Index PAGE Test Name: Test Method

No
1 2 Specific Gravity ASTM: D 1298-85
2 4 Flash Point (Open Cup & closed ASTM: D 92
cup)
3 6 Dean & Spark Apparatus ASTM: D 95
4 9 Centrifuge For Oil Testing ASTM: D 1796-88
5 12 Pour Point ASTM: D 97-66
6 15 Con. Carbon Residue ASTM: D 189-65
7 19 Calorific Value Test ASTM: D 240
8 23 Kinematic viscosity ASTM: D 445-85a
9 25 Ash Test ASTM: D 482-80
10 28 Acidity of Oil ASTM: D 664
11 31 Rust Preventing Characteristic ASTM: D 665
Test
12 36 Karl-Fisher Moisture Titrator ASTM: 1774

Standard Test Method for Relative Density

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(Specific Gravity)
Test Method No. ASTM -D 1298-99

Scope.
This method covers the laboratory determination of density, relative density (specific
gravity) or API gravity of crude petroleum products, and non-petroleum products
using a glass hydrometer. Values are measured on a hydrometer at convenient
temperature, readings of density being reduced to 15°C and readings of relative
density (specific gravity) and API gravity to 60°C.
Defination.
The ratio of the mass of a given volume of liquid at 15 °C to mass of an equal volume
of pure water at the same temperature.
Field of application
The hydrometer method is most suitable for the determination of density of mobile
transparent liquids. It can be also used for viscous oils by allowing sufficient time for
the hydrometer to reach equilibrium, or for opaque oils by applying a suitable
meniscus correction.
Summery of Method
The sample is brought to a prescribed temperature and transfer to a cylinder at
approximately the same temperature .The appropriate hydrometer is lowered into the
sample and allowed to settle. After temperature equilibrium has been reached, the
hydrometer reading is read, and the temperature of the sample is noted. The cylinder
and its contents may be placed in a water bath to avoid excessive temperature
variation.
Significance and Use.
Accurate determination of the density, relative density, or API gravity of petroleum
products is necessary for the conversion of measured volumes to volumes at the
standard temperature of 15°C or 60F. This is also a factor governing the quality of
petroleum and petroleum products.
Apparatus
 Hydrometer
 Thermometer
 Hydrometer Cylinder
Sampling
The fuel sample taken for the analysis must be representative of the entire
system. Good sampling procedure are key to good analysis and sample
must be taken in accordance with Practice D- 4057.
Operation
 Adjust the temperature of the sample.
 Transfer the sample to a clean hydrometer cylinder without splashing, to avoid the
formation of air bubbles. Remove any air bubbles formed, after they have
collected on the surface of the sample.
 Place the cylinder containing the sample in a vertical position. Ensure that the
temperature of the sample does not change appreciably during the time necessary
to complete the test, during this period, the temperature of the surrounding
medium should not change more than 2 °C
 Lower the thermometer gently into the sample. Continuously stir the sample with
the thermometer, taking care that the mercury thread is kept fully immersed. As
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soon as a steady reading is obtained, record the temperature of the sample to the
nearest 0.1°C and then remove the thermometer.
 Depress the hydrometer about two scale division into the liquid, and release it.
Allow sufficient time for hydrometer to come to rest, and for all air bubbles to
come to the surface. This is particularly necessary in the case of more viscous
samples.
 When the hydrometer has come to rest, floating freely away from the walls of the
cylinder, estimate the hydrometer scale reading to the nearest one-fifth of a full
scale division
 Immediately after observing the hydrometer scale value, again cautiously stir the
sample with the thermometer, record the temperature of the sample, Should not
this temperature differ from the previous reading by more than 0.5 °C. Repeat the
hydrometer test and then thermometer observation until the temperature becomes
stable within 0.5°C
Precaution.
 Keep away from heat, sparks, and open flame.
 Keep container closed.
 Use with adequate ventilation.
 Avoid prolonged breathing of vapour or spray mist.
 Avoid contact with eyes and skin.
 Use fume hood whenever possible.

Standard Test method for Flash Point by Cleveland Open

Cup & closed cup
Testing Method No. ASTM D 92-02a.

Scope.
This test method covers the determination of the flash and fire points of all petroleum
products except fuel oils and those having an open cup flash below 175F(79C).
Flash Point.
The lowest temperature at which application of a test flame causes the vapour of a
specimen to ignite under specified conditions of test.
Fire Point.
The lowest temperature at which a specimen will sustain burning for 5 sec.
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Sampling
The fuel sample taken for the analysis must be representative of the entire
system. Good sampling procedure are key to good analysis and sample
must be taken in accordance with Practice D- 4057.
Summary of Method.
The test cup is filled to a specified level with the sample. The temperature of the
sample is increased rapidly at first and then at a slow constant rate as the flash point is
approached. At specified intervals a small test flame is passed across the cup. The
lowest temperature at which application of the test flame causes the vapours above the
surface of the liquid to ignite is taken as the flash point. To determine the fire point,
the test is continued until the application of the test flame causes the oil to ignite and
burn for at least 5second.
Significance and Use.
 Flash Point measures the tendency of the sample to form a flammable mixture
with air under controlled laboratory conditions. It is only one of a number of
properties that 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.
 Flash point can indicate the possible presence of highly volatile and flammable
materials in a relatively non-volatile or non-flammable material.
 Fire point measures the characteristics of the sample to support combustion.

Apparatus.
 Cleveland Open Cup Apparatus.
This apparatus consists of the test cup, heating plate, test flame applicator, heater and
supports.
 Shield.
A shield 18 in. square and 24 in. high and having an open front is recommended.
 Thermometer.
A thermometer confirming to the requirements prescribed in specifications required.
Procedure.
 Fill the test cup with the sample to be tested to the level indicated by the level
mark.
 Set the expected flash point by digital switch. The testing range is 45- 370C.
 Press the START switch and a lamp in the switch lights is start the test that open
the solenoid valve. Expected flash point set appears for two second in the display.
Immediately open the needle valve for test flame and pilot flame a little, which
ignite the gas. Adjust the test flame size to about 4-mm in diameter.
 The sample temperature rises at a rate of 5-6C/ minute. Test flame application
starts at 20C before the expected flash point. The test flame application is repeated
every 1C, when the expected flash point is below 110C and every 2C, while
expected temperature is above 110C.
 When the flash point is detected, the temperature display is held and begins to
flicker. At the same time buzzer intermittently sounds for four second to notify the
flash. Further the stove begins to be cooled (the COOL lamplight) and solenoid
valve for gas is closed.
 Cooling stops after ten minute (the Cool lamp goes off). One cycle of the test is
completed at this moment.
Precaution.
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 Keep away from heat, sparks, and open flame.
 Keep container closed.
 Use with adequate ventilation.
 Avoid prolonged breathing of vapour or spray mist.
 Avoid contact with eyes and skin.
 Use fume hood whenever possible.
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Standard Test Method for Water in Furnace Oil by

Distillation with Dean Stark Apparatus.
Testing Method No. ASTM D 95 -99

Scope.
This test method covers the determination of water in petroleum products, tars and
other bituminous materials by the distillation method.
Summary of Method.
The material to be tested is heated under reflux with a water-immiscible solvent,
which co -distills with the water in the sample. Condensed solvent and water are
continuously separated in a trap, the water settling in the graduated section of the trap
and the solvent returning to the still.
Significance and Use.
Knowledge of the water content of petroleum products is important in the refining,
purchase, sale and transfer of products.
The amount of water as determined by this method (to the nearest 0.05 volume %)
shall be used to correct the volume involved in the custody transfer of oil.
Solvent-carrier Liquid.
A solvent-carrier liquid appropriate to the material being tested shall be used. The
following aromatic solvents are acceptable.
 Industrial grade Xylene.
 Petroleum or Coal tar Naphtha.
 Toluene.
APPARATUS
 500 ml round bottom flask
 graduated reflex tube
 graduated cylinder 100-ml
 long condenser
 solvent (toluene)
Sampling
The fuel sample taken for the analysis must be representative of the entire
system. Good sampling procedure are key to good analysis and sample
must be taken in accordance with Practice D- 4057.
Scope.
This practice covers procedure for obtaining representative samples of stocks or
shipment of uniform petroleum products.
Summary of practices.
A basic sampling method is available, tank sampling, which is covered in
this practice
1. Tank sample will be representative if the tank contents are homogenous from top
to bottom. This is rarely the case in actual practice. However, tank sample is
acceptable if all of the following conditions prevail.
2. The tank contains a heavy component (such as water) that clearly separate from
the main component and
3. The tank is equipped with either a swing suction or a weir on the outlet that
prevents any shipment of the heavy component; and
4. The tank samples are taken so that none of the heavy component is included.
Significance and Use.
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Sampling of petroleum and petroleum products are examined by various method of
test for the determination of physical and chemical characteristic. The result often
used for custody transfer and pricing determination. It is accordingly necessary that he
samples be representative of the petroleum products in question.
Collection of Sample.
Uniform petroleum product.
One in which spot sample from top, upper, middle, lower and outlet agree within the
precession of the laboratory tests.
Representative sample.
A sample representing a small portion of its total volume of material (for example
tank, ship, compartment, container and pipe line tenders) obtained with a precision
equal to or better than the precision of the laboratory method by this sample is to be
analysed.
All-level sample.
A sample obtained by submerging a stoppered beaker or bottle from a point as near as
possible to the draw-off level, then opening the sampler and raising it at a rate such
that it is about three-fourth full as it emerges from the liquid. An all-level sample is
not necessarily a representative sample because the tank volume may not be
proportional to depth.
Running Sample.
A sample obtained by lowering an unstoppered beaker or bottle from the top of the oil
to the level of the bottom of the outlet connection and returning it to the top of the oil
at a uniform rate of speed such that beaker or bottle is about three-fourth full when
withdrawn from the oil. The rate of filling is proportional to the square root of the
depth of immersion.
Apparatus.
Sample Containers may be clear or brown glass bottles or can. The clear bottle is
examined easily and brown glass bottle affords some protection
from sunlight. Plastic Bottles made of suitable unpigment linear polythene may be
used for the handling and storage of gas oil. Fuel oil and lubricating oil.
Procedure
 Mix the sample thoroughly. Measure exactly sample in graduated cylinder and
transfer it to the still. Take 100 ml of the solvent in other graduated cylinder.
Rinse the material adhering to the cylinder with one 50 ml and two 25-ml portion
of the solvent Drain the cylinder thoroughly after the sample transfer and each
rinsing.
 Connect the trap to the still and the condenser to the trap. Plug loosely the top, of
the condenser with cotton to avoid humidity.
 Apply heat to still, adjusting the rate of boiling by the change over switch so that
condensed distillate discharge from the condenser at the rate of 2 to 5 drops/sec.
 Continue distillation until no water is available in any part of the apparatus except
in the trap and the volume of water in the trap remains constant for 5 min.
 When the evolution of the water is complete, allow the trap and contents to cool
room temperature. Dislodge any drops of water adhering to the sides of the trap
with a wire or a glass rod and transfer them to the water layer. Read the volume of
the water in the trap.
Calculation.

P = W1 –W2 * 100
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W3
P: Water content (%)
W1: volume of the water in the trap ,ml
W2: volume of the water in Solvent ,ml
W3: volume of test sample , ml

Precaution.
 Keep away from heat, sparks, and open flame.
 Keep container closed.
 Use with adequate ventilation.
 Avoid prolonged breathing of vapour or spray mist.
 Avoid contact with eyes and skin.
 Use fume hood whenever possible.
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Standard Test Method for Water and Sediment in fuel Oil

by Centrifuge Method.
Testing Method No. ASTM D 1796 -97.

Scope
This method describes the laboratory determination of water and sediment in crude
oils by means of the centrifuge procedure. The amount of water detected in this
method is almost always lower than the actual water content.
Summary of Method.
Equal volume of crude oil and water saturated toluene are placed into a cone –shaped
centrifuge tube. After centrifugation, the volume of the higher gravity water and
sediment layer at the bottom of the tube is read.
Significance and Use.
The water and sediment content of crude oil is significant because it can cause
corrosion of equipment and problems in processing. A determination of water and
sediment content is required to measure accurately net volumes of actual oil in sales,
taxation, exchanges and custody transfers.
Apparatus.
Centrifuge Machine
A centrifuge capable of spinning two or more filled cone-shaped, 203-mm centrifuge
tubes at a speed that can be controlled to give a relative centrifugal force of a 1000
rpm at the tip of the tubes shall be used. It should be capable of maintaining the
sample temperature during the entire run at 60+_ 3C.
Centrifuge tubes.
Each centrifuge tube shall be a 230-mm cone shaped tube and made of thoroughly
annealed glass. The graduation number shall be clear and distinct, and the mouth shall
be constricted in shape for closure with a cork.
Bath.
The bath shall be either a solid metal block bath or liquid bath of sufficient depth for
immersing the centrifuge tube in the vertical position to the 100-mL mark. Means
shall be provided for maintaining the temperature at 60 +_ 3C.
Solvent.
Analytical grade of Toluene.

Sampling
The fuel sample taken for the analysis must be representative of the entire system.
Good sampling procedure are key to good analysis and sample
must be taken in accordance with Practice D- 4057.
Scope.
This practice covers procedure for obtaining representative samples of stocks or
shipment of uniform petroleum products.
Summary of practices.
A basic sampling method is available, tank sampling, which is covered in
this practice
1. Tank sample will be representative if the tank contents are homogenous from top
to bottom. This is rarely the case in actual practice. However, tank sample is
acceptable if all of the following conditions prevail.
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2. The tank contains a heavy component (such as water) that clearly separate from
the main component and
3. The tank is equipped with either a swing suction or a weir on the outlet that
prevents any shipment of the heavy component; and
4. The tank samples are taken so that none of the heavy component is included.
Significance and Use.
Sampling of petroleum and petroleum products are examined by various method of
test for the determination of physical and chemical characteristic. The result often
used for custody transfer and pricing determination. It is accordingly necessary that he
samples be representative of the petroleum products in question.
Collection of Sample.
Uniform petroleum product.
One in which spot sample from top, upper, middle, lower and outlet agree within the
precession of the laboratory tests.
Representative sample.
A sample representing a small portion of its total volume of material (for example
tank, ship, compartment, container and pipe line tenders) obtained with a precision
equal to or better than the precision of the laboratory method by this sample is to be
analysed.
All-level sample.
A sample obtained by submerging a stoppered beaker or bottle from a point as near as
possible to the draw-off level, then opening the sampler and raising it at a rate such
that it is about three-fourth full as it emerges from the liquid. An all-level sample is
not necessarily a representative sample because the tank volume may not be
proportional to depth.

Running Sample.
A sample obtained by lowering an unstoppered beaker or bottle from the top of the oil
to the level of the bottom of the outlet connection and returning it to the top of the oil
at a uniform rate of speed such that beaker or bottle is about three-fourth full when
withdrawn from the oil. The rate of filling is proportional to the square root of the
depth of immersion.
Apparatus.
Sample Containers may be clear or brown glass bottles or can. The clear bottle is
examined easily and brown glass bottle affords some protection
from sunlight. Plastic Bottles made of suitable unpigment linear polythene may be
used for the handling and storage of gas oil. Fuel oil and lubricating oil.
Procedure.
 Fill the well mixed oil sample in two centrifuge tubes to the 50 ml mark .
 Add 50 ml of the solvent (Toluene)
 Stopper the tubes tightly & shake vigorously.
 Maintain the temp. at 60 C°
 Rotate the centrifuge for 10 mints at rpm 1490.
 After 10 mints note the water contents & sediments from centrifuge tube.
Calculation.

V = V1 +V2
V= water &sediments of the sample %
V1= final volume of water &sediments per 50 ml of sample in the tube-1
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V2= final volume of water &sediments per 50 ml of sample in the tube-2

Precaution.
 Keep away from heat, sparks, and open flame.
 Keep container closed.
 Use with adequate ventilation.
 Avoid prolonged breathing of vapour or spray mist.
 Avoid contact with eyes and skin.
 Use fume hood whenever possible.
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Standard Test Method for Pour Point of Petroleum

Oil.
Testing Method No. ASTM D 97- 02.

Scope
This test method is intended for use on any petroleum oil. A procedure suitable for
black oil, cylinder stocks and non-distillate fuel oil. A procedure for testing the
fluidity of a residual oil at a specified temperature.
Summary of Test method.
After preliminary heating, the sample is cooled at a specified rate and examined at
interval of 3C° for flow characteristic. The lowest temperature at which movement of
the oil is observed is recorded as the pour point.
Significance and Use.
The pour point of petroleum oil is an index of the lowest temperature of its utility for
certain applications.
Definition
The lowest temperature at which the oil is observed to flow when cooled and
examined under prescribed condition
Apparatus
1.Test jar.
It is clear cylinder glass, flat bottom, 30-33.5 mm inside diameter, and 115-125 mm
height. To indicate sample height the jar should be marked with a line 54+_3mm
above the inside bottom.
Thermometers.
Having range –10 C° to +50 C° and should be checked immediately prior to the test
and used only if they prove accurate within +_ 1 C°.
Cork.
To fit the test jar, bored centrally for the test thermometer.
Jacket.
Metal or glass, cylindrical flat bottom, 115mm in depth,42 –50mm inside diameter. It
must be supported firmly in a vertical position in the cooling bath.
Bath.
It is maintained at prescribed temperature with a firm support to hold the jacket
vertical. The required bath temperature may be obtained by by suitable freezing
mixture. Freezing mixture commonly used for temperature down.

Sampling
The fuel sample taken for the analysis must be representative of the entire
system. Good sampling procedure are key to good analysis and sample
must be taken in accordance with Practice D- 4057.
Scope.
This practice covers procedure for obtaining representative samples of stocks or
shipment of uniform petroleum products.
Summary of practices.
A basic sampling method is available, tank sampling, which is covered in
this practice
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1. Tank sample will be representative if the tank contents are homogenous from top
to bottom. This is rarely the case in actual practice. However, tank sample is
acceptable if all of the following conditions prevail.
2. The tank contains a heavy component (such as water) that clearly separate from
the main component and
3. The tank is equipped with either a swing suction or a weir on the outlet that
prevents any shipment of the heavy component; and
4. The tank samples are taken so that none of the heavy component is included.
Significance and Use.
Sampling of petroleum and petroleum products are examined by various method of
test for the determination of physical and chemical characteristic. The result often
used for custody transfer and pricing determination. It is accordingly necessary that he
samples be representative of the petroleum products in question.
Collection of Sample.
Uniform petroleum product.
One in which spot sample from top, upper, middle, lower and outlet agree within the
precession of the laboratory tests.
Representative sample.
A sample representing a small portion of its total volume of material (for example
tank, ship, compartment, container and pipe line tenders) obtained with a precision
equal to or better than the precision of the laboratory method by this sample is to be
analysed.
All-level sample.
A sample obtained by submerging a stoppered beaker or bottle from a point as near as
possible to the draw-off level, then opening the sampler and raising it at a rate such
that it is about three-fourth full as it emerges from the liquid. An all-level sample is
not necessarily a representative sample because the tank volume may not be
proportional to depth.

Running Sample.
A sample obtained by lowering an unstoppered beaker or bottle from the top of the oil
to the level of the bottom of the outlet connection and returning it to the top of the oil
at a uniform rate of speed such that beaker or bottle is about three-fourth full when
withdrawn from the oil. The rate of filling is proportional to the square root of the
depth of immersion.
Apparatus.
Sample Containers may be clear or brown glass bottles or can. The clear bottle is
examined easily and brown glass bottle affords some protection
from sunlight. Plastic Bottles made of suitable unpigment linear polythene may be
used for the handling and storage of gas oil. Fuel oil and lubricating oil.
Procedure
 Pour the oil into the test jar to the level mark.
 Close the test jar tightly by the cork carrying the high pour thermometer
 Maintain the temperature of the cooling jacket at 0C°, test jar is placed in vertical
position in jacket
 After the oil has cooled, enough to allow the formation of paraffin wax crystal,
take care not to disturb the mass of the oil nor permit the thermometer to shift in
the oil, any disturbance will lead to low and fictitious results.
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 After cooling, at each test thermometer reading that is multiple of 3C°, remove the
test jar from the jacket carefully and tilt it just enough to ascertain whether there is
movement of the oil in the test jar. The complete operation of removal and
replacement shall require not more than 3 sec. If the oil has not ceased to flow,
transfer the jar in jacket in a second.
 Continue the test in this manner until a point is reached at which the oil in the test
jar shows no more movement when the test jar is held in a horizontal position for
5.0 sec. Record the observed reading of the test thermometer.
 Add 3 C° to the temperature recorded and report the result as the pour point.
Precaution.
 Keep away from heat, sparks, and open flame.
 Keep container closed.
 Use with adequate ventilation.
 Avoid prolonged breathing of vapour or spray mist.
 Avoid contact with eyes and skin.
 Use fume hood whenever possible.
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Standard Method of Test for Conradson Carbon

Residue of Petroleum Product.
Testing Method No ASTM D 189-01.

Scope
This method describes a procedure for the determination of the amount of carbon
residue left after evaporation and pyrolysis of oil, and is intended to provide some
indication of relative coke-forming propensities. The method is generally applicable
to relative non-volatile petroleum product, which partially decompose on distillation
at atmospheric pressure.
Significance.
It serves as a rough approximation of tendency of the fuel to form deposits in
vaporising pot-type and sleeve-type burner. The carbon residue value of gas oil is
useful as a guide in the manufacture of gas from gas oil, while carbon residue values
of crude oil residuum’s, cylinder and bright stocks are useful in manufacture of
lubricants.
Summary of Method.
A weighed quantity of sample is placed in a crucible and subjected to destructive
distillation. The residue undergoes cracking and cocking reaction during a fixed
period of severe heating. At the end of the specified heating period, the test crucible
containing the carbonaceous residue is cooled in a desiccator and weighed. The
residue remaining is calculated as a percentage of the original sample, and reported as
Conradson carbon residue.
Apparatus.
The apparatus shall consists of the following;
1. Porcelain Crucible.
Porcelain crucible wide form, glazed through out, or a silica crucible 29 to 31-
ml capacity.
2. Wire Support.
Triangle of bare nichrome wire having an opening small enough to support the bottom
of the sheet – iron crucible at the same level as the bottom of the asbestos block.
3. Burner.
Burner, Meker type, having an orifice approximately 24mm in diameter.
Sampling
The fuel sample taken for the analysis must be representative of the entire
system. Good sampling procedure are key to good analysis and sample
must be taken in accordance with Practice D- 4057.
Scope.
This practice covers procedure for obtaining representative samples of stocks or
shipment of uniform petroleum products.
Summary of practices.
A basic sampling method is available, tank sampling, which is covered in
this practice
1. Tank sample will be representative if the tank contents are homogenous from top
to bottom. This is rarely the case in actual practice. However, tank sample is
acceptable if all of the following conditions prevail.
2. The tank contains a heavy component (such as water) that clearly separate from
the main component and
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3. The tank is equipped with either a swing suction or a weir on the outlet that
prevents any shipment of the heavy component; and
4. The tank samples are taken so that none of the heavy component is included.
Significance and Use.
Sampling of petroleum and petroleum products are examined by various method of
test for the determination of physical and chemical characteristic. The result often
used for custody transfer and pricing determination. It is accordingly necessary that he
samples be representative of the petroleum products in question.
Collection of Sample.
Uniform petroleum product.
One in which spot sample from top, upper, middle, lower and outlet agree within the
precession of the laboratory tests.
Representative sample.
A sample representing a small portion of its total volume of material (for example
tank, ship, compartment, container and pipe line tenders) obtained with a precision
equal to or better than the precision of the laboratory method by this sample is to be
analysed.
All-level sample.
A sample obtained by submerging a stoppered beaker or bottle from a point as near as
possible to the draw-off level, then opening the sampler and raising it at a rate such
that it is about three-fourth full as it emerges from the liquid. An all-level sample is
not necessarily a representative sample because the tank volume may not be
proportional to depth.
Running Sample.
A sample obtained by lowering an unstoppered beaker or bottle from the top of the oil
to the level of the bottom of the outlet connection and returning it to the top of the oil
at a uniform rate of speed such that beaker or bottle is about three-fourth full when
withdrawn from the oil. The rate of filling is proportional to the square root of the
depth of immersion.

Apparatus.
Sample Containers may be clear or brown glass bottles or can. The clear bottle is
examined easily and brown glass bottle affords some protection
from sunlight. Plastic Bottles made of suitable unpigment linear polythene may be
used for the handling and storage of gas oil. Fuel oil and lubricating oil.
Procedure.
Weigh to the nearest 5-mg –10 mg of the oil to be tested in to a porcelain or
silica crucible. Place this crucible in the centre of the Skid more crucible. Apply
covers to both crucibles, one on the latter fitting loosely to allow free exit to the
vapours as formed.
 Place the bare nichrome triangle wire on stand or ring and on it the insulator. Next
centre the sheet iron crucible in the insulator with its bottom resting on the top of
the triangle, and cover the whole with the sheet iron hood in order to distribute the
heat uniformly during the process.
 Apply high heated with strong flame from gas burner, so that the pre-ignition
period will be 10 + 1.5 min. when smoke appears above the chimney, move the
burner so that the gas flame plays on the sides of the crucible for the purpose of
igniting the vapours. Then remove the heat temporarily, adjust the burner, so that
the ignited vapours burn uniformly with the flame above the chimney but not
above the wire bridge.heat may be increased, when the flame does not show above
the chimney. The period of burning the vapours shall be 13 + 1 min.
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 When the vapours cease to burn and no further blue smoke can be obtained,
readjust the burner and hold the heat to make the bottom and lower part of the
sheet iron crucible a cherry red, for 7 min. total period shall be 30 + 2 min. the
time period shall be obtained with whatever burner and gas is used.
 Remove the burner and allow the apparatus to cool until no smoke appears and
then remove the cover of the skid more crucible (about 15 min). Removes the
porcelain or silica crucible with heated tongs place in the desiccator, cool, and
weigh. Calculate the percentage of the carbon residua on the original sample.

Calculation

 Carbon residue (%) = A X 100

W
 Where:
 A = weight of carbon residue in gm,

 W= weight of sample in gm
Precaution.
 Keep away from heat, sparks, and open flame.
 Keep container closed.
 Use with adequate ventilation.
 Avoid prolonged breathing of vapour or spray mist.
 Avoid contact with eyes and skin.
 Use fume hood whenever possible.
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Standard Test Method of Calorific Value

For Fuel Oil by Bomb Calorimeter.
Testing Method No. ASTM – D 240-02/OEM

Scope.
This method covers the determination of the heat of combustion of solid and liquid
fuels. The apparatus C- 400 adiabatic calorimeter that is so easy to use and maintain
yet measures so accurately.
Summary of the procedure.
The substance to be burned is weighed in air and brought into intimate contact with an
ignition wire. The substance is burned in a bomb-calorimeter in pure oxygen at 30
bar. The burning is started by an electrical impulse through the ignition wire.
The heat evolved by burning raise the temperature of the calorimeter. Within 15
minutes after ignition the heat exchange between the bomb and surrounding inner
vessel is complete. The temperature rise is measured and is used to calculate the heat
of combustion. The value of the heat of combustion of the reference must be known
exactly. The heat evolved by combustion of the ignition wire and the production of
sulphuric acid or nitric acid must be taken into account in the calculation.
The Adiabatic Principle.
The heat evolved by combustion warms the water is stirred in the inner vessel. The
temperature of the inner vessel is used as the set point of a high-sensitivity electronic
regulator. The outer vessel, of which the cover plate is included in the water circuit, is
maintained at the same temperature as the inner vessel by either heating or cooling.
So that heat is neither taken from nor given up to the inner vessel.
Sampling
The fuel sample taken for the analysis must be representative of the entire
system. Good sampling procedure are key to good analysis and sample
must be taken in accordance with Practice D- 4057.
cope.
This practice covers procedure for obtaining representative samples of stocks or
shipment of uniform petroleum products.
Summary of practices.
A basic sampling method is available, tank sampling, which is covered in this practice
5. Tank sample will be representative if the tank contents are homogenous from top
to bottom. This is rarely the case in actual practice. However, tank sample is
acceptable if all of the following conditions prevail.
6. The tank contains a heavy component (such as water) that clearly separate from
the main component and
7. The tank is equipped with either a swing suction or a weir on the outlet that
prevents any shipment of the heavy component; and
8. The tank samples are taken so that none of the heavy component is included.
Significance and Use.
Sampling of petroleum and petroleum products are examined by various method of
test for the determination of physical and chemical characteristic. The result often
used for custody transfer and pricing determination. It is accordingly necessary that he
samples be representative of the petroleum products in question.
Collection of Sample.
Uniform petroleum product.
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One in which spot sample from top, upper, middle, lower and outlet agree within the
precession of the laboratory tests.
Representative sample.
A sample representing a small portion of its total volume of material (for example
tank, ship, compartment, container and pipe line tenders) obtained with a precision
equal to or better than the precision of the laboratory method by this sample is to be
analysed.
All-level sample.
A sample obtained by submerging a stoppered beaker or bottle from a point as near as
possible to the draw-off level, then opening the sampler and raising it at a rate such
that it is about three-fourth full as it emerges from the liquid. An all-level sample is
not necessarily a representative sample because the tank volume may not be
proportional to depth.
Running Sample.
A sample obtained by lowering an unstoppered beaker or bottle from the top of the oil
to the level of the bottom of the outlet connection and returning it to the top of the oil
at a uniform rate of speed such that beaker or bottle is about three-fourth full when
withdrawn from the oil. The rate of filling is proportional to the square root of the
depth of immersion.
Apparatus.
Sample Containers may be clear or brown glass bottles or can. The clear bottle is
examined easily and brown glass bottle affords some protection
from sunlight. Plastic Bottles made of suitable unpigment linear polythene may be
used for the handling and storage of gas oil. Fuel oil and lubricating oil.

Thermal Capacity.
The thermal capacity is evaluated by combustion of the reference substance with
known heat of combustion (preferably benzoic acid).

C = HoB . mB + Qz.

t
Where

HoB = Heat of combustion of the reference in cal/g.

Pure benzoic acid is used as the primary standard, white crystalline powder.
mB. = Weight in air of the reference substance prepared for combustion (g).
Qz. = this is sum of all the extraneous quantities of heat.

Preparation of calorimeter

 Open the cover of the calorimeter.

 Check water in the outer vessel and inner vessel maintain the required quantity
with distilled water.
Preparation of the sample and Bomb for combustion.
 Remove the cover of the bomb.
 Take the oil sample in the crucible (weight of oil should be <1 gm).
 Keep the crucible in bomb crucible stand.
 Take 10 cm ignition wire and connect between oxygen tube and ignition rod
(ignition wire should be dipped in the oil sample).
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 Tight the cover of the bomb.
 Purge and fill of the oxygen in the bomb at 30-bar pressure.
 Close the cover of the calorimeter and wait 10 minutes for temperature to equalise
between the bomb and the water in the inner vessel.
 Switch on the lens illumination, read and record the temperature on the
thermometer.
Ignition.
 Set the ignition current by rotary knob (setting 5-6).
 Operate ignition switch.
 Red signal lamp will indicate the ignition, when ignition wire is burned.
 After successful ignition, the temperature of the water in the inner vessel rises and
with in 10-12 minutes the temperature is equalised between the bomb and the
water.
 Read and record the temperature.
 Open the bomb and measure the unburned ignition wire.
CALCULATION.

Ho = C x t - (QN + QS + QZ)

mP

Ho = heating value.

C = thermal capacity(benzoic acid known).

T = temperature difference( final ignition – initial ignition temp).

QN= heat evolve by formation of aqueous nitric acid.

QS = heat evolve by the formation of aq, sulphuric acid.

QZ = length of wire used x 1.4

mP = weight of oil sample.
Precaution.
 Keep away from heat, sparks, and open flame.
 Keep container closed.
 Use with adequate ventilation.
 Avoid prolonged breathing of vapour or spray mist.
 Avoid contact with eyes and skin.
 Use fume hood whenever possible
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Standard Test Method for Kinematic Viscosity of

Transparent and Opaque Liquids.

Test Method. ASTM-D 445-01

Scope.
This test covers the determination of the kinematic viscosity of liquid petroleum
products, both transparent and opaque, by measuring the time for a volume of liquid
to flow under gravity through a calibrated glass capillary viscometer. The dynamic
viscosity can be obtained by multiplying the measured kinematic viscosity by the
density of the liquid.
Kinematic Viscosity.
A measure of the resistive flow of a fluid under gravity, the pressure head being
proportional to the density, p. for any particular viscometer, the time of flow of a
fixed volume of fluid is directly proportional to its kinematic viscosity, v = n/p where
n is the dynamic viscosity coefficient. The CGS unit of kinematic viscosity is one
centimetre squared per second and is called one stokes (symbol St). The SI unit of
kinematic viscosity is one meter squared per second and is equivalent to 10000 St.
Frequently the centistokes (symbol cst) is used.
Density.
The mass per unit volume of the fluid. The CGS unit of density is one gram per
millilitre, and the SI unit of density is one kilogram per cubic meter.
Summary of test Method.
The time is measured in seconds for a fixed volume of liquid to flow under gravity
through the capillary of a calibrated viscometer under a reproducible driving head and
at a closely controlled temperature. The kinematic viscosity is the product of the
measured flow time and the calibration constant of the viscometer.
Significance and Use.
Many petroleum products are used as lubricants for bearing, gears, compressor
cylinder, hydraulic equipment, etc. the proper operation of the equipment depends
upon the proper kinematic viscosity of the liquid. Thus the accurate measurement of
kinematic viscosity and viscosity is essential to many product specification.
The kinematic viscosity of many petroleum fuels is important for their proper use, for
example, flow of fuels through pipe line, injection nozzles and orifices, and the
determination of the temperature range for proper operation of the fuel in burners.
Sampling
The fuel sample taken for the analysis must be representative of the entire
system. Good sampling procedure are key to good analysis and sample
must be taken in accordance with Practice D- 4057.
Apparatus.
Viscometer of the glass capillary type, calibrated and capable of measuring kinematic
viscosity with in the limits of precision are acceptable.
1. Viscometer holders to enable the viscometer to be suspended in a similar position
as when calibrated. The proper alignments of vertical parts may be confirmed by
using a plumb line.
2. Viscometer Thermostat and Bath.
Any transparent liquid or vapour bath may be used, provided that is of sufficient
depth that at no time during the measurement will any portion of the sample in the
viscometer be less than 20mm below the surface of the bath liquid or less than
20mm above the bottom of the bath.
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The temperature control must be such that for the range from 15 to 100C (60 to
212F) the temperature of the bath medium does not vary by more than 0.01C
(0.02F).
3. Temperature Measuring Device.
Standardised liquid thermometer of accuracy after correction of 0.02C (0.04F) can be
used.
4. Time Device.
Any time device may be used provided that the reading can be taken with a
discrimination of 0.2 sec. And that it has an accuracy within + 0.07 % when
tested over intervals of 15min.
Operation.
Fill the sample in viscometer (U-tube), put the viscometer in water bath. Wait for
time to maintain temperature at desired condition. Suck the sample with vacuum
pump. Counting the Time (T) between specified mark with stop watch. In Furnace
oil, reverse viscometer (up-ward flow) is used.
Calculation.
Viscosity (cst) = Time x Multiplying factor.
Viscometer multiplying factor.
For HSD C-150-256 = 0.03972
C-200-237 = 0.1090
C-300-500 = 0.2257
For F.Oil R-200-500 = 0.1243.

Precaution.
 Heat gently the sample at 50C
 Mix the sample top, middle and bottom thoroughly
 Again heat the sample at 50C,
 Bath temperature does not vary by more than 0.01C during operation
 Allow the oil filled viscometer to maintain in the bath long enough to reach the
test temperature this time 30 min. Should be sufficient
 Never add or withdraw a viscometer during measuring flow time.
 For viscometer calibration use standard S-60 & S-200

Standard Test Method for Ash from Petroleum Product

Testing Method No. ASTM D-482 – 00a

Scope
This method covers the determination of ash in the range of 0.001-0.180 mass
percent, from distillate and residual fuel, gas turbine fuel, crude oil, lubricating oil,
waxes and other petroleum product in which any ash forming material present are
normally considered to be undesirable impurities or contaminant.
Summar
y of Test Method.
The sample contain in a suitable vessel is ignited and allowed to burn until only ash
and carbon remain. The carbonaceous residue is reduced to an ash by heating in a
muffle furnace at 775C, cooled and weighed.
Significance and Use.
Knowledge of the amount of ash-forming material present in a product may provide
information as to whether or not the product is suitable for use in a given application.
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Ash can result from oil or water soluble metallic compound or from extraneous solid
such as dirt and rust.
Apparatus
1.Evaporating Dish.
It is made of platinum, silica, or porcelain of 90-120ml capacity.
2.Electric Muffle furnace.
It is capable of maintaining a temperature of 775C and preferably having suitable
aperture at the front and the rear so as to allow a slow natural drought of air to pass
through.
SAMPLING
The fuel sample taken for the analysis must be representative of the entire
system. Good sampling procedure are key to good analysis and sample
must be taken in accordance with Practice D- 4057.
Scope.
This practice covers procedure for obtaining representative samples of stocks or
shipment of uniform petroleum products.
Summary of practices.
A basic sampling method is available, tank sampling, which is covered in this practice
9. Tank sample will be representative if the tank contents are homogenous from top
to bottom. This is rarely the case in actual practice. However, tank sample is
acceptable if all of the following conditions prevail.
10. The tank contains a heavy component (such as water) that clearly separate from
the main component and
11. The tank is equipped with either a swing suction or a weir on the outlet that
prevents any shipment of the heavy component; and
12. The tank samples are taken so that none of the heavy component is included.
Significance and Use.
Sampling of petroleum and petroleum products are examined by various method of
test for the determination of physical and chemical characteristic. The result often
used for custody transfer and pricing determination. It is accordingly necessary that he
samples be representative of the petroleum products in question.
Collection of Sample.
Uniform petroleum product.
One in which spot sample from top, upper, middle, lower and outlet agree within the
precession of the laboratory tests.
Representative sample.
A sample representing a small portion of its total volume of material (for example
tank, ship, compartment, container and pipe line tenders) obtained with a precision
equal to or better than the precision of the laboratory method by this sample is to be
analysed.
All-level sample.
A sample obtained by submerging a stoppered beaker or bottle from a point as near as
possible to the draw-off level, then opening the sampler and raising it at a rate such
that it is about three-fourth full as it emerges from the liquid. An all-level sample is
not necessarily a representative sample because the tank volume may not be
proportional to depth.
Running Sample.
A sample obtained by lowering an unstoppered beaker or bottle from the top of the oil
to the level of the bottom of the outlet connection and returning it to the top of the oil
at a uniform rate of speed such that beaker or bottle is about three-fourth full when
 25
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withdrawn from the oil. The rate of filling is proportional to the square root of the
depth of immersion.
Apparatus.
Sample Containers may be clear or brown glass bottles or can. The clear bottle is
examined easily and brown glass bottle affords some protection
from sunlight. Plastic Bottles made of suitable unpigment linear polythene may be
used for the handling and storage of gas oil. Fuel oil and lubricating oil.

Procedure.
 Heat the evaporating dish at 700 to 800C for 10 min. cool to room temperature in
a suitable container and weigh to the nearest 0.1mg. Dish always cooled in
disecator.
 The quantity of sample to be taken will depend upon the ash content of the
material. Weigh into the dish sufficient sample or crucible ,sufficient test
specimen to the nearest 0.1 gm yield 1 to 20 mg of ash. Weigh the sample to
nearest 0.1%. Heat the dish and sample until the contents can be ignited with a
flame. Maintain at such a temperature that a sample continues to burn at a uniform
and moderate rate, leaving only ash and carbon when the burning ceases.
 Heat the residue in the muffle furnace at 775 + 25C until all carbonaceous
material has disappeared. Cool the dish to room temperature in a suitable
container and weigh to the nearest 0.1mg.
 Reheat the dish at 775 C for 20 to 30 min. Cool in a disecator and reweigh. Repeat
the heating and weighing until consecutive weighing differ by not more than
0.5mg.

Calculation

 Ash % = w * 100
-------------
W
 Where: w= weight of ash in gm,
 W = weight of sample in gm.

Precaution.

 Keep away from heat, sparks, and open flame.

 Keep container closed.
 Use with adequate ventilation.
 Avoid prolonged breathing of vapour or spray mist.
 Avoid contact with eyes and skin.
 Use fume hood whenever possible.
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Standard Test Method for Acid Number of Oil by Titration.

Testing Method No. ASTM D 974 – 02.

Scope.
This test method covers the determination of acidic or basic constituents in
petroleum products and lubricants soluble or nearly soluble in mixture of
toluene and isopropyl alcohol.
The test method may be used to indicate relative changes that occur in an oil
during use under oxidizing condition regardless of the color or other properties
of the resulting oil. Although the titration is made under definite equilibrium
condition. The method in not intended to measure an absolute acidic property
that can be used predict performance of an oil under service condition. No
general relationship between bearing corrosion and acid number is known.
Acid number.
The quantity of base expressed in mg of potassium hydroxide per gram of
sample required to titrate a sample in the solvent from its initial meter reading to
a meter reading corresponding to a freshly prepared non-aqueous basic buffer
solution.
Summary of Test method.
The sample is dissolved in a mixture of toluene and isopropyl alcohol containing
a small amount of water and titrated potentiometrically with alcoholic potassium
hydroxide. End point persistent for 5 second. Calculate acidity with given
formula.
Significance and Use.
New and used petroleum products may contain acidic constituents that are present as
additives or as degradation products formed during service, such as oxidation
products. The relative amounts of these materials can be determined by titration with
bases. The acid number is a measure of this amount of acidic substance, in the oil
always under condition of the test. The acid number is used as a guide in the quality
control of lubricating oil formulation.
Since a variety of oxidation products contribute to the acid number and the organic
acids vary widely in corrosion properties, the test can not be used to predict
corrosiveness of an oil under service condition. No general correlation is known
between acid number and the corrosive tendency of oil toward metals.

Reagent.
KOH (0.1M).
Dissolve 6.0 gm in to one litre anhydrous isopropyl alcohol
alcohol. Standardised with pure potassium acid phythalate.
Titration Solvent.
500ml Toluene +5ml demi water +495ml of anhydrous isopropyl
alcohol.
P- Naphtholbenzein.
10gm of P-Naphthalbenzene per litre of titration solvent.
Sampling.
 Collect the sample in accordance with practice D1066 as applicable.
 27
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 Use plastic or stainless steel sample bottles, provided with rubber or plastic
stoppers.
If the water being sampled is at elevated temperature, cool to less than 35C but do not
freeze.
Scope.
This practice covers procedure for obtaining representative samples of stocks or
shipment of uniform petroleum products.
Summary of practices. A basic sampling method is available, tank sampling, which is
covered in this practice
13. Tank sample will be representative if the tank contents are homogenous from top
to bottom. This is rarely the case in actual practice. However, tank sample is
acceptable if all of the following conditions prevail.
14. The tank contains a heavy component (such as water) that clearly separate from
the main component and
15. The tank is equipped with either a swing suction or a weir on the outlet that
prevents any shipment of the heavy component; and
16. The tank samples are taken so that none of the heavy component is included.
Significance and Use.
Sampling of petroleum and petroleum products are examined by various method of
test for the determination of physical and chemical characteristic. The result often
used for custody transfer and pricing determination. It is accordingly necessary that he
samples be representative of the petroleum products in question.
Collection of Sample.
Uniform petroleum product.
One in which spot sample from top, upper, middle, lower and outlet agree within the
precession of the laboratory tests.
Representative sample.
A sample representing a small portion of its total volume of material (for example
tank, ship, compartment, container and pipe line tenders) obtained with a precision
equal to or better than the precision of the laboratory method by this sample is to be
analysed.
All-level sample.
A sample obtained by submerging a stoppered beaker or bottle from a point as near as
possible to the draw-off level, then opening the sampler and raising it at a rate such
that it is about three-fourth full as it emerges from the liquid. An all-level sample is
not necessarily a representative sample because the tank volume may not be
proportional to depth.
Running Sample.
A sample obtained by lowering an unstoppered beaker or bottle from the top of the oil
to the level of the bottom of the outlet connection and returning it to the top of the oil
at a uniform rate of speed such that beaker or bottle is about three-fourth full when
withdrawn from the oil. The rate of filling is proportional to the square root of the
depth of immersion.
Apparatus.
Sample Containers may be clear or brown glass bottles or can. The clear bottle is
examined easily and brown glass bottle affords some protection
from sunlight. Plastic Bottles made of suitable unpigment linear polythene may be
used for the handling and storage of gas oil. Fuel oil and lubricating oil.
Procedure.
Take 20.0 gm sample +100ml titration solvent +0.1ml of indicator
 28
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Titrate with 0.1M KOH solution until green end point is reached that persist for 15
sec.
Blank.
Make blank titration 100ml of titration solvent and 0.1ml of the indicator
solution. Titrate with 0.01N KOH.
Calculation

Acid number. mg. of KOH /g. = ( A—B)M*56.1

W
A = ml of KOH used for sample .
B = ml of KOH used for blank.
M = Molarity of KOH solution.
W= gram of sample used.
Precaution .
This standard may involve hazardous materials, operation, and equipment. This
standard does not purport to address all of the safety problems associated with its use.
It is the responsibility of the user of this standard to establish appropriate safety and
health practices and determines the applicability of regulatory limitation prior to use.
 29
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Standard Test Method for Rust-Preventing Characteristic of

Inhibited Mineral Oil in the Presence of Water.

Testing Method No. ASTM - D 665-99.

SCOPE.
This method is evaluate the ability of inhibited mineral oils, particularly steam-
turbine oils, to aid in preventing the rusting of ferrous parts should water
become mixed with the oil. This method is also used for testing other oil, such as
hydraulic oil and circulating oil. Provision is made in the procedure for testing
heavier-than- water fluids.
Summary of Method.
A mixture of 300mL of the oil under test is stirred with 30mL of distilled water, at a
temperature of 60C(140F) with a cylindrical steel specimen completely immersed
therein. It is customary to run the test for 24hr; however, the test period may shorter
or longer. The specimen is observed for signs of rusting and, if desired degree of
rusting.
Significance and Use.
In many instances, such as in the gears of a steam turbine, water can become mixed
with the lubricant, and rusting of ferrous parts can occur. This test indicates how well
inhibited minerals oil aid in preventing this type of rusting. This method is also used
for testing hydraulic and circulating oil, including heavier than water fluids.
APPARATUS.

 OIL Bath.
A thermostatically controlled liquid bath capable of maintaining the test sample at a
temperature of 60C. The bath shall have a cover with holes to accommodate the test
beakers.
 Beaker.
A 400mL, Berzelius-type, tall-form heating resistance glass beaker without pourout,
127mm(5 in) in height measure from inside bottom and 70mm inside diameter
measured at the middle.

 Beaker Cover.
A flat beaker cover of glass. Three holes shall be provided, one for stirrer, other for
test specimen and third for thermometer.
Stirrer.
A stirrer constructed entirely from stainless steel in the form of an inverted T. A flat
blade shall be attached to a 6-mm rod in such a way that the blade is symmetrical with
the rod and has its flat surface in the vertical plane.
 Stirring apparatus.
Any convenient form of stirring apparatus capable of maintaining a speed of 1000+_
50rpm.

 Grinding and Polishing Equipment and oven.

Sampling
The fuel sample taken for the analysis must be representative of the entire
system. Good sampling procedure are key to good analysis and sample
must be taken in accordance with Practice D- 4057.
 30
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Scope.
This practice covers procedure for obtaining representative samples of stocks or
shipment of uniform petroleum products.
Summary of practices.
A basic sampling method is available, tank sampling, which is covered in
this practice
17. Tank sample will be representative if the tank contents are homogenous from top
to bottom. This is rarely the case in actual practice. However, tank sample is
acceptable if all of the following conditions prevail.
18. The tank contains a heavy component (such as water) that clearly separate from
the main component and
19. The tank is equipped with either a swing suction or a weir on the outlet that
prevents any shipment of the heavy component; and
20. The tank samples are taken so that none of the heavy component is included.
Significance and Use.
Sampling of petroleum and petroleum products are examined by various method of
test for the determination of physical and chemical characteristic. The result often
used for custody transfer and pricing determination. It is accordingly necessary that he
samples be representative of the petroleum products in question.
Collection of Sample.
Uniform petroleum product.
One in which spot sample from top, upper, middle, lower and outlet agree within the
precession of the laboratory tests.
Representative sample.
A sample representing a small portion of its total volume of material (for example
tank, ship, compartment, container and pipe line tenders) obtained with a precision
equal to or better than the precision of the laboratory method by this sample is to be
analysed.
All-level sample.
A sample obtained by submerging a stoppered beaker or bottle from a point as near as
possible to the draw-off level, then opening the sampler and raising it at a rate such
that it is about three-fourth full as it emerges from the liquid. An all-level sample is
not necessarily a representative sample because the tank volume may not be
proportional to depth.
Running Sample.
A sample obtained by lowering an unstoppered beaker or bottle from the top of the oil
to the level of the bottom of the outlet connection and returning it to the top of the oil
at a uniform rate of speed such that beaker or bottle is about three-fourth full when
withdrawn from the oil. The rate of filling is proportional to the square root of the
depth of immersion.
Apparatus.
Sample Containers may be clear or brown glass bottles or can. The clear bottle is
examined easily and brown glass bottle affords some protection
from sunlight. Plastic Bottles made of suitable unpigment linear polythene may be
used for the handling and storage of gas oil. Fuel oil and lubricating oil.
PREPARATION OF TESTING
 Set the “power” switch at “ON” and than “PILOT” lamplights to display that the
electric current flows in the apparatus.
 Set the “MOTOR” switch at “ON” to run the motor for stirring.
 31
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 When the temperature of the bath reaches the test temperature, heat for raising the
temperature is cut off automatically and then it begins to be controlled by the
control heater.
OPERATION
 Pour 300 ml of the sample oil to be tested into beaker and place the beaker in the
oil bath held at a temp. That will maintained oil sample at 60 ± 1°C
 Insert the beaker in to a hole of the bath cover and suspend in the hole with the
beaker rim resting on the bath cover.
 The oil level in the bath shall not be below the oil level in the test beaker. Cover
the beaker with the beaker cover with the stirrer in position in the proper opening.
 Adjust the stirrer so that the shaft is 6 mm off centre in the container and the blade
is within 2 mm of the bottom of the container. Then suspend a thermometer in the
hole 56 mm in depth. Start the stirrer at a speed of 1000 rpm, and at 60 ± 1 °C
insert the polished specimen into the sample oil so that it is above 13 to 15mm
bottom of the container.
 After 30 minutes stirring, added 30 ml of demi. Water through holes. Continue
stirring at a speed of 1000 rpm for 24 hours from the time when water was added.
Stopped stirring at the end of specified period, remove the specimen, allow to
drain and wash the precipitation with petroleum benzene, and then examine the
specimen for evidence of rusting.
Precaution.
 Keep away from heat, sparks, and open flame.
 Keep container closed.
 Use with adequate ventilation.
 Avoid prolonged breathing of vapour or spray mist.
 Avoid contact with eyes and skin.
 Use fume hood whenever possible.
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Standard Test Method for Water Contents in

Transparent Oil by Karl-Fischer Moisture Titrator

Scope.
This test method covers the determination of water contents in transparent oil, such as
lubricating oil ,transformer oil etc. by karl- fischer titration method
Measurement Principle.

In the karl- fischer moisture content measurement, water reacts with iodine and sulfur
dioxide in the presence of a basic substance and alcohol.

H2O +I2 +SO2 +CH3OH +3RN 2RN.HI + RN.HSO4CH3 ----(1)

When moisture content is measured in volumetric titration ,iodine is added as titrant.

In the coulometric technique, iodine is electrolytically generated out of the anolyte
which contains iodine ions.

2l l2 + 2e ---------------------------------------(2)
As the iodine is consumed ,according to formula (1) ,the twin platinum electrode
detects the iodine consumption again triggering the electrolysis to produce iodine
according to formula (2)
According to Faradays law the quantity of generated iodine consumed is proportional
to the current generated.
In formula (1) , I2 and H2O react to each other in the ratio of 1:1 . Therefore a mole of
water (18g) is equivalent to 2*96,500 coulombs;or 10.71 coulombs/1mgH 2O .Because
iodine I2 and H2O react with each other in the ratio of 1:1.the total amount of moisture
can be determined by measuring the total amount of current required for electrolysis.
Significance and Use.
Knowledge of the water content of transparent oil is important in the refining,
purchase, sale and transfer of products.
The amount of water as determined by this method shall be used to correct the
volume involved in the custody transfer of oil.
Solvent-carrier Liquid.
A solvent-carrier liquid appropriate to the material being tested shall be used. The
following solvents are used when reagents changed.
1- 5ml of catholyte solvent.
2- 100ml of anolyte solvent.

SAMPLING
The fuel sample taken for the analysis must be representative of the entire
system. Good sampling procedure are key to good analysis and sample
must be taken in accordance with Practice D- 4057.
Scope.
This practice covers procedure for obtaining representative samples of stocks or
shipment
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Summary of practices.
A basic sampling method is available, tank sampling, which is covered in
this practice
21. Tank sample will be representative if the tank contents are homogenous from top
to bottom. This is rarely the case in actual practice. However, tank sample is
acceptable if all of the following conditions prevail.
22. The tank contains a heavy component (such as water) that clearly separate from
the main component and
23. The tank is equipped with either a swing suction or a weir on the outlet that
prevents any shipment of the heavy component; and
24. The tank samples are taken so that none of the heavy component is included.
Collection of Sample.
Uniform Transparent oil.
One in which spot sample from top, upper, middle, lower and outlet agree within the
precession of the laboratory tests.
Representative sample.A sample representing a small portion of its total volume of
material (for example tank, ship, compartment, container and pipe line tenders)
obtained with a precision equal to or better than the precision of the laboratory
method by this sample is to be analysed.
All-level sample.
A sample obtained by submerging a stoppered beaker or bottle from a point as near as
possible to the draw-off level, then opening the sampler and raising it at a rate such
that it is about three-fourth full as it emerges from the liquid. An all-level sample is
not necessarily a representative sample because the tank volume may not be
proportional to depth.
Running Sample.
A sample obtained by lowering an unstoppered beaker or bottle from the top of the oil
to the level of the bottom of the outlet connection and returning it to the top of the oil
at a uniform rate of speed such that beaker or bottle is about three-fourth full when
withdrawn from the oil. The rate of filling is proportional to the square root of the
depth of immersion.
Apparatus.
Sample Containers may be clear or brown glass bottles or can. The clear bottle is
examined easily and brown glass bottle affords some protection
from sunlight. Plastic Bottles made of suitable unpigment linear polythene may be
used for the handling and storage of gas oil. Fuel oil and lubricating oil.
Procedure:
 Turn the power switch on the back panel
 PRE-TITR .wait until ready or stable indication in front diplay.
 Take the sample in syringe and weight ( W1)
 Push the START and then inject the sample through the septum
 Weight the sample syringe after the injection of sample (W2)
 When titration completed the display will indicates “W1”.Then input the weight
W1 and press the ENTER
 After this the display will indicates the weight W2,so input the weight W2 and
again press the ENTER
 The calculated result in “ppm” prints out automatically.
Precaution.
 Weigh the sample accurately.
 Keep container closed.
 Use with adequate ventilation.
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 Avoid prolonged breathing of vapour or spray mist.
 Avoid contact with eyes and skin.
 Use fume hood whenever possible.
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