Chapter 2-Crude Assay and Test Methods

Chapter 2-Crude Assay
1
Petroleum Processing Data
and Test Methods
Simple crude distillation
All crude oils undergo separation processes through distillation,
so it is common to express the capacity a refinery in terms of
distillation capacity.
BPSD : (Barrels Per Stream Day)
Maximum number of barrels of input that a distillation facility
can process when running at full capacity under optimal crude
and product slate condition with NO allowance for downtime.
2
and product slate condition with NO allowance for downtime.
BPCD : (Barrels Per Calendar Day)
Amount input that a distillation facility can process under usual
operating conditions, making allowance for the types and grades
of products to be manufactured, environmental constraints, and
unscheduled and scheduled downtime due to maintenance,
repairs, and shutdown.
BPSD slightly > BPCD
Classification of refinery operns
Refining processes and operation classified into five basic types:
1. Distillation : Separation of Crude oil in Atm and Vacuum
columns into hydrocarbon compound based on size and boiling
point ranges.
2. Conversion process : change size or structure of hydrocarbon
molecules by decomposition, unification and reforming
3. Treatment process : Prepare hydrocarbon streams for
additional processing and to prepare finished product using
3
additional processing and to prepare finished product using
chemical or physical separation. Desalting, Hydro-
desulfurization, solvent refining, sweetening and dewaxing.
4. Blending: process of mixing and combining hydrocarbon
fractions additives, and other components to produce finished
products with specific performance properties.
5. Others include light ends recovery, sour-water stripping,
utilities, sulfur recovery etc.
Simple crude distillation
Or Petrol
4
Or Diesel
TBP Apparatus
No of stages:10-12
Capacity : 2Lit
Larger capacity
are preferable as
good amount of
Bottom.
Hot air circulation Hot air circulation
or Electric heater
Top of rectifier air
cooled reflux
condenser
TBP Apparatus
TBP Curve
Gasoline, turbine fuels,
naphtha, kerosene, gas
oil and distillate fuel
oils.
ASTM D86- Distillation
ASTM: American Society for Testing and Materials
oils.
Atmospheric pressure.
No hotter than 650F to
minimize cracking.
Correlations to correct
to TBP basis.
ASTM D86- Distillation of fractions
Mean average boiling point (MeABP)
which is the arithmetic average of the molal boiling point and the cubic volumetric
average boiling point
Heavy petroleum
products (650F+).
Vacuum conditions
10 to 40 mmHg.
ASTM D1160
10 to 40 mmHg.
Correlations to correct
to atmospheric.
Simulated Distillation Analysis
This method uses a 15 plate
column operating under a reflux
ration of 5:1.
Starts at atmospheric pressure.
ASTM D2892 & D5236
Maximum temperature of 650 F.
Switch to ASTM D5236 at o.1
mmHg pressure.
Maximum temperature of 1000 F.
Fractions of Petroleum Fractions of Petroleum
Fraction Boiling
Range / C
No of carbon
atoms per
molecule
Uses
Petroleum Below 40 1 - 4 Fuel for Petroleum
Gas
Below 40 1 - 4 Fuel for
cooking
Fraction Boiling
Range / C
No of carbon
atoms per
molecule
Uses
Petrol 40 - 75 5 -10 Fuel for car Petrol
(Gasoline)
40 - 75 5 -10 Fuel for car
engines
Fraction Boiling
Range / C
No of carbon
atoms per
molecule
Uses
Naphtha 75 - 140 7 - 14 Chemical Naphtha 75 - 140 7 - 14 Chemical
feedstock
Fraction Boiling
Range / C
No of carbon
atoms per
molecule
Uses
Kerosene 140 - 270 11 - 16 Fuel for jet
engines, engines,
cooking
and heating
Fraction Boiling
Range / C
No of carbon
atoms per
molecule
Uses
Diesel 270 - 350 16 - 20 Fuel for Diesel 270 - 350 16 - 20 Fuel for
diesel
engines
Fraction Boiling
Range / C
No of carbon
atoms per
molecule
Uses
Lubricants 300 - 350 20 - 35 Making Lubricants 300 - 350 20 - 35 Making
waxes and
lubricating
oils
Fraction Boiling
Range / C
No of carbon
atoms per
molecule
Uses
Bitumen Above 350 More than Paving Bitumen Above 350 More than
70
Paving
roads
Temperature
increases down
the column
(Petroleum Gas)
Gasoline/ Petrol
Naphtha
Kerosene/ATF
Diesel
Lubricants
Bitumen
Properties of Petroleum products
LPG (Liquified Petroleum Gas)
Mixture of Propane and butane in Liq form at a pressure
of 10-15 atmP.
Composition
Ethane Traces , Propane 25 ,i-butane 36
Butane 38, H
2
S and Mercaptans (RHS)
Quality is tested by weathering test
Residual temperature is noted after 95% of liquid is Residual temperature is noted after 95% of liquid is
vaporised.
Domestic ,maximum weathering temp is 2C.
slightly lower than this temperature may
Useful but carrying capacity of cylinder will
reduce.
RVP (Reid Vapor Pressure)
14.2 kgs domestic cylinder at a temperature of 37.8 C
has maximum RVP of 8 kg/cm
2
Copper strip corrosion test
Presence of H
2
S and mercaptans cause corrosion to
vessels.
Copper strip corrosion test
Temp : 30 C
Time : 1 hr Time : 1 hr
End result : brightness of copper strip compared
against std copper strip indicating different degree
of corrosion as ASTM 1, 1a, 1b, 2, 2a, etc.
-Not worse than ASTM 1.
H
2
S is removed by absorption of Di-Ethyl Amine
(DEA)
Traces of H
2
S and mercaptans measured by
doctors test
solution of sodium plumbite and traces of
elemental sulphur added to form black
precipitation of lead sulfide. precipitation of lead sulfide.
No moisture should be present in LPG.
Final Specification
Kerosene (140-270 C)
Heavier than Naphtha or petrol or gasolene, lighter than
diesel.
Burning quality by smoke point and flash point
Smoke Point (SP)
Height of the flame (in mm) produced by oil in stove or
lamp without forming any smoke.
Greater SP , better burning quality. Greater SP , better burning quality.
Domestic Kerosene minimum 20 mm
Smoke is produced due
to Carbon and heavy
hydrocarbon
Flash Point
Temperature of the oil at which it momentarily flashes in
the presence of air and igniting source.
For domestic kerosene , it should not be below the
ambient T. (India-35 C minimum)
Open cup and closed cup method
heated at rate of 5-6 C per minute and std flame is
Abels method
Pensky-Mertinus
heated at rate of 5-6 C per minute and std flame is
introduced every 30 sec.
Char point and Bloom
Char point is Coke and Ash left on the wick after complete
burning of the oil.
For domestic kerosene the max amount is 20 mg/Kg of oil For domestic kerosene the max amount is 20 mg/Kg of oil
burnt. If the oil contains more aromatics, more organic
char formed.
Bloom is darkness produced by the flame of the oil. It
should not be darker than standard brightness in a lamp.
Final Specification
Lubricating oil
A lubricant is a solid , semi-solid or liquid used to reduce
friction between solid surfaces.
e.g graphite , soap, mineral oil
Lubricating oil are liquid made from petroleum oils( lube
base stock) from VDU blended with soaps of fatty acids and
other additives. other additives.
Properties
Viscosity
Saybolt Method (60 cc)
Redwood Method (50 cc)
Lubricating oil
Viscosity index (VI)
Rate of change of viscosity with temperature.
Ratio of difference of viscosity (U) of oil to be used with
respect to the viscosity of petroleum oil (L) having zero VI
(aromatics) to the difference of viscosity of high VI (H) oil
(paraffinic :100 VI) to the viscosity of zero VI oil for a (paraffinic :100 VI) to the viscosity of zero VI oil for a
temperature change from 37.8 to 98.9 C
If greater than 100
All at 37.8 C
Lubricating oil
Lubricating oil
Cloud Point
Temperature at which oil becomes hazy or cloudy due to
the onset of wax crystallization or solidification.
Pour point
The Temperature at which a liquid hydrocarbon ceases to
flow or pour. flow or pour.
Method
Definite qty of sample taken and heated to 46 C to make
all the wax dissolve in oil, and cooled to 32 C before
testing.
Ice bath containing salt used to estimate the pour point.
The pour point is taken 5 F above the solid point.
Motor Spirit
Gasoline (US) or Petrol (Europe and Asia) is a term
used to describe a complex mixture of various
hydrocarbons refined from crude petroleum oil for use
as a fuel in engines.
Gasoline is a combination of hydrocarbon molecules Gasoline is a combination of hydrocarbon molecules
that have between five and 12 carbon atoms.
IGNITION
Spark Ignition (SI)
Gasoline Engines use a precisely timed electric
spark to start the combustion process.
Compression Ignition (CI) Compression Ignition (CI)
Diesel Engines use the heat produced from
compression to raise cylinder temperature above
the flash point of diesel, and inject fuel directly
into the cylinder.
DEFINITIONS
TDC
Top Dead Center
Piston at top of stroke.
BDC
Bottom Dead Center
STROKE
TDC to BDC
BDC to TDC
180 degrees of
crankshaft rotation
Bottom Dead Center
Piston at Bottom of
stroke.
FOUR CYCLE (Stroke)
4 x 180 = 720 degrees
to make one complete
cycle.
RK
FOUR STROKE CYCLE
Intake
Compression
Power Power
Exhaust
RK
INTAKE STROKE
Intake valve open
Exhaust valve closed
piston traveling down
from TDC to BDC from TDC to BDC
Air and fuel is being force
into the cylinder by the
difference between
atmospheric and cylinder
pressure
COMPRESSION
STROKE
Both valves closed
Piston traveling up BDC
to TDC to TDC
Compressing the air-
fuel mixture
POWER
STROKE
Both valves closed
Spark plug ignites the
air fuel mixture air fuel mixture
Piston is being
pushed down by the
expanding gases from
TDC to BDC
EXHAUST
STROKE
Exhaust valve open
Intake valve closed
Piston traveling up Piston traveling up
from BDC to TDC
forcing the burnt
exhaust gases from the
cylinder
RK
Motor Spirit
ASTM Distillation
Mixture of Hydrocarbons boiling range up to 200 C.
In S.I.Engine, light hydrocarbon liquid is needed for
combustion.
The required ASTM analysis of MS
Is that 10%, 50% and 90% vaporization Is that 10%, 50% and 90% vaporization
occur at max vapor temp of 70 , 125 and
180 C.
Motor Spirit
Octane no
Engine performance is measured by the maximum
power developed and the rate at which it is developed
at different engine speeds.
If the rate of power development is NOT uniform with
speed , rather it fluctuates , then this type situation is speed , rather it fluctuates , then this type situation is
called knocking or hammering of the engine.
Long chain hydrocarbons give rise to knocking. Iso-
octane as the fingerprint for measuring the engine
performance.
Octane no is, as the % of Iso-octane in a mixture of iso-
octane and n-heptane.
2,2,4-tri-methylpentane
Octane Number =100
Octane Rating
Heptane
Octane Number = 0
Motor Spirit
Octane no
The octane no lies between 0 and 100, which is measured
by co-operative fuel research (CFR) engine. The actual fuel
may have more than 100 (ie more than Iso-octane)
Engine test is carried out in at two different speeds Engine test is carried out in at two different speeds
RON-Research Octane No (600 rpm)-city driving
MON-Motor Octane No (900 rpm)-highway driving
Octane no falls with increasing speed.
Improved adding TEL (but pollution problem)
MTBE or ETBE (Methy or Ethyl Tertiary Butyl Ethers)
Motor Spirit
Corrosion
The presence of mercaptan sulfur cause corrosion.
Merox treatment process (catalytic oxidation) convert to
disulfide but releases S0 during combustion. disulfide but releases S0
2
during combustion.
Now-a-days catalytic hydro-desulfurisation unit.
Copper corrosion test for MS similar like LPG for 3 hrs.
Motor Spirit
Oxidation stability
MS is mixture from various units of a refinery. (Naphtha
reforming, cracking, by-product from petrochemical
plants (like aromatics, pyrolysis gasoline).
It contains di-olefins, which susceptible to mild It contains di-olefins, which susceptible to mild
polymerisation, producing film or gum like substance in
contact with O
2
. It is slow process but severe damage if
stored for long time.
Therefore storageability of MS is measured in terms of the
period during which fuel does NOT form any gum in a
vessel for 6 hrs and find fall in pressure.
Motor Spirit
Additives
Colour to distinguish octane no, anti-icing , anti-static ,
anti-oxidant , anti-corrosive, and octane boosting agents.
High Speed Diesel (HSD)
Boiling range of 250-360 C, not vaporizable at ambient.
Cetane Number
paraffinic hydrocarbon has a lower autoignition
temperature that that of aromatics.
Non uniform burning if rich in aromatics (shock wave or Non uniform burning if rich in aromatics (shock wave or
knocking).
defined % normal cetane in a mixture of n-cetane and
-methyl naphthalene (aromatic) which gives the same
performance as that of the diesel sample.
Diesel index
Presence of paraffinic HC in diesel related by aniline
point, which is the temperature at which aniline
solubilises the fuel in equal amounts and a homogeneous
mixture points.
Greater the paraffinic, higher the aniline point. Greater the paraffinic, higher the aniline point.
API gravity ?????
The value of DI at least 45.
Pour point
Temperature at which oil will cease to flow due to the
formation of waxy crystals. In india 6 C.
Aviation Fuels
Gasoline based for jet planes and kerosene based for
turbine planes.
Kerosene based Aviation Turbine Fuel (ATF) boiling Kerosene based Aviation Turbine Fuel (ATF) boiling
range of 150-250 C similar to kerosene.
Freezing point is to be below -50 C
BITUMEN
Asphalt is obtained from short residue (mass from the
bottom of VDU) after extraction of valuable oil by
propane.
Mainly used as paving material, paint and water
proofing agent.
At temp above 90 C , it flows like liquid and solidifies at
room Temp. room Temp.
BITUMEN
Penetration Index
The hardness or penetration quality of bitumen is
assessed by this test.
The Depth of submergence or penetration of a standard
weight through a needle penetrator.
A standard needle is allowed to penetrate under a load of A standard needle is allowed to penetrate under a load of
100 gms cone (1/100 cm) at 25 C for 5 sec.
Paving grade has a
penetration of 60/70 or
80/100.
In hot climate condition
Lower PI bitumen is preferred
BITUMEN
Softening Point ( Ball and Ring Method)
Steel ball 3.5+-0.05 gms (dia 9.53 mm) kept on casted disc
of bitumen.
The temperature at which the
sample detaches from the die and
falls, indicating the softening temp falls, indicating the softening temp
Higher the Softening point
better consistency of
bitumen.
BITUMEN
Ductility
The ductility of a bituminous material is measured by the
distance in cm to which it will elongate before breaking
when a standard briquette specimen of the material is
pulled apart at a specified speed and a specified
temperature temperature
Based on the grade the different value of ductility but
generally more than 75 cm
Petroleum Coke
Petroleum residue contains heavy HC that crack at high
temperature in the absence of air yielding Gases ,Light HC
and Black solid carbon rich residue or coke.
Greater Heavy aromatic yield greater coke.
Residue from Indian crude oil are rich with heavy aromatic
and low S , suitable for good quality coke.
Residue from Middle East not suitable for high S content is
converted to paving grade bitumen or used for catalytic
cracking.

Chapter 2-Crude Assay and Test Methods

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