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Received 1 February 2007; received in revised form 26 June 2007; accepted 12 July 2007
Available online 7 August 2007
Abstract
In this work, a novel procedure is developed to determine the amount of salt for crude oils in which the available laboratory tech-
niques are unable to provide accurate salt content values. The technique is based on measuring the salinity of the wash water that is
vigorously mixed with the crude oil (forming an emulsion) and then separating it from the water-in-oil emulsion by irradiating micro-
wave energy during few minutes. This three step process involves the emulsication of the wash water exempt of salt in crude oil, fol-
lowed by the recovery of the water by microwave heating and, nally, the analysis of the salt content using the classical Mohrs method
titration procedure. The novel technique presented here was able to provide reliable information about the salt content on Brazilian
crude oils, in a rapid manner, without need of unsafe time-consuming solvent extraction procedures.
2007 Elsevier Ltd. All rights reserved.
0016-2361/$ - see front matter 2007 Elsevier Ltd. All rights reserved.
doi:10.1016/j.fuel.2007.07.013
1242 M. Fortuny et al. / Fuel 87 (2008) 12411248
reviewed by Pal [4]. Depending upon the facilities available, a glass reference electrode; (iii) Electrometric Method [12]
standard laboratory methods may be applied which can which is based on the evaluation of the conductivity of a
involve DeanStark distillation (ASTM D-4006) [5], centri- solution of crude oil in a mixed alcohol solvent, using a
fuge separation [6], Karl Fischer titration [7], among oth- beaker and a set of electrodes. The chloride (salt) content
ers. Dierent meters have been found on the petroleum is obtained by reference to a calibration curve of conductiv-
literature for on-line monitoring of water content on pipe- ity versus chloride concentration of known mixtures.
lines or vessels. The main principles behind these meters Reasonable results for petroleum products with low vis-
include generally electrical, microwave, radiation scatter- cosity can be achieved by those three methods presented
ing, spectroscopic, ultrasonic, or density (or viscosity) before. However, some diculties arise when one deals
based techniques [4]. Most of them detect water by a mea- with high water content emulsions or crude oil with higher
surement of an electric property of the uid mixture, viscosities; hence, sample handling needs to be improved
including capacitance, conductance or dielectric properties beyond the existing standards. Considering the standard
[8]. In particular, one of the most popular sensing devices tests involving extraction procedures (the Mohrs method
used to follow the water content on crude oil streams is a and the potentiometric one), the increased viscosity of the
capacitance probe, which is widely known as a BSW mon- sample implies a totally dierent mixing energy needed to
itor where BSW means the percentage of Basic Sediment keep the homogeneity at the same desired level. Besides,
and Water in the ow stream, and consists in free water the extraction operation involving heating of very viscous
and sediment and/or emulsied water and sediment [3]. materials may represent a risk to the safety of the installa-
Once the dielectric constants of crude oil and water are tion and experimental setup. In the case of the electro-
about 2 and 80, respectively, it is possible to use a concen- metric method, mixing problems with very viscous
tric probe, which senses the apparent dielectric constant of samples can be reduced by warming until they are reason-
a uid stream by measuring its capacitance between the ably uid before the analysis; however, according to the
probe electrodes. Since dielectric constants of oil and water method, no sample shall be heated more than is necessary
vary with temperature, a temperature compensation to lower viscosity to a manageable level. Moreover, the
scheme is required. electrometric method is specically designed for crude oils,
On the other hand, the evaluation of salt content on with no remarks about the maximal water content for
crude oils is not a trivial task. This occurs because the salt which the method stands. Since the water inuences the
determinations are based on indirect methods, generally conductivity, one should expect increased uncertainties
involving the evaluation of electrical properties of crude on the salt content measured by this method when the
oil samples that are also inuenced by the water content. crude oil of interest contains signicant amounts of emulsi-
Besides, as crude oil quite often presents poor electrical ed water.
properties, salt extraction procedures are generally From the previous discussion, although the existing
required in order to distinguish the ionic/electric activity standard laboratory methods seem to be useful for deter-
associated to the saline species come from the crude oil. mining the salt contents of crude oils, the use of these meth-
Otherwise, sharper electric properties may be attained by ods implies the taking of careful considerations in the
diluting the crude oil into an appropriated solvent. As installation and the chemicals involved. As a matter of fact,
the extraction procedures also involve the use of a proper standard methods tend to fail when we are to analyze vis-
solvent (the extracting uid) such as toluene, xylene, and cous crude oils or samples with high water contents.
others, one can conclude that the crude oil salt character- In the work described herein, an improved procedure
ization depends clearly on the preparation of mixtures. was developed in order to determine the amount of salt
As a consequence, a good homogeneous condition in the for those crude oils in which the available laboratory stan-
mixture must be satised. Homogeneity is therefore the dard methods are unable to provide accurate salt content
key feature for measurements based on electrical proper- values. The technique is based on measuring the salt con-
ties, and also is crucial for a right sampling in terms of hav- tent of the wash water that was separated from the crude
ing a representative sample. oil using microwave heating, after being articially emulsi-
Basically, three standard lab-scale test methods have ed using high shear rates. The novelty of this procedure
been employed to measure salt contents in crude oils: (i) relies on the joint use of an emulsication step followed
extraction and titration by classical Mohrs method [9], by a demulsication one based on the irradiation of micro-
which involves the salt content determination by extraction wave energy. A number of experiments were performed in
and the volumetric titration method [10]; (ii) Potentiomet- order to demonstrate the feasibility of this technique. Stan-
ric method [11], that comprises the use of an electrically dard laboratory procedures generally used for salt content
heated extraction apparatus in which a weighed crude oil determination were also conducted for comparisons. The
aliquot dissolved previously in xylene is added. Specied novel procedure developed here was able to provide reli-
volumes of alcohol, acetone and water are also added into able information about the salt content on Brazilian crude
the apparatus as the extracting uid. A portion of aqueous oils, in a rapid manner, without need of time-consuming
extract is analyzed for total halides by potentiometric titra- procedures or solvents preparations. It is believed that this
tion (silver nitrate as the titrant) using a silver electrode and type of procedure can be very useful for the measurement
M. Fortuny et al. / Fuel 87 (2008) 12411248 1243
of salt content for a number of crude oils and may serve to induced molecular rotation neutralizes the zeta potential
inspire the development of a new (and more general) stan- of the dispersed droplets, thus reducing the stabilization
dard method in the future. oered by the ionic surface-active species [24], and (iv)
the preferred absorption of microwaves by water droplets
1.1. Microwave irradiation in water-in-oil emulsions causes intense internal pressure
in these droplets, resulting in the expansion of the dispersed
The microwave irradiation oers a clean, inexpensive, phase and in the reduction of the thickness of the interfa-
and convenient method of heating which often results in cial lm [23,25]. However, this latter mechanism is not
higher yields and shorter reaction times [13,14]. The heat- yet clearly proved. On the other hand, the breaking of
ing of liquids using microwaves can be explained by the chemical bonds cannot be induced by the mere absorption
interaction of matter with the electric eld of the incident of microwaves in view of the low energy of photons as
radiation, causing the movement of ions as well as that compared to the chemical bonds-associated energies [26].
of induced or permanent molecule dipoles. The movement The energy range of hydrogen bonds, ionic bonds and
of such species can cause heat generation (the so-called Van der Waals-like interactions vary between 0.04 and
dielectric heating) by two main mechanisms: dipole rota- 4.51 eV, while the microwave photons are associated to
tion, which is related to the alignment of molecules that energies varying between 1.24 106 and 1.24 104 eV
have permanent or induced dipoles with the electric eld according to the microwave frequency [15].
component of the radiation, and ionic conduction, which
refers to the migration of dissolved ions with the oscillating 2. Experimental
electric eld [15].
Besides the quick heating of the materials, some authors 2.1. Crude oil characterization
consider that the microwaves can provide specic eects
(not purely thermal) generally connected to the selective An experimental study was conducted to evaluate the
absorption of microwave energy by polar molecules performance of the dierent techniques used to measure
[16,17]. The occurrences of these eects have not been the salinity of crude oils. Three dierent Brazilian crude
explained yet [18]. In spite of that, the microwave irradia- oils were used in this study. The characteristics of these
tion has become an interesting tool for a number of appli- crude oils are summarized in Table 1 and the techniques
cations in the crude oil industry. Gunal and Islam [19] used in their characterization are described as follows.
studied the role of microwave irradiation in altering rheo- The dynamic viscosity of the dierent crude oils was
logical properties of crude oils during heating. The authors determined using a rotational rheometer (Physica Rheolab
observed an irreversible eect on crude oil viscosity, which MC1, from Anton Paar) equipped with a heating jacket.
was not detected in the absence of asphaltenes. This result The analysis consisted in measuring the shear stress as a
was supposed to be linked to the interaction of the micro- function of the shear rate keeping the sample at 30.0 C
wave with the asphaltenes, suggesting the existence of a re- (0.3 C).
orientation of their molecular structure. Similar ndings The water content (WC) of the crude oils was deter-
were obtained by Bjorndalen and Islam [20] who observed mined by the Karl Fischer (KF) reagent method, in accor-
that at higher concentration of asphaltenes, microwave dance with ASTM D-1744 procedures [27]. The solvent
irradiation leads to greater decline in viscosity, apparently used during the analysis was a mixture of dry methanol
related to some sort of re-orientation of molecules com- and chloroform (20%, v/v). For standardization of the
bined with breakdown of some of the asphaltene particles. KF reagent, distilled water was solubilized into the solvent
In the current work, microwave irradiation is employed cited before. A Metrohm KF titrator (model 836 Titrando)
for demulsication purposes. Since the pioneering work of equipped with a double platinum electrode was employed
Wolf [21], a lot of activity has been developed concerning during the water content determination tests.
the use of microwave irradiation for the demulsication The asphaltene content was determined gravimetrically
of water-in-oil and oil-in-water emulsions, providing after recovering the n-heptane insoluble fraction from the
improved results when compared to the conventional heat- oil, in accordance with the ASTM D-6560 test method
ing procedure [2225]. In short, high rates are observed for [28]. Besides containing asphaltenes, this n-heptane insolu-
the separation of water and oil phases using microwaves, ble fraction may also contain waxy substances and inor-
which have been attributed to the following mechanisms: ganic material. The asphaltenes are then recovered from
(i) microwaves quickly heat emulsions, reducing the viscos- this fraction by successive washing with n-heptane and tol-
ity of the continuous phase (oil), thus favoring the water uene, followed by solvent (toluene) evaporation. The total
droplets contact [22,23], (ii) the temperature increase can acid number (TAN) was determined by potentiometric
cause reduction in the viscosity of the rigid lm formed titration of the crude oil with alcoholic potassium hydrox-
by natural surface-active species such as asphaltenes, res- ide (KOH) solution, in accordance with the ASTM D-664
ins, oil-soluble organic acids, solids, and waxes, in the test method [29]. Prior to each titration, crude oil samples
wateroil interface, making easier the coalescence between were dissolved in a 50% v/v toluene/isopropanol solution.
dispersed water droplets [23,24], (iii) the microwave- The same automatic titrator used for Karl Fischer analysis
1244 M. Fortuny et al. / Fuel 87 (2008) 12411248
reaching a total salt concentration of 0.1 g dm3. A resisting temperatures up to 300 C and pressures up to
homogenized aliquot of neutral oil (10 cm3) was carefully 80 bar. The control system supplied with the instrument
dissolved in an organic solution containing 40 cm3 of enables us to perform heating ramps with power and tem-
xylene and 50 cm3 of mixed alcohol solvent. The solution perature conditions programmed prior to the run. A built-
was then transferred into a 100 cm3 test beaker in which in forced-air cooling system allows for a fast cooling of the
the conductivity measurements were performed. To cover vessels. The standard procedure for demulsication runs
the range of chlorides contents of interest (0 involved the use of just two quartz glass vessels, each of
430 mg dm3), known fractions of that 50 cm3 mixed alco- them lled with 40 g of emulsion. These samples were stir-
hol solvent should be replaced by standard amounts of the red throughout the tests using the magnetic stirrer, to facil-
mixed chloride solution. During the procedure, the instru- itate the contact among the water droplets in the emulsion.
ment records the corresponding conductivity signal for The total microwave irradiation time was set to 15 min for
each standard chloride concentration enabling to build an each test. During this irradiation time, the temperature was
internal calibration curve. programmed to increase from ambient to the setpoint value
Once the calibration curve was established, the salt con- (90 C) in 2 min, being kept at this value during the subse-
tent of the crude oil was determined by dissolving 10 cm3 of quent 13 min. In this way, the microwave power supplied
the crude oil sample in the organic solution (xylene/mixed by the instrument was automatically manipulated to ensure
alcohol solvent). The mixture was then hand-shaken vigor- the temperature programmed for the samples during the
ously during 1.5 min, as recommended by ASTM D-3230 heating ramp. After the irradiation time, samples were
test method. After allowing the mixture to stand for quenched by the cooling system during 10 min and the
approximately 5 min, the mixture was placed in the test water phase formed during the demulsication test was
beaker for salt content measurements. characterized in terms of salt contents. Note that, since
high mixing levels (and, ultimately, homogeneity) had been
2.2.3. New method: emulsication, microwave-assisted achieved in the rst stage, the salt concentration of the sep-
demulsication and volumetric titration method arated water would not depend on the demulsication e-
The new procedure developed here involved three ciency. In a broader sense, these emulsication and
stages. The rst stage consisted in the emulsication of demulsication stages in this new method reproduce what
the crude oil under analysis with wash water exempt of goes on during actual desalting operations: the rst stage
salts. To achieve high mixing levels, a known amount simulates the mix-valve action in the inlet stream of the
of water was added stepwise to the hydrocarbon phase, desalter vessel and the second stage reproduces the recov-
while the mixture was hand-shaken to completely incorpo- ery of a water phase containing increased salt content
rate the water, resulting in a pre-emulsion with a total vol- and a crude oil containing little unresolved water. How-
ume of 300 cm3. This mixture was then homogenized using ever, it should be pointed out that the use of microwave
an Ultra-Turrax T-25 homogenizer tted with a S25-25G irradiation allows for the separation of the water phase
dispersing tool (IKA). The ratio of water and crude oil in at relatively short time (15 min), as shown in a previous
the mixture was set to make up an emulsion with a range work of this group [13].
of 3550% (v/v) of water content. The homogenization Finally, the third stage consisted in the evaluation of the
conditions, such as the stirring frequency and the time of salt content in the water phase obtained in the previous
homogenization, were kept constant at 17,500 rpm and stage. The water phase was ltered (for oil droplets
10 min, respectively, yielding emulsions with droplet size removal) and its salt content was characterized by the vol-
distributions (DSD) with mean values in the range of umetric titration method based on the Mohr as described
320 lm, as measured by laser diraction technique before.
(Malvern Instrument Model 2000 Mastersizer).
The second stage consisted in the demulsication of the
mixture for water removal using microwave irradiation. 3. Results and discussion
This microwave assisted demulsication stage was con-
ducted using a commercial microwave reactor system 3.1. Extraction and volumetric titration method (adaptation
(Anton Paar Synthos 3000). This instrument is equipped of IP 77)
with two magnetrons able to provide 1400 W of continuous
microwave power, a rotor system in which eight vessels Extraction and titration tests were performed according
with an 80 cm3 capacity can be inserted at one time, and to the procedures described before in order to determine the
magnetic stirrer for agitation of the sample in each vessel. salt content of each crude oil. During these tests, at least
Also, an infrared sensor placed on the rotor bottom four wash cycles were employed to reach higher salt recov-
enables us to assess the surface temperature of the vessel eries for the same crude oil sample. Tests were performed in
and an immersing temperature probe (gas bulb thermosen- duplicate. The properties of the crude oils used during the
sor) placed at one reference vessel can be applied to follow tests are reported in Table 1. The results of cumulative salt
the temperature evolution of that sample during tests. The contents obtained using this procedure are displayed in
vessels were 80 cm3 in capacity and made of quartz glass, Table 2. In all cases, the salt content increased markedly
1246 M. Fortuny et al. / Fuel 87 (2008) 12411248
Table 2 Table 3
Cumulative salt content results for crude oils A, B and C from stepwise Salt content results for crude oils A, B and C from electrometric method
extraction tests and related values for the Formation Water (calculated in mg of NaCl per
Wash cycle Salt content (mg dm3) dm3 of water)
Oil WC (%) Salt content (mg dm3)
Oil A Oil B Oil C
(1) (2) (1) (2) (1) (2) Crude oila Formation water
A (lot-1) 0.45 69 3 15,378
1 29.6 29.2 35.2 23.7 15.8 13.7
A (lot-2) 0.83 153 7 18,386
2 37.4 37.9 46.1 47.8 20.0 17.8
3 45.6 45.4 51.6 51.3 23.8 22.5 B (lot-1) 0.76 279 10 36,750
C 2.10 432 9 20,581
4 53.4 53.2 54.6 60.1 25.8 24.2
a
5 75.8 67.8 Average value deviation.
6 88.8 75.2
7 92.7 86.5
8 93.4 ple per volume of water phase present in the crude assessed
9 99.4 by KF analysis. Confronting these results with those
obtained before by extraction procedures, note that much
higher salt contents were detected by the electrometric
with the number of wash cycles, meaning that the extraction method for all crude oils. Concerning the oil A, note that
procedure was unable to remove the salt from the crude oils two dierent lots were used in the tests, with sharp dier-
eciently. Tests for oils A and C yielded reproducible val- ences in the WC. In fact, changes of the WC in the crude
ues of salt content per wash cycle. However, for these oils, oil generally lead to variations of the salt content in the
it was impossible to carry on additional wash cycles beyond crude oil. As a consequence, an increase in the WC may
the 4th cycle due to the very small volume of organic phase raise the salt amount per total volume of crude. It is never-
produced. Conversely, some uctuations were observed in theless interesting to observe that the calculated salt con-
the salt content measured for oil B along the wash cycles. tent in the formation water may serve as a further proof
Also, greater amounts of organic phase were available after of validity (or not) of the values obtained through this
each wash cycle, allowing for running additional wash method. This occurs because the concentration of salt in
cycles for oil B samples. the formation water is supposed to vary between crude oils
Clearly, reported values in Table 2 show that the cumu- coming from dierent sources or explored using dierent
lative salt content increase continuously with the number methods. However, for samples coming from the same
of wash cycles for both oils A and B, suggesting that more crude oil, but with dierent WC, the salt content of this
wash cycles would be needed. It seems that the salt content water entrained in the crude is expected to be similar to
reached a steady value only in the tests with oil C. As a the salt content of the formation water, since the only dif-
consequence, results provided by this method are likely ference between these samples has been the storage time. In
to be underestimated, which means that, even after adjust- this way, the long storage time of crude oil samples pro-
ing the method including stepwise extraction schemes with duces water segregation and a natural increase of the WC
higher boiling interval, the current method yielded unreli- is generally observed. According to Table 3, one may
able values of salt contents for those crude oils. observe that the salt contents of the formation water for
For the sake of comparison with other test methods, let the two lots of oil A are very dierent (an increase of
us calculate the salt content provided by this method for 19.6% from lot 1 to the lot 2). Recall that these values of
each crude oil. Considering the average and deviation val- salt content in the formation water were calculated suppos-
ues for each oil reported in Table 2, the resulting salt con- ing that the salt contents measured by the instrument for
tent using this method was 53.3 0.1 (oil A), 96.1 4.7 the crude oil were true. Among the reasons that could
(oil B) and 25.0 1.1. It is nevertheless likely that these explain that dierence, one may consider that the calibra-
values are not entirely true (and analysis based on a dier- tion curve of the salt analyzer did not take into account
ent test method procedure should clarify this point). a number of variables that can play a role on the conduc-
tivity values measured by the instrument, such as the WC
3.2. Electrometric method (ASTM D-3230) and the water droplet size. Thus, further studies are being
conducted in the lab to investigate the use of the electro-
The electrometric method described before was applied metric method in order to build calibration curves on a
to evaluate the salt content of crude oils A (lots 1 and 2), broader range of conditions, with the inclusion of these
B (lot 1) and C. Table 3 presents the results of water con- variables, which means that the current electrometric stan-
tent determined by the KF reagent method and the salt dard method should be reviewed.
content for the dierent crude oils. These data represent On the other hand, the electrometric method is inappro-
average values of two independent tests and were used to priate to analyze samples with relatively high salt contents
calculate the respective salt content of the formation water or with salt contents beyond the range of calibration, as in
emulsied in the crude, also included in Table 3, which the case of oil C. For this crude oil, the salt content was
stands for the amount of salt (in mg) in the crude oil sam- assessed by extrapolating the calibration curve.
M. Fortuny et al. / Fuel 87 (2008) 12411248 1247
show that the existing techniques based on solvent extrac- [5] ASTM D-4006. Standard test method for water in crude oil by
tion procedures or calibration curves present some limita- distillation.
[6] ASTM D-4007. Standard test method for water and sediment in
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the extraction method provided much underestimated val- [7] ASTM 4377. Standard test method for water in crude oils by
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[12] ASTM D-3230. Standard test method for salts in crude oil (electro-
was required, but resulted in unreliable values. Moreover, metric method).
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