BRAZILIAN JOURNAL OF PETROLEUM AND GAS | v. 5 n. 1 | p.

025-033 | 2011 | ISSN 1982-0593

METHOD TO EVALUATE FOAMING IN PETROLEUM

a
Fraga, A. K.; a Rezende, D. A.; a Santos, R. F.; a Mansur, C. R. E. 1

a
Federal University of Rio de Janeiro - Macromolecules Institute

ABSTRACT
In oilfields, gravitational separation tanks are generally used to separate the oil, gas and water phases,
remove emulsifying agents present at the interfaces and permit the coalescence of water droplets
associated with the crude oil being pumped. The main problem that influences the performance of these
separators is the formation of foam. In this work, a method was developed to evaluate foaming in crude
oil in laboratory scale, reproducing the operation conditions in gas-oil separators in real fields. This
method was employed with seven crude oil samples, and the performance of silicone antifoams with
different molar masses could be tested. The results indicated that the method of evaluating the
breakdown of foam in oil by using the Aging Cell apparatus in a roller oven proved to be suitable. It was
observed that the oil viscosity is a determining factor in predicting whether or not foam will form.

KEYWORDS
Antifoams; petroleum; silicones; gas-oil separators; surface tension

1
To whom all correspondence should be addressed.
Address: Federal University of Rio de Janeiro, Macromolecules Institute, Av. Horácio Macedo, 2030 – Ilha do Fundão, 21941-
598, Rio de Janeiro, RJ, Brazil
Telephone: +55 21 2562-7209 | e-mail: celias@ima.ufrj.br
doi:10.5419/bjpg2011-0004

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1. INTRODUCTION By relying on various oilfield production data,

Mclean et al. (1995) proposed a model whereby
In oilfields, gravitational separation tanks are the asphaltenes and resins in certain oils are
generally used to separate the oil, gas and water absorbed within the gas bubbles when the
phases, remove emulsifying agents present at the pressure falls below the bubble point. As a result, a
phase interfaces and permit the coalescence of semi-rigid coating is formed, causing the foam to
water droplets associated with the crude oil being stabilize and the viscosity to decline.
pumped. Although there are many factors that
influence the performance of these separators, the Injection of silicone in gravitational separators
main problem is the formation of foam, in that it has been used for many years to control foam
hampers mechanical control of the liquid and can (Pape, 1983). The objective of this work was to
lead to spills from tanks and equipment. Moreover, develop a novel method to evaluate foaming in
foam takes up space in the tanks, reduces the crude oil and the destruction of foam with
separation capacity and efficiency, and increases antifoams that are already commonly used.
the drag of the liquid phase within the gas phase
and vice versa, sometimes to the point of requiring
shutdowns of the process (Chilingarian et al.,
2. EXPERIMENTAL
1987).

One of the ways to prevent foaming is to modify 2.1 Materials

the separator design. But this is often unfeasible
Three samples of silicone foam inhibitors, with
because of the limited space on many offshore
different molar masses, donated by Bluestar
platforms. Therefore, chemical additives known as
Silicones, SP (Brazil) were evaluated. All samples
antifoams or foam inhibitors are employed to
were used as received, and were named as S1, S2
prevent or break up the foam. This method can be
and S3.
improved by having more detailed knowledge of
the components present in the petroleum and The formulations containing the antifoams were
their contributions to its properties (Szilas, 1986). prepared by dissolving the samples in the
commercial solvent Solbrax Eco, donated by BR
Significant advances have been made in
Distribuidora, a subsidiary of Petrobras (Brazil).
understanding the role played by the different
According to the manufacturer’s specifications
components of crude oil (such as asphaltenes and (Solbrax Eco Solvent, 2008), the product mainly
resins), their percentages, elementary composition consists of a mixture of aliphatic and naphthenic
and molar masses, both in stabilizing emulsions
hydrocarbons, with less than 1 % aromatics
and foams. These fluid components give rise to
(obtained by catalytic hydrogenation, which
emulsions and the formation of foam upon being
permits converting the aromatics into naphthenes,
subjected to agitation and shear forces in the
reducing the sulfur content, saturating the olefins
presence of predominantly lipophilic natural
and eliminating polar impurities). Also according to
surfactants present in the oil (asphaltenes, resins, the manufacturer, this process allows obtaining a
naphthenic acids, among other chemical species) highly stable solvent, with only a slight odor and
(Poindexter et al., 2002; Shaban, 1995). low toxicity. For these reasons, there is interest in
With respect to the specific components of using it as a solvent in formulations employed in
crude oil, Callaghan et al. (1985) demonstrated oilfields.
that various surfactants are naturally found among
To evaluate the efficiency of the foam
these components, especially those with short inhibitors, solutions of 30 % wt/vol of each additive
carboxylic acid chains and phenols with molar mass were prepared. From these solutions, aliquots
of up to 400, which can stabilize the foam. were collected at previously calculated amounts,
Other researchers (Musser and Kilpatrick, 1998; and then added to the oil samples in order to
Poindexter et al., 2002) have shown that species contain the desired concentration of additive in
such as asphaltenes, resins or waxes tend to each system, so that all assays could be properly
stabilized foam by increasing the oil viscosity. conducted.

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The chemical composition of the samples of aliquots of the additive solutions, prepared with
silicone and Solbrax Eco solvent were determined Solbrax at a concentration of 30 % wt/vol, were
through carbon-13 nuclear magnetic resonance mixed in 15 mL of oil and the surface tension
(13C-NMR). The samples were placed without any values of these systems were measured. All tests
preparation or dissolution in a 10-mm OD test tube were run in triplicate.
containing a capillary with an adequate deuterated
solvent, so as not to coincide with the probable 2.2.2 Testing the efficiency of the
signs of the sample. The acquisition parameters of additives as antifoams
the analyses were determined under the standard
conditions established by the device’s maker, and Initially, the tests of foam formation in one of
the sample was maintained at a temperature of 30 the oil samples (crude oil 2) were performed by
C while obtaining the spectra. varying some conditions in order to observe the
influence of each one of them in the foam
Quantitative analyses were performed to formation. A total of 150 mL of each oil sample was
identify the structure of the silicone samples, as transferred to a compression cell (High
well as to determine their compositions, by the Temperature Aging Cell, Fann). This cell was then
conventional calculation method based on the sealed and connected to a compressed air line with
principle that the area under each peak is directly a rubber hose. The chamber was pressurized to 50,
proportional to the number of carbon-13 nuclei of 200 and 250 psi, measured with a manometer, and
that region. The peak areas were calculated by an held at each pressure for three minutes by shutting
integrator coupled to the device. the ball valve.

Seven Brazilian crude oil samples were used, The compression cell was placed in a Fann
donated by the Petrobras Research Center 704Es roller oven, preheated to 48 and 63 °C (three
(Cenpes). The samples were characterized degrees above the testing temperatures). The cell
regarding their densities, determined in an Anton was then allowed to rotate at 50 rpm for one and
Paar DMA 5000 digital density meter. The two hours.
procedure to quantify the density of the oil
samples was based on the ASTM D 4052 method At the end of these tests, the compression cell
(2009), using an oscillating U-tube sensor to was connected to the decompression cell, in this
measure the density. Their levels of saturated case a 100-mL graduated cylinder. It was placed
hydrocarbons, total aromatic hydrocarbons, resins vertically and the cell’s outlet was kept pointing
and asphaltenes were determined by the SARA downward. Then the cell’s valve was opened
method by means of thin-layer chromatography slightly and closed when the initial height of the
(TLC) with a flame ionization detector (FID), to foam formed inside the decompression cell
obtain the chemical composition of each oil reached 80 mL. The time count started
(Ramalho et al., 2010). immediately after the valve was shut.

The viscosity of the oil samples was determined Later, the tests with the other six oil samples
in a Haake RS 600 rheometer, using a C20/1°Ti were performed following the same procedure and
cone-plate. The analyses were performed at a under the preselected conditions (pressure: 200
shear rate interval between 30 and 80 s-1, at a psi, temperature of 60 C and conditioning time of
temperature of 60 C. 1 hour). Different aliquots of solutions containing
30 % wt/vol of silicone-based antifoaming additives
2.2 Methods were added during the tests in order to evaluate
the efficiency of these additives by the developed
2.2.1 Determination of the surface methodology.
tension of the oil samples
The foam height was read at intervals of time
The oil-air interfacial tensions were measured until constant consecutive values were attained,
by the Du Nöuy method using a Krüss K10ST digital indicating total break-up of the foam.
tensiometer, at 30 C. Firstly, the oil samples were
The percentage of foam formed in each interval
analyzed without adding any solvent. Then 2-L was calculated with Equation 1.

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H  HF  Peak(s) at 0.940 ppm: attributed to the two

Foam (% v/v)   100 (1) methyl carbon atoms located in the
HF
repeated unit of the chains;
Where H is the height reached by the foam on
 Peaks at 1.440 and 0.445 ppm: explained
the scale at each time interval, and HF is the final
as side bands, which are distortions
height reached by the liquid after all the foam was
observed in high-intensity signals caused
destroyed. All tests were run in triplicate. The
by a dispersion of the radiofrequency of an
average values of formed foam (%) and the
observed nucleus. They are more often
standard deviation (SD) were added to the
observed in highly abundant nuclei, such as
graphics.
hydrogen, phosphorus and fluorine.

The molar mass of the commercial silicone

samples was determined by integrating the areas
3. RESULTS AND DISCUSSIONS
under the signals acquired in the carbon-13
spectrum. For sample S1, the integration of the
3.1 Chemical characterization of the
area under the signal located at 1.687 ppm was
samples equal to 5.04. Thus, since this signal was attributed
The 13C-NMR analysis of silicone sample S1 is to six carbon atoms, each methyl group
shown in Figure 1. The spectra of the other corresponds to an integral value of 0.84. With this
samples showed the same chemical shifts observed information and the integral value of 94.18
in this spectrum, only differing in the intensity of corresponding to the two methyl groups of the
the signals. repeated unit, it was possible to calculate the
polymerization degree (n) of this macromolecule,
The structure of the commercial silicone which is approximately 55. Hence, the molar mass
analyzed is also shown in Figure 1 and was of sample S1 is 4,230 g/mol.
proposed based on findings in the literature
(Silverstein et al., 1991) and the chemical shifts For sample S2, the areas under the spectrum
observed in the NMR-13C spectra. In particular, one signals were 0.58 for each of the six methyl groups
has: at the ends of the chain and 98.36 for the two
methyl groups of the repeated unit, implying an
 Peak(s) at 1.687 ppm: attributed to the six “n” value of approximately 447. Therefore, the
methyl carbon atoms present at the ends molar mass is about 33,200 g/mol, which is almost
of the chains; eight times that of sample S1.

13
Figure 1. C-Nuclear magnetic resonance spectrum of S1 sample (structure shown in insert).

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Table 1. Chemical composition, density and viscosity of the crude oil samples.
SARA Unit Oil 1 Oil 2 Oil 3 Oil 4 Oil 5 Oil 6 Oil 7
Density API 13.2 21.2 24.0 26.3 27.4 28.0 28.2

Viscosity cP 1200.0 200.0 53.0 25.0 15.0 7.6 5.0

Saturated hydrocarbons wt% 35.7 40.7 47.1 45.0 32.1 39.6 27.9
Total aromatic hydrocarbons wt% 24.6 34.1 29.3 37.0 40.1 38.9 40.0
Resins wt% 32.4 22.8 22.3 15.0 21.1 20.4 26.9
Asphaltenes wt% 7.3 2.4 1.3 3.0 6.7 1.1 5.2

Sample S3 appeared to be a macromolecule contents and crude oil 3 has the highest level of
with a very high polymerization degree because saturated hydrocarbons.
the 13C-NMR spectrum showed only one intense
signal, located at 0.940 ppm. In this case, because The densities of the oil samples were expressed
it has a long polymer chain, the methyl groups at as API grade (API), according to the scale defined
the ends are diluted as a function of the low molar by the American Petroleum Institute to describe
ratio (terminal group effect), so it is more probable and classify crude oils based on their specific
that the signal was not detected by the device, or it gravity, measured at 15.6 C. The specific gravity is
coalesced with the signal of the methyl groups of inversely proportional to the API density, so
the repeated unit. Therefore, it was not possible to lighter oils have higher API grades (Mothé et al.,
calculate the polymerization degree or molar mass 2008). The oils were numbered in ascending order
of this sample, but these values are known to be of API values.
much higher than those of sample S2 (n = 447).
3.2 Testing the efficiency of the additives
The 13C-NMR analysis of the Solbrax Eco solvent as antifoams
showed various signals coalescing in a single
chemical shift range (between 11 and 39 ppm). The 3.2.1 Effect of condition variations
reason is that Solbrax is a mixture of hydrocarbons
with very similar structures. This range contains the Initially, the tests were carried out with the
chemical shifts of the 13C atoms of hydrocarbons purpose of verifying foam formation in oil sample
with linear or branched chains (Silverstein et al., 2. After that, the foam formation tests were
1991). Also, the chemical shifts of the CH2 groups in performed with the other oil samples, with or
monocyclic alkanes (from C3H6 to C10H20) can be without additives, in the preselected conditions.
observed from 22 to 28 ppm.
Foam formation in the oil sample 2 was
The presence of other compounds, such as assessed by varying one condition at a time, as in
alkanes, aromatics or heteroatoms, was not the following tests: air pressure for the foam
detected. Nevertheless, these may be present in formation (Figure 2); temperature used in the tests
very small quantities, based on the device’s (Figure 3) and conditioning time in the oven (Figure
sensitivity ( 1 %). 4). Each condition was varied, while all others
remained constant.
Table 1 shows the characterization of crude oil
samples. The SARA method indicates the levels of It can be observed that the conditioning time
saturated hydrocarbons (S), aromatics (A), resins does not affect formation and breakdown of foam
(R) and asphaltenes (A) present in the oil. Table 1 (Figure 4). On the other hand, at lower pressures
also shows the density and viscosity values of each the formation of foam is impaired, but no
oil sample. alteration was observed in the amount of time
required to the total breakdown of foam formed
The results obtained show that crude oil 1 has (Figure 2). Also, since the oil viscosity decreases
the highest content of asphaltenes and resins, with increasing temperature, the formation of
crude oils 5 and 7 have the highest aromatic foam is initially enhanced at lower temperatures,

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but breaks down more quickly with time due to From the results obtained in these tests, the
stronger draining that occurs in the so-called following conditions to carry out other foam
Plateau channels (Figueiredo et al., 1999). formation and breakdown assays were selected:
time of conditioning of 1 h (shortest time); air
250 pressure of 200 psi (the lowest pressure at which a
50 psi
200 psi
good foam level was obtained) and temperature of
200 250 psi 60 C (at which the largest volume of foam is also
generated). The results of the foaming tests with
Formed foam (%)

150 the other six oil samples are shown in Figure 5.

100
As observed in an earlier study (Poindexter et
al., 2002), which was carried out with another
50
testing method, the viscosity of the oils appeared
to be the most important factor influencing foam
0
formation. Crude oil 1, with the highest viscosity
0 50 100 150 200 250 300 (Table 1), did not produce any foam, even though it
Fi
Time (sec) contains the highest levels of foam-stabilizing
Figure 2. Percentage of foam formed on crude oil species (resins = 32.4 wt% and asphaltenes = 7.3
sample 2 as a function of time, submitted to different wt%, Table 1).
pressures, at 60 C and conditioning time of one
hour. On the other hand, crude oil 6 only generated a
small volume of foam, with low stability, facilitating
250

30 C
o drainage of the liquid. It contains small amounts of
o
45 C asphaltenes (1.1 wt%) and resins (20.4 wt%). The
200 o
60 C foam formed in crude oil 7 was even less stable.
Although it contains more asphaltenes than crude
Formed foam (%)

150
oil 6, it is less viscous.
100
Among the oils tested, samples 3, 4 and 5
provided the highest foam formation percentage.
50
Crude oil 5 has a higher amount of foam-stabilizing
species than crude oils 3 and 4, although, in
0
0 100 200 300 400 500 600 700 800
comparison with these samples, the oil sample 5
Time (sec) presented the lowest viscosity (Table 1). This fact
Figure 3. Percentage of foam formed on crude oil may have contributed to this sample being third in
sample 2 as a function of time, in different the stability test.
temperatures, at 200 psi and conditioning time of one
hour.
250

250
1 hour 200
2 hours
200
Formed foam (%)

150
Formed foam (%)

150

100

100

50

50

0
0 0 50 100 150 200
0 50 100 150 200 250 300 Tempo (sec)
Time (sec)
Figure 5. Percentage of foam formed on the crude
Figure 4. Percentage of foam formed on crude oil
oil samples as a function of time: (◄) crude oil 1; (■)
sample 2 as a function of time, submitted to different
crude oil 3; (▼) crude oil 4; (►) crude oil 5; (●)
conditioning times, at 60 C and 200 psi. crude oil 6 and (▲) crude oil 7.

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250 200

180

200 160

140
Formed foam (%)

Formed foam (%)

150 120

100

100 80

60

50 40

20

0
0
0 50 100 150 200 0 50 100 150
Time (sec) Time (sec)

Figure 6. Efficiency tests of the silicone solutions as Figure 7. Efficiency tests of the silicone solutions as
antifoaming additives in samples of crude oil 3: (●) antifoaming additives in samples of the crude oil 4:
crude oil, (■) crude oil + solbrax solvent, (▲) crude (●) crude oil, (■) crude oil + Solbrax solvent, (▲)
oil + S1 solution, (▼) crude oil + S2 solution and (◄) crude oil + S1 solution, (▼) crude oil + S2 solution
crude oil + S3 solution. and (◄) crude oil + S3 solution.

By comparing the results for crude oils 3 and 4, concentration in the oil was 40 ppm.
it was observed that the foam formed with the
To evaluate the ability of the Solbrax in breaking
previous sample was more stable. Although crude
down the foam, initially the tests were performed
oil 3 has a lower level of asphaltenes than crude oil
with only this solvent added, at the same
4 (Table 1), it has higher levels of resins and
concentration of 40 ppm. Analyses have also been
saturated hydrocarbons, making it slightly more
carried out with the silicone additives S1, S2 and
viscous. From the results obtained, crude oils 3 and
S3, in crude oil 3. All results are shown in Figure 6.
4 were chosen to test the antifoam additives in
The Solbrax solvent has little influence on the foam
subsequent assays.
stability, whilst the presence of silicone additives
3.2.2 Effect of additives reduces the initial extent of formed foam, in the
following descending order: S1 > S2 > S3. It is
In these tests, solutions of the additive samples important to point out that the additive S3 has the
in the Solbrax solvent have been prepared at highest viscosity and highest molar mass.
concentrations of 30 % wt/vol, which is the normal
The literature (Callaghan et al., 1985) shows
active material content in the antifoam
that most antifoams disperse well in the foaming
formulations used in water-oil-gas separation
solution. Nevertheless, there is normally a small
tanks. Aliquots of these formulations were added
amount of oil at the solution’s surface along with
to the crude oil samples so that the final additive
small droplets of the solution, and the quantity of

Table 2. Surface tension of crude oil samples.

S.T. of crude oil S.T. of crude oil + solvent S.T. of crude oil + additive solution
Crude oil (mN m )
–1 (a)
(mN m )
–1 (a,b)
(mN m )
–1 (a,c)

S1 S2 S3
Oil 3 29.6 28.4 23.5 23.0 23.8
Oil 4 30.0 29.2 23.5 23.5 23.8
Error = ± 0.1 mN/m
Surface tension of pure Solbrax solvent: 24.6 mN/m
(a)
S.T. = surface tension of the system;
(b)
Values gotten with the addition of 2 μL of Solbrax solvent in the crude oil
(c)
Values gotten with the addition of 2 μL of additive solution (30 % wt/vol) in the crude oil

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foam inhibitor at the surface is usually small as faster than in crude oil 3. In this case, the higher
compared to the total amount of antifoam viscosity of crude oil 3 (compared to the viscosity
dispersed in the solution. of crude oil 4) probably hindered the dispersion of
this additive.
A comparison of the surface tensions (S.T.) of
the oil-antifoam systems against those of the oils
alone (Table 2) shows that the tensions decrease in
the presence of antifoam agents and these values 4. CONCLUSION
do not vary significantly. The silicone with
intermediate viscosity (S2) had the greatest effect The method of evaluating the breakdown of
in reducing the surface tension. This behavior also foam in oil by using the Aging Cell apparatus in a
indicates that the silicone with lowest molar mass roller oven proved to be suitable. From the results
(S1) may have been adsorbed at the oil surface, but obtained in this investigation, it was possible to
was not able to inhibit foaming, i.e., there was not conclude that oils with high viscosity did not
sufficient dispersion at the surface to break down generate foam, even when they had high levels of
the foam. foam-stabilizing species (resins and asphaltenes).
On the other hand, the oils with low viscosity had a
The intermediate molar mass of sample S2 low foam volume, and the foam had low stability,
made it less soluble in crude oil 3 than sample S1, because the liquid was drained between the foam
and, in the case of sample S2, not only were the lamellae. Therefore, the viscosity of crude oils is a
silicone molecules adsorbed at the oil-air interface, determining factor in predicting whether or not
reducing the surface tension, but they were also foam will form and, if so, how its stability will be
dispersed in the oil, causing the breakdown of affected over time.
foam. The silicone sample with the highest molar
mass (S3) had the greatest foam-inhibiting effect The silicone samples performed satisfactorily in
and the lowest adsorption at the oil-air interface, the efficiency tests, except for the sample with the
since it is the least soluble in the oil, forming a lowest molar mass.
heterogeneous phase. With respect to the time of
The antifoams were more efficient in crude oil
foam breakdown, the additive S3, with the highest
3, which has a lower concentration of asphaltenes,
molar mass and highest viscosity, took longer to
than they were in crude oil 4, because the foam
work in crude oil 3 than the other additives.
inhibitors’ molecules managed to act at the surface
Chaisalee et al. (2003) also showed that of the film and to penetrate it as well, forming a
antifoam additives are initially deposited on the heterogeneous phase that was able to break down
surface of the solution in the form of large oily the foam. Hence, because crude oil 3 is more
drops. The compound is dispersed during agitation viscous, the additives’ dispersion was hampered.
of the foaming solution, and this is greatly The antifoam action at the oil surface was less
facilitated if the components diffuse well at the efficient in crude oil 4, which has an asphaltene
solution’s surface. If the compound is highly concentration nearly four times higher.
viscous and/or does not diffuse well, its dispersion
can be impaired and, as a result, the antifoam
activity can decline. Therefore, the behavior
ACKNOWLEDGMENTS
observed with sample S3 can be attributed to its
greater viscosity, which impaired its dispersion in We thank Research Center of PETROBRAS
the medium. (CENPES) for donating the petroleum samples,
The additives were also tested in crude oil 4, Bluestar Silicones (Brazil) for donating the silicone
which has a higher level of asphaltenes, that samples, and Coordenação de Aperfeiçoamento de
stabilize foam. The results are illustrated in Figure Pessoal de Nível Superior (CAPES), Conselho
7. The additive S3 was efficient in breaking down Nacional de Desenvolvimento Cientifico e
the foam in oil 4, but less so than in crude oil 3. Tecnológico (CNPq) and Fundação de Amparo à
This behavior can be related to the higher content Pesquisa do Estado do Rio de Janeiro (FAPERJ) for
of foam-stabilizing species in crude oil 4. Moreover, financial support.
sample S3 broke down the foam in crude oil 4

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Heavy Oil Behavior. SPE Paper 29243; Presented at portuguese).
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