Entec Servi¢ 

16 D Commerce 

Hueytown, Alabam 

Telephone: (205) 

Fax: (205) 491-6614 

Results of the December 15, 2005 

Compliance Testing for Emissions on 

Brick Kiln 38B located in 

Louisville, Kentucky 

LMAPCD Facility No. 0079, Permit No. 48-04-C 

Submitted to: 

General Sha e Products, LLC 

P.O. Box 3547 

Johnson City, Tennessee 37602 

Attention: Ms. Martha West 

Entec Project No. 25186 Report Submitted: January 5, 2006 

Com.•)lete•}y: 

Tomm.)/ Lotz, Jr. 

Project Manager 

Reviewed By: 

Tom Lotz Sr. 

QA/QC Manager 

hereby certify to the best of my knowledge all field sampling and laboratory analysis performed 

for this report is authentic and accurate. It has been checked for completeness and accuracy. 
Genera Shale Products 

Table of Contents 

Section 

Executive Summary 

Emissions Summary 

Detailed Test Results 

Sampling Procedures 

Location of Test Ports 

Diagram of Sampling Train 

Instrumental Data Sheets 

Test Run 1 

Test Run 2 

Test Run 3 

Particulate Field Data Sheets 

Test Run 1 

Test Run 2 

Test Run 3 

Control Room Production Data 

Quality Assurance I Quality Control Procedures 

QA / QC Checklist 

Orifice Check and Temperature Check 

Preliminary Flow and Cyclonic Check 

Analyzer Interference Checks 

Laboratory Analysis 

Instrumental Analyzer Calibrations 

Calibration Gas Certificates 

Particulate Equipment Calibrations 

Nomenclature and Test Calculations 

2 

3 

7 

12 

15 

16 

20 

24 

28 

29 

32 

35 

38 

40 

46 

47 

48 

49 

53 

60 

65 

70 

83 
Executive Summarv 

Entec Services, Inc. was retained by General Shale Products to perform emissions 

testing on Brick Kiln 38B at the Louisville facility located in Louisville, Kentucky. Mr. 

Tommy Lotz, Jr., Mr. Lalan Kirby, and Mr. Art Otero of Entec Services, Inc conducted 

the testing on December 15, 2005. Representing General Shale Products was Ms. 

Martha West who coordinated testing with the control room production activity. 

Particulate, Hydrogen Chloride, Hydrogen Fluoride, and Sulfur Dioxide emissions were 

performed on the Brick Kiln 38B Enhanced All Dry Lime Scrubber System with 

Baghouse exhaust stack. 

No difficulties were encountered in the field collection of the samples or in the 

laboratory analysis of the samples by Entec Services, Inc. 

The emissions test summary on the following page gives a detailed summary of each 

test run compared to the maximum emission limits set forth by the Louisville Metro Air 

Pollution Control District. Tests results indicate the average emissions are below 

the limits set forth by Louisville Metro Air Pollution Control District for Facility No. 

0079 permit No. 48=04-C. 

Detailed Test Results 
SOURCE OWNER: 

PLANT LOCATION: 

SOURCE(S) NAME(S): 

SOURCE(S) CONDITION: 

SOURCE(S) SHAPE: 

PROBE WASH CHEMICAL: 

SOURCE PERMIT NUMBER: 

TEST PERFORMED: 

REFERENCE METHOD TESTS: 

PROJECT MANAGER 

ENVIRONMENTAL ANALYST-PROJECTLEADER 

ENVIRONMENTAL ANALYST-ASSISTANT 

OWNER'S REPRESENTATIVE: 

RULING AGENCY 

RULING AGENCY REPRESENTATIVE: 

DATES TESTS CONDUCTED: 

ENTEC PROJECT NUMBER: 

Entec Services, Inc, 

SOURCE OVERVIEW 

General Shale 

Louisville, Kentucky 

Kiln 38 B 

Initial Compliance Testing 

Circular 

Acetone 

48-04-C 

Particulate with HCL and Gaseous Testing 

Sample Location EPA Method 

Volumetric Flow EPA Method 

Molecular Weight EPA Method 

Moisture Content EPA Method 

Particulate EPA Method 

Sulfur Dioxide EPA Method 

Mr. Tommy Lotz, Jr. 

Mr. Lalan Kirby 

Mr. Art Otero 

Ms. Martha West 

Louisville Metro Air Pollution Control District 

None 

12/15/05 

25186 

1 

2 

3A 

4 

26A 

6C 
ENTEC Services, inc. 

16-D Commerce Ave Hue town A abama 35023 

INPUT TEST DATA 

Client: General Shale Job No.: 25186 

Source: Kiln 38 B 

Field Data Symbol Uni• 

Run Number 

1 

Test Date 

Time Test Run Be__•an Ended 

Sampling Time 

Stack Area 

Barometric Pressure 

Stack Static Pressure 

Pitot Tube Correction factor 

Meter Correction Factor 

Meter Delta H @ 

Nozzle Diameter 

Meter Volume 

Meter Temperature 

A______L____, F• 

Pbar in. Hg 

P. in. H20 

Data ,==put by; Lalan Kirby 

12/15/05 

Military Time 0952-110•2 

minutes 60 

12.177 

29.36 

-0.19 

0.84 

•H@ 

D. inches 

V______._•__• dc•f 

Avg. Orifice Delta H 

.Impingers Weight Gain (Moisture) 

Silica Gel Impinger Weight Gain (Moisture) 

_Oxygen Concentration, dry basis 

Carbon Dioxide Concentration, dry basis coz 

S•ulfur Dioxide Concentration, dry basis so2 

A.•vg. Sq. Rt. of Delta P 

Stack Temperature 

Total Hydrogen Chloride collected, mg 

Total Hydrogen Fluoride collected, mg 

Total particulate collected 

*Denotes less than values= 

0.985 

in. H=0 1.951 

0.275 

41.703 

85.0 

HCL 

HF 

Test Data 

3 AVERAGE 

12/15/05 12/15/05 

1130-123•9 1308-141_____.___.___•; 

60 60 60 

29.36 29.36 29.36 

-0.19 -0.18 -0.19 

% 17.9 

0.84 0.84 

0.985 

0.84 

0.985 0.985 

1.951 1.951 1.951 

0.275 

44.249 

0.275 0.275 

42.943 42.965 

83.0 79.0 82.3 

in. H20 1.51 1.74 

grams 53.5 54.8 

grams 7.1 7.7 

17.5 

% 2.5 

15.7 

0.590 

ppm 

(in. H20) 1/2 

F 

mg 

2.4 

1.64 1.63 

51.5 53.3 

6.4 7.1 

17.7 17.7 

2.3 2.4 

10.2 2.7 

0.605 0.588 

9.53 

0.594 

mg 

mg 

222.6 

0.05 

225.0 

0.25 

220.2 

0.04 

222.6 

0.11 
ENTEC Services, inco 

16-D Commerce Ave Flue own A abama 35023 

CALCULATED TEST DATA 

Client: General Shale 

Job No.; 25186 Source: Kiln 38 B 

Uata Input By: Lalan Kirby Description Formulas Symbol Units Calculated Data Run Number 

2 3 

12115/05 12/15/05 12/15/05 

Military'time 0952-1102 1130-1239 1308-1412 

P, in. Hg 29.35 29.35 29,35 29.35 

Pm in. Hg 29.47 29.49 29.48 29.48 

V•) dscf 39.183 41.753 40.811 40.582 

V•,=• Scf 2.518 2.579 2.424 2.50___._._.__.•7 

V•,• SCf 0.335 0.363 0,302 0.333 

B• fraction 0.067 0.0658 0.0626 0.0654 

IVla g/g-mole 29.116 29.084 29,076 29.092 

M• gig-mole 28.362 28.35z 28.383 28.366 

v, ff./s 38.35 39,4" 38.14 38.634 

O• acfm 28,021 28,795 27,862 28;226 

Q, scfm 21,251 21,761 21,206 21,406 

Q•t• dscfm 19,809 20,329 19,879 20;005 

c, grldsct` 0,0009 0.0018 0.0016 0,0014 

HCLcs grldscf 1.969E-05 9.239E-05 1.512E-05 4,240E-05 

HFcs grldscf 2.544E-06 2.347E-06 2.411E-06 2!434E•06 

C•z Ibsldscf 2.61E-06 1.70E-06 4.49E-07 1.59E-06 

PMR Ib/hr 0.15 0.31 0.27 0•24 

aOzJb/hr Ib/hr 3.10 2.07 0,54 1:90 

HCl -Ibs,'hr Ibs/hr 0.003 0.016 0.003 0007; 

HF =lbsA•r Ibs/hr 

V, act 55.428 59.143 57.203 57,258 

c= gr/aci' 0.0006 0.0012 0.0011 0.0010 

Test Date 

Time Began-Ended 

1. Stack Pressure 

=Pbar P•l 13.• 

2. Meter Pressure 

P• AH 113.6 

3. Standard Meter Volume 17.64" Y* (Vm/T•)* (P•r &H 13.0 

4a. Standard Volume of Water Vapor Condensed =0.04706'W=¢ 

4b. Standard Volume of Water Collected in Silica Gel =0.04715'W= 

5. Moisture Fraction 

9. Molecular Weight Of Stack Gas. dry basis 

10. Molecular Weight Of Stack Gas. wet basis 

I. Average Stack Gas Velocity 

12. Stack Gas Flow @ Stack Conditions 

13. Stack Gas Flow @ Standard Conditions 

14. Stack Gas Flow @ Dry Standard Conditions 

15. Particulate concentration @ Standard Conditions 

15. Hydrogen Chloride concentration @ Std.Cond.,Grains/Cu.Ft. 

15. Hydrogen Fluoride concentration @ Std.Cond.,Grains/Cu.Ft. 

184 Sulfur Dioxide (SO2) Gas Concentration 

=0.01 

=(o.01 

=(O.Ol 643*HFr•)IQ=•¢ 

=C,=,= MW 1385.1 10 

!1. Particulate em=ss=ons 

(60/7000)*c.*Q•d 

1. Sulfur Dioxide (SO•) Gas emissions 

1. Hydrogen Chlor/de emissions 

1. Hydrogen Fluoride emissions 

2. Volume collected through nozzle 

=Csoz Q•=•" 60 

=(80/7000)*HCLQ•*Q•t• 

=(60/7000 )*HFQ•z•*Q=•o 

=TJP,'[O,OO2669*V•+ V•*y*prJl"m] 

Particulate concentration, @ actual conditions =0.01543"m•N. 

I.. Isokinetic Sampling Rate. Percent 100*Vnl (60"v,*A,.e) % 97 33 101 06 101 01 99 80 

Difference, (Calibration must be within 5% of original Y-factor) iiii!!iiiii!i!iii ii;! iiiii:!i:!i!i iii ii!:iil 

0.91% 

*Denotesless than values= 
Sampling Procedures 
Proced u res 

The emission rates were determined using EPA Methods 1-4, 3A, 6C, and 26A CFR 

Title 40, Part 60, Appendix A. The calibration and quality assurance procedures of EPA 

CFR 40 Part 60 Appendix A for all methods, and the "Quality Assurance Handbook for 

Air Pollution Measurement System" Volume III Stationary Source-Specific Methods 

were followed throughout the duration of the field and laboratory testing. 

The most current revision revised as of July 1, 2004, of each method (as described in 

the Federal Register) was used. 

Stack Gas Volumetric Flow 

The velocity of the gas stream was determined according to EPA Reference Method 1 

and 2 by reading the instantaneous velocity head with an inclined manometer at each 

sampling point with a calibrated S-type pitot tube attached adjacent to the sample 

nozzle. The stack pressure was measured with the static side of an S-type pitot tube. 

A calibrated pyrometer was used to measure stack temperature at each sampling point. The stack was tested for cyclonic flow according to EPA Reference Method 1. 

Stack Gas Molecular Wei.qht=lnstrumental 

The carbon dioxide concentrations were determined using EPA Reference Method 3A. 

The molecular weight of the gas was calculated using the moisture, oxygen and carbon 

dioxide content and the measured stack gas temperature. 

Moisture Content 

The moisture content used for calculating the gas stream flow rate was determined by 

measuring the amount of condensed moisture in the impinger train as described in EPA 

Reference Method 4 at the completion of each test. 

The moisture collection system consists of a series of glass impingers connected to 

silica gel loaded glass impinger attached to the outlet. Ice is placed around the 

impingers to maintain an exit temperature of <680 F. The outlet temperature of the 

impinger is monitored and recorded throughout the duration of the testing to verify the 

exit temperature is below <68 o F. 
Particulate, Hydrogen Chloride, and Hydrogen Fluorid,-- 

Preliminary data was used to determine stack temperature, pressure, and range of 

velocity heads, moisture content and stack gas dry molecular weight prior to sampling. 

The meter box was leak checked from the pump to the orifice. Initial and final leak 

checks of the sampling system and pitot lines were performed as outlined in Method 5 

and were recorded on the data sheets. The nozzle (glass with an angle of taper of 30 

degrees and of button hook design) was calibrated before and a•ter the test using a 

micrometer and was also recorded on the data sheets. 

The sampling probe was placed at each sampling point to provide a total sampling time 

of 60 minutes. The gases were drawn through a glass nozzle attached to a heated 

glass lined probe. The probe was maintained at the proper setting to obtain an exit 

temperature of above 2480 F. The gases then proceeded through borosilicate glass 

filter holder, with a Teflon frit filter support through a glas• fibe• filter to remove 

particulate matter. The filter was maintained at a temperature of above 248 o F. These 

temperatures were recorded at each point on the data sheets. 

The gases were then scrubbed through a series of four impingers to capture hydrogen 

halides and halogens and moisture. (The optional first impinger for a knockout for 

moisture was not used.) The first and second impingers contained approximately 100 

ml of a 0.1N H2SO4 solution and the third and fourth impinger contained approximately 

100 ml of a 0.1 N NaOH solution. The fifth impinger contained pre weighed silica gel to 

remove any remaining moisture. The gases pass through the impinger series in an ice 

bath to maintain a maximum exit temperature of < 68 0 F. This temperature was also 

recorded on the data sheets. The clean and cool gases then entered the meter box 

where the gas flow and temperature were measured. 

After the completion of the test the sampling train and the probe nozzle assembly was 

transferred to the cleanup area making sure no particulate was lost. The cleanup data 

was recorded. 

Particulate catches were placed in sealed petri dishes. Each acetone rinse from the 

nozzle, probe, and filter holder was combined and placed in a sealed container. For the 

group of tests an acetone blank of approximately 200 milliliters was placed in a sealed 
container. The first and second impinger contents were transferred to its tared 

container, weighed and the rinsing from the glassware were added to this container. 

The third and fourth impinger was transferred to its respective tared container, weighed 

and the rinsing from the glassware was added to this container. The silica gel from the 

fifth impinger was transferred to its respective tared container and weighed. A blank of 

the sulfuric acid solution, sodium hydroxide, distilled water and acetone was taken. All 

containers were clearly marked, logged in, and shipped to a State of Georgia approved 

certified laboratory for analysis. 

The oxygen content in the flue gas was determined using a Siemens Ultramat 23 

oxygen analyzer. The Ultramat 23 uses an electrochemical cell that consumes oxygen 

from the atmosphere surrounding the cell. The consumption of the oxygen generates a 

proportional electrical current. This current is then amplified and provides a signal 

output of 4-20ma signals, which corresponds to a full-scale range of 0-25% oxygen. 

Carbon Dioxide 

Carbon dioxide concentrations were continuously measured with a Siemens Ultramat 

23 non-dispersive infrared (NDIR) analyzer. The theory of operation for this analyzer is 

based on the principle that CO2 has a unique absorption line spectrum in the infrared 

region. The instrument consists of an infrared light source, a chopper, a measurement 

cell, and a detector. The infrared light beam emitted by the source passes through the 

measuring cell, which is filled with a continuously flowing gas sample. The light beam is 

partially absorbed or attenuated by the gas species of interest in this cell before 

reaching the front chamber of the detector. Both the front and rear chambers of the 

sealed detector are filled with a reference gas. The difference in the amount of light 

absorbed between the front and rear chambers are dependent on the concentration of 

the gas species of interest within the sample measurement cell; a pressure differential 

is thus created between the two chambers. This pressure difference is then observed 

as gas flow by the micro-flow sensor located in a channel connecting the two chambers. 

The resulting AC signal from the micro-flow sensor is rectified, amplified and linearized 

into a 4-20ma signal for output that corresponds to a full-scale 0-25% measurement 

range. 
Sulfur Dioxide 

A Western Research Model 721M SO2 analyzer provided continuous analysis of SO2 in 

the gas stream. The basic analytical principle involves quantitative measurement of the 

absorption of UV radiation by SO2 molecules. The analyzer uses a single light source, 

which emits an appropriate wavelength, illuminating the sample cell through which the 

sample is continuously passed. Narrow-band optical filters are rotated through the 

beam, and the radiation passed through the optical filters and sample cell is detected 

by a single photo-detector. The signal pulses from the photo-detector are separated by 

a multiplexor into a measuring channel and a reference channel. A log ratio amplifier 

computes the logarithm of the input signal ration, producing a signal that is proportional 

to the SO2 concentration. The dual-range analyzer has a digital readout, as well as 0- 

10.0 V DC output terminals. The full scale of the instrument was set at 100 ppm. 

Samplin_c• System 

Samples were extracted from the gas stream by a heated stainless steel probe 

maintained at a set temperature of 250 degrees Fahrenheit, through a ten (10) foot 

heated sample line that was heated to a temperature between 225 and 250 degrees, 

through a chilled sample conditioner to remove the moisture in the gas stream and 

transported to the test trailer through unheated teflon sample lines to the analyzers. 

Data Acquisition 

Concentration values were collected using a Baldwin Environmental RM Plus 

Parametrics data acquisition system. The data was recorded every fifteen-seconds and 

then averaged for each sixty-second interval. Each minute average was then averaged 

for the duration of each test run. 

During all testing, the unit was operating within normal operating parameters; at a range 

appropriate in accordance with applicable permits. 
Entec Services, Inc 

16 D Commerce Ave. Hueytown, AL 35023 

STACK DRAWING & TRAVERSE POINT LOCATION 

Client: General Shale 

Source: Kiln 38 B 

Job No. 25186 

Input By: Lalan Kirby 

Type of Traverse: Velocity (V) or Particulate (P): p 

Stack Diameter, inches: 47.26 

Stack Height, feet: 60 

Stack Properties: Inches Duct Diameters 

Upstream Disturbance: 192.0 

Downstream Disturbance: 360.0 

4.06 

7.62 

Port Type Nipple 

Stack Area, Ft2: 

Number of Ports: 

Length of Port, inches: 

Total Number of Traverse Points: 

Number of Points per diameter: 

Port Diameter 4 

12.177 

2 

4.50 

12 

6 

47.3 INCHES 

192.0 

360.0 

NCHES 

INCHES 

Inside Stack Outside Nipple 

Point No. Inches Inches 

2.1 6.6 

2 6.9 11.4 

3 14.0 18.5 

4 33.3 37.8 

5 40.4 44.9 

6 45.2 49.7 

Adjusted points diameter > 24" no point closer than 1.0 inch 

Adjusted points diameter <_ 24" no point closer than 0.5 inch 

Stack Diameters between 12-24 inches minimum points are 8 

4 points per port if the 8 2 diameters downstream and 

upstream criteria is met. 

12 
instrument Sampling Train 

In-stack 

Filter 

Three Way Valvej 

Heated 

Stainless •1 Steel •'ro•eJ 

Calibration Gas Line 

Heated Teflon Line 

F•ow Contro• 

Panel 

Communication Lines 

Data 

Acq uisition 

NOx 

$02 

O2 & CO2 

Air Sampling 

Analyzers 

Calibration 

Gases 
Method 26A Sampling Train 

Filter Exit Temperature 

i•248 F) 

Heated Filter, Filter 

Hblder and Probe 

(•248 F) 

Sensors J 

I•' lmpingerExit Temperature (<68 F) 

Manometer 

Dry Gas Meter-] 

24 
Instrumental Data Sheets 
Test Run No. 1 

Data Sheets 
Calculation Average Emissions 

Test Performed For: 

General Shale 

Louisville, Kentucky 

Kiln Stack 38B 

Initial Compliance 

Date: 12/15/05 

Calibration Gas Value 

0.00 percent 0 2 

10.00 percent 0 2 

0.00 percent CO2 

9.93 percent CO2 

0.0 ppm SO2 

50.6 ppm SO2 

Mean Reference Values: 

17.55 percent 02 

2.43 percent CO2 

18.0 ppm SO2 

Test Performed By: 

Entec Services, Inc. 

Birmingham Division 

Test Trailer 904 

Tommy Lotz, Jr. 

Run 1 

Initial Calibration 

0.05 % 

9.66 % 

Final Calibration Average 

0.01% 0.03 

9.99 % 9.83 

0.03 % 

9.59 % 

-0.05 % -0.01 

9.87 % 9.73 

3.5 ppm 

50.6 ppm 

3.4 ppm 3.46 

50.4 ppm 50.52 

Corrected Results: 

17.90 percent 0 2 

2.50 percent CO2 

15.7 ppm SO2 

Basis: 

DRY 

DRY 

DRY 

•7 
General Shale 

Louisville, Kentucky 

December 15, 2005 

Kiln 38B 

Run Number Date Tim_.._•e • 

12/15/2005 9:52:45 17.53 

12/15/2005 9:53:45 17.40 

12/15/2005 9:54:45 17.39 

12/15/2005 9:55:45 17.41 

12/15/2005 9:56:45 17.42 

12/15/2005 9:57:45 17.45 

12/15/2005 9:58:45 17.45 

12/15/2005 9:59:45 17.42 

12/15/2005 10:00:45 17.45 

12/15/2005 10:01:45 17.46 

12/15/2005 10:02:45 17.47 

12/15/2005 10:03:45 17.47 

12/15/2005 10:04:45 17.46 

12/15/2005 10:05:45 17.45 

12/15/2005 10:06:45 17.44 

12/15/2005 10:07:45 17,43 

12/15/2005 10:08:45 17.43 

12/15/2005 10:09:45 17,44 

12/15/2005 10:10:45 18.22 

12/15/2005 10:11:45 18.32 

12/15/2005 10:12:45 17.52 

12/15/2005 10:13:45 17.37 

12/15/2005 10:14:45 17.37 

12/15/2005 10:15:45 17.35 

12/15/2005 10:16:45 17.34 

12/15/2005 10:17:45 17.32 

12/15/2005 10:18:45 17.33 

12/15/2005 10:19:45 17.33 

12/15/2005 10:20:45 17.34 

12/15/2005 10:21:45 17.33 

2.37 

2.49 

2.50 

2.50 

2.49 

2.48 

2,47 

2.47 

2.47 

2.45 

2.45 

2.45 

2.45 

2.47 

2.47 

2.48 

2.49 

2.48 

1.95 

1,90 

2,37 

2.50 

252 

2.53 

2.53 

2.56 

2,55 

2.56 

2.55 

2.57 

15,1 

16.6 

23.3 

93.7 

47.6 

25.1 

19.0 

18.1 

19.2 

18.1 

17.8 

18.1 

17.6 

18.8 

18.0 

18.5 

18.0 

17.8 

9.0 

11.0 

15.9 

18.7 

19.7 

19.4 

20.6 

20.6 

20.4 

22.8 

21.2 

21.2 
12/15/2OO5 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2Q05 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

10:22:45 

10:34:45 

10:35:45 

10:36:45 

10:37:45 

10:38:45 

10:39:45 

10:40:45 

10:41:45 

10:42:45 

10:43:45 

10:44:45 

10:45:45 

10:46:45 

10:47:45 

10:48:45 

10:49:45 

10:50:45 

10:51:45 

10:52:45 

10:53:45 

10:54:#5 

10:55:45 

10:56:45 

10:57:45 

10:58:45 

10:59:45 

11:00:45 

11:01:45 

11:02:45 

Average 

17,34 

18.67 

18.33 

18,13 

18.11 

17.78 

17.53 

17.54 

17.56 

17.56 

17.56 

17.54 

17.53 

17.52 

17.52 

17.51 

17.51 

18.26 

18,33 

17.51 

17.32 

17.30 

17.33 

17.33 

17,33 

17.32 

17.33 

17.34 

17.34 

17.32 

17.55 

2.57 

1.65 

1.86 

2.01 

203 

2.27 

2.44 

2.45 

2.45 

2.45 

2.45 

2.47 

2.49 

2.49 

2.49 

2.50 

2.50 

1.98 

1.93 

2.44 

2.60 

2.62 

2.61 

2,61 

2.60 

2.61 

2.60 

2.60 

2.60 

2.62 

2.43 

21.6 

4,2 

6.1 

9.3 

10,1 

13,1 

13.1 

13.9 

13.5 

13,4 

12.6 

12.0 

12.5 

11,8 

12.6 

13.3 

14.2 

7.8 

9.0 

13.4 

15.8 

17.9 

21.6 

18.6 

19.0 

169 

17.8 

17.7 

17,7 

17,4 

18.0 
Test Run No. 2 

Data Sheets 
Calculation Average Emissions 

Test Performed For: 

General Shale 

Louisville, Kentucky 

Kiln Stack 38B 

Initial Compliance 

Date: 12/15/05 

Calibration Gas Value 

0.00 percent 02 

10.00 percent 0 2 

0.00 percent 

9.93 percent 

0.0 ppm S02 

50.6 ppm SO2 

Mean Reference Values: 

17.51 percent 02 

2.40 percent CO2 

12.5 ppm SO2 

Test Performed By: 

Entec Services, Inc. 

Birmingham Division 

Test Trailer 904 

Tommy Lotz, Jr, 

Run 2 

Initial Calibration 

0.01% 

9.99 % 

Final Calibration Average 

0.05 % 0.03 

10.03 % 10.01 

-0.05 % -0.02 % -0.03 

9.87 % 9.88 % 9.87 

3.4 ppm 

50.4 ppm 

2.3 ppm 2.86 

50.9 ppm 50.64 

Corrected Results: 

17.50 percent 02 

2.40 percent CO 2 

10.2 ppm S02 

Basis: 

DRY 

DRY 

DRY 

21 
General Shale 

Louisville, Kentucky 

December 15, 2005 

Kiln 38B 

Run Number 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

Dat__.•e Tim_._..•e • 

12/15/2005 11:31:45 18.15 

12/15/2005 11:32:45 17.34 

12/15/2005 11:33:45 17.16 

12/15/2005 11:34:45 17.16 

12/15/2005 11:35:45 17.22 

12/15/2005 11:36:45 17.32 

12/15/2005 11:37:45 17.35 

12/15/2005 11:38:45 17.34 

12/15/2005 11:39:45 17.34 

12/15/2005 11:40:45 17.35 

12/15/2005 11:41:45 17.36 

12/15/2005 11:42:45 17.36 

12/15/2005 11:43:45 17.36 

12/15/2005 11:44:45 17.37 

12/15/2005 11:45:45 17.36 

12/15/2005 11:46:45 17.39 

12/15/2005 11:47:45 17.38 

12/15/2005 11:48:45 17.36 

12/15/2005 11:49:45 17.37 

12/15/2005 11:50:45 18.13 

12/15/2005 11:51:45 18.43 

12/15/2005 11:52:45 18,37 

12/15/2005 11:53:45 18.49 

12/15/2005 11:54:45 18.46 

12/15/2005 11:55:45 18.03 

12/15/2005 11:56:45 17.87 

12/15/2005 11:57:45 17.81 

12/15/2005 11:58:45 17.49 

12/15/2005 11:59:45 17.31 

2.04 

2.52 

2.66 

2.68 

2.62 

2.55 

2.52 

2.52 

2.52 

2.52 

2.52 

2.51 

2.52 

2.52 

2.52 

2.50 

2.52 

2.53 

2.52 

2.01 

1.83 

1,84 

1.75 

1.75 

201 

2.13 

2.17 

241 

2.52 

SO•1 pp• 

10.1 

16.3 

18.3 

18.9 

17.7 

17.8 

16.3 

17.1 

15.9 

16.2 

15.1 

13.8 

13.4 

13,4 

14.8 

14.8 

-t 4:7 

14.1 

15.0 

7.4 

5.2 

4.0 

3.2 

4.2 

7.8 

7,2 

7,8 

11.6 

11.7 
2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

2 

12/15/20O5 

12/15/2OO5 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2O05 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/20O5 

12/15/2005 

12/15/2O05 

12/15/2005 

12/15/2005 

12/15/20O5 

12/15/•005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/20O5 

12/15/2005 

12/15/2005 

12/15/2005 

12:10:45 

12:11:45 

12:12:45 

12:13:45 

12:14:45 

12:15:45 

12:16:45 

12:17:45 

12:18:45 

12:19:45 

12:20:45 

12:21:45 

12:22:45 

12:23:45 

12:24:45 

12:25:45 

12:26:45 

12:27:45 

12:28:45 

12:29:45 

12:30:45 

12:31:45 

12:32:45 

12:33:45 

12:34:45 

12:35:45 

12:36:45 

12:37:45 

12:38:45 

12:39:45 

12:40:45 

Average 

18.08 

18.14 

17.32 

17.18 

17.19 

17.21 

17.23 

17.23 

17.22 

17.21 

17.25 

17.29 

17.30 

17.29 

17.31 

17.33 

17.32 

17.32 

17,33 

17.37 

18.13 

18.20 

17.47 

17.36 

17.36 

17.36 

17.38 

17.36 

17,37 

17.39 

18.07 

17.51 

2.00 

2.00 

2.48 

2.59 

2.59 

2.58 

2.57 

2.56 

2.57 

2.58 

2.54 

2.53 

2.52 

2.53 

2.53 

2.52 

2.52 

2.52 

2.52 

2.48 

1.96 

1.94 

2,37 

2.47 

2.48 

2.47 

2.46 

2.47 

2.47 

2.45 

2.09 

2.40 

6,4 

7.2 

10.9 

12.4 

13.2 

15.5 

15.2 

13.6 

13.8 

14.3 

13.6 

12.5 

11.9 

13,3 

14.1 

13.2 

14.1 

13.8 

14.1 

13,5 

7.4 

6.4 

10.6 

12,2 

12.7 

14.1 

13.2 

14.1 

12,1 

12.3 

9.3 

12.5 
Test Run No. 3 

Data Sheets 

24 
Calculation Average Emissions 

Test Performed For: 

General Shale 

Louisville, Kentucky 

Kiln Stack 38B 

Initial Compliance 

Date: 12/15/05 

Calibration Gas Value 

0.00 percent 0 2 

10.00 percent O2 

0.00 percent 

9.93 percent CO 2 

0.0 ppm 

50.6 ppm S02 

Mean Reference Values: 

17.58 percent 0 2 

2.30 percent CO2 

5.2 ppm SO2 

Test Performed By: 

Entec Services, Inc. 

Birmingham Division 

Test Trailer 904 

Tommy Lotz, Jr. 

Run 3 

Initial Calibration 

0.05 % 

10.03 % 

Final Calibration Average 

0.04 % 0.04 

9.87 % 9.95 

-0.02 % 

9,88 % 

0.01% 0.00 

9.85 % 9.87 

2.3 ppm 

50.9 ppm 

3.0 ppm 2.62 

51.6 ppm 51.25 

Corrected Results: 

17.70 percent 02 

2.30 percent CO2 

2.7 ppm SO2 

Basis: 

DRY 

DRY 

DRY 
Run Number 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

Genera Shale 

Louisville, Kentucky 

December 15, 2005 

Kiln 38B 

Dat.._•e Time 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2O05 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

13:09:15 17.62 2.28 

13:10:15 17.63 2.27 

13:11:15 17.63 2.28 

13:12:15 17.65 2.27 

13:13:15 17.68 2.25 

13:14:15 17.70 2.25 

13:15:15 17.66 2.27 

13:16:15 18.00 2.01 

13:17:15 18.56 1.67 

13:18:15 18.29 1.81 

13:19:15 18.38 1.76 

13:20:15 18.44 1.70 

13:21:15 18.31 1.78 

13:22:15 18.12 1.91 

13:23:15 18.10 1.93 

13:24:15 17.94 2.06 

13:25:15 17.63 2.25 

13:26:15 17.60 2.29 

13:27:15 17.56 2.33 

13:28:15 17.61 2.28 

13:29:15 18.09 1.98 

13:30:15 18.28 1.84 

13:31:15 17.93 2.07 

13:32:15 17.46 2.38 

13:33:15 17.35 2.48 

13:34:15 17.30 2.53 

13:35:15 17.29 2.54 

13:36:15 17.67 2,23 

13:37:15 18.33 1.83 

5.6 

5.6 

5.6 

5.2 

5.4 

4.9 

4.8 

4.0 

2.6 

2.2 

2.0 

1.9 

1.9 

2.1 

2.2 

2.9 

3.7 

3.2 

3.0 

2.7 

2.1 

1.8 

1,8 

2.1 

2.3 

2.6 

2.9 

2.8 

2.3 
3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

3 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/20O5 

12/15/2005 

12/15/2005 

12/15/20O5 

12/15/2005 

12/15/2005 

12/15/2OO5 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/20O5 

12/15/2005 

12/15/20O5 

12/15/2O05 

12/15/2O05 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2O05 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/2OO5 

12/15/2005 

12/15/2005 

12/15/2005 

12/15/20O5 

13:44:15 

13:45:15 

13:46:15 

13:47:15 

13:48:15 

13:49:15 

13:50:15 

13:51:15 

13:52:15 

13:53:15 

13:54:15 

13:55:15 

13:56:15 

13:57:15 

13:58:15 

13:59:15 

14:00:15 

14:01:15 

14:02:15 

14:03:15 

14:04:15 

14:05:15 

14:06:15 

14:07:15 

14:08:15 

14:09:15 

14:10:15 

14:11:15 

14:12:15 

14:13:15 

14:14:45 

Average 

17.23 

17.21 

17.23 

17.25 

17.25 

17.23 

17.22 

17.21 

17.25 

17.26 

17.26 

17.29 

17.72 

18.34 

17.53 

17.29 

17.27 

17.29 

17.25 

17.27 

17.25 

17.26 

17.23 

17.23 

17.24 

17.25 

17.24 

17.25 

17.23 

17.25 

17.44 

17.58 

2.51 

2.55 

2.54 

2.53 

2.53 

2.55 

2.55 

2.55 

2.53 

2.53 

2.52 

2.51 

2.18 

1.81 

2.28 

2.46 

2.48 

2.47 

2.50 

2.49 

2.50 

2.50 

2.52 

2.51 

2.52 

2.51 

2.50 

2.50 

2.52 

2.51 

2.41 

2.30 

6.5 

7.0 

7.4 

7,4 

6,9 

7.3 

7,1 

7.6 

7.9 

8.1 

7.6 

9.1 

7.1 

4.3 

5.9 

6.8 

7.2 

7.3 

7.4 

7.5 

7.6 

7.3 

7.6 

7.6 

7.9 

7.8 

7.5 

7.2 

6.7 

5.8 

10.4 

5.2 
Particulate Field Data Sheets 
Test Run No. 1 

Field Data Sheets 

29 
ENTEC Services, inc. 

15-D Commerce Ave. Hueytown, Alabama 35023 

Client: General Shale 

Source: Kiln 38 B 

Test Date: 12/15/2005 

Run Number: 1 

FIEED DATA, EPA METHOD 26A 

Traverse Point Delta P Delta H 

1-1 0.35 

1-2 0.38 

1-3 0.38 

1-4 

1-5 

1-6 

0.35 

Sq. Rt. Delta P 

0.5916 

0,6164 

0.6164 

0.5916 

0.33 0.5745 

0.30 0.5477 

2-1 0..31 

2-2 0.39 

0.36 

0.33 

2-3 

2-4 

2-5 0,36 

K-Factor 

2-6 0,34 

4.33 0.35 

0.5568 

0.6245 

0.6000 

0,5745 

0.6000 

0.5831 

0.5898 

1.52 

1.65 

1.65 

1,52 

1.43 

1.30 

1.34 

1.69 

1.56 

1.43 

1.56 

1,47 

1.51 

Stack Temp. (°F) Meter Temp. (°F) 

221 76 

222 80 

223 82 

224 84 

224 85 

222 87 

219 83 

223 86 

223 88 

224 89 

223 90 

223 90 

222.6 85.0 
ddddd• 

EEEEE 
Test Run No. 2 

Field Data Sheets 
ENTEC Services, inc. 

16-D Commerce Ave. Hueytown, Alabama 35023 

Client: 

Source: 

General Shale 

Kiln 38 B 

Test Date: 

Run Number: 

12/15/2005 

2 

FIELD DATA, EPA METHOD 26A 

Traverse Point 

1-1 

1-2 

1-3 

1-4 

1-5 

1-6 

2-1 

2-2 

2-3 

2-4 

2-5 

2-6 

K-Factor 

4175 

Delta P 

0.36 

0.28 0.5292 

0.37 

0.36 

0.38 

0.38 

Sq, Rt. Delta P 

0.6000 

0.6083 

0,6000 

0.6164 

0.6164 

0.38 0.6164 

0.40 0.6325 

0.40 

0,34 

0.40 

0.35 

0.37 

0.5325 

0,5831 

0.6325 

0.5916 

0.6049 

Delta H Stack Temp. (°F) Meter Temp. (°F) 

1.71 218 

1.33 218 

1.76 219 

1.71 

1.81 

1.81 

1.81 

1.90 

1.90 

1.62 

1.90 

1,66 

1.74 

228 

82 

82 

83 

83 

229 84 

226 84 

226 

226 

227 

228 

229 

225.0 

80 

82 

83 

84 

84 

226 85 

83.0 
dddddO• 

EEEEE 
Test Run No, 3 

Field Data Sheets 
ENTEC Services, inc. 

16-D Commerce Ave. Hueytown, Alabama 35023 

Client: General Shale Test Date: 12/1512005 

Source: Kiln 38 B Run Number: 3 

FIELD DATA, EPA METHOD 26A 

1-1 0.34 0.5831 1.62 221 

1-2 0.32 0.5657 1.52 220 

1-3 0.38 0.6164 1.81 222 

1-4 0.35 0.5916 1.66 

1-5 0.30 0.5477 1.43 

76 

76 

78 

223 79 

219 79 

1-6 0.32 0.5657 1.52 217 

2-1 0.36 0.6000 1.71 215 

2-2 0.33 0.5745 1.57 216 

8O 

77 

79 

2-3 0.37 0.6083 1.76 220 80 

2-4 0.35 0.5916 1.66 222 81 

2-5 0.39 0.6245 1.85 223 81 

2-6 0.34 0.5831 1.62 224 82 

K-Facto• 

4.75 0.35 0,5877 1.64 220.2 79.0 
E 
Control Room Production Data 

Quality Assurance / Quality 

Procedures 

Control 
QA / QC Procedures 

Specific quality assurance / quality control procedures were adhered to during this test 

project to provide valid and scientifically defensible data. For any environmental field 

and laboratory measurement, a degree of uncertainty exists in the data due to inherent 

limitations of the measurement systems employed. The objective of a QA/QC program 

is to produce data of known precision, accuracy, representation, completeness and 

comparability. The objective in this test project was to determine compliance with 

applicable air permit requirements. The final data user in this project will be Louisville 

Metro Air Pollution Control District. 

The following section details all QC procedures followed during the manual sampling 

activities. 

Velocity I Volumetric Flow Rate 

Volumetric flow rates were determined during each isokinetic test run. The following 

QC steps were adhered to during these tests: 

Reported duct dimensions were checked by physical measurements to determine 

cross-sectional duct area. 

Pitot tube coefficients were determined based on physical measurement techniques 

as delineated in Method 2 

The Type-S pitot tube was visually inspected before and after sampling. 

The pitot tube was installed on the sampling probe with the proper orientation and 

spacing from the sampling nozzle. 

Before each series of tests, thermocouple readings for the silica gel impinger exit 

temperature were checked against an N.I.S.T. traceable thermometer. 

The oil manometer was leveled and zeroed before each test run. 

Both legs of the pitot tube were leak-checked before and after sampling. 

Proper orientation of the pitot tube was maintained while making measurements. 

The roll and pitch axis of the pitot tube was maintained at 900 to the flow. 

An average velocity pressure reading was recorded at each point instead of 

recording extreme high or low values. 

The pitot/manometer umbilical lines were inspected before and after sampling for 

moisture condensate. Lines were cleared if moisture was found. 

4:1 
Molecular Weiqht Determination-Instrumental Analysis 

The carbon dioxide and oxygen concentrations were determined using EPA Reference 

Method 3A. A sample of the flue gas was extracted from the gas stream during each 

test. Moisture was removed form the sample and was analyzed on a dry basis with an 

Instrumental gas analyzer. The QC steps adhered to during these tests are located in 

the o_o_•_,qen and Carbon Dioxide Determination-Instrumental Analysis portion of the 

QA/QC procedures section. 

Moisture Determination 

Stack gas moisture content (Bv•s) was determined by dividing the mass of moisture 

collected by the impingers and silica gel impinger by the standardized volume of gas 

sampled. The following QC steps were adhered to during these tests: 

The indicating silica gel was fresh for the first run and periodically inspected and 

replaced during runs, if needed. 

The analytical balance was placed in a clean, motionless environment for weighing. 

The balance was leveled and zeroed if necessary before each weighing. 

Preliminary silica gel impinger tare weights and post-run weights were weighed to 

the nearest 0.1 g. 

Before each series of tests, thermocouple readings for the silica gel impinger exit 

temperature were checked against an N.I.S.T. traceable thermometer. 

The silica gel impinger gas exit temperature was maintained below 68°F and 

recorded at every traverse point. 

Each impinger was wiped of surface moisture before post-run weighing. 

The volume of liquid captured was measured using a graduated cylinder with 1- 

milliliter increments. 

Particulate Matter Sampling 

Accurate particulate concentrations are dependent on the mass of particulate matter 

collected by the train and recovered after sampling, and the standardized gas sample 

volume measured. QC procedures that were followed so that representative particulate 

data was collected by the sampling system were: 

Only clean, well-maintained sampling equipment was used. 

Sampling ports were inspected and cleaned prior to sampling. 

All equipment was calibrated according to EPA standards. The dry gas meter was 
fully calibrated within the past 12 months using a set of calibrated orifices. 

The sampling train components exposed to sample gas were constructed of glass, 

Teflon or stainless steel. 

Accurate barometric pressure was recorded at least once per day. 

The dry gas meter thermocouples were compared to ambient temperature prior to 

the test run as a check on operation. 

Pretest and post-test leak-checks were completed (must be less than 0.02 cfm or 

4% of the average sampling rate). 

Before each series of tests, thermocouple readings for meter temperature, filter 

hotbox, probe, and filter exit temperatures were checked against an N.I.S.T. 

traceable thermometer. 

Readings of the dry gas meter, meter orifice pressure (AH), meter temperatures, 

filter hotbox temperatures, probe temperatures, and filter exit temperatures were 

taken at every traverse point. 

Probe and filter temperatures were monitored and maintained above 248 0 F. 

The filter exit temperature was maintained above 248 0 F. 

The gas meter was read to the thousandth of a cubic foot for the initial and final 

readings. 

The sampling velocity through the nozzle was maintained within 10% of the stack 

gas velocity (isokinetic sampling rate at 100+10%). 

All nozzle/probe recovery items were pre-cleaned and kept in containers when not 

being used. 

Filter recovery used tweezers to handle the filter, and was careful to include any 

filter fibers or pieces adhering to the filter holder. 

Probe and nozzle recovery included wiping the outer surface clean of dust before 

sample recovery. Sample recovery consisted of multiple brushing of the inner 

surface and twisting/rotating the probe during recovery operations. Transfer of 

acetone rinse to the sample container was accomplished without loss of liquid. 

Nozzle and probe brushes were rinsed after brushing inner surfaces. 

Liquid levels were marked on sample containers and sealed for shipment to the 

laboratory. 

Acetone rinse blank was collected for laboratory analysis. 

Prior to the initial run a y-factor check was performed to ensure that the meter was 

operating according to the original calibration to within 3% of the original y-factor. 
For the post-test calibration the alternative Method 5 post-test calibration 

procedures were used (Emission Measurement Center Approved Alternative 

Method ALT-009). 

Oxv_qen and Carbon Dioxide Determination-Instrumental Analysis 

The carbon dioxide and oxygen concentrations were determined using EPA Reference 

Method 3A. A sample of the flue gas was extracted from the gas stream during each 

test. Moisture was removed form the sample and was analyzed on a dry basis with an 

Instrumental gas analyzer. The following QC steps were adhered to during these tests: 

Upon the 02 and CO2 analyzer's initial use in the field, an interference check was 

conducted as outlined in EPA CFR 40 Part 60 Method 20. 

In accordance with EPA Method 3A a three-point (i.e., zero, mid-, and high-range) 

analyzer calibration error check was conducted on each reference analyzer prior to 

initiating the compliance testing. These checks were conducted (after final 

calibration adjustments were made) by injecting the calibration gases directly into 

each gas analyzer and recorded the responses. 

The analyzer calibration error was less than +/- 2% of the span for the zero, midrange, and high-range calibration gases. 

Zero and upscale calibration checks were performed both before and after each 

test run in order to quantify reference measurement system calibration drift and 

sampling system bias. 

The sampling system bias was less than +/- 5% of the span for the zero and 

upscale calibration gases. 

The zero drift was less than +/- 3% of the span over the period of each run. 

The calibration drift was less than +/- 3% of the span over the period of each run. 

The reference calibration gases used in this test program are certified following 

EPA Protocol Number 1 analysis. Copies of the calibration gas certifications are 

included in the instrument calibration section. 

Sulfur Dioxide Determination-Instrumental Analysis 

The sulfur dioxide concentrations were determined using EPA Reference Method 6C. A 

sample of the flue gas was extracted from the gas stream during each test. Moisture 

was removed form the sample and was analyzed on a dry basis with an Instrumental 

gas analyzer. The following QC steps were adhered to during these tests: 
Upon the SO2 analyzer's initial use in the field, an interference check was 

conducted as outlined in EPA CFR 40 Part 60 Method 20. 

For each individual analyzer, an interference check for at least three runs during the 

initial field test on a particular source category was performed according to in EPA 

CFR 40 Part 60 Method 6C (modified Method 6 train). 

Each modified method 6 inference check was within 7% of each Method 6C test 

run. 

The results are retained and reported with each test performed on that source 

category. 

In accordance with EPA Method 6C a three-point (i.e., zero, mid-, and high-range) 

analyzer calibration error check was conducted on each reference analyzer prior to 

initiating the compliance testing. These checks were conducted (after final 

calibration adjustments were made) by injecting the calibration gases directly into 

each gas analyzer and recorded the responses. 

The analyzer calibration error was less than +/- 2% of the span for the zero, midrange, and high-range calibration gases. 

Zero and upscale calibration checks were performed both before and after each 

test run in order to quantify reference measurement system calibration drift and 

sampling system bias. 

The sampling system bias was less than +/- 5% of the span for the zero and 

upscale calibration gases. 

The zero drift was less than +/- 3% of the span over the period of each run. 

The calibration drift was less than +/- 3% of the span over the period of each run. 

The reference calibration gases used in this test program are certified following 

EPA Protocol Number 1 analysis. Copies of the calibration gas certifications are 

included in the instrument calibration section. 
ENTEC SERVICES, INC 

FIELD QA/QC CHECKLIST 

PERMIT NUMBER: L• 

LOCATION: 

CO.T O 

PERMIT LIMITS: 

TEST METHODS USED: c•Lo J• MODIFICATIONS TO METHOD: 

CONTROL AGENCY: j•?• D 0• ]•1.•. •0./.•df•_O N SITE REPRESENTATIVE: f•(• •-•____. 

ENTEC PERSONNEL: •.•:•o ,,•. •'•;•J• PLANT CONTACT: •>• 

Was Calibration Data on site? (Methods 1-5 / CEMS CAL Gas) 

Was Stack Diameter Area & Traverse Points verified on field data sheets? 

Was a 10-minute Meter Orifice Check performed? 

Results of check •',.o 

Were Temperatures Verified (Pre & Post) w/NIST Traceable Thermometer? 

Was Preliminary Traverse w/Cyclonic Flow verification performed? 

YE__ S 

 ̧6. Was previous test data on source used to determine K factor? 

Was Probe & Hot Box Temperatures maintained at 248 +/- 25 o F? 

If not, explain 

Was Filter Outlet Temperature maintained at 248 +/- 250 F? 

If not, explain 

Was Orsat or Fyrite leak checked and standardization performed as required? 

Ambient 02 Reading "----- % Ambient CO2 Reading % 

10. 

11. 

12. 

13. 

14. 

Was Tedlar Gas Sampling Bags used? If not, explain tt/c• 

Were they leak-checked? Y or N 

Were Pitot Leak_reChecks performed & recorded on each field data sheet? 

Pitot inspected? (•or N Noted Visual Defects? ,k •o-.---•. 

Was Meter Leak Checks performed & recorded on each field date sheet? 

Was Nozzle Diameter measured & recorded on each field data sheet? 

Nozzle inspected .'• or N Noted Visual Defects? •..-•..•_ 

Was Silica Gel Verified, and recorded for each test run? 

Percentage Used during test Run No.'s 1 

15. Was Acetone Lot NumberJeri,f•e)•ancJ r•;orded on Field Data Sheet 

Signature (Test Team Leader):f•,"W{ ,f./'//7/•z/xLI-}•// ,g// 

Date: 

As required: Control room data supplied by: or fax. 

Revision August 2005 DLB z•6 
ENTEC SERVICES, iNC. 

METER ORiFiCE AND TEMPERATURE CHECKS 

Date: /•/ I•- 

Meter Box Number: 

Original AH@ 

Location: 

Barometric Pressure: 

Original Y: 

Hg 

Bi-Annual Calibration Date: _,Oq i• )O• 

RUN METER FOR EXACTLY 10.0 MINUTES 

Orifice Manometer 

Reading AH equal to 

Dry Gas Meter Readings: 

Dry Gas Volume, fP 

Initial Final 

Dry Gas Meter Inlet 

Temperature, °F 

Initial 

Dry Gas Meter Outlet 

Temperature, °F 

Final Initial 

Total Volume: Average: Average: 

Vm = Volume of Dry Gas Meter 

Tm = Average Temperature of Dry Gas Meter in degrees Rankin (+460) 

PBarm = Barometric Pressure 

Final 

Yc = 10NmX 4{ 0.0319 X Tm/PBarm} 

= 10/( -7 .•ob ) x •/{ 0.0319 x ( 555,5 )/( ,9•. 3Lo )} 

Is Yc < +/- 3% of Original Y ? 

Thermocouple Check (all temperatures are in o F) NIST Traceable 

Thermocouples/I.D, 

Stack/ 

Probe 

F,ter 

Filter Exit/ ,•,Wb/ 

Meter Outlet/ •-" 

Impinger Exit/ 

Ambient Temp. Reference Temp. 

Pre Post Pre / Post 

5-5 / 5• 

5 LI 

5ff 

•q 

Revision 0 January 2005 DLB 

Acceptance Range 

+/- 7.5 o 

+/- 5.4 o 

+/- 5.4 o 

+/- 2.0 o 

+/- 5.4 o 

+/- 2.0 o 

+/- 5.4 o 
ENTEC Services, Inc. 

16 D Commerce Ave, Hueytown, AL 35023 

Preliminary Traverse & Cyclonic Flow Verification 

Client: General Shale Test Date: 12/15/05 

Source: Kiln 38 B Run No,: Preliminary Test 

Traverse Point Delta P Sq. Rt. Delta P 

1-1 0.300 

1-2 0.340 

1-3 0.350 

1-4 

1-5 

1-6 

2-1 

2-2 

2-3 

Average 

0.330 

0.300 

0.270 

0.340 

0.350 

0.340 

0.5477 

0.5831 

0.5916 

0.5745 

0.5477 

0.5196 

0.5831 

0.5916 

0.5831 

2-4 0.330 0.5745 

2-5 0.300 0.5477 0 

2-6 0.280 0.5292 0 

0.32 0.5644 

Note: Based on the preliminary traverse the flow is not considered cyclonic 

Null Reading (Angle) 

0 

Stack Temp. (°F) 

221 

225 

0 226 

0 227 

0 228 

228 

220 

0 222 

0 226 

0 228 

230 

230 

0.00 225.9 
Date 

Analyzer Model 

Component 

Analyzer Serial No. 

Span 

Cylinder ID 

CC 123630 

CC123630 

CC123630 

CC172148 

CC172148 

7/16/2004 

Ultamat 23 

Oxygen 

584 

0-25 % 

Test Gas 

CO 

02 

C02 

02 

Interference Response Test 

Concentration Analyzer Response Difference % of Span 

2O0 

5OO 

0.40 20.9 21.0 0.1 

0.20 10.08 

10.05 

10.1 

Total 

0,05 

0.15 0,60 

*Specification (EPA Method 20) Sum of interference responses must not exceed 2% of span 

% of Span Analyzer Response X 100 

Instrument Span 
Interference Response Test 

Date 

Analyzer Model 

Component 

Analyzer Serial No 

Span 

Cylinder iD 

7/16/2004 

Ultamat 23 

Carbon Monoxide 

0584 

0-1000 ppm 

Test Gas Concentration Analyzer Response 

CC123630 S02 200 

CC123630 CO 500 503 

CC123630 02 20.9 

CC172148 CO2 10.08 

CC172148 02 10.05 

Total 

Difference % of Span 

3.0 0.30 

3.00 

*Specification (EPA Method 20) Sum of interference responses must not exceed 2% of span 

% of Span Analyzer Response X 100 Instrument Span 
Date 7/16/2004 

Analyzer Model Bovar 72"1M 

Component Sulfur Dioxide 

Analyzer Serial No 8549-7 

Span 0-210 ppm 

Interference Response Test 

Cylinder ID Test Gas Concentration Analyzer Response Difference % of Span 

-1.67 CC123630 SO2 200 196.5 -3.5 

CC123630 CO 500 

0.05 CC172148 CO2 10.08 0.1 0.1 

CC123630 O2 20.9 

Total 3.4 1.32 

*Specification (EPA Method 20) Sum of interference responses must not exceed 2% of span 

% of Span Analyzer Response X 100 Instrument Span 
ENTEC Services, inc. 

Method 6C Interference Checks 

Source Category 

Power Boiler 

Power Boiler 

Power Boiler (Coal/Sludge as fuel) 

Thermal Oxidizer 

Serial Number 

721AT/7839-1 

721M/8549-7 

721 M/8549-7 

Client 

Sonoco 

Appleton 

Appleton 

Smurfit Stone 

Job No. 

24128 

24159 

24159 

Date 

9/8/04 

9/27/04 

9/28/04 

721AT/7839-1 25119 3/29/05 

Thermal Oxidizer 721M/8549-7 Smurfit Stone 25119 3/29/05 

Recovery Boiler 721M/8549-7 

No. 3 Kiln Aggregate 

No. 3 Kiln Aggregate 

ime Kiln 

Brick Kiln 

25119 

25130 

4/6/05 

721AT/7839-1 4/20/05 

Smurfit Stone 

Big River 

721M/8549-7 Big River 25130 4/20/05 

25145 6/1/05 

25144 6/22/05 

721 M/8549-7 

721M/8549-7 

Weyerhaeuser 

Pine Hall Brick 

5• 
Laboratory Analysis 
ENTEC SERVICES, iNC 

LABORATORY SAMPLES QA / QC CHECKLIST 

SOURCE TESTED: 

ANALYSIS: 

LOCATION: 

SAMPLING DATE(S): 

Description of Impinger Contents: 

Test Run No.'s 1 •__•\•_•" 2: (_•/-L•.X" 3: •{b_•r 

Impinger Contents Container Number: 

Test Run No.'s 1: •-•- 2: •'•- •. 3: • --._• 

Samples Sealed and Stored in Secure Container? (•r N 

Liquid Level Marked? •or N 

Filter ID Number: 

Test Run No.'s 1 

Description of Particulate on Filter: 

Test Run No.'s 1: 

Filter Container Number: 

Test Run No.'s 1: 

Samples Sealed and Stored in Secure Container? •3r N 

Probe Rinse Container Number: 

Test Run No.'s 1: T 2• \ 2: 1•L-2 

Samples Sealed and Stored in Secure Container? (•or N 

Liquid Level Marked? •_•r N 

Probe Rinse Reagent: 

Laboratory Blanks: 

Probe Rinse: v 

'• 

3: 

Lot Number: •'),• (• •L,j•, 

Impinger: • Filter: Other: 

Were samples analyzed by Entec Services, Inc.? Y or•l.• 

If not, Laboratory Performing Analysis: "_•-• \ 1⁄2•0•. 

If using outside laboratory services please fill out the following chain of custody. 

Signature: • q.• (L.•I;•;•, f_)# L•:L• j•;',•.•'Z L 

Date: / Signature: 

Print Name: Tim•/•. •' Signature (Project Manager or Team Leader): 

Revision 2 September 2005 TLj 54 

Print Name: 
:lient: 

City/State: 

Source: 

Job No.: 

Balance: 

Balance ID: 

Laboratory Data 

Particulate Matter Gravimetri< Analysis 

Final Weight Final Weight 2 

General Shale 

Louisville, Kentucky 

Kiln 38 B 

25186 

Denver Instrument 

P0090122 

Analyst: 

Bar. Press, In hg: 

Log Book Page No. 

Lab Amb. Temp, °F: 

Lab Rel. Humidity, %: 

Calibration (100000 mg) 

J. Lotz 

29.68 

192 

71 

31 

100000.0 rng 

J. Lotz 

29.56 

192 

78 

30 

100000.0 rng 

Filters 

Test No. 2 3 

Filter ID No. 1387 1388 1389 

1/4/05 

1/5/05 

9:10 

12:11 

Initial Weight, mg 288.6 289.9 291.6 

Average 288.6 289.9 291.6 

Final Weight, mg 289.6 290.7 291.8 

Average 289.6 290.6 291.8 

Acetone Wash 

Beaker ID No. 

Volume of Acetone, ml 

Initial Weight, mg 

Average 

119 

100 

3,704.7 

3,704.7 

123 

150 

3,946.1 

3,946.1 

134 

190 

3,680.8 

3,680.8 

1/4/05 9:10 

1/5/05 12:11 

Final Weight, mg 

Final Weight, mg 

Average 

3,705.7 3,950.3 3,684.8 

3,706.2 3,950.1 3,684.7 

3,706.0 3,950.2 3,684.8 

Acetone Blank 

Beaker ID No. BLK 

Volume of Acetone, ml 

Initial Weight, mg 

Average 

2OO 

3,787.8 

3,787.8 

1/4/05 

1/5/05 

9:10 

12:11 

Final Weight, mg 3,787.8 

Final Weight, mg 3,787.8 

Average 3,787.8 

Total Weight of Particulate Collected 

Weight of Particulate Collected on Filter, mg 

Weight of Particulate in Acetone Probe Wash, mg 

Weight of Acetone Blank, mg 

Density of Acetone 

Acetone Blank Residue Concentration, mg/g 

Percent of Acetone Blank Weight 

Weight of Residue in Acetone Probe Wash, mg 

Total Weight of Particulate Collected, mg 

0.95 

1.25 

0.00 

0.7848 

0.0000 

0.0000% 

0.00 

2.2 

0.65 

4.10 

O00 

0.7848 

0.0000 

0.0000% 

0.00 

4.7 

0.20 

3.95 

0.00 

0.7848 

0.0000 

O.OOOO% 

0.00 

4.1 

Laboratory Note: 

In no case shall a blank residue greater than 0.01 mg/g or 0.001% of the weight of the blank be subtracted from the sample weight 
ENTEC SERVICES, 

Chain of Custody 

INC. 

Client 

Contact: 

Phone No: 

General Shale 

Louisville, Kentucky 

Martha West 

Project # 25186 PC # 20595E 

Lab Name Stillbrook 

Lab Invoice # •1 i5"-• 

Entec Job No. # 25186 

Samples Collected by: 

Send Results to: 

Phone Fax Results To: 

Lalan Kirby 

Tommy Lotz, Jr C/O: Entec Services 

Kiln 38B Run1 

Kiln 38B Run2 

Kiln 38B Run3 

Kiln 38B Blank 

Kiln 38B Blank 

12/15/2005 323.0 

317.6 .1N H2SO4 

318.9 .1N H2SO4 

210.9 .1N H2SO4 

230.7 DI Water 

Signature: •J•--•_• Date: ]c• //• /•,.•Signature: 

Print Name: • Time (24hr): JLb• Print Name: 

Signature: Date: / Signature: 

Print Name: Time (24hr): Print Name: 

SPECIAL INSTRUCTIONS COMMENTS: 

56 
Envitonmental Testing Laboratory, 

30% Crawford Street 

Fairfield, AL 35064 

(205) 788-1750 

•lient: Mr. Tommy Lotz, Jr. 

Entec Services, Inc. 

16D Commerce Avenue 

Hueytown, AL 35023 

Date: 

Lab Invoice #: 22157 

December 2•, 20d5 

Project Name: General Shale Project Number: 25186 

Project Location: Louisville, Kentucky P.O. Number: 20595E 

Sample Matrix: Liquid 

Sampled By: Lalan Kirby Date Collected: December 15, 2005 

Test Method: "Methods for Chemical Analysis of Water and Wastes", EPA-600/4-79-020. 

LIQUID ASSAYS 

Lab I.D.: 66711 66712 66713 

Kiln 38B Kiln 38B Kiln 38B 

Field LD.: Run 1 Run 2 Pun 3 

PARAMETERS ............ a 

Total HCL 1.09 1.29 1.08 

!Total HF BDL BDL BDL 

DiLJUNIT8 

0.02 Total mg 

0.02 Total mg 

NUMBER 

300.0 

300.0 

22-Dec-05 

22-Dec-05 

1045 MD 

1045 MD 

Lab LD.: 

"•ield I.D.: 

•RAMETERS 

Total HCL 

Total I--IF 

Detection limit, practical 

BDL=Below Detection Limit 

*Analyst Note: 

66714 66715 

Kiln 38B Kiln 38B 

Blank Blank 

H2SO4 D.I. Water 

5.01 0.53 

BDL BDL 

D, L/UNITS 

0.02 mg/L 

NUMBER DATE 

300.0 22-Dec-05 

0.02 mg/L 300.0 22-Dec-05 

Sample volumes were measured in the laboratory to insure no change in volume occured. 

:TIME ANALYST 

1045 MD 

1045 MD 

ADEM Laboratory Certification I.D.# 40710 
STILLBROOK 

Environmental Testing Laboratory, Inc. 

305 Crawford Street 

Fairfield, AL 35064 

•205) 788-1750 

Slient: Mr. Tommy Lotz, Jr. 

Entec Services, Inc. 

16D Commerce Avenue 

Hueytown, AL 35023 

Lab Invoice #: 22157 

Project Name: General Shale Project Number: 25186 

Project L•cation: Louisville, Kentucky PoOo Number: 20595E 

Sample Matrix: Liquid 

Sampled By: Lalan Kirby Date Collected: December 15, 2005 

Lab Analyst: MD Date/Time Analyzed: December 22, 2005 @ 1045 _•est M•t_h_.•_•__.i'___M__ethods r •hemicalA___n___a_l__ysis o_f___Wat_ e f and Wastes", EPA-600/4-79-020. Method 300.0. 

QUALITY CONTROL DATA 

ERA Minerals Reference Control Lot #Pl17506 

Chloride Assayed: 48.4 mg/L 

Flouride Assayed: 3.54 mg/L 

Range: 43.8-53.2 mg/L 

Range: 3.28-4.14 mg/L 

Respectfully submitted, 

j•'John T. B)ooks 

President 

ADEM Laboratory Certification I.D.# 40710 
Blank Correction Sheet 

Company 

Project # 

Water blank 

Acid blank 

General shale MDL 

25186 

0.53 mg/I as HCI 

5o01 mgll as HCI 

0.02 mg/l 

Total HCl, mg 

Total volume ml 

Net gain (ml) plus 200 

Rinse volume, ml 

Adj Acid 

Adj Water 

Corr HCl, mg 

Reported Value, mg 

Kiln 

Run 

1.09 

323 

253.5 

69.5 

1.00 

0.04 

0.05 

0.05 

Run 2 

1.29 

317.6 

254.8 

62.8 

1.00 

0.03 

0.25 

0.25 

Run3 

1.08 

318.9 

251.5 

67.4 

1.00 

0.04 

0.04 

0,04 

from lab report 

Total volume-from lab report 

Net gain of liquid (ml) plus initial 200 ml 
Instrumental Analyzer Calibrations 
Analyzer Calibration Error 

Test Performed For: 

General Shale 

Louisville, Kentucky 

Kiln Stack 38B 

Initial Compliance 

Date: 12/15/05 

Oxygen Monitor 

Full Scale: 25.00 % 

Test Performed By: 

Entec Services, Inc. 

Birmingham Division 

Test Trailer 904 

Tommy Lotz, Jr. 

Run 

Method 3A 

Serial Number: Siemens Ultramat 23 

Cylinder Reference Gas Analyzer Difference Calibration 

Number Concentration Response Error (%) 

XC035004B/cg3 0.00 % 0.05 % 0.05 % 0.20 % 

XC636114B/cg6 10.00 % 10.09 % 0.09 % 0.37 % 

SG9161375/cgl 20.50 % 20.54 % 0.04 % 0.16 % 

Carbon Dioxide Monitor 

Full Scale: 25.00 % 

Method 3A 

Serial Number: Siemens Ultramat 23 

Cylinder Reference Gas Analyzer Difference Calibration 

Number Concentration Response Error (%) 

XC035004B/cg3 0.00 % 0.04 % 0.04 % 0.16 % 

XC636114B/cg6 9.93 % 9.89 % -0.04 % -0.16 % 

CC171266/cg2 22.10 % 21.88 % -0.22 % -0.88 % 

Sulfur Dioxide Monitor 

Full Scale: 100.0 ppm 

Method 8C 

Serial Number: Bovar Model 721-M SN 

Cylinder Reference Gas Analyzer Difference Calibration 

Number Concentration Response Error (%) 

XC636114B/cg6 0.0 ppm 0.0 ppm 0.0 ppm 0.00 % 

XC035004B/cg3 50.6 ppm 50.4 ppm -0.2 ppm -0.19 % 

CC29799/cg5 91.3 ppm 91.4 ppm 0.1 ppm 0.10 % 
Sampling System Bias and 

Test Performed For: 

General Shale 

Louisville, Kentucky 

Kiln Stack 38B 

Initial Compliance 

Date: 12/15/05 

Test Performed By: 

Entec Services, Inc. 

Birmingham Division 

Test Trailer 904 

Tommy Lotz, Jr. 

Run 

Monitor 

Type 

02 

CO 2 

CO• 

SO 2 

SO• 

Analyzer Cal 

Response 

0.05 % 

10.09 % 

O.04 % 

9.89 % 

0.0 ppm 

50.4 ppm 

Initial Cal 

Value 

0.05 % 

9.66 % 

0.03 % 

9.59 % 

3.5 ppm 

50.6 ppm 

Pre Run 

Bias (%) 

0.00 % 

-1.72 % 

3.50 % 

0.20 % 

Final Cal 

Value 

0.01% 

9.99 % 

-0.05 % 

9.87 % 

3.4 ppm 

50.4 ppm 

Post Run 

Bias (%) 

3.40 % 

0.00 % 

Total Run 

Drift (%) 

-0.16 % 

1.32 % 

-0.32 % 

1.12% 
System 

Test Performed For: 

General Shale 

Louisville, Kentucky 

Kiln Stack 38B 

Initial Compliance 

Date: 12/15/05 

Test Performed By: 

Entec Services, Inc. 

Birmingham Division 

Test Trailer 904 

Tommy Lotz, Jr. 

Run 2 

Monitor Analyzer Cal Initial Cal Pre Run Final Cal Post Run Total Run 

Type Response Value Bias (%) Value Bias (%) Drift (%) 

02 0.05 % 0.01% -0.16 % 0.05 % 0.00 % 0.16 % 

02 10.09 % 9.99 % -0.40 % 10.03 % -0.24 % 0.16 % 

CO2 0.04 % -0.05 % -0.36 % -0.02 % -0.24 % 0.12 % 

CO2 9.89 % 9.87 % -0.08 % 9.88 % -0.04 % 0.04 % 

SO2 0.0 ppm 3.4 ppm 3.40 % 2.3 ppm 2.30 % -1.10 % 

SO2 50.4 ppm 50.4 ppm 0.00 % 50.9 ppm 0.50 % 0.50 % 
Sampling System Bias and Drift 

Test Performed For: 

General Shale 

Louisville, Kentucky 

Kiln Stack 38B 

Initial Compliance 

Date: 12/15/05 

Test Performed By: 

Entec Services, Inc. 

Birmingham Division 

Test Trailer 904 

Tommy Lotz, Jr. 

Run 3 

Monitor 

Type 

02 

CO 2 

CO 2 

SO• 

SO 2 

Analyzer Cal 

Response 

0.05 % 

10.09 % 

0.04 % 

9.89 % 

0.0 ppm 

50.4 ppm 

Initial Cal 

Value 

O.O5 % 

10.03 % 

-0.02 % 

9.88 % 

2.3 ppm 

50.9 ppm 

Pre Run 

Bias (%) 

0.00 % 

-0.24 % 

-0.24 % 

-0.04 % 

2.30 % 

0.50 % 

Final Cal 

Value 

0.04 % 

9.87 % 

0.01% 

9.85 % 

3.0 ppm 

51.6 ppm 

Post Run 

Bias (%) 

-0.12 % 

-016 % 

3.00 % 

1.20 % 

Total Run 

Drift (%) 

-0.04 % 

-0.64 % 

0.12% 

-0.12 % 

0.70 % 

0.70 % 

6'4 
Certificate of Analysis: EPA Protocol Mixture Airoas Specially Gases 

Cylinder Number: CC171266 Reference Number: 

Cylinder Pressure: 1999.6 PSIG Expiration Date: 

Certification Date: 4/25/2005 Laboratory: 

Certified Concentrations 

Component Concentration 

OXYGEN 4.941% 

CARBON DIOXIDE 22,10 % 

NITROGEN Balance 

54-124034931-4 

4/25/2OO8 

ASG Chicago IL 

12722 South Wentw0•h Avenue 

Chicago, IL 60628 

www.airgas.com 

Accuracy •nal•icel F•rin--¢i-Ple Procedure 

+/- 1% Paramagnetic G1 

÷/- 1% NDIR G1 

Certification performed in accordance with "EPA Traceability Protocol (Sept. 1997)" using the assay procedures listed. Analytical Methodology does not require correction for analytical interferences. 

Notes: 

Do not use cylinder below 150 psig. 

Reference Standard •nformation 

NTRM 970514 

NTRM 980513 

Analytical Results 

1 st Component 

st Analysis Date: 

R 4,52 S 4.94 

S 4.94 Z 0 

7. 0 R 4.52 

Approval Signature 

CARBON DIOXIDE 

OXYGEN 

OXYGEN 

04/25/2005 

Z 0 Conc 4.941% 

R 4.52 Conc 4.941% 

S 4,94 Conc 4.941% 

AVG: 4.941% 

SG9182135BAL 

SG9182168BAL 

2rid Component 

1st Analysis Date: 

R 19.37 S 22•10 

S 22.09 Z 0 

Z 0 R 19.37 

19.37 % 

4.521% 

CARBON DIOXIDE 

04/25/2005 

Z 0 Conc 22.10 % 

R 19.37 Conc 22.09 % 

S 22.10 Conc 22.10 % 

AVG: 22.10 % 
Certificate of Analysis: EPA Protocol Gas Mixture 

Cylinder Number: XC036114B Reference Number: 

Cylinder Pressure: 1999.6 PSIG Expiration Date: 

Certification Date: 3/28/2005 Laboratory: 

Certified Concentrations 

Component Concentration 

CARBON DIOXIDE 9,930 % 

OXYGEN 9,997 % 

NITROGEN Balance 

83-124031311-1 

3/28/2008 

ASG Port Allen LA 

Airgas Specially Gases 

1075 Cinclare Drive 

Porl•len, LA 70767 

225.3•8.0900 Fax: 225,388,0959 

w•,,•,..awgas.com 

Certification performed in accordance with "EPA Traceability Protocol (Sept. 1997)" using the assay procedures listed. Analytical Methodology does not require correction for analytical interferences. 

Notes: 

Do not use cylinder below 150 psig. 

Reference Standard Information 

NTRM 81674 NITROGEN 

NTRM 82658 NITROGEN 

Analytical Results 

1st Component 

1st Analysis Date: 

R 7.00 S 10.08 

S 10.08 Z0.02 

Z 0,02 R 7,00 

Accuracy Analytical Principle Procedure 

+/- 1% NonDispersive Infrared G 

+/- 1% Paramagnetic G1 

Approval Signature 

• •vI,Number Concentr•tio n 

CARBON DIOXIDE XC018739B 6.89 % 

OXYGEN CC14322 9.72 % 

03/28/2005 

Z 0.03 Conc 9.990 % 

R 9.74 Conc 10,00 % 

S 10.02 Conc 10,00 % 

AVG: 9.997 % 

2nd Component 

03/28/2005 1st Analysis Date: 

Z 0.02 Conc 9.930 % R 9.73 S 10,01 

R 7.00 Conc 9.930 % S 10.02 Z 0.02 

S 10.08 Conc 9.930 % Z 0.01 R 9.75 

AVG: 9.930 % 
Tim Draheim 

rage o1: 

From: Dewayne Arnold [Dewayne.Arnold@Airgas.com] 

Sent: Thursday, April 14, 2005 2:59 PM 

To: Tim Draheim 

Subject: The cert you ask for. I'll bring by a hard copy. 

Certificate of Analys|s: EPA Protocol Gas Mixture 

Cyfincter N•n•ber:, SG9161375B•.L Reference Number: 54.12403291•I 

C•i•et •re: 1•.• •IG •ion •: 3• 

Cediflcat• •e: • L•atory: ASG Chicago IL 

Ce•ified C•cen•ons 

•a• •I•'.• • •t req•te c•¢•on for a=•l•i•l 

Notes: 

Oo not u•e cylinder 

Reference Standard I.formation 

Analyclcai Results 

I s( Component OXYGEI• 

Signature on file 

AVG: ,;0.50 .% 

4/14/2005 6 ?' 
Certificate of Analysis: EPA Protocol Gas Mixture 

Cylinder Number: XCO35004B Reference Number: 83-124041431-1 

Cylinder Pressure: 1999.6 PSlG Expiration Date: 8/1/2007 

Certification Date: 8/1/2005 Laboratory: ASG Port Allen LA 

Certified Concentrations 

C-•mponent C o n centl•a-•i o- • Accuracy---- 

SULFUR DIQXIDE 50.59 PPM +/- 1% 

N!•=_RO•EN_ Balance 

Airgas Specially Gases 

1075 Cinclare 0rive 

Port Allen, LA 70767 

225.388.0900 Fax: 225.388.0959 

www.airgas.c0m 

Conc 50.53 PPM 

Conc 50.52 PPM 

Conc 50.64 PPM 

AVG: 50.56 PPM 

Certification performed in accordance with "EPA Traceability Protocol (Sept. 1997)" using the assay procedures listed. Analytical Methodology does not require correction for analytical interferences. 

Notes: 

Do not use cylinder below 150 psig. Approval Signature ••L•• • 

Reference Standard Information 

• Balance G•s • CvI.Number Concentration, 

NTRM 81693 NITROGEN SULFUR DIOXIDE CC14464 44.4 PPM 

Analytical Results 

1st Component SUEFUR B!OXiDE 

1st Analysis Date: 07/25/2005 

R 0,304 S 0346 Z 0.000 

S 0.346 Z 0.001 R 0.305 

Z 0.000 R 0.304 S 0.347 

2nd Analysis Date: 08/01/2005 

R 0.307 S 0.349 Z 0.000 Conc 50.55 PPM 

S 0.349 Z 0.000 R 0,307 Conc 50.58 PPM 

Z 0,000 R 0.306 S 0.350 Conc 50.73 PPM 

AVG: 50.62 PPM 
Certificate of Analysis: 

Cylinder Number: CC29799 

Cylinder Pressure: 1999.6 PSIG 

Certification Date: 8/1/2005 

Certified Concentrations 

Component 

SULFUR DIOXIDE 

NITROGEN 

EPA Protocol Gas Mixture 

Reference Number: 

Expiration Date: 

Laboratory: 

83-124041423-1 

8/1/2007 

ASG Port Allen LA 

Concentration 

91.30 PPM 

Balance 

Accuracy 

+/-, 1% 

Airgas Specialty Gases 

1075 Cinclare Drive 

Port Allen, LA 70767 

226,388,0900 Fax: 225.388.0959 

wc•w, airgas.c0m 

Analytical Principle Procedure 

FTIR G1 

Certification performed in accordance with "EPA Traceability Protocol (Sept. 1997)" using the assay procedures listed, 

Analytical Methodology does not require correction for analytical interferences. 

XC017362B 

Notes: 

Do not use cylinder below 150 psig. Approval Signature 

Reference Standard •nformation 

• Balance Gas Component 

NTRM 81694 NITROGEN SULFUR DIOXIDE 

Analytical Results 

1st Component SULFUR DIOXIDE 

1st Analysis Date: 07/25/2005 

R 0.659 S 0.616 Z 0.000 

S 0.616 Z 0.000 R 0.660 

Z 0.000 R 0.660 S 0.617 

Conc 91.44 PPM 

Conc 91.36 PPM 

Conc 91.40 PPM 

AVG: 91.40 PPM 

Concentration 

98.0 PPM 

2nd Analysis Date: 08/01/2005 

R 0.667 S 0.621 Z 0.001 Conc 91.13 PPM 

S 0,622 Z 0.001 R 0.667 Conc 91.24 PPM 

Z 0.000 R 0.667 S 0.622 Conc 91.26 PPM 

AVG: 91.21 PPM 
Particulate Equipment Calibrations 
SAMPLING AND ANALYTICAL EQUIPMENT CALIBRATIONS 

All of the emission testing equipment used was calibrated according to the procedures 

outlined in the EPA CFR 40 Part 60 Appendix "A" and the Quality Assurance Handbook 

for Air Pollution Measurement Systems, Volume Ill, EPA-600/4-77-027b. 

TypeoS Pitot tube Calibrations 

The pitot tubes used for flow velocity measurement were checked for dimensions to 

verify a pitot coefficient Cp of 0.84. Documentation of the calibration and calibration 

check for dimensional measurements is provided. 

Saml•lin_• Nozzle Calibration 

Sampling nozzles were checked visually for nicks or damage and for dimensional 

calibration prior to testing by measuring the nozzle diameter in at least three planes 

using a Vernier micrometer. Measurements must agree to within +0.004-inches. 

Documentation is provided on the individual data sheets. 

Temperature Measurinq Device Calibrations 

Each temperature sensor (stack gas, dry gas meter, and impinger exit) and readout 

was calibrated at a minimum of two points over the anticipated range of use against a 

NIST-traceable mercury-in-glass thermometer. All sensors/readouts were calibrated 

prior to field sampling. Stack gas thermocouples must agree within 1.5% (expressed in 

°R) of the reference thermometer through out the entire calibration range. Dry gas 

meter thermocouples must agree within +5.4°F and impinger exit thermocouples must 

agree within +2°F. Documentation is provided. 

Dry Gas Meter Calibrations 

Dry gas meters were fully calibrated against a set of calibrated orifices. After assembly 

and leak checking, the console's pump is allowed to run for 15-minutes to warm up the 

dry gas meter and pump. For a pre-test full calibration, data are collected at five (5) 

orifice manometer (AH) settings of approximately: 0.32, 0.67, 1.2, 2.0, and 3.9 inches of 

H20. Gas volumes of at least 5 ft 3 

are used at all the orifice settings and critical 

vacuums were obtained at all of the calibration points. The individual gas meter 

correction factors (y•) are calculated for each orifice setting and averaged. The method 

requires that each of the individual correction factors fali within _+2% of the average 

71 
correction factor, or the meter be cleaned, adjusted or repaired and recalibrated. The 

orifice pressure differential (L•H@) that equates to 0.75 cfm of air at 68°F and 29.92 

inches Hg is calculated and along with the average correction factor (y) is marked on 

the meter console. 

For the post-test calibration the alternative Method 5 post-test calibration procedures 

were used (Emission Measurement Center Approved Alternative Method ALT-009). 

Prior to the initial run a y-factor check was performed to ensure that the meter was 

operating according to the original calibration to within 3% of the original y-factor. 

Analytical Balance Calibration 

The analytical balance used to weigh particulate filters and desiccated rinse samples is 

calibrated by comparing its readings against NIST Class 1 weights, with acceptable 

agreement within __.0.5 mg. The field moisture gain balance was also compared to NIST 

Class 1 weight, with acceptable agreement within + lgm. 

72 
0 
TYPE S PITOT TUBE iNSPECTiON DATA SHEET 

LEVEL 

Certification 

Parameter 

Assemb,.ly Level? 

Holes Damaged? 

Obstructed? 

A 

Z A sin •, 

W=Asine 

PA 

PB 

PA PB 

DT 

Thermocouple Cal. 

Thermocouple Cal. 

Value 

Yes 

No 

No 

0 

0 

0 

9O 

9O 

.849 

0 

0 

.425 

.425 

0 

Allowable Range 

Yes 

No 

-10 °<cd <+10 

-10 < o•2 < +10 

-5 < • 1 < +5 

-5 < •2 < +5 

for 1/4" OD, 0.526 to 0.750 

for 3/8" OD, 0.788 to 1.125 

Z < 0.125" 

W < 0.031" 

for 1/4" OD, 0.263 to 0.375 

for 3/8" OD, 0.394 to 0.563 

for 1/4" QD, 0.263 to 0.375 

for 3/8" OD, 0.394 to 0.563 

-0.063 to 0.063" 

.375 

70 

70 

0.188 to 0.375" 

Reference temp. 

Probe Thermocouple 

certify that the Type S pitot tube/probe ID # ESPo 64Cmeets or exceeds all specifications, 

criteria and/or applicable design features and is hereby assigned a pitot tube calibration 

factor Cp of 0.84 

Certified and Calibrated By: 

Date Certified: 

Lalan R. Kirby 

1/3/2005 

Annual Calibration 

?4 
ENTEC Services, •nco 

16-D Commerce Ave.Hueytown, Alabama 35023 

Calibration Date 1/3/2005 Calibrated by: Lalan Kirby 

Annual Thermocouple Calibrations 

Entec Ser•ces Temperature •Reference Therrnocouple Difference VVilhin 

Number Source Temperalure Temperature Degrees F Tolerance 

TC ambienl 67 69 y-es 

TC-2 ambient 67 67 Yes 

TC-3 ambient 64 66 2 Yes 

TC-4 ambient 62 61 yes 

FC-6 ambient 67 68 yes 

TC-7 ambient 64 64 yes 

TC-8 ambient 64 64 yes 

TC-9 ambient 67 68 Yes 

TC 10 ambient 67 68 yes 

TC-11 ambient 65 66 Yes 

TC• 12 ambient 65 66 Yes 

TC-13 ambient 65 65 Yes 

TC- 14 ambient 67 67 Y 

TC- 15 ambient 66 67 yes 

TC-16 ambient 66 67 yes 

TC- 17 ambient 66 67 Y 

TC-18 ambient 66 66 Yes 

TC-19 ambient 68 67 Yes 

TC-20 ambient 67 68 yes 

TC-21 ambient 67 67 0 Yes 

TC-22 ambient 67 67 0 Y 

TC-23 ambient 69 69 0 Y 

TC-24 ambient 67 68 yes 

TCS ambient 66 66 yes 

TCS ambient 67 67 0 Yes 

TCS ambient 66 68 Yes 

TCS ambient 64 66 2 Yes 

TCS amb!ent 6•6 •} Yes 

TCS ambient 64 64 Yes 

TCS ambient 64 66 Yes 

TCS ambient 66 66 0 Yes 

Fluke Hand Held Altek NIST 100 ICe 0 Yes 

f:lt.lke Hand Held Altek NIST !00 ICO 0 Yes 

;:luke Hand Held Altek NIST 100 I00 Yes 

Fluke Hand Field Altek NIST 1CO ICO Yes 

Blue Hand ble•d Altek NIS1 t00 !CO Yes 

LK Shernll 68 67 

Temperature i:olerance within 4./- 20 of acceptable ranges •or all thermocouples. 

Note: NIST Traceable Digital Thermome[er Serial Naraber 221209816 used reference temperature 
ENTEC Services, Inc. 

16-D Commerce Ave.Hueytown, Alabama 35023 

Calibration Date 1/'3/2005 Calibrated by 

Annual Thermocouple Calibrations 

Lalan Kirby 

Entec Se•ces Temperature '*Reference Themqocouple 

ID Number Source Temperature Temperature 

HOTBOX ambient 67 65 

HOTBOX 2 ambient 67 65 

HOTBOX ambient 67 65 

HOTBOX ambient 67 66 

HOTBOX ambient 67 65 

HOTBOX 6 ambient 67 66 

HOTBOX ambient 87 65 

HOTBOX ambient 67 66 

HOTBOX ambient 67 67 

HOTBOX 10 ambient 67 6• 

HOTBOX 11 ambient 67 66 

HOTBOX 12 ambient 68 67 

HOTBOX 13 ambient 68 67 

HOTBOX 14 ambient 88 67 

Difference 

Degrees 

Within 

Tolerance 

Yes 

Yes 

Yes 

Yes 

Yes 

Yes 

Yes 

Yes 

Yes 

Yes 

Yes 

Yes 

Yes 

G N ambient 66 67 

G N -2 ambient 66 67 

GN-3 amblent 66 67 

GN-4 ambient 66 66 

GN-5 ambient 67 88 

G N -6 ambient 67 67 

GN-7 ambient 67 68 

G N -8 ambient 66 67 

GN-9 ambient 67 68 

GN-10 ambient 67 68 

GN-11 ambient 67 67 

GN-12 ambient 68 67 

G N- 13 ambient 66 68 

G N- 14 ambient 67 67 

GN-15 amblen• 67 68 

GN- 16 ambient 67 69 

GN- ambient 66 67 

G N- 18 ambfent 66 67' 

GN-! amb',en[ 6; 

GN-20 amb;en[ 67 

GN-2 amblenl 68 69 

0 

0 

Yes 

Yes 

Yes 

Yes 

Yes 

Yes 

Yes 

Yes 

Yes 

Yes 

Yes 

Yes 

y•es 

Yes 

Yes 

Yes 

Yes 

Temperature tolerance •Nithin +/.. 20 of acceptable ranges For all thermocouples. 

Note: NIST Traceable Digital Therraometer Serial Number 22"1209816 ueed reference temperature 
Calibration complies with 

!SO 17025 

Trac•abte...•:• Certifi_cate of Calibration for Loll_i.•op 

Cert. No.,•3• •-1070700 

Thermometer 

Ma;nl:a•ning .'-'kc •; uta cy: 

Rm;atibrabon 

77 

.-•-4•,;• De •,er• h•st-mment Company.. 

Report of Traceability 

AJl Denver Inst:'ument Company weigh[s have been veritSed 0sina standards c,t mass 

traceable to the International Prototype Kilogram. (IPK)throueh_. the:' Nm•o[•a•' '-'" Institute oF 

Star•dards and Technology (NIS[),and meet or exceed speci 13cations tbr tv •e and class, 

Chain ofTraceability 

Class I/%%"eighl ranse: •: SIN: 03-J67313-21 Date: 04/04/03 

all weishts were found to be in lolerance see eh'4rl pa•e 2. 

Den cr In.•trumcn[ R,cportcd [..,: ncert:d n tie..s 

ff£f • ,3.240 m• 30,z O •• 71 n• I(J0n•,• 0.B•I2 

•ln• 0.00!2 

]',:,.'.l'l:: ,'.•F•.;:i:'. 12",•'; ;IrJ ::in,:::t.. ."-'C:. C.•,:'iCi]:. ;:,j :i:-: 7• }',.',;H] ::I•l;I,!;ll.:,;: .:l•' '.'- •:•,•.c,J ,• ),1•i ::'-... 

79 
LO• 

5-.0 >x-,9 

50 

CHEMICALS, INC. 

'•"• •-:, <::• :• 47-, 22 :, 

LOT ANALYSIS 

iTEM: 828 ACETO}TE, REAGE•TT (ACE) LOT•: P555428 

_-.:, _;,".. i<, f: ::• :-, :)% 

-_',$, ,.-: ":. :- • 

t• 3 ,'7 c; ,? • [• ..': _'*'. "'i.2,$" 

_--'f':Sg < ,-: 2, •, 5• % 
Nomenclature and Test Calculations 
NOMENCLATURE FOR OXYGEN/CARBON DiOXiDE 

Cgas 

C 

Co 

Cma 

= Effluent gas concentration, dry basis, % 

= Average gas concentration indicated by gas analyzer, dry basis, % 

= Average of initial and final system calibration bias check responses for the 

zero gas, % 

= Average of initial and final system calibration bias check responses for the 

upscale calibration gas, % 

= Actual concentration of the upscale calibration gas, % 

EQUATIONS FOR O:•/CO2 

C gas / (Cr• Co) 

)x(/o.• )/( •o•Y O.o • )= /7 

8'4 
NOMENCLATURE FOR SULFUR D•OXIDES 

Cgas 

C 

Co 

Cm 

Cma 

MW 

SO2 Ibs/hr 

385.1 x 106 

= Effluent gas concentration, dry basis, ppm 

= Average gas concentration indicated by gas analyzer, dry basis, 

ppm 

= Average of initial and final system calibration bias check responses 

for the zero gas, ppm. 

= Average of initial and final system calibration bias check responses 

for the upscale calibration gas, ppm 

= Actual concentration of the upscale calibration gas, ppm 

Molecular weight of SO2, which is equal to 64.06 

= Sulfur Dioxide mass rate in pounds per hour 

Conversion factor 

EQUATIONS FOR SO2 

Cgas (C-C 0 ) X (Cma) / (Cm Co) 

=( f•-.•: -•,• )x(•-z,,•. )/( •-• •-• •.,,•. )= /1•6, 

16• S02 Ibs/dscf = Cgas X MW / 385.1 x 10 6 

= ( /•ic • •7 )x (64.06)/(385.1 x 106) = "2, •,0::•, }:(• • 

• SO2 Ibs/mmBTU= SO2 Ibs/dscf x F-factor x ((20.9/(20.9-02)) 

= ( ) x ( )x((20.9/20.9-( ))= 

•. SO2 Ibs/mmBTU= SO2 Ibs/hr/Heat Input mmBTU/hr 

=( )/( ) 

21. SO2 Ibs/hr = SO 2 Ibs/dscf x DSCFM x 60 

=(,Z•,•,• •:-•)x( /f,• )x(60)= 3'.0 /2.•' 
As 

A• 

ACFM 

Bws 

C• 

C• 

C• 

AH 

AP 

dscf 

EA 

E/Btu 

F 

K• 

M• 

M• 

M• 

Pbar 

Pg 

Pm 

PMR 

Ps 

Pstd 

Q• 

Q• 

Qstd 

TB• 

TV•c 

TVwstd 

Tm 

Tstd 

V• 

V• 

Vrna 

Vmstd 

V• 

Vwcstd 

Vwsgstd 

W•mp 

Wsg 

Y 

NOMENCLATURE 

Cross-sectional area of stack, square feet 

Cross-sectional area of nozzle, square feet 

Actual cubic feet of gas per minute at stack conditions 

Proportion by volume of water vapor in gas stream 

Particulate concentration in stack gas, gr/dscf 

Particulate concentration in stack gas, gr/acf 

Pitot tube coefficient 

Pressure drop across orifice meter, inches water 

Velocity head of stack gas, inches water 

Cubic feet of dry gas corrected to standard conditions 

Excess Air 

Particulate Emission Rate, pounds/mmBtu 

F-factor, 9640 dscf/MMBTU's of heat input 

Constant (85.49) 

Total particulate matter collected, mg 

Molecular weight of stack gas; dry basis, Ib/Ib-mole 

Molecular weight of stack gas; wet basis, Ib/Ib-mole 

Percent of isokinetic sampling 

Barometric pressure, inches mercury 

Stack static pressure, inches of water 

Barometric pressure of dry gas meter, in. mercury 

Particulate mass rate, pounds/hour 

Absolute stack gas pressure, inches mercury 

Barometric pressure, standard conditions, 29.92 inches Hg 

Volumetric flow rate, actual conditions, ACF/min 

Volumetric flow rate, standard conditions, scf/min 

Volumetric flow rate, dry standard conditions, dscf/min 

Theoretical water vapor in the gas stream based on saturated stack conditions, proportion 

by volume (dimensionless) 

Theoretical volume of water collected based on saturated stack conditions, ml 

Theoretical volume of water vapor in the gas sample based on saturated stack conditions, 

corrected to standard temperature and pressure, scf 

Absolute average dry gas meter temperature, degree R (460) 

Absolute average stack gas temperature, degree R (460) 

Absolute temperature at standard conditions, 528 R 

Total sampling time, minutes 

Total volume collected in impingers and silica gel, gr 

Volume of gas sampled through gas meter, cubic feet 

Volume collected at stack conditions through nozzle, ACF 

Stack gas volume sampled, ACF 

Volume of gas sampled through gas meter, cubic feet 

Average stack gas velocity, feet/sec 

Volume of water vapor in gas sampled from impingers, standard cubic feet 

Volume of water vapor in gas sampled from silica gel, standard cubic feet 

Total volume collected in impingers, gr 

Total volume collected in silica gel, gr 

Dry gas meter calibration factor 
TEST CALCULATIONS 

EQUATIONS 

4a. 

4b. 

5. 

For saturated sources (No. 6 8 only): 

9. 

TBw== 10 637" {2827/(ts+365)}/Ps-- 10 6"37-{2827/( +364,8)}/( 

TVwstd Vmstd*( TBw=/1- TBw=)=( )*( )/( 

TVlc TVwstd/0.04707 =( / )= 

12. 

14. 

15. 

21. 

Md 0.44(%CO•2)+0.32(%O2)+0.28((100-(%CO2+%O2)) ,q •. =0.44( •_•' )+0.32(QtY•¢0.28(100-( + )= c? i-f 

V== 85.49 Cn* ?AP •/(T=/M=* P=) (For Iso calculation) 

=85.49*(0.84)*(, ,•" •- ••¢" 

Qa Ms* A,* 60=( 7¢ 

Q== Qa (528/T•)*(P=/29.92)=( )*(528/ )*( /29.92)= 

•:•'• •'• 

Q•t,= Q• (1- B,,,,•) (528/TD*(P•/29.92)=(2.$-:-, <7/<'.f ,•" ,,:;,'•xff )(1- ,c•. '•)*(528/U,#.7 t•,,( 2. /29.92)= / ) 

Cs=0.01543*(Mn/Vm•td)=0.01543*( ,• b 

E/Btu= (Cs/7000)*{(Fd*20.9)/(20.9-%O2)} 

=( /7000)*{( )*20.9)/(20.9-( )}= 

%EA= 100%* {(%O2)-0.5*(%CO)} {0.264(%N2) (%02)+ 0.5*(%CO)} 100%*{( )-0.5( )} {0.264( )-( )+0.5( 

PMR= C=* Q• (60/7000)=(b..c,.t,,.O,• •2 ),( l•,,fp•" )*(60/7000)= E:, ' • 7 

22. V•=T=/P•*{(0.002669) V,o+ (V•* Y P•)/T•)} 

=( •.• •/•7-t,•s<J*{(0.002669)(•i;,.. •..., )+( ql. 7o 7 

)( .<>•I )( )/( yw )}= $,,-.)'7/./7. !? $ 

C==0.01543" (MU Vn)=0.01543"( )= 

I=Vnl00/(e0*e*V•*An)=(S)q•" )100/(60)(•:-.O )( .•):;•, "t•"7•" )(•.•i,, )= )( ): 7 7 s I.•7