TEST REPOR T 

for 

General Shale 

II•oncure, NC 

Brick 

General Shale Brick 

1600 Colon Road 

Sanford, NC 27330 

(919) 774-5306 

TECH 

Air-Tech Environmental, LLC 

P. O. Box 12353 

Research Triangle Park, NC 27709-2353 

(919) 544-6338 

March 13, 2006 
Air-Tech Environmental, LLC General Shale Test Report (AT05-O391-GenSh) 

March 13, 2006 Pa eii 

Air-Tech Environmental, LLC 

Report Certification 

This report has been reviewed by the following Air-Tech Environmental, LLC personnel and is true representation a 

facility 

of the results obtained for the sampling program at the General Shale Brick 

applicable 

in Moncure, NC. The sampling and analytical methods were performed in accordance EPA reference methods except where noted in this report. 

Approvals: 

Team Leader: 

Darrell H. Doerle, Senior Staff Scientist Date 

Reviewer: 

Michael W. Hartman, Principal Scientist 
Air- Tech Environmental, LL C General Shale Test Report (AT05-O391-GenSh) 

TABLE OF CONTENTS 

1.0 

2.0 

3.0 

4.0 

Page 

INTRODUCTION 

...................................................... Executive Summary ............................................ 

1 

General Shale Results Summary Line 4 1 

............................. 

RESULTS SUMMARY 

.................................................. 

3 2.1 HF and HCI Sampling Results 2.2 Particulate Matter Sampling Results 

SAMPLING AND ANALYTICAL METHODS 

QUALITY ASSURANCE/QUALITY CONTROL 

Table 1. 

Table 2. 

Table 3. 

Figure 1. 

Figure 2. 

Tables 

HF Results Summary ............................................. HCI Results Summary 3 

............................................ PM Results Summary 4 

............................................ 4 

Figures 

Process Schematic, General Shale Line 4 Method 26A Sampling Train ............................. 6 

Appendices 

Appendix A 

Appendix B 

Appendix C 

Appendix D 

Field Data Sheets 

Appendix A. 1 Method 5/26A Data Sheets Appendix A.2 Gravimetric Analyses Appendix A.3 Example Calculations 

Analytical 

Appendix B. 1 

Appendix B.2 

Analytical Report 

Acid Gas Sample Calculations 

Dry Gas Meter Calibration Sheets 

Process Data 
Air- Tech Environmental, LL C General Shale Test Report (AT05-0391-GenSh) 

March 13, 2006 Pa el 

i.O iNTRODUCTiON 

at 

Air-Tech 

their Moncure, 

Environmental 

NC facility 

had been requested by General Shale Brick to provide testing services 

Air Pollutants), 15A NCAC 

to determine compliance with 15A NCAC 2D. 1100 (Control of Toxic 

Part 63 Subpart JJJjj 

2D. 1111 (Maximum Achievable Control Technology), and 40 CFR 

Structural Clay Products 

(National 

Manufacturing). 

Emission Standards for Hazardous Air Pollutants for Brick and 

dry line absorber (DLA) Testing was performed at the inlet and outlet of the (Kiln 4-ES-K41•rj•IO_•2 test methods employed Th ollutants of interest and in emissions characterizations are tabulated below. 

concentration 

Testing at the DLA inlet and at the stack, post DLA, was conducted simultaneously. PM 

Testing 

was reported for the outlet only. Three 60-minute test runs were conducted. 

on site to 

was 

observe 

coordinated 

the testing. 

by General Shale's Warren Paschal. Steve Hall, of the NCDENR, was 

and 

This 

results 

report presents 

of the quality 

the results of the sampling in Section 2. A description of the test methods 

respectively. 

control measures that were taken are contained in Sections 3 and 4, 

Executive Summary 

JJJJJ 

A summary 

has been 

of the 

demonstrated 

results is presented in the following table. Compliance with Subpart for HCI and HF removal efficiency the HCI rate, and the PM as well as the mass emission, mass rate.. 
Air- Tech Environmental, LL C 

General Shale Test Report (AT05-0391-GenSh) 

oMarch._13, 200• 

General Shale Results Summary 

212006 Testing. Line 4 

Run # HF HCI 

2 99.3 49.8 

Subpart JJJJJ Emission Limits: 0.057 

0.056 

0.12 

HF 

0.003 

0.004 

0.003 

0.003 

Emission Rate (/b/Ton) 

0.029 

0.028 

0.027 

PM 

0.11 

0.07 

0.10 

0.028 

Ib HF/Ton Brick or • 90% DRE; 

Ib HCl/l'on Brick or _> 89% DRE; 

Ib PM/Ton brick 
Air- Tech Environmental, LLC General Shale Test Report (AT05-0391-GenSh) 

March 13, 2006 Pa e3 

2.0 RESULTS SUMMARY 

Three test runs were conducted for the determination of PM emission rates and acid gas scrubber removal efficiency. Detailed test summaries grouped by test method are presented below. Efforts were made, successfully, to collect all samples during production of a single type 

The 

of product. 

permitted 

The 

max 

brick 

process 

production 

rate is 

rate during the testing averaged 19.93 tons per hour. (Note: 

tons/hr; target process rate is 19 tons/hr). 

20.55 tons/hr; the max normal process operation rate is 20 

Scrubber pressure drop 

The DLA lime feed rate was 110 pounds/hour. averaged 0.459" H20 during the testing. 

2.1 HF and HCI Sampling Results 

Though water droplets isokinetically at both test 

were 

locations 

not present in the gas streams sampled, all samples were collected to comply with PM sampling procedures. Summaries of the HF and HCI flue 

procedures for all 

gas 

tests 

concentrations 

did comply 

and mass rates are presented in Tables 1 and 2. Sampling operation. with the field sampling procedures pertaining to sample train 

The average HF removal efficiency was found to be 98.9%, ranging from a low of 98.6% to a 

required 

high of 99.3%. 

by the MACT. 

In all cases, 

Mass 

the removal efficiency of the DLA for HF exceeded the 90% emission rates of HF totaled produced. an average of 0.003 Ib/ton brick 

for 

HCI 

simultaneously 

removal efficiency 

performed 

averaged 

tests 

49.7% for the three tests performed. Individual values obtained ranged from mass a low of 49.1% to a high of 50.4%. The average 

mass rate 

emission 

standard 

rate 

of 

of 

0.056 

HCI was 

Ib/Ton. 

0.028 Ib/ton brick, which is less than and within the NESHAP 

Run # 

2 

3 

4 

Time 

1307-1410 

1440-1545 

1615-1728 

Table 1. HF Results Summary 

Concentration 

(ppm) 

Inlet 

83.0 

57.4 

55.1 

66:2 

Outlet 

0.60 

0.81 

0.63 

0•68 

Mass Rate (Ib/hr) 

Inlet 

7.60 

5.04 

4.08 

5.59 

Outlet 

0.05 

0.07 

0.06 

0i06 

Mass Rate (/b/ton) % 

• 

Outlet DRE 

0.003 99,3 

98.6 

0.003 98.6 

98i9 
Air-Tech Environmental, LLC General Shale Test Report (AT05-0391-GenSh) 

March 13, 2006 Pa e4 

Table 2. HCI Results Summary 

Concentration • • 

(ppm) Mass Rate (Ib/hr) 

Time 

1307-1410 

1440-1545 

1615-1728 

Run # 

2 

3 

4 

Inlet 

6.82 

6.68 

7.83 

7:06 

Outlet Inlet 

3.63 1.16 

3.43 1.10 

Outlet 

0.58 

0.53 

0:55 

2.2 Particulate Sampling Results 

Mass Rate (/b/ton) % 

Outlet DRE 

0.029 49.8 

0.028 4 49.1 

p.o28 

of 

Particulate 

Method 5. 

sampling 

The 

was performed for the determination of filterable PM using the procedures results of this testing are summarized in Table 3. Only emissions data required for the MACT and therefore are 

only DLA outlet data have been tabulated for this report. 

testing 

The average 

conducted 

emission 

during 

rate of PM was found to be 1.81 Ib/hr, These results were obtained from the production, on average, of 19.93 tons in terms of the MACT per hour of brick. Emissions were 0.091 Ib PM/ton brick, well within the requirements of Subpart JJJjj. 

Run # 

2 

3 

4 

Table 3. PM Results Summary 

Production Rate 

19.93 

19.93 

19.93 

19.93 

Concentration 

0.093 

0.0055 

0.0079 

0:076 

Particulate 

Emission Rate 

(Ib/hr) 

2.25 

1.30 

1.89 

1•8• 

Emission Rate 

(Ib/Ton) 

0.065 

0.095 
Air-Tech Environmental, LLC General Shale Test Report (AT05-0391.GenSh) 

March 13, 2006 

3.0 SAMPLING AND ANALYTICAL METHODS 

operating 

The samples 

continuously 

were collected from the exhaust of the Line 4 brick kiln, a natural gas fired process 24 hours 

emissions from 

per day, seven days per week. There was no PM control of 

schematic of the 

this source; acid gases were scrubbed in a dry lime absorber prior to exhaust. A process exhaust is contained in Figure 1. 

Inlet samples were collected from 

sampling 

a circular duct approximately 4 feet in diameter. Two 

These ports 

ports, placed at right angles, provided for access to the uncontrolled gas sample. 

A total of 12 

were 

points 

in a straight run of duct easily meeting the 8 and 2 requirements of Method 1. 

sample 

were sampled during each test. A schematic of this test location sho•,ing point location 

data. 

on the "Traverse Point Location Form" has been appended with the test 

requirements 

DLA outlet sampling was conducted at the exhaust stack. This sampling location also met the of Method 1 allowing a 12 point test to be conducted. A schematic of this location on the "Traverse Point Location Form" showing point placement has been appended as well. 

though 

Sampling was performed according to the procedures of Method 26A at both test locations, 

were collected 

only the 

simultaneously 

outlet PM results have been presented in this report. Three one hour samples 

of DLA 

at each sampling location. Concurrent with the testing readings pressure drop were made by placing a differential facility pressure gauge in parallel with the 

were not 

monitor. 

found 

These readings were taken manually at approximately 15 minute intervals and 

facility monitor 

to be significantly different than the facility monitor. An actual calibration of the was not attempted.. 

The sampling was conducted according to the procedures of EPA Method 26A. These 

in 

procedures 

dilute solutions 

entail 

of 

isokinetic 

sulfuric 

collection of a particulate sample followed by collection of acid gases 

Note that the 

acid. A schematic of this sampling train is contained in Figure 2.. caustic impingers used for the collection of diatomic halogens was not used. 

The flue gas sample was collected through a glass nozzle into a glass probe. Particulate matter 

train. 

was filtered 

This impinger 

through a heated teflon filter and then entered the impinger portion of the sampling 

followed by 

portion consisted of two impingers containing 100 ml of 0.1N sulfuric acid 

collection. 

an empty impinger, then a silica gel containing impinger used for final moisture A type S pitot tube and type K thermocouple were used to measure velocity pressures and temperatures at each sampling point. A calibrated dry gas meter was used to 

rate 

measure 

for isokinetic 

sample volume. A calibrated orifice placed on the meter outlet was used to set sample sampling. 
Air-Tech Environmental, LLC 

General Shale Test Report (AT05-0391.GenSh) 

March 13, 2006 ,,Page 6• 

Line 4 Kiln 

DLA 

>50' !>10' 

Figure 1. Process Schematic, General Shale Line 4 
Air-Tech Environmental, LLC 

General Shale Test Report (AT05-0391-GenSh) 

Ma_ r•ch 13_,• 

Fifte• 

Temperature Sensor 

Figure 2. Method 26A Sampling Train 
Air- Tech Environmental, LL C 

General Shale Test Report (AT05-0391-GenSh) 

March 13•,• 

Sample recovery resulted in the collection of the following sample fractions. 

Acetone washes, with brushing, of those portions of the sample train upstream of the filter. 

The filter. 

The sulfuric acid impinger solutions and water rinses of all exposed glass surfaces downstream from the filter to the inlet to the silica gel impinger. The silica gel. 

Acetone washes were dried down in tared beakers for the gravimetdc determination of weight gain. This gain, added to that determined for the tared filters, made up the particulate total of the sample. The total mass of PM collected was divided by the sample volume to determine particulate concentration (gr/dscf). This value was multiplied by flue gas flow rate to determine mass emission rate (Ib/hr). Mass emissions were divided by production rates to determine emissions in terms of brick production rates (Ib/ton). Complete example calculations the analytical as well as 

and run data have been appended. 

The acid matrix samples were analyzed for fluoride and chloride ions following the ion chromatography analytical procedures of Method 26A. These analyses yielded liquid concentrations for the ions of interest (ug/ml). Conversions of ion concentration to acid concentration were made on a one to one basis. These acid concentrations were then converted to total mass of the compound of interest collected using the liquid sample volume. This total mass was then converted to mass rates for each sampling location in fashion similar to the particulate matter calculations. DLA removal efficiencies were calculated based on the calculated mass rates of the compounds of interest at the inlet and outlet. Complete analytical summaries and example calculations have been appended. 

After noting the post test weight gain, the silica gel was discarded. This weight gain was added to that determined for the rest of the impinger train prior to sample recovery. The total weight gain of the impinger train was attributed to flue gas water vapor and used for flue gas moisture fraction calculations (Method 4). Flue gas fixed gas analysis was performed on bags collected during each test using the grab procedures of Method 3 using an Orsat combustion analyzer. These data, along with the velocity pressure and temperature (Method 2) determined each sample point (Method 1) during the performance of the isokinetic sampling were used to calculate flue gas volumetric flow rates used in mass rate calculations. 
Air.Tech Environmental, LLC 

General Shale Test Report (AT05-0391oGenSh) 

March13,2006 Page9 

QUALITY ASSURANCE / QUALITY CONTROL 

The Quality Assurance (QA) procedures required by the reference methodologies employed 

during the testing were strictly adhered to during the performance of this test program. Such 

adherence ensures production of useful and valid data throughout the course of the project. An 

analytical audit was not provided to Air-Tech for analysis, therefore the measures made as 

described below comprise the analytical QA. Control criteria for these measures are not 

specified in the method. The QA procedures described in this section represent an integral part 

of the overall sampling and analytical scheme. The acceptance criteria, control limits, and the 

results of these measures obtained during this testing and analysis are summarized in Table 4. 

A brief discussion of the QA measures is presented below. 

QA measures taken to provide some assessment of the quality of sample collection included 

measures of sampling rate, and the assessment of the accuracy of metered gas volumes and 

the integrity of sampling train. Sampling rates, assessed as % I•0kinetics, met method criteria 

for all test runs. Therefore, any sample bias caused by non representative collection of differing 

particle sizes (either particulate matter or water droplets) was within acceptable limits. Though 

the dry gas meters used for sample volume determination meet method criteria for accuracy the 

inlet gas meter does not meet accuracy criteria without application of the meter correction factor. 

Post test sample train leak checks meet the method criteria for Runs 2-4, the tests presented in 

this report. The initial inlet test did not pass the post test leak check and therefore Run 1 was 

not analyzed. 

The analytical measures of QA meet the method criteria for acetone purity, an assessment of 

the Method 5 analysis. The Method 26A analytical QC relies on performance of an audit to be 

provided at the NCDENR discretion. In absence of such a sample the analytical QA assessment 

was made based on the measurements tabulated in Table 4. These data show that the analysis 

suffered no significant bias due to the reagents or the sample matrix. All duplicate analysis 

show a precision of measurement of exceeding 2% of the reported value for all measurements. 

The calibration linearity indicates the results will be accurate regardless of where they fall on the 

calibration curve. 
Table 4. QA Summary 

Air=Tech Environmental, LLC 

General Shale Test Report (AT05-0391-GenSh) 

Marc_h 13, 2_0.06 Page 

Sampling 

Criteria 

% Isokinetics 

Dry Gas Meter Calibration (M26) 

Post Test Calibration Check (M26A) 

Sample Train Leak Rate (M26A) 

Analytical 

Acetone Blank (M5) 

H2SO4 Field Blank (M26A) 

H2SO4 Lab Blank (M26A) 

Lab Water Blank (M26A) 

=Matrix Spike Recovery 

Duplicate Analysis, Inlet 

Duplicate Analysis, Outlet 

Calibration Linearity 

Control Limit 

100 + 10% 

1.00 + 2% 

Yd +5% 

<0.02 cfm 

-< 0.001 wt % 

Result 

Outlet 98 99% 

Inlet 1.0212 

Outle• 0.9956 

Inlet 1.0288 

Outlet 1.0209 

Inlet 0.01 0.02 

Outlet 0.00 0.005 

HF ND 

HCl ND 

HF 109% 

HCI 102% 

HF 0.0 0.9% 

HCI 0.0- 1.2% 

HF 0.1 1.3% 

HCI O.8 1.3% 

HF R 2 0.9998 

HCI R 2 0.9994 

Inlet 101-106% 
Appendix A 

Field Data Sheets 

Appendix A.1 

Appendix A.2 

Appendix A,3 

Method 5/26A 

Data Sheets 

Gravimetric 

Analyses 

Example 

Calculations 
Appendix A.I 

Method 5/26A Data Sheets 

Sep-09-98 09:44A Air-Tech Envrnmntl 919-572-2203 P.03 

Moisture Recovery Form for Methods 4,5,6 

XAD Numl>m" 

:Numi•r -" ".. So•u•on. 

1 

2 

3 

4 

5 

6 

7 

Solution Configuration 

Total Weight Gain (g) 

Figure 14 

Moisture Recovery Form for Methods 4,5,6 
•: General Shale Brick Start Time: Date: 131 02/10/2006 End Time: Location: 1410 Inlet Initial Leak Check: 0.00@10" Run Number: 2 Final Leak Check: .02@6" 5/26A 

Total Samp_ling Time (min) Corrected Barometric Pressure (in Hg) Absolute Stack Pressure (in Hg) Stack Static Pressure (in H20) 

e Stack Temperature 

60.( 

33.80 

33.87 

1.00 

Stack 321.75 Area (sq in) 

Actual Meter Volume (cu ft) 

e Meter Pressure (in H20) 49.843 

e Meter Temperature (°F) 2.30 

Moisture Collected (g) 83.42 

Carbon Dioxide Concentration (%V) 83.80 

Oxygen Concentration (%V) 0.0 

itrogen Concentration (%V) 20.9 

Dry Gas Meter Factor 79. 

Nozzle Diameter (in) 1.021 

Pitot Constant 0.307 

Sampling Rate (dscfm) Standard Metered Volume (dscf) Standard 56.149 Metered Volume (dscm) 1.,• 

Mole Fraction Dry Stack Gas 6.56 

Dry Molecular 0.93,1 Weight 

Wet Molecular 28.8• Weight 

Stack Gas Velocity 28.12 (fpm) 

Stack 2409.81 Gas Velocity (mpm) 

Volumetric Flow Rate (acfm) 

2463.01 

734.51 

Volumetric 41218.02 Flow Rate (acmm) 

Rate (dscfm) 

Volumetric Flow Rate (dscmm) 

Percent Isokinetic 833.84 

Percent Excess Air 105.75 

Concentration (g/dscm) -1174157.30 

Concentration (kg/hr) 0.( 

Concentration (ppmv) 

1167.29 

0.00 

Emissions 0.0( (Ib/hr) 0.0( 
II 
Sep-09-98 09:44A Air-Tech Envrnmntl 9]9-572-2203 

Moisture Recovery Form for Methods 4,5,6 

P.Q3 

• Numt•" 

7 

Solution 

Amount of 

8oiution 

(g) 

lmpinger lip 

Configuration 

F•gur:e 14 

(g) 

Impinger Weight 

Initial 

(g), 

.Gm•n 

'Cg) 

total Weight Gain (g) 
': General Shale Brick Date: 02/10/2006 

Location: Inlet 

Run Number: 3 

•e: 5/26A 

Total Samp_ling Time (rain) Corrected Barometric Pressure (in Hg) Absolute Stack Pressure (in Hg) Stack Static Pressure (in H20) Average Stack Temperature (° ,F) 

Actual Meter Volume (cu ft) Average Meter Press[ire (in H20) 

.•rag Meter Temperature (°F) Moisture Collected (g) 

Carbon Dioxide Concentration (%V) 

en Concentration (%V) Dry Gas Meter Factor 

Nozzle Diameter (in) 

Pitot Constant 

•rage Sampling Rate (dscfm) Standard Metered Volume (dscf) 

Metered Volume (dscm) 

Mole Fraction Dry Stack Gas 

Dry Molecular Weight 

Wet Molecular Weight 

Stack Gas Velocity (fpm) Stack Gas Velocity (mpm) 

"ic Flow Rate (acfm) Volumetric Flow Rate (acmm) Volumetric Flow Rate (dscfm) Volumetric Flow Rate (dscmm) Percent Isokinetic 

Percent Excess Air 

Concentration (g/dscm) 

Concentration (kg/hr) 

Concentration (ppmv) 

Emissions• 

Start Time: 

End Time: 

Initial Leak Check: 

Final Leak Check: 

.000@8" 

.01@6" 

1440 

1545 

33.7• 

33.77 

1.00 

324.58 

2463.01 

47.84• 

2.16 

84.33 

74.00 

0.0 

20.9 

79.1 

1.0212 

0.307 

0.• 

0.892 

53.536 

1.516 

6,11 

0.9: 

28.84 

28.17 

2313.2z 

705,08 

3956( 

1120. 

28215. 

799.05 

1 

-1174157.30 

0.00 

0.1 

0.0• 

O.Ot 
uJ 

W 

uJ 

0 
Sep-09-98 09:44A Air-Tech Envrnmntl 919-572-2203 P.03 

Moisture Recovery Form for Methods 4,5,6 

Im#n• 

• Numb•" , 

I 

4 

5 

7 

Im•nger Tip 

COnr•juration 

Figure 14 

Impinger Weight.; i.; ::: 

Initial 

(g) 

Total Weight Gain (9) 

Moisture Recovery Form for Me£hods 4,5,6 
Facility: General Shale Brick Start Time: Date: 1615 02/10/2006 End Time: Location: 1720 Inlet Initial Leak Check: .00@6" Run Number: 4 Final Leak Check: 0 5/26A 

Total Sampling Time (min) 

Corrected 60.0 Barometric Pressure (in Hg) Absolute 29.! Stack Pressure (in Hg) Stack Static Pressure (in H20) 30.01 

Temperature (°F) 1.00 

Stack Area (sq in) 322.08 

Actual Meter Volume (cuft) 2463.01 

43.546 le Meter Pressure (in H20) 1,75 e Meter Temperature (°F) Moisture 86.7' Collected (g) 

Carbon Dioxide Concentration (%V) 72.50 

Concentration (%V) 0.0 

len Concentration (%V) 20.9 

Dry Gas Meter Factor 79.1 

Nozzle Diameter (in) 1.02" 

Pitot Constant 0.307 

Sampling Rate (dscfm) 0.84, 

Standard 0.720 Metered Volume (dscf) Standard Metered Volume (dscm) 43.173 

(%V) 1,223 

Mole Fraction Dry Stack Gas 7.32 

Dry 0.927 Molecular Weight 

Wet 28.84 Molecular Weight 28.04 Stack Gas Velocity (fpm) 

Stack Gas Velocity (mpm) 2214.• 

metric F 675.08 

Volumetric Flow Rate (acmm) 37882.7! 

Volumetric Flow Rate (dscfm) 1072.84 

Volumetric Flow Rate (dscmm) 

Percent Isokinetic 673,22 

Percent Excess Air 100.72 

Concentration (g/dscm) -1174157.31 

Concentration (kg/hr) 0.00 

Concentration (ppmv) 0.01 

Emission s (Ib/hr) 0.00 
0 
Sep-09-98 09:44A Air-Tech Envrnmntl 919-572-2203 P.03 

Moisture Recovery Form for Methods 4,5,6 

'Filtec:Numbe• 

XAD Numbe• 

Imp[nge• 

Number 

6 

Amou•t of 

Solution 

• (g) 

lmpinger Tip 

Configura6on Final 

(g) 

Impinger Weight, 

Initial 

(g) 

Total Weight Gain (g) 

G•J'n 

-.(g) 

Figure 14 

Moisture Recovery Form for Methods 4,5,6 
Traverse 

Plant 

Date 

• Location 

• t" •., 

Total Duct De tm•_b_(Distanc e A) (Inside Far Wall to Outside of NippI /Port) Nipple/Port Length (Distance B) Inside Near Wall to Outside End of Nipple/Port) Stack Depth (Dist A Dist B) Stack Width (If rectangular) .N.eare•• urbance 

Nearest Downstream Di----E•rbance 

Calculator 

Traverse 

Point 

Number 

Point Location Form 

Sample • 

Information_[ 

Number 

Schematic of Sampling Location 

(Cross Section of Duct) 

Product of Columns 

2&3 

Distance 

B 

Traverse Point Location 

from Outside of Nipple 

(sum of columns 4 & 5) 
DATA SHEET FOR VERIFICATION OF CYCLONIC FLOW 

Test No, •)•.• 

Sampling Location: 

Date: •i tO (• 

Pre-Test Velocity Leak Check: 

Post-Test Velocity Leak Check: 

Time Traverse Point 

L•P (in. H20 at 

0 Reference 

Null Point 

Rotation Angle 

(+- •) Comments 

Recorded by: 

Calibration Data 

Inclined Manometer 

Magnehelic No. 

Pitot Tube No. 

(Cal: N/A 

(Cal:__) 

(Cal:__) 

Average (Absolute Values of •): 

Sep-09-98 09:44A Air--•ech Envrnmntl 919-572-2203 P.O3 

Moisture Recovery Form for Methods 4,5,6 

XAD Number 

7 

Impinger 

Solution 

Amount of 

Solution 

Im•ing•r Tip 

Configurat•n 

Impinge• Weight 

2q q' o 

Total Weight Gain (g) 

Figure 14 

Moisture Recovery Form for Methods 4,5,6 

,Gm'n 

:Cg) 
Facility: General Shale Brick Start Time: Date: 02/10/2006 End Time: Location: Scrubber Out Initial Leak Check: Run Number: 2 Final Leak Check: M5 / HCI 

1410 

Total Sampling Time (min) Corrected Barometric Pressure (in Hg) 60.• 

Absolute Stack Pressure (_in Hg) 29.89 

Stack Static Pressure (in H20) 29.87 

Temperature (°F) -0.1 

Stack Area ..(sq in) 295-,• 

Actual Meter Volume (cu ft) 2733.! 

rage Meter Pressure (in H20) 44.2 

rage Meter Temperature (°F) 2.00 

Moisture Collected (g) 55.67 

Carbon Dioxide Concentration (%V) 

(%V) 0.0 

en Concentration (%_V) 21 

Dry Gas Meter Factor 79." 

Nozzle Diameter (in) 0.9956 

Pitot Constant 0.3 

Rate (dscfm) 0.84 

Standard Metered Volume (dscf) 0.7• 

Standard Metered Volume (dscm) 45.31 

1.283 

Mole Fraction Dry Stack Gas 

)ry Molecular Weight 0.932 

Wet Molecular Weight 28.• 

Stack Gas Velocity (fpm) 28.10 

Stack Gas Velocity (mpm) 2246.94 

684.87 

Volumetric Flow Rate (acmm) 

Flow Rate (dscfm) 

42660.14 

1208 

Volumetric Flow Rate (dscmm) Percent Isokinetic 

Percent Excess Air 

Concentration (g/dscm) 

Concentration (kg/hr) 

785.46 

98.65 

-1174157.30 

0.00 

Concentration (ppmv) 0.0q 

Emissions (Ib/hr) 0.0( 

Sep-09-98 09:44A Air-Tech Envrnmntl 919-572-2203 P.03 

Moisture Recovery Form for Methods 4,5,6 

Filt• Nurnbe¢ 

XAD Numtmr 

Im•ng• 

Number 

7 

Amount of 

Solution 

(g) 

lmpinger Tip 

Configurat}on 

Figure 14 

Impinger Woight 

Final Initial 

Total Weight Gain (g) 

.Gain 

(g) 

Moisture Recovery Form for Methods 4,5,6 
Date: 

Location: 

Run Number: 

General Shale Brick 

02/10/2006 

Scrubber Out 

3 

M5 / HCI 

Start Time: 

End Time: 

Initial Leak Check: 

Final Leak Check: 

Total Sampli_ng Time (rain) Corrected Barometric Pressure Iin Hg) Absolute Stack Pressure (inHg) Stack Static Pressure (in H20) 

perature_(°F) Stack Area (sq in)_ Actual Meter Volume (c u ft) 

;rage Meter Pressure (in H20) 

rage Meter Temperature (°F) Moisture Collected (-g) Carbon Dioxide Concentration (%V) 

n (%v) 

en Concentration (%V) Dry Gas Meter Factor 

Nozzle Diameter (_in) Pitot Con stant 

Sampling Rate (dscfm) Standard Metered Volume (dsc• Standard Metered Volume (dscm) 

Mole Fraction Dry Stack Gas 

Molecular Weight 

Wet Molecular Weight 

Stack Gas Velocity (fpm) Stack Gas Velocity (mpm) 

Volumetric Flow Rate (acmm) 

ic Flow Rate (dscfm) Volumetric Flow Rate (dscmm) Percent Isokinetic 

Percent Excess Air 

Concentration (g/dscm) 

Concentration (kg/hr) 

Concentration (ppmv) 

1440 

1545 

60.• 

297.67 

2733.97 

2.06 

59.4: 

68.7( 

0.0 

20.9 

0.9956 

0.310 

0.84 

0.763 

0.934 

28.84 

28.12 

2280.( 

694.9 

1225.92 

796.5 

98.2, 

-1174157.30 

0.00 

0.( 
"i 
Sep-09-98 09:44A Air-Tech Envrnmnt] 919-572-2203 P.03 

Moisture Recovery Form for Methods 4,5,6 

FifferNumb• 

XAD Number 

Imp[nge•" 

Number 

Impinge," 

Solution 

Amount of 

Solution 

(g) 

[mpinger Tip 

Configuratkm 

Impinger Weight 

Final Initial 

(g) 

w•ght 

(g) 

Total Weight Gain (g) 

Figure 14 

-Moisture Recovery Form for Methods 4,5,6 
Facility: General Shale Brick Start Time: 161---•- Date: 02/10/2006 End Time: 1716 Location: Scrubber Out Initial Leak Check: 0.002@10" Run Number: 4 Final Leak Check" 0.000@5" M5 / HCI 

Total Sampling Time (min) 60.0- Corrected Barometric Pressure (in Hg) 29.89 Absolute Stack Pressure (in Hg) 29.87 Stack Static Pressure (in H20) -0.19 

]ge Stack Temperature (°F) 297.17 Stack Area (sq in) 2733.97 Actual Meter Volume (cu ft) 45.124 Average Meter Pressure (in H20) 2.10 Average Meter Temperature (°F) 56.88 Moisture Collected (g) 74.40 Carbon Dioxide Concentration (%V) 0.0 

(%V) 20.9 itrogen Concentration (%V) 79.1 

)ry Gas Meter Factor 0.9956 Nozzle Diameter (in) 0.310 

Pitot Constant 0.84 

Average Sampling Rate (dscfm) 0.768 Standard Metered Volume (dscf) 46.085 Standard Metered Volume (dscm) 1.305 

7.0• Mole Fraction Dry Stack Gas 0.929 Dry Molecular Weight 28.84 

Wet Molecular Weight 28.07 Stack Gas Velocity (fpm) 2304.75 Stack Gas Velocity (mpm) 702.49 Volumetric Flow Rate (acfm) 43757.74 Volumetric Flow Rate (acmm) 1239.22 Volumetric Flow Rate (dscfm) 28310.63 Volumetric Flow Rate (dscmm) 801.76 Percent Isokinetic 98.27 

Percent Excess Air -1174157.30 Concentration (g/dscm) 0.00 Concentration (kg/hr) 0.00 Concentration (ppmv) 0.00 

Emissions ir) 0.00 

Sep-09--98 09:44A Air-.Tech Envrnmntl 919-572-2203 P.03 

Moisture Recovery Form for Methods 4,5,6 

i•m•B,ox Number 

XAD Number 

Imp/ngor 

Numbor 

4 

Implnger 

Solution 

Amount of 

Solut•n 

(g) 

[mpinger lip 

Configuration Final 

(g) 

Imp•nger Weight 

Initial 

Total Weight Gain (g) 

.G•u'n 

Fiffure 14 

Moisture Recovery Form for Methods 4,5,6 
DATA SHEET FOR VERIFICATION OF CYCLONIC FLOW 

Pre;Test Velocity Leak Check: 

Post-Test Velocity Leak Check: 

Time Traverse Point 

Null Point 

(in. H20 at Rotation Angle Reference (+ Comments 

Recorded by:, 

Calibration Data 

Inclined Manometer 

Magnehelic No. 

Pitot Tube No. 

(Cal: N/•A 

(Cal:_•) 

(Cal: 

Average (Absolute Values of 

tack 

meter 
Traverse Point Locatio 

Date 

Sampling Location 

Total Duct Depth (Distance A) 

(Inside Far Wall to Outside of Nipple 

.Nipple/Port Length (Distance B) 

/Port) •,,•. 5 " 

5.5 

Information 

Inside Near Wall to Outside End of Nipple/Port) 

Stack Depth (Dist A Dist B) 

Stack Width (If rectangular) 

Nearest Upstream Disturbance 

Nearest Downstream Disturbance 

Calculator 

Traverse 

Point 

Number 

Percent Fraction 

of Stack ID 

Stack Product of Columns 

ID 2&3 

(in) (to nearest 1/8 inch) 

/7.5 

Distance 

B 

(in) 

\/ 

Traverse Point Location 

from Outside of Nipple 

(sum of columns 4 & 5) 

/c/. / 

Schematic of Sampling Location 

(Cr.oss Section of Duct) 

Appendix A.2 

Gravirnetric Analyses 
% 

Temp: 

Oqz.ooV- o(,(3-" 

•3 o-7 z..o o V o..T29. :¢rt•) 8•. •t•3 ¢/ 
Project Name: Page 

T•me: 

% 

Temp: 

100 G 

"80, 

o2-. 
ProJec• N•me: 

T•me: 

% RH: 

T•mp: 

100 G 

IG 

-0,53 

9lOW' 

"Ta ql 

•, 6 q39 

C,9al3 

/, 0o0o I 

O, qOlo 

O, "1010 

O, "1o3o 

O, '70• S 

O, ?oqq 

O. 'lto • 

O, 

70?,4 

7oo•" 

"Io 2 ff 

?o•,o 

,/ 

V 

./ 

,/ 

V 

f 

V 
Page No._ 

Witnessed & Understood by me, Date 

To Page 

Invented by • Date 

Recorded by 

Example Calculations 
SAM PLE CALCU LATiONS 

Volume of dry gas sampled at standard conditions (68°F, 29.92 "Hg): 

V,,(std) = 

Y x Vn• x 528 × [Pbar + (J•H / 13.6] 

29.92 × (T m 

+ 460) 

Volume of water vapor at standard conditions: 

Vw = 0.04715 cf/gm x M 

w 

Fractional moisture content in stack gas: 

Mole fraction of dry stack gas: 

Md = 1 Bws 

Vm(std ) + Vw(sTD) 

Absolute stack gas pressure: 

PS • Pbar 

Static 

13.6 
Average molecular weight of stack gas (Ib/Ib.mole): 

Dry: MW• = (.32 x %O•) + (.44 x %CO•) + [.28 x {100 (%O• + %CO2)}] 

Wet: MW, = [MW d x (1 Bw,)] + (18 x Bw,) 

Stack gas velocity at stack conditions (ft/sec): 

Vs = 85.49 × .84 x •r X 

Ts + 460 

P, x 

Average stack gas volumetric flow at dry, standard conditions (DSCFM): 

528xP• x 60sec 

e,• = V, x As x M• x 

(T, + 460)x 29.92 rain 

Concentration of VOC" 

CVOC = Cth c Cm 

VOC mass loading: 

Evoc 2.49 x 10 .6 x Qs• x Cvoc 

Destruction efficiency: 

DRE (•,;..•.•) 100 

=='VOCi 
Isokinetic sampling rate (%): 

C = .0945 for English Units 

I% = 

C x Vr,(,td x (T, + 460) 

V 

s 

x t x Ps x M• x,• 

Particulate concentration (gr/dscf): 

Cs Nip × 15.43 grains 

g 

Vm(std) 

Particulate emission rate (Ib/hr). 

E • C$ 

7000 grains/Ib 

x Qsd x 

Particulate emission rate (Ib PM/ton Product)- 

E' = E / Production Rate (tons per hour) 

60 min 

hr 
Definitions 

AH 

AP 

BTU/hr 

Bws 

CM 

Cs 

CS02 

CTHC 

Dn 

DRE 

E 

EEOI 

Evoc 

Evocl 

Evoco 

E' 

Md 

MF 

M,• 

MWd 

MWs 

Pbar 

Ps 

Qsd 

Static 

t 

Tm 

TPD 

average meter orifice pressure (in. H20) 

velocity pressure (in. H20) 

area of nozzle (ft 2) 

cross sectional area of duct (ft 2) 

heat input 

mole fraction of wet gas (unitless) 

concentration of methane (ppm) 

particulate concentration (gr/dscf) 

sulfur dioxide concentrations (Ibldscf) 

concentration of total hydrocarbon (ppm) 

diameter of nozzle (in) 

destruction/removal efficiency (%) 

emission rate (Ib/hr) 

mass rate, compound of interest (Ib/hr) 

emission rate of VOC (Ib/hr) 

control device inlet mass loading (Ib/hr) 

control device outlet mass loading (Ib/hr) 

emission rate (Ib/10 • BTU) 

mole fraction of dry gas (unitless) 

mass of filter, post test (g) 

mass of particulate (g) 

mass of water collected (g) 

flue gas molecular weight, dry basis (Ib/Ib-mole) 

flue gas molecular weight, wet basis (Ib/Ib-mole) 

barometric pressure (in. Hg) 

absolute stack pressure (in. Hg) 

flue gas dry volumetric flow @ STP (ft3/min) 

stack static pressure (in. H20) 

test time (min) 

average meter temperature (°F) 

acid production rate, tons per day 
Definitions 

ms 

Pg/g 

pg/ml 

v. 

V• 

Vm(std) 

VOC 

v, 

v. 

Y 

average flue gas temperature (°F) 

laboratory result, analytical concentration of sample 

laboratory result, analytical concentration of sample 

volume of liquid aliquot analyzed (ml) 

volume of liquid recovery fraction (ml) 

actual meter volume (ft z) 

meter volume @ STP (ft •) 

non-methane hydrocarbon (ppm) 

flue gas velocity (ft/sec) 

volume of water vapor condensed (ft •) 

dry gas meter correction factor (unitless) 
Appendix B 

Analytical 

Appendix B.1 Analytical Report 

Appendix B.2 Acid Gas Sample 

Calculations 
Appendix 

Analytical Report 
A r-Tech Environmeata| 3216 S. Alston Ave. 

Durham, NC 27713 

LLC 

General Shale-Moncure 

Analytical Report 

(0206-54) 

EPA Meth o d 2 6A 

Hydrogen chloride 

Hydrogen fluoride 

Enthalpy Analytical, inc. 

Phone: (919) 850 4392 Fax: (919) 850 9012 www.enthall•y.com 

2202 Ellis Road Durham, NC 27703 5518 
I certify that to the best of my knowledge all analytical data presented in this report: 

® Have been checked for completeness 

® Are accurate, error-free, and legible 

® Have been conducted in accordance with approved protocol, and that all deviations and analytical 

problems are summarized in the appropriate narrative(s) 

® This analytical report was prepared in Portable Document Format (.PDF) and contains 91 pages. 

QA Review Performed by: Michael Steven Schapira 
Summary of Results 
Company Air-Tech Environmental 

Analyst KAM 

Parameters EPA Method 26A 

# Samp es 6 runs & 1 blank 

Client # General Shale Moncure 

Job #10206-54 

PO # Verbal 

Report Date 2/21/2006 

Compound 

Hydrogen fluoride 

Hydrogen chloride 

Hydrogen fluoride 

Hydrogen chloride 

Hydrogen fluoride 

Hydrogen chloride 

Sample ID / Catch Weight (ug) 

In-02 

109,616 

16,662 

In-03 

72,342 

15,569 

In-04 

56,026 

14,716 

Out-02 

643 

7,171 

Out-03 

868 

6,799 

Out-04 

683 

6,538 

Blank 

25.0 ND 

33.6 ND 

0206-54-results 3/1/2006 
Results 
E 

0 0 

0 0 

0 

0 

Narrative Summary 
Enthalpy Analytical Narrative Summary 

Company: Air-Tech Environmental, LLC 

Client #: General Shale-Moncure 

PO #: Verbal 

Enthalpy #: 0206-54 

Analyst: KAM 

Parameters: EPA Method 26A 

Custody 

Analysis 

Separation 

Matrix Spikes 

Blanks 

Reproducibility 

Reporting Notes 

Chris Todd of Enthalpy Analytical, Inc. received the samples at 

15.6°C on 2/15/06 after being relinquished by Air-Tech 

Environmental, LLC. Prior to analysis the samples were kept under 

lock with access only by authorized personnel of Enthalpy 

Analytical, Inc. 

The samples were analyzed according to the procedures outlined in 

EPA Method 26A. The acid (H2SO4) matrix samples were analyzed 

for the chloride (CI) and fluoride (F) ion. 

Quantitation was performed using a Hewlett Packard series 1100 

High Performance Liquid Chromatograph equipped with a Dionex 

ED40 Electrochemical detector and a Dionex ASRS-ULTRA® 

4-mm autosuppressor. 

Separation was accomplished by a Dionex IonPac AS-14A 4 mm x 

250 mm colunm, A copy of the acquisition method (0106-48.M) is 

included. 

Before and after sample analysis, calibration curves were prepared 

and analyzed. Fluoride and chloride eluted at approximately 2.8 and 

3.7 minutes respectively. Both compounds separated well and were 

easily identified. 

A 0.500-mL aliquot of a 100-fold diluted sample In-02 was spiked 

with 0.663 lag of hydrogen fluoride (HF) using 25.0 laL of a 

solution containing 26.5 lag/mL HF. The spiked sample was 

analyzed in the same manner as the other samples. The calculated 

HF spike recovery was 109%. 

A 0.500-mL aliquot of a 10-fold diluted sample In-02 was spiked 

with 1.29 I,tg of hydrogen chloride (HC1) using 25.0 laL of a 

solution containing 51.4 lag/mL HC1. The spiked sample was 

analyzed in the same manner as the other samples. The calculated 

HC1 spike recovery was 102%. 

One blank sample Blank was analyzed and reported. No blank 

adjustments were made to any of the reported data. 

OK 

The I•SO4 matrix samples were analyzed for CI and F but are 

reported as HCI and HF. The peaks listed in the "Sample 

Chromatograms" section are labeled hydrogen fluoride and 

hydrogen chloride. The additional molecular weight contribution 

from the tf is included in the results listed on each chromatogram 

and throughout the report. 
General Reporting Notes 

The following are general reporting notes that are applicable to all Enthalpy Analytical, Inc. reports, unless 

specifically noted otherwise. 

The symbol MDL represents the Minimuna Detection Limit. Below tiffs value the laboratory cannot 

confim the presence of the analyte of interest reliably. 

The symbol LOp_. represents the Limit of Quantification. Below this value the laboratory cannot 

quantitate the analyte of interest within the criteria of the method. 

The symbol ND following a value indicates a non-detect or analytical result below the MDL. 

The symbol J following a value indicates an analytical result between the MDL and the LOQ. A J flag 

indicates that the laboratory can positively identify the analyte of interest as present, but the value should 

be considered an estimate. 

The symbol E following a value indicates an analytical result exceeding 100% of the highest calibration 

point. 

The symbol DF represents a Dilution Factor. This number represents dilutions during the extraction 

and/or laboratory stages of sample treatment. The analytical result taken from a laboratory instrument is 

multiplied by the DF to get final results. 

The Sample ID MS represents a Matrix Spike. An aliquot of an actual sample is spiked with a known 

amount of analyte so that a percent recovery value can be determined. This shows what effect the 

sample matrix may have on the target analyte, i.e. whether or not anything in the sample matrix prohibits 

analysis for the analyte(s). 

The Sample ID MSD represents a Matrix Spike Duplicate. Prepared in the same manner as an MS, the 

use of duplicate matrix spikes allows further confumation of laboratory quality by showing the 

consistency of results gained by performing the sanle steps multiple times. Most methods performed by 

Enthalpy do not require analysis of an MSD. 

The Sample ID BS represents a Blind Spike. A member of the Quality Assurance department has 

created BS samples for many of the analytes Enthalpy tests for, and only QA and the Enthalpy Analytical 

ownership have access to the actual values of these samples. The laboratory analyzes them without 

knowledge of the actual value, and the spreadsheets get completed for these samples solely by the QA 

group. 

The Sample ID LCS represents a Laboratory Control Sample. Whenever spikes are prepared for our 

clients more spikes are prepared than needed. The extras (randomly chosen) are kept in-house at the 

appropriate temperature conditions. When the spike samples come back from the client for analysis, the 

LCSs (usually two are saved) are analyzed to confmn that the analyte could be recovered from the 

media, separate from the spike samples which were used on the project and which may have had issues 

caused during collection and/or transport. 

Significant Figures: Where the reported value is much greater than unity (1.00) in the units expressed 

(specifically values of 1,000 or greater), the number is rounded to a whole number of units, rather than to 

3 significant figures. For example, a value of 10,456.45 ug catch is rounded to 10,456 ug. There are five 

significant digits reported, but no confidence should be placed on more than three significant digits. 
Sample Custody 
SB•NIV.I.NO0 :I0 "ON 
Sample 

Chromatograms 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\032-36(]I.D 

0206-54 

Sample Name: In-02*•!O 

Injection Date 2/16/2006 1:26:39 PM Seq. Line 36 

Sample Name In-02•100 Location Vial 32 

Acq. Operator KAM Inj 1 

Acq. Instrument Gonzo Inj Volume 25 •i 

Acq. Method H:\LC2006QIkGONZO\METHOD\0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:\LC2006QI\GONZO\METHOD\O206-09Z.M 

Last changed 2/17/2006 3:16:28 PM by TG 

(modified after loading 

ADC1 B, Dionex ED 40 (0206-09Ak032-3601 .D) 

420 

400 

380. 

360 

340 

2 3 4 5 6 7 8 m•r 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:05:18 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCl B, Dionex ED 40 

RetTime Type 

[min] 

2.822 BB 

9.CCO 

Area Amt/Area Amount Grp 

[uS*s] [ug/mL] 

264.26773 9.17877e-3 2.42565 

Totals 2.42565 

Results obtained with enhanced integrator! 

1 Warnings or Errors 

Warning Calibrated compound(s) not found 

Instrument 3 2/17/2006 3:16:36 PM TG 

Name 

Hydrogen Fluoride 

Ilyd• 

Page i of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\032_3602.D 

0206-54 

Sample Name: In-02*101 

Sample 

Injection 

Name 

Date 2/16/2006 1:37:28 PM Seq. Line 36 In-02*100 

Acq. Operator Location Vial 32 KAM 

Acq. Instrument Inj 2 Gonzo 

Acq. Method H:\LC2006QI\GONZOkMETHOD\0106-48.M Inj Volume 25 pl 

Last changed 2/7/2006 1:48:48 PM by TG Analysis Method H:\LC2006QIkGONZOkMETHODk0206-09Z.M Last changed 2/17/2006 3:]6:28 PM by TG 

(modified after loading) ADC1 •ED 40 (•• 

Norm. 

440 

420 

400 

380 

360- 

340 

External Standard Report 

Sorted By Signal Calib. Data Modified 2/17/2006 3:05:18 PM Multiplier 1.0000 Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCI B, Dionex ED 40 

RetTime Type 

[min] 

2. 820 BB 

Area A•tt/Area Amount Grp [uS•s] lug/roLl 

260.66632 9. 17893e-3 2.39264 

Totals 2.39264 

Results obtained with enhanced integrator! 1 Warnings or Errors 

Warning Calibrated compound(s) not found 

Name 

Hydrogen Fluoride 

Instrument 3 2/17/2006 3:1.6:46 PH TG 

Page 1 of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\033-3701"D 

0206-54 

Sample Name: In-02•3 

Injection Date 2/16/2006 1:48:16 PM Seq. Line 37 

Sample Name In-02*10 Location Vial 33 

Acq. Operator KAM Inj 1 

Acq. Instrument Gonzo Inj Volume 25 pl 

Acq. Method H:\LC2006QIkGONZOkMETHOD\0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:kLC2006QIkGONZO\METHOD\0206-09Z.M 

Last changed 2/17/2006 3:16:28 PM by TG 

(modified after loading) 

No[m. 

440 

420' 

400 

380. 

360 

ADC1 B, Dionex ED 40 0206-09Ak033-3701 .D) 

340 • • ,• • • .} • 

mlr 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:05:18 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCI B, Dionex ED 40 

RetTime Type 

[min] 

2.812 

3.660 VB 

Area Amt/Area Amount Grp 

[uS*s] [ug/•] 

293.55585 1.26214e-2 3.70508 

Totals 3.70508 

Results obtained with enhanced integrator[ 

i Warnings or Errors 

Warning Calibrated compound(s) not found 

Name 

Hydrogen Chloride 

Instrument 3 2/17/2006 3:].6:57 PM TG Page 1 of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\033_3702.D 

0206-54 

Sample Name: In-02*l( 

Sample 

Injection Date 2/16/2006 1:59:02 PM Seq. Line 37 Name In-02*10 

Acq. Operator Location Vial 33 KAM 

Acq. Instrument Inj 2 Gonzo 

Acq. Method H:\LC2006QI\GONZO\METHOD\0106-48.M Inj Volume 25 •i 

Last changed 2/7/2006 1:48:48 PM by TG Analysis Method H:\LC2006QI\GONZOkMETHOD\0206-09Z.M Last changed 2/17/2006 3:16:28 PM by TG 

(modified after loading) ADC1 B, •ED 40,• 

Norm. 

440 

420 

40O 

380 

360 

34O 

2 3 4 5 6 7 8 

External Standard Report 

mi 

Sorted By Signal Calib. Data Modified 2/17/2006 3:05:18 PM Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal I: ADCI B, Dionex ED 40 

RetTime 

[mini 

Type Area Amt/Area Amount Grp Name 

[uS*s) [ug/mL] 

3.662 VB 286.55634 1.26292e-2 3.61899 Hydrogen Chloride 

Totals 3.61899 

Results obtained with enhanced integrator! 1 Warnings or Errors 

Warning Calibrated compound(s) not found 

Instrument 3 2/17/2006 3:]7:07 PM TG 

Page i of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\034-3801.D 

0206-54 

Sample Name: In-03•l[ 

Injection Date 2/16/2006 2:09:48 PM Seq. Line 38 

Sample Name In-03*100 Location Vial 34 

Acq. Operator KAM Inj 1 

Acq. Instrument Gonzo Inj Volume 25 •i 

Acq. Method H:\LC2006QIkGONZOkMETHOD\0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:kLC2006QIkGONZOkMETHOD\0206-09Z.M 

Last changed 2/17/2006 3:16:28 PM by TG 

(modified after loading) 

ADC1 B, Dionex ED 40 (0206-09A\034-3801 .D) 

420 J 

400 

380. 

• 

360. ••_ •// 

340. 

2 3 4 5 6 7 8 mm 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:05:18 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCI B, Dionex ED 40 

RetTime Type 

[min] 

2.820 BB 

Area Amt/Area Amount Grp Name 

[uS*s] [ug/mL] 

179.08839 9.18443e-3 1.64483 Hydrogen Fluoride 

Totals 1.64483 

Results obtained with enhanced integrator! 

1 Warnings or Errors 

Warning Calibrated compound(s) not found 

Instrument 3 2/17/2006 3:17:17 PM TG Page 1 of 2 
Data File H:\LC2006Qff\GONZO\DATA\FEB2006\0206_09A\034_3802.D 

0206-54 

Sample Name: In-03*10C 

Sample 

Injection 

Name 

Date 2/16/2006 2:20:36 PM Seq. Line 38 In-03*100 

Acq. Operator Location Vial 34 KAM 

Acq. Instrument Inj 2 Gonzo 

Acq. Method H:\LC2006QI\GONZO\METHOD\0106-48.M Inj Volume 25 •i 

Last changed 2/7/2006 1:48:48 PM by TG Analysis Method H:\LC2006QI\GONZO\METHOD\0206-09Z.M Last changed 2/17/2006 3:16:28 PM by TG 

AOCI•o 

(modified after loading) • 

NOIT'n. 

440 

420 

400 

380 

360 

340 

2 3 4 5 6 7 8 

External Standard Report 

Sorted By Signal Calib. Data Modified 2/17/2006 3:05:18 PM Multiplier 1.0000 Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCI B, Dionex ED 40 

RetTime Type Area Amt/Area }•nount [mini [uSes) [ug/mL] 

• 

2.818 BB 178.93808 9.18445e-3 1 64345 

Totals 

1.64345 

Results obtained with enhanced integrator! 1 Warnings or Errors 

Grp Name 

Hydrogen Fluoride 

Warning Calibrated compound(s) not found 

Instrument 3 2/17/2006 3:]7:25 PM TG 

Page i of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\O35-390]'D 

0206-54 

Sample Name: In-03*] 

Injection Date 2/16/2006 2:31:21 PM Seq. Line 39 

Sample Name In-03*10 Location Vial 35 

Acq. Operator KAM Inj 1 

Aoq. Instrument Gonzo Inj Volume 25 •i 

Aoq. Method H:\LC2006QI\GONZO\METHODX0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:\LC2006QI\GONZOXMETHODX0206-09Z.M 

Last changed 2/17/2006 3:16:28 PM by TG 

(modified after loading) 

Norm. 

440 

420 

ADC1 B, Dionex ED 4010206-09A\035-3901.D) 

_• 

2 3 4 5 6 7 8 m•__/r 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:05:18 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCI B, Dionex ED 40 

RetTime Type 

[rain 

2.812 

Area Amt/Area Amount Grp 

[uSes] [ug/mL] 

3.656 VB 280.00052 1.26370e-2 3.53836 

Totals 3.53836 

Results obtained with enhanced integrator! 

1 Warnings or Errors 

Warning Calibrated compound(s) not found 

°Name 

[[•d•,, •'l•id• 

Hydrogen Chloride 

Instrument 3 2/17/2006 3:17:33 PM TG Page 1 of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206_09A\035_3902.D 

0206-54 

Sample Name: In-03"16 

Injection Date 2/16/2006 2:42:03 PM 

Sample Name In-03*10 

Acq. Operator KAM Inj 2 Acq. Instrument Gonzo Inj Volume 25 pl Acq. Method H:\LC2006QI\GONZO\METHOD\0106-48.M Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:\LC2006QI\GONZO\METHOD\0206-09Z.M Last changed 2/17/2006 3:16:28 PM by TG 

(modified after loading) ADClB, OionexED40 020•09A•3•zg02.D) 

Norm. 

440 

420- 

400 

380 

360 

Seq. Line 39 

Location Vial 35 

340.. 

External Standard Report 

Sorted By Signal Calib. Data Modified 2/17/2006 3:05:18 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal I: ADCI B, Dionex ED 40 

RetTime Type Area Amt/Area Amount Grp [mini [uS*s] lug/roLl 

3.655 BB 280.01413 1.26370e-2 3.53853 

Totals 3.53853 

Results obtained with enhanced integrator! 1 Warnings or Errors 

Warning Calibrated compound(s) not found 

Name 

•I•±• •lu•id• 

Hydrogen Chloride 

miJ 

Instrument 3 2/17/2006 3:17:42 PH TG Page i of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\036-4001.D 

0206-54 

Sample Name: In-04*10 

Injection Date 2/16/2006 2:52:52 PM Seq. Line 40 

Sample Name In-04*100 Locatio• Vial 36 

Acq. Operator KAM Inj 1 

Acq. Instrument Gonzo Inj Volume 25 •i 

Acq. Method H:\LC2006QI\GONZO\METHOD\0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:\LC2006QIkGONZO\METHODk0206-09Z.M 

Last changed 2/17/2006 3:16:28 PM by TG 

(modified after loading) 

ADC1 B, Dionex ED 40 (0206-09Ak036-4001.D) 

2 3 4 5 6 7 8 m•r 

Zxternal Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:05:18 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCl B, Dionex ED 40 

RetTime Type Area /•Lt/Area Amount Grp Name 

[min] [uS*s] [ug/mL] 

2.815 BB 143.11507 9.18885e-3 1.31506 Hydrogen Fluoride 

3.660 

Totals 1.31506 

Results obtained with enhanced integrator! 

1 Warnings or Errors 

Warning Calibrated compound(s) not found 

Instrument 3 2/17/2006 3:17:51PM TG Page 1 of 2 
Data FJ le H:\LC2006QI\GONZO\DATA\FEB2006\0206_09A\036_4002.D 

0206-54 

Sample Name: In-04*10C 

Sample 

Injection Date 2/16/2006 3:03:42 PM Seq. Line 40 Name In-04*100 

Acq. Location Vial 36 Operator KAM 

Acq. Inj 2 Instrument Gonzo 

Acq. Inj Volume 25 gl Method H:hLC2006QIkGONZOkMETHODk0106-48.M Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:hLC2006QIkGONZOkMETHOD\0206-09Z.M Last changed 2/17/2006 3:16:28 PM by TG 

(modified after loading) ADC1B, D•-•exED40(020•09A•Z•4002.D) 

Norm. 

440 

420 

400 

380- 

360 

340 

';' 

External Standard Report 

Sorted By Signal Calib. Data Modified 2/17/2006 3:05:18 PM Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCI B, Dionex ED 40 

Area Amt/Area Amount Grp [uS*s] [ug/mL] 

140.47032 9. 18926e-3 1.29082 

RetTime Type 

[min] 

2.822 PB 

Totals 1.29082 

Results obtained with enhanced integrator! 1 Warnings or Errors 

Name 

Hydrogen Fluoride 

Warning Calibrated compound(s) not found 

Instrument 3 2/17/2006 3:17:59 PM TG 

Page 1 of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\037-4101.D 

0206-54 

Sample Name: In-04*l, 

Injection Date 2/16/2006 3:14:30 PM Seq. Line 41 

Sample Name In-04*10 Location Vial 37 

Acq. Operator KAM Inj 1 

Acq. Instrument Gonzo Inj Volume 25 •i 

Aoq. Method H:\LC2006QIkGONZO\METHOD\0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:kLC2006QIkGONZOkMETHOD\0206-09Z.M 

Last ehanged 2/17/2006 3:16:28 PM by TG 

(modified after loading) 

N( 

ADC1 B, Dionex ED 40 0206-09A\037-4101 .D) 

2 3 4 5 6 7 8 mir 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:05:18 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCI B, Dionex ED 40 

RetTime Type 

[min] 

2.012 

3.656 BB 

Area Amt/Area Amount Grp Name 

[uS*s] [ug/mL] 

iI•d• Fl•id• 

273.37628 1.26452e-2 3.45689 Hydrogen Chloride 

Totals 3. 45689 

Results obtained with enhanced integrator! 

i Warnings or Errors 

Warning Calibrated compound(s) not found 

Instrument 3 2/17/2006 3:18:09 PM TG Page 1 of 2 
Data File H:\LC2006Ql\GONZO\DATA\FEB2006\0206-09A\037_4102 .D 

0206-54 

Sample Name: 

Sample 

Injection Date 2/16/2006 3:25:16 PM Seq. Line 41 Name In-04*10 

Acq. Operator Location Vial 37 KAM 

Acq. Instrument Inj 2 Gonzo 

Acq. Method H:\LC2006QIkGONZOkMETHOD\0106-48•M Inj Volume 25 pl 

Last changed 2/7/2006 1:48:48 PM by TG Analysis Method H:kLC2006QIkGONZO\METHOD\0206-09Z.M Last changed 2/17/2006 3:16:28 PM by TG 

(modified after loading) ADC1B, Di•-•40102--•-•-9A•Z?.4102.D) 

NOnT 

44( 

420 

400 

380 

360 

340 

External Standard Report 

Sorted By 

Calib. Data Modified 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCI B, Dionex ED 40 

RetTime Type Area 

[mini [uS*s] 

3.658 BB 267.75766 1.26524e-2 3.38778 

Totals 3.38778 

Results obtained with enhanced integrator! 1 Warnings or Errors 

Signal 

2/17/2006 3:05:18 PM 

Amt/Area Amount Grp 

[ug/mL] 

Name 

II]'dzsgcn Fluszida 

Hydrogen Chloride 

Warning Calibrated compound(s) not found 

Instrument 3 2/1.7/2006 3:]8:18 PM TG 

Page 1 of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\038-4401.D 

0206-54 

Sample Name: Out-02*l 

Injection Date 2/16/2006 4:19:36 PM Seq. Line 44 

Sample Name Out-02*10 Location Vial 38 

Acq. Operator KAM Inj 1 

Acq. Instrument Gonzo Inj Volume 25 pl 

Acq. Method H:kLC2006QI\GONZO\METHOD\0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:\LC2006QI\GONZO\METHOD\0206-09Z.M 

Last changed 2/17/2006 3:16:28 PM by TG 

(modified after loading) 

420- 

400 

380- 

360 

ADC1 B, Dionex ED 40 (0206-09A\038-4401.D) 

340 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:05:18 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor wi•h ISTDs 

Signal i: ADCl B, Dionez ED 40 

RetTime Type Area Amt/Area Amount Grp 

[min] [uS*s] [ug/mL] 

2.812 

3.650 PB 132.86073 1.30110e-2 1.72865 

Totals 1. 72865 

Results obtained with enhanced integrator! 

1 Warnings or Errors 

Warning Calibrated compound(s) not found 

Name 

Hydrogen Chloride 

Instrument 3 2/17/2006 3:18:39 PM TG Page 1 of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206_09A\038_4402.D 

0206-54 

Sample Name: Out-02*iC 

Injection Date 2/16/2006 4:29:42 PM Seq. Line 44 

Sample Name Out-02*10 Location Vial 38 

Acq. Operator KAM Inj 2 

Acq. Instrument Gonzo Inj Volume 25 pl Acq. Method H:\LC2006QI\GONZO\METHOD\0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:\LC2006QI\GONZOkMETHOD\0206-09Z.M 

Last changed 2/17/2006 3:16:28 PM by TG 

(modified after loading) ADC1B, DionexED40(020•09A•Z•4402.D) 

42£ 

400 

38C 

36O 

340 • 

2 3 4 5 

• •--r-•-• 

6 7 8 mir 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:05:18 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCl B, Dionex ED 40 

RetTime Type Area 

[min] [uS*s] 

2.•12 

3.658 PB 

Amt/Area Amount Grp 

[ug/mL] 

129.38556 1.30301e-2 1.68591 

Totals 1.68591 

Results obtained with enhanced integrator! 

1 Warnings or Errors 

Warning Calibrated compound(s) not found 

Name 

Hydrogen Chloride 

Instrument 3 2/17/2006 3:18:49 PM TG Page 1 of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\O39-4501.D 

0206-54 

Sample Name: Out'0 

Injection Date 2/16/2006 4:41:14 PM Seq. Line 45 

Sample Name Out-02 Location Vial 39 

Acq. Operator KAM Inj 1 

Aoq. Instrument Gonzo Inj Volume 25 •i 

Acq. Method H:kLC2006QIkGONZOkMETHODk0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:\LC2006QIkGONZOkMETHOD\0206-09Z.M 

Last changed 2/17/2006 3:22:40 PM by TG 

(modified after loading) 

No•. 

440 

420 

400 

38O 

360 

340 

ADC1 B, Dionex ED 40 (0206-09A\039-4501 .D) 

2 3 4 5 6 7 8 • 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:22:56 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCl B, Dionex ED 40 

RetTime Type 

[min] 

2. 942 MF 

Area Amt/Area Amount Grp 

[uS*s] [ug/mL] 

164.89482 9.18594e-3 1.51471 

Totals 1.51471 

Results obtained with enhanced integrator! 

1 Warnings or Errors 

Warning Calibrated compound(s) not found 

Name 

Hydrogen Fluoride 

Instrument 3 2/17/2006 3:23:28 PM TG Page 1 of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206_09A\039_4502.D 

0206-54 

Sample Name: Ou 

Injection Date 2/16/2006 4:52:07 PM Seq. Line 45 

Sample Name Out-02 Location Vial 39 

Acq. Operator KAM Inj 2 

Acq. Instrument Gonzo Inj Volume 25 pl Acq. Method H:\LC2006QI\GONZO\METHOD\0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:\LC2006QI\GONZO\METHOD\0206-09Z.M 

Last changed 2/17/2006 3:22:40 PM by TG 

(modified after loading) ADC1B, DionexED40(020•09A\03•4502.D) 

Norm. 

440 

420. 

400 

380 

360 

340 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:22:56 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCI B, Dionex ED 40 

RetTime Type 

[min] 

2.936 MF 

3.6C8 

Area Amt/Area Amount Grp 

[uS*s] [ug/mL] 

168.29863 9.18556e-3 1.54592 

Totals 1.54592 

Results obtained with enhanced integrator! 

1 Warnings or Errors 

Warning Calibrated compound(s) not found 

Name 

Hydrogen Fluoride 

Instrument 3 2/17/2006 3:23:47 PH TG Page I of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\040-4601"D 

0206-54 

Sample Name: Out-03*l• 

Injection Date 2/16/2006 5:03:02 PM Seq. Line 46 

Sample Name Out-03*10 Location Vial 40 

Acq. Operator KAM Inj 1 

Acq. Instrument Gonzo Inj Volume 25 pl 

Acq. Method H:kLC2006QIkGONZO\METHODk0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:\LC2006QIkGONZO\METHOD\0206-09Z.M 

Last changed 2/17/2006 3:22:40 PM by TG 

(modified after loading) 

Norm. 

44O 

420 

400 

380 

360 

ADC1 B, Dionex ED 40 (0206-09Ak040-4601 .D) 

340 

2 3 4 5 6 7 8 mlr 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:22:56 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCl B, Dionex ED 40 

RetTime Type Area Amt/Area Amount Grp 

[min] [uS*s) [ug/mL] 

2.9•2 

3. 664 PB 114.16257 1 31275e-2 1.49867 

Totals 1. 49867 

Results obtained with enhanced integrator! 

i Warnings or Errors 

Warning Calibrated compound(s) not found 

Name 

Hydrogen Chloride 

Instrument 3 2/17/2006 3:24:05 PM TG Page I of 2 
Data:File H:\LC2006Ql\GONZO\DATA\FEB2006\0206-09A\040-4602.D Sample Name: Out-03*!( 

0206-54 

Injeotion Date 2/16/2006 5:]_4:00 PM Seq. Line 46 

Sample Name Out-03*10 Location Vial 40 

Acq. Operator KAM Inj 2 

Acq. Instrument Gonzo Inj Volume 25 pl 

Acq. Method H:\LC2006QI\GONZOkMETHODk0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:kLC2006QIkGONZO\METHOD\0206-09Z.M 

Last changed 2/17/2006 3:22:40 PM by TG 

(modified after loading) 

ADC1B, DionexED40(020•09A•4•4602.D) 

Norm. 

440 

420 

400. 

380 

360 

340 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:22:56 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Faotor with ISTDs 

Signal i: ADCl B, Dionex ED 40 

RetTime Type 

[min] 

2.9•2 

3. 658 PB 

Area Amt/Area •nount Grp 

[uSes] [ug/mL] 

116.14585 1.31134e-2 1.52307 

Totals 1.52307 

Results obtained with enhanced integrator! 

i Warnings or Errors 

Warning Calibrated compound(s) not found 

Name 

Hydrs•an 

Hydrogen Chloride 

Instrument 3 2/17/2006 3:24:18 PM TG Page 1 of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\041-4701"D 

0206-54 

Sample Name: Out-0[ 

Injection Date 2/16/2006 5:24:47 PM Seq. Line 47 

Sample Name Out-03 Location Vial 41 

Acq. Operator KAM Inj 1 

Acq. Instrument Gonzo Inj Volume 25 •i 

Acq. Method H:\LC2006QIkGONZO\METHODk0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:\LC2006QIkGONZO\MZTHODk0206-09Z.M 

Last changed 2/17/2006 3:22:40 PM by TG 

(modified after loading) 

Norm. 

440 

420- 

400 

380 

360 

340 

ADCl B, Dionex ED 40 (0206-09A\041-4701 .D) 

2 3 4 5 6 7 8 m•r 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:22:56 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCI B, Dionez ED 40 

RetTime Type Area Amt/Area 

[min] [uS*s] 

2.878 MF 210.14958 9.18184e-3 

Amount Grp Name 

[ug/mL] 

1.92956 Hydrogen Fluoride 

Totals i. 92956 

Results obtained with enhanced integrator! 

1 Warnings or Zrrors 

Warning Calibrated compound(s) not found 

Instrument 3 2/17/2006 3:24:33 PM TG Page i of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\041-4702.D 

0206-54 

Sample Name: Out 

Injection Date 2/16/2006 5:35:30 PM Seq. Line 47 

Sample Name Out-03 Location Vial 41 

Acq. Operator KAM Inj 2 

Aeq. Instrument Gonzo Inj Volume 25 •i 

Acq. Method H:\LC2006QIkGONZO\METHOD\0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:kLC2006QI\GONZO\METHOD\0206-09Z.M 

Last changed 2/17/2006 3:22:40 PM by TG 

(modified after loading) 

ADC1 B, Dionex ED 40 (0206-09A\041-4702.D) 

420 

40C 

380 

360 

340 

2 3 4 5 6 7 8 m•• 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:22:56 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCI B, Dionex ZD 40 

RetTime Type Area P•t/Area Amount Grp 

[min] [uSes] [ug/mL] 

2.884 MF 209.87709 9.18185e-3 1.92706 

3.560 

Totals 1.92706 

Results obtained with enhanced integrator! 

1 Warnings or Errors 

Warning Calibrated compound(s) not found 

Name 

Hydrogen Fluoride 

Instrument 3 2/].7/2006 3:24:59 PM TG Page 1 of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\042-4801.D 

0206-54 

Sample Name: Out-04 •I 

Injeotion Date 2/16/2006 5:46:20 PM Seq. Line 48 

Sample Name Out-04*10 Location Vial 42 

Acq. Operator KAM Inj 1 

Acq. Instrument Gonzo Inj Volume 25 pl 

Acq. Method H:\LC2006QI\GONZO\METHOD\0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:\LC2006QI\GONZOkMETHOD\0206-09Z.M 

Last changed 2/17/2006 3:22:40 PM by TG 

(modified after loading) 

a0[m. 

440 

420 

400 

38O 

360 

340 

ADCl B, Dione× ED 40 (0206-09A\042-4801.D) 

2 3 4 5 6 7 8 mm 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:22:56 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCI B, Dionex ED 40 

RetTime Type Area Amt/Area Amount Grp 

[min] [uS*s] [ug/mL] 

2. 942 

3. 656 PB 117.52390 1.31039e-2 1.54002 

Totals 1.54002 

Results obtained with enhanced integrator! 

1 Warnings or Errors 

Warning Calibrated compound(s) not found 

Name 

II•d• 2lu•id= 

Hydrogen Chloride 

Instrument 3 2/17/2006 3:25:12 PM TG Page 1 of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\042-4802.D 

0206-54 

Sample Name: Out-04*l< 

Injection Date 2/16/2006 5:57:11 PM Seq. Line 48 

Sample Name Out-04*10 Location Vial 42 

Acq. Operator KAM Inj 2 

Acq. Instrument Gonzo Inj Volume 25 pl 

Acq. Method H:\LC2006QIkGONZOkMETHODk0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:\LC2006QI\GONZO\METHOD\0206-09Z.M 

Last changed 2/17/2006 3:22:40 PM by TG 

(modified after loading) 

NOFF•. 

440 

420 

400 

380 

360. 

340 

ADC1 B, Dionex ED 40 (0206-09Ak042-4802.D) 

2 3 4 5 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:22:56 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCI B, Dionex ED 40 

RetTime Type Area Amt/Area Amount Grp 

[mini [uS*s] [ug/mL] 

•. 

3.656 PB 114.32556 1.31264e-2 1.50068 

Totals 1.50068 

Results obtained with enhanced integrator! 

1 Warnings or Zrrors 

Warning Calibrated compound(s) not found 

Name 

IIyd•=• Fl•id• 

Hydrogen Chloride 

Instrument 3 2/17/2006 3:25:20 PM TG Page 1 of 2 
Data File H:\LC2006QI.\GONZO\DATA\FEB2006\0206-09A\043-4901.D 

0206-54 

Sample Name: Out-0r 

Injection Date 2/16/2006 6:07:55 PM Seq. Line 49 

Sample Name Out-04 Location Vial 43 

Acq. Operator KAM Inj 1 

Acq. Instrument Gonzo Inj Volume 25 •i 

Acq. Method H:\LC2006QIkGONZOkMETHOD\0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:\LC2006QI\GONZOkMETHODk0206-09Z.M 

Last changed 2/17/2006 3:22:40 PM by TG 

(modified after loading) 

N( 

ADC'I B, Dionex ED 40 (0206-09A\043-4901.D) 

2 3 4 5 6 7 8 m•._• 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:22:56 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCI B, Dionex ED 40 

RetTime Type 

[mini 

2.896 MF 

3. 6CO 

Area Amt/Area }hmount Grp 

[uS*s] [ug/mL] 

170.70175 9.18530e-3 1.56795 

Totals 1.56795 

Results obtained with enhanced integrator! 

1 Warnings or Zrrors 

Warning Calibrated compound(s) not found 

Name 

Hydrogen Fluoride 

lI•d• l•d• 

Instrument 3 2/17/2006 3:25:36 PM TG Page 1 of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\043-4902.D 

0206-54 

Sample Name: Out-0<' 

Injection Date 2/16/2006 6:18:44 PM Seq. Line 49 

Sample Name Out-04 Location Vial 43 

Acq, Operator KAM Inj 2 

Aoq. Instrument Gonzo Inj Volume 25 •i 

Aoq. Method H:\LC2006QIkGONZO\METHODk0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:\LC2006QI\GONZOkMETHOD\0206-09Z.M 

Last changed 2/17/2006 3:22:40 PM by TG 

(modified after loading) 

420 

400 

380 

360 

ADC1 B, Dionex ED 40 (0206-09A\043-4902.D) 

External Standard Report 

mir 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:22:56 PM 

Multiplier 1,0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal I: ADCl B, Dionex ED 40 

RetTime Type 

[min] 

2.890 MF 

'3,660 

Area Amt/Area Amount Grp 

[uS•s] [ug/mL] 

175.28098 9.18481e-3 1,60992 

Totals 1. 60992 

Results obtained with enhanced integrator! 

1 Warnings or Zrrors 

Warning Calibrated compound(s) not found 

Name 

Hydrogen Fluoride 

IIyd•. @hi id• 

Instrument 3 2/17/2006 3:25:55 PM TG Page 1 of 2 
Data File H:\LC2006QI\GONZO\DATA\FEB2006\0206-09A\044-5001.D 

0206-54 Sample Blank 

Sample Name: 

Injection Date 2/16/2006 6:28:51 PM Seq. Line 50 

Sample Name Blank*4.09 Location Vial 44 

Acq. Operator KAM Inj 1 

Acq. Instrument Gonzo Inj Volume 25 pl 

Acq. Method H:\LC2006QI\GONZO\METHOD\0106-48.M 

Last changed 2/7/2006 1:48:48 PM by TG 

Analysis Method H:\LC2006QIkGONZO\METHOD\0206-09Z.M 

Last changed 2/17/2006 3:22:40 PM by TG 

(modified after loading) 

Norm. 

440 

420 

400 

380 

360 

340 

ADC1 B, Dionex ED 40 (0206-09A\044-5001 .D) 

2 3 4 5 6 7 8 mi•r 

External Standard Report 

Sorted By Signal 

Calib. Data Modified 2/17/2006 3:22:56 PM 

Multiplier 1.0000 

Dilution 1.0000 

Use Multiplier & Dilution Factor with ISTDs 

Signal i: ADCI B, Dionex ED 40 

RetTime Type Area Amt/Area Amount Grp 

[min] [uS*s] [ug/mL] 

2.942 

3. 660 

Totals 0.00000 

Results obtained with enhanced integrator! 

1 Warnings or Errors 

Warning Calibrated compound(s) not found 

Name 

Hydrogen Fluoride 

Hydrogen Chloride 

Instrument 3 2/17/2006 3:26:13 PM TG Page 1 of 2 
Appendix 

Sample Calculations 

Appendi× C 

Gas Meter Calibration 

Sheets 
O• •- 
•. • • 0 0 0 

c•c• • 

O C) 143 

0 0 
C• 0 C3 

Appendix D 

Process Data