Petroleum Refinery Lab.

Distillation Methods:
Three distillation methods are used to obtain laboratory data on crude oil:
1. True Boiling Point Distillation (TBP)
2. ASTM Distillation (ASTM)
3. Equilibrium Flash Vaporization (EFV)
The degree of separation of the fractions obtained in these methods decreases as
one moves down the list from TBP through ASTM to EFV.

Standard Test Method for

ASTM Distillation at Atmospheric Pressure D 86-04
Objective: to separate a sample of crude into different cuts by ASTM distillation at
atmospheric pressure.
Introduction:
This test method covers the atmospheric distillation of petroleum products using
a laboratory batch distillation unit to determine quantitatively the boiling range
characteristics of such products as natural gasoline, aviation gasoline and similar
products, using manual or automated equipment.
The distillation tests give an indication of types and the quality of the products
that can be obtained from petroleum, and also to compare different petroleum
types. The basic method of distillation (ASTM D-86) is one of the oldest methods
in use because the distillation characteristics of hydrocarbons have an important
effect on safety and performance, especially in the case of fuels and solvents. The
boiling range gives information on the composition, the properties, and the
behavior of petroleum and its products during storage and use. Volatility is the
major determinant of the tendency of a hydrocarbon mixture to produce
potentially explosive vapors.
The distillation characteristics are critically important for both automotive and
aviation gasoline, affecting starting, warm-up, and tendency to vapor lock at high
operating temperature or at high altitude, or both. The presence of high boiling
point components in these and other fuels can significantly affect the degree of
formation of solid combustion deposits.

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The test is carried out at atmospheric pressure and is stopped at 300°C (572°F) to
avoid thermal decomposition. The distillate and the residuum can be further
examined by tests such as specific gravity, sulfur content and viscosity.
Test results are commonly expressed as percent recovered versus corresponding
temperature, either in a table or graphically, as a plot of the distillation curve.
TBP/ASTM distillation curves: are the most important characterization properties
of the crude oil and petroleum products. Both TBP, ASTM distillation curves are
measured at 1 atm pressure. In both these cases, the boiling points of various
volume fractions are being measured.
The basic difference between TBP curve and ASTM distillation curve is that while
TBP curve is measured using batch distillation apparatus consisting of no less than
100 trays and very high reflux ratio, the ASTM distillation is measured in a single
stage apparatus without any reflux, it operates without the presence of a contact
plate and a reflux ratio of zero. Therefore, the ASTM does not indicate a good
separation of various components.

Apparatus

1. Distillation Flask - flask with a side

arm shall be of a size that is at least
50 % larger than the volume of the
charge.
2. Capacitor pass through cooling bath
3. Magnetic stirring bar. Boiling chips
can be used as an alternative.
4. An electric heating mantle covering
the lower half of the flask.
5. Thermometer
6. Graduated cylinder to receive the
distillate
7. A sample of crude oil

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Procedure:

1. Place (100) ml of the sample in the distillation flask.

2. Place few pieces of crushed glass on the bottom of the flask to control
boiling process.
3. Gradually raise the temperature, observe rising vapors and then record the
amount of distillate at the corresponding temperatures.
4. Determine the proportion of distillates and specific gravity and API Gravity
versus boiling points.
5. When you reach the boiling point to 350 oC, stop distillation process and
transfer residue to another device where complemented by fractional
distillation under reduced pressure less than 40 mm Hg.
6. Report the colour of each fraction.

Results:
Plot the distilled volume % vs. temperature (ASTM)

Discussion:
1. What information does the boiling range give on the composition and
properties of the crude oil?
2. How can distillation characteristics of hydrocarbons affect their safety and
performance?
3. What is the major determinant of the tendency of a hydrocarbon mixture
to produce potentially explosive vapour?
4. What are the factors affecting the accuracy of the results?

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Worksheet

Experiment no.: 3
Title: ASTM Distillation

Name:
Class:
Date:

Data recording for Fractional Distillation test

Volume % Temperature, oC
0
10
20
30
40
50
60
70
80
90

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Sample Calculations:
The following data are obtained from ASTM distillation test (example):

Volume percent Temperature

0
distilled C
0 (IBP) 54
5 59
10 65
20 74
30 83.5
40 94.5
50 104.5
60 114
70 125.5
80 141.5
90 173
95 178
FBP 180

Volume distilled = 96 ml
Residue left = 2 ml

1. Calculate % losses
2. Prepare ASTM Distillation Curve (Temperature vs. Volume distilled %)

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