MODELING AND ANALYSIS

Experimental study of the effect of inhibitors in wax

precipitation by different techniques
Baudilio Coto1, Carmen Martos1, Juan José Espada1, Marı́a Dolores Robustillo1 & José Luis Peña2
Department of Chemical and Energy Technology, ESCET, Universidad Rey Juan Carlos, c/Tulip

1

stoles, Madrid, Spain
an s/n, 28933 Mo
2

stoles, Madrid, Spain
Repsol Technology Centre, E-28931 Mo

Keywords Abstract
CPM, DSC, inhibitors, pour point
depressants, WAT The blocking problems in equipment and flowlines caused by precipitation of
wax solids is a well-known problem and large research efforts have been
Correspondence focused on developing procedures dealing with wax deposition. Among the dif-
B. Coto, Department of Chemical and Energy ferent alternatives, the use of chemicals is frequently used to inhibit wax precip-
Technology, ESCET, Universidad Rey Juan itation. The presence of these compounds modifies the size and/or the shape of
Carlos, c/ Tulip

stoles,
an s/n, 28933 Mo
the paraffinic solids, thus affecting their flow behavior and cold properties. In
Madrid, Spain. Tel: 34 91 4887089;
Fax: 34 91 4887068; E-mail: baudilio.
this work, a methodology based on different experimental techniques was devel-
[email protected] oped to study the effect of different additives on the crude oil behavior at low
temperature. Four commercial inhibitors were added to three crude oils in dif-
Funding Information ferent concentrations. The effect of the inhibitors on wax precipitation was
Authors thank Repsol for crude oil and studied using differential scanning calorimetry (DSC) and cross-polarized
inhibitors supply. microscopy (CPM). Obtained results for wax appearance temperature (WAT)
using DSC do not show remarkable differences regarding the presence of inhib-
Received: 11 April 2014; Revised: 14 July
2014; Accepted: 15 July 2014
itor. However, CPM analyses revealed differences in both size and shape of par-
affin solids. The results obtained in this work reveal that in some cases the
Energy Science and Engineering 2014; inhibitor does not modify the WAT values, but the morphology of the precipi-
2(4): 196–203 tated particles. In these cases, it is necessary to combine DSC and CPM analyses
to obtain reliable results.
doi: 10.1002/ese3.42

The paraffin deposition and the variables involved have

Introduction
been deeply investigated. Thus, Burger et al. [3] studied
Paraffins can precipitate during crude oil production the mechanism of wax deposition which occurred as a
operations when the oil is cooled because of heat losses result of lateral transport by diffusion, shear dispersion,
to the surroundings. The precipitation of waxes from and Brownian motion. The rate of deposition is affected
petroleum mixtures at low temperatures is an important by a number of factors such as temperature of the pipe,
flow assurance problem in oil production as it can cause flow rate, residence time, and wax concentration among
important economic losses, which may even lead to aban- others [24]. In this sense, different models have been
doning wells [1, 6, 10, 18, 25]. developed to describe wax deposition in pipelines [13].
The main variables to evaluate wax precipitation are Different techniques have been developed to mitigate
wax appearance temperature (WAT), the amount of pre- the paraffin deposition, which are commonly classified
cipitated solid as a function of operating conditions (wax into five categories: mechanical, thermal, bacterial,
precipitation curve, WPC), pour point, gel point, etc. The chemical and electromagnetic treatments. In the prac-
knowledge of these variables is crucial to estimate wax tice, the use of a single method is not effective and
precipitation potential and to determine the best strategy therefore a combination of them is rather applied [26].
to control and mitigate the problem. There is a wide vari- Among the different treatments, the use of chemical
ety of experimental techniques to determine these param- inhibitors has increased in the crude oil industry as
eters, as reported elsewhere [12, 14]. there are a number of chemicals with paraffin inhibition

196 ª 2014 The Authors. Energy Science & Engineering published by the Society of Chemical Industry and John Wiley & Sons Ltd.
This is an open access article under the terms of the Creative Commons Attribution License, which permits use,
distribution and reproduction in any medium, provided the original work is properly cited.
B. Coto et al. Effect of Inhibitors on Wax Precipitation

properties. However, there is not an inhibitor equally microscopy (CPM) were used to observe the effect of the
effective in all wells and it is usual to find a chemical different additives on the crude oil waxes at low tempera-
which performs correctly in a well but it fails in tures. The results obtained by DSC indicated a slight
another one even in the same basin [24]. Therefore, the decrease of the WAT in presence of some inhibitors, but it
application of chemical inhibitors is frequently restricted was not conclusive. The CPM results, however, show clear
to each well. differences in the size particle distribution regarding the
Wax inhibitors are usually grouped in three main cate- inhibitor used. Finally, the pour point of crude oils and
gories [20]: the resulting mixtures was determined, showing agreement
with the results obtained by DSC and CPM analyses. The
• Wax crystal modifiers
results obtained for the studied inhibitors indicate the pos-
• Detergents
sibility to use a combination of DSC and CPM analyses to
• Dispersants
study the effect of inhibitors, which do not greatly affect
Detergents and dispersants are basically surface-active the WAT values, but mainly modify the morphology of the
agents as, for example, polyesters and amine ethoxylates. precipitated particles.
They prevent or limit sedimentation of crystals by keeping The novelty of our work is to present a methodology
them dispersed as separate particles, thus reducing their which allows the optimal selection of inhibitors and com-
trend to interact with and to adhere to solid surfaces [17]. bines both the WAT value variation and the change in
Wax crystal modifiers are chemicals capable of growing solid morphology of the precipitated solid from crude oil
into wax crystals and to alter their growth and surface in the presence of wax inhibitor. When the wax inhibitor
properties. These chemicals reduce the affinity of crystals slightly affects the WAT value, additional information
to interlock and form three-dimensional networks, thereby such as particle size and shape distributions is needed.
lowering the pour point and the viscosity. For that, they These data are not commonly reported in the literature
are commonly named pour point depressants (PPD) [20, from CPM analyses and for that, this work can be of
26]. Pretreatment of crude oils with those chemicals is an importance in this field. In conclusion, this work pro-
attractive alternative to solve wax deposition problems dur- poses the combination of data related to WAT (DSC)
ing transport of crude oils along pipelines [4]. However, with those related to solid morphology (CPM) to study
the performance of these compounds is not clear. The most the performance of wax inhibitors.
accepted theory proposes a combination of mechanisms
involving nucleation, cocrystallization, and adsorption
Experimental Section
[21], but different observations have been made regarding
the influence on the crystal size and shape and its effects on
Materials
lowering the pour point [8, 9, 22]. The experimental obser-
vations reported in the literature indicate that there is not a Three dead crude oils (crude oil D-3, D-13, and G-3) and
single mechanism but a combination of them. The most four wax inhibitors (I1, I2, I3, and I4) of unknown com-
accepted theories suggest that the decrease of pour point in position and nature provided by Repsol (Repsol Technol-
the presence of crystal modifiers is frequently accompanied ogy Centre, E-28931 Móstoles, Madrid, Spain) were used
by the transition from single crystals to aggregates [20]. in this work. The main features of the studied crude oils
A number of experimental techniques have been are reported in Table 1.
reported elsewhere to study the action of PPD for the
control of wax crystallization. Thus, X-ray diffraction
Differential scanning calorimetry
[23], IR spectrometry [27], DSC [28], and rheometry
[15] have been applied to investigate into the interaction The DSC technique is widely used to study wax solidifica-
between PPD and waxes. tion, [5, 7, 16] and the interaction between inhibitors and
As described earlier, the mechanism of inhibitors on waxes [28]. This technique has the advantage of its
wax is widely studied in the literature, although the
results are not fully conclusive.
The aim of this work is not to explore the capabilities of Table 1. Characteristics of the crude oils used in this work.
DSC and CPM techniques applied to wax precipitation, Crude oil D-3 Crude oil D-13 Crude oil G-3
but to develop a methodology, based on both techniques,
to select the most appropriate inhibitors. Four chemical Origin South America South America Europe
Type Medium Medium Medium
inhibitors of unknown composition and nature were
Base Naphthenic Paraffinic Paraffinic
added in different proportions to several crude oils. Differ- API 31 27 31
ential scanning calorimetry (DSC) and cross-polarized

ª 2014 The Authors. Energy Science & Engineering published by the Society of Chemical Industry and John Wiley & Sons Ltd. 197
Effect of Inhibitors on Wax Precipitation B. Coto et al.

simplicity and fast response which makes it appropriate magnification of 209 and 509. Cooling and heating rates
for routine analyses. were provided by a temperature control stage connected
DSC calibration was carried out by using pure n-alkane to the microscope, which allows covering the temperature
within the range of n-C7 to n-C18, thus covering a tem- from
120 to 350°C. The calibration for temperature was
perature range between
90 and 30°C. The obtained carried out using the melting point of pure n-paraffins
results suggest the possibility to linearly correlate the pure (n-C14 to n-C38). A linear relationship between theoretical
n-alkane melting temperature determined by DSC and melting point of pure n-paraffins and the WAT deter-
the reference values [5]. mined by CPM was obtained.
In this work, the experimental apparatus used was a
DSC Mettler–Toledo DSC822e and the temperature pro-
file used was as follows:
(A)
• The sample is heated at 3°C/min from 25 to 80°C to
completely dissolve the solid phase and to remove any
thermal history.
• The sample is cooled down from 80 to
120°C at 3°C/
min.
• The sample is heated up from
120 to 80°C at 3°C/min.
A procedure previously developed for thermogram
integration using properties of n-paraffins as reference
was used, thereby yielding the wax appearance tempera-
ture (WAT) [5]. 50 µm

Cross-polarized microscopy
(B)
This technique is frequently used to determine the WAT
values [11, 19] and to characterize the waxes resulting
from the precipitation process [2, 16]. By using this
method, well-crystallized regions can be determined as
they present different refractive index from the hydrocar-
bon matrix.
A Nikon Eclipse 80i microscope was used in cross-
polarized mode to observe wax crystallization at a

Table 2. WAT values obtained by DSC for the crude oils and their
50 µm
mixtures with the inhibitors used in this work.

Crude Crude Crude

oil D-3 oil D-13 oil G-3
(C)
WAT (°C)
Concentration
Inhibitor (ppm) 20.7 36.4 43.0

I1 300 21.3 37.0 42.1

1000 21.6 36.5 41.1
6000 19.4 36.4 41.1
I2 300 20.8 37.4 42.1
1000 20.1 38.9 42.1
6000 20.0 37.4 42.1
I3 300 20.7 36.7 41.1
1000 20.0 36.4 41.1
6000 19.8 36.3 41.1
50 µm
I4 300 21.4 35.9 42.1
1000 19.4 34.9 39.2
Figure 1. Micrographs (209) of raw crude oil G-3 at (A) 30°C; (B)
6000 18.2 34.4 –
15°C; and (C) 0°C.

198 ª 2014 The Authors. Energy Science & Engineering published by the Society of Chemical Industry and John Wiley & Sons Ltd.
B. Coto et al. Effect of Inhibitors on Wax Precipitation

The samples were analyzed as follows:

Results and Discussion
• The sample is heated for 1 h at 50°C in an oven to
complete dissolution. Differential scanning calorimetry
• The sample is cooled down from 50 (fixed as reference)
DSC analysis is commonly used for the crude oil charac-
to 0°C at 3°C/min.
terization, especially to determine its behavior at low tem-
The WAT values were determined when the first paraf- peratures. In this work, this experimental technique was
fin wax crystals were visually identified at a magnification used to detect changes in crude oil behavior at low tem-
of 209. perature due to the presence of inhibitor. The additives
The images for further treatment were recorded at 0°C tested (I1, I2, I3, and I4) were added in different concen-
using a digital camera incorporated to the system. The trations (300, 1000, and 6000 ppm) to the studied crude
analysis of the images was carried out using Nis-Elemen- oils. The raw crude oils and the resulting mixtures (crude
tsTM software, thus obtaining the particle size and shape oil + additive) were analyzed by DSC. No qualitative dif-
distribution. ferences were detected in the thermograms of the differ-
ent samples. In order to quantify the effect of the selected
inhibitors, the WAT values of the raw crude oils and their
Pour point analysis
mixtures with the inhibitors were determined following a
This property is defined as the lowest temperature at method reported elsewhere [5]. The obtained results are
which oils flow freely at specific test conditions. It was summarized in Table 2. As can be seen, only the mixture
determined following the ASTM D97 standard test of crude oil plus I4 additive at concentration of
method. In this work, it was used as benchmark of the 1000 ppm shows a noticeable decrease on the WAT (4°C
results obtained by DSC and CPM analyses. in the case of crude oil G-3), but the obtained results are

I1 (300 ppm) I4 (300 ppm)

50 µm
50 µm

I1 (1000 ppm) I4 (1000 ppm)

50 µm
10 µm

I1 (6000 ppm) I4 (6000 ppm)

50 µm 10 µm

Figure 2. Micrographs (209) of raw crude oil G-3 mixed with the selected additives at different concentrations.

ª 2014 The Authors. Energy Science & Engineering published by the Society of Chemical Industry and John Wiley & Sons Ltd. 199
Effect of Inhibitors on Wax Precipitation B. Coto et al.

not conclusive themselves to confirm the best inhibitor.

(A) However, these results indicate that 1000 ppm is the con-
centration at which the effect of the additives can be
observed with this technique.

Cross-polarized microscopy
One of the purposes of this work is to quantitatively
detect the effect of additives in different mixtures by
50 µm
means of CPM.
The analysis procedure was optimized to correctly
(B) detect wax precipitation. Figure 1 shows the micrographs
of the raw crude oil G-3 at three temperatures (30, 15,
and 0°C). As can be seen, the amount of precipitated
waxes is much higher at 0°C, and consequently the
obtained data at that temperature seem to be more repro-
ducible. Therefore, this temperature was set in order to
carry out further CPM analyses.
50 µm
The effect of the inhibitor concentration was also
studied to confirm the results previously obtained by
DSC analysis. As an example, Figure 2 shows the
(C)
micrographs for the crude oil G-3 mixed with additive
I1 and I4 at different concentrations (300, 1000, and
6000 ppm). It can be seen how the solid wax morphol-
ogy changes as a function of the inhibitor concentra-
tion. Thus, in the case of additive I4, the particles look
like agglomerates dispersed in the organic matrix at an
additive concentration value of 1000 ppm. This effect is
50 µm
also observed in the case of additive I1, although in a
minor extent. These results suggest, in agreement to
those form DSC, that an inhibitor concentration of at
(D)
least 1000 ppm is necessary to detect significant differ-
ences.
Figure 3 shows the micrographs of the raw crude oil
G-3 and its mixtures with each additive at 0°C and
1000 ppm. As can be observed, the presence of additive
I4 affects in a larger extent than the presence of the rest
of additives. Thus, the particle morphology confirms the
50 µm change from the needle-like shape present in the raw
crude oil to agglomerate particles dispersed in the oil
matrix when adding additive I4.
(E)
In order to carry out the quantitative analysis of the
micrographs, the Nis-ElementsTM software was used.
The properties analyzed were the particle size and the
particle shape distribution. Figure 4 displays the effect
of the different additives on the particle size distribu-
tion of precipitates. It is remarkable how the addition
of additive I4 yields a particle size distribution different
10 µm from the rest of inhibitors used. Thereby, the presence
of additives I1, I2, and I3 favors equivalent diameters
Figure 3. Micrographs (209) of raw crude oil G-3 and its mixtures within the range 1–3 microns, whereas the addition of
with the selected additives (1000 ppm). (A) Raw crude oil; (B) crude additive I4 makes the particle size distribution shift
oil + I1; (C) crude oil + I2; (D) crude oil + I3; and (E) crude oil + I4. toward larger values.

200 ª 2014 The Authors. Energy Science & Engineering published by the Society of Chemical Industry and John Wiley & Sons Ltd.
B. Coto et al. Effect of Inhibitors on Wax Precipitation

Crude oil D3
D3+I1
D3+I2
D3+I3
D3+I4

Occupied area by paraffins (a.u.)

Crude oil D13
D13+I1
D13+I2
D13+I3
D13+I4

Crude oil G3
G3+I1
G3+I2
G3+I3
G3+I4

<0.5 0.5–1 1–2 2–3 3–4 4–5 5–6 6–7 7–8 8–9 >9
Equivalent diameter (μm)

Figure 4. Particle size distribution of the raw crude oils and their mixtures with the studied additives.

Crude oil D3
D3+I1
D3+I2
D3+I3
D3+I4
Occupied area by paraffins (a.u.)

Crude oil D13

D13+I1
D13+I2
D13+I3
D13+I4

Crude oil G3
G3+I1
G3+I2
G3+I3
G3+I4

<0.5 0.5–0.75 0.75–0.85 0.85–0.95 >0.95

Circularity

Figure 5. Shape distribution of the crude oils and their mixtures with the studied additives.

This different behavior is in agreement with DSC The effect of each additive on the particle shape was
results, in the sense that inhibitor I4 makes the WAT also analyzed in this work by means of the “circularity”
value decrease. This observation is related to the presence of the paraffin particles defined as follows:
of larger paraffin particles as reported elsewhere [20]. 4pArea
Therefore, among the additives tested, the additive I4 Circularity ¼ : (1)
Perimeter2
improves the behavior of the crude oil at low tempera-
tures and the effect can be detected using both experi- Figure 5 depicts the variation of this parameter as a
mental techniques reported in this work. function of the inhibitor used. In general, the additives

ª 2014 The Authors. Energy Science & Engineering published by the Society of Chemical Industry and John Wiley & Sons Ltd. 201
Effect of Inhibitors on Wax Precipitation B. Coto et al.

Table 3. Pour point values obtained for the crude oils and their mix- Conflict of Interest
tures with the inhibitors I2 and I4.
None declared.
Sample Pour point (°C)

Crude oil D-3
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