Classification and

Characterization
Crude
 Overview of Characterization

Crude of petroleum is very complex,

no attempt is made by the refiner to
analyze for the pure components that
contained in the crude oil
Important Crude Oil Properties

• API Gravity
• Sulphur Content
• Pour Point
• Carbon Residue
• Salt Content
• Characterization Factors
• Nitrogen Content
• Distillation Range
• Metal Content
 Standard Test Method for
Sulfur
• ASTM D 4294
• Energy Dispersive X-ray Fluorescence
Spectrometry
• Sweet crude or Sour Crude
• There is no sharp dividing line between
sour and sweet crudes, but 0.5% sulfur
content is frequently used as the
criterion
 Introduction
• This test method covers the determination of
total sulfur in petroleum crude and petroleum
products.
• Total sulphur is the combination of both
organic and inorganic sulphur.
• Sample must be a single-phase and either
liquid at ambient conditions, liquefiable with
moderate heat or soluble in hydrocarbon
solvents.
 Principle EDX

• When an Individual atoms excited by an

external energy source, emit X-ray
photons of a characteristic energy or
wavelength. By counting the number of
photons of each energy emitted from a
sample, the elements present is
identified and quantified.
Types of S in Crude

Organic sulphur compounds

1. Acidic S Compounds
•Alkyl mercaptan
•Phenyl mercaptan
•Cyclohexyl-thiol
2. Non Acidic Compounds
•Thiocyclo hexane
•Thiophene
•Benzothiophene

In-organic Sulphur Compounds

H2S
• The identification of elements by X-ray
methods is possible due to the characteristic
radiation emitted from the inner electronic
shells of the atoms under certain conditions.
Construction

• Source
• Collimater
• Sample
• Collimater
• Be window
• Detector
Instruments
Spectrum
 Pour Point
• The pour point of a liquid is the
temperature below which the liquid loses
its flow characteristics.
OR
• The lowest temperature at which
movement of the specimen is observed is
recorded as the pour point.

• ASTM D 97
Apparatus
 Instrument
Pour point Thermoelectrically
Jar & Cork cooled constant
temperature bath
 Pour Point Jar Dimension

Typical Constant
temperature bath
Instrument will have
the Temp -80 to 100 °C
 Specification

Cooling Medium Temp Range

Ice and water 9°C
Crushed ice and sodium chloride crystals -12 °C
Crushed ice and calcium chloride crystals -27 °C
solid carbon dioxide -57 °C
 Calculation and Reporting
• Add 3 °C to the
temperature recorded
as the pour point. Or
report both the upper
and lower pour point.
• Precision : Results of
duplicate tests shall not
differ by more than 3 °C
 Repeatability 6 °C
 Reproducibility 6 °C
 Summary
• The lower the paraffin content and the
greater the content of aromatics.
• Relies on the n-paraffin concentration
and the length of the n-paraffinic chain
• The conventional pour point tester can
measure the pour point at atmospheric
pressure and there are no relevant
standards and testers for measuring
the pour point of crude oil at high
pressure
 Mechanism

• Agglomeration of Wax Crystals

• Adsorption
• Nucleation and Growth
• Co-crystallization
Importance of Pour Point
 Carbon Residue
• This test method covers the determination of
the amount of carbon residue (left after
evaporation and pyrolysis of an oil and is
intended to provide some indication of
relative coke-forming propensities.
• This test method is generally applicable to
relatively nonvolatile petroleum products
which partially decompose on distillation at
atmospheric pressure.
 Test method
• A weighed quantity of sample is placed in a
crucible and subjected to destructive
distillation. The residue undergoes cracking and
coking reactions during a fixed time period. 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
 Calculation of the carbon residue

Carbon Residue =(Ax100)/W

• A = mass of residue, Initial – Final wt. (g)

• W = mass of sample (g)
 Types

Conradson Carbon Residue

ASTM D 524
Ramsbottom Carbon Residue
ASTM D 189
 Conradson Carbon Residue
• Porcelain Crucible
• Skidmore Iron Crucible
• Iron Crucible
• Wire Support
• Hood
• Insulator
• Burner
Experimental Setup
 Procedure

• Shake thoroughly the sample to be

tested
• Pre heat to 50 °C
• Filter through 100 mesh
• Weigh to 10 g of sample
• Apply heat
• When smoke appears igniting the
vapors.
• Cool in desiccator
• Calculate
 Ramsbottom Carbon residue
• Glass Coking Bulb
• Control Bulb
• Sample Charging
Syringe
• Metal Coking Furnace
• Temperature-Measuring
Devices
Metal Coking Furnace
 Procedure
• Shake thoroughly the sample to be tested
• Pre heat to 50 °C
• Filter through 100 mesh
• Weigh to 10 g of sample
• Heat in a metal furnace at 550°C
• For 20 min
• Cool in a desiccator
• Calculate
Correlation Data CCR & RCR
 Summary
• Carbon Residue Test will not give the actual
carbon content
• It gives the Coke content
• It gives some idea about resins
• It is important for determining the crude price
• In refinery CCR is used for assigning parameters
for atmospheric distillation column & RCR is used
for FCC
• Repeatability & Reproducibility for two results
 Reference
• Standard test methods (ASTM) for crude
oil properties
• Bhattarai, N et al., (2015) Advanced
Electron Microscopy in the Study of
Multimetallic Nanoparticles, Springer
International Publishing, Switzerland.
• Agarwal, B. K. (1991) X-ray
Spectroscopy, 2nd Eds, Springer-verlag,
Berlin.