University of Petroleum and Energy Studies, Dehradun

Manual

Petroleum Product Testing Laboratory

Table of Contents

Sr. No.Experiment Page No.

1Aniline Point03

2ASTM Distillation08

3Cloud and Pour Point13

4Drop Point16

5Flash and Fire Point20

6Moisture Content24

7Penetration Index27

8Redwood Viscometer32

9Reid Vapor Pressure36

10Smoke Point40

11Rust Preventing Characteristics44

12Freezing Point48

13Vacuum Distillation51

EXPERIMENT NO. 1ANILINE POINT

AIM:

To determine the aniline point of the given petroleum product

APPARATUS REQUIRED:

Thermometer

Stirrer

Water Bath

Air jacket

Aniline and Diesel

THEORY:

Definition:

Aniline point is defined as the minimum temperature at which equal volumes of anhydrous aniline and oil mix together.

Cetane number is defined as the percentage by volume of n-cetane in a mixture of n-cetane and -methyl naphthalene.

Diesel fuels are mainly composed of paraffins and some amount of aromatics. Aromatics present in the fuel cause abnormal ignition delay. So, aniline point test is to be conducted in the fuel, thereby verifying the quality of the diesel fuel.

High aniline point indicates that the fuel is highly paraffinic and hence has a high diesel index and very good ignition quality.

Aniline being an aromatic compound, it freely mixes with aromatics. So, a low aniline point indicates low diesel index, because of high percentage of aromatics.

Diesel index is an indication of the ignition quality of a diesel fuel. Higher the diesel index better is the ignition delay of the diesel fuel.

Self ignition temperature is low for paraffins but high for aromatics. Thus a fuel rich in aromatics burns later causing ignition delay, which gives rise to diesel knock.

Heptamethyl nonane can be used in place of -methyl naphthalene. The shorter the ignition delay period higher is the cetane number of the fuel.

SIGNIFICANCE:

To verify the quality and quantity of diesel fuel.

To assess the paraffinic and aromatic content of fuel.

Ignition delay, Diesel index, Cetane number of the fuel can be calculated.

FORMULA USED:

1. Conversion of Celsius to Fahrenheit:

F= (9/5) C+32

Where, F - Temperature in Fahrenheit.

C - Temperature in Celsius.

2. API Gravity = (141.5/specific gravity)-131.5

3. Diesel index = (Aniline point * API Gravity)/100

4. Cetane number = Diesel index-3

OBSERVATION:

Miscibility temperature of aniline and sample (diesel)= C

CALCULATION:

Conversion of Celsius to Fahrenheit: F = (9/5) C+32 =

=

API Gravity = (141.5/Specific gravity)-131.5 =

=

Diesel index = (Aniline point * API gravity)/100 =

=

Cetane number = Diesel index 3

=

=

PROCEDURE:

A water bath was taken, in which the two tubes with holder and cork fitted were to be placed.

The test tube is filled with an equal volume of aniline and given sample.

A stirrer and a thermometer is inserted inside the inner tube by means of a cork.

The air bath tube is placed between the test tube and the water bath. It is left for air circulation and uniform heating.

The sample is placed in a mantle and it is started heating. With a constant stirrer the experiment was carried out.

At a constant temperature the two liquids mixes or miscibility occurs. This point of temperature is aniline point.

Diesel, aniline and water are taken in a weighed bottle one after the other and the weights are found at 15.6C by using ice.

RESULT:

The aniline point of the sample was determined and thus the diesel index and cetane number of the sample were determined.

Aniline point of the sample

=

Diesel index of the sample

=

Cetane number of the sample

=

EXPERIMENT NO.2ASTM DISTILLATION

AIM:

To determine the distillation range of the given sample at atmospheric pressure.

APPARATUS REQUIRED:

Distillation Apparatus

Thermometer

THEORY:

The function of distillation is to separate by vaporization of liquid mixture of miscible and volatile substances into individual components. Determination of distillation range and characteristics are of great value in the evaluation of the petroleum products. Distillation Parameters like boiling point, final boiling point, and Middle Boiling Point are estimated by this experiment.

SIGNIFICANCE:

For crude oil the atmospheric distillation data gives some idea of the fractions that could be collected below 300 deg. C.

For motor spirit the 10% distillation value gives an indication of engine start condition, also the high Final Boiling Point Value indicates crankcase dilution.

For diesel fuel the presence of higher boiling compounds and hence the carbon deposit formation in the engine.

PROCEDURE: The given flask is thoroughly cleaned using solvent and dried.

The given test sample is taken inside the flask and the cork with appropriate thermometer is placed on the neck of the flask.

The flask is placed on the asbestos board and fixed to the metal condenser with a cork. The asbestos board is raised or lowered till the flask is properly supported.

The 100 cc measuring cylinder is placed below the condenser outlet.

Heater is switched ON and the temperature variation is noted. The temperature at which the first drop of distillate is collected in the measuring cylinder is noted and reported as the initial boiling point.

Heat is controlled so that the distillation proceeds at a uniform rate

Middle boiling point is the temperature at 50% of oil distillates off.

The volume of residue left after the distillation is measured and reported as non-volatile substance.

OBSERVATIONS:

The Temperature at which First Drop Fall

The Temperature at which Middle Drop Fall

Percentage of Recovery

Percentage of Non Volatile Residue

The Temperature at which Final Drop Fall

Distillation Apparatus Schematic DiagramRESULT:

The distillation characteristics of the given test sample is studied and reported below, Initial Boiling Point

Mid Boiling Point

Final Boiling Point

Percentage of Recovery

Percentage of Non Volatile Residue

EXPERIMENT NO.3

Cloud and pour point

aim:

To determine the cloud point and pour point of the given sample.

APPARATUS REQUIRED:

Constant temperature bath Thermometer Flat bottomed test tubeDEFINITION:

Cloud point:

The cloud point of petroleum is the temperature at which a cloud or haze of crystals appear at the bottom of the test jar, when the sample is cooled under prescribed conditions.

Pour point:

Pour point is the lowest temperature expressed in multiples of 3 0C at which the oil is observed to flow when cooled and examined under prescribed conditions.

theory:

The cloud point and the pour point are related to the flow conditions of crude and its products at low temperature.

The cloud point gives the rough idea of the temperature above which the oil can be handled safely, without any fear of congealing or filter clogging.

The pour point is determined to estimate the temperature at which a sample of oil becomes sufficiently solid to prevent its movement by pumping.

The pour point temperature depends to a large extent on the thermal history of the sample. Also the pour point indicates the waxy nature of the sample.

PROCEDURE: Oil is poured into the test jar up to the level mark of 51 to 57 mm. If necessary the oil is heated until it is sufficiently enough to flow.

The test jar is closed with the cork carrying the thermometer. The cork position is adjusted to make it fit properly into the tube.

The thermometer bulb is immersed so that the beginning of the capillary is 3mm below the oil surface.

The test jar surrounded by the air jacked is kept in the freezing mixture and it is allowed to cool.

The falling temperature was observed with every degree fall of temperature in the given sample. The tube was withdrawn from the air jacket for a moment of about (2-3sec) and examined. It was then replaced immediately.

The temperature at which the cloudiness appeared was noted as the cloud point.

The test tube was cooled continuously. The test tube was withdrawn often for 5 0C fall of temperature to observe the flow or pour point of the sample.

The temperature at which the oil does not flow in the tube even when kept horizontal for 5sec is recorded as pour point.

STANDARD POUR POINTS OF CRUDES USED IN INDIA:Sl.No. Crude namePour point degC

1.Ankleshwar18

2.North/Gujarat27

3.Bombay high30

4.Basrah-15

5.UMM Shaiff-15

6.High speed diesel6

RESULT:

Thus the pour point of the given sample was found.

(i) The cloud point of the sample _____0C.

(ii) The pour point of the sample _____0C.

EXPERIMENT NO. 4

DROP POINT

AIM:

To determine the drop point of the given sample.APPARATUS REQUIRED: Drop Point Tube

Drop Point Cup

Thermometer

Stirrer Stand

THEORY: Drop point is the temperature which the given sample drops its characteristics physically. It may also define as the temperature at which the thickener is so soluble in the base oil that the sample become substantially fluid.

Clay and dye thickened greases have no measurable drop point. It cannot be used to which upper operating temperature limit for grease the drop point is the temperature at which the greases gives a drop.

SIGNIFICANCE:

Drop point is the most important test for the petroleum products. It is used find the lubricant property of the given sample (Bitumen, Wax, and Grease).Drop point is also used to know the viscosity of the sample.PROCEDURE:

The appropriate beaker is taken and filled with a portion of water.

The given sample is filled in the Drop point Cup and fixed inside the Drop point tube.

The tube is kept inside the water bath. The water bath is heated electrically.

The thermometer is inserted in a beaker to note the temperature.

As the temperature increases, the sample gets melted and becomes liquid

The temperature at which the semisolid substance becomes liquid is noted and recorded.

RESULT:

The Drop points of the given samples are determined as follows,

SAMPLE I

SAMPLE II

SAMPLE III DROP POINT APPARATUS

EXPERIMENT NO. 5FLASH AND FIRE POINT

AIM:

To determine the flash and fire point of given samples.

THEORY:

Flash point and fire point can be taken as an indirect measure of volatility of products.

Flash point:

The flash point is the lowest temperature at which application of test flame causes the vapor above the oil to ignite.

Fire point:

The fire point is the lowest temperature at which the oil ignites and continues to burn for 5 seconds.

The determination of flash point of petroleum products consists of heating a given volume of liquid at standard rate of temperature rise until vapors is product to such a degree as to give a flammable mixture with air in an enclosed space or with air in an open cup, ignition resulting from the application of a small flame.

APPARATUSSAMPLE USEDRANGE ( O C )

Abel apparatusPetroleum Products 19-49

Pensky-Martens

(closed cup)Fuel oils and lubricating oils, bitumen other than cutback bitumen.>49

Cleveland

(open cup)Petroleum products except fuel oils Napthene > Iso paraffin > Paraffin.

PROCEDURE:

The sample which is to be tested for smoke point was filled in the candle socket.

The candle socket with wick was placed inside the apparatus.

The wick had ignited and height of the flame without smoke was adjusted.

The reading was noted in the scale and the experiment was repeated for different gives samples.

RESULT:

The smoke point of the given samples were observed and tabulated.

S.No.Sample

Smoke point (mm)

OBSERVATION: S.No.Sample

Smoke point (mm)

SMOKE POINT APPARATUS

EXPERIMENT NO. 11 RUST PREVENTING CHARACTERISTICS

Aim: To 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.

Apparatus: Rusting test apparatus which consists of an oil bath, beaker with cover, stirrer, test rod assembly, oven, thermometer etc.

Reagents and Materials: Distilled water, ISO VG 32 oil, tissue paper, ASTM precipitation naphtha or isooctane. Significance and Use: In many instances such as in the gears of steam turbine, water can become mixed with the lubricant and rusting of ferrous parts can occur. This test indicates how well inhibited mineral oils aid in preventing this type of rusting. This test method is also used for testing hydraulic and circulating oils, including heavier-than-water fluids. It is used for specification of new oils and monitoring of in-service oils.

Summary of the Test Method:

A mixture of 300 mL of the oil under test is stirred with 30 mL of distilled water at a temperature of 60+-10C with a cylindrical steel test rod completely immersed therein. It is recommended to run the test for 4 hr. The test rod is observed for signs of rusting.

Apparatus:

Oil bath: A thermostatically controlled liquid bath capable of maintaining the test sample at a temperature of 60+_10C. An oil having a viscosity of approximately ISO VG 32 is suitable for the bath. The bath shall have a cover with holes to accommodate the test beakers.

Beaker: A 400 mL, Berzelius-type, tall-form heat resistant glass beaker without pourout.

Beaker Cover: A flat beaker cover of glass or polymer, kept in position by suitable means such as a rim or groove. Two holes shall be provided on any diameter of the cover; one for a stirrer and the other for the test rod assembly. In addition a third hole for a thermometer.

Stirrer: A stirrer constructed entirely from stainless steel in the form of an inverted T.

Stirring Apparatus: Capable of maintaining a speed of 1000+-50 rpm.Oven: Capable of maintaining a temperature of 650C.

Procedure:

1] Clean the beaker in accordance with good laboratory procedure, wash with distilled water and dry in an oven.

2] Clean glass beaker cover and a glass stirrer by the same procedure.

3] Pour 300 mL of the oil to be tested into the beaker and place the beaker in the oil bath held at a temperature that will maintain the oil sample at 60+_10C.

4] Insert the beaker into 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.

5] Cover the beaker with the beaker cover with the stirrer in position in the proper opening.

6] Adjust the stirrer so that the shaft is 6 mm off center in the beaker containing the oil sample and the blade is not more than 2 mm from the bottom of the beaker.

7] Suspend the thermometer through the hole in the cover .

8] Start the stirrer and when the temperature reaches 60+_10C, insert the steel test rod such that its lower end is 13 to15 mm from the bottom of the beaker.

9] Continue stirring for 30 min to ensure complete wetting of the steel test rod.

10] With the stirrer in motion, remove the thermometer temporarily and add 30 mL of distilled water through its hole and replace thermometer.

11] Continue stirring at a speed of 1000+-50 rpm for 4 h from the time water was added, maintain the temperature of the oil-water mixture at 60+_10C.

12] Stop stirring at the end of the 4-h period, remove the test rod, allow to drain and then wash with ASTM precipitation naphtha or isooctane.

Interpretation of Results:1] Perform all inspections at the end of the test to determine the condition of the test rod without magnification under normal light. A rusted test rod is one on which any rust spot or rust streak is visible.

2] In order to report an oil as passing or failing, conduct test in duplicate.

3] Report an oil as passing the test if both test rods are rust-free at the end of the test period.

4] Report an oil as failing the test if both test rods are rusted at the end of the test period.

5] If one test rod is rusted while the other is free of rust, test two additional test rods. If either of these latter test rods shows rusting, report the oil as not passing the test.

Result:

Thus, the oil passes/fails the test. Rusting Test Apparatus EXPERIMENT NO. 12

FREEZING POINT

Aim: To determine the freezing point of Aviation fuels.Apparatus: Freezing point apparatus consisting of jacketed sample tube, collars, stirrer, vacuum flask, thermometer etc.

Significance and Use: The freezing point of an aviation fuel is the lowest temperature at which the fuel remains free of solid hydrocarbon crystals that can restrict the flow of fuel through filters if present in the fuel system of the aircraft. The temperature of the fuel in the aircraft tank normally falls during flight depending on aircraft speed, altitude and flight duration. The freezing point of the fuel must always be lower than the minimum operational tank temperature.

Reagents and Materials: Carbon dioxide (Solid) or dry ice for use in the cooling bath

Procedure:

1] Measure out 25+-1 mL of the fuel and transfer it to the clean, dry, jacketed sample tube.

2] Close the tube tightly with the cork holding the stirrer, thermometer and moisture proof collar and adjust the thermometer position so that its bulb does not touch the walls of the tube flask and is approximately in the center. The bulb of the thermometer should be 10 to 15 mm from the bottom of the sample tube.

3] Clamp the jacketed sample tube so that it extends as far as possible into the vacuum flask containing the cooling medium. The surface of the sample should be approximately 15 to 20 mm below the level of the coolant.

4] Stir the fuel continuously, moving the stirrer up and down at the rate of 1 to 1.5 cycles/s, except when making observations, taking care that the stirrer loops approach the bottom of the flask on the downstroke and remain below the fuel surface on the upstroke.

5] Disregard any cloud that appears at approximately -100C and does not increase in intensity as the temperature is lowered, because this is due to water.

6] Record the temperature at which crystals of hydrocarbon appear.

7] Remove the jacketed sample tube from the coolant and allow the sample to warm, stirring it continuously at 1 to 1.5 cycles/s.

8] Record the temperature at which the hydrocarbon crystals completely disappear.

Result: Thus, the freezing point of the given sample is ------------

Freezing Point Apparatus

EXPERIMENT NO. 13

VACUUM DISTILLATION

Aim: To determine the boiling range of a petroleum product at reduced pressure

Apparatus: Vacuum distillation apparatus

Scope: This test method covers the determination, at reduced pressures, of the range of boiling points for petroleum products that can be partially or completely vaporized at a maximum liquid temperature of 4000C.

Significance and Use: This test method is used for the determination of the distillation characteristics of petroleum products and fractions that may decompose if distilled at atmospheric pressure. This boiling range, obtained at conditions designed to obtain approximately one theoretical plate fractionation, can be used in engineering calculations to design distillation equipment, to prepare appropriate blends for industrial purposes, to determine compliance with regulatory rules, to determine the suitability of the product as feed to a refining process, or for a host of other purposes.

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

Procedure:

1. Place a 200 ml sample in the distillation flask.

2. Start the vacuum pump and observe the flask contents for signs of foaming. If the sample foams, allow the pressure on the apparatus to increase slightly until the foaming subsides. Apply gentle heat to assist the removal of dissolved gas.

3. Evacuate the apparatus until the pressure reaches the level prescribed for the distillation. Failure to reach the distillation pressure or the presence of a steady state increase in pressure in the apparatus with the pump blocked off, is evidence of significant leakage into the system. Bring the system to atmospheric condition using a nitrogen bleed and relubricate all joints. If this does not result in a vacuum-tight system, examine other parts of the system for leaks.Note: The most commonly prescribed pressure is 1.3 kPa (10 mm Hg).

4. After the desired pressure level has been attained, turn on the heater and apply heat as rapidly as possible to the flask, without causing undue foaming of the sample. As soon as vapor or refluxing liquid appears at the neck of the flask, adjust the rate of heating so that the distillate is recovered at a uniform rate of 6 to 8 mL/min.

5. Record the vapor temperature, time, and the pressure at each of the following volume percentage fractions of the charge collected in the receiver : IBP, 5, 10, 20, 30, 40, 50, 60, 70, 80, 90, 95and at the end point.

6. If a sudden increase in pressure is observed, coupled with the formation of white vapors and a drop in the vapor temperature, the material being distilled is showing significant cracking. Discontinue the distillation immediately and record the fact on the run sheet. If necessary, rerun the distillation with a fresh sample at lower operating pressure.

7. Lower the flask heater 5 to 10 cm and cool the flask and heater with a gentle stream of air or, preferably, with a stream of carbon dioxide. Repressure the contents of the still with dry nitrogen if it is necessary to dismantle the apparatus before it has cooled below 2000C.Warning: Repressuring the contents of the still with air while it contains hot oil vapors can result in fire explosion. It is recommended to discontinue the distillation at a maximum vapor temperature of 3500C.8. Bring the temperature of the cold trap mounted before the vacuum source back to ambient temperature. Recover, measure, and record the volume of the light products collected in the trap.

Warning: If there is a large air leak in the system and liquid nitrogen is used as the coolant, it is possible to condense air (oxygen) in the trap. If hydrocarbons are also present in the trap, a fire or explosion can result when the trap is warmed up.9. Remove the receiver and replace with another.

10. Convert the observed vapor temperature readings to Atmospheric Equivalent Temperatures (AET) using Tables 1 through 6 or the equations in Annex A7 given in the company manual.11. Report the AET to the nearest degree Celsius corresponding to the volumetric percentages of liquid recovered in the receiver.

Important Notice: In order to avoid any accident due to fire explosion, you are requested to read the above procedure very carefully and also refer to the company manual supplied with this setup for further clarifications, if any.Result: Thus, the Boiling Range of given petroleum product is -----------.

Vacuum Distillation Apparatus

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THERMOMETER

RUBBER CORK

SAMPLE CUP

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2

_1221460548.ppt

Needle Penetration

Gauge in tenths of mm

Needle Release Mechanism, 5 seconds

Loaded Weight to 100g

Standard Penetration Needle

Asphalt Sample at 250 C

_1222633648.ppt

Aniline PointApparatus

_1221365369.ppt

Vapour Pressure (Reid Method)

Gauge

Constant Temperature Bath

Temperature Controller

Stirrer

_1221367936.ppt

_1221365022.ppt

Vapour Pressure (Reid Method)

Gauge

Connector

Sample Container

Barrel

Connector

_1221206369.ppt

Chimney

Scale

Flame

Lamp

Stand

Lamp Holder

Flame Shape