AAPG 2015 Annual Convention & Exhibition, Denver, Colorado ......kerogen yield and TOC values. The only other unit that shows higher siliceous mudstone content when compared to the

I larrell Shale

Harnett sfia le

Tung Limestone

mown. umerione

Urn•Mom

ppor1.4 Ilnufteene

O rug .A1Khe, Vnl,ey Lamm nilareellus

Onondaga LIMOStOne

iskanv Sandstone

Figure 2. Stratigraphy of Lower and Middle Devonian in Appalachian Basin

(After, Wrightstone, 2009)

c ;

Mdl eel les Snake

Using XRF, SEM and Pyrolysis for an Economic Appraisal of the Marcellus Formation of Western Pennsylvania for Fracking Purposes Presented at: AAPG 2015 Annual Convention & Exhibition, Denver, Colorado, May 31" — June 3rd by Paul Comets; Chuck Stringers; Christian Scheibel; Albert Maende2; Erik Boice3

(1) Halliburton, Houston, TX, United States, (2) Wildcat Technologies, LLC, Humble, TX, United States (3) Noble Energy, Houston, TX, United States

Introduction

An economic appraisal of the Marcellus Formation of Western Pennsylvania and West Virginia (Figure 1) was done for purposes of determining its best

producible hydrocarbons-bearing facies and suitable frac stage placement. The appraisal is comprised of reservoir characterization and a geochemical study of

core and drill cuttings retrieved from a single vertical well. The analyzed well penetrated the Devonian-age Burkett, Tully Limestone, Hamilton and Marcellus

Formations as well as the top portion of the Onondaga Formation (Figure 2).

Figure 1. Marcellus Shale Play in Appalachian Basin

(EIA, 2011)

This economic appraisal seeks to demonstrate that analyses of drilled rock cuttings by using the Advanced Sample Analysis (ASA) methodology is a cost-effective

alternative to generate the essential data required for identifying the best producible hydrocarbons-bearing facies and suitable frac stage placement. ASA

methodology comprises of the use of XRF, SEM-EDX (or EDS) and Pyrolyzer. ASA data can also be correlated with MWD/LWD and wire-line tool responses.

Analyses

LaserStrat° Spectro° XEPOS Ill EDX

Analytical results from X-ray Fluorescence (XRF) provide chemical signatures of over 35 elements of the analyzed rock core or cuttings. These include the major

elements sodium, magnesium, aluminum, silicon, phosphorus, sulfur, potassium, calcium, titanium, manganese, and iron, reported as oxides in weight percent (wt

%). The minor and trace elements including chloride, vanadium, nickel, copper, zinc, arsenic, bromine, rubidium, molybdenum, thorium, and uranium are reported

in parts per million. The concentrations of potassium, thorium and uranium are computed into a theoretical gamma ray response (ChemoGR®) expressed in

American Petroleum Institute (API) equivalent units. This enables a direct comparison with gamma ray responses recorded from down-hole tools. The major

elements are utilized to model the mineralogy of the samples. In addition, some trace elements such as Ba and Zr are also utilized to model minor minerals such as

barite and zircon respectively. The modelled mineralogy is then utilized to calculate a Relative Brittleness Index (RBI) (Buller et cll., 2010), where the RBI represents

an enhancement of Jarvie's (2007) mineralogy based definition of rock brittleness for the Barnett Shale.

LithoSCAN° FEI Wellsite° SEM-EDX (EDS)

The SEM-EDX with QEMSCAN ® analysis provides accurate mineralogical composition of a rock sample through the use of the SEM with Energy Dispersive X-ray and

associated analysis program. Further, SEM-EDX analysis provides accurate porosity determination. In this analysis a 5lim Back Scatter Electron (BSE) resolution

image was used for porosity calculations. The 5µrn resolution enables identification of pore sizes in the micro-pore range of 1 to 62.5pm (Loucks et al. 2012).

HAWK° Pyrolysis and TOC

Pyrolysis instruments analyze suitably ground rock samples by using an initial isotherm to release the free oil of the rock (S1), detectable by a Flame Ionization

Detector (FID), followed by temperature ramping in an inert environment to a suitable maximum temperature that allows for FID recognition of any bitumen and

asphaltene that may be present, as well as measurement of hydrocarbons that are yielded from the break-down of the rock's kerogen component (S2), whose peak

generation temperature is recorded as the Tmax maturity parameter (Dow, 2011). On completion of the pyrolysis cycle, air is passed through the pyrolysis

instrument, while ramping the temperature to a suitable maximum that allows for the rock sample's oxidation products which consist of carbon monoxide and

carbon dioxide to be measured by Infra-Red detectors.

Abstract

An analysis of a core from the Marcellus Formation of Western Pennsylvania was

undertaken using three laboratory instruments; Spectro XEPOS® XRF, FEI Wel!site® SEM

with EDX capability and HAWK pyrolyzer. A fourth parameter that was taken into

consideration was porosity measurements from a PHIE and PHIT neutron emitting tool.

Unexpected relationships emerged from a comparison between the various downhole

curves.

Hydrocarbons that were generated from kerogen pyrolysis (S2) varied greatly in value

with the neutron probe's total porosity. Macroporosity as detected by the SEM

(analyzed greater than 5 microns) showed more agreement when compared to the

Total Organic Carbon (TOC). Macroporosity data varied with the siliceous microfossil

content, particularly radiolaria within the Marcellus Formation, and non-specific shell

hash in the overlying Burkett Formation. According to the analyses there is evidence of

redeposited or transported silica paralleling these zones.

The free oil (S1) showed a similar distribution to the S2 and indicated locations of three

prospective "sweet spots"; Burkett Formation, Upper Marcellus Formation, and Lower

Marcellus Formation. Carbonate horizons indicate low porosity due to the presence of

clay. The SEM images also show the presence in the limestone with extensive

bioturbation, shell fragments, and phosphatic enrichment. Pyrolysis analysis reveals

low TOC values within these horizons as well. The carbonate-rich, relatively oxidizing

paleoenvironment allowed various species of burrowing organisms to thrive. The

remainder of the Marcellus Formation appears to have been deposited under

substantially anoxic conditions and is largely composed of silty clay; the siltiest region is

situated near the base of the formation. The zones of lowest clay content located in the

middle of the Lower Marcellus Transgressive System Tract (TST) also contain the

greatest macroporosity and highest oil content (Si, S2). This TST sequence likely

corresponds to the best of the three prospective sweet spots.

Organic richness is optimal within the Marcellus Formation, ranging between 2 and 12

percent (%) TOC. Based on the analyses, this zone is evidently a source rock; S2 values

reported averaged greater than 5 milligrams hydrocarbons per gram of rock. The

Burkett and Tully Limestone often contains more than 2% TOC. Tmax maturity data

shows the Marcellus Formation is situated in the Condensate/Wet Gas window (Tmax

of 455 — 475 °C). The Lower Marcellus sweet spot shows a relatively low clay and high

silt content making it the best candidate for frac stage placement. This zone shows high

brittleness and elevated hydrocarbons content (S1 and S2). At the base of the Marcellus

and immediately above the Onondaga Limestone there is a very thin zone of extreme

ductility that appears to correspond to a bentonitic ash layer. The combination of

detailed lithological analyses with an appraisal of the hydrocarbons within the

Marcellus and adjacent formations allows zonation in terms of potential economic

productivity and engineering suitability for fracking purposes.

V 1-.N.AL r ec

AAPG 2015 Annual Convention & Exhibition, Denver, Colorado, May 31st — June 3rd www.wildcattechnologies.corn

°Note: Lists olthe mineralogical composition whose sum provided the LiS_Siliceous Mudstone,LiS_Argillaceous

Mudstone and DS_Carbonate analytical results

LiS_Siliceous Mudstone LiS_Argillaceous Mudstone LiS_Carbonate

1.1.11..

The siliceous and argillaceous mudstone

contents of these three formations are plotted

in Figure 4. It is very significant that, as from the

Hamilton Formation down-hole all the way to

the Lower Marcellus HST, the argillaceous

mudstone content is far higher than that of the

siliceous mudstone content. When the Lower

Marcellus TST is penetrated, there is a

crossover and the siliceous mudstone content is

greater than the argillaceous mudstone

content. It is also significant that it is the Lower

Marcellus TST that has the highest free oil,

kerogen yield and TOC values. The only other

unit that shows higher siliceous mudstone

content when compared to the argillaceous

mudstone content is the Burkett Formation. It's

free oil, kerogen yield, and TOC values however,

are lower than those of the Marcellus

Formation. Table 2 shows the summary of

pyrolysis, porosity and mineralogy values for

the studied formations

Figure 4 Siliceous and Argillaceous Mudstone contents

of the Burkett, Hamilton and Marcellus Formations

Using XRF, SEM and Pyrolysis for an Economic Appraisal of the Marcellus Formation of Western Pennsylvania for Fracking Purposes Presented at: AAPG 2015 Annual Convention & Exhibition, Denver, Colorado, May 3151 -June 3rd by Paul Comets; Chuck Stringers; Christian Scheibel; Albert Maende2; Erik Boice3

(1) Halliburton, Houston, TX, United States, (2) Wildcat Technologies, LLC, Humble, TX, United States (3) Noble Energy, Houston, TX, United States

Results The XRF, SEM, Pyrolysis and TOC analytical results for the Burkett, Tully, Hamilton, Marcellus, Upper Marcellus (U.M.) Transition Stand Track (TST), Lower Marcellus (L.M.) High Stand Track (HST) and Lower Marcellus Transition Stand Track (TST) are

summarized in Table 1 whereby the mean value for S1, S2, Tmax, TOC, OSI (Jarvie and Baker, 1984), HI, Porosity, Siliceous Mudstone, Argillaceous Mudstone and Carbonate contents are displayed. Maturity wise, a Tmax of less than 430°C is deemed to

indicate immaturity (Peters, 1986) while the Oil window is delineated by a 430 to 455° C range with the Condensate/Wet Gas zone falling within the 455 to 475° C range (Jarvie, 2012). The Dry Gas to Post Mature zone is at temperatures greater than 475° C.

Table 1. Mean 51, S2, Tmax, TOC, OSI, HI, Porosity, Siliceous Mudstone, Argillaceous Mudstone and Carbonate contents for the Burkett, Tully, Hamilton, Marcellus, Upper Marcellus (U.M.) TST, Lower Marcellus (L.M.) HST and Lower Marcellus TST

Formation

"Er

Dep. ift) Corrected

illr Sl-f ree Oil

(ingHC/g

rack)

)Se- ImPHC/13

rock)

, S' !r:', "n

Maturity

TOC (Total

Organic

Carbon)

(wt. %)

Oil Oil

Saturation

Index

151/TOC x

1001

HI

Hydrogen

Index

(52/TOC a

1001 mg

Hug TOC

Mr

LisPorosity

' -

LiS_Siliceous

Mudstone.

. Argillaceous

Mudstone .

1=

. .

'S-Csr'nste

Burkett_rnea n 6246.756275.8 5.00 6.41 470 7.16 70 89 66.92 32.78 0.34

Tully 6260.45 2.5 2.89 071 3.37 74 86 19.7 77.9 2.3

Ha mnItonnlea n 6280.25-6302.05 1.63 2.19 066 2.33 66 67 16.27 43 00.63

Ma rtes I usrnea n 6320.4-6327.7 4.42 5.51 463 6.12 78 85 1.08 20.4 62.86 15.52

U. M TST_mea n 6329 5-633 5 6.35 867 458 9.16 69 94 1.5 19.73 76.53 2.07

L.M HST_nlea n 6354.656356.5 9.6 4.36 066 5.97 159 73 1.1 19.05 79.15 0.65

L M TST_Inea n 6359.356373.2 8.72 10.93 060 11.75 81 90 4.57 02.61 4107 11.69

Ononda ga_rnea n 6375.7-6378.9 2.36 5.21 430 5.33 45 144

Hunters, I I e_nlea n 6381.6 0.13 0.17 331 0.49 27 35

From Table 1, it can be seen that all the represented formations, except for the Huntersville, have a TOC of

at least 2%, which happens to be what is considered to be the minimum TOC required for a viable shale

oil or shale gas resource system. The Lower Marcellus (L.M.) TST not only contains the highest TOC but also the highest porosity, S1 and S2 values. Therefore, it appears to have the greatest free oil content as

well as the greatest kerogen generation potential while the second in rank for these TOC, 51 and 52

parameters is the Upper Marcellus (U.M.) 1ST. The data identifies the Lower Marcellus TST and the

Burkett as containing a siliceous mudstone content exceeding 40% (by weight). All of the formations are

within the Condensate/Wet Gas zone. The maturity data for the Onondaga and Huntersville samples are

not indicative of these formation's actual maturity due to their very low yield of hydrocarbons from

kerogen (S2 parameter) which makes their Tmax maturity measurement to be unreliable. Fr“. MI. P.m 71.K DK and PermAy M SlAntHornlhon end %Want Fennitrent

Figure 3. Free oil (51), kerogen yield

(S2), TOC and porosity of the Burkett, Hamilton and Marcellus Formations

The free oil (S1), kerogen yield (52), TOC and porosity of the Burkett, Hamilton and Marcellus Formations are plotted in Figure 3 where it is evident that these three parameters parallel each other

but are at their highest within the Lower Marcellus TST. Figure 3 also shows a gradual reduction trend in S1 values in conjunction with sudden increase in porosity as the Lower Marcellus TST is

drilled deeper. Evidently this S1 trend shows free oil within macropores of the Lower Marcellus TST migrating downward to the Onondaga Formation. This migration is attributed to the down-hole

increasing content of siliceous radiolaria that, in turn, created increased porosity through diagenesis.

Table 2. Summary of pyrolysis, porosity and mineralogy values for the

Burkett, Tully, Hamilton, Marcellus, Upper Marcellus (U.M.) TST,

Lower Marcellus (L.M.) HST and Lower Marcellus TST.

lir Depth (k) Corrected

ilr 51-Free Oil

(mgHC/6 rock)

2Perogen

Yield

(mgHC/6 rock)

llr 53

(mgCO2/3 rock)

Tmax-

Maturity

(( 'C)

TOC

(Total

Organic Carbon) (wt %)

Production

Index

(51/51+52)

051

Oil Saturation

Index

(51/TOC x 100)

HI

Hydrogen

Index

(52/TOC x

100) mg HC/g TOC

1

Oxy

0

gen

Index

(S3/TOC

x100)

mg

CO23

,is2or,6i,

TOC

LiS_Siliceous

Mudstone.

LiS_Argillaceous

Mudstone* LiS Carbonate*

j

0.34

Formation

L AIL Burkett_mean 6246.75-6275.8 5.00 6.41 0.18 470 7.16 0.44 70 89 2 66.92 32.78

Range for 6 samples 4.05-6.24 5.37-7.69 0.13-0.22 468-473 6.28-8.20 0.39-0.49 61-83 85-94 2-3 52-80 19-38 0.1-0.5

Tully 6260.45 2.5 2.89 0.15 471 3.37 0.46 74 86 4 19.7 77.9 2.3

Hamilton_mean 6284.25-6302.05 1.63 2.19 0.23 466 2.33 0.51 66 67 26 16.27 43 40.63

Range for 3 samples 0.25-3.89 0.21-5.86 0.22-0.26 464-467 0.53-5.54 0.40-0.60 47-82 40-106 'l 4-49 15.3-16.9 28.4-55.2 27.9-56.1

Marcel I us_mean 6320.4-6327.7 4.42 5.51 0.208 463 6.12 0.48 78 85 7 1.08 20.4 62.86 15.52

Range for 6 samples 1.33-7.56 1.11-9.89 0.16-0.25 461-466 1.44-10.65 0.42-0.55 66-92 73-89 2-16 0.1-2.5 10.8-30.7 33.4-85.3 2.5-51.3

U.M.TST mean 6329.5-633.5 6.35 8.665 0.2075 458 9.16 0.42 69 94 2 1.5 19.73 76.53 2.07

Range for 4 samples 4.08-8.06 5.73-9.97 0.16-0.27 457-459 6.4410.26 0.40.0.46 63-79 8997 2-3 0.7-2.1 18.8-20.9 75.8-77.4 1.2-2.1

L.M HST_mear 6354.65-6356.5 9.6 4.355 0.13 466 5.97 0.68 159 73 2 1.1 19.05 79.15 0.65

Range for 2 samples 7.33-11.87 3.97-4.74 0.12-0.14 464468 5.36-6.58 0.65-0.71 137-180 72-74 2-3 0.8-1.4 18.419.7 77.9-80.4 0.40.9

L.M. TST_mear 6359.35-6373.2 8.72 10.93 0.16 464 11.75 0.45 81 90 2 4.57 42.61 41.07 11.69

Range for 9 samples 1.9-12.04 2.37-17.16 0.11-0.21 456-486 3.11-17.32 0.33-0.72 31-101 73-101 1-7 0.2-11.1 13.458.6 1.480.7 0.6-65.6

Onondaga_mean 6375.7-6378.9 2.36 5.21 0.24 430 5.33 0.28 45 144 34

Range for 3 samples 0.17-6.56 0.32-13.37 0.17-0.34 385-455 0.39-14.85 0.16-0.35 44-49 82-261 ' 1-54

Hunte rsyl I le mean 6381.6 0.13 0.17 0.27 331 0.49 0.43 27 35 55

1-.N.AL r

AAPG 2015 Annual Convention & Exhibition, Denver, Colorado, May 315t - June 3rd www.wildcattechnologies.com

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Using XRF, SEM and Pyrolysis for an Economic Appraisal of the Marcellus Formation of Western Pennsylvania for Fracking Purposes Presented at: AAPG 2015 Annual Convention & Exhibition, Denver, Colorado, May 31" -June 3 rd by Paul Comets; Chuck Stringers; Christian Scheibe'; Albert Maende2; Erik Boice3

(1) Halliburton, Houston, TX, United States, (2) Wildcat Technologies, LLC, Humble, TX, United States (3) Noble Energy, Houston, TX, United States

Illustrated here (Figure 5) are core images, mineralogy

and porosity of samples from the Burkett, Tully,

Hamilton, Marcellus, Upper Marcellus TST, Lower

Marcellus HST and Lower Marcellus TST together with

the pertinent comments rating their prospective

hydrocarbon zones.

Figure 5. Core images, mineralogy and porosity of

samples from the Burkett, Tully, Hamilton, Marcellus,

Upper Marcellus TST, Lower Marcellus HST and Lower

Marcellus TST together with the pertinent comments

rating their hydrocarbons prospectivity. *Note:

Formations core images, mineralogy and porosity

analyses by Halliburton's LithoSCAN®.

Figure 6 is a chart of the geochemical and mineralogical characterization of the well bore XRF,

SEM-EDX and pyrolysis results. As illustrated by the data, the ASA profile provides, among other

things, in-depth formation information about structural behavior and mineralogical content as

well as potential hydrocarbon zones. This information also aids in further division of the

recognized formation into chemostratigraphic units based on the rock behavior and content. For

instance, the illustration of the brittleness in the RBI column reveals rock mechanics based on

mineralogy within the respective formations that could conceivably accept efficient frac stage

placement (red). Areas in green are characterized as highly ductile and are at risk for problems

associated with frac stage placement in clay-rich formation zones.

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and pyrolysis results

Acknowledgements We are grateful to Noble Energy, Halliburton and Wildcat

Technologies for allowing the publication of this study.

We also wish to thank AAPG for giving us this opportunity to

make our presentation.

Conclusions

In conclusion, an appraisal of the Marcellus Formation of Western Pennsylvania and West Virginia was performed for purposes of determining its best

producible hydrocarbons-bearing facies and suitable landing zone. This appraisal was motivated by the need to understand the peculiar geological,

geochemical and petrophysical properties of unconventional resource systems using a more economical method that can "ground truth" data obtained

by down-hole tools and other sources. In these systems the organic-rich source rock that is usually a shale, either simultaneously serves as the reservoir

or is part of a source-reservoir hybrid system, that consists of a variety of combinations of interbedded shale, limestone, dolomite, siltstone and

sandstone rocks. At this time, a limited suite of MWD/LWD tools was employed while drilling in these systems. The same was true for wire-line logging

after the well was drilled. This economic appraisal effectively demonstrates that analyses of drilled rock cuttings by using the Advanced Sample Analysis

(ASA) methodology is an economical alternative for generating the data required for identifying the best producible hydrocarbons-bearing facies and

suitable frac stage placement.

References Buller, D. Hughes, S.N., Market, J., Petre, E., Spain, D. and Odumosu, T.; 2010. Petrophysical Evaluation for Enhancing Hydraulic Stimulation in Horizontal Shale Gas Wells. SPE

Annual Technical Conference and Exhibition, Florence, Italy, 19-22 September 2010, SPE-132990.

Dow, W. G., 2011, How Plant and Animal Remains Become Oil and Gas: A Geochemical Perspective, AAPG Search and Discovery Article # 40830. Web accessed November 20,

2013: http://www.searchanddiscovery.com/documents/2011/40830dow/ndx dow.pdf?q=%2BauthorStrip%3Adow+-isMeetingAbstract%3Amtgabsyes

EIA, 2011. Marcellus Shale Gas Play, Appalachian Basin. (http://www.eia.doe.gov/oil-gas/rpd/shaleusa5.pdf (accessed March 27, 2015))

Jarvie, D.M., 2012, Shale resource systems for oil and gas: Part 2-Shale-oil resource systems, in J. A. Breyer, ed., Shale reservoirs-Giant resources for the 21st century: AAPG

Memoir 97, p. 89-119.

Jarvie, D.M., 2007, Unconventional shale-gas systems: The Mississippian Barnett Shale of north-central Texas as one model for thermogenetic shale-gas assessment. AAPG

Bulletin, 91/4, p.475-499.

Jarvie, D.M. & Baker, D.R.; 1984. Application of the Rock-Eval III oil show analyzer to the study of gaseous hydrocarbons in an Oklahoma gas well: 187th ACS National Meeting,

St. Louis, Missouri, April 8-13, 1984. Web accessed February 15, 2015: http://wwgeochem.com/references/JarvieandBaker1984 ApplicationofRock-

Evalforfindingbypassedpayzones.pdf.

Loucks, R.G., Reed, R.M., Ruppel, S.C. and Hammes, U.; 2012. Spectrum of pore types and networks in Mudrocks and a descriptive classification for matrix-related mudrock

pores. AAPG Bulletin, 96/6, p.1071-1098.

Peters, K. E., 1986, Guidelines for Evaluating Petroleum Source Rock Using Programmed Pyrolysis, AAPG Bull. v. 70, No. 3, p. 318-329.

Wrightstone, g., 2009, Marcellus Shale - Geologic Controls on Production: Search and Discovery Article # 10206 (2009), AAPG.

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