DEPARTMENT OF CHEMICAL ENGINEERING

SCHOOL OF ENGINEERING

UNIVERSITY OF PETROLEUM & ENERGY STUDIES

October-2019

Study of Nano-composite based Pour Point Depressant for Waxy Crude oil

Submitted by
YASH CHOUDHARY, R820217134 (500060817)
ROHIT ARORA, R820217138 (500060316)
YASH GUPTA, R820217135 (500061106)
YASH SANGWAN, R820217136 (500061054)
SHIVALI DWIVEDI, R820217105 (500061666)

in

Dr. Upendra Singh Yadav Mrs. Rose Havilah Pulla

Department of Petroleum and Earth Sciences Department of Chemical Engineering
 DECLARATION BY THE SCHOLAR

I hereby declare that this submission is my own and that, to the best of my knowledge and belief,
it contains no material previously published or written by another person nor material which has
been accepted for the award of any other Degree or Diploma of the University or other Institute
of Higher learning, except where due acknowledgement has been made in text.

AUTHOR’S NAME:

YASH CHOUDHARY (500060817)

ROHIT ARORA (500060316)
YASH GUPTA(500061106)
YASH SANGWAN(500061054)
SHIVALI DWIVEDI (500061666)

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 CERTIFICATION

This is to certify that the project titled Study of Nano composite based Pour Point Depressant
for Waxy Crude oil, submitted by YASH CHOUDHARY (500060817); ROHIT ARORA
R820217138 (500060316); YASH GUPTA (500061106); YASH SANGWAN (500061054);
SHIVALI DWIVEDI (500061666) to the University of Petroleum & Energy Studies, for the
award of the degree of BACHELOR OF TECHNOLOGY in Applied Petroleum Engineering. It
is a Bonafide record of project work carried out by him/her/them under my/our supervision and
guidance. The content of the project, in full or parts have not been submitted to any other
Institute or University for the award of any other degree or diploma.

(Signature of Mentor) (Signature of Co-mentor)

Dr. Upendra Singh Yadav Mrs. Rose Havilah Pulla

Department of Petroleum Department of
and Earth Sciences Chemical Engineering

Dated: 9th October 2019

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 ACKNOLEDGEMENT

This project would not have been successful without our mentor, Dr. Upendra Singh Yadav
and our co-mentor Mrs. Rose Havilah Pulla, who gave us an opportunity to do this work. We
wish to express our gratitude for his abundantly helpful and offered invaluable assistance,
support and guidance throughout the study.
We would also like to thank Mr. Rahul Kumar, our activity coordinator who provided
resources and plans that help us in our Minor Project, Dr. P. Vijay, Head of the Department of
Chemical Engineering who provided us with an opportunity to develop the project.
Lastly but not the least, we would like to thank all those without whose support this project could
not have been a successful one.

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 ABSTRACT

In the pipeline industries, precipitation of wax crystals in crude oil has been presenting a costly
problem in the transportation and storage of crude oil. It complicates the low-temperature
properties of oil and pipeline could become completely clogged. A well-recognized and efficient
solution to these problems is Pour Point Depressant (PPDs). However, conventional PPDs (like
POA, EVA) still have some disadvantages, such as unsatisfactory performance, could be affected
by components of oil like asphaltene and have poor thermal resistibility.

Due to the effective advantages of polymer / inorganic nanocomposites, we developed

nanocomposites PPDs by dispersing nanoparticles into polymeric PPD matrices to improve the
performance of conventional PPDs. So, the use of nanocomposites as a pour point depressant for
crude oil has opened the door for the new field of research in the petroleum industry, and it is
very crucial to enhance the efficiency of a nanocomposite as a pour point depressant (PPD) to
modify the waxy crude oil.

In this present work, we will consider the Indian waxy crude oil as the model oil and synthesize
the new nanomaterial-based pour point depressant (Nano-composites) and evaluate the
performance of newly synthesized Nano-composites Pour point depressant, also compares its
performance with different traditional PPDs and other nanocomposites. We will characterize and
compare its various physicochemical and rheological properties with other nanocomposites and
PPD through various instruments like Fourier-transform infrared spectroscopy) (FTIR),
X- Ray Diffraction (XRD) and so on.

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 TABLE OF CONTENT

CERTIFICATE ................................................................................................................................3

ACKNOLEDGEMENTS .................................................................................................................4

ABSTRACT .....................................................................................................................................5

INTRODUCTION ...........................................................................................................................7

LITERATURE REVIEW ..............................................................................................................11

MATERIALSANDMETHODOLOGY .........................................................................................20

MATERIALS USED IN THE PROJECT: ....................................................................................20

METHODOLOGY………… ........................................................................................................20

RESULTS AND DISCUSSION ....................................................................................................23

CONCLUSION ..............................................................................................................................25

REFERENCES ..............................................................................................................................26

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 CHAPTER - 1

INTRODUCTION

Crude oil is an important fossil fuel, which contains saturated hydrocarbons, paraffins, aromatics,
asphaltenes, and resins, and has a complex nature. [1] Generally, paraffins are dissolved with a
balanced state in the crude oil at higher temperature,[2] but when the temperature falls below a
certain temperature, i.e., Wax Appearance Temperature(WAT),paraffins with Carbon number
C16-C40 will precipitate out and form a three-dimensional network structure thus, formed the
crystallized wax.[3,4]

Pour point depressants don't bring down the temperature at which wax precious stones start to
frame, called the cloud point or the measure of wax that is shaped—pour point depressants work
by adjusting the gem shape and size, which represses parallel gem growth. There are two known
strategies by which this might be accomplished: surface adsorption and co-crystallization.
Any decrease in an oil's pour point relies upon both the synthesis and properties of the oil, just as
the kind of pour point depressant utilized. Different elements are the substance's relative atomic
weight, its compound piece, and the substance's fixation in the oil. On the off chance that the
centralization of pour point depressant is excessively high, there might be an unmistakable
impact on thickness at higher temperatures

These Wax crystals crystallize in orthorhombic structures and appear as plates.[5] Wax crystals
cause the transition of crude oil from sol to gel. Due to the London forces which are operated
between the wax crystals and large aspect ratio of the plates, a small amount of the precipitated
wax crystals (as little as 0.5 wt.%) could form the volume spanning networks which trapped the
crude oil resulting in high pour point (PP), high yield stress, and a non-Newtonian flow behavior
of the crude oil. [6, 7] This deteriorates the rheological properties and flowability of crude oil,
generating issues in pipeline transportation and storage. The sol-gel transition of crude oil is
denoted by Gelation point (GP).[8]

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The GP, at which the elastic modulus of the oil begins to become larger than the viscous
modulus of the oil. This phenomenon of wax deposition reduces the effective diameter of
pipeline and also cause blockage of pipelines under severe low temperature conditions.[9]
Therefore, management of wax precipitation, wax gelation in flow assurance of crude oil and
emergency intervention planning can be a large challenge.[10]Common way of improving the
rheology of crude oil is using traditional Polymeric Pour Point Depressant(PPD). These are
homo and co-polymers of different monomers which can interact with the crude oil through
nucleation, adsorption, and co-crystallization mechanisms. [11] In the Pipeline industries, Comb-
like copolymer and EVA-type polymers which exhibit Pour Point Depressant Properties had
been widely used.[12,13] These two types of polymeric PPDs often contains nonpolar carbon
chains and polar groups, the nonpolar parts could take part in the precipitation process of wax
crystal through nucleation and co-crystallization effects, whereas the polar groups can increase
the repulsion effect for the deposition of wax crystals and interfere in the growth of wax
crystals.[14]

The most effective comb-like PPD for waxy crude oil is Poly(octadecyl acrylate) (POA), which
co-precipitates with wax molecules and forms island defects on the wax crystals surface, result in
blocking the growth of crystals.[15,16]These PPDs prevents the growth of wax crystal and
modifying the morphology of wax crystal. However, traditional PPDs also exhibit several
drawbacks that limit its application, including reduction in robustness under the effect of
shearing and/or heating.[17] Instead of crude oil, wax also exists in various polar substances.
Asphaltene can influence the viscosity and pourpoint of oil. Moreover, they can also decrease the
efficiency of PPD. Thus, a certain type of polymer PPD has lack in universality among different
oils. [18] Inspired by the advantages of the inorganic nanoparticles in petroleum industries, we
have been used it to enhance the performance of traditional PPDs and thus prepared the different
class of PPDs, i.e., Nano-composite PPDs.

The Nano-composites are the blend of polymer matrix as the continuous phase, inorganic
nanoparticles, fibers, carbon nanotubes, and other modifiers as the dispersed phase, and the
modifier is uniformly dispersed in the matrix material through an appropriate preparation method
to form a composite system containing a nanometre-sizedmaterial, this system material called
Nano-composite material.[19]

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In simple words, it is the coating or adsorption of organic polymer on the surface of inorganic
nanoparticles. After inorganic nanoparticles were dispersed into the polymer matrix, resultant
properties (such as mechanical, thermal, and electrical) of polymer are improved greatly as
compared to the neat PPDs. The performance of the Nano-composite depends on the
compatibility between the inorganic nanoparticles and organic polymer or by improving the
preparation method. Compared with solvent blending method, Melt Blending method with the
aid of an extruder is a more efficient method in terms of dispersing nanoparticles in the polymer
matrix.
For instance, in POA/SiO2 Nano composite produced by solution blending method, POA is
easily desorbed from the surface of Nano- silica due to poor compatibility between inorganic
Nano SiO2 and organic POA. Thus, we can enhance its performance by prepared it by Melt
Blending method results in strengthen the adhesion of POA on non-silica and improved stability
of material.

At present, Nano-composite pour point depressants are mainly divided into two types-

a) Blended Nano-Composite Pour Point Depressant

The blended Nano-composite pour point depressant is generally prepared by traditional poly -
octadecyl acrylate(POA) pour point depressant and EVA pour point depressant with inorganic
Nano particles in a certain proportion through solution blending or meltblending.Organic
Modification of inorganic Nanoparticle is another important means to improve the stability of
blended Nano composite PPD which can enhances the compatibility between Nano-particles and
polymer matrix. This is done by chemical grafting, cation exchange and intercalation of organic
molecules.
In 2016, Y. Wang used an ion exchange reaction to organically modify montmorillonite (MMT),
and prepared the Nano-composite pour point depressant (NPPD) by melt blending. They found
that NPPD has good stability in the oil phase the large electrostatic repulsion inhibits the
aggregation of wax particles, and stabilizes the oil system.[20]

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b) Polymeric Nano-Composite Pour Point Depressant

Al-Sabagh et al. introduced a polymerizable organic group on the Nano-MMT by ion exchange
reaction, and then used methyl methacrylate (MMA) to prepared the PMMA/MMT Nano-
composite pour point depressant by in-situ radical polymerization which have high compatibility
in the oil.[21] (Figure 1)

Figure 1. The mechanism of enhancement of the flow properties by the PMMA–MMT

In this present work, we will consider the Indian waxy crude oil as the model oil and synthesize
the new Nano material-based pour point depressant (Nano-composites) and evaluate the
performance of newly synthesized NPPD, also compares its performance with different
traditional PPDs and other nanocomposites. We will characterize its various physicochemical
rheological characteristics through various instruments like FTIR, XRD and so on.

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 CHAPTER - 2

LITERATURE REVIEW

First of all, Literature review will be carried out and information related to various problems
involved during the transportation of Indian heavy and waxy crude oils will be collected for
different oil fields of India. After then, heavy and waxy crude oil samples will be collected from
the different Indian oil fields. These crude oil samples will be characterized by different standard
ASTM/API methods and by using different analytical equipment's like High temperature gas
chromatography (HT-GC), Fourier transform infrared spectroscopy (FTIR) TGA/. DTA, and
DSC etc.

Rheological properties of oil samples will be investigated using a rheometer. Then Nano particle
based suitable surfactants (emulsifiers), pour point depressants (PPDs) and other requisite
additives will be identified and synthesized in the laboratory. These synthesized nanocomposites
/additives will be characterized on the basis of their physio chemical properties and by using
analytical instrument like FT-IR, scanning electron microscopy (SEM), and X-Ray Diffraction
(XRD), etc. Application of synthesized
nanocomposites will be evaluated as surfactants and pour point depressants to improve flow
ability of Indian heavy and waxy crude oils, respectively, through pipelines.

The pour point and rheological parameters of the prepared heavy crude oil emulsions and treated
waxy crude oils will be studied using pour point apparatus and rheometer, respectively. Stability
of prepared emulsions will also be investigated using bottle test method. Further, the different
factors such as Surfactant concentration, oil-water ratio, water salinity, pH etc. which affect the
flow behavior of emulsions as well as emulsion stability will be studied thoroughly. For waxy
crude oils, dosage of pour point depressants will also be optimized. A particle size analyzer will
be used to study the droplet size of oil in prepared oil-in-water emulsions. An optical Rao scope
will be utilized to study the changes in the size of wax crystals in waxy crude oil after treatment
with PPDs. Based on the results observed, scientific articles will be written and published.

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The influence of the nano-hybrid pour point depressant (NPPD) on flow properties of waxy
crude oil was studied. Rheological results showed that NPPD demonstrated better improvement
in viscosity, yield stress and pour point reduction for crude oil than the conventional polymer
PPD (N6) did Moreover, the viscoelastic behavior data showed that the NPPD doped oil had a
weaker gel network structure at a low temperature compared with N6 doped oil. Differential
scanning calorimetry results revealed that

NPPD reduced the wax appearance temperature (WAT) and the wax precipitation amount within
the temperature range from WAT to 20 C. The difference of shape and size of wax crystals in
undoped and doped oils was studied by X-ray diffraction and polarized optical microscopy. The
total interaction energy between wax particles was calculated according to the Derjaguin–
Landau–Verwey–Overbee theory using f potential. It was found that the energy barrier between
the wax particles in the NPPD doped oil was higher than that in N6 doped oil. The larger
electrostatic repulsion inhibited the aggregation of the wax particles and stabilized the NPPD
doped oil system.

The nano-hybrid pour point depressant (NPPD) was used to improve the flowability of the waxy
crude oil. The influence of NPPD on the shape and size of the wax crystals was studied. At the
dosage of 100 ppm, NPPD greatly decreased the pour point, viscosity and yield stress, and it had
a much better improvement of oil flowability than the polymer PPD N6.Time sweep
measurements showed that WCO-NPPD possessed a weaker wax structure than WCO and
WCO-N6 leading to the lower viscosity and yield stress. DSC results showed that NPPD could
reduce the WAT and wax precipitation amount of the crude oil. NPPD performed as
heterogeneous nucleation sites for the paraffin chains and refined the wax crystal particles.

The XRD and POM results confirmed that the crystal shape and size was modified by NPPD.
The wax crystals became more compact and more liquid contents were released from gel
networks. The action mechanism of NPPD was complicated, which might be the combination of
the effects of the nanoparticles and EVA.As the different crude oil or model was adopted in each
study, it was difficult to get the unified theory to explain the experiment results.

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It might be that the EVA component could co-crystalize with the paraffin chains, modified the
size and shape of wax crystals, while the nanoparticles provided heterogeneous nucleation sites
and charged the wax crystals resulting in the large electrostatic repulsion. The presence of the
nanometric component in the NPPD made a great contribution in the hindered formation of the
wax gel networks, enhanced stability of the wax crystals in the oils and thus improved
significantly the flowability of the oil.

Cunzhe He, Yanfen Ding, Juan Chen, Feng Wang, Chong Gao, Shimin Zhang, Mingshu Yang in
2019 has studied the influence of nano-hybrid por point depressant on flow properties of waxy
crude oil. Results showed that NPPD demonstrated better improvement in viscosity (reduction
was done about 82%), yield point stress and pour point reduction of crude oil (from 30.0 degree
Celsius to 3degree Celsius) using the required composition.

Zhiwei Chan, Guolin Jing, Zhengnan Sun and Chen Zeng in 2018 introduced that chemical
modifications of waxy crude oil from traditional pour point to nanocomposite pour point
depressant resulted in the better results in the latter case since it restricts the formation of three
dimensional.

Crude oils containing large quantities of waxes, and in situations where sudden temperature
drops occur, a crystalline network can be formed, generating flow difficulties in production,
transfer and offloading lines. Despite the scientific and economic importance of this
phenomenon, correlations between the behavior of petroleum in relation to its pour point are
scarce in the literature. Many crude oil samples were characterized regarding density, water
content, wax fraction (one- and two-dimensional chromatography), pour point, yield stress and
wax appearance temperature.

The results showed that the storage conditions and oil characteristics had a strong influence on
the pour point. Yield stress was influenced by initial temperature of the sample, cooling rate and
shear rate during cooling. Finally, the content of aromatic compounds in oil with low
concentration of n-alkanes can contribute to increase the pour point was one of the result which
was concluded by doing the experiments.

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The mass fraction is large, and the mass fraction of colloid and asphaltene is relatively small.
And blue Compared with sea crude oil, Changing crude oil has a relatively low wax content.
China is rich in high waxy crude oil, which has high freezing point and high viscosity. The
rheology is complex, which makes it difficult to extract and transport crude oil. Adding a
polymer pour point depressant to crude oil can change the wax crystals in crude oil. The
diversity and complexity of crude oil composition, people pour point depressant. The regular
understanding is still insufficient.

The pour point depressant, its synthesis and characterization has been widely concerned. In order
to guide the development and application of EVA type pour point depressants. The
crystallization characteristics of waxy crude oil before and after, observed by polarized light
microscope. The change of wax crystal morphology in crude oil before and after the addition,
and through the freezing point experiment and rheological experiments evaluated PA pour point
depressants for two different compositions. The pour point depressing effect of wax crude oil, in
order to find out the drop of PA on waxy crude oil.

The effects of the POA and POA/clay nanocomposite PPDs on the structural properties of
gelled Changing waxy crude oil were well studied through rheological tests, DSC analyses and
microscopic observation. Melt blending method was used here to prepare the poly (octadecyl
acrylate) (POA)/clay nanocomposite PPD, which shows much better performance on waxy crude
oil. The precipitated wax crystal amount of the crude oil at low temperatures does not change
with the addition of POA and nanocomposite PPDs, but the addition greatly weakens the
structure of the gelled crude oil.

Compared with the same dosage of POA, the addition of nanocomposite PPD further inhibits the
formation of wax crystal’s network and further weakens the structural strength and
viscoelasticity of the gelled crude oil. Increasing the dosage of nanocomposite PPD favours the
weakening of the gelled crude oil structure. The nanocomposite PPD particles can act as
nucleation templates of wax crystals and further weaken the gelled structure of waxy crude oil.

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CONCLUSION

 On individually increasing the PPD dose, the pour points of the model oil first decrease
and then increase, and nano-hybrid PPDs exhibit a better improved effect than pure EVA
(VA = 32%).
 The nanoparticle with polymer coverage is another key determinant for the effect of
nano-hybrid PPDs, indicating that the compatibility between the stearic acid-modified
ATT and EVA is better than acetic acid-modified ATT
 Compared with 200 ppm dosage of Acetic acid-modified ATT(A-AtPPD(32)) and
modified nano-SiO2 composite PPD (N-SiPPD(32)), stearic acid-modified ATT (S-
AtPPD(32)) exhibits an improved effect, which decreases the pour point of the
model oil from 30°C to −1°C.
 Adding 400 ppm N-SiPPD (32) can decrease the pour point of the model oil from 30°C
to −3°C, but adding 200 ppm S-AtPPD (32) is more efficient and economic.
 It is worth noting that the viscosity of the model system composed of 200 ppm S-
AtPPD(32) is lower than that of 200 ppm N-SiPPD(32), and similar to that of 400 ppm
N-SiPPD(32). This also indicated that adding 200 ppm S-AtPPD (32) is more
efficient and economic.
 The decrease of the mean nanocomposite PPD particle size from 6 μm (prepared by
solvent blending) to 2 μm (prepared by melt blending) changes the dispersed state of
POA molecules in oil phase and thus greatly enhances the performance of nanocomposite
PPD.
 The WAT decreases from 30.3C to 27.3C after the addition of 200 mg/kg POA. After the
nanocomposite PPD is added, the WAT of the crude oil increases gradually from 28.2 C
at 200 mg/kg dosage to 29.0 at 400 mg/kg dosage, and then to 31.3 C at 800 mg/kg
dosage.

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Author Name Description Significance Year

Fang Wang, Shimin The effect of novel nanohybrid 2011

Zhang nanohybrid materials pour-point
on the pour-point and depressant (PPD) was
viscosity depressing used to decrease the
of waxy crude oil pour point and
viscosity of waxy
crude oil

Ziyi Tu, Guolin Jing, Effect of Modified ATT/EVA 2017

Zhengnan Sun, Zhiwei nanocomposite of PPDs were
Zhen & Wei Li attapulgite/EVA on successfully
flow behavior and wax prepared via toluene
crystallization of solvent blending and
model oil the compatibility
between ATT and
EVA was improved
through chemical
modification.

Zhiwei Zhen, Guolin Nano-composite pour Improving the 2018

Jing, Zhengnan Sun & point depressants in performance of pour
Chen Zheng improving the point
rheology of waxy depressants and
crude oil improve the low-
temperature rheology
of the crude oil

Fei Yang Depressive effect of addition of PA can 2009

polyacrylate (PA) inhibit the wax
pour point depressant precipitation and
on waxy crude decrease the wax
oils appearance
temperature of waxy
crude oils.

Fei Yang, Bo Yao, Effects of pour point widen the 2015

Yalian Zhang depressant of crystallization
EVA/nano MMT temperature range and
composites on reduce wax
Changqing precipitation point of
crude oil crude oil.

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Zeheng Peng, Wei Influence of Specific three types of 2019
Wang, Huirong Surface Area and nanoparticle HNP,
Huang, Siyuan Yang, Morphology of MNP and LNP were
Jing Gong Nanocomposite Pour produced and
Point Depressant on correspondingly three
the new types of
Modification of Waxy nanocomposite pour
point depressant
HNC-PPD, MNC-
PPD and LNC-PPD
were produced
successfully.

Bo Yao ,Huanxian Li, isothermal Larger and more 2018

Fe I Yang And Guangyu crystallization compact wax crystal
Sun properties and flocs.
improved rheological The wax crystals were
performance of waxy larger and more
crude oil using compact and,
polyoctadecylacrylate- therefore, adversely
modified affected the formation
montmorillonite of a strong
composite as a pour wax crystal network,
point depressant which improved the
rheological
properties of the
POA/O-MMT
composite PPDs

ens Norrman, Nanoparticles for Adsorption data 2016

malie Solberg, ohan Waxy Crudes: Effect obtained from QCM-
Sj of Polymer Coverage D from a flat surface
blom, and Kristofer and the can be used for
Paso Effect on Wax optimization of mount
Crystallization of
coating material for
silica nanoparticles.
From the combined
data of the rheology
and DSC, it is shown
how nanoparticles
with different POA
coverage affect the
strength of the wax
crystal network.

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Yaqin Wu, Sally A. Optimization of Pour A joint effort between 2013
Thomas, and Andika Point Depressant COP’s technical
P. Sigit, Treating Rates for support laboratory and
ConocoPhillips and Crude and the COPI Kerisi
William H. Condensate Blends Project Team in
Thomason, Bill Using an Onsite Indonesia successfully
Thomason Densitometer. developed a field lab
Consulting procedure to enable
selection of the
optimum PPD treating
rate for the Kerisi
crude pipeline. This
procedure enables
reliable operation of
the pipeline at
minimum costs in
PPD treatment.

Huirong Huanga The effect of cooling influence of 2019

, Wei Wanga processes on the yield nanocomposite pour
, Zeheng Penga stress of waxy model point de-
, Kai Lia oil with pressant (NPPD) and
, Dongying Gana nanocomposite pour traditional pour point
, Shengnan Zhanga, point depressant. depressant
Yanfen Dingb ethylene/vinyl
, Haihao Wua acetate polymer
, Jing Gonga, (EVA) on the yield
stress of waxy model
oil under
different step-cooling
frequencies.

Cunzhe He Influence of the nano- The hindered 2015

, Yanfen Ding hybrid pour point formation of
, Juan Chen depressant on flow the wax gel networks,
, Feng Wang properties enhanced stability of
, Chong Gao of waxy crude oil the wax crystals in
, Shimin Zhang the oils and thus
, Mingshu Yang improved significantly
the flowability of the
oil.

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COST ESTIMATION AND RESOURCE AVAILABILITY:
The resources required are:
 Crude Oil with unknown physical properties.
 Nano-composite of different types (nano-silica, carbon tubes).
 Apparatus Required:
a) GC-MS Apparatus
b) FTIR Apparatus
c) Cloud and Pour Point Apparatus
d) Weighing Scale

It is expected that we will need money only for purchasing nano-composite and other chemicals.

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 CHAPTER - 3
MATERIALS AND METHODOLOGY

3.1 Materials used in the project :

 Crude oil
 Hexane
 Gas chromatography Apparatus
 Pour Point and Cloud Point Apparatus
 FTIR Apparatus
 Heating Mantle to heat crude oil to form liquid around 50-60 degree Celsius.
 Weighing Machine for density
 Nano-composite
 XRD Apparatus
 Polymers

3.2 Methodology :

First of all, Literature review will be carried out and information related to various problems
involved during the transportation of Indian heavy and waxy crude oils will be collected for different oil
fields of India. After then, heavy and waxy crude oil samples will be collected from the different Indian
oil fields. Fourier transform infrared spectroscopy (FTIR) (It is a technique used to obtain an
infrared spectrum of absorption or emission of a solid, liquid or gas. An FTIR spectrometer
simultaneously collects high-spectral-resolution data over a wide spectral range. This confers a
significant advantage over a dispersive spectrometer, which measures intensity over a narrow
range of wavelengths at a time.).

Rheological properties of oil samples will be investigated using a rheometer. Then Nano particle
based suitable surfactants (emulsifiers), pour point depressants (PPDs) and other requisite
additives will be identified and synthesized in the laboratory.

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These synthesized nanocomposites /additives will be characterized on the basis of their physio-
chemical properties and by using analytical instruments like FT-IR and X-Ray Diffraction
(XRD). (It is a rapid analytical technique primarily used for phase identification of a crystalline
material and can provide information on unit cell dimensions. The analyzed material is finely
ground, homogenized, and average bulk composition is determined.)

Application of synthesized nanocomposites will be evaluated as surfactants and pour point

depressants to improve flow ability of Indian heavy and waxy crude oils, respectively, through
pipelines. Then pour point and rheological parameters of the prepared heavy crude oil emulsions
and treated waxy crude oils will be studied using pour point apparatus and rheometer,
respectively. Stability of prepared emulsions will also be investigated using bottle test method.
Further, the different factors such as Surfactant concentration, oil-water ratio, water salinity, pH
etc., which affect the flow behavior of emulsions as well as emulsion stability will be studied
thoroughly. For waxy crude oils, dosage of pour point depressants will also be optimized. A
particle size analyzer will be used to study the droplet size of oil in prepared oil-in-water
emulsions.

Procedure For Gas Chromatography

SETTING OPERATING CONDITIONS

 First of all, set the Initial Temperature to 60deg. C for 2 minutes in the Method Editor.
Then, Set Ramp 1: 5.0 deg/min to 120 deg. hold for 5.00 min.
Ramp 2: 5.0 deg/min to 200 deg. hold for 5.00 min.
Ramp 3: 5.0 deg/min to 300 deg. hold for 5.00 min.
 Secondly, set the 65 min. Run-time for GC and MS.

SAMPLE PREPARATION
 Methane and Ethane are unable to mix with the crude oil and don’t form the
homogeneous solution.
 Finally, crude oil got mixed with hexane to forma dark-brown homogeneous solution and
we used it as the test solution.
 Now, we withdrew the 20 μL and 10 μL test solution through injector and inject it into
two plastic vials filled with 100 μL hexane and labelled it as and B respectively.

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  Both A and B appeared as light-brown solutions. So, we further diluted the solution by
taking out the 10μL solution from vial A through injector and put it in another vial
(labelled as C) filled with 100μL hexane and we got the crystal-clear solution.
 Now, we took out the almost whole solution from vial C through injector and then
attached the 0.2mm syringe filter to same injector and passed the solution through it and
again kept the solution in another vial D.
 We considered this solution as final injecting solution.
 We used syringe filter to remove the suspended particles from the crystal-clear solution
which could cause damage to GC equipment.

INJECTING THE FINAL SAMPLE

 Rinse Micro syringe thrice with hexane. Withdraw the hexane slowly.
(If there are air bubbles, dispense quickly to remove them).
 Further, withdraw 1.0 μL of final injecting solution from Micro syringe and inject the
solution into sample Injection port.
 After injecting, wipe-off the outside of the micro syringe immediately and again rinse
micro syringe with hexane to avoid the clogging of syringe by the solution.
 Finally, take the chromatograph after provided residence time.

Hexane A B Vial C D
Figure 2. Samples Preparation for Gas chromatography

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 CHAPTER - 4

RESULT & DISCUSSION

 Density has been calculated by using weight by volume method and the resultant density
comes out to be 0.942:
Density = (Weight/volume)
 The degree API has been calculated using the formulae:
API= 141.5/ (S.G)-131.5
And it comes out to be 18.712 which indicates that the crude oil belongs to the black crude oil
category and further studying out the properties of this crude oil indicates that GOR is generally
between 200-300 scf/STB and generally brown to black in color.
 The cloud and pour point has been calculated using pour point and cloud point apparatus
and result come out to be
Cloud Point= 39 Celsius
Pour Point= 36 Celsius
 The Fourier transform infrared radiation and gas chromatography has been done and the
results are as shown

FTIR RESULT:

Figure 3. FTIR results depicting molecular composition and structure of Crude Oil Sample.
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GAS CHROMATOGRAPHY RESULTS

Figure 4. Chromatograph for crude oil sample.

Table 1. Compounds present in Crude oil Sample

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 CHAPTER - 5

CONCLUSION

 All the experiment results will show Physico-chemical characteristics like pour point,
cloud point, API etc. of Indian heavy/waxy crude oil samples.
 Gas chromatography (GC) was performed which is a common type of
chromatography used in analytical chemistry for separating and analyzing compo
vaporized without decomposition. Typical uses of GC include testing the purity of a
particular substance, or separating the different components of a mixture.
 FTIR analysis revealed the presence of various useful functions groups which
confirmed the existence of aromatics, phenols, alcohols, ethers, esters, and aldehyde.

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