Treatmentof Waxy Oil 3

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Treatment of Waxy Oil 3
Technical Report · December 2014

DOI: 10.13140/RG.2.2.28906.72642/1
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Shivanie Mahabir Dhurjati Prasad Chakrabarti

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Treatment of Waxy Oil 3
Shivanie Mahabir*, Dhurjati Prasad Chakrabarti*
*Department of Chemical Engineering, The University of The West Indies, St. Augustine,
Trinidad and Tobago
ABSTRACT
In oil companies around the world today wax and asphaltene deposition from crude oil has proven
to be a costly problem. The objective of this study is to understand the characteristics of both wax
and asphaltene in order to test the effectiveness of solvents in the inhibition of the crystallization
and subsequent precipitation of the wax/asphaltene. Also to test the flow characteristics and its
viscosities as the concentration of the solvent being used is increased. The crude oil samples were
attained from the Southwestern Sallado oil reserve from Petrotrin-Trinmar operations at Pt. Fortin.
The solvents were tested at different concentrations in weight percentages at a temperature of 70oC
and this resulted is the PAO-100 solvent being the most suitable for sample 1(S-600) and P-103
for samples 2(S-713) and 3(S-714). The viscosity for sample 3 (S-714) was found to have a high
flow characteristic followed by samples 1 (S-600) and then 2 (S-713).
Key words: offshore, oil pipeline, kinematic viscosity, pour point, freezing point, wax
deposition.
1
AIM & OBJECTIVE
Aim: To alleviate the wax and asphaltene deposition in crude oil pipelines at Petrotrin-Trinmar
Operations.
Objective: To determine the flow characteristics of the three samples of crude oil (provided by
Petrotrin) given its varying viscosities.
INTRODUCTION
The everyday use of gasoline and diesel fuel in vehicles today would not be possible without
refining a large number of barrels per day of crude oil. The retrieval of crude oil (petroleum) is
important for creating transport fuel as well as many other products such as petroleum jelly, ice
cube trays, telephones, sun glasses, movie film and candles. This can be found deep beneath the
earth’s surface by using oil rigs both on land and in the sea to retrieve the crude oil, however there
are many problems that may be associated with gaining these barrels of crude oil per day.
In the field, the oil pipelines are often plugged by paraffin wax and asphaltene that deposits on its
walls in the production tubing, flow lines at the surface and even in the tank farms. This deposit
leads to a fall in the production rates of the oil from that well. Formation of wax/asphaltene
crystallization and deposit are dependent upon factors such as temperature, pressure, the flowing
conditions at the wellbore and the composition of the reservoir crude oil, (Towler.et.al. 2011).
Temperatures at 2000m below sea level are often about 5oC,(Brill 1998), as a result oil being
produced in deep water environments undergo rapid temperature reduction. Thus as the oil
temperature near the pipe wall cools below the cloud point or wax appearance temperature
deposition of wax/asphaltene on the inner walls occurs.
2
LITERATURE REVIEW
Trinidad and Tobago is now the leading Caribbean producer of oil and gas since the
commission of the first oil well drilling, in 1857, the petroleum industry has flourished for over
one hundred years. Trinidad and Tobago's state-owned Petrotrin refinery is the only refinery
in the country. This oil and gas company, operates two major crude and petroleum products
storage terminals with a total storage capacity of 7.7 million barrels, namely the Pointe-a-Pierre
terminal and the Point Fortin terminal, ((EIA) 2013). The products from the processed crude
oil are sold locally and to customers across the Caribbean, Latin America and the eastern
seaboard of the United States of America.
Crude oil is a mixture of many different hydrocarbons and small amounts of impurities, ((EPA)
1995). This non-renewable resource was developed from the entrapping of dead plants and
animals in the sea millions of years ago under a layer of mud which eventually formed rocks.
The pressure and heat together with no air or oxygen present, turned the remains into crude
oil. It is therefore found deep beneath the earth’s surface and can only be attained by oil
companies that can drill through the impermeable rocks to retrieve it. Refer to figure 1 below
for a diagram of the layers that has to be accessed to get to the crude oil.
Figure 1: Diagram showing the layers that has to be accessed by the oil rig,(BBC 2007).
3
In addition to drilling for crude oil the petroleum industry faces many challenges and one such
problem is the buildup of wax and asphaltene in pipe lines both at subsea levels and on land. The
precipitation, deposition and gelling of wax/paraffins are common process chemistry challenges
associated with upstream exploration and production. Furthermore, this literature survey would be
mainly based on the solutions used by Petrotrin to mitigate these arterial blockages throughout
their pipe lines. The methods are paraffin solvents, cold-finger test and the cloud-point test. These
tests are discussed in details further down in the survey but they are mainly used for screening
purposes and the solvents are used to eliminate the wax and asphaltene build up.
Parraffins, also referred to as alkanes, are the combination of one carbon and two hydrogen (CH2
groups) in succession to form straight chain paraffins. Wax is the product of paraffin deposit and
has a structure that contains more than 16carbon atoms in the paraffin series (C16-C40). Paraffins
can exist in crude oil in all three states. At standard room temperature, paraffins generally exists
in a solid form and solidify to form deposits. Therefore, "paraffin wax deposition" refers to the
solid form of paraffins that solidify to cause deposition, (Makowsky.et.al. 2010).
Asphaltene is the material present in petroleum that is insoluble in n-paraffins but soluble in
aromatic solvents such as n-heptane. At atmospheric temperature, asphaltenes in solution are
found in a solid phase. They are mostly found with paraffin wax when they are retrieved from
wells, storage tanks, or pipelines. Studies show that the amount of asphaltene precipitation
decreases as the number of carbons forming straight chain paraffins increases,(Makowsky.et.al.
2010). Therefore, the treatment of paraffin and asphaltene deposition must both be considered
together since the treatment of paraffin wax could worsen the precipitation of heavier, problematic
asphaltene compound.
The transportation of heavy crude from its production location to the refinery can require a
substantial network of pipelines (Shirley et al., 2012; Chakrabarti et al., 2011). These pipeline
networks become even more important when it comes to the success of newly developing
undersea, off shore energy projects. The pressure gradient from the subsea to pipe located on the
shore would require different amount of chemicals at different sites as well as the equipment and
storage tank farms has to be monitored for wax and asphaltene build up. Thus, the paraffin wax
and asphaltene deposition in the inner surface of the pipeline has the ability to cause severe, if not
hazardous, problems if left untreated. The formation of paraffin wax reduces flow diameter (refer
4
to figure 2), decreases overall throughput, and results in a higher pressure drop when crude is
pumped through the pipeline.
Figure 2: Pipe which has undergone a fouling process and restricts flow,(Makowsky.et.al.
2010).
The precipitation and hence the clogging of oil reservoirs, well bores and transportation pipelines
by these alkanes can be provoked by the three steps shown below:
1. Solubility/Precipitation
The drilling into a new oil reservoir can cause a pressure gradient since it would have been stored
under impermeable rocks and sands (cruse, forest) which makes up the properties of the crude oil
and hence held high pressure. The perforating of the reservoir would then allow oil to flow out
causing a decrease in pressure and temperature. This temperature reduction allows for the
precipitate of paraffin to be created and carried through the upstream oil flow.
2. Transportation and deposition of precipitate
The formation of the paraffin wax in the crude oil from the change in temperature and pressure
begins to create networks while travelling up the pipes and traps oil molecules. This combination
5
of wax and oil creates a gel matrix which in turns ends up trapping other wax crystals that are
present. Overtime the growth in the amount of wax builds up in the inner walls of the pipes. The
walls of the pipes located lower beneath the earth’s crust experiences a decrease in temperature
where the gel-like substance hardens and deposits. Refer to figure 3 below for the formation on
the tubing of the walls as the temperature of the produced fluid decreases.
Figure 3: Paraffin crystals being form on tubing walls as the temperature decreases,
(HALLIBURTON 2005).
3. Reduction in permeability due to precipitate deposition
The harden gel deposits and suspended wax crystals on the surface of the pipes limits the area
available for flow whereby it decreases the flow rate. This rough surface on the inner pipe walls
also continues to encourage the deposition and buildup of paraffin wax, refer to figure 4 below for
the diagram. This would in turn greatly affect the revenue of the oil company by having a decrease
in the amount of oil produced and/or transported.
6
Figure 4: Rough surface provides an ideal surface for paraffin deposits,(HALLIBURTON
2005).
Furthermore, there are measurements that can be conducted in order to give a general
understanding of the temperature at which wax deposition and crude oil gelling will become a
problem. The wax properties of oils have been characterized by cloud point and pour point
measurements. The cloud point is the measurement of the first visible wax formation or cloudy
appearance as the solution of oil is being cooled at atmospheric pressure. Cloud point is also
referred to as Wax Appearance Temperature (WAT). The pour point is the lowest temperature at
which the fuel continues to flow and beyond this temperature, the fuel stops flowing and starts to
freeze.
There are three main categories that wax deposition can be controlled or managed and these are
mentioned below:
1. Mechanical
The most common method of wax control is flow line pigging which can be soluble pigs that may
be made of naphthalene or microcrystalline wax and insoluble pigs are made of plastic or hard
rubber. Refer to figure 5 below for the different types pigs used to clean the pipelines. This is used
to scrape the inner pipe walls of the gel-like substance so as to prevent further buildup of wax.
7
Figure 5: Types of pigs used in pipelines, (Glendasmith 2013).
There are a few disadvantages to pigging that do not make it a viable solution to all pipeline
deposition control applications. Since the pig must be inserted and removed from the pipeline
manually, production is often interrupted even if it is for a short time. Human contact with the pig
is considered to be dangerous to some degree. As pigging is the removal of already formed
deposits, it does little to actually solve the problem of paraffin and asphaltene deposition.
There are other mechanical methods used to remediate the problem which are by using wire line
tools such as casting scrapers and gauge cutters that are used extensively to remove wax deposits
from tubing. If it becomes suck the use of gas oil, kerosene or diesel is used to soften the wax to
allow further scrapping to occur. This is only suitable for cleaning flow lines that are not
completely plugged. Scrapers also known as paraffin scrappers may be attached to wire line units,
or they may be attached to sucker rods to remove wax as the well is pumped.
2. Thermal Insulation
The use of thermal insulation to keep the fluid above the cloud point for the whole transport
through the flow line. However, once it is sent to storage the conditions, such as temperature,
would favour the formation of wax crystals and gels,(Bai.et.al 2005). Some prevention methods
along with thermal insulation include steam and electrical-heat tracing of flow lines. Another way
8
of remediating wax deposition include hot oiling and watering since wax precipitation is highly
temperature dependent.
Hot oil is normally pumped down the casing and up the tubing to melt and dissolve the wax. Higher
molecular-weight waxes tend to deposit at the high-temperature bottom end of the well. Lower
molecular-weight fractions deposit as the temperature decreases up the wellbore. The upper parts
of the well receive the most heat during hot oiling. As the oil proceeds down the well, its
temperature decreases and the carrying capacity for wax is diminished. Thus, sufficient oil must
be used to dissolve and melt the wax at the necessary depths. Hot water treatments cannot provide
the solvency effects that hot oiling can, so surfactants are often added to aid in dispersion of wax
in the water phase. This method has some disadvantages such as the method could only work well
for short flow lines and the hot oil treatments in wax-restricted wells can aggravate the problem in
the long run,(PetroWiki 2014).
3. Inhibitor injection
Chemical inhibitors can prevent wax deposition or gelling in pipelines. They can lower the WAT
or pour point or they can modify the wax crystals so as to prevent their agglomeration and
deposition,(Aiyejina.et.al. 2011). Some types of chemical inhibitors available for paraffin
prevention include:
Dispersants are a type of surfactants that helps disperse the wax crystals into the produced oil or
water. This dispersing of the wax crystals helps prevents deposition of the wax and also has a
positive effect on the viscosity and gel strength. Dispersants generally have a very low pour point
making their use suitable for cold climates. These chemicals are used in low concentrations and
can be formulated in both aqueous and hydrocarbon solutions, making them relatively safe and
inexpensive. Surfactants are a general class of chemicals that are most often used to clean vessels,
tanks, pipes, machinery or any place where wax may deposit. Surfactants or dispersants can also
be used in combination with hot oil and water treatments,(PetroWiki 2014).
Wax crystal modifiers act at the molecular level to reduce the tendency of wax molecules to
network and form lattice structures within the oil. These are chemically functionalized substances
that range from ploy-acrylate esters of fatty alcohol to copolymers of ethylene and vinyl
acetate,(Bai.et.al 2005). When the modifiers are used continuously it prevents wax deposition,
9
reduce oil viscosity and lower the wax gel strength. Concentrations of parts per million are
effective since they work at the molecular level. Wax crystal modifiers have a high-molecular-
weight and as a result they have high pour points, so their use can be limited in cold
climates,(PetroWiki 2014).
Solvent treatments can be used to treat deposition in production strings and also may be applied to
remediate formation damage. Hydrocarbon fluids consisting primarily of normal alkanes such as
condensate and diesel oil can be used, provided the deposits have low asphaltene content. Aromatic
solvents such as toluene and xylene are good solvents for both waxes and asphaltenes. This method
maybe costly and if the solvents are not removed after saturation is reached then the waxes will
precipitate and cause a more severe situation,(Bai.et.al 2005).
Crude oils with unstable asphaltene can cause problems in the operational system when blending
or high heat is being added downstream. The stability is a function of the ratio of asphaltenes to
stabilizing factors in the crude oil such as aromatics and resins. Pressure is however the biggest
impact has on the stability of asphaltene. Therefore, as the pressure of the well decreases and the
volume fraction of aliphatic components increases and it becomes unstable. Figure 6 below shows
that on the left hand side of the curve the asphaltenes are not stable whereas, on the right hand side
it is stable,(Bai.et.al 2005). Asphaltene deposition mostly occurs in the inner pipeline as the fluid
passes through the bubble point and this can then be mitigated by the use of inhibitors.
Figure 6: Asphaltene stability vs. pressure, (Bai.et.al, 2005).
10
There are various testing methods for screen and generating solutions for wax problems in pipeline
which are described below:
1. Cloud point Testing
The cloud point is the temperature of a liquid specimen when the smallest observable cluster of
hydrocarbon crystals first occurs upon cooling under prescribed conditions. The liquid is made
perfectly clear by using dry lint less filter paper and after pouring into test tube the cork and
thermometer is attached. The thermometer however, is to be resting on the bottom of the tube. It
is then placed in a cooling bath which is maintained at 1.5oC and the tube is inspected every 1oC
drop for a cloud suspension. If the cloud point is not observed at a temperature of 9oC then the
bath should be cooled even further. When observation of the cloud at the bottom of the tube is first
seen this temperature is recorded as its cloud point, refer to figure 7 below. Further cooling is
continued to confirm cloud point. This aids in determining the temperature that the crude oil should
stay above.
Figure 7: Before and after pictures of cloudy appearance been seen,(Aris 2014).
11
2. Pour-point Testing
Figure 8: Pour-point testing,(Becker 1997).

Figure 8 above shows one of the earliest method used for testing predictions of the wax deposition
rate on the surface of pipes. This method uses the heating of a sample of crude oil in a 50ml Pyrex
tube to a temperature of 160F for 30mintues,(Becker 1997). This ensures that the wax melts and
the thermometer and cork is secured as shown in the diagram. The sample is then allowed to cool
at room temperature but it is turned on its side and held at an angle of 90o then to an upright position
for 5 seconds to observe the fluid movement. This procedure is repeated for every 5F drop in
temperature until the variation is relatively constant or until the sample no longer flows. At this
temperature the pour-point is determined. This method does not give any properties of the wax
however, it creates a reliable screening for crystal modifiers chemicals.
3. Rolled-ball deposit Test/Wax solvency testing
Rolled-ball deposit test is a method used for screening chemicals by using the paraffin wax
deposits (e.g. tubing or transfer line) into 3-4g ball. The ball is placed in a container of water,
solvent or a mixture of water and solvent where it is observed. The samples are also subjected to
agitation, the contents are doubled and one set is heated while further observations takes place.
This test also determines the effectiveness of various solvents and surfactants as deposit removal
aids,(Becker 1997).
12
The lab in Santa Flora, Trinidad by Petrotrin-Trinmar operations firstly gathers both solid and
liquid samples of the crude oil or deposits to be tested. According to Diaz the liquid samples starts
with the SARA analysis this stands for the soluble aromatic, resins and asphaltene which is used
to determine the percentage of wax, asphaltene and resins there are in the crude oil sample. This
procedure also provides formulas that can calculate the percentage of each substance in the sample
and thus it will be able to validate the formation of wax/asphaltene in a particular well. This is
important because the crude oil can come from any of the 12 wells located in the Southwestern
Sallado in which he works,(Diaz 2014).
This is critical because the variation in material for example the cruse sand which is made up the
upper, lower and middle sections, gives the crude oil properties. Even though all the wells have a
possibility to develop wax/asphaltene the crude oil samples from each well would have to be
treated differently. Also by monitoring flow line pressures they are able to detect when there is a
blockage in the line caused by wax/asphaltene. For example the pressure of a pipe line at a certain
depth should be constant and if the pressure gradually increases over time then it can surely be
caused by wax/asphaltene blockages.
This would in turn result in the restriction of flow and thus a loss of production time and revenue.
The methods that they use are cloud point, solvents, paraffin dispersants and wax crystal modifiers.
The cloud point is used to determine the point at which the first visible cloud or wax formation is
seen. The pour point is for very low temperature regions therefore, it is rarely used because in the
Caribbean the temperatures below the earth’s crust is moderately cooled.
An example of the other solution methods are of the shore line pipes that would experience
deposition of wax/asphaltene. This occurs, due to the temperature and pressure gradients
experienced when compared to subsea pipelines. The use of a paraffin dispersant like a viscosity
reducer to allow the crude oil to flow easier through the lines. The reducers split oil molecules by
attaching to the water-seeking side and the other to the oil-seeking side which weakens the bond
and therefore separates them.
However, the dispersants along with the wax is then sent to the tank farms and equipment within
the industry. This wax/asphaltene would then form emulsion contents within the storage tanks if
they are not equipped to deal with the issues. Also damage to the progressive cavity pump by
having a formation on the rods would result in a hazardous situation that will eventually lead to
13
the placement of a new pump and a cost factor. Whereas, the solvents and wax crystal modifiers
would make changes at a molecular level and to the crystals it’s self in order to clear the
wax/asphaltene build up. They also injects wax crystal modifiers into the oil reservoir to prevent
the buildup in the inner walls of the pipelines. These treatments, once there is a budget for the
costly chemicals, takes place when there is an obstruction in flow or once a year.
METHODOLOGY
7.1 Wax Solvency Testing
Apparatus: -
 8 conical flasks (125ml),

 Fumehood
 Heating bath (80oC)
 Analytical balance
Materials: -
 Wax deposits (from S-138 and Barrack pore #592)

 Wax solvents PS-1000, P-103, PA0-100 (Obtained directly from Petrotrin chemical
companies) and P-Xylene.
 Distilled water
Procedure for Wax Solvency testing:-
1) Five conical flasks were each filled with 100mls of distilled water and 1gram of wax from
S-138 was added to each flask labeled A, B, C, D and E.
2) Chemicals PS-1000, P-103, PA0-100 and P-Xylene was added to the first 4 flasks at 5ml
each, note the 5th flask, E, represented the well without any chemical treatment.
3) The flasks were then placed into a water bath at 80oC where it was ensured that the water
bath level covers the level of the water in the flask at all times for roughly 3 hours.
4) At this temperature the wax was melted and it was in a flow able state.
5) The flasks were then individually removed from the bath and was agitated by shaking the
flasks until it cools, this represented the crude travelling up the tubing string to surface.
14
6) The flask(s) that kept the wax dispersed the finest as well as the one that had little or no
wax agglomerating to the inside of the flask was the best performing product.
7) This procedure was repeated but instead using the wax deposit from Barrackpore #592.
8) Steps 1 to 8 was repeated by using P-Xylene instead of distilled water and only three
chemicals were used where flask D contained P-Xylene only.
Figure 9: Pictures showing the set up for this wax ball deposit experiment containing
distilled water and P-Xylene.
Another test was performed based on the solvency tests performed by Petrotrin’s lab in Santa
Flora:
1) 50ml of the solvents PS-1000, P-103, PA0-100 was measured and poured into three
respective beakers.
2) 1.20g of wax deposit from well S-138 was weighted and placed into beakers.
3) Each flask with the solvent and wax deposit was then placed into a water bath at 45oC (at
this temperature all the wax should melt as well as this simulated temperature represented
the pipe being heated) and left for roughly 2 hours.
4) The wax ball deposits were then removed and weighted.
5) Steps 1 to 5 was repeated for the wax deposit sample from Barrackpore #592.
15
Figure 10: Picture showing the set up for the wax ball solvency test.
7.2 Cloud points testing of the crude oil samples
Apparatus: -
 2 beakers (100ml)
 1 measuring cylinder (100ml)
 2 thermometers (260oC to -10oC)
 2 retort stands
 2 Stop watches
 Fumehood
Materials: -
 Crude oil samples (S-600, S-713 and S-714)

 100 ml 99%P-Xylene
companies).
 Ice
Procedure to determine the cloud points of the crude oil sample: -

1) A sample of crude oil from Petrotrin’s oil well S-600 was attained and 50ml was measured
using a measuring cylinder then poured into a beaker. (5ml was added to compensate for the
loss of crude oil sample when transferring)
2) The beaker was placed in the heating bath at 70oC. (+2oC was added to compensate for the
loss of heat when transferring).
16
3) The sample was allowed to heat until a temperature of 72oC, where it was then transferred
to a cooling tub that contained ice and water.
4) When being removed from the water bath the stop watch was simultaneously started and the
time taken for every 5oC temperature drop was recorded until a constant temperature was
reached.
5) The results were then used to plot a cooling curve from which the cloud point of the sample
was obtained.
6) Step 1 was repeated using another sample of crude oil but with the addition of 5wt% of P-
Xylene to the beaker.
7) Then steps 2 to 5 were repeated where another cooling curve was plotted and cloud point
was determined from the turning point on the curve.
8) Steps 6 and 7 were repeated using 10wt% and 12wt% of P-Xylene.
9) Then steps 1 to 8 were repeated using crude oil samples S-713 and S-714, which was
provided by Petrotrin.
Figure 11: Picture showing the set up for the cloud point testing.
17
7.3 Pour point of the crude oil sample
Apparatus: -
 2 beakers (100ml)
 1 measuring cylinder (100ml)
 2 thermometers (260oC to -10oC)
 2 retort stands
 2 Stop watches
 Refrigerator
Materials: -

 100 ml 99%P-Xylene
companies).
 Ice
Procedure to determine the pour point of the crude oil sample: -

1) The cloud point test procedure was repeated and when a temperature of 20oC was reached
the sample was placed in the refrigerator.
2) Every 10 to 15minutes the sample was tilted at a 90o angle for 5 seconds to observe the fluid
movements.
3) The sample was then replaced back into the freezer until it was observed that the sample
stopped moving and at this instance the temperature was recorded as its pour point
temperature.
4) These pour point test therefore entailed the same wax solvents and weight percentages as in
the cloud point test.
18
Figure 12: Pictures showing the pour point test.
7.4 Testing for viscosity

Apparatus: -
 Stop watch
 5 Beakers (200ml)
 2 Measuring cylinders (25ml and 100ml)
 1 Retort Stand
 Analytical balance
Materials: -

 150ml 99% P-Xylene
 Wax solvent PS-1000, P-103, PA0-100 (Obtained directly from Petrotrin chemical
companies).
Procedure to determine the viscosity using heating:-
1) The empty beakers labeled A to E was firstly weighed using an analytical balance and its
results recorded.
19
2) A sample of crude oil from Petrotrin’s oil well S-600 was attained and 50ml was measured
using a measuring cylinder then poured into a beaker. (5ml was added to compensate for the
loss of crude oil sample when transferring). This was unknown as sample E, then the beaker
and sample was weighed and recorded.
3) The beaker was placed in the heating bath at 70oC. (+2oC was added to compensate for the
loss of heat when transferring).
4) The sample was allowed to heat until a temperature of 72oC, where 10ml was then measured
and poured into a beaker.
5) The beaker was then held at a 45o angle where the stop clock was simultaneously started
when the crude oil sample had begun to fall.
6) The clock was stopped when the drops ceased to fall and the time was recorded.
7) Steps 1 to 6 was repeated using another sample of crude oil but with the addition of 5wt%
of P-Xylene into beaker D.
8) Step 7 was repeated using 10wt% and 12wt% of P-Xylene.
9) Then steps 1 to 8 were repeated using the other wax solvents PS-1000, P-103, PA0-100 at
weight percentages 5wt%, 10wt% and 12wt%.
10) Then steps 1 to 9 were then repeated using crude oil samples S-713 and S-714, which was
provided by Petrotrin.
20
RESULTS
The wax solvency test results, refer to appendix tables 3 to 6, showed that solvent PAO-100 was the most appropriate chemical to use
for a solid sample of wax in these specified wells.
The results for the cloud point test is shown below and the pour point for all the samples were found to be -9oC.
Table 1: Cloud point of each sample when mixed with different concentrations of the respective solvents.
Sample 1 (S-600)
PS-1000 P-103 PAO-100 P-Xylene
5wt% 10wt% 12wt% 5wt% 10wt% 12wt% 5wt% 10wt% 12wt% 5wt% 10wt% 12wt%
Cloud point(oC) 30.2 32.1 33 31.8 33.6 33.8 32.2 30.2 33.4 32 29.4 32.2
Cloud point(K) 303.35 305.25 306.15 304.95 306.75 306.95 305.35 303.35 306.55 305.15 302.55 305.35
Sample 2 (S-713)
Cloud point(oC) 30.2 30 32.2 26 26 32 33.4 31.8 31.6 31 30 33
Cloud point(K) 303.35 303.15 305.35 299.15 299.15 305.15 306.55 304.95 304.75 304.15 303.15 306.15
Sample 3 (S-714)
Cloud point(oC) 40 36 37 27.2 33.8 33 32.2 36 27.8 27 30 25
Cloud point(K) 313.15 309.15 310.15 300.35 306.95 306.15 305.35 309.15 300.95 300.15 303.15 298.15
The cloud point for samples 1, 2 and 3 were 25, 37 and 31 respectfully. Refer to figures 17 to 52 below for the Cooling curve graphs.
21
8.1 Cooling curve plots for Sample 1 (S-600)
Figure 13: Cooling curve for 5wt% and crude oil only of the PS-1000 solvent for Sample 1.
22
Figure 16: Cooling curve for 5wt% and crude oil only of the P-103 solvent for Sample 1.
23
24
Figure 19: Cooling curve for 5wt% and crude oil only of the PAO-100 solvent for Sample 1.
25
Figure 22: Cooling curve for 5wt% and crude oil only of the P-Xylene solvent for Sample 1.
26
27
28
29
30
31
32
33
34
35
36
37
38
39
Table 2: Viscosity test results for each sample of crude oil at 70oC.
Wt% Viscosity, µsample (cP)
PS-1000 P-103 PAO-100 P-Xylene No Solvents
Sample 1 (S-600)
5 0.003113254 0.003055062 0.003055062 0.004137869 0.002690466
10 0.00480723 0.00473756 0.004952904 0.0051479
12 0.011272126 0.011674702 0.013075667 0.013910284
Sample 2 (S-713)
5 0.002830231 0.002746989 0.002782057 0.002985312 0.002712794
10 0.005403168 0.005230267 0.005785693 0.005998012
12 0.011272126 0.006347411 0.013910284 0.015945935
Sample 3 (S-714)
5 0.004329691 0.004273094 0.004301206 0.004604108 0.002905704
10 0.011272126 0.011081073 0.012107099 0.013620486
12 0.015945935 0.014212681 0.01556627 0.017204825
The above table 2 was calculated using the formula below:

k= Where k is the viscosity of the samples or µsample
.
Sample calculation for PS-1000 of 5wt%:

.
k or µsample = = 0.003113 cP/s
The viscosity, concentration, cloud point temperature and specific gravity were all made
dimensionless in order to attain the regression analysis. Where sample 1 (S-600) sample
calculations were shown and the same method was used for the other two samples from samples
2 (S-713) and sample 3 (S-714).
8.4 Regression Analysis sample calculations for Sample 1 (S-600)
Viscosity =
Where μsample - Viscosity of sample (cP/s)

μwater - Viscosity of water(cP/s)
40
From table 2 when the PS-1000 solvent and 5wt% for sample 1 was used:-
. /
Viscosity = = 0.10688 (refer to table 12)
. /

Concentration = = 0.05
From table 1 when the PS-1000 solvent and 5wt% for sample 1 the cloud point, T was attained:-
.
Cloud point = = = 0.1106 Where Tc - Constant 273 (oC)

Specific gravity =
Where ρsample - Density of sample (g/cc)
ρwater - Density of water(g/cc)
From table 10, refer to appendix, when the PS-1000 solvent and 5wt% for sample 1 was used:-
. .
Density of sample = = = 0.8602g/cc

. /
Specific gravity = =0.8797 (refer to table 12)
. /
Regression Analysis General Equation:
)=A× × × …………………………….…1
Where:-
μsample - Viscosity of sample (cP/s)
μwater - Viscosity of water(cP/s)
A- y-intercept
C- Concentration (wt %)
T- Cloud point temperature (oC)
41
Tc - Constant 273 (oC)
ρsample - Density of sample (g/cc)
ρwater - Density of water(g/cc)
a,b and c are constants
Equation becomes:
LN ) = LN (A) + a LN + b LN ) + c LN ( …………………….2
Now for each sample:
Sample 1: LN ) = LN (239.96) + 0.184 LN + 2.721 LN ) + 11.24 LN ( ……...3
Sample 2: LN ) = LN (43.71) + 1.125 LN + 1.114 LN ) + 2.645 LN ( ….….4
Sample 3: LN ) = LN (7.028) + 1.222 LN + (-0.135) LN ) + 2.576 LN ( ….5
The above equations, 3 to 5, were found by using the regression analysis on Microsoft Excel 2013.
Also the regression analysis results obtained for each sample are located in the appendix in tables
14 to 16.
42
DISCUSSION
The first experiment performed was the wax solvency test also known as the wax ball deposit test.
This involved the solid wax being rolled into approximately a 1g ball and then being placed in a
solvent or distilled water solution with different concentrations of solvents in a water bath for 3
hours. This experiment resulted in the PAO-100 solvent having the best results for both sample S-
138 and Barrackpore #592, refer to tables 3 to 6, in dispersing and reducing the wax ball to the
smallest size when left at the same amount of time with the other solvents. The P-Xylene did
however prove to be the most effective but due to the possible carcinogenic nature of this chemical
as well as certain safety standards that Petrotrin-Trinmar follows, its use alone in bulk is not
allowed.
The second test that was performed was the cloud and pour point tests which resulted in all the
pour point being -9oC. At this temperature the crude oil sample became very thick but was still
able to flow at a very slow pace. This was the lowest temperature that the uwi lab was able to allow
me to attain at the time when I was performing my experiment. However, dry ice should have been
used to try to reduce the temperature even further so as to allow no flow or the sample should have
been left for more than 1 hour in the freezer. Also according to the literature the standard oil
industry range for the pour point is usually between -30oC to 30oC, where low-wax crudes having
pour points below -30oC,(API 2011).
Furthermore, the solvents and dispersants used tends to keep waxes that has precipitated out of
solution from sticking together thus allowing for dehydration of the crude to take place which may
be a contributing factor as to why the pour point may not have worked. Thus a crystal modifier
should have been used to prevent the initial crystals from forming and thus would have been the
better solvent for the test.
These small weight percentages, 5wt%, 10wt% and 12wt%, where used because of the small
volume of crude oil used as well as the limited amount of solvent provided. The samples were
heated to 70oC to ensure that all the wax was in a solution state and that is the usual temperature
of the reservoir. Cooling curves were plotted after taking readings for every 5oC drop then a tangent
was inserted on the two straight portions on the graph and the point of intersection of these tangents
43
indicated the cloud point of the sample. The cloud point results showed that each sample of crude
oil with its own specified concentration had its own cloud point and cooling curve trend.
The cooling curves, refer to figures 17 to 28 in the results, for sample 1 (S-600) showed that all
the samples with the respective solvents did cool at a faster rate than the crude oil only sample.
The shape of the cooling curve also displayed a smooth negative curve when compared to the
crude oil only curve which showed that from 70oC to 65oC there was a sharp decrease and hence
a steep slope in the graph. Then from 50oC to 30oC there was a moderate decline in the curve of
the graph and hence indicated the formation of the wax being precipitated out of solution. Thus
the continued cooling of the crude oil took longer since the energy liberated was being used to
form more wax crystals as the temperature decreased.
Also as the weight percentages for PS-1000 and P-103 increased the time it took to cool the crude
oil slightly increased then decreased in time which may have been caused by the chemical nature
of the solvents or possible human reaction errors. However, for solvents PAO-100 and P-Xylene
with the increase in weight percentages the time it took to cool was shorter. Thus proving once
again that the PAO-100 solvent was the best suited for this sample of crude oil from oil well S-
600.
Sample 2 obtained from oil well S-713 showed that for all the cooling curves, refer to figures 29
to 40, the crude oil only was allowed to cool faster to room temperature than the crude oil samples
with the varying solvents at the respective weight percentages. The cloud point for the crude oil
only was found to be 37oC. This then suggests that there are certain chemical properties in the
solvents which are reacting with the crude oil to cause an exothermic reaction hence resulting in
the increased cooling rate in the graphs. The solvents PS-1000 and P-103 were the two solvents
which may have had the chemicals that made the cooling curve exceed the crude oil only graph.
Whereas the PAO-100 and the P-Xylene had part of the curve under the crude oil only graph for
the 5wt% concentrations. The 10wt% and 12wt% increase in concentration showed that the curve
had returned to its normal position under the crude oil only graph but it still took a longer time to
cool. The lower the cloud point of the crude oil would suggest that the wax precipitation would
remain low with the particular solvent and thus be able to gain better results in the mitigation of
wax/asphaltene build up in the pipe lines. So for sample 2 (S-713) the P-103 solvent was best
suited for this since the cloud point was kept the lowest.
44
Sample 3 obtained from oil well S-714 showed that the cooling curve graphs, refer to figures 41
to 52, both the crude oil only sample and the sample with the respective concentrations had an
almost linear relationship. Also the time it took to cool was shorter than the other two samples of
crude oil. Thus the solvents were able to lower the cloud points for all the samples except for the
PS-1000 sample which gained temperature due to the chemicals reaction with the crude oil. This
also proved that the P-103 solvent was best suited for sample 3 (S-714) since the cloud point
temperature was the lowest with this solvent thus suggesting that the wax/asphaltene would form
at a lower temperature and would have less frequent buildup of wax in the pipeline.
The specific wax and asphaltene percentages for these samples were not found since the sample
weren’t available when I was performing the determination of wax and asphaltene in crude oil
samples, refer to appendix for details of the experiments, when I was at the Santa Flora lab.
However, results provided by Mr. Diaz from an online archive at Petrotrin allowed me to view that
in 2009 the wax and asphaltene percentages were 5.91% and 5.47% and in 1.79% and 71.30%
respectfully for oil well S-600. This showed that the solvent (P-103) being used to treat the
asphaltene is increasing the wax content in these pipelines and this can be helped by applying the
proper amount of PAO-100 solvent for the paraffin and P-103 solvent for the asphaltene at the
appropriate concentrations.
The regression analysis was used to develop a relationship with the viscosity, concentration, cloud
point and specific gravity. This resulted in equation 1 relating the variables and by taking the Ln
of the equation, hence producing equation 2, where this can be used to make predictions of certain
outcomes for each sample.
Limitations
 Heat loss to the environment when transferring the samples.

 Human reaction time when starting the stop watch.
Precautions
 A fume hood should be used at all times during the experiment.

 Gloves, safety goggles and laboratory coats are to be worn at all times when in the
laboratory because if contacted with the skin or eyes P-Xylene may act as an irritant.
 Properly dispose of waste by having a waste bottle for the P-Xylene chemical.
45
Sources of Error
 The measuring cylinder should be cleaned every time before its use because the black crude
oil made it difficult to seen the markings, this can be seen in figure 13 on the following
page.
Figure 49: Picture showing a possible source of error

 It was difficult to make the wax ball the same size, shape and exact mass for the experiment
which may have made the results inaccurate.
 The analytical balance was ensured to be zeroed before every weighting but due to the age
of the device it could have resulted in inaccurate results.
 A fine strainer or filter paper could have been used to gather the smaller particles that were
in the conical flask for weighting.
 The tub of ice used for the cooling process made it difficult to view the thermometer at eye
level while keeping the bulb of it submerged into the sample.
 For the viscosity test a device like a viscometer should have been used because the
consistency of the 45o angle for the sample to fall was difficult to maintain.
46
CONCLUSION
From this report it can be concluded that:
 The best suited solvent for each sample were:

Sample Solvents
1 (S-600) PAO-100
2 (S-713) P-103
3 (S-714) P-103
 The viscosity of each sample became easier to flow when heated to 70oC as well as with
the addition of 12wt% of the respective solvents. However, sample 3 (S-714) was the most
flow able of all the samples.
RECOMMENDATIONS
 Tests involving simulations with pressure should have been done to determine whether it
affects the wax/asphaltene deposit.
 The experiments could have been repeated using more blends of different chemical
inhibitors in order to observe the changes in the wax/asphaltene properties.
 Also higher concentrations of weight percentages should have been used like 15wt% and
20wt% to see what other changes could be observed.
 A viscometer machine that is hooked up to a computer could be used to gather more
accurate results for the viscosity test.
47
REFERENCES
1. (API) The American Petroleum Institute. 2011 “ Crude oil Category”. Last Modified
November 2003 Accessed December 4th.
a. http://www.epa.gov/chemrtk/pubs/summaries/crdoilct/c14858.pdf
2. (EIA), US Energy Information Admistration. 2013. "Trinidad and Tobago Country
Analysis Note." Last Modified October 2013 Accessed October 8th.
http://www.eia.gov/countries/country-data.cfm?fips=td.
3. (EPA), U.S. Environmental Protection Agency. 1995. "Petroleum Refining ". Last
Modified September 1995. Accessed October 14th.
http://www.epa.gov/Compliance/resources/publications/assistance/sectors/notebooks/petr
efsn.pdf
4. Ararimeh Aiyejina, Dhurjati Prasad Chakrabarti, Angelus Pilgrim, M.K.S. Sastry. 2011.
"Wax formation in oil pipelines: A critical review." International Journal of Multiphase
Flow:37, 671-694.
5. Aris, Hanafi. 2014. ASTM D2500 cloud point testing.
6. BBC. 2007. "How crude oil was formed." Last Modified October 2007 Accessed October
8th. http://www.bbc.co.uk/bitesize/standard/chemistry/materialsfromoil/
how_crude_oil_was_formed/revision/2/.
7. Becker, J.R. 1997. Testing Methodologies. In Crude Oil Waxes, Emulsions, and
Asphaltenes. United States of America: PennWell Publishing Company.
8. B.F. Towler, O. Jaripatke, S. Mokhatab, 2011. "Experimental Investigations of the
Mitigation of Paraffin Wax Deposition in Crude Oil Using Chemical Additives."
Petroleum Science and Technology 29 (5):468-483. doi: 10.1080/10916460903394029.
9. Brill, James P. 1998. "Paraffin Deposition Phenomena in crude oil pipelines." Petroleum
Engineering Dept., The University of Tulsa, USA 43 (0926-5112):43-64. doi: 10.1007/978-
94-011-5248-8_4.
10. C. Lira-Galeana, A. Hammami, "Chapter 21 Wax Precipitation from Petroleum Fluids: A
Review," Developments in Petroleum Science from Science direct. Last modified August
2013. Accessed November 2th.
48
11. Chakrabarti D P; A Pilgrim, M K S Sastry, G Das. (2011) Identification of Liquid-Liquid
flow pattern in a horizontal pipe using Artificial Neural Networks; Chem. Eng. Comm.
198, 273 – 285.
12. Diaz, Michael. 2014. " Petrotrin Petroleum Engineer discussing the Wax/Asphaltene
problems and solutions.", October 20th.
13. Ekeh Modesty Kelechukwu, Hikmat Said Al-Salim, Ahmmed Saadi, "Prediction of wax
deposition problems of hydrocarbon production system,"Journal of Petroleum Science and
Engineering from Science direct. Last modified August 2013. Accessed November 2th.
14. Glendasmith. 2013. "Pipeline Pigging." Last Modified February 2013 Accessed October
10th. http://petrowiki.org/File%3AVol3_Page_384_Image_0001.png.
15. HALLIBURTON. 2005. Paraffin and Asphaltene Control.
16. Jack F. Tinsley, Robert K. Prud'homme, "Deposition apparatus to study the effects of
polymers and asphaltenes upon wax deposition." Journal of Petroleum Science and
Engineering from Science direct. Last modified August 2013. Accessed November 2th.
17. Lucas Makowsk, Jin Chen, David Subero, Kenny Yu, Nicholas Mcintosh. 2010. Paraffin
Wax Deposition and Control.
18. Monique B. Vermeire Ghent. 2012." Everything You Need to Know About Marine Fuels,"
19. PetroWiki. 2014. "Remediating wax deposition." SPE International, Last Modified May
2014 Accessed October 12th.
http://petrowiki.org/Remediating_wax_deposition#Mechanical.
20. Shirley R, D.P. Chakrabarti, G. Das (2012). Artificial Neural Networks in Liquid-Liquid
Two Phase Flow; Chem. Eng. Comm.199, 1520 – 1542.
21. Yong Bai, Qiang Bai. 2005. Wax and Asphaltene. In Subsea Pipelines and Risers, edited
by Qiang Bai. The Boulevard, Langford Lane Kidlington, Oxford Elsevier Limited.
22. Zubair A. Chandio,Ramasamy M,Hilmi B. Mukhtar, “Temperature effects on solubility of
asphaltenes in crude oils," Chemical Engineering Research and Design from Science
direct. Last modified September 21st. Accessed November 4th.
49
APPENDIX
50
13.1 METHODOLOGIES CONTINUED
7.5 Method for Wax Solvency
a. An empty beaker and basket was firstly labeled A to F and weighed on an analytical balance
scale where its initial weight was recorded.
b. A stirrer magnet was then placed into each beaker.
c. A solid sample of wax deposit from the pipe lines was rolled into a 5g – 6g ball and the
weight of each ball recorded and placed into the basket.
d. The beakers were then filled in a fumehood with their corresponding chemicals labeled
wax solvent A-F (WSA to WSF).
e. It was then placed into a water bath of 38oC and left with the stirrer on for 4 hours.
f. After the 4 hours each beaker was removed and allowed to cool and an observation of each
ball was made and recorded.
g. The initial weight of the watch glass was recorded before placing the remainder of the wax
ball from the basket onto the glass for weighing.
h. For any beaker that had no ball deposit remaining and fine scraps then this was said to have
no waxy residual and thus the wax was dispersed.
i. The percentage of wax remained was then calculated.
Figure 50: Set up of experiment in the water bath for wax solvency testing.
51
7.6 Determination of Wax in crude oil.
a. A sample of 2.0g was weighed and placed into a milk dilution bottle and was covered so
as to reduce the loss of light ends from the crude sample.
b. 35ml of Petroleum Ether was added to the sample and swirled.
c. 110ml of acetone was then added to the new mixture and was swirled gently to ensure
mixing.
d. It was then placed into a cooling bath containing glycol and methanol in a 1:1 ratio with a
temperature of -20oC is maintained
e. The mixture was observed until a temperature of -4oC was reached and the initial time
recorded and left for exactly 2 hours.
f. A ‘wash solution’ was prepared with Petroleum Ether / Acetone (1:3) and was also stored
in the cooling bath in a milk dilution bottle.
g. After the two hours the sample was removed and filtered through GFC filter paper by
vacuum filtration.
h. 50ml of the ‘wash solution’ was then used to rinse the milk dilution bottle and the filter
paper.
i. The residue from the filter paper is left in the Millipore funnel but it was placed on a funnel
stand with weighed crucibles placed at the bottom to collect the filtrate (wax).
j. Hot toluene was then poured in portions of 30ml, 30ml and 40ml into the funnel to rinse
its contents in a fume hood.
k. The crucibles were placed on hotplates in order to evaporate the toluene in a fume hood.
l. When it was evaporated to dryness the crucibles were placed into a desiccator for 1 hour
and was reweighed.
m. The percentage of wax was then calculated.
52
Figure 51: Set up of experiment for the determination of wax in a sample of crude oil.
7.7 Determination of Asphaltene in crude oil.
a. A sample of 5.0g was weighed into a conical flask and was covered so as to reduce the loss
of light ends from the crude sample.
b. 150ml of n-heptane was added to the sample and swirled to ensure mixing and left
overnight in a dark cupboard.
c. Forceps were then used to place Whatman #42 filter paper into the filter funnel and a glass
jar placed at the bottom to collect the filtrate.
d. The liquid mixture (sample of crude oil and n-heptane) was poured into the filter paper in
portions so that an overflow of the funnel was not created.
e. The filter paper was then washed with warm n-heptane until the filtrate runs clear.
f. The pre-weigh crucibles were then placed under the funnels and rinsed in portions with
toluene.
g. The conical flask was also rinsed and filtered with the warm toluene until the filter paper
becomes white.
53
h. It filtrate was ensured to be clear and drained properly before it was placed into the fume
hood on a hotplate to evaporate until dry.
i. The crucible was then placed in the desiccator for 1 hour and was reweighed.
j. The percentage of asphaltene was then calculated.
Figure 52: Set up of experiment for the determination of asphaltene in a sample of crude
oil.
54
13.2 RESULTS
Table 3: The weight before and after wax ball deposits from well S-138 was placed in a water
bath.
Weight (g)
Samples PS-1000 P-103 PAO-100 P-Xylene No Solvents
Before 1.06 0.95 0.98 1.03 0.94
Water After 0.94 0.65 0.00 0.00 0.79
P- Before 0.95 0.97 1.01 0.93 0.98
Xylene After 0.00 0.00 0.00 0.00 0.00
Table 4: The weight before and after wax ball deposits from Barrackpore well #592 was placed
in a water bath.
Weight (g)
Samples PS-1000 P-103 PAO-100 P-Xylene No Solvents
Before 0.98 1.09 0.96 1.09 1.03
Water
After 0.56 0.90 0.00 0.00 0.84
Before 1.05 1.01 0.98 - 0.97
P-Xylene
After 0.00 0.00 0.00 - 0.00
Table 5: The weight before and after the wax ball from well S-138 was emerged in the respective
solvents alone.
Weight (g)
Samples PS-1000 P-103 PAO-100
Before 1.16 1.22 1.19
After 0.26 0.54 0.12
Table 6: The weight before and after the wax ball from Barrackpore #592 was emerged in the
respective solvents alone.
Weight (g)
PS-1000 P-103 PAO-100
Samples
Before 1.20 1.24 1.18
After 0.12 0.42 0.08
55
Tables 7 to 9 below shows the results obtained for the cloud point and pour point tests.
Table 7: Time recorded for every 5oC drop for sample 1 (S-600) with the various solvents at the respective concentrations.
Sample 1 (S-600)
Time (mins)
o
Temp. ( C) PS-1000 P-103 PAO-100 P-Xylene No Solvents
70 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
65 0.24 0.34 0.32 0.27 0.33 0.35 0.29 0.23 0.36 0.43 0.25 0.37 0.59
60 0.58 64.80 61.20 62.40 70.80 67.20 67.80 0.44 71.40 123.00 0.52 62.40 143.40
55 84.00 88.20 81.00 81.60 120.60 90.60 82.80 73.20 94.20 201.00 80.40 80.40 257.40
50 137.40 135.60 121.20 130.80 147.00 141.00 153.60 125.40 143.40 270.00 129.60 126.00 332.40
45 192.00 190.80 143.40 184.80 204.00 199.80 215.40 181.80 195.00 366.00 184.80 148.20 429.60
40 254.40 252.00 203.40 247.20 262.80 253.80 303.00 245.40 255.60 446.40 241.20 201.60 544.80
35 327.00 328.20 261.00 316.20 366.00 329.40 380.40 326.40 317.40 561.60 306.00 267.60 663.60
30 438.60 440.40 391.80 420.00 480.60 439.80 504.00 429.00 394.20 721.80 388.80 377.40 808.80
25 601.80 616.20 550.20 555.00 634.80 571.20 677.40 601.20 554.40 916.80 542.40 505.20 920.40
20 847.20 865.80 745.80 688.20 853.80 731.40 1020.00 859.20 725.40 1175.40 781.20 688.80 1333.20
Pour Point -9
o
( C)
56
Sample 2 (S-713)
Time (sec)
Temp. (oC) PS-1000 P-103 PAO-100 P-Xylene No Solvents
70 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
65 0.37 0.32 0.34 0.21 0.31 0.31 0.27 0.23 0.25 0.34 0.19 0.29 0.38
60 69.60 63.60 63.00 30.60 64.20 64.20 34.20 26.40 33.00 31.80 19.20 31.80 64.20
55 120.00 84.00 90.60 84.60 87.00 92.40 79.20 64.80 72.60 76.80 67.20 70.20 82.80
50 150.60 130.80 144.60 137.40 138.60 148.80 125.40 84.00 89.40 129.60 78.00 86.40 127.20
45 211.80 183.60 198.60 191.40 192.60 207.00 151.80 135.60 127.80 186.00 121.20 135.00 151.20
40 269.40 240.60 262.80 256.20 254.40 249.60 207.60 186.00 180.60 247.20 145.80 187.20 189.60
35 376.80 310.80 363.00 319.20 325.80 331.80 300.00 247.80 240.60 322.80 200.40 249.60 247.20
30 504.00 426.60 438.00 420.00 444.00 422.40 391.80 327.60 321.00 484.80 259.80 329.40 318.60
25 729.60 612.60 505.80 445.80 607.80 506.40 558.60 451.20 442.80 724.20 334.20 487.20 382.20
20 1140.60 874.80 634.80 561.00 870.60 783.00 797.40 661.80 630.00 1141.80 491.40 671.40 420.00
Pour Point -9
o
( C)
57
Sample 3 (S-714)
Time (sec)
Temp. (oC) PS-1000 P-103 PAO-100 P-Xylene No Solvents
70 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
65 0.21 0.20 0.17 0.27 0.19 0.20 0.31 0.19 0.19 0.43 0.27 0.29 0.26
60 25.80 31.80 24.60 35.40 28.20 21.60 31.80 23.40 32.40 68.40 64.20 32.40 29.40
55 66.60 73.20 66.60 76.80 67.80 32.40 74.40 63.00 71.40 90.60 81.00 72.00 70.80
50 86.40 87.60 84.60 85.80 87.60 71.40 90.00 81.60 88.20 133.80 129.60 91.20 87.60
45 133.20 126.60 133.80 120.00 132.00 89.40 127.80 128.40 138.00 147.00 152.40 139.80 133.80
40 186.60 142.20 185.40 142.20 181.80 136.80 147.00 181.20 181.20 180.00 205.20 193.80 183.60
35 213.00 192.00 207.00 186.00 210.00 180.60 208.80 211.20 213.60 195.60 243.00 252.00 241.80
30 270.00 247.80 251.40 208.20 258.60 211.20 269.40 301.80 301.20 250.20 270.60 303.60 306.00
25 324.60 310.80 305.40 273.00 275.40 305.40 421.20 381.00 313.80 268.80 367.80 335.40 327.60
20 389.40 381.60 370.80 423.00 324.60 335.40 551.40 480.60 491.40 329.40 395.40 443.40 379.20
Pour Point -9
o
( C)
58
Table 10: Mass of each beaker before and after a sample.
Sample 1 (S-600)
Wt % Mass (g)
Beaker Beaker + Beaker Beaker + Beaker Beaker + Beaker Beaker + Beaker Beaker +
Sample Sample Sample Sample Sample
5 117.39 164.7 105.83 154.02 103.95 152.13 92.49 140.63 101.06 147.78
10 167.45 156.77 154.88 143.38
12 168.55 157.87 155.98 144.48
Sample 2 (S-713)
Wt % Mass (g)
5 109.68 156.75 108.66 155.84 109.27 158.35 110.54 158.1 60.53 106.7
10 159.5 158.59 161.1 160.85
12 160.6 159.69 162.2 161.95
Sample 3 (S-714)
Wt % Mass (g)
5 64.66 109.37 81.01 125.78 63.79 108.01 63.52 108.72 112.68 157.02
10 112.12 128.53 110.76 111.47
12 113.22 129.63 111.86 112.57
Volume used was 55cc.
59
Table 11: Time taken for 10ml of the samples to fall.
Sample 1 (S-600)
Wt Time (sec)
% PS-1000 P-103 PAO-100 P-Xylene No Solvents
5 126 128.4 128.4 94.8 145.8
10 81.6 82.8 79.2 76.2
12 34.8 33.6 30 28.2
Sample 2 (S-173)
Wt Time (sec)
5 138.6 142.8 141 131.4 144.6
10 72.6 75 67.8 65.4
12 34.8 61.8 28.2 24.6
Sample 3 (S-174)
Wt Time (sec)
5 90.6 91.8 91.2 85.2 135
10 34.8 35.4 32.4 28.8
12 24.6 27.6 25.2 22.8
Time taken for distilled water to fall 14s
Table 12: Table used for the regression analysis.

For Sample 1 (S-600)
Viscosity Concentration Cloud point Temp. Specific
gravity
0.106879734 0.05 0.110622711 0.879653552
0.165034883 0.1 0.117582418 0.930785391
0.386978348 0.12 0.120879121 0.951238126
0.104881982 0.05 0.116483516 0.896015741
0.162643074 0.1 0.123076923 0.947147579
0.400799003 0.12 0.123809524 0.967600314
0.104881982 0.05 0.117948718 0.895829807
0.170035941 0.1 0.110622711 0.946961645
0.448894883 0.12 0.122344322 0.96741438
0.142055343 0.05 0.117216117 0.895086071
0.176730269 0.1 0.107692308 0.946217909
60
0.477547748 0.12 0.117948718 0.966670644
0.092365202 0 0.091575092 0.868683449
Table 13: LN of table 12 used for the regression analysis.

LN of Sample 1 (S-600)
Viscosity Concentration Cloud point Temp. Specific gravity
-2.236051057 -2.995732274 -2.201629871 -0.12822714
-1.801598412 -2.302585093 -2.140615765 -0.071726543
-0.949386537 -2.120263536 -2.112964234 -0.049990852
-2.254919542 -2.995732274 -2.150005505 -0.109797299
-1.816197212 -2.302585093 -2.094945728 -0.05430036
-0.914295217 -2.120263536 -2.089010993 -0.032936176
-2.254919542 -2.995732274 -2.137505343 -0.110004832
-1.771745449 -2.302585093 -2.201629871 -0.054496688
-0.800966532 -2.120263536 -2.100915895 -0.033128354
-1.95153856 -2.995732274 -2.143735892 -0.110835397
-1.733130613 -2.302585093 -2.228477121 -0.055282389
-0.739091128 -2.120263536 -2.137505343 -0.033897437
The regression analysis used the results from table 13 above to attain the table 14 on the following
pages to develop the equations that produces a relationship between the viscosity, concentration,
cloud point and specific gravity together.
61
Table 14: Results from the Regression analysis for Sample 1 (S-600).
SUMMARY OUTPUT
Regression Statistics
Multiple R 0.886
R Square 0.784
Adjusted R 0.704
Square
Standard Error 0.320
Observations 12.000
ANOVA
df SS MS F Significance F
Regression 3.000 2.976 0.992 9.702 0.005
Residual 8.000 0.818 0.102
Total 11.000 3.794
Coefficients Standard t Stat P-value Lower 95% Upper 95% L
Error
Intercept 5.480 5.627 0.974 0.359 -7.496 18.457 -7
X Variable 1 0.184 1.061 0.174 0.867 -2.262 2.631 -2
X Variable 2 2.721 2.361 1.152 0.282 -2.724 8.166 -2
X Variable 3 11.238 12.235 0.918 0.385 -16.977 39.452 -
SUMMARY OUTPUT
Multiple R 0.822
R Square 0.675
Adjusted R Square 0.567
Observations 13.000
ANOVA
df SS MS F Significance F
62
Regression 3.000 0.190 0.063 6.232 0.014
Residual 9.000 0.091 0.010
Total 12.000 0.281
Coefficients Standard Error t Stat P-value Lower 95% Upper 95% L
Intercept -0.956 1.689 -0.566 0.585 -4.777 2.865 -4

X Variable 1 2.866 2.284 1.255 0.241 -2.301 8.034 -2
X Variable 2 4.843 3.342 1.449 0.181 -2.718 12.404 -2
X Variable 3 0.420 2.211 0.190 0.853 -4.580 5.421 -4
63
SUMMARY OUTPUT
Multiple R 0.995
R Square 0.991
Adjusted R 0.987
Square
Observations 12.000
ANOVA
df SS MS F Significance
F
Regression 3.000 3.640 1.213 278.580 0.000
Residual 8.000 0.035 0.004
Total 11.000 3.675
Coefficients Standard t Stat P-value Lower 95% Upper Lo
Error 95% 95
Intercept 1.950 0.326 5.976 0.000 1.198 2.702 1.
X Variable 1 1.222 0.260 4.704 0.002 0.623 1.821 0.
X Variable 2 -0.135 0.153 -0.885 0.402 -0.487 0.217 -0
X Variable 3 2.576 2.760 0.933 0.378 -3.788 8.940 -3
64
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Treatment of Waxy Oil 3

Technical Report · December 2014

Shivanie Mahabir Dhurjati Prasad Chakrabarti

SEE PROFILE SEE PROFILE

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2. Transportation and deposition of precipitate

3. Reduction in permeability due to precipitate deposition

Figure 6: Asphaltene stability vs. pressure, (Bai.et.al, 2005).

1. Cloud point Testing

Figure 8: Pour-point testing,(Becker 1997).

3. Rolled-ball deposit Test/Wax solvency testing

 8 conical flasks (125ml),

 Wax deposits (from S-138 and Barrack pore #592)

Procedure for Wax Solvency testing:-

 Crude oil samples (S-600, S-713 and S-714)

Procedure to determine the cloud points of the crude oil sample: -

 Crude oil samples (S-600, S-713 and S-714)

Procedure to determine the pour point of the crude oil sample: -

7.4 Testing for viscosity

 Crude oil samples (S-600, S-713 and S-714)

Procedure to determine the viscosity using heating:-

The above table 2 was calculated using the formula below:

Sample calculation for PS-1000 of 5wt%:

8.4 Regression Analysis sample calculations for Sample 1 (S-600)

Where μsample - Viscosity of sample (cP/s)

Where ρsample - Density of sample (g/cc)

ρwater - Density of water(g/cc)

Regression Analysis General Equation:

μsample - Viscosity of sample (cP/s)

μwater - Viscosity of water(cP/s)

T- Cloud point temperature (oC)

ρsample - Density of sample (g/cc)

ρwater - Density of water(g/cc)

a,b and c are constants

Now for each sample:

Sample 1: LN ) = LN (239.96) + 0.184 LN + 2.721 LN ) + 11.24 LN ( ……...3

Sample 2: LN ) = LN (43.71) + 1.125 LN + 1.114 LN ) + 2.645 LN ( ….….4

Sample 3: LN ) = LN (7.028) + 1.222 LN + (-0.135) LN ) + 2.576 LN ( ….5

 Heat loss to the environment when transferring the samples.

 A fume hood should be used at all times during the experiment.

Figure 49: Picture showing a possible source of error

 The best suited solvent for each sample were:

7.7 Determination of Asphaltene in crude oil.

Table 12: Table used for the regression analysis.

Table 13: LN of table 12 used for the regression analysis.

Intercept -0.956 1.689 -0.566 0.585 -4.777 2.865 -4

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