PETROCHEMICALS & PETROLEUM

REFINING TECHNOLOGY

LABORATORY MANUAL

EXPERIMENT 1 DETERMINATION OF FLASH POINT OF PETROLEUM PRODUCTS

EXPERIMENT 2 DETERMINATION OF API GRAVITY
EXPERIMENT 3 DETERMINATION OF VISCOSITY OF OIL
EXPERIMENT 4 DETERMINATION OF REID VAPOR PRESSURE
EXPERIMENT 5 OIL DISTILLATION ACCORDING TO ASTM METHOD

SEMESTER SEPTEMBER 2016

PREPARED BY:

LECTURERS : MS NADIA ISA

MR SYED AZHAR SYED ABD. RAHMAN
MDM NORULAKMAL NOR HADI
DR. NUGROHO DEWAYANTO

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 TABLE OF CONTENT

CONTENT PAGE

1. Introduction 2
2. Laboratory Safety Guidelines 3
3. Safety Declaration Form 7
4. Guidelines for report writing 8
5. Experiment 1 : Determination of Flash Point of Petroleum 12
products
6. Experiment 2 : Determination of Specific Gravity 16
Experiment 3 : Determination of Viscosity of Oil 18
7. Experiment 4 : Determination of Reid Vapour Pressure (RVP) 20
8. Experiment 5 : Oil Distillation according to ASTM Method 25

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 INTRODUCTION

This manual provides laboratory guidelines, safety declaration form, laboratory report format and
experimental procedures for subject of Petrochemical & Petroleum Refining Technology (CPD 20103
for Diploma and CPB 30503 for Bachelor) of Chemical Engineering Technology (Process) .

Students are compulsory to read and understand all the laboratory guidelines provided in this manual.
The safety declaration form should be submitted to the lecturer/instructor/technician before starting
the first experiment.

For the laboratory report format, the report writing guidelines and requirements are provided in order
to produce a good quality of laboratory report.

Upon completion of this course, students will understand the properties that are important in handling
petroleum and natural gas. Students will be able to independently perform accurate quantitative
measurements, interpret experimental results, perform calculations on these results and draw a
reasonable accurate conclusion.

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 LABORATORY SAFETY GUIDELINES
General Guidelines

1. Conduct yourself in a responsible manner at all times in the laboratory.

2. Be familiar with your lab experiment before you come to the lab. Follow all written and verbal
instructions carefully. If you do not understand a direction or part of a procedure, ask the
lecturer/instructor/technician before proceeding.
3. No student may work in the laboratory alone. The lab instructor/lecturer grant exceptions on a
case by case basis.
4. When first entering a laboratory, do not touch any equipment, chemicals or other materials in the
laboratory area until you are instructed to do so.
5. Do not eat, drink beverages or chew gum in the laboratory. Do not use laboratory glassware as
containers for food or beverages.
6. Smoking is strictly not allowed in any indoor area.
7. No music allowed in the laboratory. Radio (including walkman) and other entertainment devices
are not permitted.
8. No cellular phone is allowed in this laboratory.
9. Perform only those experiments authorized by the lecturer/instructor/technician. Never do
anything in the laboratory that is not called for the laboratory procedures or by your
lecture/instructor/technician. Carefully follow all instructions, both written and oral.
Unauthorized experiments are prohibited.
10. Observe good housekeeping practices. Work areas should be kept clean and tidy at all times.
11. Horseplay, practical jokes, and pranks are dangerous and prohibited.
12. Bring only your laboratory manual, worksheets and report to the work area. Other materials
(books, purses, backpacks, etc) should be stored in the cabinet.
13. Know the locations and operation procedures of all safety equipment including the first aid kit,
eyewash station, safety shower, spill kit and fire extinguisher.
14. Be alert and proceed with caution at all times in the laboratory. Notify the lecturer/instructor
immediately of any unsafe condition you observe.
15. Label and equipment instructions must be read carefully before use. Set up and use the
prescribed apparatus as directed in the laboratory instructions provided by your
lecturer/instructor.
16. Experiments must be personally monitored at all times. You will be assigned a laboratory station
at which to work. Do not wander around the room, distract other students or interfere with
laboratory experiments or others.
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17. Defeating safety devices or using equipment in a manner other than that which is intended will
be grounds for dismissal from the lab.
Clothing

1. Safety goggles and safety jacket must be worn whenever you work in lab.
2. Gloves should be worn whenever you use chemicals that cause skin irritations or need to handle
hot equipment.
3. Mask should be worn every time you prepare the chemicals.
4. Safety shoes and hard hat should be worn at all times while in the laboratory.
5. Contact lenses should not be worn in the laboratory unless you have permission from your
instructor.
6. Dress properly during a laboratory activity.
7. Long hair, dangling jewellery and loose or baggy clothing are a hazard in the laboratory. Long
hair must be tied back and dangling jewellery and loose or baggy clothing must be secured.
8. Sandal, open-toed shoes, high heels or shoes with holes in the sols will not be worn in the lab.
9. Shorts and skirts are not permitted.
10. Instructor and laboratory assistant have a right dismiss to you from the laboratory if they found
that you are not wearing proper safety clothing.

Handling of Chemicals

1. Treat chemicals with respect and understand the chemicals you are using with Material Safety
Data Sheet (MSDS). The MSDS are available in the analytical room.
2. All chemicals in the laboratory are to be considered dangerous. Do not touch, taste or smell any
chemical unless specifically instructed to do so.
3. Check the label on chemical bottles before removing any of the contents. Take only much
chemical are you need. Smaller amounts often work better than larger amounts.
4. Label all containers and massing papers holding dry chemicals.
5. Never return unused chemicals to their original containers.
6. Never use mouth suction to fill a pipette. Use pipette bulb or pipette filler.
7. Acids must be handled with extreme care. Always add acids slowly to water, with slow stirring
and swirling, being careful of the heat produced, particularly with sulfuric acid.
8. Handle flammable hazardous liquid over a pan to contain spills. Never dispense flammable
liquids anywhere near a flame or source of heat.
9. Never take chemicals or other materials from the laboratory area.

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10. Take good care when transferring acids and other chemicals from one part of the laboratory to
another. Hold them securely and in the method demonstrated by the instructor as you walk.
11. All wastes generated during the course of an experiment must be disposed of according to the
lab instructor’s directions.
12. Never mix chemicals in sink drains.
13. Sinks are to be used only for water and those solutions designated by the instructor.
14. Solid chemicals, metals, matches, filter paper, and all other insoluble materials are to be disposed
of in the proper waste containers, not in the sink.
15. Checks the label of all waste containers twice before adding your chemicals waste to the
container.
16. Cracked or broken glass should be placed in the special container for “broken glass”.
17. Keep hands away from your face, eyes, mouth and body while using chemicals. Wash your
hands with soap and water after performing all experiments.

Accidents and Injuries

1. Report any accidents (spill, breakage, etc) or injury (cut, burn, etc) to the lecturer/
instructor/technician immediately, no matter how trivial it may appear.
2. If you or your lab partners are hurt, immediately tell to the instructor.
3. If a chemical should splash in your eye(s), immediately flush with running water from the
eyewash station for at least 20 minutes. Notify the instructor immediately.
4. Spills should be cleaned up immediately.

Handling Glassware and Equipment

1. Inserting and removing glass tubing from rubber stopper can be dangerous. Always lubricate
glassware (tubing, thistle tubes, thermometer, etc) before attempting to insert it in a stopper.
Always protect your hands with tower or cotton gloves when inserting glass tubing into, or
removing it from a rubber stopper.
2. When removing an electrical plug from its socket, grasp the plug, not the electrical cord.
3. Hands must be completely dry before touching an electrical switch, plug or outlet.
4. Examine glassware before each use. Never use chipped or cracked glassware.
5. Never use dirty glassware.
6. Do not immerse hot glassware in cold water; it may shatter.
7. Report damaged electrical equipment immediately. Look for things such as frayed cords,
exposed wires and loose connections. Do not use damaged electrical equipment.
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8. If you do not understand how to use a piece of equipment, ask the instructor for help.
9. Be careful when lifting heavy objects. Lift comfortably, avoid unnecessary bending, twisting,
reaching out and excessive weights, lift gradually and keep in good physical shape.
10. Do not transfer glassware from one laboratory to another without permission from instructor.

Heating Substances

1. Do not operate a hot plate by yourself. Take care that hair, clothing and hands are a safe distance
from the hot plate at all times. Use of hot plate is only allowed in the presence of the
lecturer/instructor/technician.
2. Heated glassware remains very hot for a long time. They should be set aside in a designated
place to cool and picked up with caution. Use tongs or heat protective gloves if necessary.
3. Never look into a container that is being heated.
4. Do not place hot apparatus directly on the laboratory desk. Always use an insulated pad. Allow
plenty of time for hot apparatus to cool before touching it.
5. If leaving a lab unattended, turn off all ignition sources and lock the doors.

Ended the Experiments

1. At the end of the laboratory sessions, you should:

a) Shut off main gas outlet
b) Turn off the water inlet
c) Desk top, floor area and sink are clean
d) All equipment is cool, clean and arranged

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 SAFETY DECLARATION FORM

The Dean/Head of Campus

Universiti Kuala Lumpur
Malaysian Institute of Chemical and Bioengineering Technology
Lot 1988, Vendor City Industrial Area
Taboh Naning, 78000 Alor Gajah
Malacca

Dear Sir,

SAFETY DECLARATION
(Subject: PETROCHEMICAL & PETROLEUM REFINING TECHNOLOGY CPD 20103)

I ………………………………..…………………………………………………………. ID No
………………………. declare that I have read and understood the safety rules and regulations in
UniKL MICET. I hereby agree to abide by all the rules and regulations stated in the safety guidelines.

2. I hereby understood the contents and will disciplinary action will be taken against me, if I do not
abide by the stated rules.

3. I am fully responsible for all my actions during laboratory sessions.

Thank you.

Yours faithfully,

……………………………….
Name:
Matrix No:
Date:

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 GUIDELINES FOR REPORT WRITING

This information applies particularly to your Lab Report, and in general to all technical reports you
write thereafter.

The readership (or audience) for a technical report

Before writing a report, you must consider to whom it is addressed. For example, report “A” aimed at
a higher level of management to help them make a major decision needs a different approach
(exceptionally clear statements of the main points only, omitting most of the detail, and making
recommendations) from report “B” which serves to record some stage of work on the development of
a product and is intended for engineers at a level in the organization similar to the author’s (clarity
still very important but also some detailed discussion). Whatever the intended audience, tell them
what they need to know, based on their knowledge and interest, not a “history” of what you did. As
students, you will have to imagine an audience, which is not easy until you have some experience.
Since the CLD20402 course may possibly be your first opportunity to write an engineering report, we
ask you only to assume an audience with the same level of technical knowledge as you have at the
time of doing the experiment. However, remember that short reports are more likely to be read than
long ones containing too much detail.

Structure of a report

Organizations often have their own standard styles for the layout of reports, but they tend to differ
only in detail. A very common arrangement of the sections of a report is as follows.

Title Page Template as given by lecturer.

Summary A short (no more than 200 words) self –contained summary of the whole report
saying what was done and why, then giving the main results and conclusion. Purposes
are (i) to summarize the work for those who have no need or are to busy to read the
whole report, (ii) to provide an overview before reading the body of the report and a
reminder of the work some time later, (iii) for anyone not originally the recipient of
the report but searching for information on the broad topic, to indicate whether the
report is worth reading. Sometimes called Abstracts or Synopsis; this is arguably the
most important part of a report.

Introduction Content depends on the audience, but essentially gives the background to the work,

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 the objectives and perhaps a brief indication of what is dealt with in each of the
subsequent sections. Often, Objectives will be a separate section following the
Introduction.

Theory Depends on the topic of the report. May not be necessary but if it is, try to devise a
more helpful heading. Subsections, with appropriate subheadings e.g. “Operating
principal of a steam engine”, may be necessary.

Materials & Methods Includes brief descriptions of the materials, equipments and instrumentations, the
conditions chosen e.g. fluid flow rates, and the measurement procedure adopted (what
was recorded, at what intervals etc.); splitting this into subsections may be helpful.
Another subsection could describe how the measured data were processed to obtain
the required results; you may consider this to be “theory” but beware of describing it
before you have told the reader what was measured.

Results Should concentrate on the processed results; the reader will have been told,
algebraically how you arrived at them, in Experiment or Theory Section, and will not
be interested in all the arithmetic! (if you wish to give one example of a calculation,
put it into an Appendix.) More informative section and / or subsection titles are
helpful. The estimates uncertainty in each measured quantity) should be quoted here,
but the actual “error analysis” is best in a separate section or subsection or even
Appendix.
Tabulated and graphically-presented results should be introduced with appropriate
text, e.g. “…..is shown in Fig. 4…”or “It can be seen from the lower curve in Fig. 3
that…….” The same information does not need to be presented in both a table and
graph; use one or the other. Graphs are often more effective than tables.

Discussion Compare results with expectation, other related cases, previous experiments,
analytical or computational results; consider the implications, etc – whatever is
appropriate. Often included in the Results section as an alternative to a separate
section.

Conclusions An essential section; worth a lot of care in writing since it is likely to be the most read
section after the summary. Used to summarize the principal findings of the work and
to assess the success in meeting the stated objectives.
Try to keep it short and “punchy” and to be quantitative (e.g. “…was within 2% of
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 …..”, not “ ….was very close to…”). You should not introduce here any material
which has not been mentioned earlier in some form, under Results or Discussion.

Recommendations Common in industrial reports, to suggest further action; may be included instead in
the Conclusions section. Student sometimes use it to suggest improvements in
apparatus or measurement procedure, which is valid for experiments intended mainly
to reinforce lecture material; however such sections are best suited to reports on open
experiments.

References A list of any books, reports, journal articles, conference paper etc. which have been
explicitly quoted in the main text of the report, for a specific purpose. The reference
sections would then contain the item “[2] Smith J.M and Van Hess H.C., Introduction
to Chemical Engineering Thermodynamics, McGraw Hill, New York 2001, p.229”.
The number [2] would mean that this is the second reference cited in the text and the
item would appear second in the Reference list.

Appendices Includes the data sheets for each experiment. In addition, for information which is too
detailed to interest most readers, but could be relevant to some. Putting such material
in Appendix improves the readability of the report. Appendices are not for material
which is central to the message of the report.

Tables All tables should have a “caption” consisting of a Table Number followed by a
helpful title. Table 1 would be the first one to be quoted in the text, e.g. “all relevant
dimension of the engine is given in table 1”.

Figures Block diagrams of apparatus, graphs of results all count as “Figures” and should be
quoted in the text by number. For example, Figure 1 might be a diagram of an
equipment and Figure 2 and 3 graphs of processed results. The “rules” above
regarding tables apply equally to figures.

10
Numbering of Sections

Readers can “navigate” in a short report without the need for section numbers, but it is
generally helpful to use a numbering system as illustrated in the following examples of a contents list.

Summary

1. Introduction and theory

2. Experiments

2.1 Apparatus

2.2 Procedure

3. Results

3.1 ………. (Subsections dealing with distinct parts of the work)

3.2………..

4. Discussions

5. Conclusions

6. References

Appendices

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EXPERIMENT 1
DETERMINATION OF FLASH POINT OF PETROLEUM PRODUCTS

OBJECTIVES:

The objectives of the experiment are:

1. To find the flash point of petroleum products

2. To compare the flash points of different petroleum products
3. To compare the actual flash point with expected flash point

OVERVIEW

The ISL FP170 5G Analyzer has been designed for the automatic determination the Pensky Martens
Closed Cup Flash Point of petroleum products. The flash point of a material is an indication of its
volatility.

INTRODUCTION

Volatility is the primary characteristics of liquid petroleum products. The liquid petroleum products
are also characterized by their vaporizing tendencies such as gasoline, kerosene and aviation fuel. The
knowledge of flash point is related to the vapor tendency of the petroleum product. The flash point of
a petroleum product is the temperature to which the product must be heated under the specified
conditions of the method to give off sufficient vapor to form a mixture with air that can be ignited
momentarily by a specified flame.

From the viewpoint of safety, flash points are of most significance at or slightly above the maximum
temperatures (30-60°C) that may be encountered in storage, transportation and use of liquid petroleum
products, in either closed or open containers. In this temperature range, the relative fire and explosion
hazard can be estimated from the flash point. For products with flash point below 40°F special
precautions are necessary for safe handling.

The flash point of a petroleum product is also used by manufacturer and marketers of petroleum
products to detect contamination. A substantially lower flash point then expected for a product is a
reliable indicator that a product has become contaminated with a more volatile product, such as
gasoline. The flash point is also an aid in establishing the identity of a particular petroleum product.

PRINCIPLE OF OPERATION

A 75-ml sample is heated at a slow constant rate (5 to 6°C/min - 9 to 11°F/min) with continual stirring
in a closed brass test cup of dimensions specified by the standard method. The first test temperature is
determined from the Expected Flash Point entered by the operator. When the first test temperature is
reached, the ignition source (the test flame or the glow plug) is applied by opening the shutter of the
test cup cover and dipping the igniter into the vapor space at the top of the test cup. The igniter is
subsequently applied at the correct frequency until the vapor above the sample ignites. Stirring is
discontinued during application of the igniter. The operator can also run a non-standard flash point
test on the FP170 5G.

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THE APPARATUS

The ISL FP170 5G is compact and self contained. It can be divided into 2 parts, the control unit and
the test unit.

Control Unit

The Control Unit contains control logic boards, servo motors and also:

In the front side

- The screen,
- The keypad,
- Contrast and brightness adjusting knobs,
- Test flame and pilot light adjusting knobs,

In the back side

- The external link connectors (Printer, RS 232C / Current Loop, ALAN...)
- The mains connector and the ON/OFF switch.
- Gas alimentation nozzle.

In the lateral right side or «Connection panel»

- The connectors of the sample temperature probe, the flash detection device and the igniter.
- Gas supply connecting tubes,
- Test and stirring transmission arms housing.

The test arm has a double function: opening the test cover shutter and tip up the igniter in the test cup.
Both these arms are presented automatically during testing and are retracted into their control unit
housings at the end of testing.

Test Unit

The Test Unit containing the elements specific to the Pensky-Martens flash point method:
- The heating block - with recess (or well) to receive the test cup - and rapid cooling system,
- The standby support for the test cover (it can also receive the test cup),
The test cup and test cover with its accessories are, of course, placed in the test unit during test
running. The test cover accessories include:

EXPERIMENT
MATERIALS:

1. Kerosene
2. Diesel

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PROCEDURE:

Preparation:

1. Tests should be performed in a draught-free room or compartment. If the Analyzer is

equipped with the anti-draught shield accessory, put it in place before starting the test.
2. Make sure that the Analyzer is supported on a level, steady surface.
3. Thoroughly clean and dry all parts of the cup and its accessories before starting the test. Take
particular care to avoid the presence of cleaning agents/solvents used after a previous test.

Test:

1. Fill the test cup with the test specimen to the filling mark inside of the test cup. If too much
specimen has been added, use a syringe or similar device to remove the excess.
2. Place the cup in the heating block. The 2 protruding notches of the heating block are used as
guides for the 2 slots on the top rim of the cup.
3. Place the test cover on the test cup.
4. Turn the cover handle clockwise to block the assembly in position. Make sure that the locking
device is correctly engaged.
5. Place the stirring transmission arm manually on the cover.
6. Connect up the flash detector and the sample temperature probe and insert the probe into its
holder in the test cover, if it is not already in its test cover support.

Test Starting:

1. Select <Run menu>

2. Fill in Sample ID, Sample no, and EFP
3. Select <RUN START>
4. Wait until flash point is detected.
5. Record the reading.

Test Stop:

1. When the Flash Point is detected, an intermittent audio alarm is triggered. To stop the alarm
press the «STOP ALARM» button on the keyboard. The "End of test" screen will be
displayed.
2. Select <Quit>. Quitting gives a screen that is similar to the "Test running" screen and is called
the "End of test" screen.

Cleaning:

1. Turn the handle of the test cover anti-clockwise to unlock it.

2. Remove the cover (with the probe in its holder) and place it in the standby holder provided.
3. Carefully remove the cup and its contents.
4. Clean the cup, the test cover and all accessories with a suitable cleaning agent.

In general, all dirty accessories, including the test flame nozzle that might affect the test run result
should be cleaned.

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TUTORIAL

1. What are the expected flash point of diesel and kerosene?

2. What are the actual flash point of diesel and kerosene?
3. Is there any difference between expected and actual flash point of the samples? Discuss.
4. What are the importance of flash point to petroleum products?
5. If you have a sample of unknown and from the flash point test rig, you find out that the flash
point is 40oC, what could the material be?

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EXPERIMENT 2
DETERMINATION OF API GRAVITY

OBJECTIVES:

1. To determine specific gravity of oil using hydrometer and density meter.

2. To compare specific gravity and API gravity of different oils.

INTRODUCTION

Specific gravity () is defined as the ratio of the weight of a volume of the liquid to the weight of an
equal volume of water at the same temperature. The specific gravity of liquid in the oil industry is
often measured by some form of hydrometer that has its special scale. The American Petroleum
Institute (API) has adopted a hydrometer for oils lighter than water for which the scale, referred to as
the API scale, is

141.5
API   131.5


The most commonly used methods for determining density or specific gravity of a liquid are:

1. hydrometer
2. density meter.

The hydrometer is usually used for determining oil gravity in the oil field. When a hydrometer is
placed in oil, it will float with its axis vertical after it has displaced a mass of oil equal to the mass of
hydrometer. The hydrometer can be used at atmospheric pressure or at any other pressure in a
pressure cylinder.

The portable density meter is an accurate tool to determine the density of the sample. Density is
measured by a hollow, oscillating U-tube. The frequency of vibration of the U-tube is directly related
to the density of the liquid sample. Temperature is measured at the same time, and the instrument
automatically performs the temperature correction.

APPARATUS

The DMA 35N handheld digital density meter defines the state of the art of portable density
measurement. It had been designed for use in the most demanding industrial environments. The DMA
35N will give the density, specific gravity or % concentration of the sample by simply press the lever
on the built-in pump and within seconds the results are shown on the large, bright display. The DMA
35N consists of three main parts:

 An RS 232 interface with infrared data port

 A rubber shock protector
 Elongated filling tube
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MATERIALS:

1. Lubricating oil
2. Diesel
3. Kerosene
4. Petrol

EXPERIMENT 2A: DETERMINATION OF SPECIFIC GRAVITY USING HYDROMETER

PROCEDURE:

1. Pour the sample into the dry measuring cylinder, filling the cylinder approximately 3/4 full.
2. Allow any air bubbles that are deep in the liquid to rise to the surface.
3. Lower the hydrometer gently into the sample.
4. Stir the sample gently by raising and lowering the hydrometer.
5. Allow the hydrometer to come to rest, but not touching the side of the cylinder. If it moves to
the side, move it back to the center of the liquid and spin it gently.
6. When the hydrometer is floating freely at rest, read it to the nearest scale division. Have your
eye slightly below the level of the liquid, and raise it slowly until the surface of the liquid
appears to be a straight line across the hydrometer scale. Record the reading of density to the
nearest scale.

EXPERIMENT 2B: DETERMINATION OF SPECIFIC GRAVITY USING DENSITY

METER

PROCEDURE:

1. Introduce 2 to 5 ml of sample into the instrument by pushing and releasing the pump button.
2. After a few seconds, read the result (density) from the large digital display. (Make sure there
is no bubbles in the tube).

TUTORIAL:

1. Calculate the API gravities of each sample.

2. What does the specific and API gravities indicate?
3. Compare the findings of API results for each sample with the flash point, RVP and other
properties.

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EXPERIMENT 3
DETERMINATION OF VISCOSITY OF OIL

OBJECTIVES:

1. To determine the viscosity and torque of oil using viscometer.

2. To compare the viscosity of different type of oils.

INTRODUCTION

Viscosity is defined as the resistance of a fluid to flow and is measured as the ratio of the shearing
stress to the rate of shearing strain. Two types of fluid characterizations are:

1. Newtonian (true fluids) where the ratio of shear stress to shear rate or viscosity is constant,
e.g. water, light oils, etc. and
2. Non-Newtonian (plastic fluids) where the viscosity is not constant, e.g. drilling mud, colloids,
etc.

In the oil industry viscosity generally is expressed in centipoises, cp (1 cp=10-3 Pa-s).

Figure 1 Shear stress vs. shear rate for a Newtonian fluid.

APPARATUS

Viscostar Viscometers measure both viscosity of Newtonian and non-Newtonian liquids by measuring
the rotation resistance of a cylinder or spindle immersed into the liquid of interest. The resulting
resistance or torque is the measurement of the flow or rotational viscosity of the product. As the
resistance or torque increases, it is indicative of an increasing viscosity. Taking into account the speed
and spindle characteristics, a torque is calculated to provide a direct read-out of viscosity in either cP
or mPa.s.
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EXPERIMENT

MATERIALS:

5. Lubricating oil
6. Diesel
7. Kerosene
8. Petrol

PROCEDURE:

1. Pour the sample into the beaker.

2. Assemble the LV spindle no. 1 onto the viscometer.
3. Level the viscometer and lower the spindle into the sample until the surface of sample level
with the groove marked on the spindle. The spindle should be placed at the centre of the
beaker. Check the level of viscometer again.
4. Stir the sample for about 5 seconds at 10 RPM.
5. Wait for the dial reading to stabilize (the time depends on the sample's characteristics).
6. Record the dial reading (% torque) and viscosity.
7. Repeat with other different speed at 20, 30, 50, 60 and 100 rpm.
8. Repeat step 1 to 8 for LV spindle no. 2, 3 and 4.

Tutorial

1. Discuss the relationship between petrol, kerosene, lubricating oil and diesel.
2. Compare the findings (viscosity & torque) with naphtha.

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EXPERIMENT 4
DETERMINATION OF REID VAPOR PRESSURE

OBJECTIVES:

The objectives of the experiments

1. To determine the Reid vapor pressure of petroleum products

2. To compare the Reid vapor pressure of different petroleum products

INTRODUCTION

The volatility characteristics of petroleum fuels are very important especially for gasoline. Motor and
aviation gasoline are manufactured as liquids but they are consumed in the vapor phase.
Consequently, gasoline volatility must be high enough to assure acceptable engine start-up, warm-up,
acceleration and throttle response under normal driving (or flying) conditions. On the other hand, the
maximum volatility of a gasoline must be restricted to avoid vapor lock, vaporization losses, air
pollution, and unsafe storage and handling. The volatility considerations for other transportation fuels
like kerosene and diesel are, to some extent, similar to those for gasoline. The Reid vapor pressure
(RVP) is frequently used as an indication of volatility of liquid hydrocarbons. The RVP is defined as
the absolute pressure (i.e., psia or bar) exerted by a mixture, determined at 100 ºF (37.8 ºC) and at a
vapor to liquid ratio of 4. This is different than the true vapor pressure which is defined as the
pressure of a vapor in equilibrium with its condensed phase at a specific temperature. Although the
RVP provides a convenient approximation of the absolute vapor pressure of a partly vaporized sample
at 100 °F, it is not equivalent to the true vapor pressure. In general, RVP is lower than the true vapor
pressure due to some small sample vaporization and the presence of water vapor and air in the
confined space. The apparatus and procedures for determining the RVP are standardized and specified
in ASTM method D-323 and IP- 402 [1]. The Reid vapor pressure test is widely used as a criterion for
blending gasoline and other petroleum products. Once RVP of a fuel is known the methods provided
in the API-TDB [2] can be used to estimate true vapor pressure of a fuel or a crude oil at any desired
temperature. True vapor pressure is an important thermodynamic property related to volatility and
phase equilibrium calculations. There are a number of methods for estimating the vapor pressure.

When a pure liquid is placed in an evacuated bulb, molecules will leave the liquid phase and enter the
gas phase until the pressure of the vapor in the bulb reaches a definite value, which is determined by
the nature of the liquid and its temperature. The equilibrium vapor pressure is independent of the
quantity of the liquid and vapor present as long as both phases exist in equilibrium with each other at
the specified temperature. As the temperature is increased, the vapor pressure also increases to the
critical point, at which the two-phase system becomes a homogeneous, one-phase fluid. If the pressure
above the liquid is maintained at a fixed value (say by admitting to the bulb containing the liquid),
then the liquid may be heated up to a temperature at which the vapor pressure is equal to the external
pressure. At this point vaporization will occur by the formation bubbles in the interior of the liquid as
well as at the surface; this is the boiling point
of the liquid at the specified external pressure is seen to be identical with the variation of the vapor
pressure with temperature.

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THE APPARATUS

Reid Vapour Pressure (ASTM D323) apparatus consists of two chambers (Figure 1); a vapour
chamber (upper section) and a liquid chamber (lower section), pressure gauges and a water bath
(Figure 2).

Test Unit

1. Vapour Chamber (Upper section)

- A cylindrical vessel with inner surfaces of the ends slightly sloped to provide complete
drainage from the either end when held in a vertical position. On one end of the vapor
chamber, a gauge coupling is provided to a gauge connection. In the other end of the
vapor chamber, an opening is provided for coupling with the liquid chamber.

2. Liquid Chamber (Lower section)

- A cylindrical vessel with inner surface of the coupling end is sloped to provide complete
drainage when inverted. In one end of the liquid chamber an opening is provided for
coupling with the vapor chamber. The other end of the chamber shall be completely
closed.

Note: To maintain the correct volume ratio between the vapor chamber and the liquid chamber, paired
chambers shall not be interchanged without recalibration to ascertain that the volume ratio is within
the required limits.

Figure 1: Vapour Pressure Apparatus

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3. Pressure Gauge

- The range and graduations of the pressure gauge shall be governed by the vapor pressure
of the samples being tested in accordance with Table 1. When the gauge reading differs
from the pressure measuring device reading or dead weight tester reading when testing
gauge above 180kPa (26psi), by more than 1% of the scale range of the gauge, the gauge
shall be considered inaccurate.

Table 1 : Pressure Gauge Range and Graduations

4. Water Bath

- A large chamber where the vapor pressure apparatus can be immersed horizontally to at
least 1inch above the top of the vapor chamber. The water bath should be maintained at a
constant temperature of 37.8oC (100oF).

- The vapor pressure apparatus shall rotate at its axis 350o in one direction and then 350o in
the opposite direction in repetitive fashion.

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 Figure 2 : Water Bath

EXPERIMENT

MATERIAL

1. Diesel
2. Kerosene / Petrol
3. Lubricating oil

PROCEDURE

Preparation of the vapor pressure apparatus

1. Fill up the liquid chamber with oil sample (Diesel).

2. Assemble the liquid chamber to the vapour chamber together with a transducer connector.
3. Fill up the water bath with ¾ water.
4. Swith on the main plug and the machine.
5. Press the ‘HEAT’ and ‘START’ button on the bath control unit and wait for the bath
temperature reaches 37.8oC.
6. Assemble the vapour pressure apparatus into the water bath. Make sure the vapour pressure
apparatus is immersed completely (1inch above the vapour chamber).
7. Press the ‘TEST’, ‘STIRRER’ and ‘START’ button on the bath control unit.
8. Wait for the pressure readings to be stable or 5 minutes until the readings stabilized.
9. Record the results from the pressure digital meter (kPa/psi).
10. Repeat step 1 until 9 for different type of oil (diesel, kerosene/petrol, lubricating oil).

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Shut Down

1. Press ‘TEST’, ‘STIRRER’, ‘HEAT’ and ‘START’ button on the bath control unit. (Make sure
to follow the sequence).
2. Turn off the machine.
3. Release the water in the water bath.
4. Switch off the main plug.

TUTORIAL

1. What is the difference between Reid Vapour Pressure (RVP) and True Vapour Pressure
(TVP)?
2. Discuss the relationship of Reid Vapour Pressure (RVP) between diesel, kerosene, petrol and
lubricating oil.
3. Discuss the effects of Reid Vapour Pressure (RVP) on engine performance.

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EXPERIMENT 5
OIL DISTILLATION ACCORDING TO ASTM METHOD

OBJECTIVES
The objectives of the experiment are:

1. To determine the percentage of distilled amount against temperature of petroleum product

sample.
2. To determine the initial and final boiling points of petroleum sample.
3. To determine the quantity of various fractions of petroleum sample.

INTRODUCTION

ASTM Distillation is the most common method for obtaining distillation data (volume % distilled vs
temperature) of gasoline, naphtha, kerosene and gas oil. In ASTM distillation, 100 ml of sample is
distilled at uniform rate of 5ml per min, the distillate is condensed. The temperature of the vapour
when the first drop of condensate dripped from the condenser is recorded as the initial boiling point
(IBP). The vapour temperature is also recorded as each successive 10% is collected. When 95% has
been distilled, the burner flame may need to be increased and the maximum temperature is recorded
as the final boiling point (FBP). FBP is an important specification or way of describing gasoline,
naphtha or middle distillates.

Definitions:

Final Boiling Point (FBP) : The maximum thermometer reading obtained during the test. Usually
occurs after the evaporation of all liquid from the bottom of the flask.

Initial Boiling Point (IBP) : The temperature at the instant the first drop falls from the lower end of the
condenser tube.

Percentage Residue : Percentage volume of residue left in the flask (measured in accordance with the
standard in a 5ml flask).

Percentage Recovery : Volume measured after 2 minutes interval to successive observations agree
(measured in accordance with standard method).

Total Percentage Recovery : Combination of percent recovery and percent residue in the flask. Deduct
from 100 to obtain percentage loss.

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APPARATUS

The Distillation Unit D86 07 has been designed to cover the atmospheric distillation of petroleum
products using a laboratory batch distillation unit to determine quantitatively the boiling range
characteristics of such products such as light and middle distillates, automotive spark ignition engine
fuels, aviation gasolines, aviation turbine fuels, naphthas, kerosene and many more. Temperatures and
volumes of condensate and times are systematically recorded. The distillation (or volatility)
characteristics are calculated from the resulting data and are in turn used to determine the safety and
performance of the sample. Figure 1 shows the assembly of the apparatus.

Figure 1 : Apparatus Assembly

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MATERIAL

100ml Petrol

PROCEDURE

Preparation of the analyzer and apparatus

1. Fill up the distilling flask with 100ml of oil sample. (Be caution)

2. Place the distilling flask in the cabinet compartment. Make sure the heating flask support
platform is the correct one.

3. Place the measuring cylinder on the block support.

4. Switch ON the POWER. (Make sure the water bath temperature is stable at ambient
temperature).

5. Control the HEATER POWER starting with 10%-20% for about 5-10 minutes until the
sample starts to boil.

6. Once the first drop of liquid or can be referred to Initial Boiling Point (IBP) of the sample
starts to drop, record the TIME (min), record the TEMPERATURE (oC) of the sample being
distilled and record the VOLUME (ml) collected in the measuring cylinder.

7. Repeat Step 6 at every collected VOLUME of sample from 10ml until it reaches the Final
Boiling Point (FBP).

8. Wait until the sample distilled completely recovered. Record the FBP.

9. Control the HEATER POWER regularly (only if the sample starts to slowly boil further).
Slowly reduce the heater power when the distillation process complete.

10. Wait for the equipment to cool down. Slowly remove the distilling flask (ask for technician’s
help).

11. Record all the data as stated in the tutorial section.

TUTORIAL

1. Measure the percentage recovery (sample being distilled) in the measuring cylinder.

2. Measure the percentage residue.

3. Calculate the total percentage recovery and total percentage loss.

4. Plot graph volume % distilled (percentage recovery) versus temperature of distillation.

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REFERENCES

1. User’s Manual Herzog ASTM D86 07.

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