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:

Lotz, Tomm.)/ 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

SectionExecutive 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 23712
15162024282932353840464748495360657083Executive 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

ResultsSOURCE

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

123A426A 6CENTEC 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

7.717.5 % 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 0.11ENTEC 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 ProceduresProced 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 sealedcontainer. 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 24.50 126 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.

12instrument 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 GasesMethod 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-]

24Instrumental Data

SheetsTest Run

No.

1 Data SheetsCalculation 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

•7General 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 21.212/15/2OO5 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 4,26.19.3 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 7.89.0 13.4 15.8 17.9 21.6 18.6 19.0 169 17.8 17.7 17,7 17,4 18.0Test Run

No.

2 Data SheetsCalculation 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

21General Shale Louisville, Kentucky December 15, 2005 Kiln 38B
Run Number 22222222222222222222222222222

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 7.45.2 4.03.2 4.27.87,27,8 11.6 11.72222222222222222222222222222222 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

6,47.2 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 7.46.4 10.6 12,2 12.7 14.1 13.2 14.1 12,1 12.3 9.3 12.5Test Run

No.

3 Data Sheets

24Calculation 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 DRYRun Number
33333333333333333333333333333 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

5.65.65.65.25.4 4.9 4.8 4.02.6 2.22.01.91.9 2.12.22.93.73.23.02.72.11.81,8 2.12.32.6 2.92.82.33333333333333333333333333333333 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

6.57.07.47,46,97.37,17.67.98.17.69.17.14.35.96.87.27.37.47.57.67.37.67.67.97.8 7.57.26.75.8 10.4 5.2Particulate Field

Data

SheetsTest Run

No.

1 Field Data

Sheets

29ENTEC 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 1-51-6 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 85.0ddddd•

EEEEETest Run

No.

2 Field Data

SheetsENTEC 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 1-11-21-3 1-41-5 1-6 2-12-2 2-3 2-4 2-52-6

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

82828383 229 84 226 84 226 226 227 228 229

225.0 8082838484 226 85

83.0dddddO•

EEEEETest Run

No,

3 Field Data

SheetsENTEC 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 767678 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

8O7779 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

79.0EControl Room

Production DataQuality Assurance / Quality Procedures

ControlQA / 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.

4:1Molecular 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 wasfully 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{

,g//,f./'//7/•z/xLI-}•// Date:

As required:

Control room data supplied by: or fax. Revision August 2005 DLB z•6ENTEC 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

Average: Total Volume: 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 LI5ff •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 oENTEC 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 1-41-51-6 2-12-22-3

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

0.00 225.9Date 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

CO02C0202

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 SpanInterference 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 10.05 02

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 SpanDate 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 SpanENTEC 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 721M/8549-7 Recovery Boiler
No. 3 Kiln Aggregate
No. 3 Kiln Aggregate
ime Kiln Brick Kiln 25119 25130

4/6/05 4/20/05 721AT/7839-1 Smurfit Stone Big River Big River 721M/8549-7

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 AnalysisENTEC 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 1927131 100000.0 rng

J. Lotz 29.56 1927830 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 weightENTEC 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:

56Envitonmental 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 22-Dec-05 0.02 mg/L

300.0 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.# 40710STILLBROOK 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.# 40710Blank 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 mlInstrumental Analyzer CalibrationsAnalyzer 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. RunMethod 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 Type02

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 Type02

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 %

6'4Certificate 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 PPMCertificate 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 PPMParticulate Equipment CalibrationsSAMPLING 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
71correction 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.

720TYPE S PITOT

TUBE

iNSPECTiON

DATA

SHEET

LEVEL

Certification Parameter Assemb,.ly Level? Holes Damaged? Obstructed?

A Z A sin •, W=Asine PAPB PA PB DT Thermocouple Cal. Thermocouple Cal.

Value YesNoNo000

9O9O.84900.425 .4250

Allowable

Range YesNo

-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 7070 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

?4ENTEC 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 temperatureENTEC 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 temperatureCalibration 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 ::'-...

79LO•

5-.0 >x-,9

50CHEMICALS, 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

CalculationsNOMENCLATURE FOR

OXYGEN/CARBON DiOXiDE Cgas CCo

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

8'4NOMENCLATURE FOR

SULFUR

D•OXIDES Cgas CCoCmCma MWSO2 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 mmBTU/hr Input =( )/(

) 21. SO2 Ibs/hr

= SO 2 Ibs/dscf

x DSCFM

x 60 =(,Z•,•,• •:-•)x(

/f,•

)x(60)=

3'.0 /2.•'AsA•ACFM BwsC•C•C•AH APdscf EAE/Btu FK•M•M•M•PbarPgPmPMR PsPstdQ•Q•QstdTB• TV•c TVwstd TmTstd

V•V•VrnaVmstd 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

factorTEST 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)=

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