The document provides information about the Nigerian National Petroleum Corporation Research and Development Division (NNPC R&D). It discusses the division's core business activities including crude oil assay. Crude oil assay involves characterizing crude oil through testing to determine properties, yields from distillation, and suitability for refining. The NNPC R&D division conducts crude oil assays using distillation and other analytical techniques. The document outlines the division's vision, mission, management structure, and departments involved in crude oil testing and characterization.

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CHAPTER ONE
1.0 INTRODUCTION
1.1 THE OVERVIEW OF SIWES PROGRAMME
The Student Industrial Work Experience Scheme (SIWES) is an accepted skills
programme which forms part of the approved academic standards in the degree
programme for Nigerian Universities. In 1974, the Federal Government of Nigeria
introduced the national policy on Industrial training, called the Students,
Industrial Work Experience Scheme (SIWES). This programme is under the
umbrella of the Ministry of Education through the Industrial Training Fund (ITF),
was designed to help students acquire the necessary practical
education/experience in their fields of study and other related professions.
This is an effort which was created in order to bridge the existing gap between
the theory taught in the classroom and practice of science, agriculture, medicine,
engineering, technology and other professional programmes in the Nigerian tertiary
institutions. This programme is aimed at exposing the students to the use of
various machines and equipment’s, professional work methods and ways of
safeguarding the work areas in industries as well as other organizations and
parastatals. The programme was established basically to impact elaborate practical
understanding to students with respect to their various disciplines. It is also
intended that the student through a process of relation to academic knowledge and
practical industrial application would understand the underlying principles and
become better focused and acquire the practical applications towards excellence in
his or her discipline.

2. 2
The Students Industrial Work Experience Scheme (SIWES) programme involves
the student, the Universities and the industries. This training is funded by the
Federal Government of Nigeria and jointly coordinated by the Industrial Training
Fund (ITF) and the National Universities Commission (NUC).
Industrial training fund in its policy statement No.1, published in 1973, inserted a
clause dealing with the issue of practical skills among locally trained professionals.
Section 15 of the policy statement states inter-alia, that “Great emphasis will be
placed on assisting certain products of post-secondary school system to adopt or
orientate easily to their possible post graduate job environment. The scheme
exposes students to industry based skills necessary for a smooth transition from
classroom to the world of work. It affords student of tertiary institutions the
opportunity of being familiarized exposed to the needed experience in handling
machinery and equipment which are not available in the education institute.
1.2 AIM AND OBJECTIVES OF STUDENT WORK INDUSTRIAL
EXPERIENCE SCHEME (SIWES)
The aim and objectives of the SIWES are as follows:
 To prepare students for the work situation they are likely to meet after
graduation
 To provide students with an opportunity to apply their theoretical
knowledge in real work situation, thereby bridging the gap between
university work and actual practices.
 To expose students to work methods and techniques in handling the
equipment and machinery that may be available in universities

3. 3
 Provision of avenue for students in Nigerian universities to gain industrial
skills and experience in their course of study.
 To enlist and strengthen employers involvement in entire educational
process of preparing university graduate for employment.
1.3 IMPORTANCE OF SIWES
SIWES have a lot of importance attached to it which includes:
 It helps to improve the quality of skilled manpower of the students. The
scheme provides a forum for industries to evaluate prospective employers
and gives feedback to institutions
 The scheme gives students practical knowledge of course of study
 SIWES program exposes students to real life situation, thus supplementing
the theoretical lesson
 SIWES program establish a close collaboration between institutions and
industries, a factor which is essential for preparing people for the
workforce
1.4 INDUSTRIAL TRAINING FUND (ITF)
The ITF has an aim in those establishments that handles the SIWES programme.
Its responsibilities performed through this arm involve formulating policies and
guidelines on SIWES for dissemination to bodies participating in the SIWES
programme through;
 Regularly organizing orientation programmes for students prior to their
attachment.

4. 4
 Receiving and processing master lists and placement lists forwarded from
the institutions.
 Supervising students on industrial attachment.
 Providing logistics and materials necessary for effective administration of
the scheme.
 Providing information on companies for attachment and assisting in the
industrial placement of students.
 Ensuring the visitation of ITF officers to the supervising agencies,
institutions, employers and students on attachment.
 Continuously receiving and carrying out research into the operations of
SIWES
1.5 DESCRIPTION OF THE ORGANIZATION
The Nigerian National Petroleum Corporation, Research and Development (R&D)
Division
1.5.1 Historical Background
The (NNPC, R&D) Division was established in 1977 to solve the operational and
technical problems of the oil and gas industry through the application of the
results of scientific research and the development of technology. R&D has highly
qualified personnel and experienced engineers.
Research and Development Division (R&D) is a Corporate Service Unit (CSU) of the
Nigerian National Petroleum Corporation (NNPC) is situated in Port at NNPC EPCL
Life Camp Complex, P.M.B. 5373, Eleme.
The division renders Research and Laboratory Services to the Oil and Gas
Industries.

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NNPC, R&D business entails the provision of Research Initiatives; Technology
Development and Commercial Laboratory services to the Oil and Gas Industries.
NNPC, R&D Quality Management System covers all requirements of NIS ISO
9001:2008 excluding the design requirements in 7.3.
1.5.2 RESEARCH AND DEVELOPMENT MANAGEMENT STRUCTURE
The R&D is staffed with highly professional and skilled personnel with considerable
experience in research and laboratory services to the oil and gas industries.
Below is the Division’s organogram, depicting the administrative structure of the
company. The Group General Manager (GGM) is the Chief Executive Director of the
Division. He is supported by three general managers, one in charge of Refining and
Petrochemicals (R&P) Department, the second one in charge of Exploration and
Petroleum Engineering (E&P) Department and the third one in charge of Support
and Services (S&S) Department. The Refining and Petrochemicals Department is
made up of Petroleum Product Research and Services, Environmental Research and
Services, Analytical Services, Process and Catalysis and Chromatography sections;
Exploration and Petroleum Engineering Department is made up of Exploration
Research and services, Petroleum Engineering Research and Services, Pressure
Volume and Temperature (PVT) and Renewable Energy Research and Services and;
Support and Service Department is made up of Human Resources/Administrative,
Technical Services, Finance and Accounting and Protocol sections.
In addition, there is a Managing Director’s Division made up, Planning and Business
Development, Health Safety and Environment, Internal Audit, Collaborative
Research and the Company Secretariat and Legal Advisory Services departments.

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All the departments are supported by Sectional and Units heads. The total staff
strength is about 500.
Fig. 1.0 R&D Organizational Chart
Group General Manager
Research and Development
GGM’S Office Audit
Collaborative Research
Legal
General Manager
Support Services
General Manager
Exploration and Petroleum
General Manager
Refining and Petrochemicals
Health Safety and Environment
Planning and Business Development

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1.5.3 Vision and Mission of Research and Development (R&D)
Visions:
Nigerian National Petroleum Corporation, Research and Development Division will
be a world class petroleum research centre, driven by innovation and quality.
Mission:
Nigerian National Petroleum Corporation, Research and Development Division
carries out research, develops technology and provide laboratory services in the oil
and gas industry.
1.5.4 R&D Quality Policy Statement
Research and Development shall strive to sustain high quality delivery in carrying
out research, developing technology and providing services to the oil and gas
industry. To this end, research and development shall implement and maintain
effective quality systems based on NIS: ISO 9001: 2008 that will meet regulatory
and legal requirements as well as ensure continual improvement to meet and exceed
our customers’ expectation.
1.5.5 R&D Quality Objectives
 To meet the customers’ needs for precision accuracy sensitivity and specificity
in line with the statutory requirements of ISO 9001:2008 (Clause 8:2.1)
 To meet the commercial performance criteria, namely: timeliness and
competitive cost by efficient utilization of technological, human and material
resources.
 To make cost-effective use of the technology financial human and material
resources to provide quality services that meet customers’ expectations.

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CHAPTER TWO
NIGERIAN NATIONAL PETROLEUM CORPORATION, RESEARCH AND
DEVELOPMENT (R&D) DIVISION’S CORE BUSINESS
2.1 CRUDE OIL ASSAY
A crude oil assay is the chemical evaluation of crude
oil feedstock by petroleum testing laboratories. Each crude oil type has
unique molecular and chemical characteristics. No two crude oil types are identical
and there are crucial differences in crude oil quality. The results of crude oil assay
testing provide extensive detailed hydrocarbon analysis data for refiners, oil
traders and producers. Assay data help refineries determine if a crude oil
feedstock is compatible for a particular petroleum refinery or if the crude oil
could cause yield, quality, production, environmental and other problems.
The assay can be an inspection assay or comprehensive assay. Testing can include
characterization of the whole crude oil and the various boiling
range fractions produced from physical or simulated distillation by various
procedures. Information obtained from the petroleum assay is used for detailed
refinery engineering and client marketing purposes. Feedstock assay data are an
important tool in the refining process.
Below are the summary of the sections that carry out crude oil assay in the
Nigerian National Petroleum Corporation, Research and Development Division.
i. Petroleum Product Research and Development
 Determination of yield and distillate parameters for accurate evaluation of
price potentials of crude in the international market.
 Determination of the True Boiling Point (TBP) curve of crude oil.

9. 9
 Evaluation of crude oil for product state changes and refinery product
optimization
ii. ANS: Petroleum Products Quality Testing (PPQT)
 Whole crude characterization from well heads/flow stations (Physico-
chemical analysis)
 Crude Oil Assay (Physio-Chemical Characterization)
 Product Identification and Quality Assessment of petroleum products
 Crude Oil Finger Printing for identification
iii. Spectroscopy and Elemental Analysis (SEAL)
 Metal analysis for Crude Oil assay
 Elemental analysis (CHN&O) in petroleum and its products (no CHN Analyzer
available)
 Metal analysis in petroleum and its products
 Metal Analysis in Biological samples
iv. Water & Specialty Chemicals (WASC)
 Effluent/waste water evaluation for performance monitoring/regulatory
purposes
 Quality characterization of boiler/cooling (process) water for refineries.
 Chemical analysis for Water Potability Test.
 Water Compatibility Studies for water re-injection operations.
v. Chromatography
 Crude characterisation
 Determination of the boiling range distribution of distillate fractions
 Analysis of Overhead Gas Associates and Non- associates gases

10. 10
 Determination of Polynuclear Aromatic Hydrocarbon (PAH) by HPLC using
PDA detector in waste water, sediments and soil for environmental studies.
 Determination of Total Petroleum Hydrocarbon (TPH) in soil and water.
vi. Environmental Research and Service
 Air Quality Monitoring
 Noise pollution monitoring
 Radiation Monitoring
 Thermal monitoring
 Air Pollution Modelling
 Air Dispersion Modelling and Monitoring
 Climate Change Analysis
 Quality Test on petroleum products
vii. Process and Catalysis
 Process analysis (material and energy balance studies) of refinery and
petrochemical processes
 Process modelling and simulation of refinery and petrochemical processes
 Process integration studies and optimization of energy usage (Pinch
Analysis)
 Process optimization (linear programming) of refinery and petrochemical
processes
 Analysis, modelling and simulation of processes involved in oil and gas
production (e.g., separation of oil/gas/sand mixture, gas purification, etc.)
 Flow assurance studies of multiphase flow in pipelines and flow terminal

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2.2 LABORATORY CRUDE OIL ASSAY
Laboratory assays of crud oil and condensate are conducted to establish yield
(weight % / volume %) and the product physical/chemical properties. This is by
distillation up to 3500
c using a 15 plate theoretical column and from 3500
c to
450+0
c by high vacuum flash distillation using AUTOMAXX 9100. The Assay
results give a useful and detailed picture of the quality of oil. Yield from the
original crude oil is measured as % vol or % wt.
Light ends analyse (C1 – C5), and individual fractions are separated and tested.
Individual cuts of butanes and lighter components, light Naphtha, heavy Naphtha,
kerosene, light distillate, gas oils, vacuum gas oil, light & heavy residues receive
extensive analyses for each fraction produced by the distillation process.
Analysis on crude oil and fraction includes:
 API Gravity, Correlation (calculation)
 Specific Gravity @60/600
F, D5002
 Yield % volD664
 Water by distillation vol. %, D4006/D95
 Pour point 0
c D97 D5853
 Kinematic Viscosity D445
 Water and sediment vol. %, D96 D4007
 Reid Vapour Pressure @1000
F, psi, D323
 Sulphur wt. %, D4294
 Hydrogen sulphide mg/k, UOP163
 Wax content wt.%, BP 237
 Copper mg/kg, D5863
 Acid Number mg KOH/g,

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2.3 PROCEDURE FOR CRUDE OIL ASSAY
CRUDE OIL TREATMENT
Crude oil treatment is the process of treating and removing the unwanted element
or substance from crude to a bearable level. The chart below entails how the crude
oil is treated in the laboratory for crude Assay.
Sample received at
the laboratory
Refrigerate
sample to -50
C
Water content test
Water content
less than 0.3%
Dewatering to
less than 0.3%
No
ASTM D2892 Distillation
of crude petroleum
Determination of sample
physical properties, charge
measured and loading
Equipment preparation
and wash run
Collect the overhead gas
for analysis
Generation of
distillation cuts
Distillate Storage and
characterization (Physico-
chemical Analysis)
ASTM 536 vacuum
Distillation for reduce
crude and residue
Results Analysis
compilation and Delivery
QA/QC
Yes
Fig. 2.3.0 Flow chart for Crude Assay sample Handling and management procedure

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2.3.1 SAMPLE (CRUDE OIL) RECEIVED AT THE LABORATORY
The sample must be received in a sealed metallic container and should show no
evidence of leakage. Receive samples that meet the requirements of the sampling
procedure in accordance to practice D4057 or D4177
2.3.2 SAMPLE PRESERVATION
Cool the sample to a temperature between 00
C and -50
C by placing it in a
refrigerator for several hours (preferably overnight) before opening. For waxy or
too viscous sample, raise the temperature of sample to 50
C above its pour point.
Agitate the sample by preferably shaking or other means that are appropriate to
its size, to ensure that it is well mixed.
Fig. 2.3.2.0 Sample Preservation Method

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2.3.3 WATER CONTENT TEST
This test method describes the laboratory determination of water and sediment in
crude oils by means of the centrifuge procedure. Knowing water content in
hydrocarbons enables clients to take steps to reduce risks from corrosion, safety
problems, and infrastructure damage which can be caused from unwanted water
content levels.
Significance: The water and sediment content of crude oil is significant because it
can cause corrosion of equipment and problems in processing. A determination of
water and sediment content is required to measure accurately net volumes of
actual oil in sales, taxation, exchanges, and custody transfers.
Summary of the test: Equal volumes of crude and water saturated hydrocarbon
(Toluene) are placed into a cone-shape centrifuge tube. After centrifugation, the
volume of the higher gravity water and sediment layer at the bottom of the tube is
read.
Procedure:
Fill each of two centrifuge tubes to the 50-mL mark with sample directly from the
sample container (crude oil). Using a pipette or other suitable volume transfer
device add 50 mL of toluene, which has been water saturated at 60°C (140°F) or
71°C (160°F) Read the top of the meniscus at both the 50 and 100-mL marks. Add
0.2 mL of demulsifier solution (ethelene oxide) to each tube, using a 0.2-mL pipet
or other suitable volume transfer device, such as an automatic pipettor.
Stopper the tube tightly and invert the tubes ten times to ensure that the oil and
solvent are uniformly mixed.
In the case where the crude oil is very viscous and mixing of the solvent with the
oil would be difficult, the solvent may be added to the centrifuge tube first to

15. 15
facilitate mixing. Take care to not fill the centrifuge tube past the 100-mL mark
with the sample.
Loosen the stoppers slightly and immerse the tubes to the 100-mL mark for at
least 15 min in the bath maintained at 60 6 3°C (140 6 5°F). Secure the stoppers
and again invert the tubes ten times to ensure uniform mixing of oil and solvent.
(Warning—the vapor pressure at 60°C (140°F) is approximately double that at 40°C
(104°F).)
Place the tubes in the trunnion cups on opposite sides of the centrifuge to
establish a balanced condition. (If the tubes cannot be counter-balanced by eye,
place them, in their trunnion cups, on either side of a balance and equalize their
masses by the addition of water to the trunnion cups.) Retighten the corks and spin
for 10 min at a minimum relative centrifugal force.
Immediately after the centrifuge comes to rest, following the spin, read and
record the combined volume of water and sediment at the bottom of each tube, to
the nearest 0.05mL from 0.1 to 1mL graduations, and to the nearest 0.1mL above
1mL graduations. Below 0.1mL, estimate to the nearest 0.025mL
2.3.4 DEWATERING AND DESALTING
Crude oils are complex mixtures obtained from many parts of the world, and all
crudes contain dilute dispersion/emulsion of ultrafine water droplets containing a
variety of salts, solids and metals. These emulsions might be quite stable due to the
presence of natural surfactants in oil such as asphaltenes, resins, naphthenic acids,
fine solids, etc. Adverse effects of these impurities can result in shortened unit
run lengths and reduced equipment reliability. To prevent corrosion, plugging,
fouling of equipment, electrical desalting plants are often installed in crude oil
production units in order to remove water-soluble salts from an oil stream. The

16. 16
refiners often wash the crude oil with fresh water, add chemical (demulsifier), and
use electrical desalting vessel to remove the added water and most of the inorganic
contaminants from the crude oil.
Electrical Desalter is the typical method of crude-oil desalting. After separation
by gravity settling, crude oil can be desalted by following the steps:
• The crude oil is preheated to decrease its viscosity for easy separate water from
crud and hence easy desalt. Preheating also increases demulsifier reactivity, and
destabilizing emulsion, however, the crude temperature is limited to avoid its
vaporization in the desalter, and prevent damage to the electrical grid insulator
bushings.
• The chemicals (demulsifiers) used are surfactants which migrate to the oil/water
interface to rupture the stabilizing film around the water droplets and allows them
to merge and coalesce. Chemical usage rates vary widely with crude type, and
desalter equipment. Chemicals are more efficient with basic pH water, while
electrical desalters function much better in acid pH range. Low pH result in
excessive corrosion, while high pH permits NH4OH (added to increase pH) to
migrate into the crude. Excessively high pH can aid in stable emulsion formation; So
typical pH control will be required.
• Addition of fresh water (wash water), increase coalescence and destabilizing
emulsion. The volume of wash water can be fixed from 3 to 10%; its value is
governed by the refiner’s needs.
• Wash water mixing is applied to ensure that the added fresh water is dispersed
well so that it can be available to combine with the contaminants in the crude.

17. 17
Wash water mixing is accomplished by a mixing valve with adjustable pressure drop.
• Finally, the heavier water particles settled at the bottom while the lighter crude
floats on top. The two layers are then separated by draining (decantation).
Fig. 2.3.4.1 Dewatering Unit

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Fig. 2.3.4.2 flow diagram for desalting and dewatering
2.4 EQUIPMENT PREPARATION AND WASH RUN
This is the process of preparing the equipment (Automaxx 9100) for crude oil
distillation by carrying out simple distillation with TOLUENE to wash and clean the
vital parts of the equipment for proper crude assay result. This process is also use
to determine the condition of the equipment, whether it’s in good condition or in
bad condition.
2.5 ASTM DISTILLATION OF CRUDE OIL USING AUTOMAXX 9100
This distillation system is designed for the fully automatic distillation of crude oil
and petroleum products. Crude oil distillation can be complex and time consuming.
Our crude oil distillation system includes everything needed to perform the ASTM
methods, D2892 and D5236, for distilling crude oil. The system’s automation
minimizes the operator time needed to perform the test. The equipment design
makes the test straightforward and easier to perform.

19. 19
Fig. 2.5.0 Automaxx 9100
Distillation is a chemical process where a mixture made of two or
more liquids (called "components") with different boiling points can be separated
from each other. The mixture is heated until one of the components boils (turns to
a vapor). The vapor is then fed into a condenser, which cools the vapor and changes
it back into a liquid that is called distillate. What remains in the original container
is called the "residue. In other word, distillation is a process by which a desired
product is separated from other component of feedstock by taking advantage of
the difference in the boiling points of the various components of the feedstock. As
the feedstock is heated, the boiling temperature of some of its lighter components

20. 20
is reached. The lighter components are flashed-off as vapor from the heavier
components.
The concepts for crude oil distillation are primarily the same for both atmospheric
and vacuum distillation units. However, this section will only deal with the
fractionation tower of the atmospheric distillation unit. The degree of
fractionation in a crude oil distillation unit is measured by the temperature
difference between 95% vol. ASTM (American Standard Temperature and
Measurement) of the lighter product and 5% vol. ASTM of the adjacent heavier
product. These lighter products are composed kerosene and light gas oil. The
heavier products are composed of heavy gas oil and fuel oil. When the temperature
difference gives the 95% point of the lighter products to be less than the 5%
point of the heavier products, the difference in temperatures is referred to as an
ASTM gap. For the reverse case, the situation is referred to as an ASTM overlap.
Fractionation performance is at its best when there is an ASTM gap between the
products. As fractionation decreases, the gap becomes an overlap, a greater
number of the components of the two products are not separated. Fairly complete
fractionation may be expected in the upper regions of the fractionation tower
between lighter products such as kerosene and light gas oils. However, lower in the
fractionation column such separation is not possible. It may be pointed out, that in
the lower levels of the fractionation column, there is an ASTM overlap. During
crude oil distillation steam stripping is used to further remove the entrained light
end products from the draw of
products.

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2.5.1 ATMOSPHERIC DISTILLATION BY ASTM D2892
As the name implies, the pressure profile in atmospheric distillation unit is close to
the atmospheric pressure (760mmhg) with highest pressure at the bottom stage
which gradually drops down till the top stage of the column.
The purpose of atmospheric distillation is primary separation of various 'cuts' of
hydrocarbons namely, fuel gases, LPG, naphtha, kerosene, diesel and fuel oil.
The heavy hydrocarbon residue left at the bottom of the atmospheric distillation
column is sent to vacuum distillation column for further separation of hydrocarbons
under reduced pressure.
The temperature is highest at the bottom of the column which is constantly fed
with heat from bottoms reboiler. The reboiler vaporizes part of the bottom outlet
from the column and this vapor is recycled back to the distillation column and
travels to the top stage absorbing lighter hydrocarbons from the counter current
crude oil flow. The temperature at the top of the column is the lowest as the heat
at this stage of the column is absorbed by a condenser which condenses a fraction
of the vapors from column overhead. The condensed hydrocarbon liquid is recycled
back to the column. This condensed liquid flows down through the series of column
trays, flowing counter current to the hot vapors coming from bottom and
condensing some of those vapors along the way.
The Automaxx 9100 distillation column has 15 theoretical plates and complies fully
with ASTM D2892 and the packed column is configured to distill the crude oil at
atmospheric up to 3500
C.

22. 22
The products of atmospheric distillation include:
 LPG and lighter gases
 Straight-run gasoline
 Naphtha
 Gas Oil
 Fuel Oil (kerosene)
 Atmospheric Residuum (bottoms/asphalt)
.
Fig. 2.5.1.0 Atmospheric distillation blog flow diagram

23. 23
2.5.2 VACUUM DISTILLATION (ASTM 5236)
Crude oil is first refined in an Atmospheric Distillation Column. Fractions of crude
oil such as lighter gases (C1-C4), gasoline, naphtha, kerosene, fuel oil, diesel etc.
are separated in the atmospheric distillation column. The after taking out these
lighter hydrocarbon cuts, heavy residue remaining at the bottom of the
atmospheric distillation column needs to be refined. These heavy hydrocarbon
residues are sent to a Vacuum Distillation Column for further separation of
hydrocarbons under reduced pressure.
Fig. 2.5.2.0 Vacuum Distillation Unit

24. 24
Heavies from the atmospheric distillation column are heated to approximately
400˚C in a fired heater and fed to the vacuum distillation column where they are
fractionated into light gas oil, heavy gas oil and vacuum reside. Some heavy
hydrocarbons cannot be boiled at the operating temperature and pressure
conditions in the atmospheric distillation column. Hence they exit the bottom of
the column in liquid state and are sent to the vacuum distillation column where they
can be boiled at a lower temperature when pressure is significantly reduced.
Absolute operating pressure in a Vacuum Tower can be reduced to 20 mm of Hg or
less (atmospheric pressure is 760 mm Hg). In addition, superheated steam is
injected with the feed and in the tower bottom to reduce hydrocarbon partial
pressure to 10 mm of mercury or less. Lower partial pressure of the hydrocarbons
makes it even more easier for them to be vaporized, thus consuming less heat
energy for the process.
A typical Process Flow Diagram (PFD) of such a vacuum distillation column is
presented in the figure below. Steam ejectors can be used to suck the lighter
hydrocarbon vapors at low pressure from the top of the column. These vapors are
then cooled down to condense the steam which had been introduced in the column
earlier. The condensed oily water is removed and can be recycled to the column
after boiling it. Hydrocarbon vapors are taken out at this stage.
Two different cuts of hydrocarbons - 'light vacuum gas oil' and 'heavy vacuum gas
oil' are separated in the vacuum distillation column at different stages of the
column, based on the difference between their boiling point ranges. The liquid
being drawn at low pressure needs to be pumped. Then it is heated and partially
recycled back to the column. Part of is taken out as vacuum distillation products -

25. 25
'light vacuum gas oil' or 'heavy vacuum gas oil'. Light vacuum gas Oil is sent to a
hydrotreater and then to a 'catalytic cracking' unit to obtain smaller chain
hydrocarbons. Heavy vacuum gas oil is also sent for cracking using hydrogen in a
'hydrocracking unit' to produce smaller chain hydrocarbons.
Heavy hydrocarbons which cannot be boiled even under reduced pressure remain at
the bottom of the column and are pumped out as 'vacuum residue'. The vacuum
distillation column bottom residue can only be used for producing coke in a 'coker
unit' or to produce bitumen.
Fig. 2.5.2.1 Vacuum Distillation Flow Diagram

26. 26
2.5.3 CRUDE DISTILLATION FRACTIONS / CUTS
OG
SRG
LIGHT NAPHTHA
HEAVY NAPHTHA
KEROSENE
ATMOSPHERIC GAS OIL
LIGHT VACUUM GAS OIL
HEAVY VACUUM GAS OIL
VACUUM RESIDUE
KEY:
IBP - Initial Boiling Point
OG - Overhead Gas
SRG - Straight Run Gasoline
>IPB0
C
IBP-900
C
90-1200
C
120-1700
C
170-3000
C
300-3500
C
350-4000
C
400-4500
C
450+0
C

27. 27
2.6 PHYSICO-CHEMICAL ANALYSIS OF THE FRACTIONS / CUTS
This is the analysis or test method carried out in the laboratory to determine the
following:
 Density and API gravity
 Specific gravity
 Reid vapor pressure
 Off – gasses
 Cloud point
 Pour Point
 Viscosity
 Aniline point
 Asphaltenes, carbon residue and asphalt content
 Flash point
 fire point
 Smoke point
 Copper corrosion test
 Colour
 Antiknock quality (octane number)
 Cetane number
 Carbon Hydrogen ratio

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2.7 TEST METHOD FOR CRUDE PETROLEUM AND PETROLEUM
FRACTION/CUTS AND PROCEDURES
2.7.1 AMERICAN PETROLEUM INSTITUTE (API) GRAVITY TEST (ASTM
D1298)
API Gravity is the factor governing the quality of crude oils. However, the API
gravity of petroleum product is an uncertain indication of its quality.
API can also be determined by the following correlation:
API gravity =
This test is based on the principle that the gravity of a liquid varies directly
with depth of immersion of a body floating in it. The floating body which is
graduated by API gravity units in this method, is called API Hydrometer. The
API gravity is read by observing the freely floating API Hydrometer and noting
the graduation nearest to apparent intersection horizontal plane surface of the
liquid with the vertical scales of the hydrometer, after temperature equilibrium
have been reached. The temperature of the sample is read from separate
accurate ASTM thermometer in the sample from a thermometer which is an
integral part of the hydrometer (Thermo-hydrometer).
<
2.7.2 SMOKE POINT TEST (ASTM D1322)
Smoke point is the maximum height in millimeters of a smokeless flame of fuel
burned in a wick-fed lamp in specified design.
141.5 - 131.5
SP. Gravity @ 15.6/15.60
C

29. 29
Fig. 2.7.2.0 Smoke Point Tester (Lamp)
Significance of the test:
This test method provides an indication of the relative smoke producing properties
of kerosene and aviation turbine fuels in the diffusion flame. The smoke point is
related to the hydrocarbon type composition of such fuels. Generally, the more
aromatic the fuel the smokier the flame. A high smoke point indicate a fuel of low
smoke producing tendency.
The smoke point (Luminometer number with which it can be correlated) is
quantitatively related to potential radiant heat transfer from the combustion

30. 30
products of the fuel. Because radiant heat transfer exert a strong influence on a
metal temperature of combustor liners and other hot sections of the gas turbine, a
smoke point provide a basis for correlation of fuel characteristic with life of these
component.
Apparatus and materials/Procedure
 Smoke point lamp,
 wick of woven solid circular cotton of ordinary quality,
 Wick tube,
 Candle,
 Sample of kerosene and diesel fuel.
Procedure
 A 126 mm long dried wick is soaked in the sample and placed in the wick tube of
the candle.
 A 10-20 ml of prepared sample is introduced at room temperature into the dry
candle.
 The wick tube is placed in the candle firmly with taking care of the candle air
vent is free from fuel. A new clean, sharp razor is used to cut the wick at the
face of the holder and remove wisps and frayed ends.
 The candle is lighted and the wick adjusted so that the flame is approximately
10 mm high with 5 min.
 After burning, the candle raised until a smoky tail appears, then the candle is
lowered slowly through several stages of flame appear once.
 The maximum height of flame that can be achieved without smoking is
determined to the nearest 0.5 mm.

31. 31
 The candle is removed from the lamp rinse with heptane and purged with air to
make ready for re-use. 9.5 Result and Calculations In this experiment we have
to record the height of the flame, when we raise the candle until a smoky tail
appears then lower the flame slowly until the smoky tail disappears, To
eliminate errors due to parallax, the eye of the observer should be slightly to
one side of the centerline, so that a reflected image of the flame is seen on the
scale on one side of the central vertical white line.
2.7.3 POUR POINT TEST (ASTM D97)
The pour point of a liquid is the temperature at which below the liquid loses its
flow characteristics. In crude oil a high pour point is generally associated with a
high paraffin content, typically found in crude deriving from a larger proportion of
plant material.
Fig 2.7.3.0 Pour Point Tester

32. 32
Procedure
ASTM D97, Standard Test Method for Pour Point of Crude Oils. The specimen is
cooled inside a cooling bath to allow the formation of paraffin wax crystals. At
about 9 °C above the expected pour point, and for every subsequent 3 °C, the test
jar is removed and tilted to check for surface movement. When the specimen does
not flow when tilted, the jar is held horizontally for 5 sec. If it does not flow, 3 °C
is added to the corresponding temperature and the result is the pour point
temperature.
It is also useful to note that failure to flow at the pour point may also be due to
the effect of viscosity or the previous thermal history of the specimen.
Therefore, the pour point may give a misleading view of the handling properties of
the oil. Additional fluidity tests may also be undertaken. An approximate range of
pour point can be observed from the specimen's upper and lower pour point.
2.7.4 ANILINE POINT TEST (ASTM D611)
The aniline point of an oil is defined as the minimum temperature at which equal
volumes of aniline (C6H5NH2) and the lubricant oil are miscible, i.e. form a single
phase upon mixing. The value gives an approximation for the content of aromatic
compounds in the oil, since the miscibility of aniline, which is also an aromatic
compound, suggests the presence of similar (i.e. aromatic) compounds in the oil.
The lower the aniline point, the greater is the content of aromatic compounds in
the oil.
Determination of aniline point is a test to evaluate base oils that are used in oil
mud. The test indicates if oil is likely to damage elastomers (rubber compounds)
that come in contact with the oil. Aniline point of oil gives an indication of the

33. 33
possible tendency of deterioration of oil when it comes into contact with packing,
rubber sealing etc. in general oils with a high aromatic content are more
detrimental to rubber products than those with a low aromatic content. The
relative aromatic content of an oil is indicated by its aniline point and oils with a
high aromatic content have a low aniline point and vice versa. The higher the aniline
point of the oil, the more desirable it is for drilling fluid usage.
The aniline point serves as a reasonable proxy for aromaticity of oils consisting
mostly of saturated hydrocarbons (i.e. alkanes, paraffins) or unsaturated
compounds (mostly aromatics). Significant chemical functionalization of the oil
(chlorination, sulfonation, etc.) can interfere with the measurement, due to
changes to the solvency of the functionalized oil. The aromatic oil with a
75%aromatic content, the aniline point would be between 32.2° and 48.9°C; for
a naphthenic type containing 40% aromatic structures, it would be between 65.6°
and 76.7°C; and for a paraffinic oil with a15% aromatic content it would be
between 93.3° and 126.7°C.
Fig. 2.7.4.1 Aniline Point Tester

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2.8 HUMAN SAFETY AND ENVIRONMENT (HSE).
Safety is the state of being "safe" (from French sauf), the condition of being
protected from harm or other non-desirable outcomes. Safety can also refer to
the control of recognized hazards in order to achieve an acceptable level of risk.
HSE is a very important entity in NNPC, R&D Division. The training involves the
ways to identify the hazards involved at all the project sites, and employs
necessary preventive measure to avert accidents and fatalities and perform
regular site inspection to ensure that the safety guidelines are adhered to. I was
taught how to ensure that the projects are undergone safely and in compliance
with safety policies which are.
1. High-Risk Situations: Do not start up or shut down equipment or
installations without using the appropriate, written operating procedure.
2. Traffic: Do not exceed the speed limit.
3. Body Mechanics and Tools: Do not carry out work if you do not have the
right tools for the job and the environment.
4. Protective Equipment: Do not access installations or perform work without
wearing general or task-specific PPE.
5. Work Permits: Do not perform work without a valid work permit.
6. Lifting Operations: Do not walk or stand under a load while lifting is taking
place
7. Powered Systems: Do not perform work without checking that the power
and product supply has been rendered in-operative.
8. Confined Spaces: Do not enter a confined space until isolation has been
verified and the atmosphere checked.

35. 35
9. Work at Height: Do not work at height without a safety harness when
there is no collective protective equipment.
10. Change Management: Do not make any technical or organizational
changes without prior authorization.
2.8.1 BASIC FIRE FIGHTING
During this industrial training, we had orientation on basic firefighting by Human
Safety and Environment (H.S.E) Department to help improve our H.S.E awareness.
It was also designed to introduce to us the cause of industrial fire, prevention
principles and fighting techniques. The following are some of the basics taught:
SOURCES OF FIRE
 Mechanical heat energy
 Chemical heat energy
 Solar heat energy
 Electrical heat energy
 Nuclear heat energy
2.8.2 FIRE EXTINGUISHER
A fire extinguisher is an active fire protection device used to extinguish or control
small fires, often in emergency situations. It is not intended for use on an out-of-
control fire, such as one which has reached the ceiling, endangers the user (i.e., no
escape route, smoke, explosion hazard, etc.), or otherwise requires the expertise
of a fire department.

36. 36
TYPES OF EXTINGUISHER
 extinguisher that expels water
 extinguisher that expels foam
 extinguisher that expels dry chemical powder
FIRE EXTINGUISHING METHODS
 Cooling: this extinguishment is achieved by temperature reduction or
elimination
 Starvation: this refers to extinguishment by fuel removal
 Smothering: this refers to extinguishment by oxygen dilution
 Flame inhibition: this is extinguishment by flame inhibition
Fire extinguisher can be applied by the PASS method
 P- Pull the pin ; remove the safety pin by pulling the ring
 A- aim the nozzle; energize extinguisher by slightly squeezing the nozzle
 S- squeeze the trigger, this releases the extinguishing agent
 S- sweep from side to side
2.9 SKILLS AND KNOWLEDGE ACQUIRED DURING SIWES PROGRAMME
During my period of industrial attachment NNPC, R&D Division, I had the privilege
to hoard a lot of knowledge, mostly practical and theoretical. The SIWES
programme allowed me the opportunity to put to practice what I’ve been learning
so far as a student in the lecture room. Listed below is a summary of the skills and
knowledge I acquired;
 Knowledge about procedure for crude oil assay
 Whole Crude oil characterization. (I.e.)
i. By D86 Distillation of the crude oil

37. 37
ii. By Atmospheric distillation (ASTM D2982) Distillation Vacuum
distillation (ASTM D526)
iii. Physico-chemical properties of crude oil and products
iv. Analysis of hydrocarbon fraction/cuts
v. Analysis of the overhead gas (off-gases)
 Fuel blending
 Routine checks.
 Theoretical knowledge on major equipments, devices and instruments that aid
crude refining process, their basic operations, common problems, etc. Also,
tutoring on fire and safety in the chemical plant and measures to respond to any
form of emergency or accident.
CHAPTER THREE

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CONCLUSION, PROBLEM ENCOUNTERED AND RECOMMENDATION
3.1 CONCLUSION
The Student Industrial Work Experience Scheme (SIWES) is one of the best
ideas introduced to the university education scheme. Its relevance cannot be over
emphasized. Through the Industrial Training Fund (ITF), the SIWES programme
has shown the importance of the exposure of a student to the Industry, coupled
with the practical knowledge acquired. The programme helps students in several
disciplines of sciences, engineering and technology to experience, learn, practice
and appreciate what they are been taught in their various institutions.
In my Internship with Nigeria National Petroleum Corporation, Research and
Development (R&D) Division, I have acquired a lot of skills related Crude oil Assay
and other auxiliary processes, beyond what I previously known.
The programme has made it possible for me to have of work ethics and to mix up
with other individuals at different levels in their various working place. It exposed
me to unlimited knowledge with regard to activities carried out in my work place.
It is imperative on the part of the Industrial Training Fund (ITF) to put in place
polices to ensure the programme is regulated throughout every tertiary institution
and students benefit from the scheme. As this will go a long way in the boosting of
the Nation’s industry sector for the upcoming young labor force with prior
knowledge of the system, its practice and how to drive the Nation to become self-
sustained and efficient in production.
3.2 PROBLEM ENCOUNTERED

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 Finding a suitable place for the training with current economic situation of
the country.
 Inadequate communication between ITF area office with deployed SIWES
students to firms.
 Non-payment of monthly salary by firm or ITF to aid the student’s
ongoing SIWES programme.
 No supervision visits paid by ITF officials during Industrial training to
assess and aid the deployed SIWES student
3.3 RECOMMENDATION
My recommendations are:
1. Future participant (student) should try to submit their application to relevant
companies as much as possible before the commencement of the training period.
2. The Industrial Training Fund should partner with firms and organizations in the
country to help post students to firms with ease.
3. Students participating should know that the benefit of any industrial training
can be obtained if they are willing to learn from their supervisor and other
professionals.
4. The ITF should also carry out preliminary visit to the firms to ascertain the
operations and working conditions are favorable for an Industrial Trainee
student.
5. Payments of salaries to deployed students should be made to students during
their Industrial attachment, rather than several months after it had been
concluded.