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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.
Summary 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. 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
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
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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 un-Stoppard 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 un-
pigment 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.
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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).
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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.
• 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
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.
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
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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
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.
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Standard Test Method for Relative Density

(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
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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 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.
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Standard Test Method For Sulphur in Fuel Oil

by Non-Dispersive X-Ray Method.
Testing Method No. ASTM- D 4294-02.

Scope.
This test covers the measurement of sulphur in hydrocarbon such as
diesel ,naphtha, distillates, fuels oils, lubricating base oils only, and
non lead gasoline. The concentration range is from 0.015 to 5.0
weight %.
Summary of Method.
The sample is placed in the beam emitted from an X- ray source.
The excitation energy may be derived from a radioactive source or
from an X-ray tube. The resultant exited characteristic X radiation is
measured, and the accumulated count is compared with counts
from previously prepared calibration samples to obtain the sulphur
concentration in weight percent.
Significance and Use.
The quality of many petroleum products is related to the amount of
sulphur present. Knowledge of sulphur concentration is necessary
for processing purposes. There are also regulation promulgated in
federal state and local agencies that restrict the amount of sulphur
present in some fuels.
Apparatus.
Non- Dispersive X ray Fluorescence Analyser.
Removable Sample Cup equipped with replaceable X ray
transparent plastic film windows and providing a sample depth of at
least 3mm.
Display or printer that reads out in counts, percent sulphur or both.
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
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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
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.
REPARATION BEFORE MEASUREMENT
Turn on the power switch. After approximately 40 second, Ready
menu will appear.
SPECIFYING THE MEASUREMENT CONDITION
The Measurement time (MEAS TIMES), repetition count (REPEAT
TIMES), Calibration curve(CALB NO), and Concentration value unit
(UNIT) can be specified.
1. First COND key, F1 pressed with ready menu displayed,Condition
menu will appear.
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2. Using up- down cursor or left -right cursor to select measurement
time, repeat time and Calibration No..
3. Select Measurement time …………10,30,100,300,600sec.
4. Repeat time ………………………..1,3,5,10 time.
5. Calibration No ……………………..1,2,3,4,5,A.
6. Press the EXIT key ,F4 will return to the Ready menu.the
specified measurement condition can be checked on the Ready
menu.
ENTERING ID.
Only 6-digit ID can be entered for each sample.
1. when ID key, F2 is pressed with the Ready menu displayed , ID
menu will appear.
2. Press F1 key; NUM, 0—9, can be input.
3. Press F2 key; ALPH1; A to N can be input.
4. Press F3 key; ALPH2 , O to Z can be input.
5. Press ENT key;
6. Press the EXIT key, F4 will return the Ready menu.
Procedure:
• Fill the cell with the sample to be measured. Before filling the cell
it may be necessary to heat the sample so that it is easy to pour
in to the cll. Ensure that no air bubbles are present between the
cell window &the liquid sample.
• Measure each sample for recommended counting time 100
second with minimal delay.
• Repeat the measurement using a freshly prepared cell & a fresh
portion of sample.
• Obtain the average of the two readings for the sulfur contents.
Calculation:
The concentration of sulfur in the sample is automatically calculated
from the calibration curve.

NOW MEASUREMENT CONDITION COMPLETED, OPEN SAMPLE

CHAMBER COVER, INPUT SAMPLE,CLOSE CHAMBER COVER, PRESS
MEASUREMENT KEY. WAIT RESULT, AFTER 100 SEC. RESULT
PRINTED ON PAPER.

AUTOMATIC CALIBRATION.
• F3, key is pressed with Ready menu displayed, Calibration menu
will appear.

• Select calibration curves no 1, in the condition screen.

• Select DEG.A. in Calibration menu.

• Press the AUTO key, F1 to display the CAL(AUTO) menu. Specify

measurement time , and repetition count,
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• Select MEAS TIME (SEC)……..100, 300, 600.

• REPEAT TIMES. 1. 3. 5. 10.

• Press the EXEC key, F1. The CALSET VALUES menu will appear.

• Using the key pad, specify the standard values of the sample .
Starting
with STD # 1…….to ..20. (0.51%, 1.03%, 2.02%.) + press ENT.

• Press EXEC key F1, after completion of all setting. The CAL (SET
SAMPLE) menu will change.

• Open the sample chamber cover, place standard sample No. # 1

in the sample stand, close cover.

• Press the START key, F1 will display the CAL MEASURE menu and
output data to the printer.

• Put the STD # 2 and press START key, F1 data printed. After
three or four reading, graph is printed, with STD. Verses K (co
-efficient).after AUTO Calibration, you must check 1.03% STD. as
a sample to check the instrument accuracy.
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 Apparatus.
MKC-210

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/1mgH2O .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.
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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.
Scope.
This practice covers procedure for obtaining representative samples
of stocks or shipment
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.
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.
 15
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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.
• Avoid prolonged breathing of vapour or spray mist.
• Avoid contact with eyes and skin.
• Use fume hood whenever possible.
 16
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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
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
 17
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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.

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
 18
10

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).
• 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).
 19
10

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
 20
10

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.
 21
10
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.
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
 22
10

Standard Test method for Flash Point by

Cleveland Open 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.
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.
 23
10
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.
• 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.
 24
10

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
 25
10
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.
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
• Mix the sample thoroughly. Measure exactly sample in graduated
cylinder and transfer it to the still. Take 100 ml of the solvent in
 26
10
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
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.
 27
10

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.
 28
10
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.
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.
 29
10
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
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.
 30
10

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.
 31
10
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.
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.
 32
10
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.
• 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.
 33
10

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.
 34
10
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.
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
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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.
• 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 for determination

of contaminants in gas turbine and
diesel engine fuel by Rotating Disc
electrode Atom Emission Spectroscopy.
Testing Method No. ASTM - D 6728 - 01

Scope
This test method covers the determination of contaminants and
materials as a result of corrosion in gas turbine or diesel engine by
rotating disc electrode atomic emission spectroscopty.( RDE-AES)
.This test method provides a rapid at-site determination of
contaminants and corrosive elements ranging from fractions mg/kg
to hundreds of mg/kg in gas turbine and diesel engine fuels so the
fuel quality and level of required treatment can be determined.
Reference Documents
ASTM standards:
D 975 Specification for Diesel fuel oils.
D 2880 Specification for Gas turbine fuel oils.
Terminology
Definitions.
burn,-- in emission spectroscopy , to vaporise and excite a
specimen with sufficient energy to generate spectral radiation.
calibration—the determination of values of the significant
parameters by comparison with values indicated by a set of
reference standards. calibration curve—the graphical representation
of a relation ship between the assigned (known) values of standards
and the measured responses from the measurement system
Detection Limit.—The smallest concentration of an element that can
be measured for specific analysis conditions and data collection
periods.
Emission Spectroscopy.—measurement of energy spectrum emitted
by or from an object under some form of energetic stimulation, for
example light, electrical discharge, and so forth.
Contaminants. –material in fuel sample that may cause ash
deposition or high temperature corrosion.
Profiling – to set the actual position of the entrance slit to produce
optimum measurement intensity.
Standardisation –the process of re-establishing and correcting a
calibration curve through the analysis of at least tow known
standards.
Uptake rate – the amount of oil or fuel sample that is physically
carried by the rotating disc electrode into the arc of analysis.

Summery OF Test Method—A fuel test specimen is excited by a

controlled arc discharge using the rotating disc technique. The
radiant energies of selected analytical lines and a reference arc
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collected and stored by a way of photomultiplier tubes, charge
coupled devices, or other suitable detectors. A comparison is made
of the emitted intensities of the elements in the fuel test specimen
against those measured with calibration standards. The
concentration of the elements present in fuel test specimen are
calculated and displayed.
Significance and Use.
Operating experience of gas turbines and diesel engines has shown
that some of the ash forming substances present in a fuel can lead
to high temperature corrosion, ash deposition and fuel system
fouling. Ash forming materials may be in a fuel as oil soluble
metallo-organic compounds as water soluble salts or as solid foreign
contaminants. Their presence and concentration varies with the
geographical source of crude oil and they are concentrated in the
residual fractions during the refining process. Although distillate fuel
oils are typically contaminant free, ash forming material may be
introduced later in the form of salt-bearing water or by contact with
other petroleum products during transportation and storage.
Pre-conditioning of the fuel before it reaches the gas turbines and
diesel engine has become a prerequisite for installations that use
heavy petroleum , and also for sites that use light distillate fuel oils .
On-site fuel analysis to determine the extent of contaminants is an
integral part of fuel quality management program. It is used first to
determine the extent of the required treatment , and later the
effectiveness of the treatment. Fuel contamination specifications
vary among the different gas turbine manufacturer . However ,
without exception, each requires that contaminants as low as
possible.
Interference.
Spectral—Most spectral interference can be avoided by the judicious
choice of spectral lines. High concentrations of some elements can
have an interfering influence on the spectral lines used for
determining trace level of contaminants. Instrument manufacturer
usually compensate for spectral interference during factory
calibration. Aback ground correction system , which subtracts
unwanted intensities on the side of the spectral lines, shall also be
used for this purpose. When spectral interference can not be
avoided with spectral line selection and background correction , the
necessary correction will be made using the computer soft ware
supplied by the instrument manufacturer.

Viscosity Effects
Difference in viscosity of fuel sample will cause differernces in
uptake rate. The analysis will adversely affected if the test has a
different viscosity from the calibration samples. The hydrogen
486.10 nm spectral line shell be used for light fuel , and the carbon
387.10 nm spectral line shell be used for heavy fuels as an internal
reference to compensate for viscosity effects.
Particulate
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When large particle over 10 micro meter size are present , the
analytical results will lower than the actual concentration they
represent. Large particle size may not be effectively transported by
the rotating disc electrode.
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
1- Electrode Sharpener
2- Rotating Disc Electrode Atomic Emission Spectrometer.
3- Heated Ultra sonic Bath.
4- Sampling Boats
5- Emission Spectrometer (SPECTROIL / MOA)
Preparation of Apparatus
Warm-up burns—If the instrument has been idle for several hrs. , it
may necessary to conduct warm-up burns to stabilise the excitation
source .
Optical Profile.
Optical profile shall be performed if the instrument has been idle for
a extended period of time or if the temperature has shifted more
than 10 C since the last calibration ick.
Validation Check—A go/no go standardization check can be
performed with one or more samples.
Calibration
a-Factory Calibration—The operational range for each element is
established through the analysis of organometallic standards of
known concentration .A calibration curve for each element is
established and a correction factors are set.
b-Routine Standardisation—A minimum of two point routine
standardization shall be performed if the has been fail the
validation check.
Procedure.
Analyse the test specimen in the same calibration curve program
and manner as the standardization standards. New disc electrode
and a re-pointed rod electrode must be used. Anon plastic cover
should be used on specimen holder for a fuel samples that might
catch fire during the analysis . Two or three burns are made and an
average reading is reported as a analysis results.
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.