PETROLEUM SOCIETY PAPER 2006-062

CANADIAN INSTITUTE OF MINING, METALLURGY & PETROLEUM

Determining Bitumen, Water and Solids in Oil

Sands Ore by Using Low-Field NMR
Y. NIU
University of Calgary

A. KANTZAS, J. BRYAN
University of Calgary, TIPM Laboratory

This paper is to be presented at the Petroleum Society’s 7th Canadian International Petroleum Conference (57th Annual Technical
Meeting), Calgary, Alberta, Canada, June 13 – 15, 2006. Discussion of this paper is invited and may be presented at the meeting if
filed in writing with the technical program chairman prior to the conclusion of the meeting. This paper and any discussion filed will
be considered for publication in Petroleum Society journals. Publication rights are reserved. This is a pre-print and subject to
correction.

Abstract
In previous work, low-field nuclear magnetic resonance
(NMR) has been considered as a fast and non-destructive
method to characterize oil and water. In this work, we continue
to use the low-field NMR technique to determine the amount of
bitumen, water and solids for unconsolidated oil sand ores from
two different depositional environments. Simple T2 cut-off and
signal deconvolution are applied to the NMR spectra to
estimate bitumen and water content. Comparison results are
given. It has been found previously that in most cases, the
signals from clay bound water and bitumen overlap, thus the
estimation of fluid content needs correction. To replace the
well-known Dean-Stark extraction method, it is necessary to
seek a fast, simple, non-destructive and inexpensive method. A
densitometry technique, with simultaneous pore volume
measurement, is developed to provide the volume of the ore
sample and complement the NMR results. A density algorithm is
introduced to determine fluid and solid content. Results from
pore volume measurement are comparable with those from
Dean-Stark extraction and low-field NMR. A combined NMR-
pore volume technique appears to minimize errors compared to
Dean-Stark extraction.
Introduction
It is well known that the global oil demand has continued to
accelerate over the years and conventional oil supplies tend to
decline. Therefore, more attention turns to the unconventional
resources such as oil sands. The Alberta oil sands, the largest
source of bitumen in the world, are relatively under-exploited,
with estimated recoverable bitumen reserves of roughly 39
billion m3 and established reserves of approximately 376 billion
m3 (1). However, the varying depositional history and complex
sedimentary sequences (2) result in the formations hosting oil
sands deposits that are not homogeneous, with significant
difference in pay thickness, permeability, as well as bitumen
and water saturation. Moreover, most of the higher-quality
deposits are already producing or under development. In order
to evaluate the oil sands potential resource and generate
maximum economic returns, it is necessary to determine the
content of bitumen, water and solids properly.
Low-field nuclear magnetic resonance logging has become
popular since the 1990s for analyzing reservoir fluids and
fluid/rock interaction. Recently, considerable effort has been put

1
on the applications of NMR technology in oil sands. Such
works include bitumen viscosity determination (3, 4, 5, 6), in-situ
viscosity measurement (7, 8), the clay content estimation in
unconsolidated samples (9, 10, 11) and in-situ fluid saturation
assessment for ore and froth (12, 13). In oil sands mining
operations, a quick and accurate way to determine the bitumen,
water and solids content would improve the operating costs
efficiently. Dean-Stark extraction has been considered to be an
industry standard to measure the bitumen, water and solids (14),
but such an extraction procedure is highly time-consuming and
requires significant volumes of very expensive and toxic
solvents. Also, the sample itself is totally destroyed after the
extraction. Our research proposes a fast and non-invasive
method. A pore-volume experiment is run to determine the
amount of solids using a density algorithm. The result is
integrated with low-field NMR relaxometry to obtain the
amount of bitumen and water.
The first part of this paper describes how the low-field
NMR measurement and density algorithm work on oil sands
ore. This is followed by the description of the experiment
workflow, and the analysis for samples from two different
depositional environments. The final part shows the comparison
with Dean-Stark results. Particle size distribution is also
analyzed.
Low-field NMR on Oil Sands Ore
NMR relaxation times have proven to be an important non-
invasive probe of the physical geometry of porous media. The
theory behind NMR measurements was covered in detail in the
literature (15, 16, 17, 18). NMR measurements on rocks directly
respond to the hydrogen content of the fluids in the pore space.
The electromagnetic response of hydrogen spin nuclei can be
captured under the influence of a series of radio-frequency (RF)
pulses in an external magnetic field. That is, there are two
processes for the NMR measurement. The first one is to
polarize the hydrogen nuclei by using a permanent magnet to
create the net magnetization. This polarization process may take
several seconds, depending on the fluid types. Immediately
following the polarization period, a sequence of pulses is
applied to produce a characteristic decay signal. The Carr-
Purcell-Meiboom-Gill (CPMG) sequence is the most widely
used sequence in NMR measurement. The decay signal is
characterized by T2 relaxation times.
Most of useful information about fluid properties (15, 16, 17, 18)
can be provided by the T2 distribution, a semilog graph of
amplitude vs. T2 as obtained by an inversion algorithm of the
decay signals. In order to extract such information, the
mechanisms that produce the signal should be understood.
There are three independent physical processes involved – bulk
relaxation, surface relaxation and diffusion-induced relaxation.
Equation 1 quantifies the relationship (15).
 S  (γGTE ) D
2 The priori knowledge for this method is that the ore weight and
1 1
= + ρ2  + ......................... (1)
T2 T 2 B V  12
where,
T2B = T2 bulk relaxation
ρ2 = T2 surface relaxivity
S/V = ratio of pore surface to fluid volume
γ = gyromagnetic ratio of a proton
2
G = average magnitude of the total magnetic
field gradient over the entire sample
TE = time echo
D = molecular diffusion coefficient
For fluids in porous media, which of the three relaxation
mechanisms dominates depends on the fluid types, pore sizes,
pore surface area, and wettability. For oil sands ore measured in
laboratory based (bench-top) NMR instruments, the main
relaxation processes are the surface relaxation and bulk
relaxation (when there is no gradient magnetic field and short
TE is chosen).
Assuming the oil sands ore is fully water-wet, the bitumen
would not be in direct contact with the rock surface, but instead
separated from the solid mineral grains by at least a thin film of
water (19). Therefore, the T2 relaxation of bitumen is from the
contribution of its bulk relaxation. The bulk relaxation is
controlled by the physical properties of the fluid such as
viscosity and chemical composition (15). Bitumen is
characterized by its high viscosity, larger molecular weights and
complex chemical structures. As a result, the T2 signals of
bitumen relax very fast and generally occur as a single broad
peak under 10ms (12). The T2 relaxation of water residing in the
oil sands is the combination of bulk relaxation and surface
relaxation. The ratio S/V in equation (1) reflects the pore
geometry. In general, the smaller the pores, the faster the
relaxation. The solid part in oil sands mainly consists of very
fine to fine sands and clays, which makes the water relax very
quickly due to the restricted pore space. Based on previous
observations (12, 13), there is no sufficient separation between the
bitumen and clay-bound-water relaxation times. The
overlapping between them results from the high viscosity of
bitumen and the large surface areas of the clays. This work
continues to investigate how to partition the overlapped signals
for accurate determination of bitumen and water contents.
Density Algorithm and Pore-Volume
Experiment
The true density of a sample is defined as the ratio of the
mass to the volume occupied by that mass. Therefore,
contribution to the volume made by pores or internal voids must
be neglected when measuring the true density (20). The reason
behind this correction is the fact that an ore sample brought in
the laboratory has been exposed to both expansion and
deformation due to coring and cutting. Thus the water, bitumen
and solids content have to be corrected for the volume of the
original undisturbed sample. Consequently, in order to
calculate the true density of oil sands ore, the volume of ore
itself should be measured without air present. But it is difficult
to measure the volume by using Archimedes’ principle because
unlike conventional cemented cores, not only is oil sands ore
unconsolidated but also is the mixture of bitumen, water and
solids. To accommodate for this, a pore-volume experiment is
introduced, which is based on the principle of gas displacement.
the volume
(1) of the sample holder must be known before
experiment. A schematic diagram illustrating the methodology
is shown in Figure 1. An inert gas (e.g. Nitrogen) fills the
system space that is not occupied by the ore to a predefined
pressure. Then the gas is allowed to expand. The excess gas is
monitored as it displaces a measured volume of water. After the
water displaced by gas expansion is collected, gas laws are
applied to calculate the volume containing all pores, voids and
empty space (named as pore-volume). The value of interest, i.e.
the real ore volume can be obtained by subtracting the pore-
volume from the holder volume. Thus the true density of ore
(ρt) is easily calculated. If the density for fluid (ρf) and solids
(ρs) are given, then the content of solids and fluids can be
deduced from the following density algorithm.
The total mass of the ore sample, fluid mass and solid mass
in the ore are assigned as mt, mf and ms, respectively.
Accordingly, the volumes for each component are Vt, Vf and Vs.
Therefore,
improve the resolution of the fast-decay components such as
bitumen and clay-bound and small pores water. Also the short
TE usually negates diffusion effects from residual magnetic
gradients in the sample volume (16, 21). The product of TE and
the number of B pulses controls how much of the relaxation
spectra are measured. Complex T2 spectra may require more of
the relaxation for the analysis to function optimally (21). Longer
TW will improve the contribution of the slowest components.
The noise will be reduced when the number of trains is
increased, but the time is prolonged accordingly.

Two sets of CPMG sequences were applied in this work

mt = m f + m s ........................................................................... (2)
(Table 1). The dataset was analyzed using a multi-exponential
inversion algorithm. The magnetization decays were processed
by software, Ecofit v3.02 (developed by Numar Corporation
(22)
), to calculate a distribution of amplitudes and T2 relaxation
mf ms time constants. Bitumen and water signals were separated in
Vt = V f + Vs = + .................................................. (3) two ways. A deconvolution approach was applied, as it has been
ρf ρs used successfully in the past to discriminate between oil and
water signals in oil sands (12, 13). Alternatively, samples of bulk
By simple mathematical conversion of (2) and (3), the solid oil were obtained and it was determined that in this range of
content is calculated as follows: viscosity of bitumen, no signal was obtained beyond 2 ms. This
T2 value was also used as a cutoff between oil and water in the
ore spectra. This paper presents results using both the T2-cutoff
mt and deconvolution methods.
Vt −
ρf Work-flow
ms = ....................................................................... (4)
1 1 Figure 3 is the workflow of this study. The same sample
− would be used in the whole experiment process (no sister
ρs ρf samples were used), which minimized the mass loss and kept
the consistency of the sample. A custom-made Teflon® sample-
Thus, holder was designed to satisfy the needs in both pore-volume
and NMR measurements. After the ore sample was loaded into
the holder, the pore-volume experiment was performed first.
m f = mt − ms ............................................................................ (5) Then the holder was transferred to the NMR relaxometer for
measurement, followed by Dean-Stark extraction. The last step
Here the fluid mass (mf) is the sum of bitumen mass and was to analyze the particle size distribution of the dried solids.
water mass. The Mastersizer 2000 was used to obtain the particle size
distribution based on the laser diffraction principle (23).

Experimental Results and Discussion

Sample Description
Previous work
Samples were taken from surface mining sites on the
Athabasca area, northern Alberta. They were deposited in two The NMR signals for oil sands ore have essentially two
depositional environments – open estuarine and tidal flat. components linked to the amounts of water and bitumen. The
Before the laboratory NMR measurement and pore-volume methodology to determine the fluid content from the NMR
experiment, the two samples were totally mixed respectively spectra was proposed in previous publications (12, 13). This work
(so-called homogenizing process) and no visible sedimentary follows the same procedure. The linear relationship between the
rock features could be observed. Figure 2 showed the actual oil mass of a bulk fluid and the associated total amplitude defines
sand ores from the two facies – EC and TFS. Each sample was the amplitude index (AI).
then divided into several sub-samples.
Ai
Data Acquisition AI i = ..................................................................................... (6)
mi
In this work, ore volume was measured under very low
pressure (less than 70kPa) and ambient temperature. Nitrogen
was the probe gas. Two sets of CPMG sequences were applied
(Table 1). All NMR measurements were performed using an Where
EcoTek-FTB low-field NMR spectrometer that operated at a
frequency of 1.78 MHz. The EcoTek-FTB low-field NMR Ai = amplitude of fluid
spectrometer allows the operators to choose appropriate CPMG mi = fluid mass
parameters to control the data acquisition. The parameters i = either bitumen or water
include Time-to-echo (TE), Number of B pulses, Time-to-next
train (TW) and Number of trains. A short TE is essential to

3
 Equation (6) is fundamental in determining the fluid contents
from the ore spectrum. When the AI values for bitumen and
water are known, and the amplitude of each of them can be
determined accurately, it is straightforward to calculate the
respective mass by rearranging the equation (6). As previous
research (12, 13) indicated, because of different viscosity, the
signals for bulk bitumen and bulk water in their mixture are so
distinctive that it is easy to separate them and sum up the
respective amplitude. However, the NMR signatures of an oil
sand ore are very complex, usually containing the contributions
from bulk bitumen, water in sand, water in clays, and water in
thin films around the mineral grains if water-wet is assumed.
Therefore, it is a challenge to predict the accurate bitumen and
water amount.
Oil sands Ore
The ores from the two depositional environments were called
EC ore and TFS ore. Ten sub-samples for EC ore and seven
sub-samples for TFS ore were gathered. Each sub-sample was
measured according to the workflow diagram. The NMR
spectra are given in Figure 4 (a, b, c, d, e, f). All ore spectra
were bimodal, but the TFS ore had a larger second peak than the
EC ore. Any signal beyond the first peak is water, so this means
that TFS ore must contain much more water. Figure 4a and 4b
compared the two ores for different sets of CPMG parameters.
Due to the higher fraction of water in the TFS ore, it seemed
that it was better to set the wait time (TE) to be 10 seconds so
that the ore could have enough time for relaxation. The red lines
in Figure 4c and 4d represented the T2-cutoff lines. The
amplitudes less than T2-cutoff were assigned to be bitumen and
the rest to be water. The amplitude index of water (AIw) was
calculated from the response of 2% NaCl bulk brine, which was
fairly constant (12, 13), while the amplitude index of bitumen
(AIo) was from the measurement of the extracted bitumen,
explained in the next section. By applying equation (6), both
bitumen and water content were predicted (Table 2). Figures 4e,
4f, 4g and 4h were the results from the oil peak de-convolution
algorithm (7). The main idea behind this algorithm is to separate
the first peak into two parts: the bitumen peak and a surface
water peak because of overlapping signals of bitumen and clay-
bound water.
The spectra of ore, bitumen and water were shown clearly
after de-convolution, and the predicted content of bitumen and
water were also displayed in the Table 2. For EC ore, both of
the CPMG sets showed that T2-cutoff method gave more
amplitude in bitumen peak resulting in higher bitumen content,
while deconvolution algorithm gave more water amplitude. For
the TFS ore, the two sets of CPMG parameters showed that the
deconvolution algorithm predicted slightly more water content
and bitumen content than the T2-cutoff method did.
Bitumen
Bulk bitumen was obtained after the Dean-Stark extraction
procedure was finished. At the ambient state, the mixture
solution of bitumen and solvent (i.e. toluene) was poured into a
plastic bag that was kept open and it was left standing under the
fume-hood for at least one month to let the solvent evaporate
completely. What was left was regarded as bitumen. Figure 5
showed the NMR signals of the bitumen from EC ore and TFS
ore and Table 3 listed the signal-to-noise ratio (SNR) and T2
geometric mean (T2gm). The first set of CPMG parameters gave
a higher SNR but lower T2gm than the second set. It appeared
that the bitumen from the two depositional environments was
almost the same in terms of amplitude index AIo and T2gm. It
was also noticed that the bitumen spectra did not have zero
4
amplitude at the first T2 bin (0.1 ms). One possible explanation
could be the bitumen viscosity is extremely high and the current
spectrometer could not capture the very fast relaxation
component. Figure 6 shows the overlapping spectra of ore and
bitumen. It is interesting to note that the bitumen spectrum was
matched well with the EC ore, while the spectra of TFS bitumen
and ore had some discrepancy, which might be indicative of a
higher water contribution in the first peak.
Result Comparison
The bitumen, water and solids content from the NMR
measurement had been obtained and listed in Table 2. Table 4
gave the Dean-Stark results and pore-volume results with the
solid density assigned as 2.60 g/cm3 and the fluid density as
1.00 g/cm3. In this study, the density of bitumen was assumed to
be the same as that of water and the solids density similar to the
value for sands. It should be mentioned that the results from the
density algorithm are largely dependent on the fluid density and
solid density. Any minor change in fluid and solid densities
could generate a large discrepancy over the results. The Dean-
Stark result was averaged from the sub-sample measurements.
Figure 7 compares the result difference between NMR
measurement versus Dean-Stark, and NMR versus density
algorithm. For EC ore, the measurement difference between
pore volume and NMR was minimal and the first set of CPMG
sequences was probably more appropriate to determine the
bitumen and water content by using T2 cutoff at 2 ms (Figure 7a
and 7b). For TFS ore, the measurement difference between
Dean-Stark and NMR became less when the fluid density was
taken as 1.00 g/cm3 (Figure 7c and 7d). Because the TFS ore
spectra showed the larger second peak (see Figure 4), it could
be assumed there was more water inside the ore and perhaps the
water put more weight on the fluid density. Hence, when the
fluid density changed from 1.00 g/cm3 to 1.02 g/cm3, the
measurement of the pore-volume method matched the NMR
results better when the second CPMG set was applied and T2
cutoff at 2 ms was used. (Figures 7e and 7f).
Aside from the ore true density and ore volume, the pore
volume experiment provides other useful information such as
fluid volume (Vf ) and porosity (φ). If the water saturation (Sw)
was known, then the water mass could be obtained by Vf*φ*Sw.
Therefore, bitumen content could be determined by mass
balance. The methodology for water saturation determination
had been proposed as follows (3, 12):
Aw 1
Sw = x100 ................................................................. (7)
AI w mt
The difficulty in using NMR as a stand-alone tool to
determine bitumen and water content is that there are two
unknowns for the bitumen: the oil amplitude and its AI value.
Even if the fluid signals can be separated using the T2-cutoff or
deconvolution approach, the issue of how to relate oil amplitude
to mass remains.
In previous work (12, 13), this was done using the oil mean
relaxation time, but if the T2-cutoff approach is used, the oil
relaxation time no longer has any meaning. By combining NMR
to the pore-volume method, however, oil content can still be
determined. The pore-volume method gives the total fluid
fraction, and NMR can be used to provide the water portion of
this fluid. Oil content can then be obtained by difference. Table
5 shows predictions of oil by difference, compared against the
Dean-Stark measurement of oil content. The difference is less
than 1%, indication that this methodology has potential.
 When using the first set of CPMG parameter in the EcoTek- that the TFS ore contain much more fines than the EC ore, and
FTB Spectrometer, the run-time for each sample is about three EC ore had more large grains. If the ore is water-wet, this fact
minutes; while the second set of CPMG parameter will take confirms again that the oil sands ore with high fines had a
about 15 minutes. That is, the time-span of NMR measurement higher ability to retain water, which was also conformed to the
depends on the chosen CPMG parameters. Usually the run time NMR spectra (Figure 5). For example, the large portion of fine
will be increased with the longer wait time and more trains. The solids in TFS ore corresponds with higher overlap between the
results from pore-volume measurement for a single sample bitumen and water signals and more water at later T2 values as
come out about 30 minutes in our laboratory. Compared to the well. The clays for this work are defined according to particle
Dean-Stark extraction, the combination of NMR – Pore Volume size and not to chemical composition. The particle size less than
measurement is time-efficient. 2 µm is defined as clay. The particle size between 2 µm and 44
µm is silt. The particle size larger than 44 µm is sand (24). From
Quality Assessment of Results the observation of the Figure 10, there were no particles less
than 2 µm existed in either EC ore or TFS ore. And it could be
inferred the water signals in NMR spectra were from the very
Quality control (QC) and Reliability of NMR measurement fine pores or water film around the grains.
To maintain consistent quality in the NMR instrument
calibration and consistent quality in sample NMR measurement, Conclusion
QC standard made with 0.4M CuSO4 solution was run along
with each sample. The values were kept steady in the range of In this work, pore-volume experiment and density algorithm
amplitudes between 0.98 and 1.02. were applied to determine the fluid and solid content of oil sand
ores. This method offered extreme simplicity of operation along
By taking the second set of CMPG parameter as an example, with great speed. Two types of ores deposited in different
Figure 8 showed the normalized spectra of all sub-samples from sedimentary environments had been tested on this method and
EC ore and TFS ore. The spectra shapes were similar for each the results were compared with those from low-field NMR
ore, which verifies the reproducibility and reliability of the measurement. If some of uncertainties can be eliminated, the
NMR measurement. The bitumen spectra demonstrated the combination of pore volume-NMR would determine the content
same repeatability as well. of bitumen, water and solids accurately as a fast, economic and
non-invasive technique. These uncertain factors included the
This work also demonstrates the accuracy of pore-volume effect of the accessibility of the probe gas (i.e. Nitrogen),
measurement and the effectiveness of Dean-Stark extraction by unknown fluid density and solid density and the effect of clay
using synthetic samples. content. Results are presented for the accuracy of both the pore-
volume method and Dean-Stark extraction. Particle size
Accuracy of pore-volume measurement analysis may also be a useful tool in interpreting overlap in
bitumen and water NMR signals.
Two synthetic ores were made combining sand, 2% brine
and Cold Lake cleaned heavy oil with known density and
known mass. Each composition was added into the custom-
made sample-holder directly to avoid mass loss. The gas-
Acknowledgement
expansion experiment was then applied. The calculated density The authors would like to thank Canada Research Chair in
from the experiment was compared with the known density as Energy and Imaging and its industrial affiliates (Nexen,
shown in Table 6a and 6b. The densities obtained from the Canadian Natural, Shell, Devon, Petro-Canada and E-T Energy)
pore-volume measurement were consistently slightly lower. for financial support and Shell Canada for sample donation.
This may be caused by the insufficient Nitrogen accessibility to
all the pore spaces. Despite this offset, difference between them NOMENCLATURE
was only around 1% (Table 6c). Therefore, this density
measurement approach would be considered to be applicable. Ai = amplitude of fluid
AIw = amplitude index of water
Effectiveness of Dean-Stark (D-S) extraction AIo = amplitude index of bitumen
D = molecular diffusion coefficient
Two synthetic samples, made of sand, kaolinite rich-clay,
EC = estuarine channel
2% brine and Cold Lake heavy oil with known mass, were
G = average magnitude of the total magnetic
added into the thimble directly to ensure mass consistency.
field gradient over the entire sample
Table 7a shows the original mass for each composition. Table
mt = ore mass, g
7b is the result from the Dean-Stark extraction and Table 7c
mf = fluid mass, g
shows the mass loss by this experiment. If the efficiency about
ms = solid mass, g
Dean-Stark is expressed as: mass from Dean-Stark extraction /
SNR = signal-to-noise ratio
original mass, Table 7d shows that the D-S procedure tends to
S/V = ratio of pore surface to fluid volume
give low water mass and high oil mass. Since NMR results are
Sw = water saturation
compared against D-S values, model predictions cannot be
T2 = transverse relaxation time
expected to be better than the D-S accuracy.
T2B = T2 bulk relaxation
T2gm = T2 geometric mean
Particle size analysis TE = time echo
To further investigate the variability of ore samples and the TFS = tidal flats
ore quality, particle size distribution had been performed. Vt = ore volume
Figure 9 gives the direct sense of sand size ranges. According to Vf = fluid volume
the size class, the frequency plot (Figure 10) showed how the Vs = solid volume
EC solids and TFS solids were distributed. Table 8 confirms Greek Letters

5
 γ = gyromagnetic ratio of a proton
ρ2 = T2 surface relaxivity
ρt = true density of ore, g/cm3
ρf = fluid density, g/cm3
ρs = solid density, g/cm3
φ = porosity
Subscripts
i = index for bitumen (o) or water (w)
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16. DUNN, K.J., BERGMAN, D.J. and LATORRACA,
G.A., Nuclear Magnetic Resonance Petrophysical and
Logging Applications; Handbook of Geophysical
Exploration, Vol. 32, Pergamon Publishers, 2002.
17. FREEDMAN, R. BOYD, A., GUBELIN, G., McKEON,
D., MORRISS, C.E., and FLAUM, C., Measurement of
Total NMR porosity Adds New Value to NMR Logging;
Paper OO, SPWLA 38th Annual Logging Symposium,
1997.
18. FREEDMAN, R., Advances in NMR logging; JPT, 60-
66, January 2006.
19. CZARNECKI, J., RADOEV, B., SCHRAMM, L.L.,
SLAVCHEV, R., On the Nature of Athabasca Oil
Sands; Advances in Colloid and Interface Science 114-
115, 53-60, 2005.
20. LOWELL, S. and SHIELDS, J.E., Powder Surface Area
and Porosity; Third Edition, 1991, 250p EcoTek-FT and
FTB NMR Spectrometers User’s Guide; EcoTek
Corporation, June 2002.
21. ECOTEK CORPORATION, EcoTek-FT and FTB NMR
Spectrometers User’s Guide; June 2002.
22. NUMAR CORPORATION, User’s Guider for MRI
Echofit; NUMAR’s Corespec 100TM Echofitting
Software; 1995.
23. MALVERN INSTRUMENTS LTD., MASTERSIZER
2000 Operation Guide; MAN 0247.
24. BICHARD, A.J., Oil Sands Composition and Behaviour
Research, AOSTRA Technical Publication Series #4,
August 1987.
 Time Echo (TE), Number of B Polarization Time Number of
ms pulse (TW), s Trains

CPMG1 0.16 500 1 100

CPMG2 0.16 5000 10 40

Table 1 Two sets of CPMG parameters

CPMG1 CPMG2
EC-ore T2-cutoff Deconvolution T2-cutoff Deconvolution
Bitumen% 16.412 15.552 16.216 15.417
Water% 1.124 1.926 1.083 1.790
Fluid% 17.535 17.477 17.299 17.207
Solid% 82.465 82.523 82.701 82.793
TFS-ore T2-cutoff Deconvolution T2-cutoff Deconvolution
Bitumen% 14.020 14.043 14.819 14.844
Water% 5.599 6.126 5.744 6.280
Fluid% 19.619 20.168 20.563 21.124
Solid% 80.381 79.832 79.437 78.876

Table 2 Bitumen, Water and Solid Content Predicted by NMR Measurement

EC Bitumen TFS Bitumen

CPMG 1 CPMG 2 CPMG 1 CPMG 2
mass, g 13.76 13.76 10.67 10.67
SNR 108.33 68.26 82.90 60.00
T2gm, ms 0.53 0.59 0.53 0.60
AIo 0.057 0.053 0.058 0.056

Table 3 Bitumen NMR Outputs

EC-ore TFS-ore
D-S PV D-S PV
Bitumen% 16.537 / 13.440 /
Water% 1.069 / 6.609 /
Fluid% 17.606 17.555 20.050 19.757
Solid% 82.394 82.445 79.950 80.243

Table 4 Fluid and Solid Content from Pore-Volume Measurement and D-S

PV Fluid% NMR Sw% Oil by Difference % DS Oil% Difference

EC ore 17.555 1.083 16.472 16.537 0.065

TFS ore 19.757 5.744 14.013 13.44 -0.573

Figure 5 Comparison between the Combination of NMR vs. PV and D-S

7
 brine
syn-ore sand Cold-lake oil sand brine oil syn-ore syn-ore true
sample ID density,
tot-wt,g density,g/cm3 density,g/cm3 mass,g mass,g mass,g volume,cm3 density, g/cm3
g/cm3
syn-ore1 80.88 2.65 1.011 0.996 61.41 4.92 14.55 42.648 1.896
syn-ore2 81.18 2.65 1.011 0.996 67.65 4.54 8.99 39.045 2.079
Table 6a Synthetic Ore Density from the Known Density and Mass of Each Component

syn-ore sample sample true

sample ID syn-ore known syn-ore calculated
tot-wt,g volume, cm3 Density, g/cm3 sample ID Difference %
density, g/cm3 density, g/cm3
syn-ore1 80.88 43.115 1.876
syn-ore2 81.18 39.403 2.060 syn-ore1 1.896 1.876 1.082
Table 6b Synthetic Ore Density from syn-ore2 2.079 2.060 0.908
the Pore Volume Measurement Table 6c Difference between the Two Calculations

Table 6 Testing the Accuracy of Pore-Volume Measurement

SampleID m-sand, g m-K-clay,g 2%brine m-ColdLake Oil, g m-total, g

syn-ore1 70 10 5.045 17.66 102.705
syn-ore2 70 10 12.1 2.8 94.9

Table 7a Initial Mass Before D-S

bitumen
SampleID m-solid, g m-water, g m-oil, g Sample ID solid loss % Water loss% difference%
syn-ore1 79.98 4.8 17.925 syn-ore1 0.025 4.856 1.478
syn-ore2 80 11.62 3.28 syn-ore2 0 3.967 14.634
Table 7b Synthetic Ore Mass After D-S Table 7c Mass Loss

Sample ID solid % 2% brine Cold-Lake oil%

syn-ore1 99.975 95.144 101.501

syn-ore2 100 96.033 117.143

Table 7d Efficiency about D-S Extraction

Table 7 Testing efficiency of Dean-Stark extraction

Grain Size Description TFS solid% EC solid%

≤177µm very fine-fine sand, silt, clay 59.008 44.766

>177µm Fine sand and up 40.992 55.234

Table 8 Particle size distribution

8
 T ra n sd u c e r
G auge 6
V ent 4 5 L in e u p l e v e ls
2

Water column
N itro g e n
1 3

C e ll
7

Figure 1 System Set-up for Pore-Volume Measurement

Figure 2 The Actual Oil Sands Ore. The Left Side is EC Ore and the Right Side is TFS Ore.

Pore Volume Measurement NMR measurement Dean-Stark Extraction

Dead Volume Water Collection Dried Solid

~Two Sets of CPMG

~Repeated runs
Ore Holder Volume ~T2 cutoff Bitumen by Mass Balance

Ore Weight

Ore Volume
Particle Analysis Distribution

Figure 3 Experimental Workflow

9
 a. CPMG 1 b. CPMG 2

0.10 0.10

real Amplitude
real Amplitude
0.08 0.08

0.06 EC ore 0.06 EC ore

0.04 TFS ore 0.04 TFS ore

0.02 0.02

0.00 0.00
0.1 1.0 10.0 100.0 1000.0 10000.0 0.1 1.0 10.0 100.0 1000.0 10000.0

T2, ms T2, ms

c. EC ore under both CPMG d. TFS ore under both CPMG

0.10 0.10
real Amplitude

real Amplitude
0.08 0.08

0.06 CPMG-1 0.06 CPMG-1

0.04 CPMG-2 0.04 CPMG-2

0.02 0.02
0.00 0.00
0.1 1.0 10.0 100.0 1000.0 10000.0 0.1 1.0 10.0 100.0 1000.0 10000.0

T2, ms T2, ms

e. EC ore-decon (CPMG 1) f. EC ore - decon (CPMG 2)

0.10 0.10
abs Amplitude
real Amplitude

0.08 0.08
Ore Ore
0.06 0.06
Bitumen Oil
0.04 0.04
Water Water
0.02 0.02

0.00 0.00
0.1 1.0 10.0 100.0 1000.0 10000.0 0.1 1.0 10.0 100.0 1000.0 10000.0

T2, ms T2, ms

h. TFS ore - Decon (CPMG 2)

g. TFS ore - Decon (CPMG 1)

0.09
0.10
0.08
0.08
real Amplitude

0.07
real amplitude

Ore
0.06 Ore 0.06
0.05
Bitumen
Bitumen
0.04 0.04 Water
0.03 Water
0.02 0.02
0.01
0.00 0.00
0.1 1.0 10.0 100.0 1000.0 10000.0 0.1 1.0 10.0 100.0 1000.0 10000.0

T2, ms T2, ms

Figure 4 NMR Response for EC Ore and TFS Ore under Different CPMG Parameters

10
 Bitumen Spectra

0.09
0.08

real Amplitude
0.07
0.06 EC-oil-CPMG1
0.05 EC-oil-CPMG2
0.04 TFS-oil-CPMG1
0.03 TFS-oil-CPMG2
0.02
0.01
0.00
0.1 1.0 10.0 100.0 1000.0 10000.0

T2, ms

Figure 5 NMR Responses of Bitumen from EC Ore and TFS Ore under Different CPMG Parameters

EC ore vs. bitumen (CPMG 2) TFS ore vs. bitumen (CPMG 2)

0.09 0.09
0.08 0.08
0.07 0.07
real Amplitude
real Amplitude

0.06 0.06

0.05 EC ore 0.05 TFS ore

0.04 0.04 TFS-bitumen

EC-bitumen
0.03
0.03
0.02
0.02
0.01
0.01
0.00
0.00
0.1 1.0 10.0 100.0 1000.0 10000.0
0.1 1.0 10.0 100.0 1000.0 10000.0
T2, ms
T2, ms

Figure 6 Comparison between ore and associated bitumen

EC ore spectra - 10 subsamples TFS ore spectra - 7 subsamples

0. 10 0. 07
Normalized Amplitude

Normalized Amplitude

0. 09 EC ore1
0. 06 TFS ore1
0. 08 EC ore2
0. 05 TFS ore2
0. 07
EC ore3
0. 06 TFS ore3
0. 04
EC ore4
0. 05 TFS ore4
0. 04 EC ore5 0. 03
TFS ore5
0. 03 EC ore6 0. 02 TFS ore6
0. 02 EC ore7
0. 01 TFS ore7
0. 01
EC ore8
0. 00 0. 00
0. 1 1. 0 10. 0 100. 0 1000. 0 10000. 0 EC ore9
0. 1 1. 0 10. 0 100. 0 1000. 0 10000. 0
EC ore10
T2, ms T2, ms

Figure 8 Normalized Spectra for all sub-samples

11
 a. EC-Fluid b. EC-Solid

0.6
2.5
0.5
2.0
0.4

mass%
1.5 DS vs NMR
mass%

DS vs NMR
0.3
PV vs NMR PV vs NMR
1.0
0.2

0.5 0.1

0.0 0.0
CPMG1- CPMG1- CPMG2- CPMG2- CPMG1- CPMG1- CPMG2- CPMG2-
T 2cutoff Decon T 2cutoff Decon T 2cut off Decon T 2cutoff Decon

c. TFS-Fluid d. TFS-Solid

8.0 2.0

6.0 mass% 1.5

mass%

DS vs NMR DS vs NMR
4.0 1.0
PV vs NMR PV vs NMR

2.0 0.5

0.0 0.0
CPMG1- CPMG1- CPMG2- CPMG2- CPMG1- CPMG1- CPMG2- CPMG2-
T 2cut off Decon T 2cutoff Decon T 2cutoff Decon T 2cutoff Decon

e. TFS-Fluid f. TFS-Solid
(Fluid density = 1.02 g/cm3) (Fluid density = 1.02 g/cm3)

6.0 1.5

4.0 1.0
mass%

mass%

DS vs NMR DS vs NMR

PV vs NMR PV vs NMR
2.0 0.5

0.0 0.0
CPMG1- CPMG1- CPMG2- CPMG2- CPMG1- CPMG1- CPMG2- CPMG2-
T 2cut off Decon T 2cutoff Decon T 2cutoff Decon T 2cutoff Decon

Figure 7 Result Comparison

12
 Figure 9 Sand Size Ranges

EC vs TFS PSD

35.0

30.0
Sample Percentage

25.0

20.0 EC-solid
15.0 TFS-solid

10.0

5.0

0.0
0-2 0-44 44-62 62-88 88-125 125- 177- 250- 350- 500- 710-
177 250 350 500 710 2000

Size Band, micron

Figure 10 Particle Distribution for EC solid and TFS solid

13