Viscometer

A viscometer (also called viscosimeter) is an instrument used to

measure the viscosity of a fluid. Viscometers can measure only
constant viscosity, that is, viscosity that does not change with flow

conditions.

Redwood Viscometer

• Clean the oil cup with a suitable solvent such as carbon

tetrachloride and dry it thoroughly by using soft tissue paper or
some similar material which will not leave any fluff and clean
the jet hole with any fine thread.
• Fill the bath with water for determination at temperature 93⁰ C
or below. For higher temperatures, suitable oil of low viscosity
may be used instead of water.
• Bath should be filled to a level not less than 10mL below the
rim of oil cup at the test temperature.
• Heat the viscometer bath to a few degree above the desired
test temperature.
• Pour the prepared sample into the oil cup through a filter of
metal gauge not coarser than BS100 mesh.
• Adjust the temperature of bath until it reaches the test
temperature.
• During procedure, all the contents of the bath stirred well by
continuous stirring.
• Stir the sample during the preliminary period e.g. after the ball
valve closing the bottom of the jet by suitable means.
• Do not stir the sample during actual determination. When the
sample reaches the desired temperature, adjust the liquid level
by allowing the sample to flow out until the surface of the
sample touches the filling point.
• Stop the time recorder at the instance when sample reaches
the graduation mark of the flask and note the final reading of
the oil cup thermometer.
• Reporting the time in seconds to the nearest 0.5⁰ C for values
below 300s and to the nearest whole seconds for values above
200s.

Graphical sketch of Redwood viscometer

Saybolt Viscometer

• Viscosity determination should be done in a room free from

drafts and rapid changes in temperature.
• Typically rooms with 20⁰ to 30⁰ C temperature may be
employed.
• The oil tube first to be cleaned by an effective solvent such as
benzol and excess solvent should be removed from the oil tube.
• All oil should be passed through a 100 mesh wire strained
before it is introduced in to the oil tube.
• After the tube is cleaned, a quantity of oil to be tested,
sufficient to wet the entire surface of the tube, should be pour
in to the tube and allowed to drain put.
• The cork stopped shall be inserted not less than a quarter inch
and not more than three quarters of an inch in to the lower end
of the chamber at the bottom of the oil tube.
• The cork shall fit tightly enough to prevent the escape of oil.
The oil should be heated at a constant rate not more than 20⁰ C
below the temperature of the test.
• The oil in the oil tube shall be kept well stirred with the oil tube
thermometer.
• The bath temperature shall be adjusted until the oil
temperature remains constant.
• After thermal equilibrium reached, no further adjustments
should be made in both the temperature.
• After the oil temperature is stabilized at the desired
temperature for more than 1 minute, the thermometer is
withdrawn and surplus oil is removed.
• The receiving flask should be placed in position so that the
stream of oil from the outlet tube will strike the neck of the
flask up to the graduation mark on the receiving flask should
not be less than 10cm from the bottom of the bath.
• The cork shall be shaped from its position and at the same
instant the timer should be stopped when the bottom of the
meniscus of the oil reaches on the neck of the receiving flask.

Graphical sketch of Saybolt viscometer

Bomb Calorimeter

 The amount of heat liberated when a unit mass of fuel is burnt

completely is known as the lower calorific value.
 The amount of heat liberated when a unit mass of fuel is burnt
completely and all its vapours are condensed into liquid is
known as the higher calorific value.
 The calorific value of liquid and solid fuel is generally found by
using bomb calorimeter.

 A known quantity of fuel is taken in the crucible. The fuel is

taken by weighing in a physical balance.
 The crucible is fixed in the bomb in such a way that the fuse
touches the fuel.
 The bomb is then charged with oxygen to a pressure of 30 bar.
 The oxygen charging valve (non return valve) and release valve
are closed tightly and the bomb is placed in water bath and then
it is closed with cover.
  The water in the calorimeter is stirred and when the
temperature remains steady the reading is noted.
 The fuel is ignited by passing a current through the fuse wire.
 The temperature of the bath starts increasing after ignition and
the readings are taken at regular intervals for every ten minutes
 When the temperature shows a steady state the reading is
noted and it is the maximum temperature.
 The difference between the maximum and minimum
temperature is found and the calorific value of the given fuel is
found by using the formula.

FLASH AND FIRE POINTS OF FUELS

Flash point is the lowest temperature at which the fuel gives off
enough vapours that ignite for a moment, when a small flame is
brought near it. Fire point is the lowest temperature at which the
vapours of the oil burn continuously for at least 5 seconds when a
tiny flame is brought near it. In most cases fire points are 5C to 40C
higher than the flash point.
Cloveland open cup flash-point apparatus

 The fuel under examination is filled upto the mark in the oil cup
and then heated by heating the water-bath by a burner.
 Stirrer is worked between tests at a rate of about 1 to 2
revolutions per second.
 Heat is applied so as to raise the oil temperature by about 5C
per minute.
 At every 1C rise of temperature, flame is introduced for a
moment by working the shuttle.
 The temperature at which a distinct flash ( a combination of a
weak sound and light) appears is noted and is the flash point. 6.
The heating is continued thereafter and the test-flame is
applied as before.
 When the oil ignites and continues to burn for atleast 5
seconds, the temperature reading is noted and is the fire point.
Penskey-Maretn’s closed type apparatus

•The Pensky –Marten apparatus consists of a brass cup

mounted in an air bath and heated by a gas flame. •A
propeller-type stirrer, operated by a flexible drive, extends
from the center of the cover into the cup.
•The cover has four openings: one for a thermometer and
the others fitted with sliding shutters for the introduction of
a pilot flame and for ventilation.
•The temperature of the oil in the cup is raised at a rate of 5–
6°C/min.
•The stirrer is rotated at approximately 60 rpm. •When the
temperature has risen to approximately 15°C from the
anticipated flash point, the pilot flame is dipped into the
oil vapor for 2s for every 1°C rise in temperature
upto105°C.
•Above 105°C, the flame is introduced for every 2°C rise in
temperature.
•The flash point is the temperature at which adistinct flash is
observed when the pilot flame meets the vapor in the cup.
•The temperature at which a distinct flash ( a combination
of a weak sound and light) appears inside the cup is
noted and is the flash point.
•The heating is continued thereafter and the test-flame is
applied as before.
•When the oil ignites and continues to burn for atleast 5
seconds, the temperature reading is noted and is the fire
point.

Cloud & Pour Point

1. Refrigerated bath
2. sample fuel / lubricating oil
3. Thermocouple to m0easure the sample temperature.

•Pour the sample into the test jar to the level mark.
•Close the test jar tightly by the cork carrying the test
thermometer. Adjust the position of the cork and the
thermometer so that the cork fits tightly, the thermometer
and the jar are coaxial, and the thermometer bulb is resting on
the bottom of the jar.
•Place the test jar in the refrigerated apparatus.
o
•At each test thermometer reading that is a multiple of 1 C,
remove the test jar from the jacket quickly but without
disturbing the specimen, inspect for cloud, and replace in the
jacket. This complete operation shall require not more than 3
s.  Report the cloud point, to the nearest 1 oC, at which any
cloud is observed at the bottom of the test jar, which is
confirmed by continued cooling. A wax cloud or haze is always
noted first at the bottom of the test jar where the temperature
is lowest. A slight haze throughout the entire sample, which
slowly becomes more apparent as the temperature is lowered,
is usually due to traces of water in the oil. Generally this water
haze will not interfere with the determination of the wax cloud
point.
•Further cooling the sample will reduce the temperature of the
sample. Temperature at which no flow is observed is noted as
pour point.
DISTILLATION

• ASTM distillation
• Thermometer
• Measuring Jar
• Electric Heater

• The ASTM distillation apparatus is cleaned thoroughly and

100ml of the oil sample is filled in the conical flask.
• A thermometer is inserted into the flask to measure the
temperature of the oil. The setup is placed on a heater and is
heated.
• The temperature of the vapour when the first drop of
condensate drops from the condenser is recorded as initial
boiling point.
• The vapour temperature is also recorded for each successive
10% collected.
• The temperature of the vapour when the last drop of
condensate drops from the condenser is noted and is the
final boiling point.
• A graph is drawn between temperature and the percentage
collected with percentage evaporated along X-axis and
temperature along Y-axis.
• The graph obtained is known as the ASTM distillation curve.
Penetrometer

 The grease sample is taken in a metal cup, which has an opening

of standard size in its bottom.
 The cup is then enclosed in a glass case, having a tight lid.
 A thermometer is also inserted in the cup, so that the bulb of
the thermometer is just above the
 surface of grease sample.
 The combination is then placed in a glass beaker, containing
water and provided with a stirrer.
 The beaker is heated slowly at a rate of 1C/minute.
 As the temperature is raised. The grease sample passes from a
semi-solid to a fluid state.
 The temperature at which the first drop falls from the opening is
recorded as drop point.
CARBON RESIDUE

 This test method covers the determination of the amount of

carbon residue formed after evaporation and pyrolysis of
petroleum materials under certain conditions and is
intended to provide some indication of the relative coke-
forming tendency of such materials.

 Also in diesel fuel, the presence of alkyl nitrates, such as amyl

nitrate, hexyl nitrate, or octyl nitrate, causes a higher carbon
residue value than observed in untreated fuel, which may lead
to erroneous conclusions as to the coke-forming propensity of
the fuel.

 This Test Method detects the presence of alkyl nitrate in the

fuel.
 Indicates the tendency of the fuel to form carbonaceous
deposits. Lubricating oils containing a good percentage of
carbon in combined state.

 Carbon residue percentage in an oil is proportional to the

amount of carbon deposited in the combustion chamber.

 In addition to carbon residue, however, other conditions in the

engine also influence the carbon deposits. The determination of
carbon residue is carried out either by conradson or Rams
bottom method.

 The amount of carbonaceous residue remaining after

thermal decomposition of petroleum, a petroleum fraction, or
a petroleum product in a limited amount of air; also called the
coke-or carbon –forming propensity; often prefixed by the
terms Conradsonor Rams bottom in reference to the inventors
of the respective tests.

 The carbon residues of petroleum and petroleum products

serve as an indication of the propensity of the sample to
form carbonaceous deposits (thermal coke) under the influence
of heat.
Vapour Pressure testing equipment

The vapor pressure of petroleum or a petroleum product is

the force exerted on the walls of a closed container by the
vaporized portion of a liquid. Conversely, it is the force that
must be applied to the liquid to prevent it vaporizing
further. The vapor pressure increases with increase in
temperature and is variously expressed in terms of
millimeters of mercury, pounds per square inch, or other
equivalent units of pressure depending on common usage.
Gasoline vapor pressure depends critically on its
butanecontent, and in there finery the final adjustment of
vapor pressure of a gasoline to meet the specification is of
tenmade by butane injection.

REIDVAPORPRESSURE
The Reid vapor pressure (ASTMD 323, IP69,IP402 ) is a
measure of the vapor pressure of petroleum or a
petroleum product an oil at 37.8°C(100°F) expressed as
millimeters of mercury. The volatility of oil sample is also
defined in terms of Reid vapour pressure. This is a measure of
the vapour pressure of an oil at 38C expressed as millimeters
of mercury or in pounds per square inch and indicates the
initial tendency of a fuel to vapour lock. The reid vapour
pressure test apparatus consists of two chambers namely air
chamber and fuel chamber. Thevolume ratio of fuel and air
chamber is 4:1.
The apparatus used to determine the Reid vapor pressure
consists of a metal cylinder, or bomb, fitted with an accurate
dial pressure gauge or a mercury manometer. The bomb
consistsof two parts, an upper expansion chamber and a
lower liquid chamber. The sample is cooled and poured into
the lower chamber until it is full. The temperature of the
air in the upper chamber is taken, and the two chambers
are connected together in a gas-tight manner. The bomb is
immersed upright in a water bath at 37.8°C and shaken
repeatedly until a constant pressure reading is obtained. This
is corrected, from tables, for initial air temperature and
pressure.

ANILINEPOINT
The aniline point of an oil is defined as the minimum
temperature at which equal volumes of aniline
(C6H5NH2)and the oil are miscible, i.e. for masingle phase up
on mixing.

Two pyrex test tube i) 25 mm in diameter and 150mm in

length ii) 38 mm in diameter and 175 mm in length Thermo
meters graduated as i) -38to42°C ii) 25to105°C iii)90to170°C
Two 10 mls. Pipets, one provided with a suitable, rubber bulb
for handling aniline.

 Dry the sample by shaking for about 2 minites with an

hydrous sodium sulfate.
 Clean and dry the apparatus •Pipet 10mls. Of aniline and
10ml so f the sample into the jacketed test tube fitted
with stirrer and thermometer.
 If the material is too viscous to pipet, weigh a
quality of the sample corresponding to 10mls. At
room temperature in the test tube.
 Place the thermo meter in the test tube at the proper
level of immersion, making sure that the bulb does not
touch the side of the tube.
 Stir the mixture rapidly. Continue stirring, and allow
the mixture to cool slowly.
  The temperature at which the mixture becomes cloudy
throughout, with the separation of the aniline and oil
into discernible layers, is the aniline point of the oil.
Average of various tests is taken.

COPPER STRIP CORROSION TEST

Crude petroleum contains sulfur compounds, much 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 corrosive 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
corrosive test is designed to assess the relative degree of corrosivity
of a petroleum product.
  Place 30 ml clean sample into chemically clean, dry (25
diameter 150 mm length) test tube.
 Place the polished copper strip into the sample tube.
 Carefully slide the sample tube into the test bomb and screw
the lid on tightly.
 Completely immerse the bomb in a boiling water bath at
100±1oC for diesel and 50±1oC for petrol.
 After 120±5 minutes in the bath, withdraw the bomb.

ASH CONTENT TEST

 An Ash test is used to determine if a material is filled. The test
will identify the total filler content. It cannot identify individual
percentages in multi-filled materials without additional test
procedures being performed. An ash test cannot be used to
determine the percent carbon fiber or percent carbon black since
carbon burns off during the Ash test.

An Ash test involves taking a known amount of sample, placing

the weighed sample into a dried / pre-weighed porcelain crucible,
burning away the polymer in an air atmosphere at temperatures
above 500°C, and weighing the crucible after it is has been cooled to
room temperature in a desiccator. Ash residue remaining in the
crucible is considered filler unless the residue is less than 1%.
Residues of less than 1% are typically the result of additives that did
not burn off.

Cooperative Fuel Research Engine (CFR)

The Cooperative Fuel Research (CFR) engine is used extensively

throughout the world for testing, research, and instruction in the
performance of fuels and lubricants for the internal combustion
engine.

Principal design work on this prototype engine was accomplished by

engineers of Waukesha Motor Company, now a division of Dresser
Industries, who served on a Cooperative Fuel Research Committee
with representatives of the American Petroleum Institute, Society of
Automotive Engineers, Automobile Manufacturers Association, and
the National Bureau of Standards.
The first commercial CFR engine was designed and built in forty-five
days, beginning in December 1928, as a standardized single-cylinder
engine to be used for developing a gasoline knock-test method. First
effective in creating a recognized standard for defining fuel quality,
the engines are relevant today for basic research in exhaust emissions
and alternate fuels suitability. The knock test procedures originally
developed by the CFR committee are now maintained by the
American Society of Testing and Materials.

Fourier Transforms Infrared Spectroscopic (FTIR)

FT-IR stands for Fourier Transform Infrared, the preferred method of

infrared spectroscopy. In infrared spectroscopy, IR radiation is passed
through a sample. Some of the infrared radiation is absorbed by the
sample and some of it is passed through (transmitted). The resulting
spectrum represents the molecular absorption and transmission,
creating a molecular fingerprint of the sample. Like a fingerprint no
two unique molecular structures produce the same infrared
spectrum. This makes infrared spectroscopy useful for several types
of analysis.

The Sample Analysis Process

1. The Source: Infrared energy is emitted from a glowing black-body

source. This beam passes through an aperture which controls the
amount of energy presented to the sample (and, ultimately,
to the detector).
2. The Interferometer: The beam enters the interferometer where
the “spectral encoding” takes place. The resulting interferogram
signal then exits the interferometer.
3. The Sample: The beam enters the sample compartment where it is
transmitted through or reflected off of the surface of the sample,
depending on the type of analysis being accomplished. This is
where specific frequencies of energy, which are uniquely
characteristic of the sample, are absorbed.
4. The Detector: The beam finally passes to the detector for final
measurement. The detectors used are specially designed to measure
the special interferogram signal.
5. The Computer: The measured signal is digitized and sent to the
computer where the Fourier transformation takes place. The final
infrared spectrum is then presented to the user for interpretation and
any further manipulation.
A Simple Spectrometer Layout
Gas Chromatography Mass Spectrometry (GCMS Analyzer)
 The Gas Chromatography/Mass Spectrometry (GC/MS)
instrument separates chemical mixtures (the GC component)
and identifies the components at a molecular level (the MS
component).
 It is one of the most accurate tools for analyzing environmental
samples.
 The GC works on the principle that a mixture will separate into
individual substances when heated.
 The sample is injected into the GC inlet where it is vaporized
and swept into a chromatographic column by the carrier gas
(helium).
 The sample flows through the column and the compounds
comprising the mixture of interest are separated by virtue of
their relative interaction with the coating of the column
(stationary phase) and the carrier gas (mobile phase).
 The latter part of the column passes through a heated transfer
line and ends at the entrance to ion source where compounds
eluting from the column are converted to ions.
 A beam of electrons ionize the sample molecules resulting in
the formation of molecular ion and smaller ions with
characteristic relative abundances that provide a ‘fingerprint’
for that molecular structure.
 The mass analyzer separates the ions and is then detected.

Application

GC-MS is an instrument that combines the features of gas-

chromatography and mass spectrometry to identify different
organic compounds presents in the organic matter, which includes
Alkanes, Fatty acids, Alkenes, Sterols etc. GC-MS is becoming the
tool of choice for tracking organic compounds derived from variety
of plants as well as in their fossil counterpart, which may enable us
to understand evolution through time and may also help in
paleoclimate reconstruction.

Procedure

• Presently, geological samples will only be considered for the

analysis.
• The powdered sample amount should be approximately 30 gm
(finer than 100 mesh) and should be properly labeled and packed
without any contamination.
• Solid samples will be charged extra for crushing and grinding.
• Details (eg. Location, depth etc.,) of the samples should be
provided in the application.
• If available, TOC values should be provided.
• 15 samples will be considered in a single slot.
• Please make available the analysis related publications to
expedite the sample preparation related protocols.
• Explosive, poisonous and any hazardous sample giving rise to
toxic gases/fumes cannot be undertaken for analysis.
• Data generated will be provided on CD (Compact Disc) or DVD
(Digital VersatileDisc).

ASTM & SAE STANDARDS

SAE J183—Engine Oil Performance and Engine Service

Classification (Other Than “Energy-Conserving”)

SAE J304—Engine Oil Tests

SAE J1498—Marine Circuit Breakers

SAE Paper 830594—1981 CRC Diesel Fuel Low-Temperature

Operability Field Test

ASTM D 86—Method for Distillation of Petroleum Products

ASTM D 93—Test Method for Flash Point by the Pensky-Martens

Closed Tester

ASTM D 97—Test Method for Pour Point of Petroleum Oils

ASTM D 129—Test Method for Sulfur in Petroleum Products by the

Bomb Method

ASTM D 130—Method for Detection of Copper Corrosion from

Petroleum Products by the Copper Strip Tarnish Test
ASTM D 240—Test Method for Heat of Combustion of Liquid
Hydrocarbon Fuels by Bomb Calorimeter

ASTM D 287—Test Method for API Gravity of Crude Petroleum and

Petroleum Products (Hydrometer Method)

ASTM D 445—Test Method for Kinematic Viscosity of Transparent

and Opaque Liquids (and the Calculation of Dynamic Viscosity)

ASTM D 482—Test Method for Ash from Petroleum Products

ASTM D 524—Test Method for Ramsbottom Carbon Residue of

Petroleum Products

ASTM D 611—Test Method for Aniline Point and Mixed Aniline

Point of Petroleum Products and Hydrocarbon Solvents

ASTM D 613—Test Method for Ignition Quality of Diesel Fuels by

the Cetane Method

ASTM D 665—Test Method for Rust-Preventing Characteristics of

Inhibited Mineral Oil in the Presence of Water

ASTM D 975—Specification for Diesel Fuel Oils

ASTM D 976—Method for Calculated Cetane Index of Distillate

Fuels

ASTM D 1266—Test Method for Sulfur in Petroleum Products and

Liquefied Petroleum (LP) Gases (Lamp Method)
ASTM D 1298—Test Method for Relative Density (Specific Gravity)

ASTM D 1405—Method for Estimation of Net Heat of Combustion

of Aviation Fuels

ASTM D 1552—Test Method for Sulfur in Petroleum Products (High

Temperature Method)

ASTM D 1796—Test Method for Water and Sediment in Fuel Oils

by Centrifuge Method (Laboratory
Procedure)

ASTM D 2274—Test Method for Oxidation Stability of Distillate

Fuel Oil (Accelerated Method)

ASTM D 2500—Test Method for Cloud Point of Petroleum Oils

ASTM D 2622—Test Method for Sulfur in Petroleum Products (X-

Ray Spectographic Method)

ASTM D 3117—Test Method for Wax Appearance Point of

Distillate Fuels

ASTM D 3338—Method for Estimation of Heat of Combustion of

Aviation Fuels

ASTM D 4539—Filterability of Diesel Fuels by Low Temperature

Flow Test (LTFT)
 ASTM D 4737—Method for Calculated Cetane Index by Four
Variable Equation

ASTM D 5001—Test Method for Measurement of Lubricity of

Aviation Turbine Fuels by the Ball-onCylinder Lubricity Evaluator
(BOCLE)

Specification of Fules

Fuel specifications can vary depending on the type of fuel and its
intended use. Here are some general specifications for common types
of fuels:

Gasoline: Gasoline is a petroleum-derived fuel commonly used in

internal combustion engines. Its specifications can vary by country,
but typically include:

Octane rating: This measures the fuel's resistance to knocking or pre-

ignition. Most gasoline sold in the US is rated at 87, 89, or 91
octane.
Volatility: Gasoline should have a certain level of volatility to ensure
proper fuel delivery and engine performance in various weather
conditions.
Sulfur content: In many countries, regulations limit the amount of
sulfur that can be present in gasoline, as high sulfur content can
contribute to air pollution.
Diesel: Diesel fuel is also derived from petroleum and is used in
diesel engines. Its specifications typically include:

Cetane rating: This measures the fuel's ignition quality. A higher

cetane rating generally means better combustion and lower
emissions.
Sulfur content: Similar to gasoline, many countries regulate the
amount of sulfur allowed in diesel fuel.
Density: Diesel fuel is denser than gasoline, which affects its energy
content and can impact engine performance.

Natural gas: Natural gas is a fossil fuel that can be used to power
vehicles or generate electricity. Its specifications may include:

Methane content: Methane is the primary component of natural gas,

and its content can vary depending on the source.
Impurities: Natural gas may contain trace amounts of other gases,
such as carbon dioxide or nitrogen, that can affect its combustion
properties.
Compression ratio: When used as a vehicle fuel, natural gas is
typically compressed to increase its energy density. The
compression ratio can affect engine performance.
Ethanol: Ethanol is a renewable fuel made from plant materials,
such as corn or sugarcane. Its specifications can include:

Ethanol content: Most gasoline sold in the US contains some

percentage of ethanol, typically 10% (E10). Higher ethanol blends,
such as E15 or E85, may also be available in some areas.
Water content: Ethanol can absorb water, which can cause problems
in fuel systems and reduce performance.
Octane rating: Ethanol has a high octane rating, which can make it
useful in high-performance engines.