COGEL-02456; No of Pages 10

International Journal of Coal Geology xxx (2015) xxx–xxx

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International Journal of Coal Geology

journal homepage: www.elsevier.com/locate/ijcoalgeo

Characterization of organic matter fractions in an unconventional tight

gas siltstone reservoir
Hamed Sanei a,b,⁎, James M. Wood c, Omid H. Ardakani a, Christopher R. Clarkson b, Chunqing Jiang a
a
Geological Survey of Canada, Calgary, AB, Canada
b
Department of Geosciences, University of Calgary, Calgary, AB, Canada
c
Encana Corporation, Calgary, AB, Canada

a r t i c l e i n f o a b s t r a c t

Article history: This paper on core samples collected from the Triassic Montney Formation tight gas reservoir in the Western
Received 16 January 2015 Canadian Sedimentary Basin (WCSB) illustrates that operationally-defined S1 and S2 hydrocarbon peaks from
Received in revised form 7 April 2015 conventional Rock–Eval analysis may not adequately characterize the organic constituents of unconventional
Accepted 8 April 2015
reservoir rocks. Modification of the thermal recipe for Rock–Eval analysis in conjunction with manual peak integra-
Available online xxxx
tion provides important information with significance for the evaluation of reservoir quality. An adapted method of
Keywords:
the analysis, herein called the extended slow heating (ESH) cycle, was developed in which the heating rate was
Rock–Eval slowed to 10 °C per minute over an extended temperature range (from 150 to 650 °C). For Montney core samples
Reservoir characterization within the wet gas window, this method provided quantitative distinctions between major organic matter (OM)
Tight gas components of the rock. We show that the traditional S1 and S2 peaks can now be quantitatively divided into
Solid bitumen three components: (S1ESH) free light oil (S2aESH) fluid-like hydrocarbon residue (FHR), and (S2bESH + residual
Montney Formation carbon) solid bitumen (more refractory, consolidated bitumen/pyrobitumen).
The majority of the total organic carbon (TOC) in the studied Montney core samples consists of solid bitumen that
represents a former liquid oil phase which migrated into the larger paleo-intergranular pore spaces. Physicochem-
ical changes to the oil led to the precipitation of asphaltene aggregates. Subsequent diagenetic and thermal cracking
processes further consolidated these asphaltene aggregates into “lumps” of solid bitumen (or pyrobitumen at
higher thermal maturity). Solid bitumen obstructs porosity and hinders fluid flow, and thus shows strong negative
correlations with reservoir qualities such as porosity and pore throat size.
Although the FHR fraction constitutes a small portion of the total rock mass and volume in Montney samples it has
important implications for reservoir quality. This fraction represents a thin film of condensed, heavy molecular hy-
drocarbon residue covering surfaces of the present-time pore spaces and may represent the lighter component of
the paleo-oil that migrated into tight interstices in the Montney reservoir. The FHR fraction potentially plays an im-
portant role in wettability alteration by creating hydrophobic matrix pore networks in portions of the reservoir that
were not already filled with solid bitumen.
Crown Copyright © 2015 Published by Elsevier B.V. All rights reserved.

1. Introduction a dominant control on reservoir quality in many shale formations

The total organic carbon (TOC) content of unconventional tight gas
and shale gas plays is regarded as an important attribute for assessment
of reservoir quality and hydrocarbon productivity. TOC has positive cor-
relations with porosity and permeability in many known self-sourced
unconventional plays (Jarvie et al., 2007; Passey et al., 2010). These
positive correlations have led to a perception that organic porosity is
⁎ Corresponding author. Tel.: +1 403 292 7045.
E-mail addresses: hsanei@nrcan.gc.ca (H. Sanei), james.wood@encana.com (J.M. Wood),
ohaeriar@nrcan.gc.ca (O.H. Ardakani), clarksoc@ucalgary.ca (C.R. Clarkson),
Dennis.Jiang@NRCan-RNCan.gc.ca (C. Jiang).
(e.g., Barnett, Doig and Eagle Ford) and the primary storage mechanism
for hydrocarbons in organic-rich mudstones (Jarvie et al., 2006).
The present-day TOC content of rock samples is commonly measured
with total carbon analysers (LECO) after removal of mineral carbon (de-
carbonation by use of HCl) or with thermally programmed Rock–Eval
analysis. The bulk measurement of TOC combines various fractions of or-
ganic matter (OM) in a given sample. These OM fractions have unique
physical and chemical properties and may play different roles in the
source and reservoir quality of an unconventional petroleum rock. This
study applies a modified Rock–Eval procedure to/constitutes a small por-
tion of the quantify the amounts of various OM fractions within samples
from the Triassic Montney Formation of northeast British Columbia. The
new geochemical parameters developed in this study are integrated

http://dx.doi.org/10.1016/j.coal.2015.04.004
0166-5162/Crown Copyright © 2015 Published by Elsevier B.V. All rights reserved.

Please cite this article as: Sanei, H., et al., Characterization of organic matter fractions in an unconventional tight gas siltstone reservoir, Int. J. Coal
Geol. (2015), http://dx.doi.org/10.1016/j.coal.2015.04.004
2 H. Sanei et al. / International Journal of Coal Geology xxx (2015) xxx–xxx

with petrographic observations and various rock property measurements 3. Methodology

to provide insights into the role of OM on reservoir quality in the Montney
tight gas fairway. 3.1. Porosity and pore throat size

Porosity and pore throat size measurements were determined on 18

2. Study area
The Montney Formation is an Early Triassic tight gas reservoir up
to 320 m thick which is located to the northeast of the Cordilleran
deformation belt in the Western Canadian Sedimentary Basin
(WCSB) (Kuppe et al., 2012; National Energy Board, 2013; Wood,
2013). The Montney Formation is mainly composed of siltstone and
was deposited predominantly in lower shore face to offshore envi-
ronments (Davies et al., 1997; Edwards et al., 1994; Wood, 2013)
(Fig. 1a–b).
Core samples for this study were collected from one well in north-
eastern British Columbia: ECA CRP HZ Sunrise 03-21-080-17 W6. Drill
cores were recovered from both the Upper and Lower sections of the
Montney Formation at depths between 2126.50 and 2347.28 m. Studied
samples vary from medium (mean = 21 μm) to coarse-grained
(mean = 48 μm) siltstone in the lower and upper Montney interval, re-
spectively (Table 1).
core samples from the studied well. Porosity was measured on one-
inch-diameter plugs at ambient conditions by use of the Boyle's Law
method with helium as the gaseous medium. Samples were cleaned
with toluene and methanol, and then oven-dried at 100 °C for 24 h
prior to porosity measurement. Pore throat size distributions were gen-
erated from mercury injection capillary pressure measurements con-
ducted following established methods (Purcell, 1949) and by use of
the Washburn equation (Washburn, 1921).
3.2. Rock–Eval analysis
Dry samples weighing 50 to 70 mg were finely ground and their TOC
contents measured using the standard cycle of Rock–Eval 6® (Vinci
Technologies, France) analysis (Lafargue et al., 1998). The pyrolysis por-
tion of the standard cycle used an iso-temperature of 300 °C for 3 min
followed by increasing temperature at a rate of 25 °C per minute up to
650 °C. The amount of hydrocarbon (mg HC/g Rock) released during

Fig. 1. (a) Map of distribution of preserved Triassic strata in the subsurface of western Canada and approximate location of the studied well. (b) Stratigraphic column of Permian, Triassic
and Jurassic strata in the WCSB (modified after Davies, 1997).

Please cite this article as: Sanei, H., et al., Characterization of organic matter fractions in an unconventional tight gas siltstone reservoir, Int. J. Coal
Geol. (2015), http://dx.doi.org/10.1016/j.coal.2015.04.004
 H. Sanei et al. / International Journal of Coal Geology xxx (2015) xxx–xxx 3

Table 1
Rock–Eval-6 (standard cycle) and reservoir quality data for Montney samples from the Sunrise 03-21-080-17 W6 core (UWI: 02-15-080-17 W6/2), British Columbia.

Depth Sample TOCa PC RC RC/TOC S1 S2 S3 Tmax HIb OIc PId MinCe Median Ambient average
quantity pore throat Core grain
size Porosity size

m mg wt.% wt.% wt.% % mgHC/g mgHC/g mgCO2/g °C mgHC/TOC mgCO2/TOC wt.% mm % mm

Upper 2130.5 70.3 0.43 0.03 0.40 93% 0.15 0.13 0.19 435 30 44 0.54 4.25 0.020 6.1 40
Montney 2133.0 70.2 0.78 0.07 0.71 91% 0.37 0.26 0.28 441 33 36 0.59 2.74 0.027 6.3 50
2134.5 70.6 1.08 0.09 0.99 92% 0.47 0.50 0.23 446 46 21 0.48 2.49 0.010 5.2 50
2138.9 70.8 1.03 0.06 0.97 94% 0.32 0.23 0.24 440 22 23 0.58 2.30 0.063 8.0 60
2140.0 71.1 0.63 0.03 0.60 95% 0.19 0.10 0.24 433 16 38 0.66 2.78 0.070 8.2 60
2141.5 70.6 0.88 0.04 0.84 95% 0.25 0.15 0.24 436 17 27 0.63 3.05 0.043 7.2 50
2148.2 70.6 0.65 0.04 0.61 94% 0.25 0.19 0.20 440 29 31 0.57 2.75 0.025 6.6 50
2149.5 70.5 1.41 0.09 1.32 94% 0.44 0.49 0.20 458 35 14 0.47 2.25 0.016 6.2 50
2155.3 70.1 1.40 0.10 1.30 93% 0.53 0.54 0.17 457 39 12 0.50 2.54 0.008 5.1 40
2158.1 70.5 1.04 0.09 0.95 91% 0.45 0.41 0.34 450 39 33 0.52 8.41 0.018 5.6 40
2160.9 70.8 1.22 0.09 1.13 93% 0.38 0.50 0.27 451 41 22 0.43 5.74 0.011 4.7 40
Lower 2326.3 70.6 1.33 0.07 1.26 95% 0.38 0.40 0.15 445 30 11 0.49 1.43 0.001 3.9 20
Montney 2335.3 70.2 0.99 0.06 0.93 94% 0.37 0.25 0.10 447 25 10 0.60 1.58 0.004 4.7 30
2337.4 70.5 1.49 0.08 1.41 95% 0.42 0.47 0.11 451 32 7 0.47 1.51 0.001 4.5 20
2340.4 71.0 1.68 0.09 1.59 95% 0.49 0.56 0.12 451 33 7 0.47 1.48 0.002 4.7 20
2344.0 70.2 0.71 0.06 0.65 92% 0.45 0.26 0.13 446 37 18 0.63 6.77 0.011 4.2 20
2345.5 69.7 1.16 0.08 1.08 93% 0.56 0.33 0.10 446 28 9 0.63 1.55 0.009 5.6 20
2348.3 70.6 0.96 0.06 0.90 94% 0.44 0.25 0.11 443 26 11 0.64 1.56 0.004 4.4 20
a
Total organic carbon.
b
Hydrogen index = (S2 × 100/TOC).
c
Oxygen index = (S3 × 100/TOC).
d
Production index = (S1/(S1 + S2)).
e
Mineral carbon.

the “pyrolysis stage” of Rock–Eval analysis is measured under S1 and S2
peaks. Simultaneously, the amount of CO and CO2 released during pyrol-
ysis and then oxidation was measured to quantify the portion of
oxygen-containing OM (S3 peak; mg CO2/g Rock) and refractory inert
carbon (residual carbon; RC wt.%), respectively. Mineral carbon was ob-
tained as the sum of the CO and CO2 released during both pyrolysis and
oxidation, at a higher temperature range.
A subset of samples (n = 6) were then analyzed under a manually
devised Rock–Eval pyrolysis cycle, which is hereafter called the extend-
ed slow heating temperature (ESH) cycle. The ESH cycle is similar to the
modified Rock–Eval procedure, proposed by Jones and Tobey (1999)
(also see Jones et al., 2007) for assessment of reservoir quality from re-
sidual hydrocarbon staining oncore and drill cuttings. Both methods
propose a modified thermal recipe to describe reservoir composition
from an altered distillation and nonisothermal program. The ESH cycle
extended the minimum initial iso-temperature to 150 °C for 10 min to
allow volatilization of free hydrocarbons from the sample. This was
followed by a slow heating temperature increase of 10 °C per minute
until the maximum temperature of 650 °C was reached. The maximum
temperature was not extended beyond 650 °C to prevent the
Boudouard reaction between ~230 and 1920 °C (Lafargue et al., 1998).
Comparison of the TOC contents measured in the standard Rock–
Eval cycle and the ESH cycle showed excellent reproducibility standard
deviation (RSD) of generally less than 1% RSD with an exception of one
sample (RSD b 5.9%). The ESH cycle allowed detection of hydrocarbons
over a longer period of time. The resulting FID pyrograms were manual-
ly integrated using Rockint® software (Vinci Technologies, France) to
allow detailed analysis of the evolved peaks.
3.3. Online thermal desorption/pyrolysis–gas chromatography–mass
spectrometry/flame ionization detection (TD/Py–GC–MS/FID) analysis
To characterize the composition of hydrocarbons released in
Montney core samples as observed under Rock–Eval peaks, selected
Montney core samples were subjected to TD/Py–GC–MS/FID analysis
using a Frontier EGA/PY-3030D pyrolyzer interfaced to an Agilent GC–
MSD/FID dual detection system. The system was operated such that vol-
atile and semi-volatile hydrocarbon components released from any
given temperature range (thermal desorption and/or pyrolysis) were
analyzed online for their molecular composition. Powdered Montney
core sample (60 mg) was subjected to two stages of sequential TD–
GC–MS/FID analysis to fingerprint the free hydrocarbons, and then
followed by Py–GC–MS/FID analysis to characterize the solid organic
matter in the core. The sequential thermal desorption analysis was car-
ried out at temperature combinations of 150 °C then 380 °C, or 300 °C
then 380 °C for a duration of 3 min at each stage to observe the light-
medium and heavy hydrocarbons, respectively. Pyrolysis was conduct-
ed at 650 °C for 0.4 min after the previous sequential steps of thermal
desorption to remove the volatile components.
In both thermal desorption and pyrolysis modes, the volatile and
semi-volatile hydrocarbons thermally released from the rock samples
in the pyrolyzer furnace were immediately carried away from the pyro-
lyzer by a flow of helium carrier gas and then cryo-trapped at −186 °C
at the head of the capillary column of the GC–MSD/FID system. Upon the
completion of thermal desorption or pyrolysis, the GC–MS/FID analysis
was immediately initiated with the cryo-trapped hydrocarbons being
instantly released into the GC column for molecular level separation
based on their boiling points. The capillary column used for GC analysis
was a PONA 50 m × 0.20 mm × 0.5um, and helium was used as carrier
gas at a constant flow rate of 1 mL/min. The GC oven temperature was
initially held at 33 °C for 10 min, and then raised to 63 °C at a rate of
3 °C/min, then at 6 °C/min to the final temperature of 325 °C where it
was held for 35 min. The effluents from the GC column were split at
the column end and fed into both MSD and FID detectors for dual detec-
tion, with the former being for compound identification and the latter
for quantification. Compound identification was based on comparison
of GC retention time and mass spectra with those in the published
literature.
3.4. Organic petrology
Organic petrology was carried out on selected samples using
polished blocks made with a cold-setting epoxy–resin mixture. The
resulting sample pellets were ground and polished in final preparation
for microscopy using an incident light Zeiss Axioimager II microscope
system equipped with fluorescent light sources and the Diskus–Fossil

Please cite this article as: Sanei, H., et al., Characterization of organic matter fractions in an unconventional tight gas siltstone reservoir, Int. J. Coal
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4 H. Sanei et al. / International Journal of Coal Geology xxx (2015) xxx–xxx

system for reflectance measurements. Random reflectance measure-

ments were conducted under oil immersion by use of an ultra-fine
a
pixel size (0.3 μm) probe. The goal was to conduct more than 100 reli-
able measurements on each sample to construct a robust reflectance
histogram. In some organically lean samples, the number of measure-
ments was lower because only reliable organic particles with well- Solid Bitumen
polished surfaces were measured (Sanei et al., 2015). The measured
bitumen reflectance values were converted to the equivalent vitrinite
(random) reflectance values (%VRoeqv.) using the Bertrand and Malo re-
lationship (2001; VReqv = (RB + 0.03)/0.96).

4. Results and discussion FHR

The results of the standard Rock–Eval analysis show that the TOC
values range from 0.43 to 1.68 wt.% (mean = 1.05, Table 1). S1 represents 50µm
free light hydrocarbons, which ranges from 0.15 to 0.56 mg HC/g
(Table 1). Thermal maturity, as measured by bitumen reflectance, for
the whole core ranges from 1.25 to 1.47%VRoeqv. (median = 1.32%,
Table 2), which is approximately at the wet gas maturity window
b
(Tissot and Welte, 1984). This thermal maturity represents over 90% of
the transformation ratio and is consistent with the low S2 values
(b2 mg HC/g Rock) of the measured samples (Bordenave, 1993).
The TOC content of mudstones consists predominantly of the un-
extractable OM and includes reactive or generative OM/kerogen (Jarvie,
1991) as well as residual carbon (non-generative or inert OM; Cooles
et al., 1986; Jarvie, 1991). The relative proportion of residual carbon
FHR
(RC) to kerogen increases with thermal maturity due to progressive con-
version of pyrolysable carbon (PC) to hydrocarbon. The total weight con-
Solid Bitumen
centration of RC in rock depends on original hydrogen content (Jarvie,
1991). In most immature source rock mudstones, kerogen consists pri-
marily of the originally deposited and preserved biomass (primary kero-
gen) which has further potential to thermally crack and generate free 50µm
hydrocarbons (Tissot and Welte, 1984). However, the residual carbon
(RC) does not have potential to generate significant amounts of hydrocar-
bons. The RC fraction in mudstones can be originated from several Fig. 2. Photomicrograph (oil immersion, white incident light, 50× objective,) showing an
sources including (i) input of reworked, detrital, dead carbon at the interconnected, intergranular network of two major fractions of hydrocarbon: (i) Low
time of deposition (primary inertinite), (ii) post-depositional diagenetic reflecting, brown, amorphous, degraded fluid-like hydrocarbon residue (FHR). This frac-
tion shows a very poor polishable surface, with VRoeqv. values below 0.6%. It covers a sig-
degradation of primary kerogen or migrated oil, and (iii) thermal crack-
nificant portion of the tight intergranular pore spaces of the rocks. (ii) Solid bitumen with
ing of kerogen or migrated oil at the onset of the oil window. a good-quality polishable surface, on which the reflectance measurements were made.
RC constitutes 91 to 95% of TOC (Table 1) in the studied Montney The majority of these macerals show VRoeqv. values of approximately 1.27%, placing the
samples, suggesting only 5 to 9% of TOC in the samples has further poten- samples in the wet gas window.
tial to decompose (PC). Organic petrographic analysis of the Montney
samples shows no evidence of primary inertinite macerals and suggests
that the relative proportion of RC in the Montney is predominantly con- mostly as thin films within the interstices (Fig. 2), and (ii) solid bitumen
trolled by diagenetic and thermal decomposition of migrated oil. which is present as lump accumulations of consolidated migrabitumen
Petrographic results show that present-day TOC in the Montney sam- (sensu Jacob, 1989) with bitumen reflectance (BRo) ranging from 1.16
ples consists almost entirely of a pervasive intergranular network of to 1.38% (1.25 to 1.47%VRoeqv.; Table 2, Fig. 2). The pervasive nature of
amorphous OM (cf. Freeman, 2012). The amorphous OM can be broadly both FHR and solid bitumen is indicative of hydrocarbon migration into
classified into two fractions: (i) fluid-like hydrocarbon residue (FHR) organic-lean, siltstones of the Montney Formation early in the burial/dia-
which is dark brown, fluid to semi-fluid hydrocarbon residue present genetic history, followed by extensive diagenetic degradation and ther-
mal cracking. Oil-source rock correlation studies based on biomarker
signatures suggest that Triassic oils in the WCSB may have been sourced
Table 2
Thermal maturity values measured by bitumen reflectance, %BRo and converted to VRoeqv.
either from the Doig Formation or the Nordegg Member of the Fernie For-
values. mation (Fig. 1b; Riediger et al., 1990a; Riediger et al., 1990b). There is vir-
tually no primary aquatic or terrestrial kerogen (liptinite and vitrinite
%BRo na %VRoeqv.
macerals) in the studied Montney samples, which can be identified
(Bertrand and Malo, 2001)b
using organic petrology. This absence of marine-deposited primary kero-
Depth (m)
gen has also been observed in the Montney samples at lower thermal ma-
2130.5 1.17 19 1.25
2134.9 1.19 102 1.25 turity, which rules out the notion that all primary kerogen was thermally
2141.5 1.38 40 1.47 cracked and converted to hydrocarbons.
2155.3 1.28 65 1.37
2326.3 1.35 8 1.43 4.1. Characterization of OM in the standard Rock–Eval pyrolysis cycle
2340.4 1.16 78 1.24

Well median %Ro 1.23 1.32 FID pyrograms for the studied Montney samples typically show a bi-
a
Number of measurements. modal S2 peak (Fig. 3a) characterized by a smaller broad shoulder peak
b
VRoeqv. = (BRo + 0.03)/0.96. evolved between 300 to 450 °C followed by a more prominent broad

Please cite this article as: Sanei, H., et al., Characterization of organic matter fractions in an unconventional tight gas siltstone reservoir, Int. J. Coal
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 H. Sanei et al. / International Journal of Coal Geology xxx (2015) xxx–xxx 5

a free hydrocarbons (from either indigenous hydrocarbons or oil-based

drilling fluids).

4.2.2 . S2ESH hydrocarbon peaks

The S2ESH is measured over a wider temperature range of 150 to
650 °C at a slow ramping temperature increase of 10 °C per minute.
The S2ESH is manually integrated into two distinct peaks.

b the bimodal S2 peak in the standard Rock–Eval procedure (Fig. 3a). At
150°C 360°C 650°C
S2aESH S2bESH
S1ESH 2.42 mg HC/g
0.73 mg HC/g 2.23 mg HC/g
Free HC,
Contamination FHR Solid Bitumen
0.73 vol. % 6.76 vol. %
Fig. 3. An example of Rock–Eval 6 Flame Ionization Detector (FID) pyrogram in
(a) standard and (b) Extended Slow Heating (ESH) cycles for a core sample from the
Upper Montney Formation tight gas reservoir (2134.88 m) in the wet gas maturity win-
dow (VRoeqv. = 1.27%). (a) The bimodal S2 peak is observed, characteristically, in uncon-
ventional systems where condensed liquid hydrocarbon is retained within the rock.
(b) Two distinct peaks, S2aESH and S2bESH represent the fluid-like hydrocarbon residue
(FHR) coating the surface of the intergranular pores and the solid bitumen/pyrobitumen,
respectively.
peak released between 450 to 650 °C. The front shoulder of the S2 peak
likely represents a free hydrocarbon residue retained within the rock
after the S1 stage of thermal desorption (which did not allow sufficient
time for this fraction to be fully thermally desorbed and released).
Therefore, the total S2 peak contains a small fraction of higher molecular
free hydrocarbon (heavy oil residue). Furthermore, due to a higher ini-
tial iso-temperature (300 °C) in the standard pyrolysis cycle, a signifi-
cant amount of more volatile, oil-based invert emulsion drilling fluids
is included in S1 and mixed with legitimate free hydrocarbons in the
rock samples. At the relatively high thermal maturity of the cored
Montney intervals, most of the free hydrocarbons were cracked natural-
ly into gas and thus the S1 component of the studied samples likely con-
sist entirely of drilling mud contaminants.
4.2.2.1 . S2aESH peak. The S2aESH peak is evolved at the approximate py-
rolysis temperature range of 150 °C to 400 °C (Fig. 3b) which encom-
passes the majority of the standard S1 peak (iso 300 °C) plus part of
this temperature range, the majority of the OM is likely to remain in
the form of liquid to semi-liquid, medium to heavy range hydrocarbons
(oil residue; see section 4.2.1). This fraction likely represents the distinct
petrographically observed FHR fraction. The mean weight percent of hy-
drocarbon in this fraction is 0.07 (from 0.02 to 0.20) which equates to
approximately 0.25 vol.% of the whole rock using density values of
2.50 and 0.90 g/cm3 for the whole rock and heavy oil, respectively. It
should be noted, however, that the actual volume percentage of this
fraction in the whole rock is slightly higher than the values reported
here because the carbon content of the simultaneously released oxygen
containing OM during pyrolysis (S3) was not added due to uncertainty
over handling the S3 fraction in such a calculation S3 constitutes a very
minor portion of TOC (b 0.02 wt.%). Therefore, the reported values rep-
resent the minimum calculated volume proportion of the FHR fraction
in the whole rock. The results show that FHR comprises less than 1%
of total rock volume of the studied Montney core samples in the wet
gas window (Table 3). The small quantity of the FHR fraction deter-
mined from pyrolysis might initially seem incongruous with petro-
graphic observations showing the extensive distribution of this
fraction in the rock. Considering the mean effective present-time poros-
ity of the samples is approximately 4%, the FHR fraction coats 6 % vol-
ume of the present-time rock porosity. The nature of the FHR fraction
as a thin film over intergranular pore spaces provides an explanation
for how the small volume of this fraction is distributed extensively
throughout the samples. Furthermore, the FHR has likely lost a signifi-
cant portion of its volatile matter fraction due to diagenetic degradation
and continuous thermal cracking, and the present-day quantity of FHR
represents only a small proportion of this once significant, pervasive
fraction that existed after the migration of oil into siltstones of the
Montney Formation. At higher thermal maturity (dry gas window),
the fluid fraction of FHR is completely cracked into hydrocarbon gas
and pyrobitumen.

4.2. Characterization of OM in the extended slow heating (ESH) Rock–Eval

Table 3
pyrolysis cycle
Quantitative fractions of organic matter in the studied core using extended slow heating
(ESH) Rock–Eval cycle.
A typical FID pyrogram in the ESH cycle for the studied core (Fig. 3b)
Sample Light FHR Light FHRb Solid FHR Solid MinC
shows three distinct peaks: (i) S1ESH, (ii) S2aESH, and (iii) S2bESH. These
HC HCa bitumen bitumen
three peaks have distinct characteristics.
mg mg wt.% wt.% wt.% vol.% vol.% wt.%
HC/g HC/g
4.2.1 . S1ESH hydrocarbon peak
The ESH cycle appears to be better suited than standard Rock–Eval for 2134.88 0.73 2.23 0.07 0.20 3.25 0.73 6.76 1.71
2141.50 0.08 0.28 0.01 0.02 0.78 0.09 1.62 3.05
pyrolysis of the tight reservoir rocks in this study by allowing sufficient
2155.32 0.17 0.52 0.02 0.05 1.34 0.17 2.79 2.54
time to evolve volatile free hydrocarbons from the samples. Evolution 2337.37 0.11 0.52 0.01 0.05 1.41 0.15 2.95 1.51
of the S1ESH hydrocarbon peak (Fig. 3b) at the lower iso-temperature of 2340.42 0.11 0.52 0.01 0.05 1.62 0.16 3.38 1.48
150 °C (over a longer initial time of 10 min) represents readily volatilized 2345.51 0.13 0.62 0.01 0.06 1.10 0.19 2.30 1.55
Minimum 0.08 0.28 0.01 0.02 0.78 0.09 1.62 1.48
free hydrocarbon (light oil and gas condensates) trapped within the rock
Maximum 0.73 2.23 0.07 0.20 3.25 0.73 6.76 3.05
as well as contaminants from oil-based invert drilling mud. At higher Median 0.12 0.52 0.01 0.05 1.38 0.17 2.87 1.63
thermal maturity, where no indigenous liquid hydrocarbons are expected Mean 0.22 0.78 0.02 0.07 1.58 0.25 3.30 1.97
in the sample, the S1ESH peak provides a means to quantify the amount of a
Light HC: free light hydrocarbon in the rock, which can also be contaminated with
oil-based drilling fluid contamination. In the studied well, the S1ESH is diesel-based drilling fluids.
below 1 mg HC/g Rock and indicates a negligible quantity of volatile b
FHR: fluid-like hydrocarbon residue.

Please cite this article as: Sanei, H., et al., Characterization of organic matter fractions in an unconventional tight gas siltstone reservoir, Int. J. Coal
Geol. (2015), http://dx.doi.org/10.1016/j.coal.2015.04.004
6 H. Sanei et al. / International Journal of Coal Geology xxx (2015) xxx–xxx

4.2.2.2 . S2bESH peak. The S2bESH peak (Fig. 3b) is evolved at the approx-
imate pyrolysis temperature range of 400 °C to 650 °C. The release of
S2bESH can thus be correlated with the evolution of residual carbon
(RC%; S4 peak) from the oxidation stage which is performed within
the same temperature range. Because petrographic observations
showed no presence of primary inertinite in the samples, we assume
that the RC predominantly originated from the decomposition of the re-
maining unpyrolysable fraction of the S2bESH. In the absence of any pet-
rographically detectable primary kerogen, the total organic carbon
released under S2b and RC can be approximately equated to the concen-
tration of solid migrated bitumen in Montney rocks. In this case, the
weight percent concentration of organic carbon in the S2bESH peak
(wt. C% = S2bESH mg HC/g × 0.84; Lafargue et al., 1998) is added to
that of the RC% to calculate the bulk weight percent concentration of
the solid bitumen fraction in the studied Montney samples (Fig. 2).
This fraction constitutes 92 to 97 wt.% of the bulk TOC in the samples
and thereby dominates the reservoir effects of all other OM fractions
in the Montney rocks.
Solid bitumen is interpreted as an early oil phase that partially filled
the paleo-pore network of the Montney Formation during hydrocarbon
charging. Our proposed hypothesis is that with further diagenetic deg-
radation and increasing burial temperatures, colloidal components of
the migrated oil phase partially consolidated into solid bitumen while
the lighter fraction (S2aESH) preferentially adsorbed onto mineral sur-
faces. This fraction is regarded as FHR and petrographically character-
ized as brown films which extensively coat mineral grains.
4.3. Molecular compositions of OM fractions revealed by TD/Py–GC–MS/FID
analysis
Fig. 4a–c show the GC traces of the molecular composition of free hy-
drocarbons desorbed at ≤ 150 °C, ≤ 300 °C and 300–380 °C from a
Montney core sample. The hydrocarbon distribution patterns of the
sample are similar to normal crude hydrocarbons extracted from source
rocks and thus appear to be indigenous to the core (rather than contam-
ination from organic based drilling mud additives). This indicates that
contamination by drilling mud in the study sample is negligible.
The very small presence of hydrocarbons around C9 to C10 released
at 150 °C (Fig. 4a) suggests evaporative loss during the sample transpor-
tation, storage, handling, and preparation before lab analysis. The
≤300 °C GC trace represents the cumulative molecular composition of
the S1 peak of standard Rock–Eval analysis (Fig. 4b; including the
≤ 150 °C components). It is mainly comprised of light to medium
range of hydrocarbons up to C20. Components released between 300
and 380 °C are mostly heavy hydrocarbons with carbon number higher
than C20 (Fig. 4c). The 300–380 °C fraction represents the front shoulder
of S2 peak in standard Rock–Eval.
Integration of GC peak areas allows for quantification of the relative
proportion of each fluid OM fraction based on their temperature or mo-
lecular weight range in the studied Montney sample. The result shows
that hydrocarbons released below 150 °C roughly correspond to ≤ C9
hydrocarbons and account for about 7% of the total free hydrocarbons
in the analyzed Montney core sample. The relative proportion of initial
light hydrocarbons might be underestimated because evaporative loss
of light hydrocarbons is likely from intact core and powdered core sam-
ples. Hydrocarbons released between 150 and 300 °C, mainly in the
range of C9 to C20 were shown to account for about 80% of the free hydro-
carbons, and N C20 heavy hydrocarbons released between 300–380 °C
contribute about 13% to the volatile components in the Montney core.
These results further suggest that the S2aESH peak in the modified
Rock–Eval cycle consists mainly of medium to heavy range hydrocarbons,
confirming the fluid-like nature of this fraction (FHR) as suggested by
petrographic observations.
Fig. 5 shows the GC trace of hydrocarbons from the Montney core
sample when flash-pyrolyzed at 650 °C after the previous sequential
steps of thermal desorption to remove the volatile components. This

Fig. 4. GC traces from TD–GC–MS/FID analysis of a Montney core sample showing the composition of free hydrocarbons thermally desorbed from the rock sample at (a) 150 °C for 3 min;
(b) 300 °C for 3 min; and (c) 380 °C for 3 min after (b). Numbers denote the carbon numbers of the corresponding n-alkane peaks.

Please cite this article as: Sanei, H., et al., Characterization of organic matter fractions in an unconventional tight gas siltstone reservoir, Int. J. Coal
Geol. (2015), http://dx.doi.org/10.1016/j.coal.2015.04.004
 H. Sanei et al. / International Journal of Coal Geology xxx (2015) xxx–xxx 7

Fig. 5. GC trace from Py–GC–MS/FID analysis of the Montney core sample after thermal desorption to remove the free hydrocarbons. Gaseous hydrocarbons, benzene, toluene and C5–C6
alkanes are the dominant products, consistent with high thermal maturity and solid organic matter composed mainly of aromatic structures attached with short aliphatic chains.

fraction represents the S2bESH peak (Fig. 3b), and the remaining hydro- TOC in the Montney samples, the poor or negative correlations previ-
carbon potential of the solid bitumen. While there is a minor amount ously reported (Akai and Wood, 2014; Jarvie, 2012) between TOC con-
(1.5%) of heavy hydrocarbons released from pyrolysis that have been tent and porosity over a wide range of thermal maturities within the
trapped in the rock matrix, the GC trace is dominated by C1–C4 gaseous Montney tight gas fairway can be explained by the detrimental effect
hydrocarbon peaks which account for about 40% of the total amount of of the pore-filling solid bitumen fraction. This contrasts markedly with
pyrolyzed hydrocarbons. Benzene and toluene are the next most prom- the positive correlations of porosity and permeability with TOC content
inent peaks, contributing about 6% and 5% (respectively) to the total py- evident in other unconventional reservoirs (Jarvie et al., 2007; Milliken
rolysate hydrocarbons. Although ≥C5 normal alkanes and alkenes are et al., 2012; Passey et al., 2010).
common products from pyrolysis of Type I and II source rocks, they
are only minor components in the flash pyrolysates from Montney
core sample except nC5 and nC6. This confirms that the solid organic
matter (solid bitumen as observed under microscope) in the Montney
core samples has experienced high thermal maturity with limited po-
a Ambient porosity vs. total organic carbon (TOC)
10
tential for liquid hydrocarbon generation, and is mainly comprised of ar-
omatic structures with some short aliphatic chains. At higher thermal
8
maturity, the solid bitumen can further release volatile matter and con-
vert to refractory pyrobitumen.
Porosity (%)

6 R² = 0.1956

4.4. Role of OM fractions in reservoir quality 4

Ambient porosity in the cored intervals of the studied well ranges 2

from 3.9 to 8.2% (Table 1). Average porosity is higher for Upper Montney
samples (6.3%; depths 2127 m to 2161 m) than for Lower Montney sam-
0
ples (4.6%; depths 2326 m to 2348 m). Similarly, mean pore throat radius 0 0.5 1 1.5 2
is higher in the Upper Montney (mean = 0.028 μm) than the Lower TOC (wt.%)
Montney (mean = 0.005 μm). Higher porosity and pore throat size
values in the Upper Montney are associated with coarser grain size Ambient porosity vs. solid bitumen volume
(mean = 48 μm) compared to the Lower Montney (mean = 21 μm). b 8
The significant positive correlations between grain size and ambient
core porosity (R2 = 0.72, n = 18), and median pore throat size (R2 =
0.62, n = 18) show that grain size is an important influence on reservoir 6
quality in this particular well (cf. Wood et al., in press). R² = 0.9324
Porosity (%)

Data from the studied Montney core show a weak inverse relation-
ship between bulk TOC and reservoir quality parameters such as poros- 4
ity (R2 = 0.196, Fig. 6a) and pore throat size (R2 = 0.35, Fig. 7a).
Dramatically improved relationships are evident, however, when the
volume fraction of solid bitumen from ESH pyrolysis is used instead of 2
bulk TOC: the results show significant inverse correlations between
solid bitumen and porosity (R2 = 0.93, Fig. 6b) and pore throat size
0
(R2 = 0.76, Fig. 7b). These results indicate that the presence of solid bi- 0 1 2 3 4
tumen in the Montney is detrimental to reservoir quality (cf. Wood Solid Bitumen (vol.%)
et al., in press). The accumulation of solid bitumen obstructs a signifi-
cant portion of the paleo-porosity network and hence hinders fluid Fig. 6. Cross-plots of (a) TOC wt.% versus ambient porosity and (b) solid bitumen vol.% ver-
flow. Since the solid bitumen fraction constitutes the majority of the sus ambient porosity.

Please cite this article as: Sanei, H., et al., Characterization of organic matter fractions in an unconventional tight gas siltstone reservoir, Int. J. Coal
Geol. (2015), http://dx.doi.org/10.1016/j.coal.2015.04.004
8 H. Sanei et al. / International Journal of Coal Geology xxx (2015) xxx–xxx
Pore throat radius vs. total organic carbon (TOC)
a 0.08
Pore throat radius (µm)
0.06
0.04
0.02
R² = 0.3474
0 0
0 0.5 1 1.5
TOC (wt.%)
Pore throat radius vs. solid bitumen volume
b 0.05
Pore Throat Radius (µm)
0.04
0.03
0.02
0.01
R² = 0.7634
0.00
0 1 2 3
Solid Bitumen (vol.%)
Fig. 7. Cross-plots of (a) TOC wt.% versus median peak pore throat radius (μm) and
(b) solid bitumen vol.% versus median peak pore throat radius (μm).
The solid bitumen fraction represents a remnant of crude oil that
once migrated conventionally into water-wet reservoir rocks. Larger
molecule, high-density oils preferentially occupied large intergranular
pore spaces because capillary pressure was insufficient to force the
non-wetting oil phase into finer pore spaces associated with fine silt,
clays and grain interstices. Migration of oil into larger pores likely al-
tered the wettability of the contacted paleo-intergranular pore spaces.
Asphaltenes in high molecular, high-density oil can exhibit colloidal
behavior and a tendency to precipitate/flocculate and aggregate with
changing physicochemical conditions (Buckley and Liu, 1998; Buckley
et al., 1997; Cuiec, 1991; Hirasaki et al., 1990). We therefore suggest
that asphaltenes in the high-density fraction of the oil, which preferen-
tially occupied larger Montney paleo-pores, precipitated in bulk
forming aggregates. Subsequent increases in burial and thermal maturi-
ty, in conjunction with further diagenetic processes, resulted in consol-
idation of the asphaltene aggregates into lumps of solid bitumen. At
even higher thermal maturity, the solid bitumen transformed with in-
creasing aromaticity to pyrobitumen.
Coincident with the aggregation of asphaltenes into lumps of solid
bitumen, the polar, macromolecular fractions of crude oil adsorbed
onto mineral surfaces. Products of the latter process are represented
petrographically as thin films of brown heavy oil residue coating miner-
al surfaces and lining most of the present-day pores (Fig. 2). This frac-
tion, petrographically regarded as FHR, can be quantified from the
S2aESH peak on an ESH pyrogram. Although this fraction constitutes a
small amount of the mass or volume of the sample, it covers a large sur-
face area and hence plays an important role in reservoir wettability. It is
possible that the lower molecular and density fraction of migrating
crude oil preferentially entered tighter mineral interstices and relatively
finer intergranular pore spaces associated with smaller silt and clay
minerals. This may have led to the ionic interaction of oil and brine in
Please cite this article as: Sanei, H., et al., Characterization of organic matter fractions in an unconventional tight gas siltstone reservoir, Int. J. Coal
Geol. (2015), http://dx.doi.org/10.1016/j.coal.2015.04.004
Pyrite content vs Total Organic Carbon (TOC)
a 6
5
Pyrite (wt.%)
4
3 R² = 0.0149
2
1
2 0 0.5 1 1.5 2
TOC (wt.%)
b7 Pyrite content vs solid bitumen volume
R² = 0.8467
6
5
Pyrite (wt.%)
4
3
2
1
0
0 2 4 6 8
4 Solid Bitumen (vol.%)
Fig. 8. Cross-plots of (a) TOC wt.% versus pyrite wt.% and (b) Solid bitumen vol.% versus py-
rite wt.%.
once predominantly water wet fine pore spaces, the surface adsorption
of oil, and a change from water wet to hydrocarbon wet conditions. Re-
cent Montney studies (Lan et al., 2014a, 2014b) confirm that oil wetta-
bility is positively correlated with TOC content.
4.5. Role of pyrite and bacterial degradation in reservoir quality
There is no obvious relationship between the bulk content of TOC
and pyrite in the studied Montney samples (Fig. 8a). However, a signif-
icant positive correlation between the volume fraction of solid bitumen
and pyrite content is evident in a subset of these samples (Fig. 8b). This
correlation is consistent with petrographic observation that show close
spatial association between the pyrite minerals and integranularly accu-
mulated solid bitumen in Montney samples (Fig. 9a–c).
Most pyrite in studied samples are in the form of ‘framboids’, which
are raspberry-shaped spherical aggregates of varying size (2–50 μm),
composed of assemblages of tiny pyrite crystallites (Fig. 9a–c). Precipi-
tation of iron sulfide in the form of framboidal pyrite is long believed
to be due to bacterially-mediated decomposition of OM in anoxic condi-
tions (Folk, 2005; Love, 1957, 1962, 1967; Love and Murray, 1963; Love
et al., 1984; Raiswell, 1982; Schneiderhohn, 1923; Suits and Wilkin,
1998). This process is regarded as bacterial sulfate reduction (BSR)
which results in reaction between dissolved iron and H2S generated
from the reduction of dissolved sulfate by bacteria using sedimentary
OM (Berner, 1984; Berner and Raiswell, 1983).
Framboidal pyrite is commonly precipitated from the euxinic water
and/or within the anoxic sediments during post-depositional, early
diagenesis. However, in the case of Montney, both mechanisms can be
ruled out. This is because the Montney Formation is mainly composed
of organically lean siltstone which was deposited predominantly
under oxic conditions in lower shoreface to offshore environments
(Davies et al., 1997; Edwards et al., 1994; Wood, 2013). This depositional
 H. Sanei et al. / International Journal of Coal Geology xxx (2015) xxx–xxx
a Solid Bitumen
Framboidal pyrite
Solid Bitumen
FHR
50µm
b
Solid Bitumen
Framboidal pyrites
FHR
50µm
c arching process which worked in parallel with the other two processes
Framboidal pyrite
Solid Bitumen
Solid Bitumen
50µm
FHR
Fig. 9. (a–c) Photomicrograph (oil immersion, white incident light, 50× objective) show-
ing co-location of the bacterially-derived framboidal pyrite and lump accumulations of
solid bitumen in the intergranular paleo-pore spaces. Solid bitumen and framboidal pyrite
are both by-products of bacterial sulfate reduction of liquid hydrocarbon during early oil
migration into the Montney rocks. FHR indicates fluid-like hydrocarbon residue.
environment is supported by the petrographic observations which
indicate limited evidence of primary kerogen. If there was insufficient de-
trital OM to fuel post-depositional bacterial degradation, then bacterially-
derived framboidal pyrite in the Montney Formation was likely formed
instead by BSR of crude oil soon after migration into the formation.
Early oil migration into Montney rocks may have significantly promoted
anaerobic bacterial activity in the presence of sulfate-rich brine.
Solid bitumen and framboidal pyrite are both potential diagenetic by-
products of BSR (Machel, 2001). In addition to asphaltene flocculation
and thermal degradation leading to solid bitumen, degradation of crude
Please cite this article as: Sanei, H., et al., Characterization of organic matter fractions in an unconventional tight gas siltstone reservoir, Int. J. Coal
Geol. (2015), http://dx.doi.org/10.1016/j.coal.2015.04.004
9
oil by BSR may also have played a role in the accumulation of solid bitumen
and crystallization of framboidal pyrite in the paleo-pore spaces (Fig. 9b).
This is supported by petrographic observations showing co-location of
the bacterially-derived framboidal pyrite and accumulations of refractory
solid bitumen in the intergranular paleo-pore spaces. Since framboidal
pyrite and solid bitumen compete for available pore space, both phases
are detrimental to reservoir quality of the Montney Formation.
Evidence of bacterial degradation of crude oil in this study is based
on petrographic evidence of bacterially-derived framboidal pyrite, spa-
tial co-location of the framboids and solid bitumen, and correlation be-
tween the amounts of pyrite and solid bitumen. The BSR interpretation
will be tested by future research on the isotopic signatures of the pyrite
and solvent extraction of core samples. Such investigations will lead to
improved understanding of the relationship between solid bitumen
and reservoir quality in the Montney Formation.
4.6. Digenetic and thermal degradation of OM in Montney Formation
The results of this study suggest that migration of oil into the organi-
cally lean siltstones of the Montney succession, and subsequent diagenet-
ic and thermal degradation of oil, have ultimately defined the present-
day OM content and reservoir quality of the Montney Formation.
We suggest that the following geologic processes occurred once oil
had migrated into the Montney formation.
• Flocculation and aggregation of asphaltenes from colloidal suspension
in crude oil due to instability of the oil with further burial and changes
to pressure and temperature. This process promoted a significant
change in wettability from conventional water-wet conditions to un-
conventional mixed-wettability conditions.
• Simultaneously, the migrated oil promoted early anaerobic bacterial ac-
tivity in the presence of sulfate-rich brine. This process took place at
lower temperature (maximum reported temperature of 80–100 °C;
Machel, 2001) and stopped when burial progressed deeper.
• Progressively increasing thermal maturity with burial acted as an over-
at lower maturity but continued on to higher thermal maturity,
resulting in the cracking of oil and the formation of solid bitumen and
eventually pyrobitumen.
5. Conclusions
This study presents innovative methods for quantifying various OM
fractions within tight gas siltstone core samples from the Triassic
Montney Formation of northeast British Columbia in the Western
Canadian Sedimentary Basin (WCSB). Our results show:
1. An extended slow heating (ESH) Rock–Eval cycle provides useful
quantitative information on various OM fractions within these un-
conventional reservoir rocks.
2. There are three major OM fractions: (i) free light oil, (ii) fluid-like
hydrocarbon residue (FHR), and (iii) solid bitumen or pyrobitumen
(at higher thermal maturity).
3. The FHR fraction constitutes a small portion of the OM in Montney
samples as a thin film of condensed, heavy molecular hydrocarbon
coating the intergranular pore spaces and may represent the lighter
component of the paleo-oil that migrated into the Montney reser-
voir. The FHR fraction potentially plays a role in wettability alteration
by creating hydrophobic matrix pore networks in portions of the res-
ervoir that were not already filled with solid bitumen.
4. Solid bitumen constitutes the majority of the OM in the studied sam-
ples and represents a former liquid oil phase that migrated into the
paleo-intergranular pore network. Solid bitumen has a negative over-
all effect on reservoir quality by occluding porosity and impeding fluid
flow. Aggregation of the asphaltene fraction of migrated oil in larger
10 H. Sanei et al. / International Journal of Coal Geology xxx (2015) xxx–xxx

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and Ms. Terri Olson for the helpful constructive review of the manu- ference and Exhibition, Italy, March 28–30.
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Please cite this article as: Sanei, H., et al., Characterization of organic matter fractions in an unconventional tight gas siltstone reservoir, Int. J. Coal
Geol. (2015), http://dx.doi.org/10.1016/j.coal.2015.04.004