umbilical to connect the control console to the knockout and probe assembly; 

• Control console containing heater controls, mass flow controllers, thermocouple readouts, 

heater controls for the heated umbilical and probe, dry gas meter and data acquisition 

system. Figure 5 presents a flow diagram for the USEPA Method 30B sampling system. 

Figure 5: USEPA 30 B Sampling System Diagram 

Paired Method 30B sorbent traps were loaded into the sample probes, leak checked and placed in 

the stack. One sorbent trap was spiked and the other unspiked. Flue gas was pulled through the 

paired sampling tubes for 2 hours at a sampling rate of ~500 ml/minute. At the completion of 

sampling, the probe was removed from the stack and a post leak check was performed. The 

tubes were removed, capped and taken to the mobile lab for analysis. 
 

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An Ohio Lumex RA 915+ mercury analyzer with a RP-M324 thermal desorption attachment was 

used to analyze the carbon sorbent traps. The 915+ uses differential atomic absorption 

spectrometry to determine the mercury that is thermally desorbed from the sampling tubes. The 

system was calibrated using the following procedure: 

• The furnace is powered on and operated on Profile 1 mode which sets and holds the 

temperature at 680o

C. The sample flow is set at 2 liter/minute. The lamp is ignited and 

the system was given 1 hour to warm–up and stabilize. 

• The system was then calibrated using the three calibration points which were determined 

based on the anticipated mercury catch. The r2

 was determined for the calibration curve 

and when it met method criteria and the standards were within ±10% of their true value, 

the samples were analyzed. 

The samples will be analyzed as follows: 

• Two layers of clean aluminum foil were placed on top of a clean sheet of white copier 

paper. A quartz ladle was placed on top of the second layer of aluminum foil. A second 

piece of aluminum foil was laid beside the ladle for wrapping the glass wool plug from 

the first layer of the trap. 

• A blank sample was the first sample analyzed on the instrument to establish a background 

Hg level. 

• The samples were prepared for analysis after the blank, by removing the first glass wool 

plug which is wrapped in aluminum foil and placed in the ladle on top of the carbon from 

the first section of the sorbent tube which was poured into the ladle. A final inspection of 

the tube was performed to ensure that there were no visible signs of carbon remaining in 

the first section of the sorbent tub. Carbon that is deposited on the aluminum foil as a 

result of sample preparation is carefully poured into the ladle. 

• The carbon and aluminum foil containing the glass wool plug was placed in the ladle and 

covered with sodium carbonate and placed in the furnace for analysis. The analysis was 

initiated as the ladle was placed in the furnace. 

• The aluminum foil covering the sample preparation area was removed along with the 

plain white paper and a new set placed down for each section of the traps. The carbon and 

glass wool from the second layer was removed and placed in the ladle as previously 

described and analyzed. 

• Each subsequent sample was handled following the same procedure. 

• A calibration check sample, using a secondary standard, was prepared and analyzed 

before and after the samples to verify the system performance. 

3.2.7 USEPA Other Test Method (OTM) 27 

The USEPA OTM 27 was used to measure particulate matter emissions equal to or less than a 

nominal aerodynamic diameter of 2.5 micrometer (PM2.5). USEPA’s concern under the current 

ICR was the determination of PM2.5 emissions. To facilitate the sampling during this test 
 

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program, the OTM 27 sampling train was run without the PM10 cyclone. This approach is 

allowed under the method (see Section 2.1). 

The USEPA has established minimum sample volumes and run times for the PM2.5 sampling to 

be performed under the ICR. For the PM2.5 sampling per OTM 27, the minimum sample volume 

is 3.4 cubic meters and a minimum sampling time of four (4) hours for each sampling run. The 

nominal sampling time was used to as the primary driver. Based on historical PM data it was 

determined that 4 hours would meet EPA’s primary goal of ensuring an adequate catch to ensure 

the methods accuracy. 

The sampling train consists of: 

• Stainless steel (316 or equivalent) or Teflon®-coated stainless steel nozzles with a sharp 

tapered leading edge; 

• A PM2.5 sizing devices that meets the design specifications shown in Figures 3, 4, 5, and 

6 of Section 17 of Method OTM 27; 

• A stainless steel (316 or equivalent) or Teflon®-coated stainless steel, in-stack filter 

holder, 47 mm in diameter; 

• Stainless steel pitot tube attached to the probe with stainless steel fittings per the 

specifications in Section 6.1.1.3 of Method 5; 

• A glass lined stainless steel probe; A metering system capable of maintaining a semiisokinetic sampling rate and accurately determining the sample volume according to 

specifications in APTD-0581. 

Figure 6 presents a schematic of the standard OTM 27 sampling train. For this test program the 

sampling train back half was replaced with the OTM 28 back half and the PM2.5 sampling head 

was used without the PM10 sampling head. The sampling train was assembled per the method 

with the noted exceptions and the system leak checked. The entire assembled sample system 

was leak-checked by plugging the inlet to the probe nozzle and pulling a vacuum of at least 

15 in. Hg. A leak rate less than 0.02 cubic feet per minute (cfm) was determined and considered 

acceptable as outlined in 40 CFR 60. 
 

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Figure 6: USEPA OTM 27 Sampling Train 

The PM2.5 sampling head was wrapped with a heat strip to preheat the sampling head to a 

temperature close to the stack temperature to prevent the formation of condensation when the 

sampling head was placed in the hot flue gas. The sampling was performed per the method and at 

the completion of the test run the sampling head was removed from the stack, the system post 

leak checked (without the PM2.5 sampling head) and the nozzle was covered with Teflon to 

prevent the loss of particulate matter. The head was delivered to the sampling trailer for 

recovery. 

Once in the sampling trailer, recovery of the sample began. Recovery involves the quantitative 

transfer of particles > 2.5 micrometers; and ≤ 2.5 micrometers. A Nylon or Teflon® brush and an 

acetone rinse are used to recover the sample head. 

• Tweezers and/or clean disposable surgical gloves were used to remove the filter from the 

filter holder. The filter was placed in the petri dish that was identified as Container #1. 

Using a dry Nylon bristle brush, any particulate matter and/or filter fibers that adhere to 

the filter holder gasket or filter support screen were transferred to the petri dish and the 

container was sealed. 

• The particulate matter from the cyclone cup and acetone rinses (and brush cleaning) of 

the cyclone cup, internal surface of the nozzle, and cyclone internal surfaces, including 

the outside surface of the down comer line were quantitatively recovered. The particulate 

from the cyclone cup and the acetone (and brush cleaning) rinses of the cyclone cup were 

placed into Container #2. The container was sealed and the liquid level was marked on 

the outside. This container holds the particulate matter > 2.5 micrometers. This container 

was archived since the filterable PM is being determined with the Method 29 sampling 

train. 
 

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• Acetone rinse (and brush cleaning) of the internal portion of the exit tube of PM2.5

cyclone and the front half of the filter holder was placed into in container #3. The 

container was sealed and the liquid level was marked on the outside of the container. 

• An acetone blank (100 ml) was placed into container #4. 

The samples were shipped to the laboratory for analysis after the completion of sampling. The 

samples were analyzed using gravimetric analysis to determine the particulate mass for each PM 

size fraction based on the method. The recovery of the sample probe and back half of the 

sampling train are discussed with USEPA OTM 28, in section 3.2.8 of this document. 

3.2.8 USEPA Other Test method (OTM) 28 

USEPA OTM 28 was utilized to measure condensable particulate matter (CPM) emissions in the 

flue gas. This method includes procedures for measuring both organic and inorganic CPM. CPM 

is measured in the flue gas after passing through a filter, or in this case after passing through the 

cyclone and in-stack filter. The OTM 28 sampling train was the back half of the OTM 27 

sampling train. 

The OTM 28 sampling train consisted of: 

• Method 23 type condenser and a condensate dropout impinger without bubbler tube after 

the final out-of-stack hot filter assembly; 

• The dropout impinger is followed by a modified Greenburg Smith impinger with no taper; 

• A filter holder with a Teflon® filter meeting the requirements in Section 6.1.2 will be placed 

immediately following the modified Greenburg-Smith impinger. The connection between 

the CPM filter and the moisture trap impinger includes a thermocouple fitting that provides a 

leak-free seal between the thermocouple and the stack gas;

• A Greenburg Smith impinger containing 100 ml of water followed by an impinger containing 

silica gel to collect moisture that passes through the CPM filter.

A pretest leak-check was performed and a leak rate of not more than 0.02 actual cubic feet per 

minute (acfm) or 4 percent of the average sample flow during the test run, whichever is less was 

considered acceptable per the method. The leak-check was performed at a vacuum equal to or 

greater than the vacuum anticipated during the test run. The first two impingers of the sampling 

train were maintained separately from the back two impingers. The first two impingers were 

kept in a dry compartment at a temperature less than 85o

 F. The second 2 impingers (after the 

CPM filter) were maintained at a temperature of less than 68o F. Figure 7 present a diagram of 

the OTM 28 sampling train. 
 

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Figure 7: USEPA Method OTM 28 Sampling Train 

Once the run was completed the sampling train was leak checked from the probe back. The leakcheck was performed and a leak rate of not more than 0.02 actual cubic feet per minute (ACFM) or 4 

percent of the average sample flow during the test run, whichever is less was considered acceptable 

per the method. The leak-check was performed at a vacuum equal to or greater than the highest 

vacuum measured during the test run. 

Once the leak check was completed the probe, any cyclones, and in-stack or hot filters were 

detached from the condenser and impinger train. The short stem impinger was emptied into a 

modified Greenberg Smith impinger which was inserted in front of the short impinger. The 

impinger tip length extended below the water level in the impinger catch. 

The purge line was attached to a purged inline filter with no flow of gas through the clean purge 

line and fittings. The filter outlet was connected to the inlet of the impinger train. The nitrogen 

gas flow was started slowly while simultaneously opening the meter box pump valve(s). The 

pump bypass was adjusted and the nitrogen delivery rate changed to obtain the following 

conditions: (1) 20 liters/min or ΔH@, and (2) a positive overflow rate through the rotameter of 

less than 2 liters/min. The condenser operation and recirculating water was continued during the 

purge to maintain a temperature less than 85o F at the exit of the CPM filter. Ice was left in the 

water bath for the last two impingers to prevent removal of moisture during the purge and to 

maintain the gas temperature measured at the exit of the silica gel impinger below 20°C (68°F) 

until the sample recovery began. 
 

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The purge was continued for a period of one hour checking the rotameter and ΔH@ periodically 

to ensure the purge rate had not changed. After 1 hour the pump and the purge gas were stopped 

simultaneously. 

After the purge was complete, recovery of the sample train began: 

• CPM Container #1, Aqueous Liquid Impinger Contents. Quantitatively transferred liquid 

from the dropout and the impinger prior to the CPM filter into a clean glass sample 

bottle; 

• Rinsed the probe extension, condenser, each impinger and the connecting glassware, and 

the front half of the CPM filter housing twice with water. Recovered the rinse water, and 

added it to the same sample bottle. Marked the liquid level on the bottle. CPM 

Container #1 held the water soluble CPM captured in the impingers; 

• CPM Container #2, Organic Rinses. Followed the water rinses of the probe extension, 

condenser, each impinger and all of the connecting glassware and front half of the CPM 

filter with an acetone rinse. Then repeated the entire procedure with two rinses of MeCl2,

and saved both solvents in a separate glass container identified as CPM Container #2. 

Marked the liquid level on the jars; 

• CPM Container #3, CPM filter sample. Used tweezers and clean disposable surgical 

gloves to remove the filter from the CPM filter holder. Placed the filter in the petri dish 

identified as CPM Container #3; 

• The non CPM impinger water and the silica gel impinger were weighed in the field and 

discarded.

The samples were sent to the laboratory for processing and analysis. The lab analysis procedure 

followed the flow diagram in Figure 8. 
 

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Figure 8: Analytical Flow diagram for OTM 28 

The OTM 27/28 analysis was performed by Enthalpy Analytical located in Durham, NC. 
 

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3.3 FUEL SAMPLING AND ANALYSIS 

The fuel sampling requirements were defined in the discussion in the Supporting Statement Part 

B of the ICR. The fuel sampling requirements for this test are listed in Table 8 below. Each fuel 

sample was a composite sample which consisted of three samples collected at approximately 

equal intervals during the four hour testing period. 

Table 8 

ICR Required Fuel Analyses 

KCP&L ICR Sampling 

Sibley Generating Station

Mercury and 

non-mercury 

metallic HAP 

antimony, arsenic, beryllium, cadmium, chromium, cobalt, lead, manganese, 

mercury, nickel, selenium, chlorine, and provide the HHV and proximate/ultimate 

analyses of the coal being utilized during the test 

The fuel sampling at Sibley was performed from the feeders on the three boiler units exhausting 

into the common stack. The sampling was performed utilizing procedures similar to those in 

ASTM D2234/D2234M. Unit 3 at Sibley has eight sampling points on the feeder and Units 1 

and 2 have four sampling points each. The sampling locations are on the bottom of the coal 

chute for each of the coal feeders. Each sampling location consisted of a ball valve with a two 

inch diameter pipe nipple. The valve was opened, purged for 1 minute and a 2 pound (lb) coal 

sample collected at each location. This procedure was conduted three times over equally spaced 

intervals during each four hour emissions test, resulting in a total of 96 lbs of coal being 

collected during each flue gas emission test run. The 96 lb sample was composited into a single 

sample for analysis at the lab based on the procedures in ASTM D2013/D2013M which 

addresses reducing and dividing the gross sample into a mass suitable for the laboratory. 

 

Table 9 outlines the approved analytical methods for analyzing fuel samples. The laboratory 

being utilized for the fuel analysis used the methods presented in Table 9 or an equivalent 

method. 
 

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Table 9 

Fuel Analysis Methods 

KCP&L ICR Sampling 

Sibley Generating Stations

Analyte Fuel 

Type Method Target Reported Units of Measure 

Sample Preparation - Lab Coal ASTM D2013 Sample prep 

Higher Heating Value Coal ASTM D5865–04, Btu/lb 

Moisture Coal ASTM-D3173-03/3303 % 

Mercury Concentration Coal ASTM D6722-01 Ppm 

Total Selected Metals 

Concentration Coal 

ASTM D6357-04 for arsenic, 

beryllium, cadmium, 

chromium, lead, manganese, 

and nickel in coal 

ASTM D4606-03 for Se 

ppm 

Chlorine Concentration Coal ASTM D6721-01 ppm 

All fuel analysis was performed by Standard Laboratories Freeburg Lab - Illinois Division 

Office located in Freeburg, IL. 

3.4 PROCESS MONITORING AND OPERATING LOADS 

Coal fired utilities are expected to operate at ninety (90 %) of maximum capacity for the testing 

required under the ICR. The facility provided operating data on the Unit Load (MW), net 

generation during each test run (MWh net), fuel feed rate and steam load of each run. 
 

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4.0 QUALITY ASSURANCE AND QUALITY CONTROL 

4.1 QUALITY ASSURANCE CRITERIA 

CEC has established quality assurance and quality control (QA/QC) guidelines for providing quality 

sampling and analytical data from source tests. These QA/QC procedures were implemented to 

ensure the acceptability and reliability of the data generated. 

For the measurement of O2/CO2 utilizing a continuous emission monitor there are four primary 

criteria used to determine the methods performance: 

• Zero Drift - Less than ±3 percent of the span value 

• Calibration Drift - Less than ±3 percent of span value 

• Calibration Error - Less than ±5 percent of the calibration gas value 

• System Bias Check - Less than ±5 percent of the calibration gas value 

Table 10 

Calibration Error Test O2/CO2 

Sibley Generating Station

Date/Time 3/16/2010 7:20:41 

Analyte O2 CO2 

Units % % 

Zero Ref Cyl 0 0 

Zero Avg -0.009 0.001 

Zero Error% 0 0 

Low Ref Cyl 5.486 5.469 

Low Avg 5.437 5.431 

Low Error% 0.2 0.1 

Mid Ref Cyl 14.99 14.9 

Mid Avg 14.969 14.917 

Mid Error% 0.1 0.1 

High Ref Cyl 21.92 21.73 

High Avg 22.127 22.082 

High Error% 0.8 1.2 

 
 

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All calibration error and bias test met the method criteria. 

For the particulate matter measurements of particulate matter less than 2.5 microns there are a 

number of the method performance criteria the method must meet to be considered valid. These 

include: 

Post Meter Calibration 1 0.05 

Isokinetics 100 ±20% 

Pre and post meter box leak checks < 0.020 cu. Ft. 

D50 2.5μ ± 0.25μ 

Table 11 

Final System Bias Check 

O2/CO2 Analyzers 

 Run 1 Run 2 Run 3 

Date/Time 3/16/2010 14:10:04 3/16/2010 20:18:12 3/17/2010 2:03:35 

Analyte O2 CO2 O2 CO2 O2 CO2 

Units % % % % % % 

Zero Ref Cyl 0 0 0 0 0 0 

Zero Cal -0.009 0.001 -0.009 0.001 -0.009 0.001 

Zero Avg 0.028 0.138 -0.001 0.169 0 0.134 

Zero Bias% 0.1 0.5 0 0.6 0 0.4 

Zero Drift% 0.1 0.1 -0.1 0.1 0 -0.1 

Span Ref Cyl 5.486 5.469 5.486 5.469 5.486 5.469 

Span Cal 5.437 5.431 5.437 5.431 5.437 5.431 

Span Avg 5.382 5.393 5.404 5.526 5.408 5.505 

Span Bias% 0.2 0.1 0.1 0.3 0.1 0.2 

Span Drift% -0.1 -0.2 0.1 0.4 0 -0.1 

Ini Zero Avg -0.003 0.107 0.028 0.138 -0.001 0.169 

Ini Span Avg 5.395 5.445 5.382 5.393 5.404 5.526 

Run Avg 3.3 15.592 3.316 15.737 3.287 15.833 

Co 0.012 0.122 0.013 0.153 0 0.152 

Cm 5.389 5.419 5.393 5.46 5.406 5.515 

Correct Avg 3.355 15.972 3.368 16.061 3.335 15.99 
 

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Table 12 

QA/QC for USEPA Method OTM27/28 

Sibley Generating Station 

Parameter Run 1 Run 2 Run 3 Average Results

% Isokinetic (80-120%) 94.48 92.26 95.90 94.22 Pass 

ΔP range ( 3.80 to 9.12) passed passed passed passed Pass 

Cunningham Correction Factor ( C ) 1.0909 1.0896 1.0921 1.09 Pass 

μmeter - D50 for Cyclone IV (2.25-2.75) 2.39 2.43 2.37 2.40 Pass 

All pre and post leak checks met method criteria. 

For the filterable particulate and the multi metals train (Method 29) the sampling system must 

meet: 

Post Meter Calibration 1 0.05 

Isokinetics 100 ±10% 

Pre and post meter box leak checks < 0.020 cu. Ft. 

Table 13 

QA/QC Method 5/29 

Sibley Generating Station 

 Method Criteria Run 1 Run 2 Run 3 Average Test 

Series 

Unit # 2 - Condition 1 

Isokinetics 100 + 10 % 95.45 95.75 98.75 96.65 Pass 

Post Leak Checks - 

System < 0.020 cu. ft./min 0.000 0.000 0.017 0.001 Pass 

Post Leak Checks - Pitot stable for at least 

15 secs 0.0 0.0 0.0 0.0 Pass 

Alt-009 Results ± 5 % of original Y -3.39 -2.87 -2.82 -3.03 Pass 

In addition the metals analysis at the lab must achieve laboratory spike recoveries that meet the 

75% to 125% recovery criteria. The laboratory met all spike recovery criteria for the method. 

Mercury analysis per Method 30B’s quality assurance criteria are: 

Tube agreement ± 10% 

 Spike recoveries 100% ± 15% 

 Break through <10% 

 Spike level ± 50% of the sample catch 
 

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Kansas City Power & Light 31 CEC Project 100-208 

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For this test sequence all three runs meet the QA/QC criteria for determining the validity of the 

test. Table 14 below presents the QA/QC data for the test sequence at Sibley Generating Station. 

Table 14 

QC/QA Data for USEPA Method 30B 

Sibley Generating Station 

No Description Tube ID C, ng/g 

RD 

(Tube Agreement) B % Recovery % 

1 Run 1 A 68707 FH A 68707 117 0.83% 

2 Run 1 A 68707 BH A 1.7 1.45% 101.9% 

3 

Run 1 B 68534 FH 

Spike B 68534 216 

4 Run 1 B 68534 BH B 1.4 0.65% 

5 Run 2 A 68739 FH A 68739 100 6.28% 

6 Run 2 A 68739 BH A 0.3 0.30% 89.2% 

7 

Run 2 B 68542 FH 

Spike B 68542 186 

8 Run 2 B 68542 BH B 0.7 0.38% 

9 Run 3 A 68709 FH A 68709 102 4.61% 

10 Run 3 A 68709 BH A 0 0.00% 92.4% 

11 

Run 3 B 65430 FH 

Spike B 65430 191 

12 Run 3 B 65430 BH B 1.2 0.63% 

 Average Spike = 

100 ng 3.91% 0.57% 94.50% 

The metals analysis at the lab must achieve laboratory spike recoveries that meet the 75% to 

125% recovery criteria. The laboratory met all spike recovery criteria for the method. The 

results on a per metal basis can be found in Appendix E. 

4.2 BLANK SAMPLING TRAINS 

For each of the sampling trains a blank train was collected by recharging the first sampling train 

with reagents, assembling the train, leak checking the train at the sample location and recovering 

the sample train. 

For the metals train (Method 29) chromium, manganese, nickel, arsenic and lead were found in 

the blank train front half section at 1.82 ug, 3.8 ug, 0.59 ug, 0.63 ug and 0.27 ug, respectively. 

All of the target metals were detected in the backhalf of the sampling train at levels at or below 

the laboratory reporting limits, with the exception of chromium and nickel which were found at 

1.03 ug and 1.19 ug, respectively. The trace levels detected are minimal and have a negigible 

impact on the final results. 

The OTM27/28 blank sampling train for Filterable PM was at the method detection limit of 0.5 

mg for the filter and front half rinse. The total blank level was 0.9 mg which is nsignificant 
 

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Kansas City Power & Light 32 CEC Project 100-208 

Sibley Generating Station 

compared to the concentration detected in the samples. The condensible portion of the sampling 

train had blank train values of 2.9 (organic) and 1.8 (inorganic) ug for a total correction of 4.7 

mg. This correction is higher than the he method allowed 2 mg correction. The results indicate 

that there may be a slight positive bias in the final condensible results of approximately 2%. 

4.3 QUALITY ASSURANCE OBJECTIVES 

Data Quality Indicators (DQIs) are a simplistic way of referring to data characteristics by 

consideration of commonly used measures of environmental quality. The most commonly used 

DQIs are precision, bias (accuracy), and completeness. Accuracy is the degree of agreement of a 

measurement (or average of measurements) with an accepted reference or true value. Precision 

is a measure of mutual agreement of replicate measurements. Completeness is a measure of the 

amount of valid data compared to the amount that was expected to be obtained under correct 

operating conditions. 

Precision is typically determined by calculating the range percent (RP) when the number of data 

points is less than four but more than 2. RP is typically calculated using the equation: 

ܴܲ ൌ 100 ൈ ሺܺ௠௔௫ െ ܺ௠௜௡ሻ

ܺ௔௩௚ ൘

Table 5 lists the expected (typical) precision of the sampling methods, based on the above listed 

calculation. 

Accuracy is the extent of the agreement between an observed value (sample result) and the true 

value of the parameter being measured. Accuracy/Bias as an indicator of measurement 

confidence, percent accuracy will be calculated based on analytical results of spiked samples of 

known chemical concentrations for the metals analysis. Accuracy for an analytical method is 

typically calculated as: 

%ܴ ൌ 100 ൈ ܥ௠

ܥ௦௥௠ ൗ

Where: Cm = measured concentration of a standard 

 Csrm = actual concentration of the SRM 

when laboratory control spikes are used in the analysis. Accuracy of the other manual sampling 

methods typically cannot be measured. Table 15 lists the expected accuracy of the sampling 

methods based on the calibration procedure. 
 

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Kansas City Power & Light 33 CEC Project 100-208 

Sibley Generating Station 

Table 15 

Precision and Accuracy for Emission Test Methods 

KCP&L ICR Sampling 

Sibley Road Generating Stations 

Parameter Method Traceability or 

Audit Device 

Expected 

Precision 

Expected 

Accuracy 

Achieved

Gas Velocity Method 2 EPA Design 

Specifications 

± 18% Not 

measured 

Not 

measured 

Gas Volume Method 4, 29, 

OTM 27/28 

Wet test meter 

reference 

± 2% ± 2% ± 0.3% 

Stack /Filter 

Temperature 

Thermocouple Mercury in glass ± 1 % ± 1.5 % ± 1.5% 

Barometric 

Pressure 

Aneroid 

Barometer 

Calibrated Barometer ± 4 % ± 4 % ± 4 % 

Particulate 

weights 

Electronic 

Balance 

Class S weights ± 0.5 mg ± 0.5 mg ± 0.5 mg 

Gas Composition 

O2/CO2

EPA Method 3A NIST Traceable 

Cylinder gas 

± 25% ± 20% ± 10% 

Particle size 

weight 

Electronic balance Class S weights ± 0.2 mg ± 0.5 mg ± 0.5 mg 

Multimetals EPA Method 

29/ICAP 

Audit sample ± 20% ± 10% N/A 

Particulate 

emissions 

 EPA Method 5 

Filterable PM 

All the above ± 12.1% N/A 2.2% 

Completeness is a measure of the amount of valid data compared to the amount that was 

expected to be obtained. Completeness is calculated using: 

%ܥ ൌ 100 ൈ ܸ

ܶൗ

Where V = the number of valid samples 

 T = total number of planned samples 

For this testing program the percent completeness was 100%. 
APPENDIX A 

FIELD DATA FORMS 

























APPENDIX B 

ELECTRONIC SPREAD SHEETS 



























































APPENDIX C 

EXAMPLE CALCULATIONS 









APPENDIX D 

ANALYTICAL DATA ENTHALPY ANALYTICAL, OTM 27/28 

























APPENDIX E 

ANALYTICAL DATA PACE LABS, METHOD 29 

 

















APPENDIX F 

ANALYTICAL DATA STANDARD LABS, FUEL 

 






APPENDIX G 

CALIBRATION SHEETS, CERTIFICATIONS 

 





























APPENDIX H 

PROCESS DATA