caracterizacion crudos 2015

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New methodology for heavy oil desalination

Cristina M.S. Sad a, vina L. Santana a, Milton K. Morigaki a, Edna F. Medeiros a, Eustquio V.R. Castro a,Maria F.P. Santos b, Paulo R. Filgueiras a,

a Federal University of Esprito Santo, Chemistry Department, Laboratory of Research and Development of Methodologies for Analysis of Oils LabPetro, Av. Fernando Ferrari,

514, Goiabeiras, P.O. Box 29075-910, Vitria, Esprito Santo, Brazilb North Center University of Esprito Santo, Rod North BR101, Km 60, Coastal District, So Mateus 29932-540, Esprito Santo, Brazil

h i g h l i g h t s

Development of a new methodology to heavy crude oils desalination.

Monitoring of the desalted crude oil by ionic conductimetry.

About 99.87% of the salt present in the oil was removed.

TAN and sulfur content were reduced by around 30% after the desalination process.

a r t i c l e i n f o

Article history:

Received 15 October 2014

Received in revised form 16 February 2015

Accepted 17 February 2015

Available online 27 February 2015

Keywords:

Heavy crude oil

Total salinity index

Heavy oil desalination

a b s t r a c t

The salts present in petroleum interfere in the characterization of its physicochemical properties, and

from the measurements of these properties is established the price of crude oil. Therefore the water

and salt need to be removed before these analyses. A new desalting apparatus was developed for heavy

crude oils desalination by using demulsifier with water. The desalination process is accomplished in sev-

eral washing steps and the extracted oil salts are monitored by ionic conductivity. Operational conditions

were studied before and after the desalting process and the following parameters were evaluated: den-

sity, kinematic viscosity, total salinity index, total sulfur, total acid number and ionic conductivity. Usingthe proposed process it was possible to reduce the chloride content in the crude oil to values lower than

43mg kg1 of sodium chloride in petroleum with extraction efficiency about 99.87%. After the desalina-

tion process it was not observed significant changes in the intrinsic oil properties, and after the fourth

wash of the oil there was a reduction of approximately 33% of total sulfur and total acid number content.

These results indicate an improvement in oil quality, once the presence of sulfur compounds in the oil is

undesirable because it increases the polarity of the oil, thereby increasing the polarity of the emulsions.

These compounds are also responsible for the corrosivity of the petroleum products and produce harmful

gases during combustion. Variations about 2% in API gravity and 3% in kinematic viscosity were not sig-

nificant, indicating no change in the physical properties of the oils. The proposed procedure is faster

(about 80 min) than the salt extraction method given by ASTM D6470 (about 140 min) for four washing

cycles and it was possible to obtain a suitable condition for salt removal from heavy crude oil emulsions

without toxic reagents.

2015 Elsevier Ltd. All rights reserved.

1. Introduction

Crude oil is a naturally occurring mixture consisting pre-

dominantly of hydrocarbons and organic sulfur derivatives, nitro-

gen, oxygen and metals, and may usually be accompanied by

variable amounts of saline water or produced water, and inorganic

gases[1]. The produced water found in the oil must be removed

because it usually has a high concentration of salts in its

composition and form emulsions with viscosities greater than

the dehydrated oil that cause problems such as: changes in the

pumping system sizing and transfer, corrosion in the refining tow-

ers, fouling in pipelines, higher consumption of chemicals and

energy, need of new design of equipment throughout the produc-

tion process, transportation and refining issues [2,3].

The chemical composition of the salts present in the oils is often

found as salts of sodium, calcium and magnesium chloride, in a

lower proportion of sulfates. The amount of mineral salts varies

according to the geologic formation of the source rock and can

be as highas 200,000 mgL1 [47]. The processes of water removal

http://dx.doi.org/10.1016/j.fuel.2015.02.064

0016-2361/2015 Elsevier Ltd. All rights reserved.

Corresponding author. Tel.: +55 02740097735.

E-mail address: [email protected](P.R. Filgueiras).

Fuel 150 (2015) 705710

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or dehydration processes also result in removal of salts [7,8]. The

water-in-crude oil emulsions for heavy oils (API gravity around

16) are normally more stable than the ones for light oils [3], and

separation of liquid phases involves breaking of the emulsion that

is a fundamental step for the preparing of oil distillation. Various

processes that are used to break the emulsion with removal of

water, salts and solids can be mentioned: gravitational separation,

electrostatic separation, demulsification, chemical filtration forced

by glass wool filter, membrane separation, microwave and ultra-

sound [5,6,811].

In industrial oil processing, the typical water-in-crude oil

separation methods are not applied in isolation, they often occur

in association with other methods for desalting oil. As an example,

we can mention the gravitational separation, which in most cases

is used together with the chemical treatment (using demulsifiers)

and in some cases heat treatment [4]. The last one includes the

application of heat, which has the effect of reducing the kinematic

viscosity of the oil and increase the kinetic energy of oil molecules

facilitating their separation from water. This facilitates settling

and, consequently, salt water separation. Heat also causes changes

in the colloidal stability of droplets promoted by emulsifying

agents, helping to destabilize the emulsion [4,5]. Another feature

is the use of chemical demulsifiers, which adsorb on the water-

in-crude oil interface and change its physicochemical properties,

promoting coalescence of water droplets. The demulsifiers are

nonionic polymeric surfactants which contain a hydrophilic and a

lipophilic portion. Hydrophilic are included as parts of ethylene

oxides, hydroxyl, carboxyl and amine groups. Among the proper-

ties that are sought in demulsifiers it can be mentioned the high

speeds of adsorption in oilwater interface, movement of natural

emulsifiers that stabilize emulsions and the formation of thin

and weak films in the oilwater interface [12,13].

An efficient water-in-crude oil separation method must use heat

and some demulsifier to break the emulsion stability. But, it is also

necessary to characterize and evaluate the oil through some physi-

cochemical properties such as density (API gravity), kinematic vis-

cosity, total salinity index (TSI), sulfur content, total acid number(TAN) among others. Oil samples with high water content and con-

sequently high amounts of salts render an effective characterization

impossible becausehigh concentrations of salts mayinterfere in the

evaluation of physical and chemical propertiesof theoils[14]. From

the measurements of the physicochemical properties is established

the price of crude oil, storage and transport conditions.

It is reported that the difficulty of breaking water in oil emul-

sions of heavy oils is due to the inefficiency of the existing tools

for the treatment and monitoring of the salt content in oil. So, it

is necessary to make efforts in order to seek how to make the salt

extraction process efficient, economic and sustainable [15]. Some

laboratory methods are commonly used to extract and quantify

salts in oil, as example the method based on titration with silver

nitrate by precipitation (Mohr) [14], conductimetry [15] andpotentiometric titration [9,16]. These methods are used for the

quantification of salt content in oil. However, these methods are

not effectively applicable to heavy oils and they are also destruc-

tive methods, i.e. using toxic organic or inorganic reagents, gener-

ating final product as chemicals waste associated with the oil that

is undesirable for the products and the environment [69,17]. In

this sense, it is necessary to promote the separation of wateroil

emulsions and remove the salts present in the heavy crude oils

in order to obtain confident results for their physicochemical char-

acterization through the classic methods. Therefore, in this paper

we describe a developed apparatus that allows desalting heavy

crude oils using washing with deionized water and commercial

demulsifiers, under continuous stirring and temperature control.

The novelty of this process is the combination of heating controlwith chemical demulsifiers addition and subsequent removal of

water by gravitational separation and simultaneous measurement

of the salt content signal by conductimetric technique.

2. Methodology

2.1. Treatment of crude oil samples

In this study, it was used nine heavy crude oils samples fromproduction fields located in the sedimentary basin of the Brazilian

coast, identified as A, B, C, D, E, F, G , H and I.

The oil samples were collected from ducts in 2.0 L flasks and were

transported to the laboratory where they were processed within

two hour after arrival. The standard method ASTM D5854 [18]

was followed for all procedures using one aliquot of the collected

crude oils. In the oil characterization process, non-emulsified water

in the oil (called free water) is easily separated by applying the

gravitational method which requires decanting the oil for one hour.

After freewater separation, aliquots fromoil phase (emulsion) were

collected for the characterization procedure before and after desali-

nation process using the developed apparatus shown inFig. 1. The

water content analysis[19]in the oil emulsions was determined.

For initial characterization, oils with water content above 1% (v/v)were dehydrated with the addition of 200lL of a concentrated

commercial demulsifier at 60 (5) C commonly used in the prima-

ry processing of oils and centrifuged at 1600 (20) rpm for 15 min

[5]. These oils were denominated as dehydrated oils. After

removal of water, to verify that the dehydration procedure was

effective, the water content in oil emulsion was again determined

to verify that the water content was lower than 0.5% (v/v). Then,

the physicochemical properties of thedehydratedoils: total salinity

index (TSI), API gravity, total acid number (TAN), sulfur content and

kinematic viscosity were determined according to the ASTM stan-

dard methods.

2.2. Crude oil characterization

2.2.1. Water content

The water content was determined by potentiometric Karl

Fischer (KF) titration, in accordance with the ASTM D4377 stan-

dard method [19]. The solvent used during the analysis was a

Fig. 1. Desalting apparatus at laboratory.

706 C.M.S. Sad et al./ Fuel 150 (2015) 705710


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mixture of dry methanol and chloroform 20% (v/v). For standard-

ization of the KF reagent, distilled water was solubilized into the

solvents. A Metrohm KF titrator (model 836 Titrando) equipped

with a double-platinum electrode was employed during the water

content determination procedure. The ASTM D 4377-06 standard

method covers results in the range from 0.02% to 2% (v/v) of water

in oil. Samples with results above this limit can be analyzed by the

technique, but are not covered by this standard.

2.2.2. Total salinity index (TSI)

The TSI in the oils was determined by extracting the salts using

a mixture of solvent and water (optimized method)[9]. The subse-

quent analysis of the aqueous phase was performed by potentio-

metric titration, and the NaCl content was obtained by

potentiometric titration with the use of the digital automatic

analyzer Metrohm 809.

2.2.3. API gravity

The API gravity was determined according to ASTM D5002 [20]

and ASTM D1250[21]. First, the density was determined by inject-

ing a sample into the digital automatic densimeter analyzer Anton

Paar model DMA 5000. The measurements were conducted at

50 C then estimated at 20 C for calculating the API gravity.

2.2.4. Total acid number (TAN)

The TAN was determined by potentiometric titration of the

crude oil with an alcoholic potassium hydroxide (KOH) solution.

Prior to each titration crude oil samples were dissolved in a 50%

(v/v) toluene/isopropanol solution[22]. The same automatic titra-

tion used for Karl Fischer analysis (Metrohm 836 Titration) was

employed for the total acid number determination. However, this

one was equipped with an electrode combination suitable for

non-aqueous titrations.

2.2.5. Total sulfur content

The total sulfur content was determined according to the ASTM

D4294[23]by energy-dispersive X-ray fluorescence spectrometryusing the automatic analyzer HORIBA, model SFLA-2800. Three

calibration curves were built (0.0050.100% (w/w), 0.051.00%

(w/w), and 0.34.0% (w/w)), using 10 sulfur patterns in mineral

oil bought from INSTRU-MED, which were automatically selected

by the equipment in agreement with the sample to be analyzed.

The calibration curve verification was accomplished through the

analysis of a diesel reference sample, with seven repetitions.

2.2.6. Kinematic viscosity

The kinematic viscosity was determined according to the ASTM

D7042-04 [24]. It was analyzed by injecting a sample into the digi-

tal automatic viscosimeter analyzer Anton Paar Stabinger SVM

3000. It was measured at 50 C and 60 C then estimated at 40 C

by regression [25]. In the sector for exploration and productionof crude oil, kinematic viscosity is usually evaluated at 40 C, but

for very viscous oils their direct measurement at this temperature

generates large errors. Thus for these oils it is measured at two

higher temperatures and the value extrapolated to 40 C.

2.3. Desalting apparatus

The prototype of the developed Desalting apparatus (Fig. 1) con-

sists in a glass flask with a volumetric capacity of 3 L: 360 mmhigh

and 20 mm wide with three 24/40 joints. At the bottom of the flask

there is a flow valve (tap) with dimensions 45 mm long and 25 mm

wide for liquid output. The transfer of the washing water (water

with demulsifier) into the flask was performed usinga glass funnel.

The glass flask has a NiCr (composition 80/20) wire and capaci-tance of 3.5 Ohm m1. The NiCr wire is attached to small glass

spheres around the bottle flask. The electric current passes through

the NiCr wire and heats the emulsion (washing solution with oil),

keeping them at 60 (5) C. The voltage is monitored by a digital

multimeter, 220 volts, allowing rigorous temperature control.

At the central joint of the desalting apparatus, there is a glass

rod with dimensions 55 mm long and 25 mm wide attached to a

blade with a half-moon Teflon with dimensions of 16.5 mm long

and 10.5 mm wide coupled to a mechanical stirrer. To avoid loss of

light organic compounds during the desalination stage, one of the

upper ends has a reflux condenser with dimensions of 45 mm in

length and 6.5 mm in width with a constant flow of a refrigerant

fluid composed by water and methanol (50% v/v) at10 C coupled

to a thermostatic bath (Ethik model 521-3D), as showed inFig. 1.

At each stage of desalination, the ionic conductivity of the

washing water was determined at 25 C in a 50 ml aliquot taken

from the apparatus, with the use of a digital automatic conduc-

tometer (Metrohm 856 with a platinum metal electrode).

2.4. Reagents and standard solution preparation

It was used an ultrapure water with resistivity of 18.2 MX and

conductivity 0.05lS cm

1

at25

C, obtained in a water purificationsystem Direct Q-UV, manufactured by Millipore. The water used to

wash the oil (called washing water) was prepared adding 250 lL of

a concentrate commercial demulsifier commonly used in the pri-

mary processing of oils.

The calibration curve of the conductivityversusthe salt content

in the aqueous solution was prepared by diluting free water

originated from wells with ultrapure water. Two calibration curves

were prepared, one for very high (above 5000 mg kg1) and other

for low (less than 5000 mg kg1) values of salt content (Fig. 2).

2.5. Desalination process

The desalination process of heavy oils in the desalting apparatus

occurs by removing brine from the water in oil emulsions by wash-ing it with the washing water prepared as described above, which

was previously tested in the efficiency of breaking the wateroil

emulsion in heavy oils. The demulsifier used was a surfactant com-

posed of copolymers (ethylene oxidepropylene oxide) with differ-

ent molar ratios. The role of the demulsifier is to reduce the

interfacial tension between oil and water, promoting coalescence

of the saline water droplets. The process consisted in heating

500 ml of the oil at a temperature of 60 (5) C with continuous

stirring of 150 (5) rpm for 15 min. After 5 min of resting with

complete phase separation (water/oil), the process of removing salt

was monitored by ionic conductivity of an aliquot of 50 ml of

washing water with a platinum electrode. The desalination process

efficiency was achieved when the ionic conductivity of the wash-

ing water is below 1000l

S cm1 based on the calibration curve.

Then, it was calculated the concentration of salts in the washing

water by calculating the applied conductivity value in the linear

curve equation of the calibration. At each stage of desalination,

the total salinity index in the oil was also determined so as to eval-

uate the efficiency of desalination according to Eq. (1). After the

fourth washing stage, the oil was centrifuged to remove any resi-

dual washing water, then it was performed the characterization

of the physicochemical properties: TSI, API gravity, TAN, total sul-

fur and kinematic viscosity at 40 C in the dry oil.

Efficiency 1 TSIADATSIBDA

1

where TSIADA is after desalination average and TSIBDA is before

desalination average, determined from the conductivity of theaqueous phase from the washing water.

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3. Results and discussion

Analyses were carried to characterize the nine crude oils stud-

ied in this work. TSI, API gravity, TAN, total sulfur content and kine-

matic viscosity of each dehydrated oil sample were measured as

described above, and the results are reported in Table 1. The results

(Table 2) show that the dehydration of the selected samples was

performed with efficiency once the final water content was below

0.25% (v/v).

3.1. Optimum conditions for the desalination of heavy oils

During the desalination process it was found that heavy oils

(API gravity around 16) tend to form stable emulsions with the

water cause of the presence of natural surfactants in major quan-tity in these oils (eg. resins and asphaltenes) [13]. The mechanical

agitation around 150 (5) rpm inside the glass flask with

temperature controlled at 60 (5) C and in the presence of demul-

sifiers can favor the desalination once it promotes the destabiliza-

tion of the emulsions. It was observed that the temperature around

of 60 (5) C favored the desalination by decreasing kinematic vis-

cosity. Thus, for an efficient separation of water in oil emulsion and

with minimal loss of light organic compounds, the desalination

process temperature was maintained at 60 (5) C because exces-

sive heat can cause changes in oil properties due to loss of light

organic compounds.

3.2. Evaluation of the desalination process by conductimetric method

The desalination process can be monitored by measuring the

ions removed during the washing steps of the oil once the ionic

conductivity is related to the ionic concentration of sodium and

chloride in the water. The process can be monitored using a metal-

lic platinum electrode to determine the conductivity at 25 C. In

Fig. 2 is shown the calibration curve of the conductivity vs TSI.

The efficiency of the desalination process can be monitored by

observing the decrease of the ionic conductivity in the washing

water with the increase of the number of washing steps (Fig. 3).

For a better relation of ionic conductivity with the salt content

in the washing water, it was built two calibration curves, one for

low conductivity values (under 5000 lS cm1) and other for high

values (over 5000). This procedure was adopted for a better accu-

racy of salt content in low concentrations. The two curves present-

ed good linear relation, with a coefficient of determination (R2) of

0.988 for low salt content (Fig. 2a) and 0.997 for high salt content

(Fig. 2b). The two curves are important for monitoring the salt con-

tent since the first washing step of the oil.

The salt content in the oil was determined after each washing

step, with the measurement made in the washing water. The num-

ber of washes necessary to reduce the salt varied according to the

amount of initial salt content in each sample. The F oil had a little

different behavior from the others, with a less conductivity

decrease from the second to the third washing step (Fig. 3a). It

was observed that by increasing the number of washes, the salt

content in the samples was reduced. After four washing steps the

average TSI of the samples was reduced to 43 mg kg1 of NaCl

(Fig. 3b). This lowsalt content could be monitored by the ionic con-

ductivity under 54 lS cm1.

3.3. Desalination efficiency of oils by monitoring the physicochemical

parameters

The physicochemical properties in the oils were analyzed and

the results before and after the desalination process were com-

pared. After four washes the ionic conductivity fell in the range

of 54 lS cm1 (Fig. 3a) with average salt content around

43mgkg1 of NaCl in the washing water (Fig. 3b). The average per-centage of the desalination efficiency was 99.87%. It can also be

Fig. 2. Calibration curve conductivity (lS cm1)vsTSI (mg kg1 NaCl). (a) Curve for

a low concentration of salt and (b) curve for a high concentration of salt.

Table 1

Results for physicochemical properties of the petroleum before the desalination process.

Oil Water content % (v/v) API gravity TSI (mg k g1) Total sulfur % (w/w) TAN (mg KOH g1) Kinematic viscosity at 40 C (mm2 s1)

A 6.92 16.8 28.6 103 0.5885 3.311 558.78

B 12.14 16.5 33.1 103 0.6801 2.799 613.89

C 8.43 16.4 28.9 103 0.6411 2.922 589.76

D 15.35 16.7 39.9 103 0.5723 3.156 600.45

E 10.20 16.6 35.8 103 0.6541 3.021 578.67

F 18.82 16.8 40.9 103 0.5932 2.896 625.09

G 5.15 16.2 31.1 103 0.6399 3.187 576.88

H 3.94 16.8 19.0 103 0.5604 3.056 560.66

I 2.85 16.5 34.1 103 0.5732 2.902 589.99

Average 9.31 16.6 32.4 103 0.5932 3.093 589.76

708 C.M.S. Sad et al./ Fuel 150 (2015) 705710


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observed inTable 2that after the fourth wash, in the dehydrated

oils, there was no significant change in the intrinsic properties of

the oils. There was an average decrease of 33% in the sulfur andTAN after the four washings. These results indicate an improve-

ment in oil quality, once the presence of sulfur compounds in the

oil is undesirable because it increases the polarity of the oil, there-

by increasing the polarity of the emulsions. These compounds are

also responsible for the corrosivity of petroleum products and pro-

duce harmful gases during the distillation process [3]. This corro-

sion is caused in particular by the naphthenic acids however, its

corrosive activity is directly influenced by the presence of sulfur

in petroleum[26].

A variation of 2.41% in API gravity and 3.25% in kinematic vis-

cosity (Table 2) are not significant variations, indicating no change

in the physical properties of the oils.

For oil desalination, ASTM standard methods are commonly

used but they need to be adapted to heavy oils [16]. If this adaptionis not properly made it can put in risk all the oil characterization

after the extraction of the salt. In this sense, we see the practical

importance of developing alternative methodologies in order to

provide reliable procedures for the extraction of salts without

changing the properties of oil. The results obtained after the desali-

nation using the desalting apparatus (Table 2) showed that this

method is promising because it does not significantly alter the

properties of the oil after desalination.

4. Conclusion

This study shows the efficiency of a new desalting apparatus

developed for heavy oils and this process consists on various wash-

ing steps of the oil. It was found that desalination in various steps

is efficient and that there was no significant loss of organic com-

pounds during the process. It was required from three to four

washes of the oil to reduce their salt content to values around

329 mg kg1 in sodium chloride.

The efficiency of the desalination process could be evaluated by

the decay of the ionic conductivity in the washing water during the

desalination process. The salt content in the oil after four washes

was around 43 mg kg1 of sodium chloride, indicating high effi-

ciency of the new desalting apparatus. It was observed that theefficiency of salt removal for heavy crude oil emulsions using the

proposed procedure was higher than 99.87% for all investigated

samples. This efficient removal of salts favored a decrease in the

total sulfur and organic acidity due to the removal of hydrolysable

salts present in the samples. The average results of API gravity and

kinematic viscosity were not altered after the desalination process.

Whether maintaining the proposed conditions of agitation, tem-

perature and concentration of demulsifiers, the desalination will

occur efficiently without changing the relevant physicochemical

properties of the oil and without occurrence of losses of light

organic compounds during desalination.

Acknowledgments

The authors are grateful to Laboratory of Research and Develop-

ment of Methodologies for Petroleum Analysis (LABPETRO/UFES)

and the PETROBRAS Research Center (CENPES).

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Table 2

Average results of the physicochemical petroleum properties before and after fourdesalination processes.

Physicochemical

properties

Before

desalination

(average)

After

desalination

(average)

Variation after

desalination (%)

Water content % (v/v) 9.31 0.25 97.32

TSI (mg kg1 NaCl) 32.4 . 103 43 99.87

TAN (mg KOH g1) 3.093 2.0107 33.44

API gravity 16.6 16.2 2.41

Viscosity 40 C

(mm2 s1)

580 561 3.25

Total sulfur % (w/w) 0.5932 0.4003 33.08

Fig. 3. Variation of conductivity by number of washings for each sample (a).

Variation of total salt index by number of washings for each sample (b).

C.M.S. Sad et al. / Fuel 150 (2015) 705710 709
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