Determining Wax Type: Paraffin

or Naphthene?
Mark M. Bacon, SPE, and Laura B. Romero-Zern, SPE, University of New Brunswick,
and Ken K. Chong, SPE, Core Laboratories

Summary
Paraffin-wax deposits are known to be a worldwide problem in the
upstream petroleum industry. Considerable resources are expended
on inhibiting or removing wax deposits every year. Paraffin wax is
not the only type of crude-oil-based wax. Microcrystalline waxes,
composed of naphthene and iso-paraffin molecules, also exist but
are not well studied. The predominance of paraffin (also called
macrocrystalline) wax and paraffin-wax-inhibition techniques will
likely lead to paraffin-wax treatments being applied to naphthenebased reservoirs. It is unclear how well a paraffin-based treatment
will apply to naphthene-based oil.
The current study investigates the use of cross-polarized microscopy (CPM) to determine if a crude oil contains macrocrystalline
or microcrystalline waxes. The type of wax present in the crude oil
can be determined using crystal morphology and size. This study
demonstrates that paraffin-wax crystals are elongated structures with
statistically larger sizes than the microcrystals. Microcrystalline
waxes are shown to be statistically smaller and rounded structures.
Introduction
Wax deposition in production facilities and pipelines is a problem
that costs the upstream petroleum industry billions of dollars
worldwide every year (Bello et al. 2006). The deposits can plug
pipelines or seize equipment, leading to costly downtime and expensive remediation techniques. Wax deposition has been extensively
studied for paraffin wax, but research concerning iso-paraffinic and
naphthenic (cycloparaffin) wax is limited (Bello et al. 2006; Hammami and Raines 1999; Dobbs 1999). Currently, no definitive tests
exist to determine if a wax is paraffin- or naphthene-based. This
situation, coupled with the predominance of paraffin-wax treatments, will likely lead to paraffin-wax treatments being applied to
reservoirs that may be naphthene-based.
Wax Classification. A common classification of oil is by base type
(Speight 1999). Traditionally, oils are paraffin-based if paraffin
wax separates from the oil on cooling and asphalt-based if there is
no separation of paraffin wax. In more recent years, this definition
has been replaced by referring to the wax itself as either being macrocrystalline or microcrystalline (Garcia et al. 1998; Kumar et al.
2004; Dorset 2000; Elsharkawy et al. 2000). Macrocrystalline wax
is the most common and is composed of mostly straight-chain paraffins, while microcrystalline waxes are composed of high amounts of
naphthenic and iso-paraffinic components (Dorset 2000; Elsharkawy
et al. 2000). In some publications, macrocrystalline waxes are
simply referred to as paraffin waxes and microcrystalline waxes are
known as amorphous waxes, or mal-crystals (Kumar et al. 2004;
Elsharkawy et al. 2000; Dorset 2000).
The distinction between micro- and macrocrystalline waxes
is based on the size and shape of the individual crystals. Paraffin
crystals have been extensively studied and are known to be elongated structures in the form of rods, plates, and needles (Garcia
et al. 1998; Kan et al. 2002; Mendell and Jessen 1970). Vignati
et al. (2005) have shown that n-paraffin crystals are smaller in

Copyright 2010 Society of Petroleum Engineers

This paper (SPE 124799) was accepted for presentation at the SPE Annual Technical
Conference and Exhibition, New Orleans, 47 October 2009, and revised for publication.
Original manuscript received for review 9 September 2009. Revised manuscript received
for review 3 March 2010. Paper peer approved 8 March 2010.

December 2010 SPE Journal

the presence of iso-paraffins, suggesting that the presence of the

branched paraffins inhibits crystal growth. Hammami and Raines
(1999) explain that the branched structure of iso-paraffins leads to
delayed formation of wax nuclei and formation of unstable wax
solids. They also explain that naphthenes disrupt wax nucleation
and growth processes. In the case of microcrystalline wax, its morphology has been observed as far back as Guthrie (1960) as small,
rounded structures in comparison with paraffin crystals. These
earlier studies demonstrated that macrocrystalline (paraffin) waxes
have larger, elongated structures, while microcrystalline (naphthene and iso-paraffin) waxes have smaller, rounded structures.
CPM. CPM can be used to find the structure of wax crystals. CPM
is commonly used for determining the wax appearance temperature, or cloud point, of a crude oil (Hammami and Raines 1999;
Ferworn et al. 1997). It works on the principle that wax crystals
rotate the plane of polarized light (the crystals are referred to as
anisotropic). The use of two prisms in a cross-polar microscope
allows the field of view within the microscope to initially appear
black, but, when crystals are introduced to the system, they appear
as white spots because of the rotation of polarized light. This can
be used to determine the size and structure of any anisotropic wax
crystals (Kan et al. 2002). This direct microscopic view of wax
crystals is used to detect the formation of crystals as small as 1 m
(Hammami and Raines 1999).
Stoney Creek Oil Field. The Stoney Creek oil field, located
outside of Moncton, New Brunswick, Canada, produced oil and
gas for more than 80 years but was eventually shut down in 1991
because of production challenges and the relatively low price of oil
(Foley 1989). The field has produced roughly 1 million bbl of the
18 million bbl estimated to be in place originally, representing less
than 6% recovery to date (Leatherbarrow 1984). The field resumed
commercial production in 2007, but the same production challenges
were observed. The crude-oil flow from the field has always been
erratic in that a well will flow for a certain period of time and then
stop production for a random period of time. The cause of this was
thought to be paraffin-wax deposition (Henderson 1940; Coldham
1988). Because the field had been identified historically as having
a paraffin-wax-deposition problem, a paraffin-wax treatment had
been applied. At the time, it was thought that periodic wax formation was causing the erratic production. The treatment proved to be
unsuccessful. This failed field treatment prompted this study into the
determination of the Stoney Creek crude-oil chemistry.
This study was conducted on multiple oil samples, aiming
to determine the Stoney Creek oil base type. The comparison of
Stoney Creek crude oil to some well-known naphthenic and paraffinic reservoirs through CPM provides evidence of the naphthenic
nature of this oil.
Experimental
Samples tested under CPM were as follows: a Stoney Creek crude
oil, a Stoney Creek wax deposit, a pure paraffin wax, a condensate
oil from New Brunswick, a Canadian bitumen sample, and two
known naphthenic North Sea crude oils. For the rest of this paper,
the samples will be referred to as SC crude, SC deposit, paraffin,
condensate, bitumen, and North Sea crude, respectively.
Wax Preparation by Units of Production (UOP) Method 46-85.
With the exception of the paraffin sample and the SC deposit, all
969

other samples arrived as liquid. The cross-polar microscope used

did not have any temperature-control capabilities, so the wax
fraction had to be separated from the samples before CPM could
be used.
The standard UOP 46-85 (Paraffin Wax Content of Petroleum
Oils and Asphalts) had been previously applied to Stoney Creek oil.
The typical expected result of the UOP 46-85 test is a white filter
cake of pure paraffin wax. For Stoney Creek samples, the filter cake
was black with small white agglomerations of crystals throughout
the cake. It is thought that the white agglomerations are paraffin
wax while the predominant black wax is likely naphthenes or some
other component specific to Stoney Creek depositional history. For
the purposes of this paper, the black filter cake was taken as being
a representative wax sample of the Stoney Creek oil.
The bitumen and condensate samples were the only oils that
performed as expected under the UOP 46-85 test, giving white
to yellowish-white filter cakes with no modifications of the testing procedure. For the Stoney Creek and North Sea oils, several
modifications of the UOP 46-85 test were necessary in this work.
The basic procedure is described below:
1. The sample is dissolved in hexane and boiled on a hot plate.
Sulfuric acid is then added, and the mixture is heated until an acid
tar is formed.
2. The solution is then decanted into a separatory funnel, where it
is washed with warm water, hexane, and then warm water again.
3. The final part of the procedure is to evaporate all remaining
hexane and dissolve the remaining wax in methylene chloride.
The mixture is then cooled to 30C and filtered through a cold
fritted glass funnel.
For a typical paraffinic oil, an acid tar will be easily formed in
Step 1. The tar (mostly composed of asphaltenes) will agglomerate
in the flask, and only the remaining solution will be decanted into
the separatory funnel in Step 2. While in the separatory funnel,
the solution will form two distinct layers, one clear layer (water
or hexane) and a yellow layer (paraffin). This yellow layer is then
cooled and separated in the fritted funnel, as in Step 3. The result
of the test is a white to yellowish filter cake left on the fritted
funnel. This filter cake is paraffin wax.
For a naphthenic oil, the test becomes more complicated. The
UOP 46-85 modified procedure is described here. The expected
acid tar from Step 1 does not form, so there is no solid asphaltene
agglomeration. Because there is no agglomeration, the entire mixture is poured into the separatory funnel in Step 2. Three distinct
layers are formed for the naphthenic oils. The top layer is not the
yellowish color expected with paraffinic oils; it is a dark brown or
black. The middle layer is still a clear, water layer. A new, bottom
layer is seen composed of nearly black, heavy components. This
bottom dark layer is discarded (so is the asphaltene agglomeration
for the paraffinic oils). Another distinct difference is the formation
of stable emulsions in the separatory funnel in Step 2; these do
not occur for paraffinic oils. The warm water must be added very
slowly, along the side of the separatory funnel, to prevent these
emulsions from occurring. Once formed, the emulsions are stable
for months; therefore, this must be avoided. The top, dark layer
formed in the separatory funnel is filtered through the cold fritted
funnel, and the result from Step 3 is a black filter cake, occasionally with small white crystals seen in the filter.
To ensure reproducibility of results, both the modified and
unmodified UOP 46-85 procedure were performed in the same
time frame (approximately 9 hours of preparation, followed by 15
hours of cooling before the wax samples were examined). It is well
known that cooling rate affects crystal size, so, to be sure that the
results are comparable, the same cooling time and rate were used
for both the modified and unmodified UOP 46-85 procedure. Also,
to be certain that the UOP 46-85 was not forcing certain crystals
to change morphology or size, a sample was run once using the
UOP 46-85 modification to obtain pure wax and once without any
UOP 46-85 modification.
This modified procedure yields some unusually high wax
contents for the Stoney Creek oil, with some samples having wax
contents of nearly 70%. If this procedure returns a 70% paraffinwax content, it is likely that the Stoney Creek oil would be solid
970

at room temperature. This fact supports the hypothesis that the

modified UOP 46-85 test was not just precipitating paraffin wax,
but was likely also precipitating microcrystalline wax.
The wax resulting from the UOP 46-85 modified procedure
was taken and analyzed for wax crystal size and morphology under
CPM. The wax fractions for the SC crude, North Sea crude, bitumen, and condensate sample were obtained by this procedure. The
SC deposit was run through CPM, both as the unmodified pure
deposit and as the deposit after being prepared by the modified
UOP 46-85 test. The paraffin sample was analyzed as obtained
without any modification.
CPM. As previously stated, CPM is a technique normally used to
view wax crystals upon the cooling of crude oil. For this study,
the UOP 46-85 procedure was used to produce bulk-crystallized
fractions of crude oil wax. It is important to note the distinction
between viewing waxes under cooling conditions and the bulkcrystallized fractions used in this study. The UOP 46-85 method
to produce these bulk wax crystals does not significantly affect the
crystal size, as seen in the results of this study.
The microscope used was a Zeiss AxioImager polarizing microscope operated by the University of New Brunswick Geology
Department. This polarizing microscope is equipped with encoded
objective lenses (i.e., field of view for each magnification stored
in the software), a dedicated Zeiss AxioCam ICc3 digital camera
head, and supported by Zeiss AxioVision v. 4.7 image acquisition and processing software. The samples were studied using
cross-polarized transmitted light in orthoscopic (2.5X to 10X) and
conoscopic (20X to 50X) illumination. The length of anisotropic
target crystals in the field of view was measured manually using
the AxioVision software, with each measurement automatically
written to an associated spreadsheet file. These data sets were
subsequently processed offline. The pixel dimension for each
image was established automatically on the basis of the respective
objective encoding.
Under CPM, some crystals were easier to see than others (they
are whiter), so only crystals that appear as the brightest shade of
white were measured. Both small, rounded structures and elongated structures were measured. The size was recorded in micrometers, with approximately 60 to 200 crystals in each field of view.
For consistency, crystal sizes were reported as the longest distance
from end to end of any given crystal.
On occasion, under CPM, it can be difficult to observe wax
crystals. In those cases, the sample was usually too thick; to prevent
this from happening, the sample was dissolved in hexane and then
dropped onto the microscope slide. The hexane was then allowed
to evaporate, leaving a thin film of wax.
Results and Discussion
The resultant pure and UOP 46-85 prepared waxes were run
through CPM, and several of the images captured are shown in
Figs. 1 through 8. The images are shown at 200X magnification
for easy comparison of crystal size and morphology. Images were
taken at several other magnifications, but 200X gave the best
overall view of the crystals. It should be noted that these images
are presented as representative images with the largest countable
number of crystals possible in a field of view. It is also useful to
note that the CPM images in this paper are designed for printed
viewing, and the wax crystals tend to be easier to see in a printed
format rather than on a computer monitor.
Figs. 1 and 2 are given as much larger photographs to give
representative views of the types of crystals present in these
waxes. Fig. 1 shows the pure paraffin wax without any UOP 46-85
test preparation. It is easy to see that nearly all of the elongated
crystal structures (corresponding to straight chain paraffins) are in
agreement with the paraffin morphology reported in the literature.
Several agglomerations were seen, but these groupings were not
considered when measuring crystal size. Fig. 2 shows the wax
crystals present in the pure SC deposit sample. There was a predominance of much smaller and rounder crystals in comparison to
the paraffin-wax sample. This coincided with the expected smaller
structures present in microcrystalline waxes.
December 2010 SPE Journal

Fig. 1CPM image of pure paraffin wax without any UOP 46-85 preparation at 200X.

Fig. 3 shows the CPM image of the modified UOP 46-85 prepared condensate sample. It shows the same elongated structures
seen in Fig. 1, the pure paraffin wax. During the UOP 46-85 preparation of the condensate sample, it behaved exactly as expected.
In this case, clear layers were formed and the final product was
a yellowish-white wax cake. Condensates are generally known to
be paraffinic, so the macrocrystalline wax crystals observed under
CPM are in agreement with previous studies.
Fig. 4 is a representative image of the two different known
naphthenic North Sea crude oils. The sample was prepared using
the UOP 46-85 method and resulted in a darker yellow wax than

the condensate sample. Under CPM, the crystals were difficult to

see because they were substantially smaller than the wax crystals
of any other samples. This result is in agreement with previous
research indicating that crystal size in waxes is dependent on the
composition of the crude oil (Anderson et al. 2001). Fig. 4 does
show that the North Sea crude presents with very small, rounded
structures, indicating microcrystalline wax. The two North Sea
samples used have always been identified as being naphthenic oil,
and this result validates those findings.
The bitumen sample shown in Fig. 5 had some difficult preparation issues. Bitumen is a biodegraded type of oil known for its high

Fig. 2CPM image of SC deposit wax without any UOP 46-85 preparation at 200X.
December 2010 SPE Journal

971

Fig. 3CPM image of condensate wax with UOP 46-85 preparation at 200X.

Fig. 4CPM image of North Sea crude wax with UOP 46-85
preparation at 200X.

Fig. 5CPM image of bitumen wax with UOP 46-85 preparation at 200X.

Fig. 6CPM image of SC crude wax with UOP 46-85 preparation at 200X.

asphaltene content. The biodegradation process involves microbes that

can digest paraffin molecules so that most of what remains in bitumen
is asphaltenes and naphthenes. This leads to a UOP 46-85 preparation,
which results in a large amount of discarded acid tar (which consists
partially of asphaltenes) and little wax product at the end. This wax

product under CPM shows fewer crystals than previous samples, but
they are all seen to be small, rounded structures. These small crystals
are in agreement with the naphthenic nature of bitumen.
The Stoney Creek samples are seen in Figs. 6 through 8. Fig. 6
shows the modified UOP 46-85 prepared wax from one of the wells

Fig. 7CPM image of SC deposit wax without UOP 46-85

preparation at 200X.

Fig. 8CPM image of SC deposit wax with UOP 46-85 preparation at 200X.

972

December 2010 SPE Journal

TABLE 1CRYSTAL SIZE SUMMARY FROM VARIOUS SAMPLES USING 200X CPM
Number of O bse r v ati ons

Mean (m)

Standard Deviation

P a ra f fi n

72

12.9

5 .8

Condensate

11 4

5 .4

2.0

Macrocrystalline Wax

Microcrystalline Wax
North Sea cr ude

151

1. 7

0.5

Bitumen

64

4 .0

2. 0
2 .1

SC crude

93

3.5

SC deposit with UOP wax preparation

15 1

3. 2

1 .4

SC deposit without UOP wax preparation

2 02

3. 5

1 .6

of the Stoney Creek field. In this image, the crystals have the same
rounded structure but are larger than the crystals from the North
Sea crude. The size of these crystals is very similar to the size of
bitumen crystals analyzed in this study.
Figs. 7 and 8 are images of the SC deposit that compare a
sample before the UOP 46-85 separation and after the UOP 46-85
wax separation. It is known that the rate of cooling will affect
crystal size (Anderson et al. 2001). Because UOP 46-85 involves
several stages in which the wax is heated and cooled, a comparison
between a sample with the UOP 46-85 preparation and one without
UOP 46-85 preparation was necessary. From the two figures, it
is seen that both samples contained small, rounded structures of
approximately the same size. Visually, it appears that there is little
difference in crystal size for the SC deposit with or without the
UOP 46-85 preparation. This shows that the UOP 46-85 procedure
is not affecting crystal size.
In Figs. 6 through 8, the Stoney Creek samples show small,
rounded structures. All other CPM images of Stoney Creek samples not presented here agree with this conclusion.
A purely visual observation from the CPM experiments indicates that the paraffin and condensate samples show elongated
structures, with the condensate wax crystals being smaller. It is
also seen that all the other samples show small, rounded structures,
with the North Sea samples having the smallest crystals and all
the others being approximately the same size. For all the samples
evaluated in this work, the crystal size was measured and a statistical analysis was conducted. Table 1 shows crystal size data
and additional information, such as mean and standard deviation.
Table 2 shows the statistical analysis of the data from Table 1 in
the form of a t-test.
To compare if the crystal size means vary in a significant way
from two different data sets, a Students t-test was applied. This
type of test can statistically determine how likely it is that two
sets of data have the same mean. In this case, the test was used
to determine if the crystal size, on average, of one sample is the
same as that of another sample. The data obtained for crystal size
by CPM in this study differed slightly from normal distribution. In
this case, the deviation from the normal distribution is acceptable

because the t-test is known to be insensitive to deviations from

normal distribution provided the data set is large enough (Everitt
2002). This study was performed at a 95% confidence level, so
any probabilities below 0.05 confirm that the mean is statistically
different.
The results shown in Table 1 indicate that the mean of the
macrocrystalline wax size obtained from paraffin (12.9 m) and
condensate (5.4 m) samples is larger than the mean size of any
of the microcrystalline waxes evaluated, as was expected from
visual inspection. The microcrystalline waxes have very similar
crystal sizes (ranging from 3.2 to 4 m), with the exception of the
North Sea crude (1.7 m), which was also expected from simple
visual inspection. Table 1, however, does show that the standard
deviations on the mean crystal sizes are large enough that another
statistical method must be applied before the mean crystal sizes
can be compared. The t-test analysis at a confidence interval of
95% was conducted, and the results of the statistical analysis are
presented in Table 2.
Table 2 shows that the paraffin sample crystals are statistically
larger than the condensate sample crystals. The condensate crystals
are also seen to be statistically larger than the bitumen crystals,
which are the largest of the microcrystalline waxes evaluated.
These observations clearly indicate that all of the macrocrystalline
crystals are statistically larger than the microcrystalline crystals.
Within the microcrystalline waxes, the North Sea wax crystal size
is statistically smaller than all of the other microcrystalline waxes.
The remaining microcrystalline waxes (SC deposit with UOP
preparation, SC deposit without UOP preparation, SC crude, and
bitumen) all have crystals of statistically the same size. To summarize, the order of crystal sizes from larger to smaller is paraffin >
condensate > SC deposit without UOP = SC deposit with UOP =
SC crude = bitumen > North Sea.
Future Work
This paper was intended to set the framework for ultimately demonstrating that CPM can aid in optimizing wax-treatment methods.
The purpose of this paper is to show that CPM is a simple and
effective tool to visualize the size and morphology of wax crystals.

TABLE 2PAIRED t-TEST ANALYSIS ON DATA FROM TABLE 1 AT A CONFIDENCE INTERVAL OF 95%
Sample Crude Oil A

Sample Crude Oil B

Probability

Means significantly different?

17

Yes

Yes

Paraffin

Condensate

5.4410

Condensate

B itume n

2 .45 10

North Sea

B itum en

6.7710

13

Yes

North Sea

SC crude

3 .9 3 1 0

11

Yes

North Sea

SC deposit with UOP

3.9410

23

Yes

Bitumen

S C crude

0. 124

No

Bitumen

SC deposit without UOP

0.059

No

SC deposit with UOP

SC deposit without UOP

0. 0 8 1

No

December 2010 SPE Journal

973

This allows the identification of the type of wax and establishes

the difference between paraffin and naphthenic waxes. Future work
will demonstrate that CPM can be used to observe changes in wax
crystal size and morphology after being treated with a wax inhibitor. In conjunction with viscosity and pour-point changes, this will
be a valuable addition to optimizing wax-treatment methods.
Conclusions
Several oil samples were obtained from various sources to establish
their crystal structure size and morphology. Two of the samples
naturally existed as a wax, but the remaining wax samples were
separated from the oil source by using either the original UOP 4685 test or a modified version of the UOP 46-85 test for paraffin-wax
content. The pure and precipitated waxes were viewed under a
cross-polarized microscope. The anisotropic nature of wax crystals
allows their size and shape to be determined by CPM. Macrocrystalline (paraffin) waxes were found to have larger, elongated
structures compared with the smaller, rounded microcrystalline
(naphthene and iso-paraffin) waxes. It was statistically demonstrated that paraffin crystals are the largest of the wax samples
studied. The bitumen and Stoney Creek samples have the same
size microcrystals, and the known naphthenic North Sea crude
shows similar microcrystals of a much smaller size. CPM was
seen to be a simple and effective way to determine the base type
of oil through the identification of wax-crystal morphology. When
viewed by means of CPM, paraffin-based crude oils have elongated
wax crystals while naphthenic and iso-paraffinic crude oils have
rounded and smaller wax crystals.
Acknowledgments
The authors would like to thank Darcy Spady, Terry Brown, Edwin
Macdonald, and Glen Northrup from Contact Exploration for their
continuous support and for allowing the publication of these results.
We would also like to thank Contact Exploration and NSERC-CRD
for financial support. Thanks to Chris McFarlane for CPM training
and for allowing us to use the cross-polar microscope, and to Xu
Liang Li for helping with the UOP wax preparation.
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Mark Bacon, SPE, is currently a thermal system sales and service representative for Champion Technologies specializing in
team-assisted gravity drainage projects in Alberta, Canada. His
research interests include crude-oil characterization, thermal
recovery, and wax characteristics. He holds a BS double major
degree in biology and chemistry from Acadia University and an
MS degree in chemical engineering from the University of New
Brunswick. Laura Romero-Zern, SPE, is currently an associate
professor at the Chemical Engineering Department, University
of New Brunswick. Her research interests include crude-oil characterization, chemical and polymer flooding, polymer-gel and
foam-gels applications for reservoir conformance improvement, among others. She holds a PhD degree in chemical and
petroleum engineering from the University of Calgary, Alberta,
Canada. Ken Chong, SPE, is reservoir fluids manager with Core
Laboratories in Calgary, Alberta, Canada. He has 20 years of
experience in oil- and gas-production-related chemistry. He
holds a BS double major degree in chemistry and biochemistry from the University of Victoria, a PhD degree in applied
chemistry, and an MBA degree from the University of Calgary.
He was a Natural Sciences and Engineering Research Council
post-doctoral fellow with Imperial Oil.

December 2010 SPE Journal