Page 1 from 30 pages Prof. Dr.

Elshafie Gad
Experiments of Petroleum Course

Prof. Dr. Elshafie A. M. Gad

Chemistry Department

College of Applied Sciences

Um-Ulqura University
Page 2 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
Contents

1. Standard Test Method for API Gravity of Crude Petroleum and Petroleum
Products ASTM D 287-92

2. Standard Test for Refractive index of hydrocarbon liquids ASTM D1218-92 (re-
approved 1998)

3. Standard test method for distillation of petroleum products at atmospheric

pressure (ASTM D 86-99a / IP 123/99)

4. Standard test method for distillation of petroleum products at reduced pressure

(ASTM D 6611-99 (

5. Standard test method for Calculating Viscosity Index from Kinematic Viscosity
at 40 and 100 oC ASTM D 2270-93 / IP 226/91 (95)

6. Standard Test Method for Smoke Point of Kerosene and Aviation Turbine Fuel
ASTM 1322-97 / BS 2000: Part 57 1995/ IP 57/95

7. Standard Test for Pour point of Petroleum Products ASTM D 5853-95 / IP

441/99 (95)

8. Standard Test Method for Aniline point of Petroleum Products and hydrocarbon
solvents ASTM D 611-82

9. Standard Test Method for Flash Point by Pensky-Martens Closed Cup Tester
(ASTM D 93-99c / IP 34/99)

10. Standard Test for Water in Crude Oil by Distillation ASTM4006-81/ IP 368/97

11. Standard Test Method for Sulfur in Petroleum Products (Lamp Method) ASTM
D6611 -98

12. Standard Test Method for Saybolt Color of Petroleum Product (Saybolt
Chromometer Method) ASTM D156-94
Page 3 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course

1. Standard Test Method for API Gravity of Crude Petroleum

and Petroleum Products
ASTM D 287-92
IP 189/98 IP 190/98
BS 2000: Part 189-190 1998

General scope
Absolute density: the unit block sizes for a particular substance at a given
temperature and unity g/cm3

Specific Gravity: the absolute density of matter is divided by the density of

water at the same temperature

This method depends on determination of API Gravity of a crude oil and its
derivatives that have a liquid vapor pressure (180 kPa) or (26 Psi) or less using
API gravimeter at a temperature of 15.5 oC (60 oF). The American Petroleum
Institute adopted the temperature 60 oF equivalent to 15.5 oC to measure the
density of petroleum products and therefore remember 60/60 in most scientific
journals. To convert temperature from Celsius to Fahrenheit and vice versa
9
o
F o C   32
5
5
o
C  ( o F - 32 ) 
9

API Gravity
141.5
API Gravity   131 .5
sp. g. @ 60
60
Page 4 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
Crude petroleum oil can be classified according to the API gravity as follows:
1. Heavy oil has values less than 20 oAPI.
2. Medium oil lies in the range between 20 and 30 oAPI.
3. Light oil has values more than 30 oAPI.

Instruments:
 API gravimeter (see Figure 1)
 Glass cylinder (2.5 cm diameter)

Procedure

1. Adjust the temperature of the sample:

2. Transfer the oil sample to be measured to Tester measurement with

avoid having air bubbles or evaporation of light components,
taking into account that the ambient temperature no more than ± 2
° C of the temperature of the sample.

3. Put gently API gravimeter in the sample.

4. Record the point where API gravimeter is free float on the surface
of the sample

Figure 1
Page 5 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
API gravity
Page 6 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
2. Standard Test for Refractive index of hydrocarbon liquids.
ASTM D1218-92 (re-approved 1998)

Refractive index is an important property of liquids to signify purity.

Refractive index definition: the refractive index or index of

refraction n of a substance (optical medium) is a dimensionless
number that describes how light, or any other radiation, propagates
through that medium. It is defined as

where c is the speed of light in vacuum and v is the speed of light in

the substance. For example, the refractive index of water is 1.33,
meaning that light travels 1.33 times slower in water than it does in
vacuum.
Page 7 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
Apparatus:
Abbe refractometer device is used to determine the refractive index, It consists
of a number 2 glass prism to break the light beam and two lenses to assemble
the light beams.

Abbe Refractometer

Refractive index of some solvents

2,2,4 trimethylpentane nD = 1.3900
Methylcyclohexane nD = 1.4200
Toluene nD = 1.4900
Page 8 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course

3. Standard test method for distillation of petroleum products

at atmospheric pressure
ASTM D 86-99a / IP 123/99

Scope

This test method covers the atmospheric distillation of petroleum

products using a laboratory batch distillation unit to determine
quantitatively the boiling range characteristics of such products as
light and middle distillates, automotive spark-ignition engine fuels,
aviation gasolines, aviation turbine fuels, 1-D and 2-D regular and
low sulfur diesel fuels, special petroleum spirits, naphthas, white
spirits, kerosines, and Grades 1 and 2 burner fuels.
The test method is designed for the analysis of distillate fuels; it is not
applicable to products containing appreciable quantities of residual
material.
This test method covers both manual and automated instruments.
Unless otherwise noted, the values stated in SI units are to be
regarded as the standard. The values given in parentheses are
provided for information only.
This standard does not purport to address all of the safety concerns, if
any, associated with its use. It is the responsibility of the user of this
standard to establish appropriate safety and health practices and
determine the applicability of regulatory limitations prior to use.
Page 9 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
This method includes fractional distillation at normal atmospheric
pressure conditions using distillation unit system per batch (Batch
distillation unit) to set over boiling each petroleum distillates. A
process Tdzeai petroleum raw materials with a wide boiling range of
petroleum products boiling range is relatively limited. The separation
process is based on the different vapor pressure of hydrocarbon
components and their boiling points.

Device
• Distillation flask (100 ml)
• Capacitor pass throug cooling bath
• Heater
• ASTM 7C/IP5C thermometer
• Graduated cylinder to receive the distillate
Page 10 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course

ASTM Atmospheric distillation apparatus

Method:

1. Sample is placed in the distillation flask.

2. Some pieces of crushed glass is placed in the bottom of the flask
to control boiling.
3. Gradually raise the temperature, observe rising vapors, then
record the amount of distillate at the corresponding
temperatures.
4. Determine the proportion of distillates and specific gravity, API
Gravity and refractive index versus boiling points.
Page 11 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
o
5. When you reach the boiling point to 350 C, Stop
distillation process and transfer residue to another device
where complemented by fractional distillation under
reduced pressure less than 40 mm Hg.
Page 12 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
4. Standard test method for distillation of petroleum products
at reduced pressure
ASTM D 6611-99

Scope
This test method covers the determination, at reduced pressures, of
the range of boiling points for petroleum products that can be partially
or completely vaporized at a maximum liquid temperature of 400°C.
Both a manual method and an automatic method are specified.

Test Method
The sample is distilled at an accurately controlled pressure between
0.13 and 6.7 kPa (1 and 50 mm Hg) under conditions that are
designed to provide approximately one theoretical plate fractionation.
Data are obtained from which the initial boiling point, the final
boiling point, and a distillation curve relating volume percent distilled
and atmospheric equivalent boiling point temperature can be prepared

Manual and automatic vacuum distillation

Page 13 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course

Vacuum distillation apparatus

Page 14 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
5. Standard test method for Calculating Viscosity Index from
Kinematic Viscosity at 40 and 100 oC.
ASTM D 2270-93 / IP 226/91 (95)

Definition
The viscosity index is an arbitrary number indicating the effect of
change of temperature on the kinematic viscosity of an oil. A high
viscosity index signifies a relatively small change of kinematic
viscosity with temperature

Scope
This practice covers the procedures for calculating the viscosity
index of petroleum products, such as lubricating oils, and
related materials from their kinematic viscosities at 40 and
100°C. In order to calculate viscosity index, Kinamatic viscosity
of oil or lubricants should be measured at specified temperature
40 & 100 oC .

Kinematic Viscosity
Absolute viscosity of a fluid divided by its density at the same
temperature of measurement. It is the measure of a fluid’s
resistance to flow under gravity, as determined by test method
ASTM D 445. To determine kinematic viscosity, a fixed volume
of the test fluid is allowed to flow through a calibrated capillary
tube (viscometer) that is held at a closely controlled
Page 15 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
temperature. The kinematic viscosity, in centistokes (cSt), is the
product of the measured flow time in seconds and the
calibration constant of the viscometer.

VI (Viscosity Index)
An arbitrary scale used to show the magnitude of viscosity
changes in lubricating oils with changes in temperature. Oils
with low VI number such as VI=0 ("zero") have high
dependence of viscosity change on temperature. They thicken
quickly with decreasing temperature, and thin out quickly with
increasing temperature. Oils with high VI number such as
VI=200, will still thicken with decreasing temperature but not as
rapidly, and also will thin out with increasing temperature, but
again not as much as low VI oil.

For Oils of 0 to 100 VI

Extracted values of L & H from the attached ASTM table and
apply the following equation:
L U
VI   100 (1)
LH

L & H values is determined from the attached table, U value is

the measured kinematic viscosity at 40 0C
Page 16 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
For Oils of 100 VI and greater

 Anti log N  1 
VI     100
 0.00715 

N  (log H  log U ) log Y

where
Y = kinematic viscosity of oil in centistokes at 100°C.
L = kinematic viscosity in centistokes at 40°C of an oil of 0
viscosity index and having the same kinematic viscosity at
100°C as the oil whose viscosity index is to be calculated.
H = kinematic viscosity in centistokes at 40°C of an oil of 100
viscosity index, and having the same kinematic viscosity at
100°C as the oil whose viscosity index is to be calculated.
U = kinematic viscosity in centistokes at 40 °C to be listed in
the body of the table. When the tables are being used in the
normal manner, this is also the kinematic viscosity at 40°C of
the oil whose viscosity index is being determined.
Page 17 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
Page 18 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course

Example 1

What is the viscosity index of an oil for which the observed

kinematic viscosities are 79.61 cSt at40°C and 9.12 cSt at
100°C?
Page 19 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
6. Standard Test Method for Smoke Point of Kerosene and
Aviation Turbine Fuel.
ASTM 1322-97 / BS 2000: Part 57 1995/ IP 57/95
Scope
This test method provides an indication of the relative smoke
producing properties of kerosines and aviation turbine fuels in a
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 indicates a
fuel of low smoke producing tendency. This test method covers
two procedures for determination of the smoke point of
kerosine and aviation turbine fuel, a manual procedure and an
automated procedure, which give results with different precision

Smoke point apparatus

Page 20 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
Page 21 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course

7. Standard Test Method for No Flow Point and Pour Point of

Petroleum Products
ASTM D7346 - 12
ASTM D 5853-95
IP 441/99 (95)

Significance and Use

The no flow point of a petroleum product is an index of the
lowest temperature of its utility for some applications. Flow
characteristics, such as no flow point, can be critical for the
proper operation of lubricating systems, fuel systems, and
pipeline operations. Petroleum blending operations require
precise measurement of the no flow point.

This test method can determine the temperature of the test

specimen with a resolution of 0.1°C at which either crystals
have formed or viscosity has increased sufficiently, or both, to
impede flow of the petroleum product.

The pour point of a petroleum product is an index of the lowest

temperature of its utility for certain applications. Flow
characteristics, like pour point, can be critical for the correct
operation of lubricating oil systems, fuel systems, and pipeline
operations
Page 22 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
Pour point

The pour point of a liquid is the lowest temperature at which it

becomes semi solid and loses its flow characteristics. In crude
oil a high pour point is generally associated with a high paraffin
content.

Scope

This test method covers the determination of the no flow point

temperature and pour point of petroleum products using an
automatic instrument.

Apparatus for pour point test

Page 23 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course

Method:

7. Place the sample in the tube up to the mark described.

8. Preheat the sample in a water bath until the temperature

enough to move oil. Raise the sample temperature 9
degrees Celsius higher than the expected pour point
without stirring.

9. Close the tube with stopper and thermometer and place it

in the cooling system until the paraffin wax crystals is
observed. Not shake the tube when the sample
examination.

10. Start temperature control when the thermometer

reading 9 oC above the degree of expected pour point.

11. Record thermometer readings each 3 degrees lower,

tilted the test tube and observe the movement of oil until
sample temperature does not move

12. This degree is called the spill point.

Page 24 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
8. Standard Test Method for Aniline point of Petroleum
Products and hydrocarbon solvents
ASTM D 611-82

Significance and Use

The aniline point (or mixed aniline point) is useful as an aid in

the characterization of pure hydrocarbons and in the analysis of
hydrocarbon mixtures. Aromatic hydrocarbons exhibit the
lowest, and paraffins the highest values. Cycloparaffins and
olefins exhibit values that lie between those for paraffins and
aromatics. In homologous series the aniline points increase
with increasing molecular weight. Although it occasionally is
used in combination with other physical properties in correlative
methods for hydrocarbon analysis, the aniline point is most
often used to provide an estimate of the aromatic hydrocarbon
content of mixtures.

Scope

These test methods cover the determination of the aniline point

of petroleum products and hydrocarbon solvents.

Test Method A is suitable for transparent samples with an

initial boiling point above room temperature and where the
aniline point is below the bubble point and above the
solidification point of the aniline-sample mixture.
Page 25 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
Test Method B, a thin-film method, is suitable for samples too
dark for testing by Test Method A.

Test Method A
Page 26 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
Chemicals

 Dry petroleum samples to be measured for aniline point

using anhydrous sodium sulfate.
 Dry aniline using pure sodium hydroxide granules on the
same day of the experiment.

Method:

 Place 10 ml of the sample with an equal amount of pure

aniline in the test tube.

 Keep the tube inside the glass jacket and then put it in a

water bath where temperature rises gradually.

 Record the temperature at which oil sample completely

dissolved in an equal amount of aniline.

Page 27 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course

Test Method B
Page 28 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course

9. Standard Test Method for Flash Point by Pensky-Martens

Closed Cup Tester (ASTM D 93-99c / IP 34/99)

Scope
These test methods cover the determination of the flash point
of petroleum products in the temperature range from 40 to
360°C by a manual Pensky-Martens closed-cup apparatus or
an automated Pensky-Martens closed-cup apparatus

Procedure A is applicable to distillate fuels (diesel, kerosine,

heating oil, turbine fuels), new lubricating oils, and other
homogeneous petroleum liquids not included in the scope of
Procedure B.
Procedure B is applicable to residual fuel oils, cutback residua,
used lubricating oils, mixtures of petroleum liquids with solids,
petroleum liquids that tend to form a surface film under test
conditions, or are petroleum liquids of such kinematic viscosity
that they are not uniformly heated under the stirring and heating
conditions of Procedure A.
Page 29 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course
Test method

A brass test cup of specified dimensions, filled to the inside mark with
test specimen and fitted with a cover of specified dimensions, is
heated and the specimen stirred at specified rates, by either of two
defined procedures (A or B). An ignition source is directed into the
test cup at regular intervals with simultaneous interruption of the
stirring, until a flash is detected

Method:

 Fix the device in a place far away from air currents.

 75 ml of the sample is placed in the copper cup.
 Run the gas flame.
 Raise the temperature gradually.
 Do not open the lid from the cup to keep the non-volatile
vapors.
 Record the temperature when blinking happens, then stop
heating.
 The Flash Point will be reset to a new sample and record the
temperature at which it occurs blinking.
 Leave the device to cool down. Then raise the tested
sample then clean the copper cup
Page 30 from 30 pages Prof. Dr. Elshafie Gad
Experiments of Petroleum Course

Pensky-Martens-closed cup apparatus