Pollution Control System Evaluation

and Source Emissions

Testing General Blue Ridge,

Shale Virginia

Brick

Co.

Compliance Plant 36 Kiln DLA Inlet DLA Outlet

Emissions

Testing

July 15, 2008 Entec Project

No.: 28164

16oD Commerce

Avenue

Hueytown,

Alabama

35023 Phone: (205) 491=6676

Fax (205) 491-6614 www.entecservices.comEn ec Services, inc. 16 D Commerce

Avenue Hueytown, Alabama

35023 Telephone: (205) 491-6676 Fax: (205) 491-6614 Results of the July 15, 2008 Compliance Emissions

Testing P•ant 36 Kiln DLA |nlet and Outlet

at the General Shale

Brick Company

located

in Blue Ridge,

Virginia Submitted to: General Shale

Brick

Company P.O. Box 3547 Johnson City, Tennessee

37602 Attention: Ms. IVlartha

West Entec Project

No. 28164 Completed By:

Art Otero Project Leader Report

Submitted

July 29, 2008 Reviewed By:

Tom Lotz Technical Services

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.General Shale

Brick Table of Contents

Section Executive

Summary Emissions

Summaries Detailed Test Results Sampling Procedures Diagram of Sampling

Train Diagram of Method

26A Sampling

Train Field Data Sheets

DLA Inlet Test Run No, 1 Test Run No. 2 Test Run No. 3 Field Data Sheets

DLA Outlet Test Run No. 1 Test Run No. 2 Test Run No. 3 Control Room Production

Data Quality Assurance

/ Quality

Control

Procedures Field QA / QC Checklist Meter Orifice and Temperature

Check Sheet Fyrite / Orsat Standardization

Sheet Test Protocol QSTI Documentation Laboratory Analysis Equipment Calibration Safety Documentation Test Nomenclature

and Calculations 125121618192024273O3135384143485055586974809193Executi Entec Services,

Inc. was retained

by General

Shale Brick Co. to perform

compliance emissions testing at the inlet and outlet of the DLA (Dry Line Adsorber)

for Plant 36 Kiln at the facility

located

in Blue Ridge, Virginia.

Mr. Art Otero, Mr. Johnathan

Cochran,

Mr. David Bowman

and Mr. Trent McMahan

of Entec Services,

Inc. conducted

the testing on July 15, 2008. Representing

General

Shale was Ms. Martha

West who coordinated

re- testing. Mr. William

Klepper

represented

the Virginia

Department

of Environmental

Quality (VDEQ). General Shale Manufactures

brick exterior

building

material.

Shale and clay are mined, crushed and sent through

a screening

process

prior to brick forming

by extrusion.

Once the brick is extruded,

it is dried and fired in a tunnel kiln at approximately

20000 F. The facility operates

two kilns (A and B) with a common

exhaust.

After being fired, the brick is cooled, packaged

and shipped

to various

locations.

The kiln emissions

are controlled

with an ohlmann

type DLA (Unit #6). The exhaust

stack is located

outside

the kiln building

on the east side. Entec Services,

Inc. did not deviate

from the Test Protocol

(enclosed)

nor did not encounter any difficulties

or problems

during the sampling

of this emissions

source.

The emissions test summaries

on the following

pages give a detailed

summary

of each test run compared to the maximum

emission

limits set forth by the Virginia

Department

of Environmental Quality

(VDEQ).

Tests results

indicate

that the ACL/HF

results

were below the applicable

permit

limit as set forth by •fDEQ Permit

No. V/•. 20447.0

0

0

0 "0 ¢•

O• 0 •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

ASSISTANT ENVIRONMENTAL ANALYST

ASSISTANT OWNER'S REPRESENTATIVE: RULING AGENCY RULING AGENCY

REPRESENTATIVE: DATES TESTS CONDUCTED: ENTEC PROJECT

NUMBER:

Entec

Services, Inco SOURCE OVERVIEW
General Shale Plant 36 Blue Ridge, VA DLA Inlet Annual Compliance

Re-Testing Square Acetone VA-20447 HCI/HF Testing Sample Location Volumetric Flow Molecular Weight Moisture Content HCI/HF Mr. Art Otero EPA Method EPA Method EPA Method EPA Method EPA Method

Mr. Trent McMahan Mr. Johnathan

Cochran Ms. Martha West Virginia Department

of Environmental

Quality Mr. William Klepper 07/15/08 28164 23426AENTEC Services,
16-D Commerce Ave. Hue o•t_•, Alabama 35023 INPUT TEST DATA Client: Source: General Shale Plant 36 DLA Inlet Field Data Run Number Test Date Time Test Run Began Ended Sampling T•ime 1 07/15/08 Job No.:

28164 Data Input By_

Art Otero

Military Time 1057-1200 minutes 60

Test Data
07/15/08 1316-1421 60

AVERAGE 07/15/08 1509-1613 6O 6O Stack Area Barometric Pressure Stack Static Pressure Pitot Tube Correction

factor Meter Correction

Factor A•__•____

Ft•

23.36•1

23.361 Pl•ar in. Hg

30.13

30.13 • in. H20

0.37

0.38 • 0.84

0.84 0.952 0.952 Meter Delta H @ Nozzle Diameter o___.__._•___, Meter Volume v,• •leter Temperature t•_• 23.361 30.13 0.37 0.84

30.13 0.37 0.84

•,vg. Orifice Delta H .•H mpingers Wei ht Gain (Moisture)

• ,•H@

in. H20___

1.867

1.867 inches 0.375

0.375 dcf 43.965

39.686 °F 89.7

102.7 in. H20

1,57

1.14 grams 51.7

43.8

0.952

0.952 1.867 1.867 0.375 0.375 48.832 44.161 104.8 99.1 1.87 1.52 53.1 49.5 •ilica Gel Impinger Weight Gain (Moisture) )xygen Concentration,

dry basis ;arbon Dioxide Concentration,

dry basis vg. Sq. Rt. of Delta P tack Temperature •tal Hydrogen

Chloride collected,

mg !!al Hydrogen

Fluoride collected,

mg

W88

grams

12.1

7.5 O2 %

17.0

17.0 CO2 %

3.0

3.0 (sqrt z•p),v• (in. H20) 1•= 0.340

0.291 ts °F

358.3

354.3 HCL mg

84.4

70.8 HF mg

284.0

245.0

11.1

10.2 17.0 17.0 3.0 3.0 0.374 0.335 354.3 355.6 105.0 86.7 300.0 276.3ENTEC Services,
16-D Commerce Ave. Hueytown, Alabama 35023 CALCULATED TEST DATA Client: Source: General Shale Plant 36 DLA Inlet Description

_/ Formulas Run Number Test Date •'ime Began-Ended Military Time 1. Stack Pressure Pb•r P•/13.( p= in. Hg 2. Meter Pressure Pb•r ,*-H 13.6 p• in. Hg 3. Standard Meter Volume 17.64" y* (Vn.JTm)* (pbaf AH 13.6 4a. Standard Volume of Water Vapor Condensed 4b. Standard Volume of Water Collected in Silica Gel

=0.04706"Wi, =0.04715°W, 5. Moisture Fraction 9. Molecular Weight Of Stack Gas, dry basis 10. Molecular Weight Of Stack Gas, wet basis

0.32'(0z)+ 0.44'(C02)+o.2a*(loo-(o2).(c0•))
11. Avera e Stack Gas Velocit 12. Stack Gas Flow @ Stack Conditions

85.49'C *(sqrt z•p)a *SQRT((T,) (p,*Mw)
13. Stack Gas Flow @ Standard Conditions 14. Stack Gas Flow @ Dry Standard Conditions t4b. Hydrogen Chloride concentration

@ Std.Cond.,Grains/Cu.Ft. 14b. Hydrogen Fluoride concentration

@ Std.Cond.,Grains/Cu.Ft. =5b. Hydrogen Chloride emissions, Ibs per hour 5b. Hydrogen Fluoride emissions, Ibs per hour 2. Volume collected through nozzle 4. Isokinetic Sampling Rate, Percent =(0.01543°H C Lpg)/Q=l• =(0.01 S43*H Fme)/Q,•,• =(60/7000)*H C LQ=¢•*O,•< =(60/7000)*H FQ,td*Q.I, =TJP,*[0.002669*V=o+ V•*¥*P•T• 100*Vn

Vm(=td)

dscf Vw,gf=ld} scf Bw, fraction Md g/g-mole M, g/g-mole

HFcs gr/dscf

HF -tbs/hr Ibs/hr

%
ost Meter Odfice Cal. (EMC ALT-009 Yqa) Difference, (Calibrat must be within 5% of ori•linal Y-factor} AVERAGE Job No.:

28164 Data In ut.E.•.,•

Art Otero Calculated Data 2 t 3 07/15/08 07/15/08

07/15/08 1057-1200 1316-1421

1509-1613 30.16 30.16

30.16

30.16 30.25 30.21

30.27

30.24 40,626 35.787

43.943

40.119 2.433 2.061

2.499

2.331 0.571 0.354

0.523

0.483 0.0688 0.0632

0.0644

0.0655 29.160 29.160

29.160

29.160 28.392 28.455

28.442

28.429 23.90• 20.3•6 •26.19•

23.485 33,503 28,541

36,710

32,918 21,780 18,•46

23,983

21,470 20,280 17,468

22,439

20,062 0.032 0.031

0.037

0.033 0.t08 0.106

0.105

0.106 5.57 4.57

7.09

5.74 18.75 15.82

20.26

18.2•8 67.115 58.475

71.891

65.82•7 101.69 104.00

99.41

101.70
0.9496 0.9064

0.9454

0.9338 1.91%SOURCE OVERVIEW
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

ASSISTANT OWNER'S REPRESENTATIVE: RULING AGENCY RULING AGENCY

REPRESENTATIVE: DATES TESTS CONDUCTED: ENTEC PROJECT

NUMBER: General Shale Plant 36 Blue Ridge, VA DLA Outlet Annual Compliance

Re-Testing Circular Acetone VA-20447 HCI / HF Testing Sample Location Volumetric Flow Molecular Weight Moisture Content HCI/HF Mr. Art Otero EPA Method EPA Method EPA Method EPA Method EPA Method

Mr. David Bowman Ms. Martha West Virginia Department

of Environmental

Quality Mr. William Klepper 07/15/08 28164 123426AENTEC Services,

inc. 16-D Commerce Ave. Hue_.•own, Alabama 35023 INPUT TEST DATA Client: Source: General Shale Plant 36 DLA Outlet Field Data Run Number Test Date Time Test Run Began Ended Sampling Time Stack Area Barometric Pressure Stack Static Pressure Pitot Tube Correction

factor Meter Correction

Factor Meter Delta H @

Meter Temperature Zkvg. Orifice Delta H i Nozzle Diameter Meter Volume
mpingers Weight Gain (Moisture) .•ilica Gel Impinger Weight Gain (Moisture) )xygen Concentration,

dry basis ;arbon Dioxide Concentration,

dry basis •vg. Sq. Rt, of Delta P ;tack Temperature otal Hydrogen

Chloride collected,

mg otal Hydrogen

Fluoride collected,

mg

Symbol

Units

Job No.:

28164 Data In By:

Art Otero Test Data 2 3

AVERAGE Military Time minutes 07/15/08

AsPbarP•Cp
¥&H@D.Vmtm Ft in. Hg in. H20

in. H20 inches dcf

1057-1200 6O 27.883 30.13 -0.12 0.84 0.978

Wlrnp

O2CO2 (sqrt &P)avo

HCL HF

F in. H20 grams grams %

Fmgmg

1.856 0.366 40.651 85.8 1.42 44.7 6.316.5 3.0 0.337 326.9 63.1 21.8

07/15/08 1317-1419 6O 27.883 30.13 -0.13 0.84 0.978 1.856 0.366 40.042 88.2 1.42 45.4 8.316.0 4.5 0.338 329.3 59.2

07/15/08 1507-1610 60

60 27,883 30.13 30.13 "0.11 -0.12 0.84 0.84 0.978 0.978 1.856 1.856 0.366 0.366 40.312 4O.335 95.2 89.7 1,39 1.41 45.9 45.3 8.1 7.6 16.0 16.2 4.0 3.8 0.334 0.336 329.9 328,7 55.5 59.3 19.5 20.6

10ENTEC Services,

inc. 16-D Commerce Ave. Hueytown• Alabama 35023 CALCULATED TEST DATA Client: General Shale Plant 36 Source: DLA Outlet Description Run Number Formulas

Symbol

Units
Test Date Time Began-Ended 1. Stack Pressure P•r Pg/13.£ Meter Pressure 3. Standard Meter Volume 17.64" y* (Vn.JTm)* (Ps=, •,H 13.6 4a. Standard Volume of Water Vapor Condensed =0.04706*W•mp 4b. Standard Volume of Water Collected in Silica Gel =0.04715*W=[ Moisture Fraction 9. Molecular Weight Of Stack Gas, dry basis 10, Molecular Weight Of Stack Gas, wet basis

=(V,•std) Vw=•i=td))/(Vw<o•,•)

V,=•(ot,• Vm(,•dll 0.32*(0=)+ 0.44"(CO2)+0.28"(100-(O=)-(COa)) Md*(1-Bw=)+10.0*(Bw, 11, Average Stack Gas Velocity 12. Stack Gas Flow @ Stack Conditions

85.49*Cp*(sqrt •'P)av•*SQRT((T,)

(P,*M•) 60*V•*A= 13. Stack Gas Flow @ Standard Condilions Q**(T,•,•T,)*(pJp,t 14. Stack Gas Flow @ Dry Standard Conditions 14b. Hydrogen Chloride concentration

@ Std.Cond.,Grains/Cu.Ft.

Q,*(1 ew.) '(l".,•JT,)*(pJp,•) ={0,01543*HCL•g)/Q,I 14b. Hydrogen Fluodde concentration

@ Std.Cond.,Graine/Cu.Ft. 15b. Hydrogen Chloride emissions, Ibs per hour 15b. Hydrogen Fluoride emissions, Ibs per hour !2. Volume collected through nozzle !4. Isokinetic Sampling Rate, Percent =(0.01543*HF•g)/Q=t =(60/7000)*H C LQ,td*Q,t =(60/7000)*H FQ=t•*Q=t =T=/P= *[0.002669'V;¢+ Vm*Y*pr,.jT•] 100*Vn (60*v=*An*e)
'ost Meter Orifice Cal. (EMC ALT-009 Yqa) Difference, (Calibration must be within 5% of original Y-factor Pm

M=M,

Q.

HCLcs HFcs

V. Military Time In. Hg in. H dsct scf scf fraction g/g-mole g/g-mole

acfm scfm dscfm gr/dscf gr/dscf Ibs/hr Ibs/hr

Job No.:

28164 Data ,•,u, •,.

utero Calculated Data
07/15/08 07/15/08

07/15/08

AVERAGE
1057-1200 1317-1419

1507•1610 30.12 30.12

30.12

30.12 30.23 30.23

30.23

30.23 38.846 38.101

37.872

38.273 2.104 2.137

2.160 0.297 0.391

0.382 0.0582 0.0622

0.0629

2.133 0.357 0.0611 29.140 29.360

29.280

29.260 28.492 28.653

28.571

28.572 23.20 23.18

22.97

23.118 38,820 38,781

38,425

38,675 26,212 26,105

25,847

26,055 24,686 24,480

24,222

24,463 0.025 0.024

0.023

0.024 0.009 0.008

0.008

0.008 5.30 5.03

4.69

5.01 1.83 1.73

1.65

1.74 61.088 60.359

60.080

60.509 100.09 99.00

99.45

99.51
0.9764 0.9896

0.9797

0,9819 -0.40%

11Sampling Procedures

12Procedures The emission

rates were determined

using EPA Methods

1, 2, 3, 4, and 26A of the CFR Title 40, Part 60, Appendix

A and Part 63 Subpart

JJJJJ (Brick MACT).

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

version

for each method

(as described

in the Federal Register) was used. Stack Gas Volumetric

Flow Methods

1 and :• 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

Weiqht

Method

3 The carbon

dioxide

and oxygen

concentrations

were determined

using EPA Reference Method 3 (Fyrite Method).

A sample

of the flue gas was extracted

from the gas stream during each test. These samples

were analyzed

with a Fyrite gas analyzer.

The molecular weight of the gas was calculated

using the moisture,

oxygen

and carbon

dioxide

content and the measured

stack gas temperature. Moisture Content

Method

4 The moisture

content

used for calculating

the gas stream

flow rate was determined

by measuring the amount

of condensed

moisture

in the impingers

in the sampling

train as described in EPA Reference

Method

4 at the completion

of each test. Ice is placed around the impingers

and the outlet temperature

of the impinger

is monitored

and recorded throughout the duration

of the testing to verify the temperature

is less than 68 o F.

13_H__y__d•o_clen Chloride

/ Hvdroqen

Fluoride

Method

26.• 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 after the test using a micrometer

and was recorded

on the field data sheets. The sampling

probe was placed at each sampling

point to provide

a total sampling

time of sixty (60) minutes.

The gases were drawn through

a Teflon coated

nozzle attached

to a heated glass lined probe.

The probe was maintained

at the proper settings

to obtain an exit temperature

of greater

than 2480 F during sampling.

The gases then proceeded through borosilicate

glass filter holder,

with a Teflon frit filter support

through

a Teflon filter to remove

particulate

matter.

The filter was maintained

at a temperature

of greater

than 248 o F. These temperatures

were recorded

at each point on the field data sheets. The gases were then scrubbed

through

a series of four pre-weighed

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 H2SO,•

(acid) solution

and the third and fourth impingers

contained approximately 100 ml of a 0.1 N NaOH (alkaline)

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 o 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. The cleanup

data was recorded. Each impinger

was weighed

for moisture

first verified

for moisture,

then the first and second impinger

contents

were transferred

to its container,

weighed

and the rinsing from the glassware

were added to this container.

The third and fourth impinger

was discarded. The silica gel from the fifth impinger

was weighed.

A blank of the sulfuric

acid solution 14was taken. These

containers

were clearly

marked

and transported

to our office. The samples were shipped

to Stillbrook

Laboratory.

15Entec Services,

Inc 16 D Commerce

Ave. Hueytown,

AL 35023 STACK DRAWING

& TRAVERSE

POINT LOCATION Client: General Shale Plant 36 Job No. 28164 Source: DLA Inlet Input By: Art Otero Equivalent Diameter, inches:

58.00 Type of Traverse: Velocity (V) or Particulate

(p) Length (Side with ports):

58 Width (Depth of port):

58 Port Type:

Nipple

Port Diameter Stack Properties:

Inches Stack Area, Ft2: 23.361 _P Length of Port, inches: 4 Total Number of Traverse Points:

25 Required Matrix: 5 x 5 4.0" Number of Points per port:

5 Duct Diameters

Ports Available: 3 0.58 Matrix Used: 8 x 3 3.10 Number of Points per port:

8 Upstream Disturbance:

33.6 Downstream Disturbance

180.0

58.0 INCHES 58.0 •NCHES

33.6 INCHES Inside Stack

Outside Nipple Point No. Diameter; Inches

Diameter; Inches 3.6 7.6 2 10.9 14.9 3 18,1 22.1 4 25.4 29.4 5 32.6 36.6 6 39.9 43.9 7 47.1 51.1 8 54,4 58.4

80.0 INCHES

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 9 if the 8 / 2 diameters downstream

and upstream criteria is met.

16Entec Services,

Inc 16 D Commerce

Ave. Huoytown,

AL 35023 STACK DRAWING

& TRAVERSE

POINT LOCATION Client: General Shale Plant 36 Source: DLA Outlet Job No. Input By: 28164 Art Otero Type of Traverse: Velocity (V) or Particulate (P):

p Stack Diameter, inches:

71.5 Stack Height, feet:

100 Stack Properties:

Inches

Duct Diameters Upstream Disturbance:

168.0

2.35 Downstream Disturbance:

840.0

11.75

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

71,5 INCHES

8o(• NCHES

Point No.

Inside Stack

Outside Nipple Inches Inches 3.1 8.1 2 10.4 15.4 3 21.2 26.2 4 50.3 55.3 5 61.1 66.1 6 68.4 73.4

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. 27.883 25.00126

17Method 26A

Sampling Train

Filter Exit Temperature (>2480 F) •

[2SO_._• • lmpinger Exit Temperature

Exhaust•.•
[•

i l•ry Gas Meier

18DLA Inlet Field Data

Sheets

19Test Run

No.

1 DLA In•et

2OENTEC Services,

inc. 16-D Commerce Ave. Hueytown, Alabama 35023 Client: General Shale Plant 36 Test Date: Source: DLA Inlet Run Number:

7/15/2008

HYDROGEN CHLORIDE

HYDROGEN

FLOURIDE

FIELD DATA, EPA METHOD

26A
Traverse Point

Delta P

Sq. Rt. Delta P

Delta H • Stack Temp. (°F) 0.17 0.4123

2.26

353 o2 0.18

0.4243

2.39

357 1-3 0.15

0.3873

1.99

361 1-4 0.13

0.3606

1.73

362 1-5 0.12

0.3464

1.60

363 1-6 0.09

0.3000

1.20

365 1-7 0.08

0.2828

1.06

365 1-8 0.08

0.2828

1.06

368 2-1 0.14

0.3742

1.86

330 2-2 0.19

0.4359

2.53

343 2-3 0.14

0.3742

1.86

357 2-42-52-6 0.10 0.09

0.3162 0.3000

1.33 1.20

362 364

Meter Temp. (°F) 828384858687878889909O9192 0.09 0.3000

1.20

366

91 2-7 0.08

0.2828

1.06

368

92 2-8 0.08

0.2828

1.06

364

92 3-1 0.14

0.3742

1.86

345

92 3-2 0.13

0.3606

1.73

350

92 3-3 0.12

0.3464

1.60

357

92 3-4 0.10

0.3162

1.33

359

93 3-5 0.10

0.3162

1.33

360

93 3-6 0.11

0.3317

1.46

361

93 3-7 0.11

0.3317

1.46

360

94 3-8 0.11

0.3317

1.46

360

94 K-Factor 13.30 0.12

0.3405

1.57

358.3

RQ "7

21•ZZZ

•
EEE LUENTEC SERVICES,

iNC. METHOD 26A SAMPLE

RECOVERY

DATA SHEET Client / Location: Run No.:

1 Irnpingers 1 Final Wt.

726 Initial Wt.

691.3 Net Weight

34.7_General

Shale / DLA Inlet

Sampling

Date(s):_7-15-2008 Recovery Date: 7/15/2008 2 3

4 663.7 708.9

729.0 650.6 706.0

728.0 13.1 2.9 Description of Impinger

Contents: Silica Gel Color: Impingers and 2 (0.1N H2SO4)Contents

Container No.: Run No.: Impingers Final Wt. Initial Wt. Net Weight 1.0 Total Moisture

Recovered

By: AO 5 6 Silical Gel

63.8 Grams Percent Spent:

J•'

% Liquid Level Marked / Sealed:

• N 2 Recovery

Date: 7/15/2008 1 2

3

4 728,7 666.2

711,2

729.3 696.9 656.8

708,9

729,0 31.8 9.4

2.3

0.3 Description of Impinger

Contents: Silica Gel Color: Impingers and 2 (0.1N H2SO4)Contents

Container No,: Run No.:

3

Recovery

Date: 7/15/2008 Impingers 1

2

3

4 Final Wt.

734.3

665.4

713.7

729.9 Initial Wt.

694.3

655.4

711.2

729.3 Net Weight

40

10

2.5

0.6 Description of Impinger

Contents:

_•,M= Silica Gel Color: Impingers and 2 (0.1N H2SO4)Content

Container No.: • BLANKS: Probe Rinse:

0.1N H2SO4: Recovered

By: AO 5 6 Silical Gel "•.• 805.2
Total Moisture

51.3 Grams Percent Spent: ,,/•

% Liquid Level Marked / Sealed:

(• N Recovered By: AO 5 6 Silical Gel

Total Moisture

64.2 Grams Percent Spent:

//•"

% Liquid Level Marked / Sealed:

(• N 0.1N NaOH:

Filter:

23Test Run

No.

2 DLA Inlet

24ENTEC Services,

inc. 16-D Commerce Ave. Hueytown, Alabama 35023 Client: General Shale Plant 36 Test Date:

7/15/2008 Source: DLA Inlet Run Number:

2

HYDROGEN CHLORIDE-

HYDROGEN

FLOURIDE

FIELD DATA, EPA METHOD

26A Trave• Delta P

•

DeltaH•

Stack Te•

• 1-1 0.12 1.60

341

95 1-2 0.10

0.3162

1.33

346

96 0.10 0.09

0.3000

1.20

350

96 1-4 0.07

0.2646

0.93

353

96 1-5 0.07

0.2646

0,93

359

98 0,07 0.2646

0.93

358

99 0.07 0,2646

0.93

360

100 0.08 0.2828

1.06

362

101 0.08 0.2828

1.06

362

102 0.09 0.3000

1.20

360

102 0.09 0.3000

1.20

342

102 0.08 0.2828 1-61-71-8 2-12-22-3 2-42-52-62-72-83-13-2 0.07 0.10 0.07 1.06

343

103 0.2646 0.93

333

103 0.3162 1.33 0.2646 0.06 0.2449 0.09 0.3000 0.09 0.3000 3-3 0.12

0.3464 3-4 0.10

0.3162 3-5 0.10

0.3162 3-6 0.09

0.3000 3-7 0.08

0,2828 3-8 0.07

0.2646

0.09 K-Factor 13.30 347 0.93 359 0.80 362 1.20 362 1.20 366 1.60 351 1.33 353 1.33 354 1.20 359 1.06 359 0.93

105

362

0,2911 1.14

354.3

105107 106106 106 107 107 106108 108

25dddC• ¢

LE•z

CZZZ•

EEETest Run

No.

3 DLA Inlet

27ENTEC Services,
16-D Commerce Ave. Hueytown, Alabama 35023 Client: General Shale Plant 36 Test Date: Source: DLA Inlet Run Number:

7/15/2008 3

HYDROGEN CHLORIDE

HYDROGEN

FLOURIDE

FIELD DATA, EPA METHOD 26A
Traverse Point

DeltaP

Sq'Rt'DeltaP

DeltaH

Stack Temp.(OF)

Meter Temp. (oF) 1-1 0.15

0.3873

1.99

364

106 1-2 0.16

0.4000

2.13

363

106 1-3 0.15

0.3873

1.99

365

105 1-4 0,13

0.3606

1.73

346

105 1-5 0.12

0.3464

1.60

344

105 1-6 0.13

0,3606

1.73

336

106 1-7 0,15

0.3873

1.99

338

106 1-8 0.14

0.3742

1.86

357

106 2-1 0.15

0.3873

1.99

360

105 2-2 0,15

0.3873

1.99

365

105 2-3 0.13

0.3606

1.73

369

106 2-4 0.14

0.3742

1.86

369

105 2-52-62-72-83-13-23-33-43-5 0.3464 0.3464 0.3606 0.3742

3-63-73-8
K-Factor 13.30 0.12 0.12 0.13 0.14 0.15 0.15 0.16 0.14 0.13 0.12 0.15 0.16

0.14

0.3873

1.60

351 1.60 1.73 352 342 1.86 346 1.99 353 0.3873 1.99

361 0.4000 2.13

364 0.3742 1.86

368 0.3606 1.73

368 0.3464 1.60

351 0.3873 1.99

332 2.13

1.87 0.4000

105105105105 104104 104104104104103 339 103

354.3

28O

•-5

ooDLA Outlet Field Data

SheetsTest Run

No.

1 DLA Outlet

31ENTEC Services,

inc. 16-D Commerce Ave. Hueytown, Alabama 35023 Client: Source: General Shale Plant 36 DLA Outlet Test Date: Run Number:

7/15/2008

HYDROGEN CHLORIDE

HYDROGEN

FLOURIDE

FIELD DATA, EPA METHOD

26A
Traverse Point

Delta P

Sq. Rt. Delta P

Delta H

Stack Temp. (°F) Meter Temp. (°F: 0.3317 1.37

327

76 0,3742 1.74

327

81 1-11-21-31-41-51-6 2-12-22-32-42-52-6 0.11 0.14 0.12

0.3464

1.49

327 0.12 0.3464

1.49

326 0.10 0.3162

1.24

326 0.11 0.3317

1.37

325 0.12 0.3464

1.49

327 0.13 0.3606

1.61

327 0.11 0.3317

1.37

328 0.11 0.3317

1.37

328 0.10 0.3162

1.24

329 0,10 0.3162

1.24

326

85868787888888888787

K-Factor 12.41 0.11

0.3374

1.42

326.9

85.8

32ENTEC SERVICES,

iNC. METHOD 26A SAMPLE

RECOVERY

DATA SHEET Client / Location:

_General

Shale / DLA Outlet Run No.:

1

Recovery

Date: 7/15/2008 Impingers 2

3

4 Final Wt.

711.9

709.1

723.9

715.3 Initial Wt.

682.7

696.6

721.0

715.2 Net Weight

29.2

12.5

2.9

0.1 Sampling

Date(s):_7-15-2008 Recovered

By: 5 6

Description of Impinger

Contents:

Clear Silica Gel Color: Mixed Impingers and 2 (0.1N H=SO4)Contents

Container No;: 9-1 Run No.: Impingers Final Wt. Initial Wt. Net Weight

2

Recovery

Date: 7/15/2008 1 2

3

4 721.8 710.4

725.2

719.3 686.3 701.9

723.9

719.2 35.5 8.5

1.3

0.1

Initial Wt. Clear Mixed R-2

Net Weight Description of Impinger

Contents: Silica Gel Color: Impingers and 2 (0.1N H•SO4)Contents

Container No.: Run No.:

3

Recovery

Date: 7/15/2008 Impingers 1

2

3

4 Final Wt.

719,9

710,7

726.8

721.1 686.8 701,3

725.2

719.3 33.1 9.4

1.6

1.8 Description of Impinger

Contents:

Clear Silica Gel Color: Mixed Impingers and 2 (0.1N H•SO4)Content

Container No.: BLANKS: Probe Rinse:

R-3 0.1N H2SO4:

X AO Silical Gel 850.4

Total Moisture

51.0 Grams Percent Spent:

,/' •'• % Liquid Level Marke•i / Sealed:

• N Recovered By: AO 5 6. Silical Gel • 8.3 Total Moisture

53.7 Grams Percent Spent:

/•-"

% Liquid Level MarkecJ/Sealed:

O N Recovered By: AO 5 6 Silical Gel

Total Moisture

54.0 Grams Percent Spent:

15 Liquid Level Marked / Sealed: 0.1N NaOH:

Filter:

34Test Run

No.

2 DLA Outlet

35ENTEC Services,

inc. 16-D Commerce

Ave. Hueytown, Alabama 35023 Client: Source: General Shale Plant 36 DLA Outlet Test Date: Run Number:

7/15/2008 2

HYDROGEN CHLORIDE

HYDROGEN

F/OURIDE

FIELD DATA, EPA METHOD

26A
Traverse Point 1-11-21-31-41-51-62-12-22-32-42-52-6

K-Factor 12.41

Delta P

Sq. Rt. Delta P

Delta H

Stack Temp. (°F) 0.11 0.3317

1.37

329 0.13 0.3606

1.61

331 0.12 0.3464

1.49

331 0.10 0.3162

1.24

332 0.12 0.3464 0.11 0.3317 0,13 0.3606 0.10 0.3162 0.12 0.3464

1.49

330 1.37 319 1.61 330 1.24 331 1.49 330 0.12 0.3464

1.49

331 0.11 0.3317

1.37

332 0.10 0.3162

1.24

326

329,3

Meter Temp. (°F) 868585858687898990919293

36n>OI

ddd• •zzz•o•Test Run

No.

3 DLA OutletENTEC Services,

Inco 16-D Commerce

Ave. Hueytown, Alabama 35023
Client: Source: General Shale Plant 36 DLA Outlet Test Date: Run Number:

7115/2008 3

HYDROGEN CHLORIDE

HYDROGEN

FLOURIDE

FIELD DATA, EPA METHOD

26A

Traverse Point 1-11-21-31-41-51-6

Delta P 0.12 0.12

0.3464 0.10 0.10 0.13 0.11 2-1 0.12 2-2 0.12 2-32-42-5

K-Factor 12.41 0,10 0.11 0.11 2-6 0.10

0.11

Sq. Rt. Delta P

Delta H 0.3464 1.49 1.49

Stack Temp. (°F) 330

0.3162 1.24 0.3162 1.24

331 0.3606 1.61 0.3317 0.3464 0.3464 0.3162 0.3317 0.3317 0.3162 1.37 1.49 1.49 1.24 1.37 1.37 1.24

1.39 0.3338 Meter Temp. (°F) 91 330 91 331

332 328 33O 330 327 329 331330

329.9 93939496969698989898

95.2

39dddr• •ZZZ

•
EEEControl Room

Production Data

41Production Data The following

information

was received

by email from Ms. Martha

West of General

Shale Brick Company

for the testing performed

at their facility in Blue Ridge, Virginia,

on July 15, 2008.

Plant 36 Kiln

07-15=2008 Differential Pressure

0.36 inches Production 15.88 tons/hr Coal Usage Gas Usage •.Limestone Feed

1550 Ibs/hr 10,540 scf/hr 200 Ibs/hr

42Quality Assurance / Quality

Control Procedures

43QA / 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 the Virginia Department of Environmental

Quality

(VDEQ).

The following

section

details

all QC procedures followed

during the manual

sampling

activities. Velocity / Volumetric

Flow Rate Methods

1 and 2, 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 90 o 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.

44Molecular Weiqht

Determination

Fvrite Analysis

Method

,• The carbon

dioxide

and oxygen

concentrations

were determined

using EPA Reference Method 3. A sample

of the flue gas was extracted

from the gas stream during each test. The samples

were analyzed

with a Fyrite gas analyzer.

The following

QC steps were adhered to during these tests:

• The sampling

train was leak checked

before and after each samples

was taken.

• The samples

were run in triplicate

for accuracy.

® Standardization

was performed

to audit the reagents

and the operators

technique. A known mixture

of CO2 and 02 was analyzed

and repeated

with 3 consecutive values +/- 0.5 percent

of the known value.

,, Two NIST traceable

gas cylinders

were run against

the instrument

to audit the accuracy of the analyzer

and the analyzer

operator

technique.

One cylinder contained 2 to 4 percent

02 and 14 to 18 percent

CO2. The second

cylinder contained 2 to 4 percent

CO2 and about 15 percent

02. Moisture Determination

Method

4 Stack gas moisture

content

(B•vs) was determined

by dividing

the mass of moisture collected by the impingers

or stainless

steel condenser

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 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. @

45procedures that were sampling system

were: HCI/HF Samplinq

I•ethod

26A Accurate particulate

concentrations

are dependent

on the HCI/HF

concentrations

from the stack gas by the use of a series of specialized

reagents

in the impingers

and recovered after sampling,

and the standardized

gas sample

volume

measured.

QC followed so that representative

data was collected

by the 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 or Teflon. 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

(•H), meter temperatures, filter hotbox

temperatures,

probe temperatures,

and filter exit temperatures

were taken at every traverse

point. The filter exit temperature

was maintained

at greater

than 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. The 0.1 N H2SO4 capture

liquid in the first two impingers

was recovered

and placed into a container

for analysis

of HCI/HF. Each impinger

and connecting

glassware

was rinsed with distilled

water three times and added to the respective

container.

46The H2SO4 solution

was collected

for laboratory

analysis. Liquid levels were marked

on sample

containers

and sealed

for shipment

to the laboratory. 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).

475.6.7. ENTEC

SERVICES, INC FIELD QA/QC

CHECKLIST

PERMIT NUMBER:

• TEST METHODS

USED: CONTROL AGENCY:

• TYPE CONTROL

DEVICE: MODIFICATIONS TO METHOD: ON SITE REPRESENTATIVE: ENTEC PERSONNEL:

• PLANT CONTACT:

._•rl•f• •.. YE_._ S Was Calibration

Data on site? (Methods

1-5 / CEMS CAL Gas) Was Stack Diameter

I Area & Traverse

Points verified on field data sheets?

%// Was a i 0-minute

Meter Orifice Check •e performed? Results of check

(• • •/• --• Were Temperatures

Verified

w/NIST Traceable

Thermometer? v Was Preliminary

Traverse

wl Cyclonic

Flow verification

performed? Was previous

test data on source used to determine

K factor? v / Was Probe & Hot Box Temperatures

maintained

at 248 +/- 25 ° F? If not, explain 8. Was Filter Outlet Temperature

maintained

at 248 +/- 25 ° F? If not, explain

4• Jr.'l,,

.• c 9. Was Orsat or Fyrite leak checked

and standardization

performed

as required? Ambient 02 Reading

•3,.• % Ambient

CO2 Reading•3_____% 10. Was Tedlar Gas Sampling

Bags used? If not, explain Were they leak-checked?

Y or N 11. Were Pitot Leak,.•hecks

performed

& recorded

on each field data sheet? Pitot inspected?•or

N Noted Visual Defects?

•/• 12. Was Meter Leak Checks performed

& recorded

on each field date sheet? 13. Was Nozzle Diameter

measured

& recorded

on each field data sheet? Nozzle inspected?•)or

N Noted Visual Defects?

/4•/•..& 14. Was Silica Gel Verified,

and recorded

for each test run? Percentage Used during test- Run No.'s 1" i•' 2: t• 3: • 15. Was Acetone

Lot NU•nd

recorded

on Field Data Sheet Signature (Test Team Leader):

,•.•/•'A,/• Date:

Revision 2 December

2005 DLB 48 via •o•.•.•i•, email, or fax.ENTEC SERVICES, INC FIELD QA/QC

CHECKLIST

5.6.7. soo c PERMIT

NUMBER: TEST METHODS

USED:

•.•A• CONTROL AGENCY: ENTEC PERSONNEL: LOCATION:

_•

PERMIT LIMITS: MODIFICATIONS TO METHOD: ON SITE REPRESENTATIVE: PLANT CONTACT:

.•r•

Was Calibration

Data on site? (Methods

1-5 / CEMS CAL Gas) % Was Stack Diameter

/ Area & Traverse

Points verified on field data sheets?

X Was a i 0-minute

i•lete,•Orifice

Check performed? Results of check

/,J•S• •< Were Temperatures

Verified w/NIST Traceable

Thermometer? )• Was Preliminary

Traverse

w/Cyclonic

Flow verification

performed? _• Was previous

test data on source used to determine

K factor? ._• Was Probe & Hot Box Temperatures

maintained

at 248 +/- 25 ° F?

• If not, explain 8. Was Filter Ou.tlet T,emperat•ure

maintained

at 248 +J- 250 F? Ifnot, explain..•+

,•- •,•'•' •F•," 9. Was Orsat or•leak

checked and standardization

performed

as required? Ambient 02 Readin----g

¢•.•,•

% Ambient

CO2 Reading

O % 10. Was Tedlar Gas Sampling

Bags used? If not, explain Were they leak-checked?

Y or N 11. Were Pitot Leak,•hecks

performed

& recorded

on each field data sheet? Pitot inspected?•/or

N Noted Visual Defects? 12. Was Meter Leak Checks performed

& recorded

on each field date sheet? 13. Was Nozzle Diam.et.er

measured

& recorded

on each,field

data sheet? Nozzle inspected

.'•)or N Noted V sual Defects?

.••1• 14. Was Silica Gel Verified,

and recorded

for each test run? Percentage Used during test- Run No.'s 1: •/_•_• 2: 15. Was Acetone

Lot Number

v•,•/recorded

on Field Data Sheet Signature (Test Team
As required:

Control room data supplied by: __•f" Revision 2 December

2005 DLB 49

Date:

or fax.ENTEC SERVICES, iNC. METER ORiFiCE

AND

TEMPERATURE CHECKS Client: Date: Meter Box Number:. Original •H@ ..___j_•_.•. Location:

• Barometric Pressure:

====__•0,

•' "Hg Original Y: • BioAnnual Calibration

Date:

• Orifice Manometer Reading •H equal to Dry Gas Meter Readings:

RUN METER

FOR EXACTLY

10.0 MINUTES Dry Gas Volume,

•t z Initial

Total Volume: Vm = Volume

of Dry Gas Meter

Final

Dry Gas Meter inlet Temperature, °F initial
Average: Average Temperature

of Dry Gas Meter in degrees

Rankin

(+460) PBarm Barometric

Pressure Dry Gas igleter Outlet Temperature, °F Initial
Average: Final

Yc = 10NrnX

•/{ 0.0319

X Tm/Paa•n}

= 101( •,q'q•,

)X •/•

= ( l, ;•

) × ( o,•.•

) = • Is Y¢ < +/- 3% of Original

Y ? •

/•,•3% Thermocouple Check

(aB temperatures

are in o F) NIST Traceable Thermocouples / I.D, Stack (Pest Required) Probe / Filter Box / Filter Exit / Meter Outlet / Impinger Exit Other Ambient

Temp.

Reference

Temp.

Acceptance

Ra.ge
+1-7.5 o +/- 5.4 o +/- 5.4 o +1- 2.0 o +1- 5.4 o +/- 2.0 ° Field Checks

Perfermed

By (Signature): Revision September

2005 DLB 50 +k5.4 °

OK?ENTEC SERVICES, iNC. METER ORiFiCE

AND

TEMPERATURE CHECKS

Meter Box Number: Original AH@

1. Barometric

Pressure:

%•, I•

Hg Original Y: •cFT•; Bi=Annual Calibration

Date:

• RUN METER

FOR EXACTLY

10.0 MINUTES Reading •H equal to Dry Gas Meter Readings:

Dry Gas Volume,

ft •
Initial •,,o,o. ooo Total Volume:

Final

Dry Gas Meter Inlet Temperature, °F Initial
Average: Final

Vm = Volume

of Dry Gas Meter Tm= Average

Temperature

of Dry Gas Meter in degrees

Rankin

(+460) PBarm = Barometric

Pressure Dry Gas Meter Outlet Temperature, °F lnitia! Final
Average:

Yc = 10NmX

•/{ 0.0319

X Tm/PBarm}

= 10/( "7.$•/

) X •/{ 0.0319

X ( -•Z,,,¢

)/( 3o,/•

)• =( /.'•o.•

) × ( 0,7•/7

)= 0.475 Is Yc < +/- 3% of Original

Y ? •es

0. •; .o• Thermocoup•e Check

(all temperatures

are in o F) NIST Traceable

ID•/,•5=•7/ Thermocouples I I.D. Stack (Post Required) Probe I 7 Filter Box / Filter Exit / Meter Outlet Ambient

Temp.

Reference

Temp.

Acceptance

Range

OK? +/-7.5 +/- 5.4 +/- 5.4 +/- 2.0 o +/- 5.4 o Impinger Exit / •_•- •_•

•" Other / Field Checks

Performed

By (Signature):

• R•visioa September

2005 DLB 51 +/- 2.0 o +/- 5.4 o•ac•-.•_f# •.,•.•,"

ISO/IEC

1702..•3 AND ANSI/N(.SL

Z540oi 4,•,,,,,,,,,, ,:,•.,.•,,;,;•. •,o.• Cert. No.: 4378•i 42i 759 Yraceable@ Certificate

of Calibration

for LolliE£#

Thermometer Instrument Identification: Entac 8e•lcos, Inc., t6-D Commerce Avenue, A•ln: Lalan Kirby, Hueylown, AI. 35023 U.&A. R•4A;935101 Model: 06-664-27

S/N: 221335674

Manufacturer.

Conhol Company • -; ................................................................................................. .•tandards/Ec pment: ....................................................... Descr._•iption ,_Sel•iAI NLImbet_

Due Date

NIS1- Traceable

Refe "e ice Temperature Probe 149

8/14/07

A67"1303l•- Thermislor Module A27129

7/10/07

100020 z6g4 emperalure Calibra lion Bath TC'155

g3139 Temperature Probe i57

11!01/06

A5815063 'l'hem•islor Module A• 7118

8/23t07

A6823089 Temperature Calibralion Balh TC191

A,12238 technician: 68

Procedure:

CAL-03 Cal Date: '10/'19/06

Cat DLle: 10/'19/0;' Test Conditions:

21.5°C

56.0 %RH 1012 mBar Calibration Data:

• .•o• •om.)al

As Lefl Inl'ol

Min

Max

• • •. 0059

II This Instrument

was calibraled using Instrumenls

Traceable to National Institute of Standards and Technology,

".,',,•qL','6• Maintaining Accuracy:

CONTROL

COMPANY

4455 Rex Road Friendswood,

TX77546

USA Phone 281 482-1714

Fax 281 482-9448

service@comrol3.com

www,control3,com Control Company is ISO 1702.5 Callbralion Laboralory Accrediled by (A2LA) Amedcan Assodalion fo• Laboralory Acbre(filafil3n

at• No 1750,0 I. Conlral Company is ISO 9001 Qualily Cerlilie•J by (DNV De( Norske Ved Ced licale No, CERT O1805-AO IOU. Inlemalional Labotalory Accredilalion C:ooperalion LAC} M.Illilaleral Reco•nilion Arrangement

52VELOCITY TRAVERS•E

FORM Source: •)Z--A-

• Project No.: •q,•'t• Stack I.D., (Inches) Date: •-/•e•

Barometric

Press., in. Hg.: •./•

Ambient

Temperature:•' Pitot ID: •#-•

Pitot Cp: •

Temperature

Device:

•/• Run No.

Time PortlPoint /&P, in.H20/ Temp. OF Deg. from 900 to Null

3 o.t•

•z•

o

Run No.

Time

Run No.

Time Port/Point AP, in.H20

Temp. °F Port/ Point

AP, in.HzO

Temp. °F

AVG Pitot Leak Check

02 / PreTest • ¢ C02 Post Test R S Static Pressure % Moisture Wet Bulb Dry Bulb AVG Pitot Leak Check Pre Test R S Post Tes: R S % Moisture Wet Bulb Dry Bulb 02 CO2 Static Pressure

Checked By AVGPitot Leak Check Pre Test R S Post Test R S % Moisture Wet Bulb Dry Bulb

O2 CO2 Static Pressure

Checked By

Revision March 2005 LRK 53Plant: • Source: •,, j•J•=l•r Date: 7- l•-•" Pitot ID: •••
Run No.

Time Port Point &P, in.H=O

VELOCITY

TRAVERSe=

FORM Project No.: Stack I.D., (Inches)_•=•i Barometric Pr•s?•/•/Hg.:

.•(0, 3 Ambient

Temperature: Pitot Cp:.

Temperature

Device:

•"
Temp. °F Deg. from 900 to Null •,zo •3•

o

a. (o •y

0 b, to •¢•

o

Run No.

Time

Run No.

Time Port Poin &P, in.HzO

Temp. °F Port Point

&P, in.H20

Temp. °F

AVG Pitot Leak Check PreTest ¢ ¢
Post Test%Moisture Wet Bulb Dry Bulb 02

•'• co•,, 3' Static Pressure •9.3q Checked By

AVG Pitot Leak Check

02 Pre Test R S CO2 Post Tes R S Static Pressure % Moisture Wet Bulb Dry Bulb Checked By AVGPitot Leak Check Pre Test R S Post Test R S % Moisture Wet Bulb Dry Bulb

02 CO2 Static Pressure

Checked By

Revision March 2005 LRK 54ENTEC SERVICES, iNC. FYR•TE / ORSAT

STANDARDIZATION

Source: •d=A

gl/•//d//•/•£-]

L Orsat / • Leak Check: Date of Test: _•--/.C-Og Date of Standardization: Orsat/•ID

#: •=•.

Vendor GasConcentration, (%) Carrier Gas Container Type Cylinder ID # Date of Expiration Calibration

Gases Tank

Tank1 Actual CO202

Net Actual

Net 3.0

3 Actual Net •.O Average Net Volume

Known Value

Difference

Tank2 Actual CO2

Net/•.o

2 Actual Net

3 Actual Net Average Net Volume

Known Value

Difference

55Certificate of Analysis

Date ef A na•ysis: Customer Name: Grade of Product:

7tlz•I200,5 PR]MARY

.STAN DARD Reference

Number; Part Nunibe•: 87-.!10858887-14 XO3N t81 P 15AC225 Component Requested Actual Concentration C.oncentrat!o,9 OXYGEN 3.000 %

2,993 % CARBON DiOXiDE

t&00 %

15,97 % NITROGEN Balance Balance Relative Uncertain•

of A•t•cal

Value: +t- I% of component

or +t- 0,02% of absolute, which ever is lower. Primary Standard

.gas mixtures

are traceabte

to N.I.S.T weights

and/or N.I.S.T gas mixture reference materials. Ap•tm,.,al Sigr•atute

•/

t" /

Page

56Certificate of Analysis

Date Of Analysis: Customer Name: Grade of Product:

•14/2005 PRIMARY

STANDARD

Reference

Number: Par• Number:

87-110858887•5 X03NI82P15AC226 •linder Number CC2t 4139

Notes:

_C_ omponent CARBON

DIOXIDE OXYGEN NITROGEN

:Re:quested •tratio_rl 3,000% 15,00 % Balance

Actual Co, nee_ ntratio_•

Baiance Relative Uncertain•

of Anal tical Value. +t. "•% of component

or +t. 0,02% of absolute; which ever is lower. Primary Standard

gas mixtures

are traceable

to N,I,S,T weights

and/or N,LS,T gas mixture Approvat Sign•l.ure

57Test Protocol

58Pollution Control System Evaluation

and Source Emissions

Testing June 19, 2008 Mr. Frank Adams Virginia Department

of Environmental

Quality
Test Protocol

Reference

Letter General Shale Roanoke

VA Permit VA-20447 Plant 36 DLA Scrubber

inlet & Outlet HCI Removal

Efficiency
Dear Mr. Adams, Please find attached

the test protocol

for General

Shale

Roanoke,

Virginia

facility Plant 36 Dry Lime Adsorber

(DLA) Baghouse

Stack.

The protocol

outlines

the test procedures, the QA/QC

requirements,

and example

calculations.

Testing

has been scheduled to be conducted

on Tuesday

July 15th, 2008.

Testing

will be conducted during one day. The facility will supply all operation

parameters

to meet permitting requirements under the MACT and will be included

in the final report. If you should have any additional

questions

about the protocol

please

call me at 205- 491-6676 or my cell at 205° 613-5473

and will make any changes

as required. Sincerely, Entec Services

inc. Lynn Beane Operations Manager

16-D Commerce

Avenue

Hueytown,

Alabama

35023

Phone: (205) 491-6676

Fax (205) 491- 6614 www.entecservices.com
59Entec Services, lnc, 16-D Commerce

Avenue Hueytown, Alabama

35023 Telephone: (205) 491-6676 Fax: (205) 491-661,$

Test Protocol

for the DLA Baghouse

Stack Emissions Efficiency

Testing

at the Genera• Sha•e

Company

Plant 36 located

in Roanoke, Virginia
Submitted to: General Shale P.O. Box 3547 Johnson City, Tennessee

37602 Attention: Ms. Martha

West CC: Virginia

Department

of Environmental

Quality

Entec Project

No. 28164 Reviewed By: Protocol

Emailed:

June 20, 2008 Completed By:

Tom Lotz QA/QC Manager Lynn Beane Operations Manager

6oScope of Work Entec Services

will conduct

testing per the requirements

of General

Shale

Roanoke, VA Facility

Title V Operating

Permit

No. VAo20447.

Testing

will be conducted

for hydrogen chloride

emissions

removal

efficiency

on the D/A system

per requirements

of Part 63 Subpart

JJJJJ

Brick MACT.

The proposed

test program

will take one (1) day to complete.

Entec will perform

the testing on Tuesday

July 15, 2008 upon approval

of this test protocol

with an approximate

start time of 9:00 am. Procedures Testing will follow EPA Test Methods

1-4 w 26A (Hydrogen

Chloride)

of the CFR Title 40, Part 60, Appendix

A and Part 63 Subpart

JJJJJ.

The calibration

and quality assurance procedures

of EPA CFR 40 Part 60 Appendix

A and Part 63 for test Methods 1-4 w/26A

of the "Quality

Assurance

Handbook

for Air Pollution

Measurement

System" Volume III Stationary

Source-Specific

Methods

will be followed

throughout

the duration of the field testing

and laboratory

analysis.

The most current

CFR revision

of each method (July 1, 2006) will be used.
It is understood

that the State of Virginia

may at their discretion

bring audit samples

to the test team for analysis

in conjunction

with the other samples

as required. The following

paragraphs

summarize

the methods

to be used, detailed

test procedures, QA/QC procedures,

and other documentation

to be used for this test program. Stack Gas Volumetric

Flow The velocity

of the gas stream

will be determined

according

to EPA Reference

Method 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

will be measured

with the static side of an S-type pitot tube. A calibrated

pyrometer

will be used to measure

stack temperature

at each sampling point. The stack will be tested for cyclonic

flow according

to EPA Reference

Method

2. Stack Gas Molecular

Weiqht The carbon

dioxide

and oxygen

concentrations

will be determined

using EPA Reference Method 3. A grab sample

of the flue gas will be extracted

from the gas stream

during each test run and analyzed

using a Fyrite analyzer.

The molecular

weight of the gas will 61be calculated

using the moisture,

oxygen

and carbon

dioxide

content

and the measured stack gas temperature.

The Fyrite sampling

system

will be verified

to be leak free prior to the analysis. Moisture Content

('Combined

w/Method The moisture

content

used for calculating

the gas stream

flow rate is determined

by measuring the amount

of condensed

moisture

in the series of impingers

in the sampling train as described

in EPA Reference

Method

4 at the completion

of each test. The moisture content

will be conducted

in conjunction

with EPA Method

26A. The moisture

collection

system

consists

of a series of impingers.

Ice is placed

around the impingers

to maintain

a temperature

<680 F. The outlet temperature

of the impingers is monitored

and recorded

throughout

the duration

of the testing

to verify the temperature is below <68 o F.
Hd_Hy_d_Eo•e n Chloride Preliminary data will be 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 will be leak checked

from the pump to the orifice.

Initial and final leak checks of the sampling

system

and pitot lines will be performed

as outlined

in Method 26A and will be recorded

on the data sheets.

The nozzle

(glass or Teflon lined with an angle of taper of 30 degrees

and of button hook design)

will be calibrated

before and after the test using a micrometer

and will be also recorded

on the data sheets. The sampling

probe will be placed at each sampling

point to provide

a total sampling time of at least 60 minutes

and a volume

of at least 31.8 cubic feet. The gases will be drawn through

a glass nozzle attached

to a heated

glass lined probe.

The probe and filter will be maintained

at the proper setting to obtain a temperature

of greater

than 248 0 F. The gases then proceeded

through

borosilicate

glass filter holder,

with a Teflon frit filter support

through

a tarred Teflon or quartz fiber filter to remove

particulate

matter. The exit of the filter will be maintained

at a temperature

of greater

than 248 0 F. These temperatures will be recorded

at each point on the data sheets. The gases will be then scrubbed

through

a series of five impingers

(optional

impinger not included)

to capture

hydrogen

halides

and halogens

and moisture.

The optional

first impinger for a knockout

for moisture

will not be used since the source

it is a dry 62baghouse system.

The second

and third impingers

will contain

approximately

100 ml of a 0.1N H2SO4 solution

and the fourth and fifth impingers

will contain

approximately

100 ml of a 0.1 N NaOH solution.

The sixth impinger

will contain

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 o F. This temperature

will be also recorded on the data sheets.

The clean and cool gases then entered

the meter box where the gas flow and temperature

will be measured. After the completion

of the test leak rate determinations

will be made. Then thesampling train and the probe nozzle assembly

will be transferred

to the cleanup

area making sure no sample

will be lost. The cleanup

data will be recorded. The first, second

and third impinger

contents

will be transferred

to its tarred container, weighed and the rinsing from the glassware

will be added to this container.

The fourth and fifth impinger

contents

will be transferred

to its respective

tarred container,

weighed and the rinsing from the glassware

will be added to this container.

The silica gel from the fifth impinger

will be transferred

to its respective

tarred container

and weighed.

A blank of the sulfuric

acid solution,

sodium

hydroxide,

distilled

water and acetone

will be taken. These

containers

will be clearly

marked

and transported

to the laboratory

for analysis.
An approved

and accredited

laboratory

will perform

all of the laboratory

analysis. QA / QC Procedures Specific quality assurance

/ quality control procedures

will be 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

is to determine

compliance

with applicable air permit requirements.

The final data user in this project

will be the State of Georgia Department

of Environmental

Quality. The following

section

details all QC procedures

to be followed

during the sampling.

63Velocit=y / Volumetric

Flow Rate Volumetric flow rates will be determined

during each isokinetic

test run. The following QC steps will be adhered

to during these tests:

= Reported

duct dimensions

will be checked

by physical

measurements

to determine cross-sectional duct area.

o Pitot tube coefficients

are determined

based on physical

measurement

techniques as delineated

in Method

2 before and after each test.

= The Type-S

pitot tube are visually

inspected

before and after sampling.

® The pitot tube is 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 are checked

against

an N.I.S.T.

traceable

thermometer. The oil manometer

is leveled

and zeroed before each test run. Both legs of the pitot tube are leak-checked

before and after sampling. Proper orientation

of the pitot tube is maintained

while making

measurements.

The roll and pitch axis of the pitot tube is maintained

at 90 o to the flow. An average

velocity

pressure

reading

is recorded

at each point instead

of recording extreme high or low values. The pitot/manometer

umbilical

lines are inspected

before and after sampling

for moisture condensate.

Lines are cleared

if moisture

is found. Molecular Weiqht

Determination

Fyrite Analysi• The carbon

dioxide

and oxygen

concentrations

are determined

using EPA Reference Method 3. A sample

of the flue gas is extracted

from the gas stream

during each test. The samples

are analyzed

with a Fyrite gas analyzer.

The following

QC steps are adhered to during these tests:

, The sampling

train is leak checked

before and after each sample

is taken.

• The samples

are run in triplicate

for accuracy.

" Standardization

is performed

to audit the reagents

and the operators

technique.

A known mixture

of CO2 and O2 is analyzed

and repeated

with 3 consecutive

values +/- 0.5 percent

of the known value. Two NIST traceable

gas cylinders accuracy of the analyzer

and the are run against

the instrument

to audit the analyzer operator

technique.

One cylinder contains 2 to 4 percent

02 and 14 to 18 percent

CO2. The second

cylinder

contains 2 to 4 percent

CO2 and about 15 percent

02. 64Moisture Determination Stack gas moisture

content

(B•vs) is determined

by dividing

the mass of moisture collected by the impingers

or stainless

steel condenser

and silica gel impinger

by the standardized volume

of gas sampled.

The following

QC steps are adhered

to during these tests:

• The indicating

silica gel is fresh for the first run and periodically

inspected

and replaced during runs, if needed. The analytical

balance

is placed in a clean, motionless

environment

for weighing. The balance

is leveled

and zeroed

if necessary

before each weighing. Preliminary silica gel impinger

tare weights

and post-run

weights

are weighed

to the nearest 0.1 g. Before each series of tests, thermocouple

readings

for the silica gel impinger

exit temperature are checked

against

an N.I.S.T.

traceable

thermometer. The silica gel impinger

gas temperature

is maintained

below 68°F and recorded

at every traverse

point. Each impinger

is wiped of surface

moisture

before post-run

weighing. The volume

of liquid captured

is measured

using a graduated

cylinder

with 1- milliliter increments. HCI Samplinq

Method

26A Hydrogen Chloride

concentrations

will be determined

from the stack gas by the use of a series of specialized

reagents

in the impinger

train and recovered

after sampling,

and the standardized

gas sample

volume

measured.

QC procedures

that will be followed

so that representative

data will be collected

by the sampling

system

were:

• Only clean, well-maintained

sampling

equipment

will be used.

• Sampling

ports will be inspected

and cleaned

prior to sampling.

• All equipment

will be calibrated

according

to EPA standards.

The dry gas meter will be fully calibrated

within the past 12 months

using a set of calibrated

orifices.

, The sampling

train components

exposed

to sample

gas will be constructed

of glass or Teflon. Accurate barometric

pressure

will be recorded

at least once per day. The dry gas meter thermocouples

will be compared

to ambient

temperature

prior to the test run as a check on operation. Pretest and post-test

leak-checks

will be 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 65hotbox, probe,

and filter exit temperatures

will be checked

against

an N.I.S.T. traceable thermometer. Readings of the dry gas meter, meter orifice pressure

(•H), meter temperatures, filter hotbox

temperatures,

probe temperatures,

and filter exit temperatures

will betaken at every traverse

point. Probe and filter temperatures

will be monitored

and maintained

at greater

than 248 0 F.The filter exit temperature

will be maintained

at greater

than 248 0 F. The gas meter will be read to the thousandth

of a cubic foot for the initial and final readings. The sampling

velocity

through

the nozzle will be maintained

within 10% of the stack gas velocity

(isokinetic

sampling

rate at 100±10%). All nozzle

recovery

items will be pre-cleaned

and kept in containers

when not being used. The 0.1 N H2SO4

capture

liquid in the first two impingers

will be recovered

and placed into a container

for analysis

of HCI/HF. The 0.1 N NaOH capture

liquid in the last two impingers

will be recovered

and placed into a container

for analysis

of CI/F (if needed). Each impinger

and connecting

glassware

will be rinsed with distilled

water three times and added to the respective

container. The H2SO4 solution

will be collected

for laboratory

analysis. Liquid levels will be marked

on sample

containers

and sealed for shipment

to the laboratory. Prior to the initial run a y-factor

check will be performed

to ensure

that the meter will be operating

according

to the original

calibration

to within 3% of the original

y-factor. If required

a three point post-test

calibration

of the meter box will be performed

at the calibration

point nearest

to the average

delta h at a vacuum

greater

than that seen during the test. The recalibration

value shall be 5% of the original

value or less.

66TEST CALCULATIONS EQUATIONS 1. Ps= Pbar +(Pg/13.6)=( +

/13.6) 2. Pr•= Pba, +(&H/13.6)=( +

/13.6) 3. V•nste=17.64

V,n Y (Prn/Tr,)=17.64*( )*(

)*( 4. Vwste 0.04707

VI0=0.04707"( )= 5. Bws= Vwstd/(Vmstd

+ Vwstd)=(

)/(

+

)=

/ )=

For saturated

sources

(No. 6 8 only): If No. 6 is less than No. 5 source is considered

saturated 6. TB,•s= (106.37. {2827/(ts+365)}/ps

10 6'37"{2827/(

+365)}/( 7. TVwste= V,•te*( TBw,/1-

TB,•s)=(

)*( 8. TV•c= TV,•ste/0.04707

=(

/ 0.04707

)= 9.

12.13.14.15.16.

19.
20. )/( 1
Me= 0.44(%CO2)+0.32(%O2)+0.28((100-(%CO2+%O2)) =0.44(

)+0.32(

)+0.28(100-(

+ )= Ms= Me (1- Bw•)+18

B,,•=(

)*(1-

)+18( Vs= 85.49 Cp* •/AP 85.49*(0.84)*(

)*•/(

/((

)( ea= Vs As 60=(

)(

)(60)= es ea (1- gws) (528fT•)*(Ps/29.92)=( )(1-

)*(528/ Cs=0.01543" (Mn/Vr•,te)=0.01543*( /

)= PMR= C•* Qs (60/7000)=( )*(

)*(60/7000)= Vn=Ts/Ps*{(0.002669) V=c+ (Vrn Y Prn)/Trn)} =( /

)*{(0.002669)( )+(

)(

)( I=Vn100/(60*e*V•*A,)=( )100 / (60)(

)(

)( %EA= 100%* {(%O2)-0.5*(%CO)}

/ {0.264(%N2)

(%02)+ 0.5*(%CO)} 100%*{( )-0.5(

)} / {0.264(

)-(

)+0.5( Cs @ 50% EA= Cs/1 -[{1.5(%O2)-0.133(%N2)-0.75(%CO)}/20.9] =( / 1-[{1.5(

)-0.133(

)-0.75( Ib/mmBtu= (Cs/7000)*{(Fe*20.9)/(20.9-%O2)} =(

/7000)*{(

)'20.9)/(20.9-( )}=

)))= )*( /29.92)=

)/( )}= )= )}/20.9]=

67ASA•ACFM gwsC•C.CpAH APdscf EAE/Btu FM•MaM•IPbarPgPmPMR P•PstdQ.Q•TBw• TV•c TVwstd TmTstdVicVmV.V•Vmstd V•Vwstd 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 Deionized water blank residue concentration,

mg/g 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, lb/lb-mole Molecular weight of stack gas; wet basis, lb/lb-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 "Hg Volumetric flow rate, actual conditions,

ACF/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, ml 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,

standard cubic feet Dry gas meter calibration

factor -)

68QSTI Documentation0 o• • 0

<

7000o0Laboratory Analysis

74Environmental Testing Laboratory, 305 Crawford Street Fairfield, AlL 35064 (205) 788-1750 LaD tuvolce

•: AUlY/

Client: Mr. Tom Lotz Entec Services, Inc. 16D Commerce

Avenue Hueytown, AL 35023 Date: July 24• 2008 Project Name: General Shale Project Number:

28164 Project Location:

N/A P.Oo Number:

N/A Sample Matrix: Liquid Sampled By: Art Otero Date Collected:

July 15, 2008 Test Method:

"Methods

for Chemical

Analysis of Water and Wastes", EPA-600/3-83. LIQUID ASSAYS

Total HCL 63.1

59.2

55.5 0.02 To•l mg 300.0

22-Jd-08

1530 Tot• • 21.8

20.4

19.5 0.02 To•l mg 300.0

22-Jul-08

1530 :':'•'Z'Z'7"7"Z'Z.:.7.:.:. Vol•e 295

325

295

• •5•5

22-J•-08

1530

Total HCL 84.4

70.8

105 0.02 Total mg 300.0

22-Jul-08

1530

MD Total I-• 284

245

300 0.02 Total nag 300.0

22-Jul-08

1530

MD 1"1"i+1"51-1-551-i.'. Volume 305

310

310

mL :::::::::::::::::::::::::

22-Jul-08

1530

MD

'TotalHCL BDL !i!iiiiii!i!i!iiiiiiii!Sii

iiiii!!Siiiiii!iiii!iiiii

0.02mg/L

300.0

22-Jul-08

1530

MD Total Volume Detection limit, practical BDL=Below Detection

Limit

.:.:.:.:-:.:.:.:.:.:.

.:.:.:.:.:+:.:.:.:..

:.:.:.:.:.:.:.:.:.:.:.:- 195 <':':':':':':':':'::':': mL

22-Jul-08

1530

MD 22-Jul-08 1530

MD Respectfully submitted,

President ADEM Laboratory

Certification

I.D.# 40710 75Environmental Testing Laboratory•

Inc. 305 Crawford Street Fairfield, AL 35064 (205) 788-1750 )Client:
Project Name: Project Location: Sample Matrix: Sampled By: Lab Analyst: Test Method:

Mr. Tom Lotz Entec Services, Inc. 16D Commerce

Avenue Hueytown, AL 35023 Date: July 24, 2008

General Shale Project Number:

28164 N/A P.O. Number:

N/A Liquid Art Otero Date Collected:

July 15, 2008 MD Date/Time

Analyzed:

July 22, 2008 @ 1530 "Methods for Chemical

Analysis of Water and Wastes", EPA-600/3-83.

Method 300.0. QUALITY CONTROL

DATA ERA Minerals

Reference

Control Lot #P135506 Chloride Assayed:

51.5 mg/L Fluoride Assayed:

2.51 mg/L Range: 44.8-53.8

mg/L Range: 2.29-3.07

mg/L

Respectfully subn•tted,

John T. Brooks President ADEM Laboratory

Certification

I.D.# 40710 76Client Contact: Phone No: ENTEC

SERVICES, INC. Chain of Custody
General Shale Tom Lotz 250-491-6676

Project #

28164

PO # Lab Name

Stillbrook

Laboratories Lab Invoice # • ./• • Entec Job No. # Samples Collected

by: Send Results to: Phone Fax Results To:

Art Otero Tom Lotz C/O: Entec Services or Client 205-491-6676 7/15/2OO8 Run 1 DLA Outlet Run 2 DLA Outlet

7/15/2008 HCI, HF Run 3 DLA Outlet

7/15/2008 HCI, HF Run 1 DAL Inlet Run 2 DLA Inlet Run 3 DLA Inlet

7/15/2008 7/15/2O08 7/15/2008 7/15/2008 Blank HCI, HF

H2SO4 HCI, HF HCI, HF HCI, HF HCI, HF

H2SO4 H2SO4 H2SO4 H2SO4 H2SO4 H2SO4

Print Name:

Tom Lotz

Time (24hr):

10:30 Print Name:

Signature: Date:

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

Print Name:

SPECIAL INSTRUCTIONS

COMMENTS:

77ENTEC SERVICES, INC LABORATORY SAMPLES

QA/QC

CHECKLIST

RECOVERED BY: •

PROJECT

NO: SAMPLING DATE(S): METHOD(S):. RECOVERY DATE: /3 Description of Impinger

Contents: Test Run ao.'s t" •../•,a r • Impinger Contents

Container

Number: Test Run No.'s 1: ]'•_•/

2: •" •-

3:

/•Z-3 Samples Sealed and Stored in Secure Container?(f•or

N Liquid Level Marked?

(•r N Filter ID Number: Test Run No.'s 1: /4J,•

2"----•.. 3.•" Description of Particulate

on Filter: Test Run No.'s 1" Filter Container

Number: Run No.'s 1: Test

• 3:"7 Samples Sealed and Stored in Secure Container?

Y or N Probe Rinse Container

Number: Test Run No.'s 1" /•.• Samples Sealed and Stored in Secure Container?

Y or N Liquid Level Marked?

Y or N Probe Rinse Reagent:

/k) ,A

Lot Number:_

/b/• Laboratory Blanks: Probe

Impinger:

•

Filter:

Other: Rinse: Were samples

analyzed

by Entec Services,

Ipc.? Y or(E) If not, Laboratory

Performing

Analysis"

"--•t'//,•/'00

•

Signature: -•/'•///

/ (/'/" "• /t••- Date: ""7" I ]'7"/ • Signature: Print Name:../}q

L//•..rO Time (24hr):

• •/: •)

Print Name: Signature r Team Leader): Date: Revision 2 September

2005 TLj 78ENTEC SERVICES, LABORATORY SAMPLES

QA/QC

CHECKLIST

PROJECT No:__ SAMPLING DATE(S): METHOD(S): RECOVERY DATE: Description of Impinger

Conterjts: Test Run No.'s 1: •__/£.o/d•

2: Impinger Contents

Container

Number: Test Run No.'s 1: •_ -//

2: Samples Sealed and Stored in Secure Container? Liquid Level Marked?

Y or N Filter ID Number: Test Run No.'s 1:

/hJ/& "----'--'2T Description of Particulate

on Filter: Test Run No.'s 1:

f•.,6•

• 5. Filter Container

Number: ") Test Run No.'s 1:

/•,

2: Samples Sealed and Stored in Secure Container? Probe Rinse Container

Number: Test Run No.'s 1 :. I•'/•

2: Samples Sealed and Stored in Secure Container? Liquid Level Marked?

Y or N 7. Probe Rinse Reagent:

• •

Lot Number: 8. Laboratory

Blanks: Probe Rinse: Impinger:

)(k

Filter: Were samples

analyzed

by Entec Services,

Inc.? Y or(!• If not, Laboratory

Performing

Analysis:

"• ;/_LL•r•e

k YorN

YorN

3: YorN

Other:

*** If using outside

laboratory

services

please fill out the following

chain of custody. Signature: •el•/

•

Date: G//ZIOZ

Signature:

•&
Pdnt Name: Print Name:

• ••••. Signatu•r or Team Leader): Revision 2 September

2005 TLj Date:,

79Equipment Calibrations

8OSAMPLING 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

System,%

Volume

III, EPA-600/4-77o027b. Tv'pe-S 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. ,$amplin_cl 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 degrees 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

(/•H) 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

fall within +2% of the average 81correction factor, or the meter be cleaned,

adjusted

or repaired

and recalibrated.

The orifice pressure

differential

(AH@) 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-O09). 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.

82w

0o

.o

g o

1.1.1z
D_

0000 •C• oooo

84

o •

0• oooo•TYPE S PITOT

TUBE

iNSPECTiON

DATA

SHEET
Parameter Value Assembl• Level?

Yes Holes Dama

No Obstructed? No 0•1 0 o•2 0

A Z A sin

009090.9880 W A sin e

0 PA .494 PB .494 PA" PB

0 DT .375 Thermocouple Cal.

67 Thermocouple Cal.

67

Allowable

Ran_a__•L• YesNoNo -10 < o•1 < +10 -10 < o•2 < +10 -5 < • < +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" OD, 0.263 to 0.375 for 3/8" OD, 0.394 to 0.563 -0.063 to 0.063" 0.188 to 0.375" Reference temp. Probe Thermocouple Certification certify that the Type S pitot tube/probe

ID # ESP- 62B meets 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 12/21/2007 Annual Calibration

85TYPE S PITOT

TUBE

iNSPECTiON

DATA

SHEET

Parameter Assembl)/Level? Holes Damaged? Obstructed?

0A Z A sin y W A sin e PAPB PA PB DT Thermocouple Cal. Thermocouple Cal.

Value YesNoNo00009O9O.90900.429 .4290.3756767

Allowable

RaneL YesNoNo -10 < (zl < +10 -10 < (z2 < +10 -5 < •1 < +5

for 1/4" OD, 0.526 to 0.750 for 3/8" OD, 0.788 to 1.12 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" OD, 0.263 to 0.375 for 3/8" OD, 0.394 to 0.563

Reference temp. Probe Thermocouple Certification certify that the Type S pitot tube/probe

ID # ESP- 74B meets 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 12/21/2007 Annual Calibration

86Tom Lotz ENTEC Services,

nc. 16-D Commerce Ave.Hueytown,

Alabama 35023 Calibration Date:

12/31/2007 Calibrated by: Annual Thermocouple

Calibrations Entec Services

Temperature

**Reference

Thermocouple ID Number

Source

Temperature

Temperature TC-1 ambient

66

65 TC-2 ambient

66

65 TC-3 ambient

66

66 TC-4 ambient

66

67 TC-6 ambient

66

66 TC-7 ambient

66

65 TC-8 ambient

66

65 TC-11 ambient

66

65 TC-12 ambient

66

66 TC-13 ambient

66

67 TC-14 ambient

66

67 TC-15 ambient

66

65 TC-16 ambient

66

65 TC-17 ambient

66

65 TC-19 ambient

66

66 TC-20 ambient

66

65 TC-21 ambient

66

67 TC-22 ambient

66

66 TC-23 ambient

66

65 TC-24 ambient

66

65

Difference Degrees F

0

0

0

0

0

Within Tolerance Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes Yes TCS- ambient

66

65 Yes TCS 2

ambient

66

65 Yes TCS 3

ambient

66

65 Yes TCS 4

ambient

66

67 Yes TCS 5

ambient

66

66

0

Yes TCS 7

ambient

66

65 Yes TSC -8

ambient

66

65 Yes TSC -9

ambient

66

65 Yes TSC -10

ambient

66

66

0

Yes TSC -11

ambient

66

65 Yes TSC -12

ambient

66

65 Yes TSC -13

ambient

66

66

0

Yes TSC -14

ambient

66

65 Yes TSC -15

ambient

66

65 Yes TSC 16

ambient

66

67 Yes Fluke Hand Held

ambient

66

66

0

Yes Fluke Hand Held 2

ambient

66

66

0

Yes Fluke Hand Held 3

ambient

66

66

0

Yes

..I, ce within /- 2 F of acceptable ranges for all thermocouples. Note: NIST Traceable Digital Thermometer

Serial Number 72083241 was used as reference temperature 87ENTEC Services,
16-D Commerce Ave.Hueytown,

Alabama 35023 Calibration Date:

12/31/2007 Calibrated by:

Tom Lotz
Annual Hot Box Thermocouple

Calibrations
Entec Services

Temperature

**Reference

Thermocouple

Difference

Within D Number

Source

Temperature

Temperature

Degrees F

Tolerance HOTBOX ambient

66

67

2

Yes HOTBOX 2

ambient

66

67

2

Yes HOTBOX 3

ambient

66

66

2

Yes HOTBOX 4

ambient

66

65 Yes HOTBOX 5

ambient

66

67

2

Yes HOTBOX 6

ambient

66

67 Yes HOTBOX 7

ambient

66

66

2

Yes HOTBOX 8

ambient

66

66 Yes HOTBOX 9

ambient

66

65

0

Yes HOTBOX 10

ambient

66

65 Yes HOTBOX 11

ambient

66

67 Yes HOTBOX 12

ambient

66

67 Yes HOTBOX 13

ambient

66

65 Yes HOTBOX 14

ambient

66

67 Yes Temperature tolerance within +/- 2 F of acceptable

ranges for all thermocouples. Note: NIST Traceable Digital Thermometer

Serial Number 72083241 was used as reference temperature

88ENTEC Services,

inc. 16-D Commerc, e Ave.Hueytown,

Alabama 35023 Calibration Date:

12/31/2007 Calibrated by:

Tom Lotz Annual Gooseneck

Thermocoup

e Calibrations
Entec Services

Temperature

**Reference

Thermocouple

Difference

Within ID Number

Source

Temperature

Temperature

Degrees F

Tolerance GN-1 ambient

65

65 Yes GN-2 ambient

65

66 Yes GN-3 ambient

65

65 Yes GN-4 ambient

65

64

0

Yes GN-5 ambient

65

65 Yes GN-6 ambient

65

64

0

Yes GN-7 ambient

65

63 Yes GN-8 ambient

65

65 Yes GN-9 aml•ient

65

66 Yes GN-10 ambient

65

65 Yes GN-11 ambient

65

65

0

Yes GN-12 ambient

65

66 Yes GN-13 ambient

65

64

2

Yes GN-14 ambient

65

64 Yes GN-15 (Mini HB

ambient

65

66 Yes GN-16 (Mini HB)

ambient

65

65

2

Yes GN-17 ambient

65

64 Yes GN-18 (Mini HB)

ambient

65

66 Yes GN-19 (Mini HB)

ambient

65

66 Yes GN-20 (Mini HB)

ambient

65

65 Yes GN-21 ambient

65

64 Yes ambient 65

65 Yes tolerance within ÷/- 2 F of acceptable

ranges for all thermocouples. Note: NIST Traceable Digital Thermometer

Serial Number 72083241 was used as reference temperature

899OSafety DocumentationPollution Control System Evaluation

and Source Emissions

Testing DAILY PROJECT

SAFETY

MEETING

FORM (Toolbox Safety Meeting) Meeting Coordinator:j•=• Job Title:

• Topic of Safety Meeting:

• / co •.•- • L,J•

• ¢ inform•tion Discussed:

•

C)',•=.

• • • ,• • • • Required PPE: (Check

Required) • Hard Hat __•
• Steel Toed Boots • Safety Glasses Ear Plugs • Gloves

/ Hot Gloves Other Requirements;

(List as needed)Safety

Harness

or Fall Protection Special Clothing

(Blues / Greens

/ Tyvex) CO Personnel

Monitor Respirator (w/PM or Gas Cartridges) Long Sleeve

Shirt Attendees: Name (Print)

5) Signature

6)7)8)9) Facility required

additional

safety training

prior to entering

site: Video Safety Class•

Literature

• Rev 3: -3-06 •r No Training Clas• (MSHA)

92Test Nomenclature and

CalculationsNOMENCLATURE

TV•oTVwstd mmTstdVr•V•VmaVmstd V.Vwcstd Vwsgstd WimpWsg Y 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

94EQUATIONS TEST

CALCULATIONS DLA inlet-

Run 1

1. Ps=Pbar+(Pg/13"6) •O"ii•

+ 2. Pm=Pbar+(AH/13"6) 30-• 3. V•ta=17.64*

V•* Y* (P=•)

17.64"( 4a. V•c(std)

0.04706*

Wisp

0.04706*( 4b. Vwsg(std)

0.04715

W,g

0.04715"( 5. B,.= Vwstd/(Vmstd

+ Vwstd)

•, For saturated

sources

(No. 6 8 only): • TBws= (1 0 6.37- {2827/(ts+365)}/p, • TVwste= V•ste*( TB•s/1- TB•s) • TV•o= TV•st•0.04707

10.11.
12.

14.15.

21.22. 10637{2827/(

+364.8)}/( )*(

)/(1

)= )/( )= Me= 0.44(%CO2)+0.32(%O2)+0.28((100-(%CO2+%O2)) 0.44(

•

)+0.32(

i'7

)+0.28(100-(

,•

+ Ms=Md(1-Bws)+18B,s= (2•o1(O

)*(1- ,(• (8%•

)+18( Vs= 85.49* Cp* •/AP* •/[Ts / (Ms* Ps)] =85.49*(0.84)*( ,5• 5 )%/( •--8,59 ea Vs* As* 60

(Z'•,•I

$1 & )( )(60) Qs Qa* (528/Ts)*(Ps/29.92) )*( )*(528/

/29.92) Qs'd Qa (1- B•,s) (528/Ts)*(Ps/29.92) /

)= )*20.9)/(20.9-( )} C•=0.01543" (ME Vmstd)

0.01543"( E/Btu= (Cs/7000)*{(Fd*20.9)/(20.9-%O2)} /7000)*{( %EA= 100%* {(%O2)-0.5*(%CO)}

/ {0.264(%N2)

(%02)+ 0.5*(%CO)} 100%*{( )-0.5(

)} / {0.264(

)-( )*(

)+0.5( )*(60/7000) PMR= Cs* Qstd (60/7000) V•=Ts/Ps*{(0.002669) V•o+ (V• Y Pm)FFm)} (•, 5 / ,I•#9•,•)*{(0"002669)( Ca=0.01543" (Mn/Vn)

0.01543"( /

)= I=Vn100/(60*•9*Vs*An)

95