Saturday, January 12, 2013

Petroleum: Elementary Lab Testing of Petroleum Products.. by SAAD ABDUL WAHAB

 

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INDEX

  1. ASTM Color of Petroleum Products (ASTM Color Scale)
  2. Flash and Fire Points by Cleveland Open Cup Tester
  3. Calorific Value of Liquid Hydrocarbon Fuels by Bomb Calorimeter
  4. Kinematic Viscosity of Transparent and Opaque Liquids
  5. Metals by Graphite Furnace Atomic Absorption Spectrometer in Petroleum Products
  6. Oxidation and Nitration by FTIR
  7. Pour Point of Petroleum Products
  8. Density, Relative Density (Specific Gravity), or API Gravity of Crude Petroleum and Liquid Petroleum Products by Hydrometer Method
  9. Water in Petroleum Products by Distillation.



ASTM Color of Petroleum Products (ASTM Color Scale)

1.0       Apparatus
                                                                                             
1.         Colorimeter
2.         Sample Container
3.         Beakers

2.0       Reagents and Materials

2.1        Solvent Kerosene (Having Color lighter than +21 Saybolt Color) for diluting of dark sample.
2.2        Distilled Water

3.0       Procedure
           
3.1        Place a sample container, filled to a depth of at least 50 mm with distilled water in the compartment of the colorimeter.

3.2        Place the sample in its container in the other compartment.

3.3        Cover the containers to exclude all exterior light.

3.4        Switch on the light source and compare the color of the sample with that of the standard glasses.

3.5        Determine for two field comparators which glass matches the color of the sample; or if an exact match is not possible, then use that glass which possesses the next darker color.


1.            Calculations & Report

         Report the color of the sample as described in equipment’ user manual





  
Flash and Fire Points by Cleveland Open Cup Tester

1.0       Apparatus
                                                                                             
4.         Cleveland Open Cup Flash Point Apparatus
5.         ASTM Thermometer
6.         Natural Gas Source
7.         Beakers

2.0       Reagents and Materials

2.1        Acetone
2.2        Xylene

3.0       Procedure
           
3.1        Fill the test cup with the sample to the filling mark inside of the test cup.

3.2        Place the test cup on the center of the heater.

3.3        The temperature of the test cup and the sample shall not exceed 56°C below the expected flash point.

3.4        Light the test flame and adjust it according to equipments’ instructions.

3.5        Apply the heat at a rate, increases in 14 to 17°C /min.

3.6        When the sample temperature is approximately 56°C below the expected flash point, decrease the heat so that the rate of temperature rise during the last 28°C before the flash point is 5 to 6°C/min.

3.7        Apply the ignition source when the temperature of the sample is 28°C below the expected flash point and each time thereafter at a temperature reading that is a multiple of 2°C.

3.8        Discontinue the ignition source.

3.9        Cool the sample to room temperature and clean with xylene and acetone.

1.            Calculations & Report

Record as the observed flash point the reading on the temperature measuring device.





Calorific Value of Liquid Hydrocarbon Fuels by Bomb Calorimeter

1.0       Apparatus
                                                                                             
8.         Bomb Calorimeter
9.         Oxygen with Cylinder

2.0       Reagents and Materials

2.1        Benzoic Acid, Standard
2.2        Gelatin Capsules
2.3        Methyl Orange Indicator
2.4        Methyl Red Indicator
2.5        Mineral Oil
2.6        Sodium Hydroxide
2.7        Sodium Carbonate
2.8        2,2,4-Trimethylpentane (isooctane)
2.9        Cellophane tape

3.0       Procedure
           
3.1        Follow the equipment’s user manual provided by supplier.

2.            Calculations & Report

Note the reading as on equipment.



Kinematic Viscosity of Transparent and Opaque Liquids


1.0       Apparatus
                                                                                             
1.1        Viscometers Tubes
1.2        ASTM Thermometer
1.3        Temperature-Controlled Bath
1.4        Viscometer Holders
1.5        Stop Watch
1.6        Suction Bulb
1.7        Beakers
1.8        Funnel

2.0       Reagents and Materials

2.1        Acetone
2.2        Xylene
2.3        Petroleum spirit
2.4        Toluene
2.5        Paraffin Oil
2.6        DI Water
2.7        Certified Viscosity Reference Standards


3.0       Procedure
           
3.1        Select a clean, dry, calibrated viscometer.

3.2        When the test temperature is below the dew point, fill the viscometer in the normal manner as required.

3.3        Place rubber stoppers into the tubes to hold the test portion in place, and insert the viscometer into the bath.

3.4        After insertion, allow the viscometer to reach bath temperature, and the remove the stoppers.
            Note the time and temperature when sample is reached to the specific point on viscometer tube.

3.            Calculations & Report

Calculate the kinematic viscosity

v = C x t


            Where:

            v = determined kinematic viscosity value, mm2/s,
            C = calibration constant of the viscometer, mm2/s2, and
            t =   measured flow times.
            Calculate the dynamic viscosity

                                                                      η = v x ρ x 10-3

            Where:
            η = dynamic viscosity, mPa·s,
            ρ = density, kg/m3, at the same temperature used for the determination of the kinematic viscosity, and
            v = kinematic viscosity, mm2/s.



Metals by Graphite Furnace Atomic Absorption Spectrometer in Petroleum Products

1.0       Apparatus
                                                                                             
10.       Graphite Furnace Atomic Absorption Spectrometer (GF-AA)
11.       Analytical Balance
12.       Nitrous Oxide Gas + Cylinder
13.       Acetylene Gas + Cylinder
14.       Air Cylinder
15.       Beakers
16.       Volumetric Flasks
17.       Pipettes

2.0       Reagents and Materials

2.1        Kerosene, Pure
2.2        Nitric Acid
2.3        Hydrogen Peroxide
2.4        Organic Metals Standards for AA
2.5        Filter Papers

3.0       Procedure
           
3.1        Follow the equipment’s user manual provided by supplier.

4.            Calculations & Report

Note the reading as on equipment.


Oxidation and Nitration by FTIR

1.0       Apparatus
                                                                                             
18.       FTIR
19.       Beakers

2.0       Reagents and Materials

2.1        Acetone
2.2        IPA

3.0       Procedure
           
3.1        Follow the equipment’s user manual provided by supplier.

5.            Calculations & Report

Note the reading as on equipment.



Pour Point of Petroleum Products

1.0       Apparatus
                                                                                             
1.        
2.         Pour Point Apparatus D-97
3.         Thermometers
4.         Flat bottom Glass cylindrical Test Jar


2.0       Reagents and Materials

2.1        Acetone
2.2        Ethanol
2.3        Methanol
2.4        Petroleum Naphtha
2.5        Solid Carbon Dioxide
2.6        Cork


3.0       Procedure

3.1 Pour the sample into the test jar to the level mark. When necessary, heat the specimen in a water bath until it is just sufficiently fluid to pour into the test jar.
3.2 Close the test jar with the cork carrying the high-pour thermometer.
3.3 Adjust the position of the cork and thermometer so the cork fits tightly, the thermometer and the jar are coaxial, and the thermometer bulb is immersed so the beginning of the capillary is 3 mm below the surface of the specimen.
3.4 See that the disk, gasket, and the inside of the jacket are clean and dry.
3.5 Place the disk in the bottom of the jacket.
3.6 Place the gasket around the test jar, 25 mm from the bottom.
3.7 Insert the test jar in the jacket. Never place a jar directly into the cooling medium.
3.8 Pour points are expressed in integers that are positive or negative multiples of 3°C.
3.9 Begin to examine the appearance of the sample when the temperature of the sample is 9°C above the expected pour point (estimated as a multiple of 3°C).
3.10 At each test thermometer reading that is a multiple of 3°C below the starting temperature remove the test jar from the jacket.
3.11 To remove condensed moisture that limits visibility wipe the surface with a clean cloth moistened in alcohol (ethanol or methanol).
3.12 Tilt the jar just enough to ascertain whether there is a movement of the specimen in the test jar.
3.13 The complete operation of removal, wiping, and replacement shall require not more than 3 s.
3.14 As soon as the specimen in the jar does not flow when tilted, hold the jar in a horizontal position for 5 s, as noted by an accurate timing device and observe carefully.
3.15 If the specimen shows any movement, replace the test jar immediately in the jacket and repeat a test for flow at the next temperature, 3°C lower.
3.16 Continue in this manner until a point is reached at which the specimen shows no movement when the test jar is held in a horizontal position for 5 s.
3.17 Record the observed reading of the test thermometer.



6.            Calculations & Report

Add 3°C to the temperature recorded above and report the result as the Pour Point, ASTM D 97.



Density, Relative Density (Specific Gravity), or API Gravity of Crude Petroleum and Liquid Petroleum Products by Hydrometer Method

1.0       Apparatus
                                                                                             
20.       Hydrometers (Range 0.650 - 1.150)
21.       ASTM Thermometers
22.       Hydrometer Cylinder
23.       Constant-Temperature Bath
24.       Stirring Rod

2.0       Procedure
           
3.1        Cool the sample and apparatus around 5 to 10°C.

3.2        Mix the sample well.

3.3        Transfer the sample to the clean, temperature stabilized hydrometer cylinder without splashing, to avoid the formation of air bubbles.

3.4        Insert the appropriate thermometer and stir the test portion with a stirring rod.

3.5        Record the temperature of the sample and remove the thermometer and stirring rod from the hydrometer cylinder.

3.6        Lower the appropriate hydrometer into the liquid and release when in a position of equilibrium, taking care to avoid wetting the stem above the level at which it floats freely.

3.7        For low viscosity transparent liquids observe the meniscus shape when the hydrometer is pressed below the point of equilibrium about 1 to 2 mm and allowed to return to equilibrium.

3.8        If the meniscus changes, clean the hydrometer stem and repeat until the meniscus shape remains constant.

3.9        For opaque viscous liquids, allow the hydrometer to settle slowly into the liquid.

3.10      Allow sufficient time for the hydrometer to come to rest.

3.11      When the hydrometer has come to rest floating freely away from the walls of the cylinder, read the hydrometer scale reading.



7.            Calculations & Report

Calculate as per following table:
Material
Density at 15°C kg/m3
Density at 20°C
kg/m3
Relative Density
at 60/60°F
°API
Crude petroleum
53A
59A
23A
5A
Petroleum products
53B
59B
23B
5B
Lubricating oils
53D
59D
-
5D



Water in Petroleum Products by Distillation

1.0       Apparatus
                                                                                             
1.         Distillation Assembly D-95
2.         Heater
3.         Metal Still (Copper or Brass Lid)

2.0       Reagents and Materials

2.1        Petroleum Ether
2.2        Glass Beeds or boiling aid
2.3        Graduated Cylinder
2.4        Beakers

3.0       Procedure
           
3.1        Measure the suitable sample in a graduated cylinder and transfer it to the still.
3.2       Rinse the material adhering to the cylinder with one 50-mL and two 25-mL portions of the petroleum ether.
3.3        Weigh viscous samples directly into the still and add 100 mL of the petroleum ether.
3.4      In cases of material with low-water content when large samples must be used, a solvent-carrier liquid volume in excess of 100 mL may be necessary.
3.5        Glass beads or other boiling aids may be added, if necessary, to reduce bumping.
3.6      Assemble the components of the apparatus, choosing the trap in accordance with the expected water content of the sample and making all connections vapor and liquid tight.
3.7      Insert a loose cotton plug in the top of the condenser to prevent condensation of atmospheric moisture inside it.
3.8        Circulate cold water through the jacket of the condenser.
3.9     Apply heat to the still, adjusting the rate of boiling so that condensed distillate discharges from the condenser at the rate of two to five drops per second.
3.10     Continue distillation until no water is visible in any part of the apparatus except in the trap and the volume of water in the trap remains constant for 5 min.
3.11      When the evolution of water is complete, allow the trap and contents to cool to room temperature.
3.12      Read the volume of the water in the trap.
            Solvent Blank

3.13      The water content of the petroleum ether shall be determined by distilling an equivalent amount of the petroleum ether used for the test sample and testing as described as above.

8.            Calculations & Report

Water, % (V/V) =   (Volume in water trap, mL) - (Water in solvent blank, mL) x 100
                                                  Volume in test sample, mL

  For Viscous Samples

Water, % (V/m) =  (Volume in water trap, mL) - (Water in solvent blank, mL) x 100
                                                    Mass of test sample, g

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