425 S*ufh i\Tain SN., Suite 201

Anu Arbor'" tuIiehigan J81lì4

'îel: 7 34.9Í3 "2$80 Fax: 734,668.1541

Re:

JuIy 1,2009

Mr. Terry Sanner

Southwest District Office

Ohio EPA DAPC

401 East Fifth Street

Dayton, OH 43377

Submittal of Emissions Testing Report

Bellefontøine Gøs Producers, LLC (permit #p0I0B6g0

Bellefontaine, Ohio

Dear Mr. Sanner:

Attached find the final report for emissions testing conducted at Bellefontaine

Gas Producers, LLC on June 3,2009. The testing *ut conducted to demonstrate

compliance with the emissions limits specified in Air Pollution Permit-to-Install

nnd Operøte, Permit No, P0103690. The testing was conducted in accordance with

the Intent to Test notification sent to and approved by the OEPA prior to testing.

As indicated in the report, emissions from the tested, representative internal

cornbustion engine comply with both NSps (40 cFR, pirt 60,subpart lllf and

OEPA Permit limits. The report contains all test and support datå thai are the

basis for this determination.

If you have any questions concerning the report or any portion of the test

program, please contact me.

Sincerely,

DTE BIOMASS ENERGY

Thomas Durham

Environmental Engineer

enc. "PM, SOz, NOx, CO, and NMOC Emissions Testing Report,,

cc: M. Kotyk - DTE Biomass Energy (w / o enclosure)

G. Autolitano - Bellefontaine Gas producers ,LLC (w / o enclosure)

D. Terry - Bellefontaine Gas producers, LLC (with enclosure)

K

DïE Energy"

PM, SOz, NOx, CO, AND NMOC EMISSIONS

TESTING REPORT

Ohio Permit to lnstail No. pOl0g690

UNIT 3

BELLEFONTAINE GAS PRODUCERS, LLC

BELLEFONTAINE, OHIO

June,2009
DfE Energy' K

CONTENTS

Section Page

EXECUTTVE SUMM4RY........... ................tV

r. 0 !NTRoDUCT|ON..... ........ 1

2.0 souRcE DEscR¡pTroN........ ........1

3.0 SAMPLING AND ANALYTICAL PROCEDURES .........,.2

3.1 STACK GAS VELOCTTY AND FLOWRATES (USEPA METHODS 1-21 ......3

3.1.1 Sampling Method..... .....................3

3.1.2 Method 2 Sampling Equipment............... ........................3 3,2 OXYGEN AND CARBON D|OXIDE (USEPA METHODS 3A) ......3

3.2.1 Sampling Method..... .....................3

3.2.2 Oz I COz Sampling Train .............3

3.2.3 Sampling Train Calibration .........4 3.3 MOISTUREDETERMINATTON(USEPAMETHOD4)...................................4

3.3.1 Sampling Method..... .....................4 3.4 PARTICULATE MATTER (USEPA METHOD 5).......... .................4

3.4.1 Filterable Particulate Sampling Method (USEPA METHOD 5)......................4

3.4.3 Quality Control and Assurance............ ........5 3.5 SULFUR DIOXIDE, OXIDES OF NITROGEN AND CARBON MONOXIDE

(usEPA METHODS 6C,78 AND 10)... ....................5

3.5.1 Sampling Method..... ....................,5

3.5.2 SOz, NO*, and CO Sampling Train......... ........................6

3,5.3 Sampling Train Calibration .........6 3.6 METHANE (USEPA METHOD r8)........... .....................6

3.6.1 Sampling Method..... .....................6

3.6.2 CH4 Sampling Train ....................7

3.6.3 Sampling Duration & Frequency............... ......................7

3.6.4 Sampling Analysis ........................7 3.7 TOTAL HYDROCARBON COMPOUNDS (USEPA METHOD 25A) .............7

3.7.1 Sampling Method..... .....................7

3.7.2 THC Sampling Train ....................7

3.7.3 Sampling Train Calibration .........8

3.7.4 Sampling Duration & Frequency............... ......................8 3.8 QA/QC AND POST TEST PROCEDURES......... ..........8

3.8.1 Quality Control and Assurance (O2, CO2, SO2, NO*, and CO) ..... ................8

3.8.2 Quality Control and Assurance (NMOC).............. .........9 3.9 DATA REDUCTION.......... ..........9

4.0 oPER.ATING PARAMETERS.... ....................10

ii
DïE Energy' K

5.0 RESULTS .....10

6.0 cERTtFtCATtON STATEMENT............ .........11

Result Table

Particulate Emissions Testing Results

SO2, NOx, CO, NMOC Emissions Testing Results

Fiqures

1 Unit 3 Stack Drawing & Exhaust Sampling point Location 2 USEPA Method 5 Samplíng Train 3 USEPA Method 3N6CnEl10 Sampting Train 4 USEPA Method 18 Sampling Train 5 USEPA Method 254 Sampling Train

Appendices

A OEPA Test Plan B Equipment and Analyzer Calíbration Data C Example Calculations D Particulate Data E RawAnalyzer Data F Operational Data G Analytical Data

i¡i
DïE Energy"

EXECUTIVE SUMMARY

DTE Energy Corporate Services, LLC (DECS), a DTE Energy Company (DTE)

performed emissions testing at Bellefontaine Gas Producers, LLC, located in

Bellefontaine, Ohio. The fieldwork, performed on June 3, 2009 was conducted to

satisñ7 requirements of the Ohio Permit to lnstall No. P0103690 and EPA 40 CFR Part

60 Subpart JJJJ. Emissions tests were performed on Unit 3 for particulate matter

(PM), sulfur dioxide (SOz), oxides of nitrogen (NO"), carbon monoxide (CO), and nonmethane organic compounds (NMOC).

The results of the emissions testing are highlighted below:

Emissions Testing Summary

Bellefontaine Gas Producerc, LLC

Bellefontaine, OH

Unit 3

Operational Horsepower - 2,233 BHp

June 3, 2009

Unit 3 Sulfur Dioxide

(lb/MMBtu)

Oxides of

Nitrogen

lolBHn-Hrì

Carbon

Monoxide

lalRHn-Hrl

NMOC

(s/BHp-Hr)

Particulate

(lb/MMBtu)

Permit Limit 0.5 0.60 3.0 1.0 0.062

Test 1 0.01 0.52 27 ND 0.004

Test 2 0.01 o52 27 ND 0.002

Test 3 0.01 0.52 27 ND 0.002

Average 0.01 0.52 2.7 ND 0.003

IV
DIE Energy"

1.0 INTRODUCTION

DTE Energy corporate services, _LL_c (DEcs), a DTE Energy company (DTE) performed emissions testing at Bellefontaine Gas Producer!, LLC, Iocated in Bellefontaine, Ohio, The fieldwork, performed on June 3, 2OOg, was conducted to satisfy requirements of the Ohio Permit to lnstall No. p0103690 and EpA 40 CFR Paft 60 Sub-Part JJJJ.

Testing was performed pursuant to Title 40, Code of Federal Regutations, paft 60, AppendixA (40 CFR SO0 App.A), Methods 1-S, 6C, 7F_,10,1g, anã 25A.

The fieldwork was performed on one representative engine in accordance with EpA Reference Methods and DECS lntent to Test & Test Þlan Submittal Lettei, urfrì.f,

was submitted to Ohio Department of En

on March 11, 2009. The following D

program: Mr. Mark Grigereit, Environ

Environmental Technician and Mr. Fran

was the project leader. Mr. Grigereit h

testing for DTE Energy and private consu

of source testing experience testing for D

Mr. Thomas Durham, Environmental Engíneer, DTE Energy Resources, LLc

rocess coordination for the testing program. Mr. Dave Terry, power

, Shaw Environmental & lnfrastructure Group provided on-site support of the units. Mr. Terry Sanner, Environmental Specialist with the

Pollution Control, SW District Office of the OEPA reviewed the Test

Plan and observed the testing.

2.0 SOURCE DESCRIPTION

The Bellefontaine Gas Producers, LLC power generating facility, located at 2g46 US Route 68 North, Bellefontaine, Ohio is a power generating"facility. The facility consists of three (3) similar landfill gas-fired intãrnal combustion engines with associated electrical generators

The systems are caterpillar G352oc - 12oo RPM 1600 kw Engine Generator sets. The sources utilize landfill gas from the Cherokee Run Landfilltiproduce energy that is sent to the electrical grid. All testing was performed while the enginã was operating at full load conditions (2,233 B lp). See Figure 1 for a diagram of the tested units' stack dimension and sampling location.
3.0 SAMPLING AND ANALYTICAL PROCEDURES

DTE Energy obtained emissions measurements in accordance with procedures

specified in the USEPA Standards of Performance for New Stationary Sources. The

sampling and analytical methods used in the testing program are indicated in the

table below.

Sampling Method Parameter Analysis

USEPA Methods 1-2 Exhaust Gas Flow Rates Field data analysis and

reduction

USEPA Method 3A Oxygen & CO2 lnstrumental Analyzer

Method

USEPA Method 4 Moisture Content Field data analysis and

reduction

USEPA Method 5 Particulate Matter Gravimetric Analysis

USEPA Method 6C Sulfur Dioxide

U ltraviolet Fluorescence

lnstrumental Analyzer

Method

USEPA Method 7E Oxides of Nitrogen

Chemiluminecent

lnstrumental Analyzer

Method

USEPA Method 10 Carbon Monoxide

NDIR

lnstrumental Analyzer

Method

USEPA Method 18 Gaseous Organic

Compounds (Methane)

GC

Analytical Method

edlarru Bao Samn

USEPA Method 254 Total Hydrocarbon

Compounds

FID

lnstrumental Analyzer

Method

2
DÌE Energy'

3.1 STACK GAS VELOCITYAND FLOWRATES (USEPA METHODS T.2)

3.1.1 Sampling Method

Stack gas velocity traverses were conducted in accordance with the

procedures outlined in USEPA Method 1, "sample and Velocity Traverses for

Stationary Sources," and Method 2, "Determination of Stack Gas Velocity and

Volumetric Flowrate." Two (2) sampling ports were utilized on the Únit's

exhaust duct, sampling at four (4) points per port for a total of eight (8) points.

Sampling was conducted in conjunction with the gaseous emissiõns testing.

A cyclonic flow check was performed prior to the flowrate testing. Testing in

the stack demonstrated that no cyclonic flow is present. Data has béen

included in Appendix D demonstrating the absence of cyclonic flow.

3.1.2 Method 2 Sampling Equipment

DTE Energy's EPA Method 2 sampling

incline manometer, S-type pitot tube (Co

thermocouple.

equipment consisted of a 0-10"

= 0.84) and a Type-K calibrated

3.2 OXycEN AND CARBON D|OX|DE (USEPA METHOD 3A)

3.2.1 Sampling Method

Oxygen (O2) and Carbon Dioxide (COt emissions were evaluated using

USEPA Method 34, "Gas Analysis for carbon Dioxide, oxygen, Excess Aii

and Dry Molecular Weight (lnstrumental Analyzer Method)". The analyzers

utilize paramagnetic sensors. Testing was pedormed simultaneously with the

particulate emissions testing and consisted of triplicate 60-minute sample

runs.

3.2.2 02l CO2Sampling Train

The DECS EPA Method 3A sampling system consisted of (1) a single-point

sampling probe (placed in the center of the stack), (2) a heated TeflonrM

sampling line, (3) a Universal@ gas conditioner with particulate filter, (4) a

flexible unheated reflonrM sampling line, (5) a servomax 1400 ozlcoz gas

analyzer, (6) appropriate USEPA Protocol 1 calibration gases, and (7) anllO

Plexer@ Data Acquisition System.
Energy'

3.3

Refer to Figure 3 for a schematic of the Oz, COz, SOz, NO", and CO

sampling train.

3.2.3 Sampling Train Galibration

The Oz and COz analyzers were calibrated according to procedures outlined

in USEPA Method 7E. Zero, span, and mid range calibration gases were

introduced directly into the analyzer to determine the instruments linearity. A

zero and míd range span gas for each dilluent was then introduced through

the entire sampling system to determine sampling system bias for each

analyzer at the completion of each test.

MOTSTURE DETERMTNATTON (USEPA METHOD 4)

3.3.1 Sampling Method

Determination of the moisture content of the exhaust gas was performed

using the method described in USEPA Method 4, "Determination of Moisture

Content in Stack Gases". The moisture was collected in glass impingers, and

the percentage of water was then derived from calculations outlined in

USEPA Method 4. Moisture determinations were made in conjunction with

particulate sampling.

PARTTCULATE MATTER (USEPA METHOD 5)

3.4.1 Filterable PaÉiculate Sampling Method (USEPA METHOD 5)

USEPA Method 5, "Determination of Particulate Emissions from Stationary

Sources" was used to measure the filterable (front-half) particulate

concentrations (see Figure 2 for a schematic of the sampling train). Three

60-minute test runs were conducted.

The DECS Method 5 modular isokinetic stack sampling system consisted of

(1) a staÍnless-steel button-hooknozzle, (2) a heated glass-lined probe, (3) a

heated 4" glass filter holder with a glass fiber filter, (4) a set of four

Greenburg-Smith (GS) impingers with the first and second each containing

100 milliliters (mL) of HzO, the third dry and a fourth impinger containing

approximately 300 grams of silica gel desiccant, (5) a length of sample line,

and (6) an Environmental Supply@ control case equipped with a pump, dry

gas meter, and calibrated orifice.

3.4

4
3.5

DTE Energy"

After completion of the final leak test for each test run, the filter was

recovered, and the probe, nozzle and the front half of the filter holder

assembly were brushed and rinsed with acetone. The acetone rinses were

collected in a pre-cleaned sample container. DECS labeled the container with

the test number, test location, test date, and marked the level of liquid on the

outside of the container. lmmediately after recovery, the sample containers

were placed in a cooler for storage.

The acetone rinses were transferred to clean pre-weighed beakers. The

beakers were weighed following room-temperature evaporation, and then

desiccated to a constant weight (<0.5mg variability). Filters were dried in a

desiccator to a constant weight (<0.5mg variability). The data sheets

containing the initial and finalweights on the filters and beakers can be found

in Appendix G.

Collected field blanks consisted of a filter blank and acetone solution blank.

The acetone blank was collected from the rinse bottle used in sample

recovery. The blank filter and acetone were collected and analyzed following

the same procedures used to recover and analyze the fìerd sampres.

The impinger solution volume was measured to determine moisture content of

the gas stream. After measuring and recording the liquid volumes, the

solution was discarded

Field data sheets for Method 5 sampling can be found in Appendix D.

3.4.3 Quality Gontrol and Assurance

All sampling and analytical equipment was calibrated according to the

guidelines referenced in EPA Method 5.

Calibration data can be referred to in Appçndix B.

SULFUR DIOXIDE, OXIDES OF NITROGEN AND CARBON MONOXIDE

(usEPA METHODS 6C, 7E AND 10)

3.5.1 Sampling Method

Sulfur dioxide (soz) emissions were evaluated using USEPA Method 6c,

"Determination of Sulfur Dioxide Emissions from Stationary Sources". The

SO2 analyzer utilizes an ultraviolet fluorescence detector. Oxides of nitrogen

(No, emissíons were evaluated using USEPA Method 7E, "Determination of

oxides of Nitrogen Emissions from Stationary sources", The No" analyzer
DïE Energy' K

utilizes a Chemiluminecent detector. Carbon monoxide (CO) emissions were

evaluated using USEPA Method 10, "Determination of Carbon Monoxide

Emissions from Stationary Sources". The CO analyzer utilizes an NDIR

detector.

3.5,2 SOz, NO,, and CO Sampling Train

The EPA Methods 6C, 7E and 10 sampling system consisted of (1) a singlepoint sampling probe (placed in the center of the stack), (2) a heated

TeflonrM sampling line, (3) a Universal@ gas conditioner with particulate filter,

(4) a flexible unheated TeflonrM sampling line, (5) a Bovar-Western

Research SO2 gas analyzer, TECO 42i Chemiluminecent NO/NO" gas

analyzer, and TECO 48i NDIR CO gas analyzer, (6) appropriate USEPA

Protocol 1 calibration gases, and (7) an l/O Plexer@ Data Acquisition System.

Refer to Figure 3 for a schematic of the 02, COz, SOz, NO*, and CO

sampling train.

3.5.3 Sampling Train Galibration

The sampling train was calibrated according to procedures outlined in

USEPA Method 7E. Zero, span, and mid range calibration gases were

introduced directly into the analyzer to determine the instruments linearity. A

zero and mid range span gas for each pollutant was then introduced through

the entire sampling system to determine sampling system bias for each

analyzer at the completion of each test.

3.6 METHANE (USEPA METHOD 18)

3.6.1 Sampling Method

Methane (CH¿) emissions were evaluated using USEPA Method 18,

"Measurement of Gaseous Organic Compound Emissions by Gas

Chromatography (TedlarrM Bag Sampling)". This method involves the

collection of exhaust gas in a Tedlartt b"g, which is then analyzed at an offsite laboratory by gas chromatography (GC)

Results from the methane sampling were used to determine the non-methane

organic compound concentration from the source. Methane emissions were

subtracted from total organic compound emissions (as determined by Method

254).
DTE Energy.

3.6.2 CH4 Sampling Train

The Method 18 sampling system followed the procedures specified in

section 8.2.1,lntegrated Bag sampling & Analysis. The sampling system

consisted of (1) an un-heated TeflonrM sampling line (kept to the minimum

length required) located after the heated sampling line and immediately

before the JUM 1094, (2) a sampling lung with 1O-liter TedlarrM bag, and (3)

a vacuum pump with regulator.

Refer to Figure 4 for a schematic of the Method 18 sampling train.

3.6.3 Sampling Duration & Frequency

Methane samples were collected simultaneously with the total hydrocarbon

(THC) testing. The vacuum pump flowrate was set to allow for a constant

rate, integrated sample, collected for the duration of each test run.

3.6.4 SamplingAnalysis

DECS labeled the tedlar bag samples with the test number, test location and

test date. The samples were shipped overnight via Federal Express on the

day that they were collected. Methane analysis was performed on the

following day. Analysis, performed by Enthalpy Analytical Laboratory,

Durham, NC followed guidelines of EpA Method 1g, including triplicate

analysis and a spike recovery study. Analytical results for M18 arelocated in

Appendix G.

3.7 TOTAL HYDROCARBON COMPOUNDS (USEPA METHOD 25A)

3.7.1 Sampling Method

Total hydrocarbon compound (THC) emissions were evaluated using USEpA

Method 25A, "Determination of Total Hydrocarbon Emissions from Stationary

Sources (lnstrumentalAnalyzer Method)". The THC analyzer utilizes a flame

ionization detector (FlD). The FID measures total hydrocarbon compounds.

3.7.2 THC Sampling Train

DECS' EPA Method 254 sampling system consisted of (1) a single-point

sampling probe (placed in the center of the stack), (2) a heated TeflonrM

sampling line, (3) a JUM 1094@ THC gas analyzer, (4) appropriate certified

calibration gases, and (5) a ThermoWestronics@ Data Acquisition System.

7
DTE Energy"

Refer to Figure 5 for a schematic of the THC sampling train.

3.7.3 Sampling Train Galibration

ln accordance with USEPA Method 25A, a 4-point (zero,low, mid, and high)

calibration check was performed on the THC analyzer. The analyzer was

calibrated with propane in the 0-1,500 ppm range. Calibration drift checks

were performed at the completion of each run.

3.7.4 Sampling Duration & Frequency

The THC gaseous emission testing was performed simultaneously with the

other emissions sampling. Data was recorded at 4-second interuals and

average over 1-minute periods.

3.8 QA/QC AND POST TEST PROCEDURES

3.8.1 Quality Control and Assurance (O2, CO2, SO2, NOr, and GO)

All sampling and analytical equipment was calibrated according to the

guidelines referenced in Methods 34, 6c, 7E, and 10. calibration gases

were EPA Protocol 1 gases and the concentrations were within the

acceptable ranges (40-60% mid range and span) specified in Methods 3A

and7E. Calibration gas certification sheets are located in Appendix B.

DTE performed converter efficiency testing by directly challenging the NO*

analyzer with a nitrogen dioxide (NOz) calibration gas of 49.63 ppm. Results

from the converter efficiency test demonstrated that the analyzer met the

requirements of Method 75(ec t).

Eq. 1

Eff.,^^ -Co,, - 

49'5 ' ,r No2 - =99o/o ç, 59.63

8
IDTE Energy.

3.8.2 Quality Control andAssurance (NMOC)

The THC sampling equipment was calibrated with propane (c¡Ha) according

to the guidelines referenced in Methods 254. Calibration gases were EpA

Protocol 1 gases and the concentrations were within the acceptable ranges

(25-35% low range, 45-55% mid range and 80-100 span).

An analyzer response factor (RF) of 3 was applied to the CHa concentration

in the exhaust gas, as determined by Method 18 sampring. The cHa 1"g

methane) was converted to CJJ+^(", propane) in order to subtract the CH¿ from the

THC measured in 1¡" ¡"¡6Go' z).

Eq.2

NMoc : THCrrrlosc3Hs) -(cn ^rfrrr^,) = ro, t#) = ND

Calibration gas certification sheets are located in Appendix B.

3.9 DATA REDUCTION

Data collected during the emissions testing was reported according to

emissions limits specified in the facility's OEPA Permit to lnstall No. polOeOgO

and EPA Subpart JJJJ. Particulate and SOz emissions were reported as

pounds per million Btu (lb/MMBtu). Oxides of nitrogen, CO, and NMOC were

reported as grams per brake horsepower hour (g/BHp-Hr).

Emissions calculations are based on calculations located in USEPA Methods

1-5 and 19. A fuel factor for the landfill gas was determined from landfill gas

sampling at the inlet to the engine. Example calculations are presented in

Appendix C and landfill gas analysis is presented in Appendix G.

Non-methane organic compound emissions are reported as non-detect (ND).

Methane is collected via Method 18 (GC) and reported as methane. The

concentration is then divided by 3 per Method 254 so that methane can be

subtracted from the total hydrocarbon concentration (reported as propane)

established by testing with a FlD,

I
DÏE

4.0

Energy'

OPERATING PARAMETERS

The test program included the collection of generator load (kW), engine speed

(RPM), inlet manifold air pressure (psi), fuel upper heating value (BTU), fuel

flow (scfm) and generator operating hours (kW-hour).

Operationaldata are located in Appendix F.

RESULTS

The results of the testing indicate that Unit 3 is in compliance with emissions

concentrations stated in Ohio Permit to lnstall No. P0103690 and EPA 40

CFR Part 60 Subpad JJJJ. Testing was performed while the engine was

operating at the maximum rated horsepower.

Emissions Testing Summary

Bellefontaine Gas Producers, LLC

Bellefontaine, OH

Unit 3

Operational Horsepower - 2,233 BHp

June 3, 2009

5.0

Unit 3 Sulfur Dioxide

(lb/MMBtu)

Oxides of

Nitrogen

lolRHn-Hrl

Carbon

Monoxide

lolBHo-Hr)

NMOC

(g/BHp-Hr)

Particulate

(lb/MMBtu)

Permit Limit 0.5 0.60 3.0 1.0 0.062

Test 1 001 052 27 ND 0.004

Test 2 001 0.52 27 ND 0.002

Test 3 001 0.52 27 ND 0.002

Average 0.01 0.52 2.7 ND 0.003

10
DIE Energy" K

6.0 C ERTI FICATION STATEMENT

"l certify that I believe the information provided in this document is true, accurate, and

complete. Results of testing are based on the good faith application of sound

professionaljudgment, using techniques, factors, or standards approved by the

Local, state, or Federal Governing body, or generally accepted in the trade."

This report prepared by:

Environmental Management and Resources

DTE Energy Corporate Services, LLC

This report reviewed by:

Supervisor, Stationary Source & Ambient Monitoring

Environmental Management and Resources

DTE Energy Corporate Services, LLC

11
DïE Energy'

RESULTS TABLES
Results Table I

Gaseous Emissions Testing Results

Unit 3

Bellefontaine Gas Producers, LLC

Bellefontaine, OH

Parameter Run I Run 2 Run 3 Aver

Sampling Date

Sampling Start Time

Load (BHp)

Flowrate (scfm)

Flowrate (dscfm)

Average 02 Content (%, dry)

Average O, Content (%, dry, corrected)1

Average CO Concentration (ppmv, dry)

Average CO Concentration (ppmv, dry, corrected)1

Average GO Concentration (ppmv, dry, corrected)2

Average CO Emission Rate (lb/hr)

Average CO Emission Rate (gram/BHp-Hr, dry)

Average NO" Concentration (ppmv, dry)

Average NO,. Concentration (ppmv, dry, corrected)1

Average NO" Goncentration (ppmv, dry, corrected)2

Average NO, Emission Rate (lb/hr)

Average NOx Emission Rate (gram/BHp-Hr, dry)

Average SO2 Concentration (ppmv, dry)

Average SO2 Concentration (ppmv, dry, corrected)1

Average SO2 Concentration (ppmv, dry, corrected)z

Average S02 Goncentration (lb/MMBtu)

Average THC Concentration (ppmv as C3H6)

Average CHa Concentration (ppmv as CH4)

Average CHo Concentration (ppmv as C3Hu)3

Average NMOC Concentration (ppmv)

Average NMOC Concentration (ppmv, corrected)2

06/03/09

0804-0904

2,233

5,726

5,038

8.0

8.1

584.7

601.6

277.8

13.22

2.7

69.6

71.1

32.8

2.57

0.5

4.9

4.9

2.3

0.01

545

1,730

577

ND

ND

I

06/03/09

0952-1052

2,233

5,762

5,045

8.0

8.1

579.0

597.5

276.0

1 3.15

2.7

69.7

71.4

33.0

2.58

0.5

5.4

5.6

2.6

0.01

550

1,723

574

ND

ND

06/03/09

1132-1232

2,233

5,796

5,071

8.1

8.2

573.1

591.9

274.1

13.09

2.7

68.7

70.7

32.7

2.57

0.5

5.8

5.9

2.7

0.01

557

1,690

s63

ND

ND

5,761

5,051

8.0

8.1

578.9

597.0

275.9

13.2

2.7

69.3

71.1

32.8

2.6

0.5

5.4

5.5

2.5

0.01

s51

1 ,714

571

ND

ND

lcorrected for analyzer drift as per USEPA Method 7E

2 al15Yo02

3corrected 

as C3

kW:killowatts

02 : oxygen

CO : carbon monoxide

NO* : oxides of nitrogen

ND : non-detection (less than zero)

THC : total hydrocarbons

CHa : methane

C3H6 : propane

NMOC : non-methane organic compounds
Results Table 2

Particulate Emissions Testing Results

Bellefontaine Gas Producers LLC

Bellefontaine, OH

June 3, 2009

Start Time

Stop Time

Meter Temperature ïm (oF)

Meter Pressure - Pm (in. Hg)

Measured Sample Volume (Vm)

Sample Volume (Vm-Std)

Condensate Volume (Vw-std)

Gas Density (Ps(std) lbs/ft3)

Total weight of sampled gas (lbs)

Nozzle Size - An (sq. ft,)

lsokinetic Variation - |

Average Stack Temperature - Ts (F)

Molecular Weight Stack Gas- dry (Md)

Molecular Weight Stack Gas-wet (Ms)

Stack Gas Specific Gravity (Gs)

Percent Moisture (Bws)

Water Vapor Volume (fraction)

Pressure - Ps ("Hg)

Average Stack Velocity -Vs (ft/sec)

Area of Stack (ft2)

Exhaust Gas Flowrate

Flowrate (acfm)

Flowrate (scfm)

Flowrate (dscfm)

Particulate

oncentration

lb/1000|b (dry)

lb/10001b (wet)

lb/1000 lb (wet, corrected to 50% EA)

Particulate Emission Rate

culate Goncentration

Percent 02

Fuel Factor (F¿)

lb/scf (C6)

lb/MMBtu

71.92

30.12

39.12

38.36

5.39

0.07396

3.24

0.0001709

103.4

877.1

30.11

28.62

0.99

12.33

0j23

29.85

173.93

1.40

14,571

5,761

5,051

lb/hr

70.50

30.12

38.48

37.84

5.16

o.o7407

3.19

0.0001709

102.3

72.44

30.12

39.23

38.43

5.47

0.07393

3.25

0.0001709

103.7

72.81

30.12

39.65

38.82

5.55

0.07388

3.28

0.0001709

104.3

876.9

30.11

28.66

0.99

12.01

o.120

29.85

172.82

1.4

877.4

30.11

28.60

0.99

12.45

o.125

29.85

174.00

1.4

877.O

30.1 0

28.59

0.99

12.52

0.125

29.85

174.96

1.4

8.1

8,714

1.664E-07

0.002
DTE Energy" K

FIGURES
IDTE Energy'

Stack Diameter 16"

Figure No. 1

DTE Tesi Traifer

Velocity Measurement Points

Distance From

lnner Wall

1.07

4.00

12.00

14.93

Source Diaqram

Bellefontaine Gas Producers, LLG

ck Sampling Group

tal Management &
DTE Energy"

Figure No. 2

USEPA Method 5

Heated Probe M Pyrex Glass Liner & SS Nozzle

Management & Resources
Energy"

Heated Sample Line

Calibration Line Data Acquisition System

Flow Controller

Calibration Gas

Figure No.3

USEPA Methods 3N6Cl7El1O

Site:

Bellefontaine Gas Producers, LLC

Bellefontaine, OH

Sampling Date:

June 3, 2009

Stack Sampling Group

Environmental Management &

Western Research SO2

TECO 42i NOx Analyzer

c""O

Conditioner

I

TECO 48iCO Analyzer

Servomax O2|COZ Analyzer
IDïE Energy'

Figure No.4

USEPA Method l8

JUM 1O9A

Tedlar Bag

Heated Sample Line

Teflon Sample Line

Vacuum Pump

Site:

Bellefontaine Gas Producers, LLC

Sampling Date:

llefontaine, OH

June 3,2009

Stack Sampling Group

Environmental Management &
IDTE Energy'

Figure No.5

USEPA Method 254

J.U.M. IO9A

Methane/Non-Methane

Total Hydrocarbon Analyzer

Flow Controller

Sampling Date:

Bellefontaine Gas Producers, LLG June 3, 2009

Stack Sampling Group

Environmental Management &
DIE Energy.

APPENDIX A

OEPA TEST PLAN
,* l-! Siiu+Ìi: :1,{,¡É¡1. S+sct.. .ìl¡it* Íi{liii

,iiÍ:íì,.Irir+r. l'¿f il.:i:í,e..ut .¿ù l: û,{

Ii"i;: ,¡ i,$ ìtÐ +&),I Ë.:r:rs: ?..14_ì[)i-.t8iir].

IITE tu*wgry

It4arch 11,2009

Mr, Terrv Sarlrre'r

Ohio EPA DAPC

Southlvest Dístrict ()ffi ce

401 East Fifth Streert

Dayton, OII 43311

ü'!Fì Ênergg kieswrces

Rer Intent to Test î¡ Test pløn Subtnittal

Bcllefontøíne G,as Producers, LLC (pertnit No, p010-q6g0)

Bellefontaíne, öhio

Dear lvfr Sanner:

On behalf of Bcllefontaine Gas Procìucers, LI-C (BGI'j), DTE Errergy Resources, Inc. is pleasecl to

submit the attached Intent to Test arrd Test Plan for rerriew and-approval. In accordarrce with

Ohio Envirortmental Protection Agency - Dil'isior.r <¡f Air Pollution Control, Permit-to-Insta.ll and

Operate No- P0103690, BGP operates three internal combustiorr engines at the facility (Ir001, p002

anct P003). The attached Test Ptan prese'nts the methodology proposecl for the Compliance

Demonstratio., BGI) proposes April 15, 2009 as the clate fclr tesiing.

The CAT 3520C engirres installed at the site are iclentical rnodels ancl lvere all installed cluring the

same period by the same personnel. z\s prevíously irclicated in the NSIjS Commencement of

Const¡uction Notification, the 'buiit date' fc¡¡ all th¡c'e engines are between Nlay 73-17,200g. With

resPect to manufacturing and installatiory the engines are as identical as possiÛle,

In consideration of both the truly identicaì nature of the engines, and clf the unusual financial

Pressures facin¿¡ businesses at this time, BGP is requesting that OEPA allow for a Compliance

Demonstration based on ihe testing of olrly onc' of the three IC engines, From a technical

perspective it is our belief that there is absolutely no reason, at this time in the tife cycle of the

engines, to exPect that their emission profiles are different. Similarly, in a time of nearly

unprececlented fi¡ancial uncertainty BGP, like all businesses, is aggressively looking fr-lr lvavs to control exPenses' We believe that this one en6;ine test approacÈ, pr"runtr,r"ry'iittl" ¡ìsk of

undiscor,'ered non-compliance, while allowing tlGP to ccmtinue to serve the community of

Bellfontaine through the 'berreficial use' operati<r of the plant.

-A.s mentionecl, pending your approval of the this plan, testing is scheclulecl for Apriì 1.5,2009. I can be corrtactecl at Q3Q 3t2-82j4 or af durh-amt@clteelrerqli.com if you have any questions

or need aclclit.ional info¡nration.

Silce'rel1.,

RCES

Environmental lìngineer

Gary Autoìitano, lJellefontaine Cas procf ucers, Ll,C
INTENT TO TEST NOTIFICAT|ON (One Emissions Unit per Sheet)

A. Facility Contact lnformation:

Name Bellefontaine Gas proCucers. LLC

Address

Contact person Mr. Gary Autolitano

Telephone (O) 570.383.7170 _ 

(Ce[) 570.446.g256

E-mait

B. Test Location lnformation:

Name Bellefontaine Gas producers, LLC

Contact person Mr. Garv Autolitano

Proposed Test Date -April 1S,2009

Proposed Start Tme 09;00am

Testing Firm lnformation;

Name DTE Energy Corporate Services, LLC

Address 6'100 WestWarren, Detroit, Ml 4g210

Contact Person Mr. Mark Gricereit __

Telephone(O) 313.897.1324 (Cell) 313.412.030s

E-mail qrigereitm@dteenergv_coq

Address 2946 US Route 6g North. Bellefontaine. OH 4331 1

Telephone (O) 570.383.7170 (Ceil) _

Facility Premise No.

Emissions Unit pTl NoSCC Number

0546015002

P0103690

20'100802

c' Test Plan and Emissions unit lnformation Table: List the applicable information under each respective column heading

Are anv modifications, or altematives as spelled out within the test methods, being proposed? yes D Uo El lf ,,no,,, then no modifications or altematives, however minor, will be accepted' lf yes' list each test method and section beíng modífied, and attach a detailed modification description and justification:

Sourceistestingtocomplywith(checkalllhatapply):StatePTl8StatePTo8TitleV[NSPSxMAcT[*',

t 

T:î: :::,Ï::Ï:i ',::":_:i:::1" .|. i:rousfrnul 

of the emissions unit siven in irs permft-ro-insrail or oermir-ro-operate? 1 .600 kw electricar oursut

thetest? Yes EI No ! tfno,attachexplanation.

Specifo how the operating rate will be dernonstrated during testing:

Sampling Location(s); lnlet I Ouflet EJ Simuttaneous fl

Fuel Sampling: Coal - proximate n Ultirnate El Ot¡er n

Power outout will be mgnitored throuohout the test

Will Cyclonicflowcheck(s)beconducted? yes El t¡o E

If other, specifl:

Emission rate to be calculated using: F_Factor EJ Uttimate Coal Analysis ü Otner fl I other, speciry:

Has any maintenance or parls replacement been performed on the emissions unit or the control eguipment within the last year? yes ü r.¡o El lf yes, briefly describe:

(Note: some maintenance' such as installing new filter bags in a baghouse, or replacing the activated carbon in an adsorber, may disqualifli the emission. *i*l performance test until a sufficient amount of time has elapsed to ensure a lest which will be representative of normal operations.)

tsm¡sston unit # /

Descriotíon

Control

Eouioment

Monitoring

Equipment

rouuranr(sj to be lested EPA Test Method(s) Number of

Samplinq Points

Total Time for

Sample Run

Number of

P001-P003 Samplino Runs

Landfill GasFíred Engines

None None TSP, SO2, NOx, CO,

Methane, THC

tvt l-c, w¡orJr lvt/ts, lvl1u,

M18, M25A

appropriate

number per

proposed mefhods

60 min

E' Sample Train calibratlon: All affected measuring and rnonitoring equipment should be calibrated within 60 days of the schedufed testing. ohio EpA I Uo7
1a.

Test Plan - Bellefontaine Gas Producgrs- .LLÇ

CAT G3520C lG Enqing,S.tack Ëxhausts

lVames, tÍtles, and telephone numbers for the persannel directly involved with

study are listed in the following table:

fftrs

1b.

Name and Title Company Telephone

Gary Autolitano

Facility Manager

Bellefontaine Gas

Producers, LLC

2946 US Route 68 North

Bellefontaine, OH 43311

(570) 38s-7170

Mr. Thomas Durham

Enviro nmental Engineer

(DTE Energy Resources)

DTE Energy Resources

425 S. Main Street

Suite 201

Ann Arbor, Ml 48104

(734) 302-8234

Mr. Mark Grigereit

Air Quality Specialist

(DTE Environmental)

DTE Energy Corporate

Seruices, LLC

6100 West Warren

Avenue

Room H136

Detroit, Ml 48210

(313) 897-1s24

Type of industrial process or combustíon facility:

The Bellefontaine Gas Producers, LLC facility is located at 2946 US Route 68 North,

Bellefontaíne, Ohio. The facílity is associated with the Cherokee Run Landfill. Bellefontaine

Gas Producers operates three Caterpillar G3520C reciprocating engines with associated

generator sets, The engines are fueled by landfill gas generated by the fandfill and produce

electricity which is sent to the electric grid.

Type and quantity of raw and finished materials used in the process.'

The engines are landfill gas-fired internal combustion reciprocating units, Fuel consumption

varies with fìeld pressure and heat content of the gas. Perlinent engine operating

parameters will be measured throughout each emissions test.

Description of any cyclical or batch operatíons which would tend to produce variable

emissions with time:

The engÍnes operate per contract with electricity providers on an as needed basis with load

varying according to fuel supply, Operation is dependent on landfill gas field pressure.

Three (3) engines (Engines P001-P003) operate at the facility. Testing witl be performed on

one representatíve engine at 90-100% speed and torque to meet Ohio PTI Requirements.

1c.

1d.
7e. Basic operatlng parameters used to regulate fåe process;

Operating parameters used to regulate the engine Íncludes speed (RPM) and torque,

Additional Parameters monitored will include fuel fiow, BTU content, inlet & exhaust

temperature & pressure, torque (bhp) and fuel air ratio. Operating parameters will be

documented during each test.

Rated capacity of the process and process rate duríng the testing:

Testing of the engine_will be completed during maximum (g0-100% speed and torque)

operating conditions. Testing will consist of triplícate 60-minute tests.

Type of control device associafe d with ffie process..

N/A

Operating parameters of the control device:

N/A

Rated capacity and efficiency af the control devÍce:

NiA

Applicable permit number and emission limits for the process to be fesfed;

The Bellefontaine Gas Producers, LLC landfifl gas-fired engine emissions are regulated by State of Ohio Permit to lnstall No. P0103690. The parameters to be tested and their

associated permit limits are listed in the following table:

Table A:

Identify all pollutants to be measured:

See Table A,

Description of the sampling train(s) to be used, includíng schematic diagrams if appropríate:

All emissions testing will be performed according to USEPA Methodology. Sampling train

diagrams are depicted in the aftached figures (see Appendix A figures 2-s).

PartÍculate (PM) sampling will be conducted utilizing Method 5. Testing will consist of triplicate 60-minute test runs.

Suffur Dioxide (SOz), oxides of nitrogen (NO*), and carbon monoxide (CO) testing will be completed according to Methods 6C, 7F*, and 10, respectively. Þrior to telting, a

1f.

2a.

2b.

2c.

3-

4.

5.

Source ïarget Emission Emission Limii

Gram/Ho-hr Lb/mmBTU

2233HP Caterpíllar

G3520C

Particulate 0.062

Sulfur Dioxide (SOr) 05

Oxides of Nitroqen (NO") 0_60

Carbon Monoxide (CO) 3.0

Total Volatíle Organic Compounds

(voc) 1.0
6.

stratifícatíon test will be performed according to Method 78. Testing will be performed in

conjunction with Method 5. Method 1 - Method 4 data required in the permit will be

collected from the Method 5 testing.

Total volatile organic sampling (VOC)will be performed according to lVethod 254. A single

sarnpling point will be selected in the center of the stack according to the method. Testíng

will be performed in conjunction with Method 5. Method 1 - Method 4 data required in the

perm,it wifl be collected from the Method 5 testing. Testing will be performed utilizing

calibration gases of propane bafanced [n nÍtrogen.

Methane sampling will be performed according to Method 18 (Tedlar Bag Collection). The

methane samples will be collected in conjunction with the VOC samples as 60-minute

integrated bag samples. Sampling will be performed in triplicate and sent to an

independent laboratory for analysis.

Detailed sampllng and analysis procedures, includíng the appllcable standard

methods referenced:

Sampling and analysís methods will include the following:

Parameter Method Analytical Method

Exhaust gas

flowrates USEPA Methods 1, 2 Field Data Analysis and Reduction

Molecu[ar

weight USEPA Method 3A Paramagnetic Analyzer

Particulate

Matter USEPA Method 5 Gravimetric Analysis

SOz USEPA Method 6C NDIR Analyzer

NO" USEPA Method 7E Chemiluminescent Analyzer

CO USEPA Method 10 NDIR Analyzer

Methane USEPA Method l8 Gas Chromatography

VOC USEPA Method 254 Flame lonízation Detector
USEPA MEthod 1, ,'SAMPLE AND VELOCITY TRAYERSES FoR slÁiloA/ÁRy souRcEs", and Method z, ,'DETERM\NAwaN oF srÁcK vELoclry AND FLoWRATE (TYPE-9 PITOT TTJBE)" will be used to measure exhaust gas flowrates in combination with sther methods utilízed.

USEPA MCthOd 3A, ''ÐETERMINATION OF OXYGEN AND CARBON DIOXIDE coNcENTRAnOTS /N EMTSSIONS FROM STATTONARy SOURCES f/tVSrR TJMENTAL

ANALYZER PROCEDURE)", will be used to measure exhaust gas moleðular weight.

USEPA MCthOd 5, "DETERMINATION OF PARTICULATE MATTER EMÍSS/O/VS FROM STATIONARÍ SOURCËS", wifl be used to measure total solid particulate exhaust gas

emission rates.

USEPA MCthOd 6C, ''DETERMINATION OF SULFUR DIOXIDE E,IIISSIOA/S FROM STATIONARy SOURCES (!^,SIRLIñ/IENT,4L ANALZYER PROCËDURE)',, wÌil be used to

measure exhaust gas SO2 concentrations.

USEPA MEthOd 7F., ''DETERMINATION OF OX'DES OA/ NÍTROGEN

O9NGENTRArO/VS IN EMISSIO^IS FROM STATTONARr SOURCES (INSTRUMENTAL

ANALZYER PROCEDURE)'1 will be used to measure exhaust gas NO¡ òoncentrations.

USEPA MCthOd 10, ,'DÊTERMINATION OF CARBON MONOXIDE EM'ss,o,Vs FRIM srATIoNARvsouÆcEs lrNsrRUfvlENTAL ANALYZER pRocEDUREl", wiil be used to

rneasure exhaust gas CO concentratíons.

USEPA MEthOd 1B, .,MEASUREMENT OF GASEOUS ORGANIC COMPOUND

EMISSIONS BY GAS CHROMATOGRAPHY", wilf be used to determine the methane

emission concentrations.

USEPA MCthOd 25A, ''DETERMINATION OF TOTAL GASEOUS ORGANIC CONCENTRATION USTNG A FLAME IONIZATTON ANALYZER", will be used to determine the total volatile organic compound concentrations.

7. The number and length of samplÍng runs which utilt constitute a complefe úesf..

All of the emission testing will be conducted simultaneously. Testing wili be comprised of triplÍcate 60-minute sampling runs.

8" Ðímensioned sketches showing all sampling ports in

downstrearn dìsturbances or obstructions ofgas flow:

Sampling will be conducted at the exhaust stack locations

(see Appendix A figure 1).

relation to the upstream and

depicted in the attached figures
Flow (scfm)

10.

11.

12.

13.

14.

9. Estimated flue gas conditions sucfi as temperature, moisture and veloclty:

The estímated flue gas conditions based on similar engines tested:

Load (kW) Temperature

1,500-1,600 900-1,000

Projected process operating eonditíons during whìch the fesfs will be run:

The engine will be tested during normal operations. The testing will take place will the

engines is operating at the maximum load possible (>90% of rated capacity),

ÐescrÍption of any process or çontrol equipment data to he collected durÍng the

fesfing;

Data to be collected during each day of testing will include the following:

-Engine Speed (RPM)

-Load/ Power (kW)

-Gas Fuel Flow (SCFM)

-Fuel BTU Content

-Fuel/ Air Ratio

DescrÍptlon of any manitoring data to be collected duríng ffte fesf period (e.9. -

contÍ n uous emisslo n mon ítori ng data) :

N/A

Chain of Custody procedures;

Standard chain of custody procedures will be followed for all testing,

Field quality assurançe/quality control procedures fe.g. - field blanks, sample

storage and transport methods):

The sampling team wíll prepare and calíbrate field-sampling equipment and perform quality

assurance/quality control (OA/OC) consistent with the employed USEPA methodology. To

ensure accuracy of the 02, CO2, SO2, NO¡ and CO analyzers, a set of three (3) calibration

gases per analyzer will be injected through the reference sampling system to demonstrate

the linearity of the analyzers, The three gases will consist of a known concentration of

calibration gas, balanced in nitrogen. Calibration levels include span-100% of range (high

level), at 40-60% of span (mid), and at <20o/o of span (low). Additionally, the NO¡ analyzer

will be calibrated with a 40-60 pprn NO2 calibration gas to demonstrate converter efficiency

of >90%.

To ensure accuracy of the VOC analyzer, a set of four (4) calibration gases will be injected

through the reference sampling system to demonstrate the linearity of the analyzer,

Ranges are as follows: 80-90%, 45-55o/o,25-350/o of span and zero, The gases will consist
15.

of a known concentration of propane in nitrogen. All gases wlll be documented EpA Protocol Number 1, traceable to National lnstitute of Standards and Technology (NIST)

Reference Materials.

Methods 5 will follow QA/OC standards as described in the methodofogy. The sampfing team will prepare and catibrate fietd-sampling equipment and -þerlorm qualit!

assuranceiquality control (OA/OC) consistent with thõ employed USEPA methodology.

Method 18 will follow QfuaC standards as described in the methodology. Additionally,

samples will be anafyzed within 48 hours of collection to assist in ensuring accuracy.

Laboratory qualíty assurâncelquatity eontrol procedures utílized as paft of the fesfing.'

Calibrations for USEPA Methods 34, 6C, 7E and 10 will follow protocof stated in USEpA

Methods and will utilize appropriate calibratíon gases. Method b gravimetric analysis will be completed by DTE Energy's internal laboratory. Weights wíll bã collected in a climate

controfled weight roorn, on a scale which is certified annually and calibrated daily with 3

genified weights (2.00009, 30.00009, 100.00009). Method 5 samples wiil be *uighuO to

0.00059 constant weight

An lndependent laboratory, contracted to perform Method 18, will be instructed to perform

all analysis and QA/QC procedures according to the appropriate methodology.

Names and titles of personnel who will be pertorming the testing:

The testíng will be performed by DECS's Environmental Stack Test ánd Ambient Monitoring

(STAM) group, with the exception of Method .18 analysis,

16.

Mr. Mark Grigereit, Specialist QSTI DËCS

Mr. Fred Meinecke, Technician DECS

Methods 1B

Project Leader

Lead Technician

Enthalpy Analytical, Inc

22O2 Ellis Road

Durham, NC 27703-5518

Phone

Fax

919.850.4392

919.850.9012

The emission test report will include the items found on Ohio EPA General Testing And Reporting

Requirements form. lncluded in the report will be a site description with the reãson for testing,

source descriptions, a summary of results, our sampling and analytical procedures, and test

results and discussion.
APPENDIX A

FIGURES
DTE Emergy.

Stack Diameter 16" Velocity Measurement Polnls

Distance From

Points lnner WAIì

1 0.70

2 2.U

3 4.74

4 11.26

5 13.66

6 15.30

Figure No. 1

Source Diaqram

Site:

Bellfontaine Gas Produeers, LLC

tack Sampling Group

mentaf Management &
Heated Probe W Pyrex Glass Liner & SS Nozzte

Figure No. 2

USEPA Mêthod 5

msnagement& Resourceg
llTE Energy'

Figure No.3

USEPA Methods 3A/7El10

TECO 42i NOx Analyzer

TECO 48i CO Analyzer

Servomax OzrcA? Analyzer

Flow Controller

Heated Samle Líne

Calibratìon Line

lfontaine Gas Producers, LLC

lefontaine, OH Stack Sampling Group

Environmental Management &
IDTE Energy"

Probe (Center of Stack)

TeflonSampeLne

-'--

Vaccum Pump

Bldg Roof

Figure No. 4

USEPA Method 18

Stainless

/

Flow

Tedlar Bag

!!!!!!=:t=!!=!!::!=!=!=:

Sampling Group

ironmental Management &

Bellfontaine Gas Producers, Ll-C

Bellefontaine, OH

Sampling Date:

April, 2009
DTË Energy"

Figure No.5

USEPA Method 254

Flow Controller

Heated Samle Line

J.U,M. 1O9A

Methane/Non-Methane

Total Hydrocarbon Analyzer

Sampling Date:

April,2009

Site:

Bellfontaine Gas Producers, LLC

Bellefontaine, OH k Sampling Group

Environmental Management &
Energy

APPENDIX B

EQUIPMENT AND ANALYZER CALIBRATION DATA
Environmental Supply

#r

APEX TNSTRUMENTS

EPA Method 5

522 Series Meter Box Calibration

Pre-Test Orifice Method

English Meter Box Units, English K' Factor

FiLename: s:\srAM Group\srAM Group rnfo\cal-ibrations\Meter l\ lo3-r2-og Fulr caribration-xlsl522oRpR5

!dLe: ------

Barometric Pressure: --------> Theoretical Critical Vacuum: --->

3/12/09

29.8L (in. Hs)

14-06 (in- Hcr)

Model #:

Serial #:

!!!!!!!!!

IMPORTÀNT

TMPORT.ANT

!!!!:!!t!

The 

For valid 

criticat 

test 

orifice 

resuLts, 

Coefficient, 

Èhe AcEuar vacuum shoul-d be 1 to 2 in- Hq greater than the Theoretical critical vacuum strom abowe- K', must be ent.ered in Bnglish..itr, (rt)^3*(des R)^0-5l((in-Hg)*(nin)).

__- DRY GAS METER READTNGS -CRITICÀ! ORTFTCE READINGS_

dH Time (in H2o) (nin)

0.58 l-1 .00

L.l-0 10-00

1.80 9 .00

3.30 8.00

5.30 6.00

Volume

rnataa_t

(cu ft)

951.200

955.159

962 -242

969.303

978.010

Vofume

Final

(cu ft)

956-159

962.242

969 -303

978.010

985-089

cM7 3

eMSl65-0

55 .0

65 .0

65.0

6s .0

Volume Inít.iaL Tery)s- Final Temps. TotaL lnLet OuÈl_et Inl_et OutLet (cu ft) (deq F) (des F) (deg F) (deg F) 4.959 63.0 63 .0 66.0 66.0

6 _ 083 66.0 66.0 69.0 58.0

7 -06L 69.0 68 _ 0 73.O 69 .0 8.707 73.0 69.0 7s.o 70-0 8.079 75-0 70-0 77.0 70_o

Orifice K' Orifice

SeriaI# CoefficienE

(number) (see above)

cM48 0 -342 cM55 0.456 cM63 0 _ 58?

0.813

t.072

Actua1 -- tunbient Temperature --

Vacuum Initial Final Average (in Hg) (degr F) (des F) (deg F) 15.s 65.0 6s.0 15.5 65.0 65_0

15.5 65.0 65.0 15.5 6s-0 65.0 l-5.5 55.0 6s.0

RESULTS * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * *

-_- DRY GAS METER --- ORIFICE -- DRY GÀS METER _- ORTFICE

VOLUME VOIT'ME

CORRECTED :ORRECTED

Vn(std) Vm(std)

(cu ft) (liters)

4.919 141.0

6.083 a72 -3

7 -040 I99 _4

8.680 24s -8 8.075 228.7

VOLUME VOIJUME VOI,UME

CORRECTED CORRECTED NOMINÀL Vcr(std) Vcr(std) Vcr (cu ft) (liters) (cu fr) 4.892 l_38.5 4.884 5.930 167 -9 5 .920

6 _87 6 194.7 6.86s 8.464 239 .7 8.450

7.903 223 .8 7 .890

CA]JIBRATION FÀCTOR

Y

Value Variatíon

(nunber) (nunber)

0.982 0.00s

0 -975 -0.003

0 .977 -0.001- 0.97s -0.002

0 .979 0.001

Average Y -------> 0.9"ì8

CA.LIBRÀTION FACTOR

dHG

Value Value Variation (in I{2O) (m H2o) (in H2o) r_.655 42.03 -0 - 043 1.7s6 44.61 0-058 L-727 43.86 0 -029 1.648 41 - 85 -0.0s1 1.705 43.32 0-00?

1.598 43-L3

Note: For calibration Factor Y, the ratio of the reading of Ehe calibration meter to the dry gas meter, acceptable tolerance of individuar, varues from the average is +-0-02.

For orifice calibration Factor dll@, the orífice differential pressure in inches of H2o that equates to o-25 cfm of air at 68 F and 29-92 índnes of/'3la â..êntãLììÁ È^rôr>ñ^- ^r acc,eptab,é tolerance of ì-¡i,-l indiwidual values from the average is +_g-2-

3t12t2009

Dare: 3-12^ol
APEX INSTRUMENTS

EPA Method 5

522 Series Meter Box CaLibration

Pre-Test orifíce Method

English Meter Box Units, Englj.sh K, Factor

Fil-ename: S:\STÄM Group\STAM Group Info\Calibrations\Meter l\t05-11-09 FuLL calíbration.xlsl522ORPR5

Model #:

SeriaL #:

tttttttft

IMPORTANT

IMPORTANT

ttttttttt

EnvirorunenC.al Supply Dâte: ------

Barometric Pressure:

Theoretical Critícal Vacuum: --->

6/rr/09

29 -10 (in. ttg)

13 .73 ( in. Hs)

For valid test results, the Actual Vacum should be 1 to 2 in. Hg greaLer than the Theorecicaf criticaf Vacuw shown above. The Critical Orifice Coefficient, K', musr be entered in Engtish uníts, (ft)^3*(deS R)^0-5/((in-Hg¡*(nin)).

--- DRY GAS METER REAÐINGS -CRITICÀI ORTFICE READTNGSdH Time (ín H2O) (min)

0.56 10.00

1.10 10.00

1.75 5 - 00

3 .30 6.00

5.20 5-00

VoIume

Initial

(cu ft)

128-100

1_32 .628

I38.737

I42 .650

1,49 .L7 5

Volume

Final

(cu fE)

L32.62A

L38 -737

r42 -650

L49 _1,75

155.936

0.456

0 .587

0-813

L.OL2

63 .0

63 .0

63-0

63 .0

63_0

volume IniEial Temps- Final Temps- Total lnlet Outl-et Inlet Outlet (cu ft) (deg F) (deg F) (des F) (desr F) 4-528 65.0 63-0 66.0 63-0

6 - r.09 66.0 63 .0 67 .0 66 _ 0

3.913 67_0 66-0 69-0 66-0

6-525 69.0 66-0 70-0 64-0 6.761 70.0 64-0 71.0 62-0

Orifice K' Orifice

Serial* Coefficient

(nunber) (see above)

cM48 0.342

cM55

cM63

cM73

cM81

Àctua1 -- Am.bj-ent Temperature --

Vacum Initial Final Àverage

(in Hg) (deg F) (deg F) (degr F)

1s.5 63_0 63.0

1s.5 63.0 63.0

r-5-5 53_0 63.0

15.5 63-0 63.0

15-5 63.0 63-0

VOLIIME VOLUME

CORRECTED :ORRECTED

vm(std) vm(std)

(cu ft) (Iiters)

4-440 I25 -7

s - 984 769 .5

3.828 108-4

6_406 181.4

6.675 t-89 _ 0

VOLUME VOLUME VOLUME

CORRECTEÐ CORRECTED NOMINAL Vcr(std) Vcr(std) vcr

(cu ft) (liters) (cu ft)

4 -349 1,23 .2 4.43L

5 - 800 1,64 -3 5 - 909

3.736 105-8 3.806

6 .209 175.8 6.326

6_44I t82_4 6.s63

CA],IBRÀTION FACTOR

Y

Value Variation

(nunber) (nunber)

0 - 980 0.008

0-969 -0-003 0-976 0-004

0 .969 -0 - 003

0.965 -0 _ 00?

Average Y -------> 0.972

CÄ].IBRATION FACTOR

dHe

Value Value Variation (in H2o) (mn H2O) (in H2o)

1.635 41.53 -0 - 082

1.801 45.74 0.084

L.72I 43.72 0-005

1-696 43.0'7 -0-021

L -73A 43 .96 0 - 014

1-71,7 43.61 <------- Average dH@

Note: For calibràÈion FacEor Y, the raLio of the read.ing of the calibration meter Èo the dry gas meter, accepÈable tolerance of individual values from the average is +-0.02.

For Orifice Calibrat.ion Faclor dHG, thg2orífíce differential pressure in inches of H20 that equaÈes Eo 0-25 cfm of air at 58 F and29-92 inchesglf ng, accepffible tolerance of individual values from the average is +-0.2.

srcNED: Ø/t r h.u{ -.^... [o-ti-ay

6t11t2009
9.2.I.L Eefore beginnìng the fiefd test (a set of

three rurrs usually cons[iüutes a f ield test) , operate t]re

metering systenl (r. e- / ptrnrp, wolume meter', and orif ice) altlre 'H.., pressure clifferenLial f:or I0 minutes. Recor:d the

vo.l-rlme collected, the DGM temperature, and the ba.romeLriq

pre.ssì.-rre. CalcuÌate a DGM cal-íbration check value, Y", as

foll-ows :

10 .V

Id

0.0319 Ttì

D

bar l

where:

Y" = DGM cal-ibrat-ion check val-ue, di-merrsionless.

10 = Rr¡.n time, mín.

9.2.L.2 Compare the Y.- val-rre with Ehe dry gas meter

calj-brat j-on factor Y to determine that: 0.97Y < Y" < 1.03Y

ff tl:e Y. valure is not wiLhin Lhis ral:l"ge, t-he vo-Lurne

met,ering system sLiould be irivesl-igated before beginni.ng t-he

test .

Time =

o( Vm{c,") =

u 

ç 

Vmlpost) =

' Têmp1o,"¡ =

Temp1oo.1¡ =

D- lbarAþ\= l, {o18

/= o.,9'3å o 1T (o.r7q):

l-o3(o.q'1Ê)=

c),1."18'l

l,aùI 3

,03 1g T

m Y,=

r 0,1502

T.*,1 8t,,,"",^*
Ënergy"

Nozzle Verification

Date: {r" Z-fSq Verified by: ft'Y1

Where:

1, 2, 3, = Nozzle diameter measured on a different diameter (in)

Tolerance = measure within 0.001 in.

ÀD = Maximum difference in any two measurements (in)

Tolerance = 0.004 in.

D avs = Average of Dr, Dz, Ds.

Nozzle

ldentification

#

D1 (in) Dz (in) Dg (in)

^D 

(in) Davg

5 Tvpe o"/77 O" lzz 0, /7å O. ao I 62 i77
Dimensions

3116" < Dqn,e) <3/8"

Pn=Pe o*/-0.01

1.05 Dt <P(n,s) <1.50 Dt

Z< 0.32 cm (1/8") @ No

S-Type Pitot Tube Verification Checklist

Pass

(Yes/No)

W < 0.08 cm (1132") @ No

Pitot ldentification #: 01

Pitot Tube Correction Factor:

Date Verified:

Verified bv:
Ø-'z)

L'Uat,

-lr" 

I

st

(n'z¿

sq"ìh ¿

-Yl

oÐ

(uzz)

5'qth

o'l

a3

8Eå-s'*rþh

h"ìB "'8.|.8-a 

zqhT"zBþl

o"Ç-oo

stif

uu Çq 

(zzrÐ -Crú¿A6 5'bl, 

S:,l,hl{'ål,t t_ ?û S 

I Bobþ- 

'obh

(z'er-'(t 

'flo"o

w

ll-"ltzv¡ 8=t 

--*'5; tQoZ'çQ 

"-,\wfll*

- Çn 

'.ON

Gsn)

UhLI

b"c>

*çÐ-''f

l;Lt-,-açLh 

-E'hBh

1-çbüz'5bb

C) Q.Q*O aL 

õ

fo'or Fb'b" 

-Ez'o¡

87'øt þzst" 

\e'o-\oo-ç"ç

rcî

sgB

èe

-¡E

L9E,

(rr

i-ltr

\he

o

ã[

f.e"B

Èro

æ

d'ò j-'"f'Ll

\,o

ca$i

8s 

")L.\ S 

ìÉ 

o'Ð

-LLZtC\,

U

-7bb

c>o'o

õ

7Ub

r) aa 

"O

h'o- 

-s 

bg 

'e¡ I - 

'd

-æ

b- I 

tc'

ÇroO-
System Data by Run and Sample

ReportDate 61312009

Source Identification DTE BioGas

Test Persoffiel

UnitName

Run 1

Number 6 3 2OO9 Level H

Date Hour Minute FF 02% Status Mins COz% Status Mins SO2 ppm Statûs Mins NOx ppm Status Mins CO ppm Status Mins 613/2009 B 5 9780 8.038 I I 11.117 1 t 4.t49 1 I 69.015 1 1 588.596 1 1

6/312009 E 6 9780 8.012 1 I 11.140 1 I 4.t39 I I 68.119 1 r 585.358 1 1

6/3/2009 I 7 9780 8.021 1 I 11.128 I I 4.238 I 1 69.433 I I 591,.942 I 1

613/2009 I 8 9780 8.017 I I 11.134 I 1 4.289 1 I 68.289 1 r 585.035 1 I

6/312009 8 9 9780 8.014 I I 11.13s I I 4.4t0 tr 1 69.943 1 l 591.633 I I

613/2009 8 10 9780 8.044 I I LI.I2t I I 4.431 I I 69.952 1 I 586.711 1 I

6/3t2009 8 11 9780 8.015 I 1 11.148 1 I 4.506 I 1 72.263 1 I 586.933 1 I

6/3/2009 8 12 9780 8.026 I 1 11.135 I 1 4.295 I 1 70.198 1 I 584.560 1 I

8 13 9780 8.021 I I 17.134 1 I 4.338 I I 71.863 I I 586.'.139 1 I

6t3t2009 8 14 9780 8.043 I 1 1.118 I I 4.438 I I 7r.t23 I I 586.409 I I

6/3/2009 8 15 9780 8.035 I I II.t22 I 1 4.530 I I 65.127 1 1 s82.299 l 1

61312009 I 16 9780 8.045 I I Il.I24 I 1 4.648 I I 72.882 1 I 58',1.298 r 1

613/2009 8 17 9780 8.026 I I 11.136 I 1 4.643 1 I 61.100 I 1 584.962 1 I

8 18 9780 8,025 I I ll.t42 I I 4.815 i 1 68.886 I I 585.239 l I

6/3/2009 8 19 9780 7.995 I I t.ts''t I 1 4.828 I I 71.424 I 1 587.288 1 1

6/3/2009 I 20 9780 7.998 I l II.ts4 1 I 4.807 I I 12.685 i 1 588.633 r I

B 21 9780 8.036 I I I.L25 1 1 4.890 I I 7t.234 1 I 589.781 1 1

6/312009 8 22 9780 7.99',1 I I 11.160 I 1 4.9s3 I r 68.186 I 1 583.141 1 I

6/3/2009 I 23 9780 8.030 I 1 Il.t43 1 i 5.030 I I 74.056 I I 589.974 I 1

6/3/2009 8 24 9780 8.038 1 I II.r32 1 I 5.12A I 1 65.014 I I 583.436 1 I

6/312009 8 25 9780 8.002 l I 11.170 I r 5374 I 1 73.006 I I s86.326 1 I

8 26 9780 7.9',t8 I I 11.189 1 I 5.180 I 1 69.538 1 I 594.877 I r

61312009 I 27 9780 8.001 r I II.t73 1 I 4.946 1 1 7r.948 1 1 592.102 1 l

613/2009 8 28 9780 7.99r I I 11.178 1 I 4.815 tr 1 6716s 1 I 588.653 1 I

6t3t2009 8 29 9780 8.036 1 I I.132 1 1 4.698 1 r 68.916 1 I s85.813 I I

61312009 8 30 9780 8.004 I 1 11.156 1 1 4.6s5 1 I 69.882 1 1 583.286 1 l

613t2009 8 31 9780 8.025 I 1 11.145 I 1 4.6s9 1 1 69.309 1 I 581,984 1 1

6/3/2009 I 32 9780 8.035 I 1 lt.r42 I 1 4355 I I 67.845 I r 582.505 I 1

61312009 8 33 9180 8.041 1 I 11.t32 I 1 4.763 1 1 64.851 1 1 581.s11 1 I

I 34 9780 7.987 I I 11.180 I 1 4.E90 I 1 7t.269 I I s8L274 1 1

613/2009 8 35 9780 7.992 1 1 LI.T7I 1 1 5.041 1 I 68.963 1 l 588.183 1 1

6/3/2009 8 36 9780 8.002 r I 11.t74 l I 5.259 1 1 71.867 1 I .0s2 1 I

6/3/2009 8 37 9780 8.011 i I Il.t64 I I 5.419 I I 1r.399 1 1 585.140 1 I

6/3/2009 8 38 9780 '1.992 I 1 Ir.r79 I I s.374 1 1 69.511 1 I 588 1 1

Certdas System Developed by Cartwright &Associates Little Rock, AR. Ph (501) 791-3655
System Data by Run and Sample

Report Date 61312009

Source Identification DTE BioGas UnitName

Run 1

J

H

Test

Nurnber 6 3 2009 Level

Date Hour Minute FF 02% Status Mins CO2% Status Mins SO2 pom Stattrs Mins NOx ppm Status Mins COppm Status Mins 61312009 B 39 9780 8.002 I I 11.170 1 I 5.107 1 1 73.097 1 I 590.142 1 I

I 40 8.003 I I 11,159 1 I 4.898 I 1 68.259 1 I 588.475 I 1

ot'tzutJ9 E 4l g7g0 8.017 I I 11.149 1 I 4.766 I 1 73.st4 I I 590.819 I I

6/3/2009 B 42 e780 8.048 I I 11.118 I I 4.189 I I 67.355 I I 588.070 1 1

I 43 9780 8.017 I I 11.139 1 1 4.856 1 I 66.290 1 I 580.268 1 1

6t'3t2UU9 8 44 9780 8.043 I 1 LI,I22 1 1 s.083 1 1 69.037 I 1 5',79.532 1 I

613/2009 8 45 9780 8.016 I I 11,145 1 1 5.140 I I 70.782 1 1 s'71.783 I I

61312009 8 46 9780 8.009 I 1 11.153 I I 5.30'.'t 1 I 67.307 I I 580.675 I I

bt'stzutJ9 8 47 g7g0 8.019 1 1 It.L49 1 I s.302 I 1 72.265 I I 583,613 I 1

61312009 8 48 9780 8.055 1 I 11,113 I I 5.4s3 I 1 66.694 1 I 57'Ì.54t I I

6t3t2009 I 49 9780 8.0tr3 I I 11.1s4 1 I s.462 I 1 70.470 1 I 577.636 1 I

61312009 8 s0 9780 8.02^r I 1 11.138 I 1 s.37L 1 I 70.714 I I 579.371 1 I

6/3/20Ue I 5t 9780 8.038 I 1 11.134 I I 5.2s9 1 1 65.219 1 1 s'76.240 1 I

6/3/2009 I 52 9780 8.013 I I 11.156 1 I 5.282 1 I 68.077 1 I s76.697 1 I

6/3/2009 8 53 9780 7.980 I I 11.188 I 1 5.369 I I 68.261 1 I 583,051 1 1

61312009 I 54 9780 7.994 I I rl.I74 l I s.442 1 I 72.092 1 I 581.1s9 1 l

6/3/2009 8 55 9780 7.985 t I 11.181 1 I s.309 I I '73.466 I I 578.248 1 1

8 56 9?80 7.99r I I n,rÌs I I s.t7r I I 69.010 1 I s84.487 I 1

6tJtzUU9 U 57 9780 7.992 1 I Lt.I76 I I 5.255 I I 67.14\ 1 1 582.529 1 I

61312009 8 58 9780 8.011 I I 11.159 I 1 s.171 1 I 69.668 1 I 582.23'.7 I I

6/3/2009 8 59 9780 8.009 I r 11.1s9 I 1 s.118 I I 70.409 I I s83.114 1 I

613/2009 9 0 9780 8.004 I I 11.1s9 I I 5.102 I I 70.056 1 I 583.385 1 I

613/2009 9 I 9780 8.021 I I 11.148 I 1 s.080 I I 68.178 1 I s83.246 1 1

61312009 9 2 97BO ''t.99I I 1 LT,T72 1 I 5.138 1 I 69.979 1 I s85.081 I r

61312009 9 3 9780 8.001 I 1 Ir.162 1 I s.I34 1 I 67.86t I I s84.962 1 I

613t2009 9 4 9780 8.012 I I 11.155 1 l 5.202 1 I 72.730 1 I 582.294 1 1

8.0i5 60 11.1s0 60 4.932 60 69.s90 60 584.692 60

Certdas System Developed by Cartí,tight &Associqtes Little Rock, AR, Ph (50j) 79I-3655
Post-test System Calibration

Source Identification DTE BioGas

Test Personnel mqlfu1fu

Number 6 J 2009

UnitName Eng_3

RunNumber I

End Time & Date 6/3/2009 9: M.00

Analyzer

Span

Value

System

Reference

Value

System

Calibration

Resnonse

System

Error

f%o ofsuan)

System

Error Limit

l% ofsoanl

System

Calibration

Status

Zero Gas O2Yo 18.370 0.000 0.000 0.000 5.000 PASS

Mid Gas 02% 18.370 10.050 9.924 0.686 5.000 PASS

Zero Gas CO2% 18.280 0.000 0.042 0.230 5.000 PASS

MidGas COz% 18.280 10.230 9-997 1.275 5.000 PASS

Zero Gas SO2 19.500 0.000 0.659 3.379 5.000 PASS

Uoscale Mid Gas SO2 19.500 9.220 8.410 4.754 s.000 PASS

Zero GasNOx 490.100 0.000 0.854 0.174 5.000 PASS

U rscale Mid Gas NOx ppm 490.100 179.900 174.682 1.065 5.000 PASS

ZeroGasCO 995.200 0.000 0.976 0.098 5.000 PASS

Mid Gas CO 99s.200 484.300 470.458 1.391 5.000 PASS

Certdøs Systent Developed by Cartwright &. Associates Little Roch AR. Ph (501) 791-3655
System Data by Run and Sanrple

ReportDate 61312009

Source Identification DTE BioGas

Test Personnel

Number 6 3 2009

UnitName

Run 2

_3

ineLwel H

Date Hour Minute FF O2%o Stattrs Mins COz% Status Mins SO2 oom Status Mins NOx opm Státus Mins CO ppm Status Mins 61312009 9 s2 9780 8.003 I I 11.181 I I 5.381 I 1 69.s40 1 I 581.373 1 1

6/312009 9 53 9780 8.010 I I tt.I74 I 1 s,254 tL I 70.374 1 1 583.473 1 r

6t3t2t¿09 9 54 g7g0 8.021 I I 11,163 I 1 s.244 I 1 70.748 I I 578.309 I I

6t3t2tJï9 9 55 9780 8.015 I I 11.160 I I 5,370 I I 69.070 1 I 581.969 1 1

613/2009 9 s6 9780 8.028 I 1 11,1s0 I i s.399 I 1 7r.316 1 1 585.388 1 I

btJtzuuv 9 57 9780 8.016 I 1 II.t57 1 1 s.372 I I 68.579 I I 578,159 1 1

6/312009 9 s8 9780 8.042 I ll.t4r r 1 5.265 1 I 7t.329 1 I s82.296 1 1

9 59 9780 8.005 I I Il,t77 l I 5.469 I I 7I.487 1 1 582.494 1 1

61312009 l0 0 9780 8.0i4 I I ll.t76 I I 5.486 I 1 68.871 1 I 584.1s9 1 I

6t3t20tJ9 l0 I g7g0 8.009 I r 11.188 I I 5.41',1 I 1 71..460 1 I 583,390 1 1

6/312009 10 2 9780 8.020 I I 11.163 1 1 5.399 I r 68.035 1 1 .s78 1 I

t0 3 9780 8.034 I t 11.150 I 1 5.382 I I 66,156 I I .130 1 I

613t2009 10 4 97S0 8.044 I 1 11.133 I 5.300 I r 69.299 I 1 573.s38 1 I

6t3t2009 l0 5 9780 8.024 I I 11.145 I I s.181 I I 68.527 I I 573,42s I l

6t3/2009 10 6 9780 8.035 I I 11.139 I 1 4.9s2 I r 69.967 I I 574.680 1 1

6t3t2009 l0 7 9780 8.019 I 1 11.148 I I s.065 I I 71.320 1 I s74.18s 1 I

613/2009 10 I 9780 8.036 I 1 Il.r32 1 1 5.121 1 1 70.254 1 1 5B1.192 1 I

613/2009 10 9 9780 8.047 I 1 11'127 I I 5.116 I l 74.886 1 1 579.t8'.7 I I

613/2009 t0 l0 9780 8.060 I I .r20 1 1 5.088 1 I 66.747 1 I 574.0T1 1 1

10 ü 9780 8.037 1 I Il.r43 I 1 5.085 I r 70.53I I I s72392 1 1

6/312009 10 t2 9780 8.026 I I 11.1s3 I 1 5.t44 I r 65.518 I 1 .319 1 1

6/3/2009 10 13 9780 8.029 1 I Il.ts7 1 1 5.199 I l 68,316 1 I 574.695 1 r

6/3/2009 10 14 9780 8.029 I l ,156 I I 5.323 I I 68.506 I 1 s71ß38 1 I

613/2009 10 15 9780 7.998 I I II.t'72 r r 5.473 1 1 69.304 l 1 5',75.905 1 I

6/312009 10 16 9780 7.98r I I 11.196 I i 5.440 1 1 75.651 I I 584.901 1 I

6/3/2009 10 11 9780 8.023 I l i1.160 1 I 5.389 I I 73.340 1 1 586.875 I 1

6/312009 10 18 8.029 I 1 ll.t4e I 1 s.369 I r 68.611 I 1 578.016 I 1

l0 19 9780 8.011 I l 11.165 I I 5.415 1 I 67.680 I I 576.591 1 I

61312009 l0 20 9780 8.005 I I 1.t63 l I 5.489 I l 69.450 I I 578.s44 1 l

6/3t2009 10 21 9780 8.009 I l 11,157 1 I 5.484 1 I 69.537 I I 585.282 I I

6t3t2009 10 22 9780 8.032 1 l .r32 1 1 s.363 1 r 66.964 I 1 s7s.276 I 1

6/3/2009 10 23 9780 8.010 I I 11.145 1 I 5.4','Ì9 1 I 73."741 1 1 57'7.047 I 1

6/3/2009 10 24 9780 8.016 I I tt.t42 I I 5.483 1 l 69.926 I I 584.524 1 l

613/2009 10 2s 9780 8.028 I I 11.136 I r 5.546 I I 72.227 I 1 s77.83r 1 1

Certdas SystemDeveloped by Cartwright &Associates Little Rocþ, AR. Ph (S0I) 79j-365s
System Data by Run and Sample

ReportDate 6/312009

Source Identífication DTE BioGas UnitName

Run 2

J

H

Test Personnel

63 2009 ine Level

Date llour Mintrte FF 02% Staürs Mns CO2% Status Mins SO2 ppm Status Mins NOxppm Status Mins CO ppm Status Mins otst¿uuv ru ¿6 y7ü0 8.008 I I II.I57 I I 5.624 I I 68.679 1 I 580.317 I 1

6t3t2UV9 l0 21 g7E0 8.021 1 I 11.154 I 1 s.734 I I 69.15't I I 583.s48 1 I

6/3/2009 10 28 9780 8.010 1 1 11.159 1 I s,667 1 I 70.082 I I 1.106 I I

6/3/2009 10 29 9780 8.032 I 1 11.138 I I s.591 I I 72.214 1 l s82.220 1 1

6t'3t2uue l0 30 9780 8.023 I 1 11..143 I 1 5.575 1 I 67.373 1 1 577.40s 1 I

6t 3tzu1J9 l0 31 9780 8.019 1 l 11.156 I I s,526 1 I 72.688 1 I 578.510 1 I

613/2009 10 32 9780 8.007 1 11.165 r I 5.566 1 I 70.229 1 I s80.313 I 1

6t'JI2UtJ9 l0 33 9790 8.012 I I 11.168 1 I 5.512 1 I 69.128 1 1 578.311 1 I

6t3t2009 10 34 9780 8.020 I I tI,lse I 1 5.469 I I 69.006 I I 580.63r I I

6t3t200e l0 3J 9780 8.018 I 1 11.159 I 1 5.449 I I 66.090 I 1 576.752 1 1

10 36 9780 8.018 I 1 11.762 I I 5.490 I I 68.987 1 1 577.044 1 I

6t3/2009 10 31 9780 8.042 1 I Il.t32 1 1 5,492 1 I 65.413 1 1 573.t71 I 1

6t3t2009 l0 3E 9780 8.024 1 I It.tsz 1 1 5.500 I I 70.425 1 1 574.453 1 I

613/2009 10 39 9780 8.001 I 1 11.171 I 1 5.550 I I 69.249 1 1 575.432 1 I

t7 r0 40 9780 7.968 I I 11.193 I 1 5.695 I I 70.239 I 1 581.605 1 I

6/3/2009 10 4t 9780 1.999 1 1 ll.I73 I I 5.628 1 1 72.429 I 1 584.296 1 1

6t3t200e l0 41 9780 8.038 1 r 11.138 I 1 s.608 I 1 67,550 I 1 577.686 I I

6t3t20ue l0 43 9780 8.001 1 1 11.180 1 I 5.608 1 1 70.100 1 I 5'.73.059 I I

6/3t2009 10 44 9780 8.024 I I 11.159 1 I s.s92 I r 69.094 1 1 s7'l.594 1 I

6t3t2tJv9 10 45 9780 8.003 I I II.L75 1 1 5.593 1 I 67.626 1 I 579.510 1 I

10 46 9780 8.021 I I 11.148 I I 5.638 I I 70.273 I I 577.469 I I

6/312009 10 4'',1 9780 8.004 1 I lI.t61 1 I 5.66E I I 69.290 I I 575.778 1 r

6/3/2009 l0 48 9780 7.983 l 1 tt,t94 I I s321 1 I 7I.45s I I 582.296 I I

6/3/2009 10 49 9780 '7.987 1 I 11.191 I I s.724 1 1 72.546 1 I 582.998 I I

6/3/2009 10 50 9780 8.040 1 l t1.132 I 1 5.728 1 1 67.ß95 1 1 579.474 1 I

613/2009 10 st 9780 8.007 1 I 11.1s5 1 I 5.701 1 1 67.800 I 1 576.586 1 I

8.018 60 11.157 60 5.443 60 69.705 60 578.976 60

Certdas System Developed by Cartwright & Associates Little Rock, AR. Ph (S0l) 79l-3655
Post-test System Calibration

Source Identification DTE BioGas

TestPersonnel mgfu/fb

ReoortNumber 6 3 2009

UnitName Eng_3

RunNumber 2

EndTime &Date 6/3/2009 11:10.00

Analyzer

Span

Value

System

Reference

Value

System

Calibration

ResDonse

System

Error

(% ofspan)

System

ErorLimit

lolo of soan)

System

Calibration

Status

Zero Gas O2o/o 18.370 0.000 0.006 0.033 5.000 PASS

Upscale Mid Gas 02% r.8.370 10.050 9.918 0.719 s.000 PASS

ZeroGasCO2% 18.280 0.000 0.079 0.432 5.000 PASS

Upscale Mid Gas CO2o/o 18.280 10.230 9.948 t.543 5.000 PASS

Zero Gas SO2 19.500 0.000 0.671 3.441 5.000 PASS

le Mid Gas SO2 19.500 9.220 8.593 3.2t5 5.000 PASS

Zero Gas NOx 490.100 0.000 0.000 0.000 5.000 PASS

rscale Mid Gas NOx pom 490.100 179.900 175.I70 0.96s 5.000 PASS

Zero Gas CO 995.200 0.000 1.220 0.123 5.000 PASS

Mid Gas CO 995.200 484.300 468.s05 1.587 5.000 PASS

Certdas Syslem Developed by Cartwright & Associøtes Little Rock, AR. Ph (501) 791-3655
System Data by Run and Sample

ReportDate 61312009

Source Identification Unit Name

Test Personnel Run 3

Number 6 3 2009

J

Level H

Date Hour Minute FF 02% Status Mins COz% Status Mins SO2 ppm Status Mns NOxupm Status Mins CO ppm Status Mins

ot Jt¿wy r r J¿ g'löu 8.095 I 1 11,121 1 1 5.383 1 r 68.373 1 I 579.600 1 I

613/2009 11 33 9780 8.078 1 1 11,097 I 1 5.779 1 I 61.996 1 I 570.585 I I

o[ilTuve ll 34 9780 8.089 1 1 1L079 I 1 5.963 I I 69.1s9 1 1 572.299 1 I

6tJt¿uu9 lt 35 9780 8.068 I 1 11,098 I 1 6.2s3 I I 6s.529 1 1 568,693 1 I

u3t2rJ09 11 36 9780 8.042 I 1 II,r27 I 1 6.094 I I 61.263 1 I 72.045 1 I

6t3tz00e lt 37 9780 8.036 1 I IL.t44 1 I 5.976 I I 72.124 1 1 575.616 1 1

6t3tzuu9 lt 3E 9790 8.055 1 I 11,138 1 I 5.781 1 1 67.t36 1 I 577.6rt 1 I

613/2009 11 39 9780 8.048 1 I lLt43 I I s.589 1 I 70.941 1 1 575.003 1 I

11 40 9780 8.030 tr I Lr46 l 1 5.611 I I 68.684 1 I 575.282 I I

61312009 11 41 9780 8.028 I I 11,1s6 I 1 5.651 1 1 69.701 1 r 74.409 1 1

11 42 9780 8.051 I I 11,13s I 1 5325 I r 69.L94 1 I 576.780 1 1

6tJt¿uu9 ll 43 9780 8.027 I I 11,146 I I s.655 1 I 68.798 1 r 76411 11 44 9780 8.041 I I 11,140 I I 5.634 I I 68.908 1 I 575.511 1 I

6t3t2009 11 45 9780 8.044 I I 11.14s 1 1 5.681 1 I 70.284 I I 5x2.Ir4 l 1

61312009 11 46 9780 8.059 I I tt,I43 1 I 5.6st 1 1 66.980 1 1 574.183 I I

6t3tztJ09 tl 47 g7E0 8.058 I I 11.14s 1 1 s308 1 1 67.792 1 1 570.888 1 1

61312009 11 48 9780 8.073 1 I tLI2s I 1 5.s16 1 I 65.322 1 I 572.460 1 I

613/2009 11 49 9780 8.059 1 I tLr42 1 I 5.s79 1 1 67.050 1 1 566.061 1 I

613/2009 11 50 9780 8.033 I I 11.163 I 1 5.788 I I 73.8',73 1 1 577.832 1 1

6t3tztJve tl 51 9780 8.048 I 1 11,138 I 1 5.7e0 1 I 72.182 1 1 581.344 1 I

61312009 11 52 9780 8.039 1 I ILt47 I I 5.858 1 I 7I.034 1 I 579,848 1 I

6t3t2009 11 53 9780 8.056 I I 11.14s 1 I 5.734 1 1 69.186 1 I 577.835 I 1

6/3/2009 11 54 9780 8.037 I r lLr67 1 I 5.681 1 I 66.696 1 r 575.146 1 I

613/2009 ll 55 9780 8.072 I 11.140 1 1 5.748 1 r 68.108 1 I 574.913 1 I

61312009 11 56 9780 8.04s I I 11.157 1 I 5.803 1 r 68.691 1 1 571.627 1 I

613.12009 11 s7 9780 8.081 1 I IL.r32 I 1 5.737 I I 70.674 1 1 575.t12 1 l

61312009 tl 58 9780 8.099 I I 11,108 1 1 5.667 1 I 68.183 1 I 567j97 I I

6/3/2009 11 59 9780 8.079 I 11.120 I 1 5.77I I l 70.748 1 1 566.803 1 1

613/2009 12 0 97E0 8.040 I I llt62 t 1 5.787 1 I 66.23L 1 1 573.261 1 I

6/312009 t2 I 97E0 8.041 l 1 tLr66 l 1 5.719 I I 74.232 1 I 57'1.2L6 1 1

6/312009 t2 2 9780 8.043 I I 11.153 1 1 s.680 I 1 68.169 1 r 573.754 I I

6/312009 t2 3 9780 8.057 I I 11,13s 1 1 5.682 I I 67.833 1 1 s7l.r62 1 I

6/312009 L2 4 9780 7.975 1 r 11.200 1 1 5.736 1 I 69.626 1 I 577.425 1 1

6/312009 t2 5 9780 8.007 I 1 i 1.171 I I 5.747 1 I 1l.o3s 1 1 s82.674 1 1

Certdas SystemDevelaped by Cartwright & Associates Little Rock, AR. ph (S0l) 79l-3655
System Data by Run and Sample

Report Date 6/312009

Source ldentific¿tion DTE BioGas UnitName J

H

Test Fersonnel

Nu¡nber 6 3 2009

Run 3

Level

Date ,IÌour Minute FF 02% Status Mins COz% Stafts Mins SO2 ppm Status Mins NOxppm Status Mins CO pþm Status Mins atstzuuy tz ó g7E0 8.028 I I 11.15s I 1 5.7t8 1 1 1t.879 1 r 515 691 ',r 

1

9780 8.046 I I 11,140 1 I 5.596 I I 67.s06 1 1 576.487 1 I otrt4vuy L¿ ü 9'lðu 8.082 I 1 11.113 1 I 5.612 I I 68.038 I t 511 017 1 1

otst4uvy u I 9780 8.057 1 I Il,t32 1 1 5.663 1 I 69.805 1 I 56q 65q 1

6t5t¿utJ9 LZ t0 8.046 1 I ll.t44 1 I 5.s90 I I 68.624 1 I 569 656 1

öt Jt luvy L'¿ I I g7E0 8.000 I I 11,182 1 1 5.670 I I 74.316 I I 514ji4 1

ötJt¿uvy Iz t2 g7ßo 8.035 I 1 Il,t52 I I 5.749 I I 70jt2 I I 5Rû 11' 1

6tstz0ue 12 13 9780 8.037 1 r tLr42 1 I 5.809 1 I 67.162 1 I 510141 1

öt3t¿uu9 l2 14 9780 8.053 1 i 11,128 I I 5.783 1 I 67.142 1 I 567Rrl 1

t2 I 97E0 8.051 1 r ll,t32 I I s360 I 1 66.922 1 I 56\116 1

6t3t¿uue Iz 16 g7g0 8.043 1 I 11.13s I I 5.824 I 1 66.759 1 I 11ã11¿. 1

bt3tztJïg 12 I7 9780 8.0t0 1 I 11,112 1 I 5.716 I 1 7t.6tt 1 I 5',72.824 I 1 otst¿vuy t¿ lü 8.065 I 1 11.114 I I 5.705 I 1 65.225 1 I 564. 1 1

ötst¿uu9 I2 l9 97AO 8.067 I I 11.119 l I 5.832 I I 66.669 1 1 565.640 1 1

9780 8.027 1 1 11,155 I t 6.013 I 1 67.018 1 I 466 9t) 1 r

6t3t2009 t2 2L 9780 8.022 I 1 11,160 1 1 s.e3l I 1 67.366 1 I 514891 1

bt3tzuue t2 22 g7g0 8.031 1 I 11,156 I I 5.859 I I 68.351 1 1 57'.7.499 1 I

otJlzuue L2 23 g7g0 8,02e 1 I 11,1s9 1 I 5.e24 I 1 68.901 1 I 575.676 1 1 þt't¿uu9 l2 z4 gTEo 8.045 1 I 11,148 I I s.92',r I I 66.920 1 I 57I.684 1 I

otst¿uuy t'¿ 25 9780 8.019 1 I 11'162 1 1 5.969 I I 6'.7.671 1 I 570.189 I 1

otJr¿uue L2 26 g7g0 8.040 1 1 11,143 I t 5.636 1 I 69.406 1 I 574.sI2 I 1

6t3t'¿uu9 tz 27 g7g0 8.059 1 I Il,t25 I I 5.604 1 1 64.259 1 I 569.B60 1 I

otst¿uu9 L2 '28 9780 8.027 I 1 11.155 I I 6.009 1 1 71.328 1 I 572.t92 1 I

6t3/2009 t2 29 9780 8.053 1 1 11,130 I 1 5.99L I 1 6s.21r 1 I 574.915 I I

otstzuuv L2 30 9780 8.032 tr 1 11.154 I I 5.995 1 I 70.204 1 I 566.530 1 1

6t3t20u9 L2 31 9780 8.022 1 I 11,164 1 I 5.854 1 1 71.650 1 I s73129 1 1

8.047 60 11.141 60 5.765 60 68j07 60 573.t32 60

certdas systemDeveloped by cartwright &Associates LittleRock, AR. ph (501) 7gI-36s5
Post-test System Calibration

Sowce Identification DTE BioGas

Test Personnel

UnitName

Run

6 3 2009 End Time &Date 6/3/2009 12:59.00

Zero Gas O2o/o

le Mid Gas O2o/o

ZeroGasCO2%

le Mid GasCO2o/o

Zero GasSO2

Mid Gas SO2

Zero Gas NOx

Mid Gas NOx

ZeroGasCO

MidGas CO

Analyzer

Span

Value

System

Reference

Value

System

Calibration

Status

10.015

Certdas Syslem Developed by Cartwright & Associates Little Roch AR Ph (501) 791-3655
DIE Energy'

APPENDIX F

OPERATIONAL DATA
Bellefontaine Gas Producers LLC

GC 3520C IC ENGINE

Bellefontaine OHIO

June 3, 2009

Run 1

Run Time: 0804-0904

Description

vatue 1 vatue z vatue J

Unit 0804 0833 0902 AVc

Engine Speed

Generator Total Real Power

lntake Manifold Air Flow

Gas Fuel Flow

Generator Total kW hours

Gas Fuel Correction Factor

RPM 1 199.00 1201 .00 1 199.00 1199.67

kw 1624.97 1521.95 1614.95 1587.29 PSI 47 .2Q 47.20 47.30 47.23

scFM 561.00 570.00 564.00 565.00

kW hours 3370032.00 3370783 3371551 3370788.67

% 99.00 99.00 99.00 99.00
Bellefontaine Gas Producers LLC

GC 3520C IC ENGINE

Bellefontaine OHIO

June 3, 2009

Run 2

Run Time: 0952-1052

Description Unit

Value I

1001 1036 1102 AVG

Engine Speed

Generator Total Real power

lntake Manifold Air Flow

Gas Fuel Flow

Generator Total kW hours

Gas Fuel Correction Factor

RPM

KW

PSI

SCFM

kW hours

o//o

1200.00

1577.95

47.00

563.00

Unavailable

99.00

1201.00

1617.99

47.00

568.00

Unavailable

99.00

1199.00

1599.99

47.10

568.00

3374713

99.00

1200.00

1598.64

47.03

566.33

3374713

99.00
Bellefontaine Gas Producers LLC

GC 3520C IC ENGINE

Bellefontaine OHIO

June 3, 2009

Run 3

Run Time: 1132-1232

Description Unit

value'l

1135

value 2

1202

value 3

1234 AVG

Engine Speed

Generator Total Real Power

lntake Manifold Air Flow

Gas Fuel Flow

Generator Total kW hours

Gas Fuel Correction Factor

RPM

KW

PSI

SCFM

kW hours

%

1203.00

1614.95

46.70

559.00

3375611.00

99.00

1201.00

1615.96

47.13

564.67

3376361.3

99.00

1 199.00

1645.96

46.70

562.00

3376307

99.00

1201.00

1586.97

48.00

573.00

3377166

99.00
DTE Energy" K

APPENDIX G

ANALYTICAL DATA
DTE Energgr

Limit of Detection: 0.5 mg

Analytical Method (USEPA): 5

Analytical Laboratory Report

PM Testing

DTE Energy Corp.

Bellefontaine Gas Producers LLC

Bellefontaine, OH

Sampling Date: June 03, 2009

(1) correction equation = sample net wt. gain/blank net wt. gain) x (sample vol./blank vol.)

Source

ID

Test # Beaker

Number

Beaker

initial wt.

(o)

Beaker

Final wt.

(q)

Beaker

Volume

(mL)

Beaker

net wt. gain

(q)

Beaker

net wt. gain

corrected(1) (<

Beakers-250m1

Unit3-1

Unit3-2

Un¡t3-3

1

2

3

Btk

30

31

32

33

104.3028

105.1061

102.7229

103.0700

104.3059

105.1076

102.7235

103.0701

50

50

50

50

0.0031

0.0015

0.0006

0.0001

0.0030

0.0014

0.0005

0.0000

Source

ID

Test # Filter

Number

Filter

initial wt.

(q)

Filter

Final wt.

(q)

Filter

net wt. gain

(q)

4" Filters

Unit3-1

Unit3-2

Unit3-3

1

2

3

Btk

73

74

75

76

0.6032

0.5990

0.6002

0.5966

0.6048

0.6005

0.6017

0.5966

0.0016

0.001s

0.0015

0.0000

Total

net wt. gain

Gorrected

0.0046

0.0029

0.0020
ÐTE Earergy"

Facility:

Sounce:

SanrplínE Date:

Source

ID

Beakers

Limit of Detection: 0.5 mg

Analyst(s):

Date:

P\

Detroit Edison Company

G ravametric Analytical Laboratory Report

ÊþT6v SeA.'. t. ' ß* .

44J t.r- 1

Beaker

Finalwt.-2

0f. ¡o6i iô6. tat2

a2,72 95

(1) correction equation = sample net wt. gain/blank net wt. gain) x (sample vol./blank vol.)

- b:i:.r tt
Frida;', jr-rne 12, ZOO9

8:33 AM

Clicnt Samplc lD: Enginc lnlct #l

L¿b ID#: 0906123414

Rpt Limtt

1/,1

Amount

(%t

øf{-r-cs LrD.

L tlt(jr,, tvt y 5r'¡,'¡C Js Si/ril(', /-¡i.fl

ComÞound

File Name:

D¡1. FåctoÊ

9060505

1.00

Date of Collection: 6/3J09 J2;l 5:00 PM

Oxygen

Nitrogen

Carbon Monoxide

Mêthane

Carbon Dioxide

Ethâne

Ethene

Acetylene

Propane

lsobutane

Butane

Neopehtânê

ìsopentane

Pentane

c6+

Hydrogen

Totâl BTU/Cu-F- =51û

TotêlSp. Gravity - 0,95

Contá¡nèl Type: I Lite¡ Tedlar Bag

0.10

0.10

0.010

0.0001 0

0.010

0.0010

0.0010

0.0010

0.0010

0.00r0

0-0010

0-0010

0.0010

0-0010

0.010

0.010

't_3

10

Not Detecled

50

37

Not Detecled

Not Detected

Not Delected

0.0027

Not Detecfëd

Nol, Detecled

Nót Detêcled

It'lot Detacled

Not Detected

0.013

0.23

Pâge 6of12

Unfiled Notes Pase I
DTE Energy Corporate

Services, LLC

6100 W. Warren

Detroit, MI 48210

Bellefontaine

Analytical Report

(060e -2t)

EPA Method 18 (Bøgs)

Methane

Enthalpy Analytical, lnc.

Phone: (919)850 -4392 I Fax: (919) 850 -9012 / www.enthatpy.com

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

o Have been checked for completeness

o Are acc¡trate, error-free, and legible

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

problems are summarized tnthe appropriate nanative(s)

. This analytical report was prepared in Portable Document Format (.PDF) and contains 75 pages.

Q.A. Review Performed byl Mchael Steven Schapira

EA#0609-21 Page2of75

'û81

Ll''J
Summary of Results
CompanylDTE Energy Corp Services

Analystll(AM

Parametersl EPA Method 18

# Samplesl3 Bags

Client #l Bellefontaine

Job #10609-21

PO #lVerbal

Report Datel6/9/2009

nd Sample lD / usted Concentration

Run 2

Methane 1,723

Run I

1,730

Run 3

1,690

EA# mÐ?|nrBCry'.4ror zs 6112t2009
Results
CompanylDTE Energy Corp Services

AnalystlKAM

,arametersl EPA Method'l I

# Sampbsl3 Bags & '1 S/R bag

Client #l Bellefontaine

Job #10609-21

PO #lVerbal

Report Datel6/9/2009

MDL 0.500 (ppm)

LoQ 3.00 (ppm)

Compound Methane

Lower Curue Limit 3.00 (ppm)

Upper Curve Limit 80,600 (ppm)

Samp e

ID

Lab lD

#1

Lab lD

#2

Lab lD

fJ

Ret

Time

(min)

Ret

Time

(min)

Ret

Time

(min)

%Dift

Ret

Conc

#1

(ppm)

Conc

#2

(ppm)

Conc

#3

(ppm)

o/o Dill

Conc

Avg

Conc

(ppm)

DF

Rec

Eff

(!")

Adj

Conc

(ppm)

Qua

Run 1 02580301.D 025B0302.D 02580303.D 0509-78R.M 160 160 1.60 0.1 1.752 1 744 1.736 o4 1 744 1 101 1 730

02680402.D

02780502.D

EA# 0m94j1''.,8ßg_ç"p ot zs 611212009
v2.02 Validated by MSS 3f 6/09

Whatwas the conc ofthe

bag before spik¡ng?

U' (before

What was added fo the bag?

Volume Added

Volume Added

Volume Added

Tolâl Vol (mL) vaporized

Total Vol (mL) added as ges

Othervolume (mL) Added

Volume (mL) used in anêlysis

Whaf volume was ¡n the

bag alter analysís?

Or¡ginal volume in the bag (mL)

Total volume added (mL)

Dilulion Factor caused by add¡tion

Dilulion Adjusled Base Conc (ppm) "U"

Theorelical Spike Conc (ppm) 'S"

Energy

Spike & Recovery

Unspiked Sample lDlRun 1

T = after sp¡ke concentrêt¡on

%Recovery=(T-U)/Sx100

U = before spike conæntration S = theoret¡cal sp¡ke concentration

Whãt was the conc of the

bag after spik¡ng?

Final Concentration (ppm)

RECOVERY

T

C ¡ent

Job

PO

Report

1

6/3/09 8:04 A[/|

614109 12:46 PM

614109 2:20 PM

Delta 28142i00

Hours

32:46:00

Analyzed

Spiked

Spike Analyzed

Della

189

6/5/09 'fl:06 PÀ,

than or¡oinel hold

6/t22009 5:58 PM

EA#0609-21 PageT of75

0609-2t-h18bag-res % Recovery
NarratÍve Summary
Comnanv DTE Enerey Corp. Services

Analvst KAM

Parameters EPAMethod 18

# Samnles 3 Baes

Enthalpy Analytical Narrative Summary

Client # Bellefontaine

Job # 0609-21

PO# Verbal

Report Date June 9. 2009

Erin ortiz of Enthalpy Analytical, Inc. received the samples on 6/4/09 at

ambient temperature after being relinquished by DTE Energy Corporate

services, LLC. The samples were received in good condition. prior to

and during ahalysis, the samples were kept under lock with access only

to authorized personnel by Enthalpy Analytical, Inc.

The samples were analyzed for methane using the analyticalprocedures

in EPA Method 18, Measurement of Gaseous Organic Compound

Emissions by Gas Chromatography (40 CFRPart 60, Appendix A).

The standards and samples were analyzed following the procedures

specified in section 8.2.I,Integrated Bag Sampling and Analysis.

All samples and standards were introduced directly to the column using

an automated 6-port valco gas sampling valve equipped with a stainless

steel loop. Methane was referenced to certified gas phase standards.

The Agilent Technologies Model 6890, Gas Chromatograph ("Gummo"

sli{ us00028451) was equipped with a Flame Ionization Detector and a

Restek Rtx-l, 30 m x 0.32mm (Sn\f 666512) capillary column.

The calibration curve is located in the back of this report and referenced

in the Analysis Method column on the Detailed Results page.

For each calibration curve used, the first page of the curve contains all

method specific parameters (i.e., curve type, origin, weigh! etc.) used to

quantify the samples. The calibration curve section also includes a table with the Retention Time (RetTime), Level (Lvl), Amount

(corresponding units), Area, Response Factor (Amt/Area) and the

analyte Name. The calibration table is used to identify (by retention

time) and quantifr each target compound.

The acquisition method WAX.M is included in the Curve/eA

Chromatograms section of this report.

Custody

Analysis

Calibration

Chromatographic

Conditions

H

EA# 0609-21 Page g of75
Enthalpy Analytical Narrative Summary

QC Notes

(continued)

As required by section 8.4.2, Recovery Study for Bag Sampling, a

recovery study is performed on a bag sample. The bag sample Run 7

was spiked at 2:20 PM on 614109. The recovery efficiency value meets

the method-required limit of between 70 and 130%. The recovery

efficiency value is used to adjust the results following equation 18-7

from sectionI2.8.

All sample preparation and analytical holding times specified in the

method were met.

Reporting Notes These analytical results are reported on a wet basis. The user of this

report should determine the %o moisture in the sample and correct the

reported value to ppmvd as appropriate.

Enthalpy Analytical, Inc. is accredited to perform this method for

compliance purposes by the National Environmental Laboratory

Accreditation Conference OfELAC) through the Louisiana

Environmental Lab or atory Accreditation Program (LELAP), certificate

number 04010.

The results presented in this report are representative of the samples as

provided to the laboratory.

H EA# 0609-21 Page 10 of75
General Reporting Notes

The following are general reporting notes that are applicable to all Enthaþ AnalTticaT,Inc. reports, unless

specifi cally noted othen¡¡ise.

o The symbol MDL represents the Minimum Detection Limit. Below this value the laboratory carurot

confrm the presence of the analyte of interest reliably.

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

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

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

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

indicates that the laboratory can positively identifu the analyte ofinterest as presen! but the value should

be considered an estimate.

o The symbol E following a value indicates an arnlytical result exceedng 100% of the highest calibration

point.

. The syrnbol D,F 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

muþlied by the DF to get final results.

o 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 confirmation of laboratory quality by showing the

consistency of results gained by perfonning the same steps multiple times. Most methods performed by

Enthalpy do not require analysis of an MSD.

o The Sample ID B,S repÍesents a Blind Spike. A member of the Quality Assurance deparhnent has

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

goup.

o 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 confirm 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.

o 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.

')

EA# 0609-21 Page 1 1 of75
Sample Custody
EA# 0609-21 Page 13 of75
Sample

Chromatograms
Data File c: \GC2O09Q2\GUMMo\DATA\JUN09\cC10?pc106\02580301. D

Sample Name: 0609-2I Run 1

Acq. Operator

Acq. Instrument

Inj ection Date

Acq" Method

Last changed

Analysis Method

Last chanqed

kam

Gummo

04-Jun-09, 12:46:05

Seq. Line

Location

rnj

3

Vial 25

I

fnj Volume Exte rnal

G : \Gc20 0 9Q2 \GUMMO\METHoDS \WAX. M

5/12/2009 4:42:20 PM by tbo

G : \GC2 O O 9Q2 \GUMMO\METHODS \O 509-7 BR. M

6/5/2009 1:07:35 PM

400

350

300

250

200

150

100

External- Standard Report

Sorted By :

Calib. Data Modified :

Multiplier i

Diluti-on :

Use Multiplj-er c Dilution

Signal 1: FID2 B,

Signal

5/29 /2009 5 : 50 : 04 PM

1.0000

1.0000

Eactor with ISTDs

RetTime Type Area Amt/Area Amount

[min] [pA*s] [ppn]

| ------ | ---------- I ---------- | ---------- |

1.603 pv 621 .53241 2.'19771 1751.55176

Totals : 1751. 551? 6

Grp Name

-- t-------

Methane

*** End of Report ***

Gumno Reprocess 6/5 /2009 1:07: 39 pM

EA# 0609-21 Page 15 of75

Page 1of1
Data Fil-e c : \Gc2009Q2\GUMMo\DATA\JUN09\GC107PG106\02580302. D

Sample Name: 0609-27 Run 1

Acq. 0perator

Acq. Instrument

f nj ecti-on Date

Acq. Method

Last changed

Analysis Method

Last changed

kam

Gummo

04-Jun-09, 13:02:,04

Seq.Line

Location

rnj

3

Vial 25

2

ln j VoJ-ume Exte rnaÌ

c : \GC2 00 902 \GUMMO\METHODS \WAX. M

5/I2/2009 4:,42:20 PM by tbo

G : \GC2 0 0 902 \GUMMO\METHoDS \0509-7 BR. M

6/5/2009 1:07:35 PM

pA

450

400

350

300

250

200

150

100

50

External Standard Report

Sorted By

Calib. Data Modified

Mul tip J- ie r

Diluti on

Use Multipl-ier & Difution

Signal 1: FfD2 B,

RetTime Type Area

[min] [pA*s ]

r------t----------l

1.603 PV 624.650't0

Totals :

S igna I

5 /29 /2009 5 : 50 : 04 PM

1.0000

1.0000

Factor wlth ISTDs

Aml/Area Amount

Ippm]

l----------l

2 .19771 17 43. 50832

r'143.50832

Grp Name

--t-------

Methane

*** End of RePort ***

Gummo Reprocess 6/5/2009 1:07:48 PM

EA# 0609-21 Page 16 of75

Page 1of1-
Data File G: \GC2009Q2\cUMMo\DATA\,IUNO9\GCl07PG106\02580303. D

Sample Name: 0609-21 Run 1

Acq. Operator

Acq. lnstrument

lnj ection Date

Acq. Method

Last changed

Analysis Method

Last chanqed

kam

Gummo

04-Jun-09, 13: l-B:03

Seq. Line

Location

rnj

3

Viaf 25

3

Inj Volune External

G : \GC2 0 0 902 \cUMMo \METHODS \ldAX . M

5/L2/2009 4:42:20 PM by tbo

G : \GC2 O O 902 \GUMMO\METHODS \O 5O 9-78R. M

6/5/2009 l-:07:35 PM

107PG1

o

n

¡.*

pA

450

400

350

300

250

200

150

100

50

Externaf Standard Report

Sorted By

Calib. Data Modified

Multiplier

Dilution

Use MuftipJ-ier c Difution

Signal 1: FID2 B,

Ret.Time Type Area

[min] [pA*s]

t------t----------

1. 604 PV 622.00848

Totals l

Signal

5/29/2009 5:50:04 PM

1.0000

1.0000

Factor with ISTDs

Amt/Area Amount

lppml

I ---------- | ---------- I

2.19711 t]36.13355

1136.13355

Grp Name

--t-------

Methane

*** End of Reporl ***

Gummo Reprocess 6/5/2009 1:07:57 PM

EA#0609-21 Page 17 of 75

Page 1of1
Data File G: \GC2009Q2\GUMMo\DATA\JUNO9\cC107PG106\02680401. D

Sample Name: 0609-2L Run 2

Acq. Operator

Acq. fnstrument

Inj ection Date

Acq. Method

Last changed

Analysis Method

Last changed

kam

Gummo

04-Jun-09, 13:34:05

S eq . l,ine

I.ocation

rnj

Inj Vo1ume

4

V:-aI 26

1

External

c : \GC2 0 0 902 \cUMMo\METHODS \WAX. M

5/72/2009 4:42:20 PM by tbo

G : \GC2 0 0 9Q2 \GUMMO\METHODS\050 9-7 8R. M

6/5/2009 1:07:35 PM

pA

450

400

350

300

250

200

150

100

50

External Standard Report

Sorted By

Calib. Data Modified

Multiplier

Di-lution

Dilution

Signal

5/29/2009 5:50:04 PM

1.0000

1.0000

Factor with ISTDs

Area Amt,/Area Amount

lpA*s I [ppm]

| ---------- | ---------- | ----------

624.39380 2.197!1 I'142.19129

71 42 .'t 91,29

Use Multiplier

Signal 1: FID2

RetTime Type

Imin] t------

1.604 PV

Total-s :

&

B,

Grp Name

t--t------

Methane

*** End of Report ***

Gummo Reprocess 6/5/2009 1:08:09 PM

EA# 0609-21 Page 18 of75

Page 1of1
Data Fife c: \GC200902\GUMMo\DATA\,IUN09\cC10?pc106\02680402.D

Sanp1e Name: 0609-2I Run 2

Acq. Operator

Acq. fnstrument

lnj ection Date

Acq. Method

Last changed

Analysís Method

Last chanqed

: kam

: Gummo

: 04-,Jun-09, 13:50:04

Seq. T,ine

Locatlon

rnj

Inj Volune

4

ViaI 26

2

Exte rnal

G : \GC2 0 0 9Q2 \GUMMO\METHoDS\tÌAX. M

5/L2/2009 4:42;20 PM by tbo

G : \GC2 0 0 9Q2 \GUMMO\METHODS\ 05 O 9-78R. M

6/5/2009 1:07:35 PM

pA

450

400

350

300

250

200

150

100

50

External Standard Report

Sorted By

Calib. Data Modified

Multiplier

Diluti on

Use MultipIi-er e Dilution

Signal 1: FID2 B,

RetTime Type Area

lninl [pA*s] t------l----------l

1.605 PV 679.62617

Totafs:

S ignal

5/29/2009 5:50:04 PM

1.0000

1.0000

Factor with ISTDs

Amt/Area Amount

lppml

t----------

2.19711 7129.48568

7129.48568

Grp Name

¡--t------

Methane

*** End of Report ***

Gummo Reprocess 6/5/2009 1:08:19 pM

EA#0609-21 Page 19 of75

Page 1of1
Data Eile G : \GC2009Q2\GUMMO\DATA\JUN09\GC107PGl06\02680403. D

Sample Name: 0609-2I Run 2

Acq. 0perator

Acq. Instrument

Inj ection Date

Acq. Method

Last changed

Analysis Method

Last changed

kam

Gummo

04-Jun-09, 74:06:,01

Seq. Line

Locati-on

lnj

4

Vial- 26

a

J

Inj Volume Exte rnaf

G : \GC2 009Q2 \GUMMO\METHoDS \WAX. M

5/72/2009 4:42:.20 PM by tbo

G : \GC2 0 0 9Q2 \GUMMO\METHoDS \ 05 0 9-7 8R. M

6/5/2009 1:07:35 PM

I 06\02680403.D)

pA

450

400

350

300

250

200

150

100

50

Externaf Standard Report

Sorted By

Calib. Data Modifíed

MuIti-plier

Difution

Use Multiplier

Signal 1: FID2

RetTime Type

Imin] t------l

1.604 PV

Totals:

S i gnal

5/29 /2009 5 : 50: 04 PM

1.0000

1.0000

Factor with ISTDs

Amt,/Area Amount

Ippm]

| ---------- I ----------

2.19171 L'136.61668

11 36 . 61668

Grp Name

t--t------

Methane

e D1lut ron

B,

Area

IpA*s]

622 .7Br5B

*** End of Report ++*

Gummo Reprocess 6/5/2009 1:08:27 PM

EA# 0609-21 Page 20 of75

Page 1ofL
Data Fife c: \GC2009Q2\cUMMo\DATA\JUNO9\GC107pc106\02?80501. D

Sample Name: 0609-21 Run 3

Acq. Operator

Acg. Instrument

fnj ection Date

Acq. Method

Last chang.ed

Analysis Method

Last changed

kam

Gummo

04-Jun-09, 74:22:70

Seq. Line : 5

Location :, Vial 2'7

Inj: 1

Inj Volurne: External

G : \Gc2 0 0 9Q2 \GUMMO \METHODS \WAX . M

5/72/2009 4:42:20 PM by tbo

G : \cC20 0 9Q2 \GUMMO\METHODS \ 050 9-7 BR. M

6/5/2009 1:07:35 PM

pA

450

400

350

300

250

200

150

100

50

External Standard Report

Sorted By

Calib. Data Modified

Multipl-ier

Dilution

Use Muftiplier

Signal 1: FID2

RetTime Type

Imin] t-----t

1. 604 PV

Total-s:

Signal

5/29/2009 5:50:04 PM

1.0000

1.0000

Factor with ISTDs

Amt/Area Amount

lppml

| ---------- | ----------

2.'191,t1 1698.58283

1698.58283

Grp Name

t--t------

Methane

e Dilut ron

B,

Area

_ i:i::1_ _ _

608.55493

*** End of Report ***

EA#0609-21 Page21 of75

Gummo Reprocess 6/5/2009 1:08:37 pM Page l-of1
Data FiIe Gr \GC2009Q2\GUMMO\DATA\JUNO9\cC107PG106\02780502. D

Sample Name: 0609-21 Run 3

Acq. 0perator

Acq. lnstrument

fnjection Date

Acq. Method

Last changed

Analysis Method

Last changed

kam

Gummo

Seq.Line

Location

5

ViaI 21

2

Exte rnal

04-Jun-09,74:,38:.1,2 Inj

Tnj Volume

G : \cC2 0 0 9Q2 \cUMMo \METHODS \WAX. M

5/12/2009 4:42:20 PM by tbo

G : \GC20 0 902 \GUMMO\METHODS\ 0 509-7 8R. M

6/5/2009 l,:07:35 PM

pA

450

400

350

300

250

200

150

100

50

t'.- @o

o qo

o

External Standard Report

Sorted By

Ca1ib. Data Modified

Multiplier

Dilution

Use Multipl-ier e Dilution

Sì-gnal 1 : EI D2 B,

RetTine Type Area

lninl [pA*s ]

t------t----------l

1 . 604 PV 670 .1 6263

Totafs:

S ignal

5/29/2009 5:50:04 PM

1.0000

1.0000

Factor with ISTDs

Amt,/Area Amount

lppml

Grp Name

t----------t--t-----

2.191L1 I104.14483 Methane

r104.'14483

*** End of Report ***

Gummo Reprocess 6/5/2009 1:08:46 PM

EA# 0609-21 Page 22 of75

Page 1of1
Da ta File G : \cC2 0 0 9Q2 \cUMMo\DATA\,lUN0 9 \Gc1 0? pc1 0 6 \02780503 . D

Sample Name: 0609-27 Run 3

Acq. Operator

Acq. fnstrument

Inj ection Date

.A,cq. Method

Last changed

Analysis Method

Last chanqed

kam

Gummo

04-Jun-09, 14:54:18

Seq. l,ine

Location

-Ln j

5

ViaI 21

1

J

Inj Volume Exte rnaf

G : \GC2 0 0 9Q2 \GUMMo\METHoDS\WAX. M

5/1.2/2009 4:42:20 PM by tbo

G : \cC2 00 9Q2 \cUMMo\METHoDS \0 50 9-7 BR. M

6/5/2009 1:07:35 PM

pA

450

400

350

300

250

200

150

100

50

External Standard Report

Sorted By

Ca1ib. Data Modified

Multiplie r

Di lution

Use Multiplier & Dilution

Signa1 1: FID2 B,

RetTime Type Area

[min] [pA*s ]

t------t----------

1.604 PV 610.7s098

Totafs :

Siqnal

5/29/2009 5:50:04 PM

1.0000

1.0000

Factor with ISTDs

Amt/Area Amount

lppml

| ---------- | ----------

2 .'7 9171 7't 0 4 .11229

7104.'t1229

Grp Name

t--t------

Methane

*** End of Report ***

Gunmo Reprocess 6/5/2009 1:08:55 pM

EA# 0609-21 Page 23 of 75

Page 1of1
Da ta File G : \GC2 0 0 9Q2 \GUI'4MO\DATA\JUNo9\GC1 0 7PG1 0 6\0 1? B0 2 0 1 . D

Sample Name: N2 Blank

Acq. ôperator : kam

Acq. fnstrument : Gummo

Tnjectlon Date : 04-Jun-09, 10:44:55

Inj Volume

: G : \GC2 00902\GUMMO\METHODS \hlAx.M

pA

450

400

350

300

250

200

150

100

50

External Standard Report

Sorted By

Ca1ib. Data Modlfied

Multiplier

Di.lution

Signal

5/29/2009 5:50:04 PM

1.0000

1.0000

Fãctor with ISTDs

Amt/Area Amount

lppml t----------

Use Multiplier

Signal 1: FID2

RetTime Type

lminl

l------l

1.594

Totals :

Grp Name

t--t------

Methane

1- Vlarnings or Errors i

Vüarning : Calibrated compound(s) not found

Gumrno Reproeess 6/5/2009 1:09:05 PM

EA# 0609-21 Page 24 of75

Page Iof2
Data File G : \GC2009Q2\GUMMO\DÄTA\JUN09\cC107pc106\01780202.D

Sample Name I N2 Bfank

Acq. Operator

Acq. Instrument

lnj ection Date

Acq. Method

T,as t changed

Analysis Method

LasÇ changed

kam Seq. Line : 2

Gummo Location : Vial 17

04-Jun-09, 12:15;36 tnj : 2

Inj VoIume: External

G: \Gc2 0 0 9Q2 \GUMMo\METHODS \WAX. M

5/I2/2009 4:42:20 PM by tbo

G : \GC2 O O 9Q2 \GUMMO\METHODS \O5O 9-7 BR. M

6/5 /2009 1 : 07 : 35 PM

pA

450

400

350

300

250

200

150

100

50

Externaf Standard Report

Sorted By

Calib. Data Modified

Multipl ie r

Diluti on

Use Muftiplier & Dilution

Signal 1: FlD2 B,

RetTime Type Area

lminl [pA*s ]

t------t----------

L -594

Totafs :

S ignal

5/29/2009 5:50:04 PM

1.0000

1.0000

Factor with ISTDs

Amt/Area Amount

lppml

| ---------- | ---------- I

0.00000

Grp Name

--t-------

Methane

t hlarnings or Errors :

l{arning : Calibrated compound(s) not found

Gummo Reproces s 6/5/2009 1:09:14 pM

EA# 0609-21 Page 25 of 75

Page Iof2
Data File c : \cC2 00 9Q2 \GUMM0\DATA\,IUN09 \GC107 PG10 6\0 1?802 03 . D

Sample Name: N2 Blank

Acq. Operator

Acq. Instrument

lnj ection Date

Acq. Method

Last changed

Analysis Method

Last changed

kam

Gummo

04-Jun-09, 12;30:01

Seq. Line

T,ocation

rnj

¿

ViaI 17

3

Inj Volune Externalc : \cC2 0 0 9Q2 \GUMMO\METHODS \I^IAX. M

5 / 1.2 / 2009 4 : 42:,20 PM by tbo

c : \GC2 0 0902 \GUMMo\METHODS \ 050 9-7 BR. M

6/5/2009 1:07:35 PM

External Standard Repor

Sorted By

Calib. Data Modlfied

SignaI

5/29/2009 5:50:04 PM

1.0000

1.0000

Factor with ISTDs

Area A¡nt/Area Amount

lpA*s I [ppm]

| ---------- I ----------

Multiplier

Di lution

Use MuJ-tiplier

Signal 1: FfD2

RetT j-me Type

lmin] l------l

1.594

Totals :

& Dilut 10n

B,

Grp Name

t--t------

Methane

0.00000

1 Ìdarnings or Errors :

[nlarning : Calibrated cornpound (s ) not f ound

pA

450

400

350

300

250

200

150

100

50

Gurnmo Reprocess 6/5/2009 1:09:23 PM

EA# 0609-21 Page 26 of75

Page 1-of2
Data File G : \cC2 00 9Q2 \GUMMO\DATA\,IUNO 9\GC1 0? pcl 07 \02 58030 1 . D

Sample Name: 0609-21 Run 1 Sp

Acq. Operator

Acq. Instrument

fnj ection Date

Acq. Method

Last changed

Analysis Method

Last changed

kam

Gummo

05-Jun-09, 20:.06:31

Seq. Line

Location

rnj

a

J

Vi-a] 2 5

1

fnj Volune External

G: \GC2 0 0 902 \cUMMo\METHODS \ldAX. M

5/72/2009 4:42;20 PM by tbo

G : \cc2 0 0 9Q2 \cUMMo\METHODS \0 509-? 8R. M

6/5/2009 1:25:03 PM

(modified after loadj-ng)

pA

450

400

350

300

250

200

'150

100

50

External Stairdard Report

Sorted By

Ca1ib. Data Modified

Multiplier

Dilution

S ignal

5 /29 /2009 5: 50 : 04 PM

1.0000

1.0000

Use Multiplier Factor with ISTDs

Signal 1: EID2

& DíÌution

B,

RetTime

_iil:1_

1.600

Totafs

Type Area

lpA*sl t------t----------l

PB 1152.9189s

Amt,/Area

2 .1 9176

Amount

lppml t----------l

321't.97'78't

3211.91181

Grp Name

--t-------

Methane

*** End of RePor¡ *'t*

Gummo Reprocess 6/5/2009 B:34:48 pM

EA#0609-21 Page27 of75

Page 1of1
Data File G : \GC2 0 0 9Q2 \cUMMo\DATA\.lUN0 9\GC107 PG107\ 02 580302 . D

Sample Name: 0609-2L Run 1 SP

Acq. Operator

Acq. Instrument

Injection Date

Acq. Method

Last changed

Analysis Method

Last changed

kam

Gummo

05-Jun-09, 20:22:,27

Seq.Lìne

l,ocation

lnj

Inj Volume

3

Vial 25

2

External

G: \GC2 0 0 902 \GUMMO\METHODS \WAx. M

5/72/2009 4:,42:20 PM by tbo

G : \Gc2 00 9Q2 \GUMMO\METHoDS \0509-7 8R. M

6/5/2009 'l:25:.03 PM

(modified after loading)

pA

450

400

350

300

250

200

150

100

50

External Standard Report

Sorted By

Cafib. Data Modified

Multiplier

Dilution

S ignal

5/29/2009 5:50:04 PM

1.0000

1.0000

Use Multiplier Factor with TSTDs

Signal 1: FID2

& Dilution

Þ

RetTime Type Area Amt/Area Amount Grp Name

lminl [pA*s ] [ppm] l------ l----------l ---------- I -------- -r-- r---------

1. 602 PB 7141 .82056 2.'79116 3203.14'156 Methane

Totals : 3203 -'1 41 6

*** End of Report ***

Gummo Reprocess 6/5/2009 B:34:56 PM

EA# 0609-21 Page 28 of75

Page 1of1
Da ta File c : \GC2 00 9Q2 \GUMMO\DATA\ JUNO 9 \cC1 0? pcl07 \ 02 5803 03 . D

Sample Name: 0609-27 Run 1 Sp

Acq. Operator

Acq. Instrument

Inj ection Date

Acq. Method

Last changed

Analysis Method

Last changed

kam

Gummo

05-Jun-09, 20:,38:.76

Seq.Line

Locati-on

rnj

Inj Volume

3

ViaI 25

3

Bxternal

G: \GC2 0 0 9Q2 \GUMMo\METHODS \t^lAX . M

5/12/2009 4:42:20 PM by tbo

G : \GC2 O O 9Q2 \GUMMO\METHODS \ O5O 9-? 8R. M

6/5/2009 7:25:03 PM

(modified after loading)

pA

450

400

350

300

250

200

150

100

50

External Standard Report

Sorted By

Calib. Data Modified

Multipl i e r

Dllution

Use Multiplier c Dilution

Signal 1: FID2 B,

RetTime Type Area

lninl [pA*s ]

t------t----------l

1.602 PB 1151.56189

Totafs :

Signal

5/29/2009 5:50:04 PM

1.0000

1.0000

Factor with ISTDs

Amt/Area Amount

lppml t----------l

2 .191,76 3214 .t9074

32I4.19014

Grp Name

Methane

*** End of Report ***

Gummo Reprocess 6/5/2009 10:17:33 pM

EA# 0609-21 Page 29 of75

Page 1of1
Curve(s)/QA PoÍnt(s)

Chromatograms
Me thod c : \cC2 0 0 9Q2 \GUMMO\METHODS \ O 5 0 9- 7 BR. M

Calibration Table

Ca1ib. Data Modified

Calcul-ate

Based on

Rel. Reference Window Äbs. Reference nüindow

Re1. Non-ref. Vfindow

Abs. Non-ref. Window

Use Multiplier e Diluti

Uncafibrated Peaks :

Partial Calibration :

Correct Aff Ret. Times:

Curve Type

Origin

VÍeight

5/29/2009 5:L2:02 PM

External_ Standard

Peak Area

2.000 z

0.000 min

2.000 z

0.000 min

on Factor with ISTDs

not reported

Yes, ldentified peaks are recalibrated

No, only for identified peaks

: Linear

: Connected

: Linear (Resp)

Recalj-bration Settj_ngs :

Average Response : Average alJ_ calibrations Average Retention Time: Floating Averag.e New 75E'

Calibration Report Options :

Printout of recalibrations within a sequence:

Cafibration Table after Reca1i_bration

Normal Report after Recalibration

If the sequence is done with bracketing:

Resul_ts of first cycle (ending previous bracket)

Signal 1: FID2 B,

Signal 2: FID1 A/

RetTime Lv1 Amount Area Amt,/Area Ref Grp Name

[min] Sig [ppm]

| -- | -- | ---------- | ---------- | -----_____ | ___ t__ | ______

I-594 I 21 3.00000 1.09191 2.74i41 Methane 22 20.00000 6.86-728 2.9\236 23 45.00000 15.91A34 2.87.t55 24 101.20000 36.35231 2.7838-7

25 1000.00000 356.6"7L72 2.80370

26 1,.00200e4 3'tri.0s184 2.69569

2'7 8.06000e4 2.8'7560e4 2.BO2e2

Peak Sum Table

Name startrime EndTime use Response Multiplier rsrD lminl [min] Reference factor peak

- | ------- I ------- I ---------- | -------- | __________ I ___________

as ethane 1.655 1.890 None 1.45L4 1.0000 None

as propane 1.890 2.500 None 9.9gO2e-1 1.0000 None

as butane 2 .500 3. 950 None i .4S6Le-t 1. 0O0O None

as pentane 3.950 6.050 None 6-OB29e-I 1.0000 None

as hexane 6. 050 7. 850 None 5.3075e-1 1. 0000 None

as heptane 7.850 11.500 None 4.45g8e-1 1.0000 None

Harpo 5/29/2009 5:44:37 pM

EA# 0609-21 Page 31 ofTS

Page L of 2
MEthod G : \GC2 O O9Q2 \GUMMO\METHODS\ 05 O 9-? 8R. M

0

0

EA# 0609-21 Page 32 o'f 75
Data Fil-e G : \GC2 009e2 \GUMMO\DATA\APRO 9 \cC1 07pcO 74 \ O1 BBOT 01 . D

Sample Name: 9e707pq074 *1_I

Acq. Operator

Acq. fnstrument

Injection Date

Acq. Method

Last changed

Analysis Method

Last changed

: stg

: Gummo

: 2L-Apr-09, 02 :10:18

Seq. Line

Location

rnj

fnj Volume

1

Vial 18

1

External

: G : \GC2009Q2\GUMMO\METHODS\!vAX. M

: 4/2/2009 10:51:55 AM by kam

: G: \GC2009Q2\GUMMO\METHODS\0509-7BR.M

: 5/29/2009 5:21:31 PM

(modified after loadinq)

pA

90

80

70

60

50

40

30

20

10

External Standard Report

Sorted By

Ca1ib. Data Modified

Multiplier

Dilution

Use Multiplier

Signal 1: FfD2

RetTime Type

fmin] t------l

1.597 PV

Totals :

SignaJ5/29/2009 5:12:02 PM

1.0000

1.0000

Factor with fSTDs

Area Amt/Area Amount Grp Name

lpA*sl [ppm]

I ---------- | ---------- | -- | --------- 1.07959 2.81159 3.03535 Methane

3 . 0353s

& Dilut 10n

B,

*** End of RePort ***

Harpo 5/29/2009 5:29:46 pM

EA# 0609-21 Page 33 of75

Page 1of1
Data File G : \cC2009Q2\GUMMO\DATA\APRO9\cC107PG074\01880702. D

Sample Name: qclOlpq)1 4 #77

Acq. Operator

Acq. Instrument

f nj ectj-on Date

Acg. Method

Last changed

Analysis Method

Last changed

Gummo

2!-Apx-09, 02:26:17

Seq. Line

Location

rnj

'l

Viaf 18

2

Inj Volume ExternalG : \GC2 0 0 9Q2 \GUMMO\METHODS \ViAx. M

4/2/2009 10:51-:55 AM by kam

c: \GC2 0 0 9Q2 \GUMMO\METHODS \ 05 0 9- ? BR. M

5/29/2009 5:27:31 PM

(modified after foadinq)

FlD2 B, (G:\GC2009Q2\GUMMO\DATA\APR09\GC1 07PG074\01 880702.D)

pA

90

80

70

60

50

40

fo

30 --l Ë

JÔl>

20 1 - n

,oJ ffË i u Ë i

(ÐÌ-q

o

ExLernal Standard Report

Sorted By

Cal1b. Data Modified

Multiplier

Dil-ution

Signal

5/29/2009 5:]-2:02 PM

1.0000

1.0000

Use MuJ-tipller ç Dil-ution Factor with ISTDs

Signal 1: FID2 B,

RetTime Type Area Amt/Area Amount Grp Name

lminl [pA*s] [ppm]

| ------ | ---------- I ---------- t---------- | -- | ---------

1.598 PB 7.08572 2.871-41 3.0524'l Methane

Totals : 3.05241

*** End of Report ***

Harpo 5/29/2009 5:29:52 PM

EA# 0609-21 Page 34 o'f 75

Page I of L
Data File G: \GC2009Q2\GUMMO\DATA\APR09\GC107PG074\01880703. D

Sample Name: gcI}lpqOl 4 #1L

Acq. Operator

Acq. Instrument

Injection Date

Acq. Method

Last changed

Analysis Method

Last changed

òL9 -tGummo

21--Apr-09 , 02:42:04

Seq. T,ine

Location

rnj

Inj Vol-ume

1

Vial- 18

a

J

External

G: \GC2 0 0 9Q2 \GUMMO\METHODS \VíAX . M

4/2/2009 10:51:55 AM by kam

G : \GC2 0 0 9Q2 \GUMMO\METHODS \ 05 0 9-7 BR. M

5/29/2009 5:2'7:31 PM

(modified after loading)

pA

90

80

70

60

50

40

30

20

'10

External- Standard Report

Sorted By

Ca1ib. Data Modified

Multiplier

DiLution

Signal

5/29/2009 5:1.2:02 PM

1.0000

1.0000

Use Multiplier ç Dj-lution Factor with ISTDs

Signal 1: FlD2 Bl

RetTime Type Area Amt,/Area Amount Grp Name

lrnin] [pA*s] [pprn]

| ------ I ---------- | ---------- | ---------- | -- | ---------

1.598 PB 1. 11043 2 .81702 3 .1-2\45 Methane

Totals : 3.12145

*** End of Repor¡ ***

Harpo 5/29/2009 5:29;59 PM

EA# 0609-21 Page 35 of75

Page L of L
Data Fif e G : \GC2 0 09Q2 \GUMMO\DATA\APR0 9\cC1 07pcO? 4 \ 01980 601 . D

Sample Name: gcI07pq074 #\2

Acg. Operator

Acq. Instrument

fnjection Date

Acq. Method

Last changed

Analysi-s Method

Last changed

stg

Gummo

21-Apr-09, 01,:,22238

Seq. Line

Location

Tnj

lnj Vo1ume

6

Vi-al 19

1

External

G: \GC2 O O 9Q2 \GUMMO\METHODS \WAX. M

4/2/2009 10:51:55 AM by kam

G : \GC2 O O 9Q2 \GUMMO\METHODS\ O5 O9-7 8R. M

5/29/2009 5:27:31 PM

(modified after loadinq)

pA

90

80

70

60

50

40

30

20

10

External- Standard Report

Sorted By

Cafib. Data Modlfied

MuJ-tiplier

Dilution

Use Multipfier c Difu

Sígnal 1: FfD2 B,

RetTlme Type Area

[min] [pA*s ]

t------t----------

1.596 PV 6.90681

Total-s :

Signal

5/29/2009 5=1-2:02 PM

1.0000

1.0000

tron Factor with ISTDs

Amt,/Area

t----------l

2 .'7 9433

Amount Grp Name

Ippm] t--l------ 19.30011 Methane

19.30011

*** End of Report ***

Harpo 5/29/2009 5:30:06 pM

EA# 0609-21 Page 36 of75

Page 1of1
Data Fife c: \GC2009Q2\GUMMO\DATA\APR09\cC107pc074\01980602 . D

Sample Name: gcL07pg074 #1,2

Acq. Operator

Acq- fnstrument

Injection Date

Acq- Method

Last changed

Analysis Method

Last changed

stg

Gummo

21--Apr-09, 01:38:34

Seq. Line

Locati-on

rnj

Inj Volume

6

Vi-al- 19

2

External

G : \GC2 O O 9Q2 \GUMMO\METHODS\VüAX. M

4/2/2009 10:51:55 AM by kam

G : \cC2 0 0 9Q2 \GUMMO\METHODS \ 050 9-7 BR. M

5/29/2009 5:2'l:31 PM

(modified after loading)

External Standard Report

Sorted By

Ca1ib. Data Modified

Multiplier

Dilution

Use Multiplier

Signal 1: ElD2

RetTime Type

lminl

l------

1.596 PV

Totafs :

Signal

5/29/2009 5:1-2:02 PM

1.0000

1.0000

Factor with ISTDs

Amt/Area Amount

Ippm]

6 .8817 6 2 .19434

Grp Name

r----------t--l

19.24676 Methane

1-9 .246't 6

& Dilutton

B,

Area

lpA* s l

*** End of Report ***

Harpo 5/29/2009 5:30:13 PM

EA#0609-21 Page 37 of 75

Page lofl
Data FiIe G : \Gc2 0 0 9Q2 \GUMMO\DATA\APR0 9\cC107PGO7 4 \01 980 603 . D

Sample Name: qc1-01p9074 #12

Acq. Operator

Acq. Instrument

Injection Date

Acq. Method

Last changed

.Analysis Method

f,ast changed

. ùL9

: Gummo

: 21-Apr-09, 01,:54221

Seq. Line

Location

rnj

6

Viaf 19

J

Inj Volume ExternalG: \GC2 0 0 9Q2 \GUMMO\METHODS \vüAX . M

4/2/2009 10:51:55 AM by kam

G : \GC2 0 0 9Q2 \GUMIVO\METHODS\ 0s 0 9-7 BR. M

5/29/2009 5:2'l:31 PM

(modified after loadinq)

pA

90

80

70

60

50

40

30

20

t0

Externaf Standard Report

Sorted By :

Ca1ib. Data Modifi-ed :

Multiplier :

Difution :

Use Multiplier c Di-lution

Signal 1: FID2 B,

RetTime Type Area

Signal

5/29/2009 5:72:02 PM

1.0000

1.0000

Factor with ISTDs

Amt,/Area Amount Grp

IPPm]

Name

lminl IpA*s]

1.597 PV

Totals :

6.80720 2.19438 1-9.021-92 Methane

L9 -02192

*** End of Report ***

Harpo 5/29/2009 5:30:20 PM

EA# 0609-21 Page 38 of75

Page 1of1
Data Fife G: \GC2009Q2\GUMMO\DATA\APR09\GC107pcO74\02080501. D

Sample Name: 9c107pq074 #13

Acq. Operator

Acq. fnstrument

lnjection Date

Acq. Method

T,ast changed

Analysis Method

Last changed

stg

Gummo

21--Apr-09, 00:34:40

Seq. T,ine

Location

rnj

Inj Volume

5

VíaI 20

1-

ExternalG: \GC2 0 0 9Q2 \cUMMo\METHODS \WAX . M

4/2/2009 10:51:55 AM by kam

G : \GC2 O O 9Q2 \GUMMO\METHODS \ O5 O 9-7 8R. M

5/29/2009 5:2'1:31 PM

(modified after loadinq)

External Standard Report

Sorted By

Cai-ib. Data Modified

Multiplier

Dil-ution

Signal

5/29/2009 5:72:02 PM

1.0000

1.0000

Use Multiplier Factor with ISTDs

Siqnal 1: FID2

& Dil-ution

Þ

RetTime Type Area

lminl [pA* s ]

t------t----------

1.598 PV 75.94104

Totafs :

Amt,/Area

l----------l

2.79252

Amount

lppml

44.5]-513

44.51,513

Grp Name

t--t------

Methane

x** End of Report ***

Harpo 5/29/2009 5:30:30 PM

EA# 0609-21 Page 39 of75

Page 1of1
Data Fife G: \GC2009Q2\GUMMO\DATA\APR09\GC107PG074\ 02080502 .D

Sample Name: qc107p9074 #13

Acg. Operator

Acq. ïnstrument

Inj ection Date

Acq- Method

Last changed

Analysis Method

Last changed

. ù L9

: Gummo

: 21-Apr-09, 00: 50:36

Seq. Line

Locati-on

Tnj

Tnj Vol-ume

5

Vial 20

2

Externaf

G : \cC2 0 0 9Q2 \GUMMO\METHODS \wAx . M

4/2/2009 10:51:55 AM by kam

G : \GC2 00 9Q2 \GUMMO\METHODS \ 05 0 9-7 BR. M

5/29/2009 5:27:31 PM

(modified after loadinq)

External Standard Reporl

Sorted By

Cafib. Data Modified

MuJ-tiplier

Dilution

Use Multiplier

Signal 1: FID2

RetTj-me Type

Imin] t------l

1.596 PV

Totals :

SignaI

5/29/2009 5:1,2:02 PM

1.0000

1.0000

Factor with ISTDs

Amt/Area Amount

lPpml

l----------l 2.'792s7 44.83'tB6

44.83186

Grp Name

-- | -------

Methane

e Dilut 10n

D

Area

lpA* s l

----------l

76 .05646

*** End of Report ***

Harpo 5/29/2009 5:30:36 PM

EA# 0609-21 Page 40 of75

Paqe lofL
DAtA FilE G: \GC2OO9Q2\GUMMO\DATA\APRO9\GC1O7PGO74\02OBO503. D

Sample Name: gcl07pq074 #13

Acq. Operator

Acq" Instrument

Inj ection Date

Acq. Method

Last changed

Analysls Method

Last changed

: Gummo

:2l-Apr-09,01:06:35

Seq. Line

Location

rnj

fnj Volume

5

Vial- 20

3

External

G: \GC2 O O 9Q2 \GUMMO\METHODS \WAX . M

4/2/2009 10:51:55 AM by kam

G : \cC2 0 0 9Q2 \GUMMO\METHODS \ 05 0 9-7 BR. M

5/29/2009 5:2'7:31 PM

(modifled after loadinq)

'ol ffì n e

Externaf Standard Report

Sorted By :

Cafib. Data Modified :

Multiplier :

Difution :

Use Multiplier c Dilution

Signal- 1: FID2 B,

RetTime Type Area

[min] [pA*s ]

t------t----------l

1 - 596 PV 15. 91650

Totals :

Slgnal

5/29/2009 5:L2:02 PM

1.0000

1.0000

Factor with ISTDs

Amt/Area Amount

Ippn] t----------l

2 .19252 44 " 44'7 24

44 .441 24

Grp Name

--t-------

Methane

*** End of Report ***

Harpo 5/29/2009 5:30:42 pM

EA# 0609-21 Page 41 of75

Page 1of1
Data File c: \GC2009Q2\GUMMO\DATA\APR09\cC107PGO74\021B0901. D

Sample Name: qc1,07pq07 4 #1,4

Acq. Operator

Acq. fnstrument

Inj ection Date

Acq. Method

Last changed

Analysis Method

Last changed

stg

Gummo

21"-Apr-09 , 09:1-'l :43

Seq. Line

Location

rnj

9

VíaI 21-

1

Inj Volume External

G: \GC2 0 0 9Q2 \GUMMO\METHODS \WAx . M

4/2/2009 10:51:55 AM by kam

G : \GC2 0 09Q2 \GUMMO\METHODS\05 09-7 8R. M

5/29/2009 5:34:41 PM

ExternaÌ Standard Report

Sorted By

Calib. Data Modifi-ed

Multlplier

Dilution

Use Multiplier &

Sj-gnal 1: EfD2 B,

RetTime Type Area

[min] [pA*s ]

¡------t----------

1 . 593 PV 36 .2'7 6'7'1

Totafs :

Signal

5/29/2009 5:L2:02 PM

1.0000

1.0000

Factor with ISTDs

Amt,/Area Amount

Ippm]

| ---------- | ----------

2 .191_15 1_01" .27 554

10r.21554

Grp Name

t--t------

Methane

Difut aon

*** End of Report ***

Harpo 5/29/2009 5z4l:50 PM

EA#0609-21 Page42of75

Page 1of1
Data File G: \GC2009Q2\GUMMO\DATA\APR09\cC107pGO?4\02180902. D

Sample Name: 9c707pq074 #74

Acq. Operator

Acq. Instrument

Injection Date

Acq. Method

Last changed

Analysis Method

Last chanoed

stg

Gummo

2I-Apr-09,09:33:49

Seq. Line

Location

rnj

9

YiaI 27

2

Inj Volume External

G: \GC2 O O 9Q2 \GUMMO\METHODS \WAX . M

4/2/2009 10:51:55 AM by kam

G : \GC2 O O 9Q2 \GUMMO\METHODS\ O5 O 9- ? BR. M

5/29/2009 5:34:41- PM

External Standard Report

Sorted By

Cafib. Data Modified

MultipJ-1er

Dilution

Use Multiplíer & Difution

Signal 1: FID2 B,

RetTj-me Type Area Amt,/Area Amount Grp Name

lminl [pA*s ] [ppm]

| ------ t---------- | ---------- | ---------- | -- | ---------

1.593 PV 6-28415 2.191,'75 1-0I.29i82 Methane

Totafs : 101 .29'lB2

*** End of Report ***

Slgnal

5/29/2009 5:12:02 PM

1.0000

1.0000

Factor with ISTDs

Harpo 5 /29 /2009 5: 4'7 :57 PM

EA# 0609-2'1 Page 43 of 75

Page Lofl
Data Fil-e G : \cC2 0 0 9Q2 \GUM'4O\DATA\APR0 9 \ GCI01 PG07 4\ 02 180 9 03 . D

Sample Name: gcl07pg074 #I4

Acq. Operator

Acq. Instrument

Injection Date

Acq. Method

Last changed

Analysis Method

Last changed

stg

Gummo

21--Apr-09 , 09 :, 49 z 31

Seq. Line

Location

rnj

9

Vial 21

3

Inj Volume External

G: \GC2 0 0 9Q2 \GUMMO\METHODS \WAX . M

4/2/2009 10:51:55 AM by kam

G : \GC2 00 9Q2 \GUMMO\METHODS \0509-7 BR. M

5/29/2009 5:34:41 PM

pA

'140

120

100

80

60

40

20

External Standard Report

Sorted By

Cafib. Data Modified

Multiplier

Dilution

Use Multiplier

Signal 1: EID2

RetTime Type

Imin]

l------l

1.593 PV

Total-s :

Signal

5/29/2009 5:]-2:.02 PM

1.0000

1.0000

Factor with fSTDs

Amt,/Area Amount

lppml

| ---------- | ----------

2.'791_74 101.88583

101.88583

Grp Name

t--l------

Methane

& Dilutl_on

D

Area

[pA* s ]

36.49542

*** End of Report ***

Harpo 5/29/2009 5:48:03 PM

EA# 0609-21 Page44of75

Page lof1
Data F11e G : \GC2 0 0 9Q2 \GUMMO\DATA\APR0 9\GC1 07PGO 7 6\0 1 9BO 1O 1 . D

Sample Name: 9c107pq076 #15

Acq. Operator

Acg, ïnstrument

fnjection Date

Acq. Method

Last changed

Analysis Method

Last changed

Sample Info

^l ò L9-

Gummo

23-Apr-09, 7L:0L¡12

Seq. Line

Location

rnj

1

Vial 19

1

Inj VoJ-ume Externaf

G: \GC2 O O 9Q2 \GUMMO\METHODS \WAX . M

4/2/2009 10:51:55 AM by kam

G : \GC2 0 0 9Q2 \GUMMO\METHODS \05 0 9-7 8R. M

5/29/2009 5:32:00 PM

(modifíed after l-oading)

Methane Only

pA

1400

1200

1 000

800

600

400

200

External Standard Report

Sorted By

Calib. Data Modified

MultipJ-ier

Dilution

Use Multiplier c

Signal 1: FID2 B,

RetTime Type Area

[min] [pA* s ]

t------l----------

1.592 PB 363.40607

Totals :

Signal

5/29/2009 5:L2:,02 PM

1. 0000

1.0000

Factor with ISTDs

Amt,/Area Amount

Ippm]

2.'79120 1014.338s3

1014.33853

Grp Name

l--t------

Methane

Dilut 10n

*** End of Report ***

Harpo 5/29/2009 5:32;05 pM

EA#0609-21 Page 45of 75

Page 1of1
Data F1Ie G : \GC2 00 9Q2 \GU¡04O\DATA\APR0 9\GC107 PGO7 6 \01980102 . D

Sample Name: 9c107pq076 #15

Acq. Operator

Acq. fnstrument

lnj ection Date

Acq. Method

Last changed

Analysis Method

Last changed

Sample Info

stq

Gummo

23-Apr-09, 11: 17 : 06

Seq. Line

Location

rnj

1

Vial 19

2

Inj Volume External

G : \GC2 O O 9Q2 \GUMMO\METHODS \WAX . M

4/2/2009 10:51:55 AM by kam

G : \GC2 O O 9Q2 \GUMMO\METHODS\0509-7 8R. M

5/29/2009 5:32:00 PM

(modified after loading)

Methane Only

pA

1400

1200

1 000

800

600

400

200

Externaf Standard Report

Sorted By

Calib. Data Modified

Multiplier

Dilution

Use Multiplier e Dil-ut

Signal 1-:, TID2 B,

RetTime Type Area Amt/Area Amount Grp Name

Inin] lpA* s l Ippm]

1_ - 593 PB

Totals :

357 . 05508 2 -1 9120 996 - 61.206 Methane

996 .6L206

ron

Signal

5/29/2009 5:1,2:02 PM

1.0000

l-.0000

Factor with ISTDs

*** End of Report ***

Harpo 5/29/2009 5:32211 PM

EA# 0609-21 Page 46 of75

Page lofl-
Data Fil-e c : \cC2 0 0 9Q2 \GUMMO\DATA\APRO9 \cC107PGO7 6 \ 01980 1 03 . D

Sample Name: gc107pqO76 #15

Acg. Operator

Acq. ïnstrument

fnj ection Date

Acq. Method

Last changed AnaÌysis Method

Last changed

Sample fnfo

stg Seq. L j_ne : 1

Gummo Location : Viaf 19

23-Apr-09, 1L:24:.29 nj: 3

lnj Volume : Externaf

G: \GC2 O O 9Q2 \GUMMO\METHODS \ÍfAX . M

4/2/2009 10:51:55 AM by kam

G : \cC2 0 0 9Q2 \GUMMO\METHODS\ 05 0 9- 7 BR. M

5/29/2009 5:,32:00 PM

(modified after loading)

Methane OnJ-y

pA

1400

1200

1 000

800

600

400

200

c, c

ñ

E

d)

t

$

o¡ q?

N

C\¡

o

External Standard Report

Sorted By

Caflb. Data Modified

Multiplier

Dilution

SignaI

5/29/2009 5;1,2:02 PM

1.0000

1. 0000

Use Multiplier ç Difution Factor with ISTDs

Signal 1: FID2 Bl

RetTime Type Area Amt/Area Amount Grp Name

[min] [pA*s] [ppm]

| ------ | ---------- I ---------- | ---------- | -- I ---------

1.594 PB 349.55222 2-79120 9'75.61052 Methane

Totafs : 975 -61052

*** End of Report ***

Harpo 5/29/2009 5:32:.20 PM

EA#0609-21 Page47 of75

Page 1 of 1

Data File G: \GC2009Q2\GUMMO\DATA\APR09\cC10?PGO76\02180401. D

SampJ-e Name: qc107pq076 #16

Acq. Operator

Acq. ïnstrument

Injection Date

Acq. Method

T,ast changed

Analysis Method

Last changed

Sample lnfo

Gummo

23-Apr-09 , 11 : 51 : 18

Seq. Line

Location

rnj

4

Vial 21

1

lnj Volume External

G : \GC2 0 0 9Q2 \GUMMO\METHODS \WAX. M

4/2/2009 10:51:55 AM by kam

G : \GC2 00 9Q2 \GUMMO\METHODS \05 0 9-7 8R. M

5/29/2009 5:32:00 PM

(modified after loading)

Methane Only

pA

1400

1200

I 000

800

600

400

200

Externaf Standard Report

Sorted By

Ca1ib. Data Modified

Multiplier

Dilution

Use Multiplier c Difution

Signal 1: EID2 Bl

RetTime Type Area

[nin] [pA*s ]

t------t----------l

1.594 PB 3713.00903

Totafs :

Signal

5/29/2009 5:L2:02 PM

1.0000

t-.0000

Factor wíth fSTDs

Amt,/Area Amount

IPPm] t----------l

2.1911-4 1.03635e4

1. 03635e4

Grp Name

--t-------

Methane

*** End of Report ***

Harpo 5/29/2009 5:32:,34 PM

EA# 0609-21 Page 48 of75

Page 1of1
Data Fife G: \cC2009e2\GUMMO\DATA\APRO9\GC1O7pco7 6\021B04O2.D Sampì-e Name: gc107pg076 #16

*:: Acq. ?f::"o' ' rts seq. Line : 4

Instrument : Gummo Location: Vial 21 lnjection Date : 23-Apr-09, I1_:5g:42 -""-';;i 

: "':

r¡rJ . Z

G: \GC2oo9e2\GUMM.\METH.DS\wAX. 

rnj volume

4/2/2009 10:51:55 AM by kam

G : \GC2 O O 9Q2 \GUMMO\METHODS\ O5 O9-7 BR. M

5/29/2009 5:32:O0 PM (modified after loading)

Methane Only

External Ä,cq. Method

Last changed

Analysis Method

Last changed

Sample Info

External Standard Repor

Sorted By

Ca1ib. Data Modified

Multiplier

Dilution

& Dilution

B,

Signaì_

5/29/2009 5:12:02 pM

1.0000

1.0000

Factor with ISTDs

Area Amt,/Area Amount Grp Name [pA*s] Ippml

| ---------- I ---_______ | __ | _________ 3701.8'1280 2.i9IL4 1.03325e4 Merhane

1. 03325e4

Use Multiplier

Signal 1: FID2

RetTime Type

[min] t------l

1.594 PB

Totals :

*** End of Report ***

larpo 5/29/2009 S:32-.42 pM

EA#0609-21 Page49 ofTS

Page 1of1
)ata File G: \GC2009Q2\GUMMO\DATA\APR09\GC107PGO76\02180403' 

D

iample Name: gc107PgO76 +16

Acq. Operator

Acq. fnstrument

Injectíon Date

Acq. Method

Last changed

Analysis Method

Last changed

Sample Tnfo

: stg

: Gummo

: 23-APr-09, t2:O'1 t0'l

Seq. Line

Location

Tnj

Tni Volume

4

YLa:. 21

3

External

G: \GC2 O 0 9Q2 \GUMMO\METHoDS \WAX ' M

4/2/2009 10:51:55 AM bY kam

G : \GC200 9Q2 \GUMMO\METHODS\0509-7 BR' M

5/29/2009 5:32:00 PM

(modifÍed after loading)

Methane OnlY

Externaf Standard Repor

Sorted BY

Ca1lb. Data Modi-fied

MultiPlier

Dilution

Signal

s/29/2009 5"L2z02 PM

1. 0000

1. 0000

Factor with ISTDs Use MultiPlier

Signal 1: EID2

RetTime TYPe

Imin]

l------l

1.593 PB

Totals :

& Difution

B,

Area

[pA* s ]

----------l

3136.21368

Amt/Area Amount

IPPm]

t----------

2.'19114 1-.04285e4

L -04285e4

Grp Name

t--l------

Methane

*** End of Report ***

pA

1400

1200

't 000

800

600

400

Ilarpo 5/29/2009 5"32:48 PM

EA# 0609-2',l Page 50 of 75

Page 1of1
Data Fife G: \GC2009Q2\GUMMO\DATA\APR09\GC107PG074\02181401-. D

Sample Name: 9c101p9014 #77

Acq. Operator

Acq. fnstrument

fnjection Date

Acq. Method

Last changed

Analysis Method

Last changed

: Gummo

:, 2I-Apr-09 , 22 232:00

Seq. Llne

Location

Tnj

Inj Volume

74

Vial 21

1

Externaf

G : \GC2 0 0 9Q2 \GUMMO\METHODS \WAX. M

4/2/2009 10:51:55 AM by kam

c : \GC2 00 9Q2 \GUMMO\METHODS\ 05 09-7 8R. M

5/29/2009 5:31:26 PM

(modified after loadinq)

pA

14000

1 2000

I 0000

8000

6000

4000

2000

External Standard Report

Sorted By

Ca1ib. Data Modified

Multiplier

Diluti-on

Use Muftiplier & Dil-ution

Signal 1: FID2 B,

RetTime Type Area Amt,/Area Amount Grp Name

[min] [pA*s ] [ppm] t------t---------t----------t-l--l-----

1.581 PB 2.87722e4 2.19a1-4 8.030?3e4 Methane

Totals : 8.03073e4

*** End of Report ***

Signal

5/29/2009 5:12:.02 PM

1.0000

1.0000

Factor with ISTDs

Harpo 5/29/2009 5:31.t29 PNI

EA# 0609-21 Page 51 of75

Page 1of1
DAIA FilE G: \GC2OO9Q2\GUMMO\DATA\APRO9\GC1O?PGO74\0218]-402. D

Samp1e Name: qc107pg0?4 #17

Acq. Operator

Acq. fnstrument

Tnjection Date

Acq. Method

Last changed

Analysis Method

Last chanqed

stg

Gummo

27-Apr-09 , 22: 48:,04

Seq. Lj-ne

LocaLion

rnj

Inj Volume

I4

Yial- 2L

2

External

G : \cC2 0 0 9Q2 \GUMMO\METHODS \WAx . M

4/2/2009 10:51:55 AM by kam

G : \GC2 O O 9Q2 \GUMMO\METHODS\ O5 O 9-7 8R. M

5/29/2009 5:31:26 PM

(modified after loading)

pA

14000

1 2000

1 0000

8000

6000

4000

2000

Externaf Standard Report

Sorted By

Cal-ib. Data Modified

Multiplier

Difution

Use Multiplier

Signal 1: FlD2

RetTime Type Area Amt,/Area .Amount Grp Name

lminl [pA*s] [ppm]

I ------ t------- -- t---------- t----------t--l ---------

1.582 PB 2.88351e4 2.19114 8.0482'te4 Methane

Totafs: 8.0482'le

*** End of Report ***

: Signal

: 5/29/2009 5:!2:02 PM

: 1.0000

: l-.0000

& Dilut ion Factor with TSTDs

D

Harpo 5/29/2009 5:31:36 PM

EA#0609-21 Page 52of 75

Page 1of1
Data File G : \cC2 0 0 9Q2 \GUMMO\DATA\APRO 9\cC107PG07 4 \02 181 4 03 . D

Sample Name: qclOlpq)l4 #I7

Acq. Operator

Acq. Instrument

Inj ection Date

Acq. Method

Last changed.

Analysis Method

Last changed

stg

Gummo

21--Apr-09 , 23 :,0 4:08

Seq. T,ine

Location

rnj

74

via:. 2t

3

fnj Volume External

G: \GC2 0 0 9Q2 \GUMMO\METHODS \WAx . M

4/2/2009 10:51:55 AM by kam

G : \GC2 0 0 9Q2 \GUMMO\METHODS\0s 0 9-7 8R. M

5/29/2009 5:31:26 PM

(modified after loadinq)

External Standard Report

pA

14000

12000

I 0000

8000

6000

4000

2000

Sorted By

Calib. Data Modified

Multlplier

Di-lution

Signal

5/29/2009 5:12202 PNj

1.0000

1.0000

Factor with ISTDs

Amt/Area Amount

lppml

| ---------- | ---------- |

2-'l9LI4 8.00023e4

- 8.00023e4

Use Multiplier 10n

Signal 1: FID2

RetTime Type

lmin]

l------l

1.584 PB

Totals :

e Difut

D

Area

lpA* s l

2.86630e4

Grp Name

--t-------

Methane

*** End of Report ***

Harpo 5/29/2009 5:31:42 PM

EA# 0609-21 Page 53 of75

Page 1of1
Data File c : \GC2 00 902 \GUMMo\DATA\ JUNO 9 \cC10 7 PG1 0 6\02 180 1 0 1 . D

Sample Name: qc107pg74 #13

Acq. Operator

Acq. lnstrument

Injection Date

Acq. Method

Last changed

Analysis Method

Last changed

kam

Gummo

04-Jun-09, 09:5'1 :46

Seq. Line

Locatíon

rnj

Inj Volume

1

Vial 21

1

External

G : \GC2 0 0 902 \GUMMo\METHODS \WAX . M

5/12/2009 4:42:20 PM by tbo

G : \GC2 00 9Q2\GUMM0\METHODS \0509-7 BR. M

6/5/2009 10:57:49 AM

A\JUNO9\GC 1 OTPG 1

pA

45

40

ÒE

30

25

20

15

10

5

External Standard Report

Sorted By

Ca1ib. Data Modified

Multiplier

Di lution

Use Multipfier c Dilution

Signal 1: FID2 B,

RetTime Type Area

[mín] [pA*s ]

t------t----------l

1.598 PV 14.98742

Totafs:

S igna 1

5/29/2009 5:50:04 PM

1.0000

1.0000

Factor with ISTDs

Amt/Area Amount

Ippm]

l----------l 2.19267 41.83't28

47.83'128

Grp Name

--t-------

Methane

*** End of Report ***

Gummo Reprocess 6/5/2009 1:04:39 PM

EA#0609-21 Page 54of75

Page Lofl
Data File c : \GC2 009Q2\GUMMO\DATA\JUN09\Gc107PGIO6\02180102. D

Sample Name: gc107pq?4 #13

Acq. Operator

Acq, fnstrument

Inj ection Date

Acq. Method

Last changed

Analysi-s Method

Last chanqed

kam

Gummo

04-Jun-09, 10:13:40

Seq.Line

Location

rnj

1

Vial- 21

2

lnj Volume Externalc: \GC2 0 0 902 \cUMMo\METHODS \WAX . M

5/72/2009 4:42:20 PM by tbo

c : \GC2 0 0 9Q2 \GUMMO\METHODS\ 0 50 9-78R. M

6/5/2009 10:57:49 AM

pA

45

40

35

30

25

20

15

10

5

External Standard Report

Sorted By

Ca1ib. Data Modified

Multiplier

Diluti on

Use Muftiplier c DiÌution

Signal 1: FID2 B,

RetTime Type .Area

lminl [pA*s ]

l------l----------

1.599 PV 74.99452

Totals:

Signal

5/29/2009 5:50:04 PM

1.0000

1.0000

Factor with ISTDs

Ant/Area Amount

lPPml

| ---------- I ----------

2.19267 41.87386

41.87386

Grp Name

t--t------

Methane

*** End of Report ***

Gummo Reprocess 6/5/2009 1:04:49 PM

EA# 0609-21 Page 55 of75

Page 1of1
Data File G: \GC2009Q2\GUMMO\DATA\JUN09\GCl-07PG106\02180103. D

SampIe Name: gc107pg74 #1-3

Acq. 0perator

Acq. ïnstrument

Inj ection Date

Acq. Method

Last changed

Analysis Method

Last chanqed

kan

Gumrno

04-Jun-09, 10:29:33

Seq. line

Locatíon

rnj

lnj Volume

1

VíaI 21

3

Externaf

G: \GC2 0 0 902 \cUMMo\METHODS \i^lAX. M

5/L2/2009 4:,42:20 PM by tbo

G : \GC2 0 0 9Q2 \GUMMO\METHoDS \05 09-7 BR. M

6/5/2009 10:57:49 AM

External Standard Report

Sorted By

Ca1ib. Data Modified

Multiplie r

Difution

Use Multipfier & Dilut

Signal 1: FID2 B,

Signal

5/29/2009 5:50:04 PM

1.0000

1.0000

10n Factor with ISTDs

RetTime Type Area Amt/Area Amount Grp Name

[min] [pA*s ] [ppm]

| ------ | ---------- | ---------- t---------- | -- | ---------

l-.599 PV 14.93088 2.'19262 4I.69621 Methane

Totals : 4I.69627

*** End of Report ***

Gummo Reprocess 6/5/2009 1:04:59 PM

EA# 0609-21 Page 56 of75

Page lofl-
Data FiIe G: \GC2009Q2\GUMMO\DATA\JUNO9\cC107PG106\02180701. D

Sample Name: gc107pg74 #13

Acq. Operator

Acq. Instrument

Inj ection Date

Acq. Method

Last changed

Analysis Method

Last changed

kan

Gummo

04-Jun-09, 17:02:38

Seq. Line

Location

rnj

't

Vial 21

1

Inj Volume Exte rnal

c : \GC2 0 0 9Q2 \GUMMO\METHODS \!fAX. M

5/12/2009 4:42:20 PM by tbo

G : \GC20 0 902 \GUMMO\METHoDS \050 9-7 8R. M

6/5/2009 10:57:49 AM

pA

45

40

35

30

25

20

15

10

5

External Standard Report

Sorted By

Calib. Data Modified

MulLipli e r

Di l-uti on

Use Multiplier c Dílutíon

Signal 1: FID2 B,

RetTíme Type Area

[nin] [pA*s ]

t------t----------

1.599 PV 15.?0?94

Totafs:

Sì-gnal

5/29/2009 5:50:04 PM

1.0000

1.0000

Factor with ISTDs

Amt,/Area Amount

lppnl

| ---------- | ----------

2.'19254 43.8651-0

43.86510

Grp Name

t--t------

Methane

*** End of Report ++*

Gurnmo Reprocess 6/5/2009 1:05:11 PM

EA# 0609-21 Page 57 of75

Paqe 1of1
Data Fil-e G: \GC2009Q2\GUMMO\DATA\JUNO9\GC107PG106\02180702. D

Sample Namer gc107pg74 #13

Acq. Operator

Acq. Instrument

Inj ection Dat.e

Acq. Method

Last changed

Analysis Method

l,ast changed

kam

Gummo

04-'Jun-09, I'1 :I8:25

Seq. Line

Location

lnj

Inj Volume

1

Vial 2l2

External

c : \GC2 0 0 9Q2 \GUMMO\METHODS \llAX. M

5/L2/2009 4:42:20 PM by tbo

G : \GC2 00 9Q2 \cUMMo\METHoDS \0 509-7 BR. M

6/5/2009 10:57:49 AM

External Standard Report

Sorted By

Calib. Data Modified

Multlpl ier

Diluti on

Use Multiplier

Si-gnal 1: FID2

RetTine Type

Imin]

t------

1. 600 PV

Totals:

Signal

5/29/2009 5:50:04 PM

1. 0000

1.0000

Factor wìth ISTDs

Amt./Area Amount

lppnl

t---------- 2.'79254 43.88166

43.88166

Grp Name

t--t------

Methane

& Dilut ron

D

Area

lpA*sl t----------l

15.71387

*** End of Report ***

Gummo Reprocess 6/5/2009 l-:05:19 PM

EA# 0609-21 Page 58 of75

Page 1of1
Data File c: \GC2009Q2\GUMMO\DATA\JUN09\GC107PGIO6\02180703. D

Sample Name: gc107pg74 #13

Acq. Operator

Acq. Instrument

Inj ection Date

Acq. Method

Last changed

Analysis Method

Last chanqed

karn

Gumno

04-Jun-09, 17:34:15

Seq. Line

Location

rnj

Inj Volume

'7

Vial- 27

3

Externaf

G : \GC2 0 0 9Q2 \cUMMo\METHODS \WAX. M

5 / 12 /2009 4:, 42: 2 0 PM by tbo

G : \GC2 0 0 902 \GUMMO\METHODS \ 0509-? BR. M

6/5/2009 L0:57:49 AM

D)

@

6

ñ

pA

45

40

35

30

25

20

15

10

5

External- Standard Report

Sorted By

Calib. Data Modified

Mul tip 1i- e r

Dílution

Use Muftiplier e Dilution

Signal 1: FID2 B,

Ret.Tíme Type Area

[min] [pA*s] i------t----------

1.600 PV 15.69332

Totafs:

S Í gnal

5/29/2009 5:50:04 PM

1. 0000

1.0000

Factor with ISTDs

Amt/Area Amount

Ippm]

| ---------- | ----------

2.79254 43.82429

43.82429

Grp Name

t--t------

Methane

*** End of Report ***

Gummo Reprocess 6/5/2009 1:05:,29 PM

EA# 0609-21 Page 59 of75

Page 1of1
Data FiIe G: \GC200902\GUMMO\DATA\,IUN09\cC107PG107\02180101. D

Sample Name: 9c107p9107 #13

Acq. Operator

Acq. lnstrument

Inj ection Date

Acq. Method

Last changed

Analysis Method

Last changed

kam Seq. Line : L

Gummo Location : ViaI 21 05-Jun-09,76:,05:,23 tnj: 1

Inj Volume : External

G : \cC2 0 0 902 \GUMMC \METHoDS \l^jAX . M

5/72/2009 4:42:20 PM by tbo

G : \GC2 0 0 902 \GUMMo\METHODS \ 050 9-7 BR. M

6/5/2009 1:25:03 PM

(modified after loading)

, lG:\GC2009O2\GUM

dJ

c

G

c

c)

=

-s

aoI, @Jì

@F

180101.D)

o

o

ñ

pA

450

400

350

300

250

200

150

100

50

o

q

@

@@SNOô ññ

@

n

o

+

ONoh@c! @

a?

$

t-.

@

10

External Standard Report

Sorted By : Signal

Calib. Data Modified : 5/29/2009 5:50:04 pM

Multiplier : 1. 0000

Dilutlon : 1.0000

Use Mufti-p1ier & Dilution Factor with ISTDs

Signal 1: FID2 Bf

RetTime Type Area Amt,/Area Amount Grp Name

[min] [pA*s ] tppml

| ------ | ---------- | ---------- | ---------- | -- | ---------

1.599 PV 15.73393 2.19254 43.93764 Methane

Totafs | 43 .931 64

*** End of RePo¡¡ ***

Gummo Reprocess 6/8 /2009 9:08:57 AM

EA# 0609-21 Page 60 of 75

Page 1 of 1
Data FiIe c: \cC2 009Q2\GUMMO\DATA\.IUN09\GC107Pc107\02180102 . D

Sample Name: 9c107p9107 #13

Acq. Operator

Acq. Instrument

Inj ection Date

Acg. Method

Last changed

Analysis Method

Last changed

: kam

: Gummo

: 05-Jun-09, 76:,2I:,23

Seq.Line

T,ocation

rnj

1

VLaI 27

2

Inj Volume Exte rnal

G : \GC2 0 0 9Q2 \GUMMO\METHODS \l/iAX. M

5/12/2009 4:42:20 PM by tbo

G : \cC200 9Q2 \GUMMO\METHoDS \ 0 509-7 BR. M

6/5/2009 'l:25:03 PM

(modified after loadinq)

102

o

s

ñ

pA

450

400

350

300

250

200

'150

100

50

External Standard Report

Sorted By

Ca1ib. Data Modified

MuIti-plier

Dilution

Use Muftiplier & Dilution

Signal L: EID2 Bl

RetTime Type Area

lminl [pA*s ]

r------t----------l

1.597 PV 15.87698

Totals :

Si gnal

5/29/2009 5:50:04 PM

1.0000

1.0000

Factor with ISTDs

Amt,/Area Amount Grp Name

Ippm] t----------l--t-----

2.19253 44.33692 Methane

44.33692

*** End of Report ***

Gummo Reprocess 6/8/2009 9:09:06 AM

EA# 0609-21 Page 61 of75

Page lofL
Data Fife G: \GC2009Q2\GUMMO\DATA\,IUN09\GC107pc107\02180103. D

Sample Name: 9c107p9107 #13

Acq. Operator

Acq. lnstrument

lnj ection Date

Acq. Method

Last changed

AnaJ-ysis Method

Last changed

kam

Gummo

05-Jun-09, 16:37:08

Seq.Line

T,ocation

rnj

1

Vial- 21

3

lnj Volume External

G : \Gc2 0 0 9Q2 \GUMMo\METHoDS \WAX. M

5/72/2009 4:42:20 PM by tbo

G : \GC2 O O 9Q2 \GUMMO\METHODS \05 O9-7 BR. M

6/5/2009 ?:25:03 PM

(modified after loadinq)

pA

450

400

350

300

250

200

'150

'100

50

External Standard Report

Sorted By CalÍb. Data Modified

Multiplier

Dilution

S i gnal

5/29/2009 5:50:04 PM

1.0000

1.0000

Use MuÌtiplier Factor with TSTDs

Signal 1: FID2

& Dilution

D

RetTime Type Area

lmj-nl [pA*s] t------t----------l

1.59? PV 15.73795

Totafs:

Amt/Area

2 .1 9254

Amount

lppml t----------

43.94888

43.94888

Grp Name

l--t------

Methane

*** End of Report ***

Gummo Reprocess 6/B /2009 9: 09: 19 AM

EA#0609-21 Page62of75

Paqe 1of1
Data Fif e c : \GC2 00 9Q2 \GUMMO\DATA\,IUN0 9\cC1 07 PG107 \ 021804 0 1 . D

Sample Name: qc701pgl 4 +13

Acq. Operator

Acq. lnstrument

Inj ection Date

Acq. Method

Last changed

Analysis Method

Last changed

kam Seq. Line ; 4

Gummo Location : Vial 21

05-Jun-09, 20:54:00 Inj : 1

Inj Volume : External

G : \GC2 O O 9Q2 \GUMMO\METHODS \WAX. M

5/72/2009 4:42:20 PM by tbo

G : \GC2 0 0 902 \cUMMo\METHoDS \ 0 5 09-7 8R. M

6/5/2009 7:25:03 PM

(modifi-ed after loadíng)

TA\JU

t-q?

s

pA

450

400

350

300

250

200

150

100

50

0) C

õ

E

(¡)

_o

ø-: |æ

N

N(ì

6

n

\t

ñ

O@eOOo ñôi

e

Ì.- oì

s

s@q

@

@G

External Standard Report

Sorted By : Signal

Ca1ib. Data Modified : 5/29/2009 5:50:04 PM

Multiplier : 1.0000

Di-lution : 1.0000

Use Mul-tj-p1ier c Dilution Factor with TSTDs

Signal 1: FID2 B,

RetTime Type Area A¡nt,/Area Amount Grp Name

[min] [pA*s] [ppn]

| ------ | ----------l ---------- | ---------- | -- I ---------

1.599 PV 15.59427 2.19255 43.54166 Methane

Total-s: 43 .54"t 66

*** End of Report +**

Gummo Reprocess 6/B/2009 9:07:40 AM

EA# 0609-21 Page 63 of75

Page 1 of L
Da ta Fil-e G : \GC2 0 0 9Q2 \GUMMO\DATA\JUNO 9\GC1 07 pG1 O7 \02 180 4 02 . D

Sample Name: gc107pg74 +13

Acq. Operator

Acq. Instrument

Injection Date

Acq. Method

Last changed

Analysís Method

Last changed

kam

Gurnmo

05-Jun-09, 2L:.09:46

Seq. Line

Location

rnj

Inj Vo1ume

4

Vial 21

2

External

G : \GC2 0 0 9Q2 \cUMMo\METHODS \WAX. M

5/12/2009 4:42:20 PM by tbo

G : \GC2 O O 902 \GUMMO\METHODS \O5O 9-7 BR. M

6/5/2009 7:25:03 PM

(nodified after loading)

pA

450

400

350

300

250

200

150

100

50

External Standard Report

Sorted By

Ca1ib. Data Modified

Multiplier

Di luti on

Use Multiplier & Dilution

Signal 1: FID2 B,

RetTime Type Area

lminl [pA*s ]

t------t----------

1.599 PV 15.56863

Totals i

Signal

5/29 /2009 5: 50: 04 PM

1.0000

1.0000

Factor with ISTDs

Amt,/Area Amount

lppml

| ---------- | ----------

2 .7 9256 43 . 4't 626

43 . 41 626

Grp Name

t--t------

Methane

*** End of Report ***

Gummo Reprocess 6/B/2009 9:07:58 AM

EA# 0609-21 Page 64 of 75

Page 1of1
Data File G: \GC200902\GUMMO\DATA\JUN09\GC107PG107\02180403.D

Sample Name: gc107pg?4 +13

Acq. Operator

Acq. Instrument

Inj ection Date

Acq. Method

Last changed

Analysis Method

Last changed

kam

Gummo

05-Jun-09, 21:25:35

Seq. Line

Location

rnj

4

Vial 21

3

Inj Volume ExternaL

c : \cC2 0 0 902 \GUMMO\METHODS \WAX. M

5/72/2009 4:,42:,20 PM by tbo

G : \GC200 9Q2 \GUMMO\METHODS \05 0 9-7 BR. M

6/5/2009 7:25:03 PM

(modified after loading)

, 

(G: TA\JUN09\GC1 07PG 1 07\021 80403.D)

@\t

ñ

pA

450

400

350

300

250

200

150

100

50

4' c

(EE

o

lN- o

,9ooó Ëfì C ol

læN N

f.- N

u?

@tr @

o?

\f

@(o

@

@\t

@

@N

External Standard Report

Sorted By : Signal

Ca1lb. Data Modified : 5/29/2009 5:50:04 PM

MuJ-tiplier 1 1.0000

Dil-ution : 1.0000

Use Multiplier e Dilution Factor with ISTDs

Signal 1: îlDz B,

RetTime Type Area Amt/Area Amount Grp Name

[min] [pA*s] [ppm]

| ------ I ---------- r ---------- | ---------- | -- | ---------

1. 600 PV 15.51795 2.'19256 43.33480 Methane

Totals: 43.33480

*** End of Report ***

Gummo Reprocess 6/B /2009 9: 08 : 08 AM

EA# 0609-21 Page 65 of75

Page 1 of 1
method: G: \GC2 0 0 9Q1\GUMMO\METHODS \I/VAX . M

Modifled on: \/37/2009 at 1:24:1-0 PM

6890 GC METHOD

OVEN

Initial temp: 40 rC (On) Maximum temp: 250 'C Initial time: 4.00 min Equilibration time: 0.20 min

Ramps:

# Rate Final temp Final t.im

1 15.00 10 0.07

2 30.00 200 1.00

3 0.0(off)

Post temp: 50 'C

Post time; 0.00 min

Run time: 11.40 rnin

FRONT INLET (SPlIT/SPLTTLESS) BACK INLET (SPLIT/SPLITLBSS)

Mode: Split Mode: Split

Initial temp: 160'C (On) Ini_tial temp: 160 'C (On)

Pressure: 1.83 psí (On) Pressure: 5.27 psi (On)

Split ratio: 1 ;1 Split ratio: 0. 5: 1

Split ffow: 5.3 mllmin Split flow: 1.0 ml/min

Total ffow: 16. B ml/nin Total flow z 9 .4 ml/min

Gas saver: Off Gas saver: Off

Gas type: Hydrogen Gas type: Hydrogen

COLUMN 1 COLUMN 2

Capillary Column Capillary Cofumn

Model Number: Ä,1fteck EC-Wax Model Number: Restek RTX-1

30m*0.53mm 1.2un

Max temperature: 260 rC Max temperature: 340 'C Nominal length: 30 . 0 n Nominal length: 30 . 0 m

Nominal diameter: 530 . 00 um Nominal diameter : 320. 00 un

Nominal film thickness: 1.20 um Nominal film thickness: 4.00 um

Mode: constant fl-ow Mode: constant flow

f nitial f low: 5.3 ml,/min Tnitial f low: 2 . 1 nl,/min

Nominal init pressure: 1.83 psi Nominal init pressure: 5.28 psi

Average velocÍty: 40 cmlsec Average vefocity:, 40 cm/sec

Inlet: Front Infet Tnlet: Back Infet

Outlet: Front Detector Outfet: Back Detector

Outlet pressure: ambient Outlet pressure: ambient

FRONT DETECTOR (F]D) BACK DETECTOR (FID)

Temperature: 250 tC (On) Temperature: 250 rC (On)

Hydrogen flow: 40.0 mllmín (On) Hydrogen flow: 40.0 mllmin (On)

Air flow: 450.0 ml/min (On) Air flow: 450.0 mtlmin (On)

Mode: Constant makeup flow Mode: Constant makeup flow

Makeup flow: 45.0 ml/min (On) Makeup ffow: 45.0 nllmin (On)

Makeup Gas Type: Nitrogen Makeup Gas Type: Nitrogen

Flame: On Flame: On

El-ectrometer: 0n Electrometer: On

Lit offset : 2 .0 Lit offset : 2 .0

STGNAL 1 SIGNAL 2

Data rate: 20 Hz Data rate: 20 Hz

Type: front detector Type: back detector

Save Data: On Save Data: On

Zero: 0.0 (Off) Zero: 0.0 (Off)

Range: 0 Range: 0

Fast Peaks: Off Fast. Peaks: Off

Gummo 4/1,/2009 11:04:10 AM kam

EA# 0609-21 Page 66 of75

Page I of 2
EA#0609-21 Page 67 of75
Sequence : G: \GC2009Q2\GUMMO\SEQUENCE\GC1OTpGO?4. S

Sequence Table (Front Tnjector):

Method and fnjection fnfo Part:

Line Location SampleName

DataFile LimsÏD

Method lnj SampleType InjVolume

1 Vial 16

2 vía]- 76

3 Vial- 16

4 Viaf 16

5 Vial 4

6 Viaf 3

'7 YíaI 2

I Vial- 1

9 Vial 6

10 Viaf 1

l-1 Vial- 3

72 Vial- 4

13 Vial 1

14 Vial 5

15 Vial- 1

1-6 Vlal- 6

I7 Vial 1

gc10 7p907 4

gctl1pg07 4

gc101pg07 4

gc707pgO1 4

qc1,01p907 4

9c1,07p907 4

gct01pg07 4

Bfank

gc707pg07 4

Bfank

qc1,07p907 4

9cL01pq01 4

Blank

qc1,07p907 4

Bfank

gc107pg07 4

Blank

WAX

VfAX

WAX

VüAX

VüAX

WAX

VüAX

PAUSE

WAX

PAUSE

WAX

VüAX

PAUSE

WAX

PAUSE

!üAX

PAUSE

Method

#1

+2

#3

+4

+13

#72

#11

#1-4

4

3

3

J

3

3

3

1

3

1

3

3

1

3

1

3

1

SampIe

Sample

Sample

Sample

Sample

Sample

Sample

Sample

SampIe

Sample

SampIe

Sample

Sample

SampIe

Sample

Sample

Sample

#15

+16

#r1

#18

Sequence Table (Back Tnjector):

Method and Injectj-on fnfo Part:

l,ine Location SampleName

DataFile LimslD

rnj SampleType InjVolume

1

2

3

4

5

Vial 32

Vial- 32

víal- 32

\IiaI 32

Vial 20

gc707pg07 4

qc1,07p907 4

gc707pg07 4

gcI07pg07 4

gcl07pq07 4

#1

+2

#3

#4

#13

VIAX

VfAX

vÍAx

WAX

WAX

4

3

3

3

3

SampIe

Sample

Sample

Sample

Sample

Harpo 6/I/2009 1,0:42: 14 AM

EA# 0609-21 Page 68 of 75

Page 1-of2
Li-ne l,ocation SampLeName

DataFile LimsfD

rnj

EA#0609-21 Page69of75
SEqUCNCE : G: \GC2OO9Q2\GUMMO\SEQUENCE\GC1O7PGO76. S

Sequence Table (Front Tnjector):

Method and Injection fnfo part:

Line Location SampleName

DataFile LimsfD

Method lnj SampJ-eType fnjVolume

1 Vial 3

2 YiaI 4

3 Vial 4

4 Viaf 5

5 ViaI 13

6 Vial 14

7 Vial 15

B ViaI 13

9 via:. L2

10 vial 11

11 Vial 10

1-2 Vial 9

13 Vial 8

14 Vial 7

1-5 Vial- 16

16 Vial 16

1-'l Vlal 5

18 1'Iiú. 2

19 Vial 1

20 Vial 1

9c107pq076 +15

gc107pg07 6 +1,6

gc107pg07 6 #16

9c107pq076 #16

gcL01pg064 #1 & +5

qcl07pq064 #1 c #5

gic107pg064 #l- c #5

Blank

Blank

VüAX

I/üÄx

vüAx

WAX

WAX

VüAX

WAX

VfAX

VÍAX

WAX

VfAX

WAX

V{AX

WAX

Ï\ÏAX

WAX

WAX

WAX

WAX

PAUSE

3

3

J

a

J

3

a

J

3

3

3

a

J

3

a

J

3

3

3

2

3

3

4

1

Sample

SampJ-e

Sample

Sample

Sample

Sample

SampJ-e

Sample

Sample

Sample

Sample

Sample

Sample

Sample

Sample

Sample

Sample

Sample

SampIe

Sampl-e

Sequence Table (Back lnjector):

Method and Injection fnfo part:

Line Location SampleName

DataFile LimsID

Method rnj SampleType InjVolume

3

3

l_

2

Vial 19 qc|)1pgOl6

Viaf 20 qc1,01p9076

VÍAX

VüAX

#15

#16

Sample

Sample

Harpo 6/1/2009 I0:42:21 AM

EA# 0609-21 Page 70 of75

Page 7of2
Sequence : G: \GC2 OO9Q2\GUMMO\SEOUENCE\GC1O7PG1O5. S

Sequence Table (Front fnjector):

Method and Injection fnfo part:

Line location SampleName

DataFile LimsID

Method rnj SampleType InjVolume

1 Vial

2 ViaI

3 Vlaf

4 Vial5 Vial

6 Vial

7 Vial

I Vial

9 Vial

10 Vial

11 Vial

72 VialN2 Blank

paus e

paus e

qc10?pq106

gc10?p9106

9c107p9106

paus e

i,{AX

WAX

t^TAX

WAX

ü]AX

PAUSE

I^IAX

PAUSE

i¡]AX

WAX

I^ïAX

PAUSE

Method

E

J

1

9

10

11

1

5

1

76

76

76

1

+1

+2

+3

3

3

3

3

3

1

3

1

3

3

3

1

Sample

Sample

Sample

S ampl e

SampIe

SampIe

Sample

Sample

SampIe

S anpl e

SampÌe

S ampJ- e

Sequence Tabl-e (Back Tnjector):

Method and Injection lnfo part:

Line Location SampleName

DataFile LimsID

rnj SanpleType InjVolurne

1 Viaf 21

2 ViaI 7'l

3 Vial 25

4 ViaI 26

5 vial- 2'7

6 Vial 17

7 Vj-aI 2L

B Vial 17

9 Vial 32

10 Vial 32

gc107pg74 #13

N2 Blank

0609-2L Run 1

0609-27 Run 2

0609-2I Run 3

paus e

gc701pg7 4 #1.3

paus e

gc10?p9106 *1

gc107pgL06 #2

I,[AX

I,VAX

t/üAx

I,{AX

Î^iAX

PAÜSE

I,{AX

PAUSE

tVAX

L{AX

EA#0609-21 Page72

3

3

3

3

3

1

3

1

3

3

of 75

Sample

Sample

Sample

Sanple

Sanple

Sample

Sample

Sample

Sample

SampIe

Gummo 6/5/2009 I:06:02 PM kam Page Lof2
Line location SampleName

trA#0609-21 Page 73 ofTS