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EXPERIMENT 4
OIL FIELD QUALITY CONTROL TEST
CLOUD POINT AND POUR POINT DETERMINATION
BY
AMUSAT, ISLAMIA DASOLA
125/18/2/0152
IN PARTIAL FULFILMENT OF REQUIREMENTS FOR PETROLEUM
ENGINEERING LAB III COURSE
(PEE 513)
15TH OF DECEMBER, 2022.
ii
ABSTRACT
In this experiment, the cloud and pour point of the Nigerian Niger Delta Crude oil were determined so as
to ascertain the temperature at which wax crystallizes and precipitates during crude transportation. Six (6)
crude samples were collected and analysed in the laboratory and the results showed that each of the samples
had varying cloud points; Sample A -21o
C, Sample B - 12 o
C, Sample C - 21 o
C, Sample D - 19 o
C, Sample
E -8.5o
C and Sample F โ€“ 8.7 o
C with a mean value of 17.6 o
C. Same trend was also exhibited by the pour
points; Sample A โ€“ 1.4 o
C, Sample B - 6o
C, Sample C - 17 o
C, Sample D - 11o
C , Sample E โ€“ 8.5 o
C and
Sample F โ€“ 8.7 o
C with a mean value of 8.76 o
C. It was then concluded that wax deposition during crude
transportation in the region can be prevented especially in onshore pipelines if efficient preventive measures
are put in place being that the region in the tropics with a minimum ambient temperature of 180C. Factors
that affect cloud and pour point of crude oil were also highlighted and recommendations that will help
prevent crude oil from wax crystallization and precipitations were given.
iii
TABLE OF CONTENTS
TITLE PAGE i
ABSTRACT ii
TABLE OF CONTENTS iii
LIST OF FIGURES iv
LIST OF TABLES v
INTRODUCTION 1
THEORY 3
AIM AND OBJECTIVES 4
MATERIALS AND APPARATUS 4
METHODOLOGY 6
RESULTS AND DISCUSSION 7
CONCLUSION AND RECOMMENDATIONS 14
REFERENCES 15
iv
LIST OF FIGURES
Figure 1: Manual cloud point and pour point tester 5
Figure 2: Graph of specific gravity against pour point 8
Figure 3: Graph of specific gravity against cloud point 9
Figure 4: Graph of specific gravity against cloud point 12
Figure 5: Graph of specific gravity against pour point 13
v
LIST OF TABLES
Table 1: Results showing pH, Density, Specific Gravity, Cloud and Pour Point of Crude Samples. 7
Table 2: Table of specific gravity and pour point 8
Table 3: Table of specific gravity and cloud point 9
1
INTRODUCTION
Crude oil is a naturally occurring mixture, consisting predominantly of hydrocarbons, sulphur, nitrogen and
metals. Crude oils are complex but mainly paraffinic, naphthenic and aromatic. Crude oils contain all
normal alkenes from C1 to C120. However, this percentage rises to 35% in highly paraffinic and decreases
to zero in highly bio graded oils. Nigeria has a substantial reserve of paraffinic crude oils known for their
good quality (low sulphur, high API gravity), and containing moderate to high contents of paraffinic waxes.
Waxy crude oils have undesirably high pour points and are difficult to handle where the flowing and
ambient temperatures are about or less than the pour-point and high pour point oil reservoirs are usually
part of the developed oilfields in various regions worldwide. Waxy crude oils also exhibit Bingham non-
Newtonian flow behaviour below the cloud point due to wax crystallization. The Nigerian Niger Delta
crude oil, which is the mainstay of Nigerian economy, exhibits waxiness, with deposits in the range of 30-
45 %. During its transportation, because oil temperature at initial station is higher than the ambient
temperature, the oil temperature continues to decrease, and when it decreases to the wax precipitation point
of crude oil, wax crystal in crude oil starts to precipitate, grow, and deposit on the pipe wall finally;
sediments on pipeline will reduce the effective flow area of the pipeline, increase friction, and thus reduce
transmission capacity of the pipeline. Also, production tubing had waxed up in several cases and this had
resulted in the expensive maintenance procedure of wax cutting which involves using scrapers conveyed
by wire line. Billions of dollars has been lost to its prevention and remediation. Wax deposition in crude
oils has been a problem in crude transportation for a long time and the difficulties in pipeline transportation
are due to this complex nature of crude oil, which cause a variety of difficulties during the production,
separation, transportation and refining of oil. When a waxy crude oil is cooled, the heavier paraffinic
constituents begin to separate as solid crystals once the solubility limit is exceeded. Thermodynamically,
the solid-liquid phase boundary temperature, that is the maximum temperature at which the solid and liquid
phases co-exist in equilibrium at a fixed pressure, is the wax appearance temperature (WAT). It is also
known as the Cloud Point which depends on wax concentration, the crystallization habit of wax, and the
shear stability of different wax structures. Crude oil starts to lose its flow characteristics when wax
crystallization begins to occur. The lowest temperature at which the oil is mobile is termed Pour Point.
Therefore, cloud points and pour points are of immerse importance of any liquid in fuel to prevent all the
problems encountered in pipeline during crude transportation.
Cloud point is the temperature at which the oil becomes cloudy and the first particles of wax crystals are
observed as the oil is cooled and gradually under standard conditions. The cloud point of any liquid fuel is
an indicator of how well the fuel will perform and indicates the tendency of the oil to plug under cold
weather conditions. Cloud point can be measure both manually and automatically.
2
Pour point is the lowest temperature below which the fuel loses its flow characteristics. It is the opposite of
cloud point as it is refers to the lowest temperature at which we can observe the movement of oil and also
we can pump the fuel easily.
Factors Affecting Cloud and Pour Points of Crude Oil
There are certain factors that directly affect the cloud and our point of crude oil. Proper management of
these parameters will help control the rate with which crude oil reaches its cloud and pour point. These
parameters are discussed as follows;
Temperature Differential: Wax deposit decreases with an increase in temperature difference. The drop in
wax deposition rate with increase in temperature difference could be attributed to the extra heat gained or
added in the solution, which would further move the solution away from its cloud point. Hence the process
of crystal formation and their deposition is a function of temperature difference. Since wax deposition is
directly affected by cloud and pour point, there exists a direct relationship between these temperature points
and temperature differential between the waxy crude and pipeline wall.
Paraffin Wax Content: The amount of paraffin wax in a crude oil sample affects its cloud and pour point
temperatures. Wax deposition has a higher tendency to occur in crude oils with high paraffin wax content
than those with lesser paraffin wax because wax can easily agglomerate when it is high in content than
when it is not. As such, the amounts of paraffin wax present in a crude sample directly affect the rate at
which it will reach its cloud and pour point.
Flow rate: Higher flow shear, which is a function of flow rate, leads to lesser but likely harder wax deposit
build up. Thus wax deposition gradually decreases with increase in flow rate and turbulence. The effect of
increasing flow rate, decreasing the amount of wax deposited or entrapped oil in the deposited, This can be
explained; that as the velocity of the moving stream increases, the molecules gain more energy with a
corresponding increase in temperature which would reduce the tendency with which the waxy crude would
reach its cloud and pour point.
Surface Properties: Properties such as density, specific gravity and viscosity are determinants of the cloud
and pour point of crude oil sample. There exists a relationship between density and specific gravity. Also,
viscosity is affected by specific gravity because the denser a fluid, the more viscous it becomes. Since
viscosity directly affects cloud and pour point, it is essential to state that the higher the density, specific
gravity and viscosity of crude oil sample, the more its tendency towards reaching its cloud and pour point.
3
THEORY
Due to flow assurance problems encountered during crude transportation using pipelines in the oil and gas
industry, it has become of paramount importance to study the different factors that enhance wax deposition
in pipelines. Several researchers have done work on the subject matter and have been able to predict using
scientific methods conditions that promote wax deposition while also professing ways to combat its
undesirable occurrence. Amongst the numerous researches done, some are discussed here. It was stated that
the main components of the heavy fraction of hydrocarbon which participate in the solid phase formation
include asphaltenes, diamondoids, petroleum resins and wax. Petroleum wax consist mainly saturated
paraffin hydrocarbons with number of carbon atoms in the range of 18-36. Wax may also contain small
amounts of naphthenic hydrocarbons with their number of carbon atoms in the range of 30-60. Wax usually
exists in intermediate crudes, heavy oils, tar sands and oil shales. There are three main factors that affect
wax deposition in flow systems are flow rate, temperature deferential, and cooling rate, as well as surface
properties. The mechanism of wax deposition could be summarized as the following four types: molecular
diffusion, shear dispersion, Brownian diffusion and gravity settling, in which molecular diffusion was
generally considered as the most important mechanism causing wax deposition. Shear dispersion, Brownian
diffusion and gravity settling had little influence on wax deposition, namely molecular diffusion was
dominant mechanism of wax deposition. Shear dispersion also had an influence on wax deposition, but the
main cause was still molecular diffusion, the process of wax deposition could be described by the following
steps:
๏ถ Gelation of the waxy oil on the cold surface
๏ถ Diffusion of waxes towards the gel layer from the bulk
๏ถ Internal diffusion of these molecules through the trapped oil
๏ถ Precipitation of these molecules in the deposit
๏ถ Counter diffusion of de-waxed oil out of the gel layer. This proposition was confirmed by
measuring the carbon number distribution in the sample of wax deposition layer under different
experimental time.
4
AIM AND OBJECTIVES
The aim of this experiment is to determine the cloud and point of crude oil samples obtained from the Niger
Delta region of Nigeria and, to make some analytical predictions and recommendations base on the results.
The specific objectives are listed below;
๏ถ To determine the temperature at which the sampled crude oil becomes semi solid and loses their
flow characteristics.
๏ถ To compare the cloud and pour point of the different crude samples.
๏ถ To make recommendations as to how wax deposition can be prevented during crude transportation
Materials and Apparatus
Material
Crude samples with a known pH, density and specific gravity.
Apparatus
Cloud point and Pour point tester with the following components parts;
๏ถ Test jar
๏ถ Cork carrying thermometer
๏ถ Jacket
๏ถ Gasket
๏ถ Disc
๏ถ Cooling bath containing salt and crushed ice.
5
Figure 1: Manual cloud point and pour point tester
6
METHODOLOGY
The initial temperature, pH and specific gravity of the crude oil samples were determined before
commencing the experiment.
Procedure for Cloud point Determination.
๏ถ A suitable freezing mixture of salt and crushed ice in cooling bath was prepared.
๏ถ The oil was poured into the test jar up to the etched mark.
๏ถ At each test thermometer reading i.e. the multiple of 1c, inspect for cloud.
๏ถ Reading which reveals the distinct cloud or haze in the oil at the bottom of jar is the cloud point.
Procedure for Pour Point Determination.
๏ถ The oil was continue to cool further
๏ถ As soon as the oil in the jar doesnโ€™t flow when the jar is titled, the test tube was hold horizontally
for 5 seconds and observe it carefully
๏ถ As oil shows movement under these conditions, the cooling bath was replaced and repeat the
procedure for next temperature 3ยฐc or lower.
๏ถ The procedure was continued till no movement is observed
๏ถ The pour point was taken at 3o
c above the solid point.
7
RESULTS AND DISCUSSION
Table 1: Results showing pH, Density, Specific Gravity, Cloud and Pour Point of Crude Samples.
PARAMETER SAMPLE A SAMPLE B SAMPLE C SAMPLE D SAMPLE E SAMPLE F
pH 8.2 8.7 8.3 8.8 8.6 8.3
DENSITY
(kg/m3
)
850 790 830 900 810 880
SPECIFIC
GRAVITY
0.88 0.81 0.83 0.9 0.86 0.91
POUR
POINT(O
C)
1.4 6 17 11 8.5 8.7
CLOUD
POINT(O
C)
21 12 21 19 15 18
8
Table 2: Table of specific gravity and pour point
Specific gravity Pour point
0.88 14
0.81 6
0.83 17
0.9 11
0.86 8.5
0.91 8.7
Figure 2: Graph of specific gravity against pour point
0
5
10
15
20
0.8 0.82 0.84 0.86 0.88 0.9 0.92
Pour
point
Specific gravity
Specific Gravity against Pour point
9
Table 3: Table of specific gravity and cloud point
Specific gravity Cloud point
0.88 21
0.81 12
0.83 21
0.9 19
0.86 15
0.91 18
Figure 3: Graph of specific gravity against cloud point
0
5
10
15
20
25
0.8 0.82 0.84 0.86 0.88 0.9 0.92
Cloud
point
Specific gravity
Specific gravity against cloud point
10
DISCUSSION
Table 1 shows the results of the experiments carried out to determine pH, density, specific gravity, cloud
and pour point of the six (6) crude oil samples.
From the table, it can be noticed that the cloud points of crude samples A, C and D have temperature limit
that is higher than the least expected annual mean temperature (180
C) being that Nigeria has a tropical
climate with the exception of sample B which implies that wax deposition can be easily prevented in the
region. Also from the table, it is evident that the pour points of the samples are below ambient temperature
especially for onshore pipeline facilities in the Niger Delta region. A critical look at Table 1 shows that
sample C has the highest pour point while sample A has the lowest pour point signifying that sample C has
the highest paraffin content while sample A has the lowest paraffin content. Figure 2 shows that a linear
relationship exists between specific gravity and pour point of the crude samples. It is also shown in Figure
3 that a linear relationship exists between specific gravity and cloud point of the crude samples. This linear
trend for crude oils is reported by Modesty (Kelechukwu, 2011).
11
QUESTION 3
Assuming the minimum ambient temperature of the area where these samples were collected is 18ยฐC;
suggest three preventive measures against wax formation.
Mechanical method: Includes running scrappers in the borehole and pigging in pipelines at an intervention
frequency.
The chemical methods: Inhibitors include pour point depressants (PPD), crystal modifiers, dispersants and
solvents.
The thermal methods: Include heat retention, active heating such as thermal insulations, bottom hole
heaters, hot oil circulation and steam circulation
12
QUESTION 4
MODEL FOR CLOUD POINT
Y=41.29x โ€“ 18.049
At specific gravity = 0.7, 0.75, 0.8, 0.85, 0.9, 0.95
Cloud point; Y= 41.29(0.7) โ€“ 18.049 = 10.854
Y= 41.29(0.75) โ€“ 18.049 = 12.919
Y= 41.29(0.8) โ€“ 18.049 = 14.983
Y= 41.29(0.85) โ€“ 18.049 = 17.048
Y= 41.29(0.9) โ€“ 18.049 = 19.112
Y= 41.29(0.95) โ€“ 18.049 = 21.177
Figure 4: Graph of specific gravity against cloud point
0
5
10
15
20
25
0 0.2 0.4 0.6 0.8 1
Cloud
point
Specific gravity
Specific gravity against Cloud point
13
MODEL FOR POUR POINT
Y=21.4516x + 8.746
At specific gravity = 0.7, 0.75, 0.8, 0.85, 0.9, 0.95
Pour point; Y=21.4516(0.7) + 8.746 = 10.462
Y=21.4516(0.75) + 8.746 = 10.584
Y=21.4516(0.8) + 8.746 = 10.707
Y=21.4516(0.85) + 8.746 = 10.829
Y=21.4516(0.9) + 8.746 = 10.952
Y=21.4516(0.95) + 8.746 = 10.075
Figure 5: Graph of specific gravity against pour point
10
10.2
10.4
10.6
10.8
11
0.7 0.75 0.8 0.85 0.9 0.95 1
Pour
point
Specific gravity
Specific gravity against pour point
14
CONCLUSION AND RECOMMENDATIONS
Wax deposition has long been an issue in the oil and gas sector, and researchers have focused heavily on
how to determine and regulate it. The cloud and pour point, which has been the subject of this research, is
an important component in wax deposition because it determines when crude oil starts to crystallize into
wax and lose its flow properties. The researcher has noted that a few variables that affect cloud and pour
point temperatures can be controlled to reduce the likelihood of wax crystallization and deposition.
Therefore, in order to avoid wax deposition, midstream companies participating in the transportation of
crude oil should properly and efficiently handle these parameters.
The crude oil from the Nigerian Niger Delta can be easily managed, especially onshore under circumstances
that will help minimize wax deposition. After that, precautions such installing heaters along flow lines to
help maintain crude temperature above the fluid's cloud point should be taken. Additionally, the usage of
chemical solvents like Pour Point Depressants (PPDs) and wax inhibitors should be promoted. According
to (Bagdat and Masoud, 2015), the best way to prevent paraffin from depositing inside of pipes is to treat
them internally with Ethylene Tetra-Fluoro Ethylene (ETFE). Therefore, its use can be encouraged rather
of the rigid PVC pipes and steel pipes that are frequently used in the oil and gas sector for crude oil.
15
REFERENCES
Adewusi, V. A., (1997). Prediction of wax deposition potential of hydrocarbon systems for viscosity-
pressure correlations. Fuel 76:1079-1083.
Agrawal, K.M., Khan, H.U., Surianarayanan, M., Joshi, G.C., (1990).Wax Deposition of Bombay High
Crude Oil under Flowing Conditions, Fuel, 69, 794-796.
Ajienka, J.A., Ikoku, C.V., (1997). Waxy crude oil handling in Nigeria: practices, problems and prospects,
Energy sources. 12(4): 463-478.
Al-Besharah, J.M., Salman, O.A., and Akashah, S.A., (1987). Viscosity of crude oil blends. Industrial and
Engineering Chemistry Research, 26, 2445โ€“2449.
Bern, P.A., Withers, V.R., Cairns, J.R., (1980). Wax Deposition in Crude Oil Pipelines. 206-1980-MS,
European Offshore Petroleum Conference and Exhibition, London.
Burger, E.D., Perkins, T.K., Striegler, J.H., (1981). Studies of Wax Deposition in the Trans-Alaska Pipeline.
Journal of Petroleum Technology, 33, 1075-1086.
Elijah Taiwo, John Otolorin and Tinuade Afolabi (2012). Crude Oil Transportation: Nigerian Niger
DeltaWaxy Crude, Crude Oil Exploration in the World, Prof. Mohamed Younes (Ed.), ISBN: 978- 953-51-
0379-0, In Tech, Available from:http://www.intechopen.com/books /crude-oil-exploration-in-
the world/crude-oil-transportationnigerian niger-delta-waxy-crude-oil
Kelechukwu, E.M., (2011). Prediction of wax deposition risk of Malaysian crude from viscocity-
temperature correlation for dead crude. Int. J. Sci. Adv. Technol., 1: 89-100.

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ISLAMIYA EXPERIMENT 4.pdf

  • 1. i EXPERIMENT 4 OIL FIELD QUALITY CONTROL TEST CLOUD POINT AND POUR POINT DETERMINATION BY AMUSAT, ISLAMIA DASOLA 125/18/2/0152 IN PARTIAL FULFILMENT OF REQUIREMENTS FOR PETROLEUM ENGINEERING LAB III COURSE (PEE 513) 15TH OF DECEMBER, 2022.
  • 2. ii ABSTRACT In this experiment, the cloud and pour point of the Nigerian Niger Delta Crude oil were determined so as to ascertain the temperature at which wax crystallizes and precipitates during crude transportation. Six (6) crude samples were collected and analysed in the laboratory and the results showed that each of the samples had varying cloud points; Sample A -21o C, Sample B - 12 o C, Sample C - 21 o C, Sample D - 19 o C, Sample E -8.5o C and Sample F โ€“ 8.7 o C with a mean value of 17.6 o C. Same trend was also exhibited by the pour points; Sample A โ€“ 1.4 o C, Sample B - 6o C, Sample C - 17 o C, Sample D - 11o C , Sample E โ€“ 8.5 o C and Sample F โ€“ 8.7 o C with a mean value of 8.76 o C. It was then concluded that wax deposition during crude transportation in the region can be prevented especially in onshore pipelines if efficient preventive measures are put in place being that the region in the tropics with a minimum ambient temperature of 180C. Factors that affect cloud and pour point of crude oil were also highlighted and recommendations that will help prevent crude oil from wax crystallization and precipitations were given.
  • 3. iii TABLE OF CONTENTS TITLE PAGE i ABSTRACT ii TABLE OF CONTENTS iii LIST OF FIGURES iv LIST OF TABLES v INTRODUCTION 1 THEORY 3 AIM AND OBJECTIVES 4 MATERIALS AND APPARATUS 4 METHODOLOGY 6 RESULTS AND DISCUSSION 7 CONCLUSION AND RECOMMENDATIONS 14 REFERENCES 15
  • 4. iv LIST OF FIGURES Figure 1: Manual cloud point and pour point tester 5 Figure 2: Graph of specific gravity against pour point 8 Figure 3: Graph of specific gravity against cloud point 9 Figure 4: Graph of specific gravity against cloud point 12 Figure 5: Graph of specific gravity against pour point 13
  • 5. v LIST OF TABLES Table 1: Results showing pH, Density, Specific Gravity, Cloud and Pour Point of Crude Samples. 7 Table 2: Table of specific gravity and pour point 8 Table 3: Table of specific gravity and cloud point 9
  • 6. 1 INTRODUCTION Crude oil is a naturally occurring mixture, consisting predominantly of hydrocarbons, sulphur, nitrogen and metals. Crude oils are complex but mainly paraffinic, naphthenic and aromatic. Crude oils contain all normal alkenes from C1 to C120. However, this percentage rises to 35% in highly paraffinic and decreases to zero in highly bio graded oils. Nigeria has a substantial reserve of paraffinic crude oils known for their good quality (low sulphur, high API gravity), and containing moderate to high contents of paraffinic waxes. Waxy crude oils have undesirably high pour points and are difficult to handle where the flowing and ambient temperatures are about or less than the pour-point and high pour point oil reservoirs are usually part of the developed oilfields in various regions worldwide. Waxy crude oils also exhibit Bingham non- Newtonian flow behaviour below the cloud point due to wax crystallization. The Nigerian Niger Delta crude oil, which is the mainstay of Nigerian economy, exhibits waxiness, with deposits in the range of 30- 45 %. During its transportation, because oil temperature at initial station is higher than the ambient temperature, the oil temperature continues to decrease, and when it decreases to the wax precipitation point of crude oil, wax crystal in crude oil starts to precipitate, grow, and deposit on the pipe wall finally; sediments on pipeline will reduce the effective flow area of the pipeline, increase friction, and thus reduce transmission capacity of the pipeline. Also, production tubing had waxed up in several cases and this had resulted in the expensive maintenance procedure of wax cutting which involves using scrapers conveyed by wire line. Billions of dollars has been lost to its prevention and remediation. Wax deposition in crude oils has been a problem in crude transportation for a long time and the difficulties in pipeline transportation are due to this complex nature of crude oil, which cause a variety of difficulties during the production, separation, transportation and refining of oil. When a waxy crude oil is cooled, the heavier paraffinic constituents begin to separate as solid crystals once the solubility limit is exceeded. Thermodynamically, the solid-liquid phase boundary temperature, that is the maximum temperature at which the solid and liquid phases co-exist in equilibrium at a fixed pressure, is the wax appearance temperature (WAT). It is also known as the Cloud Point which depends on wax concentration, the crystallization habit of wax, and the shear stability of different wax structures. Crude oil starts to lose its flow characteristics when wax crystallization begins to occur. The lowest temperature at which the oil is mobile is termed Pour Point. Therefore, cloud points and pour points are of immerse importance of any liquid in fuel to prevent all the problems encountered in pipeline during crude transportation. Cloud point is the temperature at which the oil becomes cloudy and the first particles of wax crystals are observed as the oil is cooled and gradually under standard conditions. The cloud point of any liquid fuel is an indicator of how well the fuel will perform and indicates the tendency of the oil to plug under cold weather conditions. Cloud point can be measure both manually and automatically.
  • 7. 2 Pour point is the lowest temperature below which the fuel loses its flow characteristics. It is the opposite of cloud point as it is refers to the lowest temperature at which we can observe the movement of oil and also we can pump the fuel easily. Factors Affecting Cloud and Pour Points of Crude Oil There are certain factors that directly affect the cloud and our point of crude oil. Proper management of these parameters will help control the rate with which crude oil reaches its cloud and pour point. These parameters are discussed as follows; Temperature Differential: Wax deposit decreases with an increase in temperature difference. The drop in wax deposition rate with increase in temperature difference could be attributed to the extra heat gained or added in the solution, which would further move the solution away from its cloud point. Hence the process of crystal formation and their deposition is a function of temperature difference. Since wax deposition is directly affected by cloud and pour point, there exists a direct relationship between these temperature points and temperature differential between the waxy crude and pipeline wall. Paraffin Wax Content: The amount of paraffin wax in a crude oil sample affects its cloud and pour point temperatures. Wax deposition has a higher tendency to occur in crude oils with high paraffin wax content than those with lesser paraffin wax because wax can easily agglomerate when it is high in content than when it is not. As such, the amounts of paraffin wax present in a crude sample directly affect the rate at which it will reach its cloud and pour point. Flow rate: Higher flow shear, which is a function of flow rate, leads to lesser but likely harder wax deposit build up. Thus wax deposition gradually decreases with increase in flow rate and turbulence. The effect of increasing flow rate, decreasing the amount of wax deposited or entrapped oil in the deposited, This can be explained; that as the velocity of the moving stream increases, the molecules gain more energy with a corresponding increase in temperature which would reduce the tendency with which the waxy crude would reach its cloud and pour point. Surface Properties: Properties such as density, specific gravity and viscosity are determinants of the cloud and pour point of crude oil sample. There exists a relationship between density and specific gravity. Also, viscosity is affected by specific gravity because the denser a fluid, the more viscous it becomes. Since viscosity directly affects cloud and pour point, it is essential to state that the higher the density, specific gravity and viscosity of crude oil sample, the more its tendency towards reaching its cloud and pour point.
  • 8. 3 THEORY Due to flow assurance problems encountered during crude transportation using pipelines in the oil and gas industry, it has become of paramount importance to study the different factors that enhance wax deposition in pipelines. Several researchers have done work on the subject matter and have been able to predict using scientific methods conditions that promote wax deposition while also professing ways to combat its undesirable occurrence. Amongst the numerous researches done, some are discussed here. It was stated that the main components of the heavy fraction of hydrocarbon which participate in the solid phase formation include asphaltenes, diamondoids, petroleum resins and wax. Petroleum wax consist mainly saturated paraffin hydrocarbons with number of carbon atoms in the range of 18-36. Wax may also contain small amounts of naphthenic hydrocarbons with their number of carbon atoms in the range of 30-60. Wax usually exists in intermediate crudes, heavy oils, tar sands and oil shales. There are three main factors that affect wax deposition in flow systems are flow rate, temperature deferential, and cooling rate, as well as surface properties. The mechanism of wax deposition could be summarized as the following four types: molecular diffusion, shear dispersion, Brownian diffusion and gravity settling, in which molecular diffusion was generally considered as the most important mechanism causing wax deposition. Shear dispersion, Brownian diffusion and gravity settling had little influence on wax deposition, namely molecular diffusion was dominant mechanism of wax deposition. Shear dispersion also had an influence on wax deposition, but the main cause was still molecular diffusion, the process of wax deposition could be described by the following steps: ๏ถ Gelation of the waxy oil on the cold surface ๏ถ Diffusion of waxes towards the gel layer from the bulk ๏ถ Internal diffusion of these molecules through the trapped oil ๏ถ Precipitation of these molecules in the deposit ๏ถ Counter diffusion of de-waxed oil out of the gel layer. This proposition was confirmed by measuring the carbon number distribution in the sample of wax deposition layer under different experimental time.
  • 9. 4 AIM AND OBJECTIVES The aim of this experiment is to determine the cloud and point of crude oil samples obtained from the Niger Delta region of Nigeria and, to make some analytical predictions and recommendations base on the results. The specific objectives are listed below; ๏ถ To determine the temperature at which the sampled crude oil becomes semi solid and loses their flow characteristics. ๏ถ To compare the cloud and pour point of the different crude samples. ๏ถ To make recommendations as to how wax deposition can be prevented during crude transportation Materials and Apparatus Material Crude samples with a known pH, density and specific gravity. Apparatus Cloud point and Pour point tester with the following components parts; ๏ถ Test jar ๏ถ Cork carrying thermometer ๏ถ Jacket ๏ถ Gasket ๏ถ Disc ๏ถ Cooling bath containing salt and crushed ice.
  • 10. 5 Figure 1: Manual cloud point and pour point tester
  • 11. 6 METHODOLOGY The initial temperature, pH and specific gravity of the crude oil samples were determined before commencing the experiment. Procedure for Cloud point Determination. ๏ถ A suitable freezing mixture of salt and crushed ice in cooling bath was prepared. ๏ถ The oil was poured into the test jar up to the etched mark. ๏ถ At each test thermometer reading i.e. the multiple of 1c, inspect for cloud. ๏ถ Reading which reveals the distinct cloud or haze in the oil at the bottom of jar is the cloud point. Procedure for Pour Point Determination. ๏ถ The oil was continue to cool further ๏ถ As soon as the oil in the jar doesnโ€™t flow when the jar is titled, the test tube was hold horizontally for 5 seconds and observe it carefully ๏ถ As oil shows movement under these conditions, the cooling bath was replaced and repeat the procedure for next temperature 3ยฐc or lower. ๏ถ The procedure was continued till no movement is observed ๏ถ The pour point was taken at 3o c above the solid point.
  • 12. 7 RESULTS AND DISCUSSION Table 1: Results showing pH, Density, Specific Gravity, Cloud and Pour Point of Crude Samples. PARAMETER SAMPLE A SAMPLE B SAMPLE C SAMPLE D SAMPLE E SAMPLE F pH 8.2 8.7 8.3 8.8 8.6 8.3 DENSITY (kg/m3 ) 850 790 830 900 810 880 SPECIFIC GRAVITY 0.88 0.81 0.83 0.9 0.86 0.91 POUR POINT(O C) 1.4 6 17 11 8.5 8.7 CLOUD POINT(O C) 21 12 21 19 15 18
  • 13. 8 Table 2: Table of specific gravity and pour point Specific gravity Pour point 0.88 14 0.81 6 0.83 17 0.9 11 0.86 8.5 0.91 8.7 Figure 2: Graph of specific gravity against pour point 0 5 10 15 20 0.8 0.82 0.84 0.86 0.88 0.9 0.92 Pour point Specific gravity Specific Gravity against Pour point
  • 14. 9 Table 3: Table of specific gravity and cloud point Specific gravity Cloud point 0.88 21 0.81 12 0.83 21 0.9 19 0.86 15 0.91 18 Figure 3: Graph of specific gravity against cloud point 0 5 10 15 20 25 0.8 0.82 0.84 0.86 0.88 0.9 0.92 Cloud point Specific gravity Specific gravity against cloud point
  • 15. 10 DISCUSSION Table 1 shows the results of the experiments carried out to determine pH, density, specific gravity, cloud and pour point of the six (6) crude oil samples. From the table, it can be noticed that the cloud points of crude samples A, C and D have temperature limit that is higher than the least expected annual mean temperature (180 C) being that Nigeria has a tropical climate with the exception of sample B which implies that wax deposition can be easily prevented in the region. Also from the table, it is evident that the pour points of the samples are below ambient temperature especially for onshore pipeline facilities in the Niger Delta region. A critical look at Table 1 shows that sample C has the highest pour point while sample A has the lowest pour point signifying that sample C has the highest paraffin content while sample A has the lowest paraffin content. Figure 2 shows that a linear relationship exists between specific gravity and pour point of the crude samples. It is also shown in Figure 3 that a linear relationship exists between specific gravity and cloud point of the crude samples. This linear trend for crude oils is reported by Modesty (Kelechukwu, 2011).
  • 16. 11 QUESTION 3 Assuming the minimum ambient temperature of the area where these samples were collected is 18ยฐC; suggest three preventive measures against wax formation. Mechanical method: Includes running scrappers in the borehole and pigging in pipelines at an intervention frequency. The chemical methods: Inhibitors include pour point depressants (PPD), crystal modifiers, dispersants and solvents. The thermal methods: Include heat retention, active heating such as thermal insulations, bottom hole heaters, hot oil circulation and steam circulation
  • 17. 12 QUESTION 4 MODEL FOR CLOUD POINT Y=41.29x โ€“ 18.049 At specific gravity = 0.7, 0.75, 0.8, 0.85, 0.9, 0.95 Cloud point; Y= 41.29(0.7) โ€“ 18.049 = 10.854 Y= 41.29(0.75) โ€“ 18.049 = 12.919 Y= 41.29(0.8) โ€“ 18.049 = 14.983 Y= 41.29(0.85) โ€“ 18.049 = 17.048 Y= 41.29(0.9) โ€“ 18.049 = 19.112 Y= 41.29(0.95) โ€“ 18.049 = 21.177 Figure 4: Graph of specific gravity against cloud point 0 5 10 15 20 25 0 0.2 0.4 0.6 0.8 1 Cloud point Specific gravity Specific gravity against Cloud point
  • 18. 13 MODEL FOR POUR POINT Y=21.4516x + 8.746 At specific gravity = 0.7, 0.75, 0.8, 0.85, 0.9, 0.95 Pour point; Y=21.4516(0.7) + 8.746 = 10.462 Y=21.4516(0.75) + 8.746 = 10.584 Y=21.4516(0.8) + 8.746 = 10.707 Y=21.4516(0.85) + 8.746 = 10.829 Y=21.4516(0.9) + 8.746 = 10.952 Y=21.4516(0.95) + 8.746 = 10.075 Figure 5: Graph of specific gravity against pour point 10 10.2 10.4 10.6 10.8 11 0.7 0.75 0.8 0.85 0.9 0.95 1 Pour point Specific gravity Specific gravity against pour point
  • 19. 14 CONCLUSION AND RECOMMENDATIONS Wax deposition has long been an issue in the oil and gas sector, and researchers have focused heavily on how to determine and regulate it. The cloud and pour point, which has been the subject of this research, is an important component in wax deposition because it determines when crude oil starts to crystallize into wax and lose its flow properties. The researcher has noted that a few variables that affect cloud and pour point temperatures can be controlled to reduce the likelihood of wax crystallization and deposition. Therefore, in order to avoid wax deposition, midstream companies participating in the transportation of crude oil should properly and efficiently handle these parameters. The crude oil from the Nigerian Niger Delta can be easily managed, especially onshore under circumstances that will help minimize wax deposition. After that, precautions such installing heaters along flow lines to help maintain crude temperature above the fluid's cloud point should be taken. Additionally, the usage of chemical solvents like Pour Point Depressants (PPDs) and wax inhibitors should be promoted. According to (Bagdat and Masoud, 2015), the best way to prevent paraffin from depositing inside of pipes is to treat them internally with Ethylene Tetra-Fluoro Ethylene (ETFE). Therefore, its use can be encouraged rather of the rigid PVC pipes and steel pipes that are frequently used in the oil and gas sector for crude oil.
  • 20. 15 REFERENCES Adewusi, V. A., (1997). Prediction of wax deposition potential of hydrocarbon systems for viscosity- pressure correlations. Fuel 76:1079-1083. Agrawal, K.M., Khan, H.U., Surianarayanan, M., Joshi, G.C., (1990).Wax Deposition of Bombay High Crude Oil under Flowing Conditions, Fuel, 69, 794-796. Ajienka, J.A., Ikoku, C.V., (1997). Waxy crude oil handling in Nigeria: practices, problems and prospects, Energy sources. 12(4): 463-478. Al-Besharah, J.M., Salman, O.A., and Akashah, S.A., (1987). Viscosity of crude oil blends. Industrial and Engineering Chemistry Research, 26, 2445โ€“2449. Bern, P.A., Withers, V.R., Cairns, J.R., (1980). Wax Deposition in Crude Oil Pipelines. 206-1980-MS, European Offshore Petroleum Conference and Exhibition, London. Burger, E.D., Perkins, T.K., Striegler, J.H., (1981). Studies of Wax Deposition in the Trans-Alaska Pipeline. Journal of Petroleum Technology, 33, 1075-1086. Elijah Taiwo, John Otolorin and Tinuade Afolabi (2012). Crude Oil Transportation: Nigerian Niger DeltaWaxy Crude, Crude Oil Exploration in the World, Prof. Mohamed Younes (Ed.), ISBN: 978- 953-51- 0379-0, In Tech, Available from:http://www.intechopen.com/books /crude-oil-exploration-in- the world/crude-oil-transportationnigerian niger-delta-waxy-crude-oil Kelechukwu, E.M., (2011). Prediction of wax deposition risk of Malaysian crude from viscocity- temperature correlation for dead crude. Int. J. Sci. Adv. Technol., 1: 89-100.