Term Paper ChE 402 Group 2A1

Chemical Engineering laboratory V
CHE 402
Term Paper
Bangladesh University of Engineering and
Technology
Term Paper
Course No.: CHE 402
Course Title: Chemical Engineering Laboratory –V
Submitted by-
Group 02 (A1)
Musfekur Rahman (1702006)

Mahdia Mahmud (1702007)
Numaer Tahnun (1702008)
Abir Podder (1702009)
Kazi Araf Sayeed (1702010)
Statement of Academic Integrity
The authors of this term paper hereby affirm that all the works of this paper, based on
the sessional course Chemical Engineering Laboratory-V (CHE-402), are carried out
by constructive teamwork without directly copying or following any academic
dishonesty. Any type of plagiarism was avoided while completing this report and all
the scientific sources are cited accordingly.
The authors also like to state that if any kind of academic dishonesty is found within
this report, we as a team will take full responsibility for that.
Authors
Musfekur Rahman
Mahdia Mahmud
Numaer Tahnun
Abir Podder
Kazi Araf Sayeed
i
Abstract
The assessment of specific properties of petroleum products along with respective
quality evaluation requires appropriate standards. The ASTM (American Society for
Testing and Materials) standards are applicable for determining properties of a wide
variety of petroleum products including crude oils, lubricating grease, automobile and
aviation gasoline, hydrocarbons, and other naturally occurring energy resources used
for various industrial applications. Each of these standards are strategized based on
some specific tests allowing petroleum refineries and chemical processing plants to
appropriately analyze these fuel oils against existing standards and monitor their quality
towards safe and efficient utilization. The following text contains elaborate discourse
on the conducted experiments which were aimed to assess the characteristic features of
some selected fuels like lubricating oil, kerosene, petrol and diesel. An overall twelve
experiments were performed for property evaluation of the said petroleum products. All
apparatus required for these tests were assembled according to the prescribed methods
of ASTM standards and the specified step by step procedures were followed for
obtaining accurate results. Density, specific gravity and API gravity measurement,
determination of mercaptan content (Doctor Test) were performed for kerosene, petrol
and diesel. Flash point and fire point were tested for kerosene and diesel samples
whereas cloud point, pour point, copper corrosion characteristics and aniline point were
determined for diesel sample only. ASTM distillation was performed with a petrol
sample while the gross calorific value of coal was measured with a bomb calorimeter.
Apart from these, the smoke point of kerosene was also measured. Essential properties
of lubricating oil, such as, water and bottom sediment content, ASTM color and
viscosity index were also tested against specified standards. All the resultant values
deemed comparable to the available literature values and the overall results were found
reasonable. The knowledge of these test methods will be essential and efficient for
determining fuel characteristics in fields of petroleum and chemical industries as well
as serve as a guide for quality surveillance.
ii
Acknowledgment
The authors would like to extend their sincerest gratitude to the respected teachers of
the course Chemical Engineering Laboratory-V (CHE 402) who have worked
relentlessly to provide insights into the theoretical background of the experiment, the
significance of the test methods and guided us throughout. We would like to thank Dr.
Kawnish Kirtania, Associate Professor, Mrs. Kaniz Fatema, Assistant Professor, Md.
Burhan Kabir Suhan, Lecturer and Zarin Tasnim Juthi, Adjunct Lecturer for their
constant support.
We are extremely grateful to the lab technicians who have helped us to complete every
experiment during the sessional course.
Authors
Musfekur Rahman
Mahdia Mahmud
Numaer Tahnun
Abir Podder
Kazi Araf Sayeed
iii
Table of Contents
Statement of Academic Integrity ............................................................................. i
Abstract ................................................................................................................... ii
Acknowledgment ................................................................................................... iii
List of Tables ......................................................................................................... ix
List of Figures ......................................................................................................... x
Introduction............................................................................................................. 1
3.A Aniline Point Determination of Diesel Oil (ASTM D 611-04) ....................... 5
3.A.1 Scope........................................................................................................ 5
3.A.2 Terminology............................................................................................. 5
3.A.3 Significance ............................................................................................. 5
3.A.4 Apparatus and Chemicals ........................................................................ 5
3.A.5 Procedure ................................................................................................. 6
3.A.6 Result and Discussion .............................................................................. 7
3.B Water and Bottom Sedimentation for Used and Fresh Lube Oil (ASTM D
1796-97) .......................................................................................................... 8
3.B.1 Scope........................................................................................................ 8
3.B.2 Significance ............................................................................................. 8
3.B.3 Apparatus and Setup ................................................................................ 8
3.B.4 Procedure ................................................................................................. 9
3.B.5 Result and Discussion ............................................................................ 10
3.C Doctor Test for Kerosene, Diesel and Petrol (IP 30/46) ............................... 11
3.C.1 Scope...................................................................................................... 11
3.C.2 Terminology........................................................................................... 11
3.C.3 Significance ........................................................................................... 11
3.C.4 Apparatus, Setup and Reagents.............................................................. 11
3.C.5 Procedure ............................................................................................... 11
3.C.6 Result and Discussion ............................................................................ 12
3.D Density, Specific gravity and API gravity by hydrometer method (ASTM D
iv
1298-99) ........................................................................................................ 14
3.D.1 Scope...................................................................................................... 14
3.D.2 Terminology........................................................................................... 14
3.D.3 Significance and Use ............................................................................. 15
3.D.4 Limitations ............................................................................................. 15
3.D.5 Apparatus ............................................................................................... 15
3.D.6 Experimental Setup ................................................................................ 16
3.D.7 Experimental Procedure ......................................................................... 17
3.D.8 Results and Discussion .......................................................................... 17
3.E ASTM color test for fresh lube oil (ASTM D 1500-03) ............................... 19
3.E.1 Scope...................................................................................................... 19
3.E.2 Terminology........................................................................................... 19
3.E.3 Significance and Use ............................................................................. 19
3.E.4 Limitations ............................................................................................. 20
3.E.5 Apparatus ............................................................................................... 20
3.E.6 Experimental Setup ................................................................................ 20
3.E.7 Experimental Procedure ......................................................................... 21
3.E.8 Results and Discussion .......................................................................... 21
4.A ASTM Distillation of petrol (ASTM D 86-04) ............................................. 23
4.A.1 Scope...................................................................................................... 23
4.A.2 Terminology........................................................................................... 23
4.A.3 Significance and Use ............................................................................. 25
4.A.4 Limitations ............................................................................................. 25
4.A.5 Apparatus ............................................................................................... 25
4.A.6 Experimental Setup ................................................................................ 26
4.A.7 Experimental Procedure ......................................................................... 27
4.A.8 Results and Discussion .......................................................................... 28
4.B Detection of Copper Corrosion from Petroleum Products for Diesel (ASTM
D 130-04) ...................................................................................................... 33
v
4.B.1 Scope...................................................................................................... 33
4.B.2 Terminology........................................................................................... 33
4.B.3 Significance and Use ............................................................................. 33
4.B.4 Apparatus ............................................................................................... 33
4.B.5 Reagents and Materials .......................................................................... 35
4.B.6 Experimental Set-up .............................................................................. 36
4.B.7 Experimental Procedure ......................................................................... 37
4.B.8 Result and Discussion ............................................................................ 38
4.C Viscosity and Viscosity Index of Lube Oil (ASTM D 88-94; D 2161-93; D
2270-93) ........................................................................................................ 39
4.C.1 Scope...................................................................................................... 39
4.C.2 Terminology........................................................................................... 39
4.C.3 Significance and Use ............................................................................. 40
4.C.4 Apparatus ............................................................................................... 41
4.C.5 Experimental Set-up .............................................................................. 42
4.C.6 Experimental Procedure ......................................................................... 42
4.C.7 Result and Discussion ............................................................................ 43
4.D Smoke Point of Kerosene (ASTM D 1322-97) ............................................. 46
4.D.1 Scope...................................................................................................... 46
4.D.2 Terminology........................................................................................... 46
4.D.3 Significance ........................................................................................... 46
4.D.4 Apparatus ............................................................................................... 47
4.D.5 Experimental Setup ................................................................................ 48
4.D.6 Procedure ............................................................................................... 49
4.D.7 Observed Data........................................................................................ 49
4.D.8 Result and Discussion ............................................................................ 49
5.A Calorific value of solid fuel by bomb calorimeter (ASTM D 2015-96)........ 51
5.A.1 Scope...................................................................................................... 51
5.A.2 Terminology........................................................................................... 51
vi
5.A.3 Significance ........................................................................................... 52
5.A.4 Apparatus ............................................................................................... 52
5.A.5 Experimental Setup ................................................................................ 54
5.A.6 Procedure ............................................................................................... 55
5.A.7 Observed Data........................................................................................ 56
5.A.8 Result and Discussions .......................................................................... 56
5.B Cloud Point and Pour Point Determination for Diesel (ASTM D 2500-02; D
97- 04) ........................................................................................................... 58
5.B.1 Scope...................................................................................................... 58
5.B.2 Terminology........................................................................................... 58
5.B.3 Significance ........................................................................................... 59
5.B.4 Apparatus ............................................................................................... 59
5.B.5 Experimental setup................................................................................. 60
5.B.6 Procedure ............................................................................................... 60
5.B.7 Results and Discussion .......................................................................... 61
5.C Flash Point and Fire Point Determination for Kerosene and Diesel (ASTM D
93-02) ............................................................................................................ 63
5.C.1 Scope...................................................................................................... 63
5.C.2 Terminology........................................................................................... 63
5.C.3 Significance ........................................................................................... 64
5.C.4 Apparatus ............................................................................................... 67
5.C.5 Experimental setup ................................................................................ 67
5.C.6 Procedure ............................................................................................... 68
5.C.7 Result and discussions ........................................................................... 68
Conclusion ............................................................................................................ 70
Nomenclature........................................................................................................ 71
References............................................................................................................. 72
Appendices ........................................................................................................... 74
Appendix A.1 ................................................................................................... 74
vii
Appendix A.2 ................................................................................................... 75
Appendix A.3 ................................................................................................... 76
Appendix A.4 ................................................................................................... 77
Appendix A.5 ................................................................................................... 78
Appendix A.6 ................................................................................................... 79
viii
List of Tables
Table 3.A-1: Recorded temperatures during heating and cooling and corresponding
aniline point of diesel. .................................................................................................... 7
Table 3.B-1: The recorded percentage of water sediment in the fresh and used lube oil.
...................................................................................................................................... 10
Table 3.C-1: Observation and result of doctor test petrol, kerosene and diesel sample
with doctor test. ............................................................................................................ 12
Table 3.D-1: Observed data for specific gravity and API gravity for diesel, petrol and
kerosene samples ......................................................................................................... 17
Table 3.D-2: Calculated data for density of diesel, petrol and kerosene at 60/60°F. .. 18
Table 4.A-1: Observed data of ASTM distillation of petrol ........................................ 28
Table 4.A-2: Standard distillation data ........................................................................ 30
Table 4.C-1: Observed data for Saybolt viscosity measurement ................................. 43
Table 4.C-2: Calculated data of kinematic viscosity and Viscosity Index .................. 43
Table 4.D-1: Table for smoke point of kerosene ......................................................... 49
Table 5.B-1: Table for observed Data for Cloud and Pour Point Determination of Diesel
...................................................................................................................................... 61
Table 5.C-1: Table for observed data for flash and fire point test of kerosene and diesel
...................................................................................................................................... 68
ix
List of Figures
Figure 3.A-1: Schematic diagram of the experimental setup for the aniline point
determination of diesel. .................................................................................................. 6
Figure 3.A-2: Schematic diagram of the experimental setup for the aniline point
determination of diesel. .................................................................................................. 6
Figure 3.B-1: Schematic diagram of the top view of centrifuge machine. .................... 9
Figure 3.B-2: Schematic of two centrifuge containing fresh and used lube oil. ............ 9
Figure 3.C-1: Test tube containing doctor solution and sample fuel. .......................... 12
Figure 3.D-1: Experimental setup for determining API gravity and specific gravity of
fuels .............................................................................................................................. 16
Figure 3.E-1: Schematic diagram of the colorimeter for determining ASTM color of
fresh and used lube oil ................................................................................................. 20
Figure 4.A-1: Schematic diagram for distillation of petroleum product ..................... 26
Figure 4.A-2: A graphical representation of the relation between the temperature (°C)
and the distillate recovered (%) ................................................................................... 29
Figure 4.B-1: Experimental Setup for Copper Strip Corrosion Test ........................... 36
Figure 4.B-2: Pressure vessel for Copper Strip Corrosion Test................................... 36
Figure 4.C-1: Experimental setup for determining viscosity and viscosity index ....... 42
Figure 4.D-1: Smoke Point Lamp ................................................................................ 48
Figure 5.A-1: Schematic diagram of standard test method for gross calorific value of
coal by adiabatic bomb calorimeter ............................................................................. 54
Figure 5.B-1: Schematic diagram of the experimental setup of the Cloud point and pour
point determination for diesel ...................................................................................... 60
Figure 5.C-1: Schematic diagram of flash point and fire point determination for
kerosene and diesel ...................................................................................................... 67
Figure 0-1: Setup of thin film apparatus of method B [3] ........................................... 74
Figure 0-2: Details of the equipment of test method A [3] .......................................... 74
Figure 0-3: Construction details about centrifuge tube................................................ 75
x
Introduction
The demand of petroleum in our day-to-day life doesn’t need any further explanation.
From transportation to household usage, every s of petroleum. It has been served as a
fuel for transportation, a source of electricity to power industries and equipment, a raw
material to make fertilizer to enhance food production, and a source of plastic to make
a variety of items. Moreover, another vast industry named as “Petrochemical Industry”
is also highly dependent on the distillated products of petroleum. There is a high
demand of these petrochemical products in everyday life. The petroleum industries
have to be very cautious to meet up the daily demand of petroleum. A petroleum
industry mainly consists of several processes such as discovery of petroleum well,
extraction of crude oil from well, refining and storage of different petroleum products,
transportation and supplying of petroleum products.
According to Statistica, in 2019, the global demand of petroleum oil was 99.7 million
barrels per day. In 2020 the demand fell to 91 million barrels per day due to the COVID-
19 pandemic. However, it has been projected that the demand will increase nearly to
101.2 million barrels per day in 2023. And this increment in demand will go on and on
[1]. According to CEIC, in Bangladesh, the consumption of oil in 2020 was 155 barrel
per day which decreased from 175.72 barrel per day in 2019. This implies to the huge
demand in our country [2].
After refining the crude oil, a number of useful products are separated from it. Some of
these products are Liquified Petroleum Gas, petrol, diesel, octane, naphtha, lubricating
oil, furnace oil, bitumen etc. Usage and supply mechanism of these products varies due
to different properties of the products. For determining the exact property, a number of
experiments are carried on over these petroleum products.
There are number of experiments under several methodology that can be followed to
determine the properties precisely. American Society for Testing and Materials is the
organization that approved the procedure for testing the petroleum products. ASTM
methods are followed to determine the physical, chemical and chemical properties of
oils. Boiling point, residue, density, viscosity, solubility, flowability etc. properties can
be measured by these experiments. These petroleum standards enable oil refineries as
well as other processing industries to properly inspect and process these fuel oils and
guarantee their quality for safe and effective usage.
1
The experiments that are performed are as follows:
Experiment 3:
(a) Aniline point determination of diesel oil (ASTM D 611-04)
(b) Water and bottom sedimentation for fresh and used lube oil (ASTM D 1796-97)
(c) Doctor test for kerosene, diesel and petrol (IP 30/56)
(d) Density, sp. gravity and API gravity by hydrometer method (ASTM D 1298-99)
(e) ASTM color test for used and fresh lube oil (ASTM D 1500-03)
Experiment 4:
(a) ASTM Distillation of petrol (ASTM D 86-04b)
(b) Detection of copper corrosion from petroleum products for diesel (ASTM D 130-
04)
(c) Viscosity and viscosity index/ lube oil (ASTM D 88-94; D 2161-93; D 2270-93)
(d) Smoke point of kerosene (ASTM D 1322-97)
Experiment 5:
(a) Calorific value of solid fuel by bomb calorimeter (ASTM D 2015-96)
(b) Cloud point and pour point determination for diesel (ASTM D 2500-02; D 97-04).
(c) Flash point and fire point for kerosene and diesel (ASTM D 93-02)
2
Bangladesh University of Engineering and Technology
Course No.: CHE 402

Experiment No.: 03
Name of the Experiment:
A. Aniline Point Determination of Diesel Oil (ASTM D 611-04)

B. Water and Bottom Sedimentation for Used and Fresh Lube Oil (ASTM D 1796-
97)
C. Doctor Test for Kerosene, Diesel and Petrol (IP 30/46)
D. Density, Specific Gravity and API Gravity by Hydrometer Method (ASTM D
1298-99)
E. ASTM color test for used and fresh lube oil (ASTM D 1500-03)
Date of Performance: 12 June 2022

Date of Submission: 31 August 2022
Submitted To-
Kaniz Fatema
Assistant Professor
Department of Chemical Engineering
3
Name of the Experiment
3. A Aniline Point Determination of Diesel Oil (ASTM D 611-04)
3. B Water and Bottom Sedimentation for Used and Fresh Lube Oil
(ASTM D 1796-97)
3. C Doctor Test for Kerosene, Diesel and Petrol (IP 30/46)
Prepared by
Musfekur Rahman Dihan
Id: 1702006
L-4 T-1
Group 2 (A1)
Partners’ Id
1702007
1702008
1702009
1702010
4
3.A Aniline Point Determination of Diesel Oil (ASTM D 611-04)
3.A.1 Scope
The standard test method (D 611-04) is applicable for finding the aniline point of
hydrocarbon and petroleum products. It contains five methods from A to E. Test method
A covers the sample whose initial boiling point is above the aniline point and the
solidification point of the aniline sample mixture. Test method B is for darker sample,
and test method C and D is applicable for the sample that vaporizes at the aniline point.
Test method E is for automatic apparatus. For determination of mixed aniline point is
also covered by this test method [3].
3.A.2 Terminology
Aniline Point: Defined as minimum equilibrium solution temperature of an equal

volume of aniline and sample [3].
Mixed aniline point: Defined as minimum equilibrium solution temperature of the

mixture containing two volumes of aniline, one volume of sample, and one volume of
n-heptane [3].
3.A.3 Significance
Aniline point or mixed aniline point is used as the measurement of the aromatic
hydrocarbon content in a sample. It is a great tool for characterization of the
hydrocarbon. Aromatic hydrocarbon gives a lower aniline point whereas paraffin gives
higher values. Higher aromatic compound in a sample oil is not desirable as it may
cause detrimental effects. In the homologous series, the higher the carbon content in the
chain, the higher the aniline point [4].
3.A.4 Apparatus and Chemicals
The schematic diagram for determining the aniline point of the diesel is given in Figure
-3.A-1 and a detailed design of the equipment is given in Appendix A.1. Other
apparatus that is required for this study are-
Heating and Cooling Bath: Transformer oil was used as the liquid heating and cooling
bath because aniline is hygroscopic.
Thermometers: A thermometer ranging from 100°C was used for the temperature
recording.
5
A stirrer, test tube, and a digital balance were also used in this test method. Aniline,
diesel, and transformer oil were used as chemicals.
3.A.5 Procedure
10 mL of aniline and 10 mL of the dried diesel sample were taken into the test tube
fitted with the stirrer and thermometer. A thermometer was mounted above the bottom
point of the test tube but immersed in the mixture. The position was checked to avoid
contact between the side wall and the mercury bulb. For the heating bath, transformer
oil was used. A thermometer is also set for measuring the temperature of the heating
medium. The oil was heated uniformly with the aid of an electrical heating source.
When the solution reached the point of complete miscibility, the corresponding
temperature was recorded. After that heating was turned off and the system was allowed
to cool. When the mixture got separated, the temperature was recorded. The final
aniline point was determined by taking average values.
Figure 3.A-1: Schematic diagram of the experimental setup for the aniline point determination of diesel.
Figure 3.A-2: Schematic diagram of the experimental setup for the aniline point determination of diesel.
6
3.A.6 Result and Discussion
Aniline point is the indication of the aromaticity of fuel oil. A higher aniline point is
usually desired as the paraffin content is higher. The aromatic compound usually
becomes miscible with aniline at low temperatures because aromatic oil has a higher
amount of unsaturated cyclic rings with is more compatible with the aniline structure.
In our study, the aniline-diesel sample became miscible at 70°C during the heating cycle
and then got separated at 68°C during the cooling. The aniline point is recorded to be
69°C which is the average value (Table 3.A-1). A study suggested the aniline point of
diesel to be 145°C [5]. Aniline point depends on the type of the sample that is used,
purity of the sample, and protocols that are used
Table 3.A-1: Recorded temperatures during heating and cooling and corresponding aniline
point of diesel.
Temperature
Aniline Point
(°C)
Heating 70
Cooling 68
Average 69
These values are taken by doing only a single study. As recommended by ASTM, the
precision of the test can be improved if repeatability, and reproducibility is obtained. If
this experiment could have been done more than once, then the result could be more
accurate.
7
3.B Water and Bottom Sedimentation for Used and Fresh Lube Oil
(ASTM D 1796-97)
3.B.1 Scope
This test method ASTM D 1796-97 is used to determine the water and sediment content
in fuel oil by using a centrifugal machine under laboratory condition. This is only valid
if the water and bottom sediment content range from 0-30 volume %. For the residual
oil type fuel, this test method is not applicable [6].
3.B.2 Significance
Water and bottom sediment are harmful to the fuel oil when it is used in equipment as
the water may cause corrosion and erosion caused by sediment content. It is also
important for determining the actual amount of fuel oil present under specified
conditions for pricing, taxation, and custody transfer [6].
3.B.3 Apparatus and Setup
Centrifuge: A centrifuge capable of spinning two or more filled cone-shaped 203 mm

(8 in.) centrifuge tubes at a speed that could be controlled to give a relative centrifugal
force (rcf) of between 500 and 800 at the tip of the tubes was used. The revolving head,
trunnion rings, and trunnion cups, including the cushions, were soundly constructed to
withstand the maximum centrifugal force capable of being delivered by the power
source. The trunnion cups and cushions firmly supported the tubes when the centrifuge
was in motion. The centrifuge was enclosed by a metal shield strong enough to
eliminate danger in case of any breakage.
Centrifuge Tubes: Each centrifuge tube shall be a 203 mm (8 in.) cone-shaped tube,
conforming to the dimensions given in Appendix A.2, and made of thoroughly annealed
glass.
Figure 3.B-1 and 3. B-2 provides the schematic diagrams of the experimental setup and
the centrifugal tubes. Other details of the equipment are provided in Appendix A.2.
8
3.B.4 Procedure
Two centrifuge tube was filled up 100 mL with fresh and used lube oil respectfully.
Then the centrifuge tubes were placed in the trunnion cups on opposite sides of the
centrifuge to establish a balanced condition. Two of four trunnion cup rings in the
centrifuge were used. After that, the tubes were rotated for about 2 hours at 3600 rpm.
The centrifuge was kept enclosed using a metal shield during rotation. At the end of the
operation, the sediment in the centrifuge tube containing used and fresh lube oil was
observed and recorded.
Figure 3.B-1: Schematic diagram of the top view of centrifuge machine.
Figure 3.B-2: Schematic of two centrifuge containing fresh and used lube oil.
9
3.B.5 Result and Discussion
Water and bottom sediment determination are crucial for the operative viewpoint. If the
oil contains water and other sediments, they can cause corrosion and erosion in the parts
of the equipment. In the study, it is found that there is no bottom sediment in the used
and fresh lube oil. Used lube oil contained 1.6% (v/v) of water in it whereas fresh lube
oil is free from water. In hydraulic oil and turbine oil, it is recommended to have water
below 0.1%. But usually used lube oil gets contaminated with water content due to
heavy operation as a lubricant. During the study, the level of water sediment is taken
from eyesight measurement which could give a slight variation of exact result to the
recorded values. Another possible error could raise from the unsound condition of the
centrifuge machine.
Table 3.B-1: The recorded percentage of water sediment in the fresh and used lube oil.
Percentage of Water
Lube Oil
(v/v)
Fresh 0%
Used 1.6%
10
3.C Doctor Test for Kerosene, Diesel and Petrol (IP 30/46)
3.C.1 Scope
This test method is applicable for the detection of mercaptans in motor fuel, kerosene,
and similar petroleum products. But this is inappropriate if the fuel contains a slight
amount of peroxide [7].
3.C.2 Terminology
Mercaptans: It is an organosulfur compound, commonly referred to as thiols, having

the common structure of R-SH. They have a distinct odor and may cause corrosion if
present in the fuel [7], [8].
Doctor Solution: Sodium plumbite solution (Na2O3Pb) which is prepared from sodium
acetate and sodium hydroxide (NaOH).
3.C.3 Significance
The doctor test is used for quick detection of mercaptans and hydrogen sulfide in
petroleum products because the presence of these compounds can lead to the
deterioration of materials used in transportation, storage, and consumption. A negative
result in the doctor's test ensures that the concentration of these compounds is
insufficient to cause such problems in normal use [7], [8].
3.C.4 Apparatus, Setup and Reagents
Three test tubes were taken for the doctor's test. These test tubes are of 50 mL of
capacity with a glass stopper. The schematic of the test tube is provided in Figure 3. C-
1. Doctor solution is the main reagent for this test method along with some pure dry
Sulphur stored in a container.
3.C.5 Procedure
10 mL of kerosene, diesel, and petrol were taken in 3 different test tubes. Then, the test
tubes were shaken for some time after mixing with a reasonable amount of sodium
plumbite solution. After that, a small quantity of powdered sulfur was added to each of
the 3 test tubes, and the test tubes were shaken again. Finally, the test tubes were
observed for any discoloration of the Sulphur floating at the oil-water interface or any
discoloration of either of the phases.
11
Figure 3.C-1: Test tube containing doctor solution and sample fuel.
3.C.6 Result and Discussion
Doctor test is done to find out the qualitative identification of mercaptan or H2S content
in the fuel which may cause corrosion and catalyst deactivation if gets contact. None of
the samples taken for the test (petrol, kerosene, and diesel) showed any discoloration
upon the addition of the doctor solution. So, three samples showed a negative result for
the doctor test.
Table 3.C-1: Observation and result of doctor test petrol, kerosene and diesel sample with
doctor test.
Discoloration of sulfur or of
Sample Result
either phase
Diesel None Negative
Petrol None Negative
Kerosene None Negative
12
Name of the Experiment
3.D. Density, Specific gravity and API gravity by hydrometer method
(ASTM D 1298-99)
3.E. ASTM color test for fresh lube oil (ASTM D 1500-03)
4.A. ASTM Distillation of petrol (ASTM D 86-04)
Prepared by-
Mahdia Mahmud
Id - 1702007
Level - 4, Term - 1
Group 02 (A1)
Partners’ Id-
1702006
1702008
1702009
1702010
13
3.D Density, Specific gravity and API gravity by hydrometer method
(ASTM D 1298-99)
3.D.1 Scope
The standard laboratory test method involving the use of a glass hydrometer is
employed to determine the density, specific gravity and API gravity of crude petroleum,
petroleum products, or blends of petroleum and nonpetroleum products that are
generally handled as liquids and have a Reid vapor pressure of 101.325 kPa (14.696
psi) or less. The test is carried out either at a reference temperature or at any other
convenient temperature in which case the measured values are corrected in
correspondence to the reference temperature using the Petroleum Measurement Tables.
These tables can also be used to determine equivalent values of measured density,
specific gravity and API gravity in other units at different reference temperatures [9].
API gravity of a crude oil product characterizes transportability of the product however
a precise correlation is difficult to obtain [10].
3.D.2 Terminology
Density – Density of a substance is defined as mass of the substance per unit volume
at 15°C and 101.325 kPa. The standard unit used for measurement is kilograms per
cubic meter e.g., the density of water is 999.1026 kg/m3 at 15°C.
Relative density or specific gravity – It is a dimensionless number which is defined

as the ratio of the mass of a given volume of liquid at a particular temperature to the
mass of an equal volume of pure water at the same or different temperature with both
reference temperatures being explicitly stated. Common reference temperatures include
60/60°F, 20/20°C, 20/4°C.
API gravity – API gravity is a special function of relative density or specific gravity at
60/60°F, expressed as °API. It can be measured from specific gravity using the
following equation –
141.5
°API = 60 − 131.5
sp gr ( o )
60 F
14
3.D.3 Significance and Use
During custody transfer, precise determination of the density, relative density (specific
gravity), or API gravity is essential in order to convert measured volumes of petroleum
and its products to their masses, or vice versa, at the standard reference temperatures.
This test method is best applicable for the determination of the density, relative density
(specific gravity), or API gravity of transparent low viscosity. This test method can also
be effectively utilized for viscous liquids by granting adequate time for the hydrometer
to reach equilibrium, and for opaque liquids by performing an appropriate meniscus
correction. Volume correction errors are minimized while utilized in conjunction with
bulk oil measurements by observing the hydrometer reading at a temperature close to
that of the bulk oil temperature. Density is a significant indicator of quality for
automotive, marine and aviation fuels, where it affects storage, handling and
combustion. The density, relative density (specific gravity), or API gravity of crude
petroleum is a key factor determining its quality and pricing however, this property
does not provide any definite estimation unless associated with other features of the
product [9]. The most crucial characteristics of petroleum products that affect their
market price are the sulfur content and relative density. Typically, low sulfur content
of crude oil is preferred which can be correlated to its API gravity [11].
3.D.4 Limitations
 This test method is not applicable for liquid petroleum products that have a Reid
vapor pressure above 101.325 kPa (14.696 psi) [9].
 The test method is relatively less suitable for highly viscous, opaque, waxy or
volatile liquids and requires special treatment [9].
3.D.5 Apparatus
1. Hydrometer: A graduated glass hydrometer is used. It is scaled in the units of

density, specific gravity and API gravity as required. The hydrometer should
conform the specifications of ISO 649-1 and other specification mentioned in
the ASTM data sheet D-1298−99𝜖2.
2. Thermometers: Thermometers conforming to specifications of the American
society for testing and materials, or the institute of petroleum are used.
3. Hydrometer cylinder: Material of construction may be clear glass, plastic or
metal. The inside diameter of the cylinder shall be at least 2.5 cm greater than
15
the outside diameter of the used hydrometer and the height of the cylinder shall
be such that the hydrometer floats in the test sample with at least 2.5 cm
clearance between the bottom of the hydrometer and the bottom of the cylinder.
4. Constant temperature bath: It is employed when the sample requires a test
temperature much above or below the room temperature.
3.D.6 Experimental Setup
Figure 3.D-1: Experimental setup for determining API gravity and specific gravity of fuels
16
3.D.7 Experimental Procedure
The test was done for three petroleum products: diesel, petrol and kerosene. The
samples were brought to the specified test temperature and in each run a test portion of
a sample was transferred to the hydrometer cylinder which has been brought to
approximately the same temperature as the sample. Then the appropriate hydrometer
was lowered into the sample, and it was allowed to freely attain an equilibrium position
while floating. The hydrometer was given enough time to reach a steady state allowing
any present air bubbles to escape. Two different types of hydrometers were used, one
for measuring the specific gravity and the other for measuring API gravity. The
hydrometer scale reading was observed and noted for the specific test temperature for
all three samples to determine their respective specific gravity and API gravity.
3.D.8 Results and Discussion
Room temperature = 31°C = 87.8 °F
Table 3.D-1: Observed data for specific gravity and API gravity for diesel, petrol and
kerosene samples
Specific Gravity
Sample API gravity (°API)
(87.8°/87.8°F)
Diesel 0.826 39°
Petrol 0.757 55°
Kerosene 0.785 49°
Using the data from Table 3. D-1, necessary calculations were made. A sample
calculation can be found in the Appendix A.3. The obtained data from the calculations
were compiled and tabulated in the following table.
17
Table 3.D-2: Calculated data for density of diesel, petrol and kerosene at 60/60°F.
Specific Gravity Density (60°/60°F)

Sample API gravity (°API)
(87.8°/87.8°F) (kg/m3)
Diesel 0.826 39° 830
Petrol 0.757 55° 759
Kerosene 0.785 49° 784
It is typical to use parameters like density, specific gravity or API gravity for evaluating
product quality and assigning suitable price to a petroleum product. This hydrometer
method is a suitable procedure for determining specific gravity and API gravity. It
provides a correlation between API gravity and specific gravity at the reference
temperature (60/60°F) which enables determination of the value of one property by
measuring the other one. The literature values for the density ranges from 875 to 850
kg/m3 for diesel, from 715 to 780 kg/m3 for petrol and from 775 to 840 kg/m3 for
kerosene [12]. The calculated values from the test fall under these ranges giving
acceptable results.
18
3.E ASTM color test for fresh lube oil (ASTM D 1500-03)
3.E.1 Scope
This test method deals with the visual determination of the color of a wide range of
petroleum products such as heating oils, lubricating oils, diesel fuel oils and petroleum
waxes. The result of the test is reported as “ASTM color” of the respective sample.
More refined products are lighter in color.
3.E.2 Terminology
ASTM color: The ASTM color is defined in the ASTM d 1500 standard as a two-digit
number color scale to grade oil and other petroleum products. The scale is defined by
16 glass standards of specified luminous transmittance and chromaticity, graduated in
steps of 0.5, from 0.5 corresponding to the lightest color to 8.0 corresponding to the
darkest color. It is intended for a wide variety of petroleum products such as lubricating
oils, heating oils, diesel fuel oils, mineral insulating oil and solid petroleum waxes and
has been adopted by other standardizing bodies (i.e: ISO 2049) [13].
3.E.3 Significance and Use
In petrochemical industries, color is a key indicator for grading and quality surveillance
of petroleum-based products. It is a preliminary grading characteristic for such products
as it can be readily observed and compared to available standards. In certain cases, the
color of the product indicates the degree of refinement of the material, in other cases it
may indicate extent of contamination. Increased turbidity can indicate solid
contamination of lubricating oils. A color range can thus be used for both quality control
and contamination monitoring. If the color range of a particular product is known, then
a deviation from that color may indicate possible contamination or quality degradation.
However, color alone is not a credible parameter describing product quality and should
not be used indiscriminately in product specifications without proper association with
other relevant properties [13].
19
3.E.4 Limitations
Determination of the color of refined petroleum products having color lighter than 0.5
ASTM color is not possible by using this method.
3.E.5 Apparatus
1. Colorimeter: It is an instrument which consists of a light source, glass color

standards, sample container with cover, and a viewing piece as illustrated in
Figure 3. E-1.
2. Sample Container: A clear glass sample jar is used for routine tests. The
standard practice is to use a specified cylindrical, clear glass jar with a flat
bottom of 30 to 32.4 mm internal diameter and 115 to 125 mm of external
height, and a wall thickness no greater than 1.6 mm [13].
3.E.6 Experimental Setup
Figure 3.E-1: Schematic diagram of the colorimeter for determining ASTM color of fresh and
used lube oil
20
3.E.7 Experimental Procedure
The used colorimeter housed two compartments for two sample containers. One sample
container was filled with distilled water up to a level of 50mm and was inserted in one
of the compartments of the colorimeter. Through the compartment, the standard glasses
were viewed. In the other compartment, the container with the lubricating oil sample
was placed. Both the containers were covered from external light. The light source was
switched on and the color of the sample was compared to that of the standard glasses.
The color dial was rotated to change the color of the standard glasses until an exact
match was found for the sample’s color. The color index for the matching color was
noted down as the ASTM color of the sample. Two lubricating oil samples were
analyzed using this procedure, a fresh lubricating oil and a used lubricating oil. The
ASTM color for both the samples were reported according to standard practices.
3.E.8 Results and Discussion
The color of the fresh lube oil was observed to be an intermediate between standards 4
and 4.5. The color of the fresh lube oil was hence reported as L4.5 ASTM color. The
color of the used lube oil sample was darker than the maximum standard possible in the
used calorimeter which was 5. Therefore, the color of the used lube oil was reported as
D5 ASTM color as per standard reporting.
The ASTM color found from this particular procedure cannot be cross referenced with
results obtained from other similar tests and can only be compared with literature
values, which are obtained using the same test procedure. The ASTM color is a good
basic indicator for rudimentary estimation of quality, and degree of refinement of a
petroleum product and a pre-alarm for possible contaminations. However, more
rigorous and robust procedures are required for the precise determination of these
important specifications of the petroleum product.
21
Course No.: CHE 402

Experiment No.: 04
A. ASTM Distillation of petrol (ASTM D 86-04)
B. Detection of copper corrosion from petroleum products for diesel
(ASTM D 130-04)
C. Viscosity and viscosity index/ lube oil (ASTM D 88-94; D 2161-93;
D 2270-93)
D. Smoke point of kerosene (ASTM D 1322-97)
Date of Performance: 19 June 2022

Date of Submission: 31 August 2022
Submitted To-
Kaniz Fatema
Assistant Professor
22
4.A ASTM Distillation of petrol (ASTM D 86-04)
4.A.1 Scope
This test method involves the atmospheric distillation of petroleum products using a
laboratory batch distillation unit for determining the boiling range characteristics of
products such as natural gasolines, 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, naphtha, white spirits, kerosene
and Grades 1 and 2 burner fuels. The method is applicable for both manual and
automated equipment [14].
4.A.2 Terminology
 Charge volume: The total volume of the specimen (100mL) that is charged to
the distillation flask at the specified temperature at which the test run was
carried out.
 Decomposition: The term ‘decomposition’ refers to the breakdown of a larger
hydrocarbon molecule through pyrolysis or cracking which yields smaller
molecules with relatively lower boiling points than the original molecule.
 Decomposition point: Lowest corrected temperature reading at which the
decomposition of the liquid in the flask starts to occur.
 Dry point: The corrected temperature reading that is observed at the instance
of evaporation of the last drop of liquid from the lowest point in the distillation
flask. This is exclusive of any drops of film of liquid on the side of the flask or
on the temperature sensor. The dry point is used in correlation with special
purpose naphtha, such as those used in the paint industry. Dry point is
substituted for the end point (final boiling point) whenever the sample cannot
consistently fulfill the precision requirements.
 Dynamic Holdup: The amount of substance present in the neck and sidearm of
the flask, and in the condenser tube during the distillation.
 Emergent Stem Effect: The offset in temperature reading caused by using total
immersion mercury-in-glass thermometers in the partial immersion mode.
When the mercury thread is partially immersed, the emergent portion is likely
to be at lower temperature than the immersed portion. This lower temperature
at the emergent portion results in a shrinkage of the mercury thread.
23
 End point (EP) or final boiling point (FBP): The corrected maximum
thermometer reading obtained during the test generally after the evaporation of
all liquid from the bottom of the flask.
 Front End Loss: Loss due to evaporation during transfer from receiving
cylinder to the distillation flask, vapor loss during the distillation, and
uncondensed vapor in the flask at the end of the distillation are referred as the
front-end loss.
 Initial boiling point (IBP): The corrected thermometer reading which is
observed at the moment when the first drop of condensate falls from the lower
end of the condenser tube.
 Percent recovered - the volume of condensate observed in the receiving
cylinder, expressed as a percentage of the charge volume, associated with a
simultaneous temperature reading. The maximum percent recovered is called
the percent recovery.
 Percent residue: The measured volume of residue in the flask is expressed as
a percentage of the charge volume and this is called the percent residue.
 Percent loss (or observed loss): It is the percentage of the charge volume that
is not recovered as the condensate. Mathematically, Percent loss =100 - (Percent
total recovery).
 Percent total recovery: The sum of percent recovery and the residue in the
flask is described as the percent total recovery.
 Percent evaporated: It is the sum of the percent recovered and the percent loss.
 Rate of change (slope): The change in temperature reading per percent
evaporated or recovered.
 Temperature lag - The offset between the temperature reading obtained by a
temperature sensing device and the true temperature at that time.
 Corrected Temperature Reading: The temperature reading corrected for
barometric pressure.
24
4.A.3 Significance and Use
The basic test method of performing a simple batch distillation to determine the boiling
range characteristics of a petroleum product has been in use for as long as the petroleum
business has been. The boiling range characteristics or the volatility of hydrocarbons,
especially fuels and solvents, have a significant impact on the safety and performance
of the material. Moreover, the boiling range provides information on the composition,
the properties, and the behavior of the fuel during storage and use. The distillation
characteristics are critical for automotive and aviation gasolines as these affect starting,
warm-up, and the proclivity to vapor lock at elevated operating temperatures or
altitudes, or both. The presence of components with a high boiling point in these and
other fuels can have a substantial effect on the degree of solid combustion depositions.
Volatility affects the rate of evaporation and hence is crucial in the application of a wide
variety of solvents, especially for solvents used in paints. Distillation limits are
frequently stated in petroleum product specifications, commercial contract agreements,
process refinery/control applications, and regulatory compliance [14].
4.A.4 Limitations
Though the method is suitable for the analysis of distillate fuels, it is not applicable to
products with significant residual material content [14].
4.A.5 Apparatus
The key components of the batch distillation unit were the distillation flask, the
condenser and associated cooling bath, a metal shield or enclosure for the distillation
flask, the heat source, the flask support, the temperature measuring device, and the
receiving cylinder to collect the distillate.
1. Distillation Flask: The flask was made of heat resistant glass and the flask was
constructed with a ground glass joint. Glass beads were added to the flask to prevent
bumping during heating.
2. Condenser and an associated cooling bath: The condenser was made of seamless
noncorrosive metal tubing with the following dimensions- 560 ± 5 mm in length, an
outside diameter of 14 mm and a wall thickness of 0.8 to 0.9 mm.
3. Metal shield or enclosure: This was used as a protective measure. Nevertheless, it
allowed easy access to the burner and to the distillation flask during operation. The
25
shield was equipped with at least one window to observe the dry point at the end of the
distillation.
4. Heater: A gas burner capable of producing the first drop from a cold start within the
specified time and continuing distillation at the specified rate was used as the heat
source.
5. Flask support: The setup consisted of an adjustable system onto which the heater
was mounted with provision for placement of a flask support board above the heater.
The entire assembly was adjustable from the outside of the shield.
6. Receiving cylinder (Graduated cylinder): The receiving cylinder had a capacity to
measure and collect 100 mL of liquid. The shape of the base ensured that the empty
receiver did not topple when placed on a surface inclined at an angle of 13° from the
horizontal.
7. Thermometer: A mercury-in-glass thermometer was used for measuring the
temperature inside the flask.
4.A.6 Experimental Setup
Figure 4.A-1: Schematic diagram for distillation of petroleum product
26
4.A.7 Experimental Procedure
1. 100 mL of petrol sample was distilled in a batch distillation unit at ambient

pressure under conditions that were designed to provide approximately one
theoretical plate fractionation. The assemblage of the apparatus was ensured to
be specified.
2. The sample was transferred to a distillation flask and was heated by a heater;
vapor was produced which was then condensed in a condenser, surrounded by
a cooling water bath kept at 0°C by ice-water mixture. The condensate was then
collected in a graduated receiving cylinder placed at the condenser tube's bottom
end.
3. Heating was controlled in order to maintain the time interval between the first
application of heat and the time taken to reach the initial boiling point within
the limit of a certain value. Moreover, heating was carried on in the same
controlled rate to ensure uniform rate of condensation.
4. To reduce distillate loss from evaporation, the open end of the receiving cylinder
was covered with a piece of blotting paper, or similar material that had been
trimmed to fit the condenser tube.
5. The start time was noted, and the initial boiling point was then observed and
recorded. During the time interval between reaching the initial boiling point and
the end of the distillation, decomposition point was observed and data of
recovered volumes of distillate at respective temperatures were noted. This was
done by observing the volume of condensate to the nearest 0.5 mL at a certain
time interval until two successive observations agree. The volume in the
receiving cylinder was measured and recorded as percent recovery to the nearest
0.5 mL.
6. When the residual liquid within the flask was approximately 5 ml, heat was
adjusted to a final setting so that the time from the 5 ml of liquid residue in the
flask to the end (final boiling) point would meet the requirements. The end (final
boiling) point and dry point were observed and noted down. Subsequently,
heating was stopped.
7. The flask was then allowed to cool down until no more vapor was observed.
The flask was then disconnected from the condenser and its contents were
poured into the graduated cylinder. The flask was allowed to drain until no
27
appreciable rise in the volume of liquid in the graduated cylinder was observed.
The volume in the graduated cylinder was measured to the nearest 0.1 mL, and
the reading was recorded as the percent total recovery.
4.A.8 Results and Discussion
Observed Data:
Sample = 100 mL
Initial boiling point = 50 °C
Dry point = 185°C
Distillate recovered = 96.5 mL
Residue recovered = 2.0 mL
Table 4.A-1: Observed data of ASTM distillation of petrol
Amount of distillate Temperature

Observation Number
(mL) (°C)
1 5 63
2 10 68
3 20 77
4 30 99
5 40 102
6 50 118
7 60 132
8 70 154
9 80 179
10 90 234
11 95 284
28
100
90
80
70
60
Percent 50
recovery (%)
40
30
20
10
0
0 50 100 150 200 250 300
Temperature (°C)
Figure 4.A-2: A graphical representation of the relation between the temperature (°C) and the
distillate recovered (%)
Using the data from Table 4. A-1, necessary calculations were made, and a
characteristic plot was drawn for percent recovery in volume against the temperature
which is shown in Figure 4. A-2. A sample calculation can be found in the Appendix
A.4. The obtained data from the calculations were compiled and are given below –
 Initial boiling point = 50°C
 Dry point = 185°C
 Percent recovery = 96.5%
 Percent total recovery = 98.5%
 Percent loss = 1.5%
 Percent evaporated = 98%
29
The distillation data provides the boiling range but not for the specific components. The
obtained results can be compared to the standard distillation data given below:
Table 4.A-2: Standard distillation data
Boiling Range (°C) Product

0-70 Light gasoline
70-140 Benzene
140-180 Naphtha
180-250 Kerosene
250-350 Gas oil
In this experiment, 10% of the sample evaporated before 70°C. So, it can be assumed
that 10% of the sample was light gasoline. About (60 - 10) % = 50% of the sample
evaporated within range of 70°C to 140°C. This fraction might be considered as
benzene. After that, (80 - 60) % = 20% of the sample evaporated between 140°C and
180°C. This fraction can be assumed to be naphtha. About (90 - 80) % = 10% of the
sample had evaporated at up to 250°C, followed by the evaporation of the remaining
5% of the recovered sample. These fractions of the sample can be classified as kerosene
and gas oil, respectively. During the experiment, small portion of the sample was lost
which was absent from the recovered condensate and the residue. Probable underlying
reason can be -
1. Dynamic holdup
2. Front end loss
During distillation, some amount of the sample adhered to the neck and sidearm of the
flask and to the condenser tube. This amount is called the dynamic holdup. Front end
loss is the loss due to evaporation during transfer from receiving cylinder to distillation
flask, vapor loss during the distillation and uncondensed vapor in the flask at the end
of the distillation.
This distillation is used for analyzing the volatility of the oil signifying its pace of
evaporation. Highly volatile oils pose the threat of fire hazard and significant loss
during storage and handling. Various products can be obtained from crude oil and each
of these products have their own use. As ASTM distillation gives the boiling range of
30
the product along with an estimate of the volatility of said product, therefore, it is quite
useful for determining oil quality. Consequently, this method of distillation is a
commonly used process for determining the specifications of most of the products.
31
4.B. Detection of copper corrosion from petroleum products for

diesel (ASTM D 130-04)
4.C. Viscosity and viscosity index of lube oil (ASTM D 88-94; D
2161-93; D 2270-93)
Prepared by-
MD.Numaer Tahnun
Id- 1702008
Level-4, Term-1
Group 02 (A1)
Partners’ Id-
1702006
1702007
1702009
1702010
32
4.B Detection of Copper Corrosion from Petroleum Products for
Diesel (ASTM D 130-04)
4.B.1 Scope
This test method covers the detection of the corrosiveness to copper of aviation
gasoline, aviation turbine fuel, automotive gasoline, cleaners (Stoddard) solvent,
kerosene, diesel fuel, distillate fuel oil, lubricating oil, natural gasoline or other
hydrocarbons having a vapor pressure no greater than 124 kPa (18 psi) at 37.8°C. Some
products, particularly natural gasoline, may have a much higher vapor pressure than
would normally be characteristic of automotive or aviation gasoline. For this reason,
exercise extreme caution to ensure that the pressure vessel containing natural gasoline
or other products having high vapor pressure are not placed in the 100oC (212oF) bath.
Samples having vapor pressures in excess of 18 psi (124 kPa) may develop sufficient
pressure at 100oC to cause rupture of the pressure vessel. This method does not purport
to address all of the safety concerns.
4.B.2 Terminology
Corrosion: It is a chemical process where a metal is eaten and reducing its activity. It
occurs naturally.
4.B.3 Significance and Use
Crude petroleum contains sulfur compounds, most of which are removed during
refining. However, of the sulfur compounds remaining in the petroleum product, some
can have a corroding action on various metals and this corrosivity is not necessarily
related directly to the total sulfur content. The effect can vary according to the chemical
types of sulfur compounds present. The copper strip corrosion test is designed to assess
the relative degree of corrosivity of a petroleum product.
4.B.4 Apparatus
• Copper Strip Corrosion Pressure Vessel: It is constructed from stainless steel

according to the dimensions required. The vessel shall be capable of withstanding
a test pressure of 700 kPa gage (100 psi). Alternative designs for the vessel’s cap
and synthetic rubber gasket may be used provided that the internal dimensions of
33
the pressure vessel are such that a nominal 25-mm by 150-mm test tube can be
placed inside the pressure vessel.
• Test Tubes: These are made of borosilicate glass of nominal 25-mm by 150-
mm dimensions. The internal dimensions shall be checked as acceptable by use of
a copper strip. When 30 mL of liquid is added to the test tube with the copper strip
in it, a minimum of 5-mm of liquid shall be above the top surface of the strip.
• Test baths: All test baths shall be able to maintain the test temperature within
(+- 1 ºC) of required temperature. The bath should be deep to submerge one or
more pressure vessel. There shall be provision of suitable supports to hold the test
tubes in a vertical position. As a liquid bath medium, water and oil have been found
satisfactory and controllable at the specified test temperature. The bath temperature
is maintained by an electric heating system inside.
• Temperature Sensing Device (TSD): They can monitor the desired test
temperature in the bath to within an accuracy of (1°C) or better is used.
• Polishing Vise: It is used for holding the copper strip firmly without marring
the edges while polishing. Any convenient type of holder may be used if the strip
is held tightly and that the surface of the strip being polished is supported above the
surface of the holder.
• Viewing Test Tubes: Flat glass test tubes, are convenient for protecting
corroded copper strips for close inspection or storage.
• Forceps: This is either made of stainless steel or polytetrafluoroethylene
(PTFE) tips and used for handling the copper strips.
• Timing Device: This device is used for measuring test duration.
34
4.B.5 Reagents and Materials
• Wash Solvent: Any volatile, less than 5 mg/kg sulfur hydrocarbon solvent may
be used if it shows no tarnish at all when tested for 3 h at 50°C (122°F). 2,2,4-
trimethylpentane (isooctane) of minimum 99.75 % purity is the referee solvent.
• Surface Preparation: 00 grade or finer steel wool or silicon carbide grit paper
or cloth of varying degrees of fineness including 65-µm (240-grit) grade, 105-µm
(150-mesh) size silicon carbide grain or powder and absorbent cotton (cotton wool)
can be used for polishing materials. A commercial grade is suitable, but
pharmaceutical grade is most commonly available and is acceptable.
• Copper Strips Specification: Copper strips of approximately 12.5-mm (1⁄2-
in.) wide, 1.5 to 3.0-mm (1⁄16 to 1⁄8-in.) thick and 75-mm (3-in.) long from smooth-
surfaced, hard temper, cold-finished having 99.9 + % purity are used for. Electrical
bus bar stock is generally suitable. The strips can be repeatedly used but should be
discarded when the strips surface shows pitting that cannot be removed by the
specified publishing procedure.
• Ashless Filter Paper or Disposable Gloves: During final polishing, to avoid
contamination from individual disposable gloves can be used.
35
4.B.6 Experimental Set-up
Figure 4.B-1: Experimental Setup for Copper Strip Corrosion Test
Figure 4.B-2: Pressure vessel for Copper Strip Corrosion Test
36
4.B.7 Experimental Procedure
• Surface Preparation: Firstly all blemishes from all six sides from the surface
were removed using 00 grade or finer steel wool or silicon carbide paper. It was
ensured that the prepared copper strip is protected from oxidation prior to final
preparation, such as by immersing the strip in wash solvent from which it can be
withdrawn immediately for final preparation or which it can be stored for future
use. A sheet of silicon carbide paper was taken on a flat surface and moistened
with kerosene or wash solvent. Then the strips was rubbed against the silicon
carbide with a circular motion,protecting the stripnfrom contact with the fingers by
using ashless filter paper .The surface of the strips can also be prepared from motor-
driven machines..
• Final Preparation: After removing the strip from wash solvent, firstly the ends
followed by the sides were polished. This time silicon carbide grain powder with
105- mm(150mesh) was used. Circular motion was not needed rather rubbing in the
direction of long axis was made. All metal dust from the strip was removed by
absorbent cotton pad. After cleaning it was immediately immersed in the prepared
sample.
• Immersing the copper strip in diesel oil: The copper strip was then immersed
in the test tube containing diesel oil and the test tube was set inside the test bomb
by immersing it in a water bath of (50 ± 1oC) in such a way so that the test tube was
held firmly and in a vertical position.
• Immersing the test bomb in water bath: The bomb was then immersed in a
boiling water bath at (100 ± 1oC) and kept it there for approximately 3 hrs. Then the
test bomb was withdrawn and immersed in tap water for a few minutes for bringing
it in normal temperature.
• Strip examination: Then the test bomb was opened, the copper strip was
immediately withdrawn using forceps and immersed in wash solvent. It had to be
handled very carefully so that any type of marking or staining could be avoided.
After withdrawing the copper strip, it was dried with filter paper by blotting only.
Then it was observed by comparison against the copper strip corrosion standard to
measure the degree of corrosion if taken place. The copper strip and the standard
strip had to be held in 45o angle towards the light.
37
4.B.8 Result and Discussion
Observed data:
Sample = Diesel oil
Before the experiment, the color of the copper strip was “freshly polished”
After the experiment, the color of the copper strip was found to be dark orange.
Classification of corroded copper strip = 1b (from color chart)
Designation of the sample = Slight tarnish (from color chart)
Corrosion copper strip (2h/100⁰C), Classification 1b
An individual performing the test will report the results as a number followed by a letter
according to the ASTM ranges These ranges include freshly polished, slightly tarnished
(1a to 1b), moderately tarnished (2a to 2e), dark tarnish (3a to 3b), and corrosion (4a to
4c).
From the experiment, it was found the diesel was not fully pure as it changed the copper
strip color by reaction. Small amount of Sulphur content was present in that diesel. As
the strips did not corrode too much, we can assume that small S contents were present.
One of the main problems was that the color identification was done by bare eye. Also
it is quite problematic to distinguish between slight and moderate tarnish. . So, the result
can vary for person to person. It would be great if we could do the test several times but
due to time constraints it was not possible.
38
4.C Viscosity and Viscosity Index of Lube Oil (ASTM D 88-94; D
2161-93; D 2270-93)
4.C.1 Scope
This test method covers the empirical procedures for determining the Saybolt Universal
Viscosities or Saybolt Furol Viscosity of petroleum products at specified temperatures
between 40℃ and 100℃. The procedure of obtaining viscosity index of petroleum
products such as lubricating oils, and related materials from their kinematic viscosities
at 40 and 100°C.
Two methods of calculation are given as follows:
• Method A (for oils of 0 to 100 viscosity index)

• Method B (for oils of 100 or greater viscosity index)
4.C.2 Terminology
Efflux Time: Processing and storage vessels in the chemical and related industries
appear in a large variety of shapes. The time required to empty these vessels off their
liquid contents is known as efflux time .
Saybolt Universal Viscosity: The corrected efflux time (seconds) of 60 mL of sample

flowing through a calibrated universal orifice of Saybolt viscometer under specified
conditions is termed as Saybolt Universal Viscosity. The viscosity value is reported in
Saybolt Universal Seconds, abbreviated SUS, at a specified temperature
Furol: Furol is an acronym of “Fuel and road oils.”
Saybolt Furol viscosity: The corrected efflux time in seconds of 60 mL of sample

flowing through a calibrated Furol orifice of Saybolt viscometer under specified
conditions is termed as Saybolt Furol Viscosity. The viscosity value is reported in
Saybolt Furol seconds, abbreviated as SFS, at a specified temperature. This is
approximately 1⁄10 of the universal viscosity.
Viscosity Index: It is an arbitrary unitless number used to characterize the variation of

the kinematic viscosity of a petroleum product with temperature. It is mostly used to
characterize the viscosity-temperature behavior of lubricating oils. The lower the VI,
39
the more the viscosity is affected by changes in temperature. The higher the VI, the
more stable the viscosity remains over temperature fluctuations.
4.C.3 Significance and Use
The viscosity measurement method is useful to characterize some oil products as an

element in the uniformity of shipments and supply sources. The viscosity index is a
widely used and accepted measure of the variation in kinematic viscosity due to changes
in the temperature of a petroleum product between 40 and 100˚C.. A higher viscosity
index shows that cinematic viscosity decreases less at a higher temperature. The
viscosity index is used in practice as a single number indicating temperature
dependence of kinematic viscosity.
40
4.C.4 Apparatus
• Saybolt Viscometer: The viscometer is constructed entirely of corrosion-

resistant metal. The orifice tip, Universal or Furol, is constructed as a replaceable
unit in the viscometer. A nut should be provided at the lower end of the viscometer
for fastening it in the bath. The viscometer is mounted vertically in the bath and the
alignment is tested with a spirit level on the plane of the gallery rim. A cork or other
suitable means should be provided to prevent the flow of sample until the start of
the test.
• Bath: The bath serves both as a support to hold the viscometer in a vertical
position as well as the container for the bath medium. The bath is equipped with
effective insulation and with an efficient stirring device. The bath is provided with
a coil for heating and cooling and with thermostatically controlled heaters capable
of maintaining the bath within the functional precision level. The heaters and coils
should be located at least 30 mm from the viscometer. The bath medium should be
at least 6 mm (0.25 in.) above the overflow rim.
• Saybolt Viscosity Thermometers: A thermometer is used for reading the
temperature of the sample.
• Bath Thermometers: Saybolt Viscosity thermometers or any other temperature
indicating means of equivalent accuracy is used as bath thermometer.
• Filter Funnel: It is equipped with interchangeable 150μm (No.100) and 75-μm
(No.200) wirecloth meeting the ASTM requirements with respect to the wire cloth.
41
4.C.5 Experimental Set-up
Figure 4.C-1: Experimental setup for determining viscosity and viscosity index
4.C.6 Experimental Procedure
The viscometer was cleaned properly by solvent. The flask was placed below the
bottom of the viscometer. The bath with water was maintained at test temperature.
The sample was placed in the viscometer container and a cork stopper was inserted at
the bottom of the viscometer. Snapping the cork, the timer was started.
The timer was stopped the instant at which the bottom of the oil meniscus reaches
graduation mark (60 ml). Step 3-6 was repeated for two different temperatures (40°C
and 100°C). The efflux time (seconds) to the nearest 0.1 sec was recorded.
42
4.C.7 Result and Discussion
Table 4.C-1: Observed data for Saybolt viscosity measurement
Obs. No. Volume of lube oil Temperature Saybolt

Universal
(ml) (℃)
Viscosity
equivalent
to (SUS)
1 60 40 677
2 60 100 106
Table 4.C-2: Calculated data of kinematic viscosity and Viscosity Index
Temperature Kinematic Viscosity Viscosity Index
(°C) (cSt)
40 145 177.15
100 21.95
Petroleum-based hydraulic fluid has a variety of desirable characteristics, including

lubricating and anti-wear properties, so it is often the preferred fluid for hydraulic
systems. The viscosity of a lubricant is actually its resistance to flow and shear. It is
affected by contamination with water, particles or other lubricants, oil ageing. The
viscosity index number indicates the extent of thickness, or resistance to flow, with
temperature changes. The viscosity of a lubricant has a big influence on the
performance and long-life of your machinery. By selecting a lubricant with an
appropriate viscosity index for application, maintenance costs and downtime can be
minimized. The accuracy of the calculated viscosity index is dependent only on the
accuracy of the original viscosity determination. In this experiment after using the table
values, the kinematic viscosities were found as 145 cSt at 40°C and 21.95 cSt at 100°C)
while viscosity index was found to be above 100. Hence second method was used and
determined viscosity index was 177.15. The high value of viscosity index of the tested
oil indicated that this oils’ viscosity did not change remarkably with temperature
change. From kinematic viscosity, at a higher temperature the oil has a low resistance
43
to flow due to the reduction of the force of cohesion, which diminishes with
temperature, predominates with liquids
44
4.D. Smoke point of kerosene (ASTM D 1322-97)
5.A. Calorific value of solid fuel by bomb calorimeter (ASTM D 2015-96)
Prepared by -
Abir Podder
Id – 1702009
Level – 4, Term – 1
Group 02 (A1)
Partners’ Id –
1702006
1702007
1702008
1702010
45
4.D Smoke Point of Kerosene (ASTM D 1322-97)
4.D.1 Scope
The procedure described in this test method is used to determine the smoke point of
kerosene and aviation turbine fuel. However, it is not the intent of this standard to solve
every safety issue. Therefore, it is the user's obligation to implement adequate safety
measures.
4.D.2 Terminology
 Kerosene - Kerosene is the collective term given to the class of refined

petroleum distillates that are used as fuel and lighting. It has a boiling point
between 1400°C and 300°C. These homogenous distillates are low in viscosity,
sufficiently refined to be relatively stable, light in color, and free of smoky or
unpleasant odors.
 Smoke Point - It is described as the highest flame height in millimeters at which
a certain oil will burn without emitting smoke, as evaluated by the use of a
smoke lamp under specific conditions.
4.D.3 Significance
This test method gives a general idea of how well kerosene produces smoke. Typically,
paraffin has a cleaner burn than aromatic fuel. A fuel with a high smoke point has a low
tendency to produce smoke. The potential radiant heat transfer from the fuel's
combustion products is quantitatively related to the smoke point. The smoke point
serves as a foundation for the connection of fuel properties with the life of these
components because radiant heat transfer has a significant impact on the metal
temperature of combustor liners and other hot section sections of gas turbines.
46
4.D.4 Apparatus
 Smoke Point Lamp - In order to prevent eye strain when seeing the flame, a
medium-density cobalt glass was employed. Exactly level with the zero point on
the scale, the top of the wick guide was. On either side of a white or black strip of
2 mm in width, the scale was written in white lines on a black piece of glass. It
featured a 50 mm range, graded in 1 mm increments, with larger lines at every 5
mm and figures every 10 mm. A useful tool was offered to efficiently raise or reduce
the flame. The overall movement was smooth and regular, covering a distance of at
least 10 mm. In order to avoid the development of numerous images, the glass
entrance window was bent.
 Wick - It is made out of solid circular loom-woven cotton of average quality, and
it has the following features –
 Casing – 17 ends, 66 tex by 3
 Filling – 9 ends, 100 tex by 4
 Weft – 40 tex by 2
 Picks – 6 per centimeter
47
4.D.5 Experimental Setup
Figure 4.D-1: Smoke Point Lamp
48
4.D.6 Procedure
1. The sample was burned in a standard lamp with a gradated millimeter scale in
the background and a flame height that could be adjusted.
2. In order to determine the smoke point, the wick was raised until a smoky flame
developed, and then it was lowered until the smoky tail abruptly vanished.
3. The smoke point of kerosene was determined by measuring the height of the
flame to the nearest millimeter.
4.D.7 Observed Data
Table 4.D-1: Table for smoke point of kerosene
Flame Type Height of flame (mm)

Maximum flame height without smoke 22 mm
4.D.8 Result and Discussion
The sample's smoke point was measured to be 25.0 mm. A fuel with a greater smoke
point has a lesser tendency to create smoke. Aromatics typically burn with a smoky
flame. Straight chain paraffin, branched paraffin, naphthene, and aromatics are the
types of molecules in sequence from lowest smoke point (least smoky) to highest smoke
point (least smoky). An essential Jet Fuel specification is smoke point. In this
experiment, the smoke point light was positioned vertically, and the test was conducted
at room temperature out of caution. Kerosene would lose radiative heat up to a height
of 25 mm before burning, according to the observed smoke point of 25 mm. To avoid
parallax mistakes, the observer's eye was slightly off-center, causing the flame to appear
as both a reflected image on the scale and as the flame itself when it was viewed from
the other side of the central vertical white line.
49
Course No.: CHE 402
Course Title: Chemical Engineering Laboratory – V
Experiment No.: 05
A. Calorific value of solid fuel by bomb calorimeter (ASTM D 2015-96)
B. Cloud point and pour point determination for diesel (ASTM D 2500-02; D 97-
04)
C. Flash point and fire point determination for kerosene and diesel (ASTM D 93-
02)
Date of performance: 26-06-22
Date of Submission: 31-08-22
Submitted to –
Dr. Kawnish Kirtania
Associate Professor
50
5.A Calorific value of solid fuel by bomb calorimeter (ASTM D
2015-96)
5.A.1 Scope
According to this test, the adiabatic bomb calorimeter is used to determine the gross
calorific value of coal and coke. The values given in British thermal units and SI units
should be taken as the standard. The additional information are kept in parentheses.
This standard does not claim to resolve any safety issues relevant to its application. The
user of this standard is accountable for establishing suitable safety and health
precautions and determining whether any regulatory restrictions apply before use.
5.A.2 Terminology
 Calorific Value - The heat produced when a unit amount of a material combusts
under specific circumstances. The units used in this test procedure are Btu/lb.
Depending on the situation, the calorific value may alternatively be stated in
cal/g or in SI units (J/g).
 Gross Calorific Value - The amount of heat energy released during the
complete combustion of a specified air-gas mixture under a constant pressure,
with all combustion products returning to the reactants' initial temperatures and
any water produced during the combustion being in a liquid state.
 Net Caloric Value - The quantity of useable thermal energy created when a fuel
is burnt in circumstances comparable to those in which it is normally used.
 Calorimeter - It consists of the bomb and its contents, the colorimeter vessel
with stirrer, the water in which the bomb is immersed, and the portions of the
thermometer and the ignition leads within the calorimeter vessel.
 Corrected Temperature Rise - The calorimeter's temperature change as a
result of the bomb's internal mechanism, adjusted for any impacts that were
recorded.
 Energy Equivalent or Heat Capacity or Water Equivalent - The amount of
energy necessary to increase the calorimeter's temperature by an arbitrary unit.
The gross calorific value is the amount that, when multiplied by temperature
rise, then corrected for extraneous heat effects, and divided by the sample's
mass, is obtained.
51
𝐸∆𝑇− 𝑒1 − 𝑒3 − 𝑒3
So, Gross Calorific value of Coal, Qv = 𝑚
Where,
E = energy equivalent of the sample, cal/⁰C
ΔT = temperature rise in the calorimeter, ⁰C
e1 = Thermochemical energy corrections for the test for heat of formation of
HNO3
e2 = Heat of formation of H2SO4 – heat of formation of HNO3
e3 = Heat of combustion of ignition wire
m = mass of sample (coal) taken, g
5.A.3 Significance
If the buyer and seller agree to this, the gross calorific value is used to calculate the
total calorific content of the quantity of coal represented by the sample for payment
reasons. The gross calorific value may be used to assess the efficacy of beneficiation
operations or for research. It is utilized in computing the calorific value vs sulphur
content to evaluate if the coal satisfies regulatory criteria for industrial fuels.
5.A.4 Apparatus
 Test Space - The experiment should be conducted in a space that is free from drafts
and that can be maintained at a relatively constant temperature for the duration of the
measurement. Direct sunshine and radiation from other heat sources should be blocked
from the equipment. It is ideal to have a thermostat-controlled room temperature and
relative humidity.
 Combustion Bomb - It should be made of materials that won't be sufficiently
impacted by the combustion process or its byproducts to add detectable heat input or
change the final result. The bomb must be constructed so that all liquid combustion
products may be totally recovered by cleaning the inside surfaces. A test cannot have
any gas leaks. The bomb must be able to survive a hydrostatic pressure test of 20 MPa
(3000 psig) at room temperature without pushing any component above its elastic limit.
 Balance - There should be a laboratory balance having capability to weigh the
sample to the nearest 0.0001 g. The balance should be checked periodically to
determine is accuracy.
 Calorimeter Vessel - It needs to be constructed of metal, coated to prevent tarnish,
and have extremely polished outside surfaces. When the calorimeter is put together, the
52
bomb will be entirely submerged in the water due to its size. A mechanism that fully
and evenly stirs the water while putting out the least amount of heat is required. Starting
with the same temperatures in the calorimeter, room, and jacket, continuous stirring for
10 minutes is not allowed to increase the temperature of the calorimeter by more than
0.01°C (0.02°F). The submerged section of the stirrer must be connected to the outside
via a low-heat conductivity medium.
 Jacket - It should be a water-filled, double-walled jacket that completely encloses
the calorimeter. To reduce convection currents, the sides, top, and bottom of the
calorimeter vessel must be around 10 mm from the inner wall of the jacket. The
calorimeter vessel's mechanical supports must have the least amount of thermal
conduction feasible. A mechanism for fully and uniformly churning the water in the
jacket with little heat input is required.
 Thermometer - The calorimeter and the jacket both include thermometers for
measuring temperature. Here is a thermometer that measures a liquid in a glass. A 56℃,
56℉, 116℃, or 117℉ type ASTM standard thermometer may be used.
 Thermometer Accessories - To read liquid-in-glass thermometers to one tenth of
the lowest scale division, a magnifying glass is needed. This must have a lens and holder
made to prevent parallax from introducing any appreciable mistakes.
 Sample Holder - It should be an open crucible made of platinum, quartz, or a
suitable base metal alloy. Base-metal alloy crucibles are appropriate if, after a few test
firings, the weight does not appreciably alter.
 Ignition Wire - The wire has to be 100 mm long and 0.16 mm in diameter (No. 34
B & S gage) whether it is made of iron or a nickel-chromium (Chromel C) alloy. Under
the condition that steady ignition energy is supplied, platinum or palladium wire, 0.10
mm diameter (No. 38 B & S gage), may be employed. All calibrations and calculations
of the calorific value must be done with the ignition wire's length or mass constant.
 Ignition Circuit - It should provide the ignition wire with 6 to 16 V of alternating
or direct current because it is utilized for ignition. The circuit must have an ammeter or
pilot light to show that the current is flowing.
53
5.A.5 Experimental Setup
Figure 5.A-1: Schematic diagram of standard test method for gross calorific value of coal by
adiabatic bomb calorimeter
54
5.A.6 Procedure
1. A specified quantity of coal was measured using a 0.0001g weighing scale.

2. The bomb was cleaned, drained, and then allowed to dry. The bomb was
assembled before being tested, and 1.0 mL of water was added.
3. The ignition wire was connected to the ignition terminals using a fuse wire that
was measured and attached with just enough slack to allow contact with the
sample.
4. The bomb was put together and loaded with oxygen at a constant 32 atm
pressure. A calorimeter vessel was filled with the specified amount of water
after 2000g of water was weighed.
5. Once inside the calorimeter vessel, the constructed bomb was tested for oxygen
leaks. The calorimeter vessel was then put inside the jacket. The stirrers were
linked, the electrodes were attached, and the thermometers were set up.
6. To reach equilibrium, the system was given five minutes. The thermometer
reading was carefully examined as the fuse was lit after the initial temperature
was measured, shortly before the fuse wire was lit.
7. The final temperature was measured when three measurements taken
consecutively matched within one-tenth of the smallest thermometer
subdivisions; at this point, it may be presumed that the temperature has
increased to its final equilibrium value.
8. Later, the bomb was taken out by opening the lid. A consistent rate of pressure
release was used. The device was examined for any unburned samples or sooty
deposits before being opened because this test was to be discarded.
9. In order to calculate the original length, the whole length of the unburned
ignition wire was measured.
55
5.A.7 Observed Data
Mass of the sample taken (coal), m = 0.9716 g
Initial Temperature, T1 = 29.96℃
Maximum Temperature, T2 = 32.63℃
5.A.8 Result and Discussions
A gross calorific value of 6798.89 cal/g was obtained from the experiment. The gross
calorific value of common anthracite coal, which is about 8500 cal/g, is lower than the
value reported in the literature. The differences are the result of a number of factors.
Not all coal is created equal. Our experimental coal and the coal from the literature had
clearly different compositions. Utilizing dry coal for the experiment is recommended.
But because the coal's humidity was not under control in our lab, it is possible that this
contributed to the inaccuracy. As soot signifies unburnt or partially burned sample coal,
it should be avoided during the experiment. Since we were given information without
conducting an experiment, the existence of soot could not be determined. The calorific
value may be significantly reduced in the presence of soot. Due to time constraints, it
was not possible to handle the equipment and follow the proper protocols throughout
the experiment. It is important to have a consistent supply rate of oxygen when
pressurizing the bomb since doing otherwise might cause the powder material to burst
out and cause the experiment to fail. Additionally, part of the N2 that was trapped in
the bomb during the charge of O2 created NOx upon burning. Before utilizing it to
calculate the needed fuel, the bomb calorimeter had to be calibrated using a known fuel.
Earlier, benzoic acid was used to standardize this area. Some data were assumed
throughout the computations (heat of formation of HNO3, H2SO4 of combustion of
ignition wire). A perfectly adiabatic system is not conceivable in an experiment, hence
the system lost heat during the whole duration. The cooling adjustment, which should
have been performed in the computation but wasn't, should be implemented to fix this
problem. The entire gross calorific value has been considerably impacted by all of this.
56
Name of the Experiments:
5B. Cloud point and pour point determination for diesel (ASTM D 2500-02; D 97-04)
5C. Flash point and fire point determination for kerosene and diesel (ASTM D 93-02)
Prepared by-
Kazi Araf Sayeed
Student ID: 1702010
Level- 4, Term- 1
Dept: ChE
Group: 02 (A1)
Partner’s Student ID - 1702006
1702007
1702008
1702009
57
5.B Cloud Point and Pour Point Determination for Diesel (ASTM D
2500-02; D 97- 04)
5.B.1 Scope
1. This test method covers only petroleum products and biodiesel fuels that are
transparent inlayers 40 mm in thickness, and with a cloud point below 49°C.
2. 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 andhealth practices and determine the applicability
of regulatory limitations prior to use.
3. Several ASTM test methods offering alternative procedures for determining
pour points using automatic apparatus are available. None of them share the
same designation numberas Test Method D 97. When an automatic instrument
is used, the ASTM test method designation number specific to the technique
shall be reported with the results.
5.B.2 Terminology
The relative amount of wax present in an oil sample is directly affected by two major
conceptsnamely, the cloud point and the pour point.
Cloud Point: In petroleum products and biodiesel fuels, the temperature of a liquid
specimen when the smallestobservable cluster of wax crystals first appears upon cooling
under prescribed conditions is knownas the cloud point. To many observers, the cluster
of wax crystals looks like a patch of whitish ormilky cloud, hence the name of the test
method. The cloud appears when the temperature of the specimen is low enough to
cause wax crystals to form. For many specimens, the crystals first form at the lower
circumferential wall of the test jar where the temperature is lowest. The size and
position of the cloud or cluster at the cloud point varies depending on the nature of the
specimen.Some samples will form large, easily observable, clusters, while others are
barely perceptible.
58
Pour Point: In petroleum products, the lowest temperature at which movement of the
test specimen is observedunder prescribed conditions of test is known as the pour point.
In other words, the pour point of aliquid is the temperature at which it becomes semi
solid and loses its flow characteristics. Duringthe test, as the pour point is reached when
the oil does not flow for 5 seconds even when the testingtube kept horizontal.
5.B.3 Significance
The pour point of a petroleum specimen is an index of the lowest temperature of its
utility for certain applications such as flow of oil into the engine in cold weather country
and the pumping of oil industry.
For petroleum products and biodiesel fuels, cloud point of a petroleum product is an
index of the lowest temperature of their utility for certain applications.
5.B.4 Apparatus
Test Jar: A clear, cylindrical glass, flat bottom, 33.2 to 34.8-mm outside diameter and
115 and 125-mm height. The inside diameter of the jar may range from 30 to 32.4 mm
within the constraint that thewall thickness be no greater than 1.6 mm.
Thermometers: A thermometer ranging from 200C to -100C.
Cork: A cork to fit the test jar, bored centrally to take the test thermometer.
Jacket: A watertight cylindrical jacket of glass or metal, flat bottom, about 115 mm in
depth, with inside diameter 9.5 to 12.5 mm greater than the outside diameter of the test
jar.
Disk/cork/felt: A disk of cork or felt 6mm in thickness and of the same diameter as the
inside of the jacket.
Gasket: A ring gasket about 5mm in thickness, to fit snugly around the outside of the
test jar and loosely inside the jacket. This gasket may be made of cork, felt, or other
suitable material, elastic enoughto cling to the test jar and hard enough to hold its shape.
The purpose of the ring gasket is to preventthe test jar from touching the jacket.
Ice Bath: A cooling bath of a type suitable for obtaining the required temperatures. The
size and shape of the bath are optional but a support, suitable for holding the jacket
firmly in a vertical position, is essential. For determination of pour points below
59
two or more baths are needed. The requiredbath temperatures may be maintained by
refrigeration if available, otherwise by suitable freezing mixtures. In the experiment
water and sodium chloride crystals was used to achieve up to -120C.
5.B.5 Experimental setup
Figure 5.B-1: Schematic diagram of the experimental setup of the Cloud point and pour point
determination for diesel
5.B.6 Procedure
The cooling medium was prepared using ice and sodium chloride crystal in a jar.
Sodiumchloride was used to lower the melting point of ice which essentially helps to
reach muchlower temperature in the cooling medium. The cooling bath was insulated
using white cork sheet.
The sample oil(diesel) was poured into the test jar till it is half filled with oil. The jar
wasclosed tightly using the cork carrying the test thermometer.
The test jar was then submerged into the cooling medium and a piece of cloth was used
toinsulate the top of the cooling bath and the test jar.
The test jar was kept to cool the fuel and the temperature was observed along with the
fluid condition. With the help of thermometer temperature was noted. With every 30C
60
fallof temperatures, tube was withdrawn for a moment to find out for the cloudiness.
The cloud point was noted when the first sign of cloudiness was observed.
To find the pour point, the cooling was continued, and same procedure was repeated.
With every degree fall of temperatures, the tube was withdrawn for a moment to find
outfor the flowability of the oil. The temperature was noted as pour point when the oil
did not flow for 5 seconds even when kept horizontal.
5.B.7 Results and Discussion
Observed Data
Table 5.B-1: Table for observed Data for Cloud and Pour Point Determination of Diesel
Test name Temperature (0C)
Cloud Point -7
Pour Point -14
From literature the cloud point of diesel is found to be -40C and the pour point was found
to be -180C. From the experiment the cloud point was found to be -70C which is slightly
lower than the literature value. But for the pour point the temperature was found to be -
140C which is slightly higher than the literature value [15].
For a specific oil the criteria of pour point fixation depend upon two factors namely
climatic conditions and storage (handling). The climatic condition involves the
temperature and pressure at that time of that location. The storage (handling) involves
the effect of operational pressure andtemperature in the pump and pipeline. But in the
experimental lab this dissimilarity mainly caused by the purity of the diesel oil. To
decrease the pour point of diesel scientists are constantly experimenting by adding
additives to produce more winter resistant diesel. In India the Indian Oilhas already
introduced a special winter-grade diesel with a low pour-point of -330C.
Fuel, at minimum ambient temperature must be free flowing. The pour point reveals a
great importance in the countries where freezing temperatures are encountered. The
point indicates thelowest temperature of fluidity of the fuel. Below this temperature
fluidity of the oil is seized. This point is highly important for the automobile industry.
61
Also, at close approach of pour point the viscosity increases which increases the
pumping cost of oil in the industry. Since the cloud point and pour point were well
below the room temperatures, this oil specification may not be that muchof important in
our country instead which is highly important in the cold weather country.
62
5.C Flash Point and Fire Point Determination for Kerosene and
Diesel (ASTM D 93-02)
5.C.1 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- up apparatus.
These test methods are applicable for the detection of contamination of relatively non-
volatile or non-flammable materials with volatile or flammable materials.
The values stated in SI units shall 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
priorto use.
5.C.2 Terminology
Flash point: The flash point is known as the lowest temperature corrected to a
barometric pressure of 101.3 kPa (760 mm Hg), at which application of an ignition
source causes the vapors of a specimen of the sample to ignite under specified
conditions of test. The test specimen is deemed to have flashed when a flame appears
and instantaneously propagates itself over the entire surface of the test specimen. When
the ignition source is a test flame, the application of the test flame may cause a blue
halo or an enlarged flame prior to the actual flash point. This is not a flash point and
shall beignored.
Fire Point: The temperature at which the petroleum fuel vapor can burn continuously
for 5 seconds when tested in flash point apparatus are called fire point and it occurs after
the flash point by 3 - Atthis temperature it does not only ignite but also produces a
flame. The flash and fire point designaterespectively the temperature at which the vapor
above an oil will momentarily flash or explode in
63
presence of a flame and the temperature at which the vapors are evolved rapidly enough
to burn continuously.
5.C.3 Significance
The flash point temperature is one measure of the tendency of the test specimen to form
aflammable mixture with air under controlled laboratory conditions. It is only one of a
number of properties which must be considered in assessing the overall flammability
hazard of a material.
Flash point is used in shipping and safety regulations to define flammable and
combustible materials. One should consult the regulation involved for precise
definitions of these classifications.
These test methods should be used to measure and describe the properties of materials,
products, or assemblies in response to heat and an ignition source under controlled
laboratory conditions and should not be used to describe or appraise the fire hazard or
firerisk of materials, products, or assemblies under actual fire conditions. However,
results ofthese test methods may be used as elements of a fire risk assessment which
considers all of the factors which are pertinent to an assessment of the fire hazard of a
particular end use.
These test methods provide the only closed cup flash point test procedures for
temperaturesup to 370°C (698°F)
64
5.C.4 Apparatus
Pensky-Martens Closed Cup Apparatus: This apparatus consists of the test cup,
test cover and shutter, stirring device, heating source,ignition source device, air bath
and top plate.
Temperature Measuring Device: It is a thermometer having a range as shown as

follows and conforming to the requirementsprescribed in specification.
Ignition Source: Natural gas flame, bottled gas flame, and electric ignitors (hot wire)
have been found acceptablefor use as the ignition source.
5.C.5 Experimental setup
Figure 5.C-1: Schematic diagram of flash point and fire point determination for kerosene and
diesel
67
5.C.6 Procedure
 The cup was rinse with the sample (kerosene and then diesel) and then filled up
to the mark.
 The cup containing the sample was placed into the stove. The thermometer
was insertedinto the sample. The stirrer was connected with the motor and was
inserted into the sample.
 The sample was heated at a slow, constant rate (9-110F/min) with continual
stirring in aPensky-Marten closed tester.
 The ignition source was ignited. The small flame was directed into the cup at
regular intervals with simultaneous interruption of stirring. Near the flash point
the with every 10C the small flame was directed into the cup. When the flame
was blown off by a soundand flash, that point was noted as the flash point.
 The heating and the same procedure were continued until the sample ignites and
continuesto burn for about 5 seconds. This point was noted as the fire point of
that sample.
5.C.7 Result and discussions
Observed Data
Table 5.C-1: Table for observed data for flash and fire point test of kerosene and diesel
Sample Flash Fire

point point
Kerosene 530C 600C
Diesel 680C 730C
Preservation of fuels with respect to the ambient condition is a highly significant issue.
It is necessary to determine the flash and fire points of the fuel since they indicate
whether a certain fluid can be kept under a given situation or not. The flash point and
fire point of a fuel depends on the atmospheric pressure and contaminants present in
the fuel which has effect on the volatility of the fuel. From our experiment the flash
68
point and the fire point of kerosene were found to be 53C and 60C respectively and
for diesel were found to be 68C and 73C respectively at atmospheric pressure of the
laboratory. If kept at a temperature over the fire point (60°C for kerosene and 73°C for
diesel), the fuel might provide a fire risk. Since temperatures in our nation rarely rise
beyond 45°C, kerosene may be utilized without running the danger of a fire hazard.
The flash point of a petroleum fuel is indicative of the fuel to produce a combustible
vapor space at that certain temperature. Fuels with lower flash point than ambient
temperature are explosives and catch fire easily at the contact with an ignition source.
So, for marketable fuels it is a must tohave a fix flash point temperature to avoid fire
hazar
69
Conclusion
Different types of liquid and solid fuels are used every day all over the world to meet
the growing energy demand of the human civilization. Hence, certain key properties of
these fuels are of utmost importance for the safe and optimum use of them. The term
paper's objective was to determine the quality of liquid and solid fuels, as well as
lubricants, using ASTM criteria.
The aniline point of a hydrocarbon is a measure of its aromatic content; a high aniline
point indicates a high-quality fuel. When a fuel with a high aromatic component is
burned, incomplete combustion results in the formation of carbon particles (smoke). As
a result, pollution is created, and energy is wasted. That is why aniline point
measurement is needed to find out the aromatic content of the fuel beforehand. The The
water and sedimentation content of a fuel is necessary to not only estimate the corrosion
the fuel can cause to equipment, but also to accurately measure net volumes. Sulfur-
containing fuel creates SOx, which pollutes the air and also corrodes equipment.
Density, specific gravity, and API gravity are essential parameters to determine product
quality and suitable transportation method. ASTM color is a very good consideration
for the initial identification of petroleum product. Batch distillation of a fuel can show
the percentages of light and heavy hydrocarbons contained in it. The calorific value of
materials helps to test its suitability as an efficient fuel, and to properly give it a
monetary value. Cloud point and pour point of a fuel are important parameters to
remember when selecting a fuel for harsh weather or operating conditions. The flash
and fire point of a fuel measures the flammability of it; thus, it helps to assess the hazard
associated with it.
All engines are designed and manufactured for a fuel that has certain characteristics. In
the US, the industry organization that defines the consensus on fuels is the American
Society for Testing and Materials (ASTM). ASTM fuel standards are the minimum
accepted values for properties of the fuel to provide adequate customer satisfaction
and/or protection. The automotive, aerospace, and other sectors, as well as various
geological and chemical processing factories, can properly examine and process these
characteristics of fuel oils thanks to the ASTM petroleum standards, assuring their
quality for safe and effective usage.
70
Nomenclature
Symbol Description Unit

ASTM American Society for Testing and Materials -
IP Institute of Petroleum -
AP Aniline Point °C
E Energy equivalent of calorimeter cal/°C
e1 Heat of formation of HNO3 cal
e2 Heat of combustion of ignition of wire cal
e3 Heat of formation of H2SO4- Heat of formation of HNO3 cal
m Mass of sample gm
𝜇 Dynamic viscosity Centipoise
𝜗 Kinematic viscosity Centistoke
SFS Saybolt Furol Second s
SUS Saybolt Universal Second s
VI Viscosity Index -
71
References
[1] N. Sönnichsen, “Daily demand for crude oil worldwide from 2006 to 2020,
with a forecast until 2026.” https://www.statista.com/statistics/271823/daily-
global-crude-oil-demand-since-2006/ (accessed Aug. 31, 2022).
[2] “Bangladesh Oil Consumption, 1971 – 2022 | CEIC Data.”

https://www.ceicdata.com/en/indicator/bangladesh/oil-consumption (accessed
Aug. 31, 2022).
[3] A. Drews, “Standard Test Methods for Aniline Point and Mixed Aniline Point
of Petroleum Products and Hydrocarbon Solvents,” Man. Hydrocarb. Anal. 6th
Ed., pp. 152-152–7, 2008, doi: 10.1520/mnl10847m.
[4] K. Wang, X. Sun, S. Xiang, and Y. Chen, “Development of new algorithm for
aniline point estimation of petroleum fraction,” Processes, vol. 7, no. 12, 2019,
doi: 10.3390/PR7120912.
[5] O. E. Agwu, A. N. Okon, and F. D. Udoh, “A Comparative Study of Diesel Oil

and Soybean Oil as Oil-Based Drilling Mud,” J. Pet. Eng., vol. 2015, pp. 1–10,
2015, doi: 10.1155/2015/828451.
[6] H. L. Samples, “Standard Test Method for Water and Sediment in Fuel Oils by
the Centrifuge Method,” Test, vol. 97, no. Reapproved, pp. 1–6, 2002.
[7] “IP 30/56 Doctor Test”.
[8] S. C. Bajia, R. J. Singh, B. Bajia, and S. Kumar, “Determination of sulfur

content in petroleum products–an overview,” J. Sulfur Chem., vol. 38, no. 4,
pp. 450–464, 2017, doi: 10.1080/17415993.2017.1289530.
[9] S. J. Rand, “Astm D1298 Density,” ASTM Int., vol. 05, p. 221, 2003.
[10] F. Sánchez-Minero, G. Sánchez-Reyna, J. Ancheyta, and G. Marroquin,

“Comparison of correlations based on API gravity for predicting viscosity of
crude oils,” Fuel, vol. 138, pp. 193–199, 2014, doi: 10.1016/j.fuel.2014.08.022.
[11] A. Demirbas, H. Alidrisi, and M. A. Balubaid, “API gravity, sulfur content, and
desulfurization of crude oil,” Pet. Sci. Technol., vol. 33, no. 1, pp. 93–101,
2015, doi: 10.1080/10916466.2014.950383.
72
[12] M. A. Fahim, T. A. Alsahhaf, and A. Elkilani, Fundamentals of petroleum
refining. 2010.
[13] ASTM International United States, “Standard Test Method for ASTM Color of
Petroleum Products ( ASTM Color Scale ) 1,” Annu. B. ASTM Stand., vol. 05,
no. October 1959, pp. 1–5, 2011.
[14] “ASTM D 86-04b, Standard Test Method for Distillation of Petroleum

Products at Atmospheric Pressure,” 2004, [Online]. Available: www.astm.org,
[15] A. H. Saeedi Dehaghani and R. Rahimi, “An experimental study of diesel fuel
cloud and pour point reduction using different additives,” Petroleum, vol. 5, no.
4, pp. 413–416, 2019, doi: 10.1016/j.petlm.2018.06.005.
73
Appendices
Appendix A.1
Details about the apparatus setup of the aniline point determination test method [1].
Figure 0-1: Setup of thin film apparatus of method B [3]
Figure 0-2: Details of the equipment of test method A [3]
74
Appendix A.2
Details of the equipment of water and bottom sediment for fresh and used lube oil.
Figure 0-3: Construction details about centrifuge tube
75
Appendix A.3
Sample Calculation for Experiment 3D
Observed API reading of diesel = 39 °API

Temperature of the diesel sample = 31°C = 87.8 °F
141.5
°API = 60 − 131.5 = 39 °API
sp gr ( o )
60 F
141.5 141.5
∴ Specific gravity = API gravity + 131.5 = = 0.830
39 + 131.5
Density (60°/60°F) of diesel = 830 kg/m3.

Observed API reading of petrol = 55 °API
Temperature of the petrol sample = 31°C = 87.8 °F.
141.5
°API = 60 − 131.5 = 55 °API
sp gr ( o )
60 F
141.5 141.5
55 + 131.5
Density (60°/60°F) of petrol = 759 kg/m3.

Observed API reading of kerosene = 49 °API
Temperature of the kerosene sample = 31°C = 87.8 °F
141.5
°API = 60 − 131.5 = 49 °API
sp gr ( o )
60 F
141.5 141.5
49 + 131.5
Density (60°/60°F) of kerosene = 784 kg/m3.
76
Appendix A.4
Sample Calculation for Experiment 4A
Distillate recovered 96.5

Percent recovery = × 100% = 100 × 100% = 96.5%
Volume of Sample
Residue recovered 2
Percent Residue = × 100% = 100 × 100% = 2%
Volume of Sample
Now, Percent total recovery = Percent recovered + Percent Residue

= (96.5 + 2) % = 98.5%
Percent Loss = 100% - Percent total recovery
= (100 – 98.5) %
= 1.5%
And percent evaporated = Percent recovered + Percent Loss
= (96.5 + 1.5) %
= 98 %
77
Appendix A.5
Sample Calculation for Experiment 4C
At 40℃, Saybolt Universal Viscosity, t40 = 677 SUS

At 100℃, Saybolt Universal Viscosity, t100 = 106 SUS
From the table, kinematic viscosity value corresponding to 106 SUS, Y = 21.95
mm2/s < 70 mm2/s
kinematic viscosity value corresponding to 677 SUS, U = 145 mm2/s
Now the values of L and H are to be obtained from the table.
L = 576
H = 261.4
Procedure A:
𝐿−𝑈
Viscosity index, VI = 𝐿 − 𝐻 × 100
576 − 145
= × 100
576 − 261.4
= 136.99
As the calculated VI is greater than 100, the VI must be calculated by the Procedure
B.
Procedure B:
𝑙𝑜𝑔 𝐻 − 𝑙𝑜𝑔 𝑈
N= 𝑙𝑜𝑔 𝑌
𝑙𝑜𝑔 261.4 − 𝑙𝑜𝑔 145

= 𝑙𝑜𝑔 21.95
= 0.19
𝑎𝑛𝑡𝑖𝑙𝑜𝑔 𝑁 − 1
VI = + 100
0.00715
𝑎𝑛𝑡𝑖𝑙𝑜𝑔 0.15 − 1
= + 100
0.00715
= 177.15
78
Appendix A.6
Sample Calculation for Experiment 5A
The energy equivalent of coal (the heat required to increase 1℃ temperature of 2000g
water
by combustion), E = 2485 cal/℃
Mass of the sample taken (coal), m = 0.9716 g
Initial Temperature, T1 = 29.96℃
Maximum Temperature, T2 = 32.63℃
Assuming,
Correction factors (added heat):
For heat of formation of HNO3, e1 = 10 cal
For (heat of formation of H2SO4 – heat of formation of HNO3), e2 = 10 cal
For heat of combustion of ignition wire = 2.3 cal/cm × (Li – Lf) cm = 10 cal
𝐸∆𝑇− 𝑒1 − 𝑒3 − 𝑒3
Gross calorific value of sample coal, Qv = 𝑚
2485×(32.63−29.96)− 10 − 10 − 10
= 0.9716
= 6798.89 cal/g
= 6798.89 kcal/kg
79

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Chemical Engineering laboratory V

Musfekur Rahman (1702006)

Kazi Araf Sayeed

Kazi Araf Sayeed

Acknowledgment ................................................................................................... iii

List of Tables ......................................................................................................... ix

List of Figures ......................................................................................................... x

3.A Aniline Point Determination of Diesel Oil (ASTM D 611-04) ....................... 5

3.A.3 Significance ............................................................................................. 5

3.A.4 Apparatus and Chemicals ........................................................................ 5

3.A.5 Procedure ................................................................................................. 6

3.A.6 Result and Discussion .............................................................................. 7

3.B.2 Significance ............................................................................................. 8

3.B.3 Apparatus and Setup ................................................................................ 8

3.B.4 Procedure ................................................................................................. 9

3.B.5 Result and Discussion ............................................................................ 10

3.C.3 Significance ........................................................................................... 11

3.C.4 Apparatus, Setup and Reagents.............................................................. 11

3.C.5 Procedure ............................................................................................... 11

3.C.6 Result and Discussion ............................................................................ 12

3.D.3 Significance and Use ............................................................................. 15

3.D.4 Limitations ............................................................................................. 15

3.D.5 Apparatus ............................................................................................... 15

3.D.6 Experimental Setup ................................................................................ 16

3.D.7 Experimental Procedure ......................................................................... 17

3.D.8 Results and Discussion .......................................................................... 17

3.E.3 Significance and Use ............................................................................. 19

3.E.4 Limitations ............................................................................................. 20

3.E.5 Apparatus ............................................................................................... 20

3.E.6 Experimental Setup ................................................................................ 20

3.E.7 Experimental Procedure ......................................................................... 21

3.E.8 Results and Discussion .......................................................................... 21

4.A ASTM Distillation of petrol (ASTM D 86-04) ............................................. 23

4.A.3 Significance and Use ............................................................................. 25

4.A.4 Limitations ............................................................................................. 25

4.A.5 Apparatus ............................................................................................... 25

4.A.6 Experimental Setup ................................................................................ 26

4.A.7 Experimental Procedure ......................................................................... 27

4.A.8 Results and Discussion .......................................................................... 28

4.B.3 Significance and Use ............................................................................. 33

4.B.4 Apparatus ............................................................................................... 33

4.B.5 Reagents and Materials .......................................................................... 35

4.B.6 Experimental Set-up .............................................................................. 36

4.B.7 Experimental Procedure ......................................................................... 37

4.B.8 Result and Discussion ............................................................................ 38

4.C.3 Significance and Use ............................................................................. 40

4.C.4 Apparatus ............................................................................................... 41

4.C.5 Experimental Set-up .............................................................................. 42

4.C.6 Experimental Procedure ......................................................................... 42

4.C.7 Result and Discussion ............................................................................ 43

4.D Smoke Point of Kerosene (ASTM D 1322-97) ............................................. 46

4.D.3 Significance ........................................................................................... 46

4.D.4 Apparatus ............................................................................................... 47

4.D.5 Experimental Setup ................................................................................ 48

4.D.6 Procedure ............................................................................................... 49

4.D.7 Observed Data........................................................................................ 49

4.D.8 Result and Discussion ............................................................................ 49

5.A Calorific value of solid fuel by bomb calorimeter (ASTM D 2015-96)........ 51

5.A.4 Apparatus ............................................................................................... 52