SPE 64992
Paraffin Deposition in Oil Production
María del Carmen García, SPE, PDVSA-Intevep
Copyright 2001, Society of Petroleum Engineers Inc.
This paper was prepared for presentation at the 2001 SPE International Symposium on
Oilfield Chemistry held in Houston, Texas, 13–16 February 2001.
This paper was selected for presentation by an SPE Program Committee following review of
information contained in an abstract submitted by the author(s). Contents of the paper, as
presented, have not been reviewed by the Society of Petroleum Engineers and are subject to
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Abstract
Paraffin deposition problems in oil production, transportation
and storage will be presented. An experimental methodology
for deposits characterization and paraffin deposition control,
oriented toward the identification of “tailor made” preventive
or remedial treatments, will be shown. Research results
including some correlations between oil composition and wax
appearance temperature (WAT), as well as paraffin inhibitors
efficiency, will be presented. The knowledge provided in this
paper has direct application to paraffinic crude oils
productivity enhancement in terms of costs reduction
(cleaning and deposits removal), and oil production
improvement. On the other hand, correct selection of a
prevention treatment will avoid extremely expensive and
inefficient “trial-and-error” procedures, and even severe
formation damages due to eventually paraffin deposition in the
reservoir. This last phenomenon can be a consequence of the
precipitation of crude oil paraffin’s heaviest components after
improper operations, like “hot-oil” treatments. The designed
experimental strategy starts with the deposit analysis, which
includes a preliminary physical separation of the organic and
inorganic components. The organic fraction characterization,
in terms of its hydrocarbon components, allows to
discriminate between wax and asphaltenes plugging. Once the
paraffin deposition problem is identified, the original crude oil
characterization is carried out. Specific compositional
characteristics of the crude oil allow to select an adequate
paraffin deposition treatment, based on previously established
correlations. An example selected from field operations
carried out in Venezuelan facilities, will illustrate the benefits
derived from this methodology.
Introduction
Wax deposition during paraffinic crude oil production and
transport is one of the most serious problems faced in
downhole and surface operations. These deposits are mainly
constituted by n-paraffins (linear alkanes) and small amounts
of branched paraffins and aromatic compounds.1 Naphthenic
(cyclic) and long chain paraffins also have a notorious
contribution to microcrystalline waxes and have remarkable
influences on macrocrystalline growing patterns. 2 The carbon
number of paraffinic molecules present in wax deposits is
known to be higher than 15 atoms. Advanced analytical
techniques had allowed to detect up to 160 carbon atoms in
these deposits.3-12
It has been found that light paraffinic fractions along with
the absence of a well defined maximum or a multimodal shape
of the carbon number distribution curve, are responsible for
keeping the crude oil pour point low enough even at high
concentrations of heavier paraffins.13 A good correlation
between oil composition and polymeric paraffin inhibitors
activity was recently found.14-20 Paraffinic crude oils have
been classified into two structural categories, considering their
molecular weight distribution, C24+ paraffins concentration
and (n-/cyclo+isoparaffins) ratio. Also, different responses to
commercial paraffin inhibitors were obtained by these two
crude oil types, assessing the inefficiency of some paraffin
inhibitors for crudes rich in C24+ alkanes.15 It was
demonstrated, through these previous studies, that there is a
complex interaction between crude oil fractions (specially
paraffin classes distribution) and the tendency of the crude oil
to precipitate wax.
There are numerous methods used to handle paraffin
deposition. These can be divided into two categories: removal
(mechanical, thermal, chemical) and prevention or inhibition
(dispersants, crystal modifiers). Usage of an effective paraffin
inhibitor has a potential for significant savings versus removal
procedures. Since paraffin characteristics and contents vary
drastically from reservoir to reservoir, production problems
and solutions also vary. Methods that are effective in one
system are not always successful in other reservoirs or even in
various wells within the same reservoir.21
The main goal of this work was to design an experimental
methodology for deposits characterization and paraffin
deposition control treatments, oriented toward the
identification of “tailor made” preventive or remedial actions,
adequate for the particular crude oil composition and
2 MARÍA DEL CARMEN GARCÍA
physicochemical properties. This technique has direct
application to paraffinic crude oils productivity enhancement
in terms of costs reduction, and oil production improvement,
avoiding extremely expensive and inefficient “trial-and-error”
procedures.
Experimental
Samples
7 paraffinic crude oils (tank or dead oils) from Venezuelan
reservoirs (reference oils), and 11 commercial paraffin
inhibitors were used for this study. For the case history, 50 g
of a deposit, obtained after pigging the production tubing of a
paraffinic crude from an Eastern Venezuela reservoir well,
were studied. The sample, a waxy brown solid with a strong
hydrocarbon odor, resembled the tubing inner wall shape and
was very difficult to pulverize due to its hardness (see Fig. 1).
Additionally, a sample of the crude oil produced in the same
well was received for characterization studies.
Reference Crude Oils Characterization
Physicochemical properties (pour point and API gravity) as
well as wax content and carbon number - molecular weight
distribution of the 7 reference crude oils were measured.
Crude Oil Physico-Chemical Properties. Pour point
measurements were made following the ASTM D-97 method
(values in °C). API gravity was determined following ASTM
D1298 method (values in °API at 60 °C).14-15
Wax content. Wax fraction quantification in crude oils was
performed by a combination of two previously reported
analytical methods.14,15,23,24 The method involves removal of
polar materials, followed by precipitation and cold filtration
employing methyl ethyl ketone (MEK) as solvent and a
temperature of -30 °C. 25 These drastic conditions allowed an
exhaustive wax separation due to the short chain of the solvent
and the very low temperature used.26
Carbon Number Distribution. High Temperature
Simulated Distillation (HTSD) boiling range analysis was
performed on a Hewlett-Packard HP-5890 equipment with an
AC TBP 750 configuration developed by Analytical Control.
The column used was an HT HP cross-linked methyl silicone,
whose dimensions were 0.53 mm id. x 5 m l., 0.09 µm film
thickness,. The oven temperature was programmed within a 40
- 430 °C range at 10 °C/min, keeping the final temperature for
10 minutes. The injector temperature was programmed within
a 100 - 430 °C range at 25 °C/min, and the FID detector
temperature was maintained at 450 °C all along the run. The
He carrier gas flow was set at 20 mL/min. Sample solutions
were prepared by dissolving 100 mg of crude oil in 1 mL of
carbon disulfide (CS2, Fisher analytical grade), to make a
concentration of 10 % wt/v. The injection volume was 1.5 µL.
This technique allowed to obtain the carbon number
distribution of the crude oil paraffinic components by
comparison with paraffin references. Also the concentration of
C24- components was obtained from the distillation curve.
Molecular Weight Distribution. The crude sample was
analyzed by gel permeation chromatography (GPC) in order to
obtain its molecular weight distribution. Two 7.5 mm id. x 30
SPE 64992
cm l. columns, in series, were used. 102 - 107 Å (Mixed) and
100 Å styrene-divinyl benzene gels were the nominal pore
sizes of the packing material. Toluene was used as diluent
(Sigma-Aldrich, HPLC grade), set at a flow rate of 1 mL/min.
Differential refractive index was selected for detection and the
whole system was maintained at 40°C. 70 µL of sample
solution (0.1 % w/v) was injected. Calibration was performed
with C12-C38 paraffins.14,15
Deposit Analysis
Deposit analysis techniques included solubility studies,
separation of the organic and inorganic fractions, and organic
portion characterization (hydrocarbon families and boiling
point distribution)
Solubility tests. The solubility of the deposit in different
organic solvents (methylene chloride, chloroform, n-heptane,
benzene, toluene and xylene), ranging from room temperature
up to the solvent boiling point, was evaluated in a qualitative
way (visual test for turbidity).
Polarity fractions separation. Deposit solubility fractions
were separated following the sequence shown in Fig. 2. 20 g
of the deposit were placed in a Soxhlet extractor, fitted with a
round bottomed flask containing 400 mL of a methylene
chloride / methanol 95:5 mixture, a reflux condenser, a
magnetic stirrer and a heating mantle. The sample was
extracted for 21 h, followed by another extraction step with a
mixture of toluene / iso-propanol 95:5 (24 h), and then with
xylene / n-buthanol 95:5 for other 24 h. The three extraction
solutions were evaporated in a rotary evaporator to dryness,
until constant weight was achieved.
Carbon Number Distribution. High Temperature
Simulated Distillation (HTSD) boiling range analysis was
performed at the same conditions described above.
Hydrocarbon families determination in the organic
fractions. Saturate, aromatic, resin and asphaltene
hydrocarbon family concentrations (S.A.R.A.) were measured
by means of Thin Layer Chromatography with Flame
Ionization Detection (TLC-FID), as previously described.22
The concentrations are given in weight %. For heavy
paraffinic fractions it was necessary to rise the toluene elution
temperature up to 70 °C, in order to avoid their retention in the
origin, due to crystallization during elution.
M-2 Crude Oil Characterization
M-2 crude oil wax content, carbon number and molecular
weight distribution (HTSD and GPC), and hydrocarbon
families determination (S.A.R.A. by TLC-FID), was
performed using the experimental procedures described above
for the reference crude oils and deposit.
Chemical Treatment Selection. Additives activity was
evaluated by the addition of 4000 ppm of the commercial
product to the crude under study. After mild heating and
thoroughly homogenization, pour point measurements were
made, using ASTM-97 standard method. Crude samples with
no additives were used as controls for each determination.
SPE 64992 PARAFFIN DEPOSITION IN OIL PRODUCTION
Results and Discussion
Reference Crude Oils Characterization
As shown in Table 1, crudes M-4, N-9, N-4 and N-6 afforded
the highest wax content values among the 7 reference crude
oils, ranging from 40 to 53 wt %. Additionally, these oils have
the lowest concentrations of C24- hydrocarbons (23 to 48). On
the other hand, there is a slight, but not negligible, difference
in pour points and API gravity between both groups of crude
oils. All these characteristics, besides the monomodal GPC
molecular weight distribution curve, and the narrow HTSD
chromatograms, afforded by the first 4 crude oils, allow us to
group them into Type I oil category. 14,15 These crude oils also
have a characteristic physical behavior that affect field
operations due to severe paraffin deposition during
production, transport and storage. They are also resistant upon
the addition of paraffin inhibitors, which represents an
additional difficulty to the paraffin deposition control
management (Table 2).
The last 3 crude oils, corresponding to the Type II
category, have smaller wax contents (24 to 33 wt %), larger
C24- hydrocarbon concentrations (61 to 69 wt %), lower pour
points and higher API gravities (Table 1). They also respond
to the addition of some of the commercial paraffin inhibitors
evaluated in this job (A2, 2B, C9 and D7), showing significant
pour point depressions when compared with untreated samples
of the same crude oils (Table 2).
M-2 Deposit Analysis Crude Oil Characterization
Dissolution tests performed in M-2 deposit afforded a very
low solubility in organic solvents at room temperature.
Improved dissolution was obtained when the temperature was
increased. Xylene showed the best behavior when used as
solvent at 65°C.
Deposit continuous extraction, with different organic
solvent mixtures, allowed us to assess the mass balance shown
in Table 3. It was found that the sample contained more than
99 wt% of organic materials. The “Organic 3” fraction
constituted 45 wt% of the deposit, representing a significant
proportion of heavy hydrocarbons, which are soluble only in
high boiling point organic solvents, as found also in the
solubility tests described above.
HTSD of the three organic fractions of the deposit, and
M-2 crude oil afforded the C24- concentrations found in
Table 3. Chromatograms of M-2 crude oil and one of the
fractions are shown in Fig. 3. These results are in accordance
with the solubility experiments, in terms of the significant
abundance of heavy (C24+) hydrocarbons in “Organic 2 and
3” fractions (molecular weight distribution from C40 up to
C120). “Organic 1” fraction and M-2 crude oil have the same
C24- concentration (65 wt%), with a distribution between C11
and C52 (mean in C26), and also identical HTSD
chromatograms, which suggests that this particular fraction
consists of adsorbed crude on the deposit surface. The crude is
washed out in the first extraction step, leaving the deposit free
on any other materials but the heavy hydrocarbons.
The extracted organic fractions and M-2 crude oil
characterization by means of TLC/FID are in accordance with
3
the former findings, as shown in Table 3. “Organic 1” fraction
has approximately the same composition than M-2. On the
other hand, “Organic 2 and 3” fractions are rich in saturate
compounds, result that, along with the high wax content in M-
2 crude oil (37.35 wt%), confirms the paraffinic characteristics
of the deposit.
Treatment Selection.
In order to select the most efficient treatments for the
dissolution of the deposit and for M-2 crude oil paraffin
crystallization inhibition, a closely inspection of the
experimental results was needed.
Deposit dissolution. Accordingly with the solubility
experiments, which demonstrated that the deposit was easily
dissolved in aromatic organic solvents at 65 °C, a xylenes
mixture was adopted as the best cleaning option. It also can be
substituted by higher alkyl benzene combinations. Field tests
with these solvents showed excellent results in the obstruction
removal and flow restarting.
Paraffin Crystallization Inhibition. Inhibition treatment
selection is more complex, taking into account previous
findings which demonstrated that specific paraffin inhibitor
efficiency is strongly related to the crude oil composition,
statement that must be considered during additive selection for
field operations.14,15
Results presented in Table 2 show that only Type II crude
oils afforded significant pour point reductions when treated
with some commercial paraffin inhibitors (A2, 2B, C9 and
D7). Comparison of C24- concentration afforded by M-2
crude oil (65 wt%), as can be seen in Table 3, with the data
presented in Table 1 for Type II reference crude oils (61 to 69
wt%), along with the substantial similarity found between a
typical Type II and M-2 crude oils GPC distributions (Fig. 4),
allowed us to assign this crude in Type II category.
At this point we can assume that any of the four
commercial paraffin inhibitors may have activity when added
to M-2 crude oil, in terms of pour point reduction.
Accordingly with this hypothesis, product D7 was selected for
laboratory tests, since it was the less expensive of the series.
Table 4 shows the effect of this paraffin inhibitor on this
crude pour point, and its comparison with the results afforded
by typical Type I and II crudes (N-9 and G-8 respectively). A
pour point reduction of 6 °C when M-2 crude oil was treated
with additive D7, confirms the hypothesis.
Chemical stimulation record of well M-2 is shown in Fig.
5. In treatment A, performed before this study was carried out,
an inefficient additive was used, as is demonstrated by a
plateau and a further decrease in oil production after the
injection of this product. Treatment B, performed when the
production reached its minimum value (50 bbls/d, in
September 1999), included a better additive (identified as D7
in this work), which rose the production rate during the past
10 months.
Conclusions
1. Crudes with low concentration of heavy paraffins and
bimodal/ wide molecular weight distributions afford
4 MARÍA DEL CARMEN GARCÍA
important pour point depression by the action of paraffin
inhibitors. Specific paraffin inhibitors efficiency is
strongly related to the crude oil composition.
2. Structural comparison between crude M-2 and typical
Type I and II crude oils, allowed to locate this crude in
Type II category, accordingly with C24- hydrocarbons
concentration and molecular weight distribution. This
empirical assignation allowed to decide whether or not an
inhibition treatment could be successful, and, in this
particular case, permitted to select D7 commercial
product for paraffin crystallization prevention treatment.
3. When wax deposits, constituted mainly by high molecular
weight paraffin molecules, are already formed in the
production or transportation tubing, dissolution treatments
using aromatic solvents at high temperature, can be
selected for remotion – cleaning procedures.
Nomenclature
C24+ = Alkyl hydrocarbon chain with more than 24
carbon atoms
C24- = Alkyl hydrocarbon chain with less than 24
carbon atoms
Wt% Weight percent
CH2Cl2 = Methylene chloride
MeOH = Methanol
Acknowledgements
I thank Petróleos de Venezuela, S.A. for funding provided.
Lante Carbognani and Pablo Manrique, from PDVSA-Intevep,
are respectively acknowledged for helpful discussions and
samples, and Wilfredo Briceño, from PDVSA-EP, for field
data provided. Finally, PDVSA-Intevep, is acknowledged for
permission to publish this paper.
References
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SPE 64992
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SPE 64992 PARAFFIN DEPOSITION IN OIL PRODUCTION 5

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TABLE 1. REFERENCE CRUDE OILS CHARACTERISTICS

a
Type Crude Wax (Wt %) C24- (Wt %) Pour Pont (°C) Gravity @ 60°F (°API)

M-4 49.35 37 45 35.5

I N-9 40.34 48 39 37.2

N-4 52.77 23 37 42.5

N-6 46.46 18 48 32.6

G-8 25.35 62 33 43.3

II O-7 33.14 61 39 41.8

N-1 23.62 69 36 41.1

a
Paraffins with less than 24 carbon atoms in their chains

TABLE 2. VARIATION OF CRUDES POUR POINT IN THE PRESENCE OF

SOME PARAFFIN INHIBITORSa

Additives

Type Crude A2 A75 2B B1 B5 C3 C9 D7 Q7 P3

M-4 0 +3 0 0
I N-9 -3 0 0
N-4 -3
N-6 +3 +3 +3 0

G-8 -6 -12 -3 -3 -18 -9 0

II O-7 -5 -9 +5
N-1 -15
a
Untreated crude oil used as reference. Values in °C.
6 MARÍA DEL CARMEN GARCÍA SPE 64992

TABLE 3. COMPOSITION OF WELL M-2 DEPOSIT AND CRUDE OIL

Hydrocarbon families (Wt %)

Sample Fraction Wt % Wax (Wt %) C24- (Wt %) Saturates Aromatics Resins Asphaltenes

Organic 1 25.10 65 75.7 21.1 2.1 1.0

Organic 2 30.10 NIL 99.5 NIL 0.3 0.2

Deposit Organic 3 44.45 NIL 99.5 NIL 0.2 0.3

Total Organic 99.65 93.4 5.4 0.8 0.4

Inorganic 0.35

Whole Crude Mass balance 100.00 37.35 65 75.4 23.0 0.8 0.8

TABLE 4. EFFECT OF D7 PARAFFIN INHIBITOR

ON CRUDE OILS POUR POINT,
INCLUDING THE M-2 CASE HISTORY

Crude Pour Point (°C)

Control Additivated Variation

N-9 36 36 0

G-8 39 30 -9

a
M-2 33 27 -6

a
Case history Fig 1. Deposit found in the production tubing of well M-2

Deposit

CH2Cl2/MeOH 95:5

Organic 1 Insoluble 1

Toluene/Iso-propanol 95:5

S.A.R.A.
Organic 2 Insoluble 2
Xylene/Buthanol 95:5

S.A.R.A.
Organic 3 Inorganic

S.A.R.A.

Fig 2. Solid deposit fractionation using extraction with organic solvent mixtures
SPE 64992 PARAFFIN DEPOSITION IN OIL PRODUCTION 7

Type I
C26

a)

C11 a)

C52

Type II
Time

C60 C34 C28 C15 C9 C5

C54

b)

b)

C40
C120

Time C60 C34 C28 C15 C9 C5

Fig 3. HTSD a) M-2 crude oil and b) Deposit “Organic 2” Fig 4. GPC Chromatograms of a) Type I and Type II,
fraction and b) M-2 crude oils

140

120
Oil production (bbls/d)

100

80

60
Treatment A
40

20 Treatment B

0
ct
ov
ay

ay
99

ar

00

ar
r

r
g
n

n
l

l
b

b
p

Ja c
Ju

Ju
Ap

Ap
De
Au
Fe

Fe
Ju

Ju
Se
O
M

M
M

M
n-

n-
Ja

Date

Fig 5. Production and stimulation history of well M-2 from January 1999 to July 2000