LAB DISTILLATION

AND SIGNIFICANCE
BY

S.K. CHHIBBER
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 DISTILLATION
 IT is the main criteria for separating and
refining of hydrocarbons.
 Used for the preparation of feed stock
 Controlling the quality of the product
 Preparation of pure hydrocarbons as per the
requirements

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 TYPES OF DISTILLATION
 Non fractionating distillation (Raleigh
vaporisation )
 ASTM/IP distillation
 Equilibrium flash evaporation.
 Semi fractionating (Hempels,Sarina still
distillation )Fractionating distillation (Tru
boiling point )
 Spinning band column

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NON FRACTAING DISTILLATION
 Liquid mixture is partially vaporized and
the vapor and liquid are allowed to
separate. There is an increase of
concentration of the more volatile
components in the vapor phase and the
less volatile components in the liquid
phase.
 Vaporization effected by heating the
liquid or reducing the pressure.
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RAYLEIGH`S VAPORIZATION
 Though ideal but practiced rarely
 Flask contain sample is dipped in the
thermostatic bath, the vapors formed
leave the flask without coming in
contact with the liquid. i.e. number of
contact is just one.

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 ASTM DISTILLATION-D86
 IT is a std. distillation
 Has good repeatability/reproducibility
 Simple & consume less time
 It is used to know the boiling range of motor
gasoline, aviation gasoline, special boiling
point sprit, naptha,kerosene, ATF, &diesel
cuts etc.

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 OUT LINES OF THE METHOD
 100 ml sample is taken in RB distillation flask.
Heated under controlled conditions, the
temperature at which 1st. Drop detached from
the condenser is known as IBP.After it on
every 10% distillation the temp. is recorded till
highest temp. is reached when drop in temp. is
observed & known as FBP.Residue &loss
during distillation is also recorded.

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 ATMOSPHERIC DISTILLATION
ASTM D86 / IP 123 / P18
Apparatus and operating conditions
 Flask capacity : 125 ml
 Sample quantity : 100 ml
 Condenser temp. Depends on fuel
 Time for application heat IBP: 5-15 min
 Av. Rate of recovery : 4-5ml / min
 Time for 95 rec , to FBP : 3-5 min
 No reflux
 for gasoline, kerosene and diesel.
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 EQUILIBRIUM FLASH
VAPORISATION
 To obtain EFV curve sample is heated to certain
temperature and pressure to get percentage vaporized.
This will give one point on EFV curve.
 To get other points experiments are repeated with same
sample heated to different temperature but at same
pressure.
 EFV is plotted corresponding to percentage recovered v/s
temperature.
 Very useful design data for distillation.
 Co-relations to relate EFV curves with TBP & ASTM
curves have been developed as it is time consuming.
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 ASTM DISTILLATION-D1160

 Used for heavy petroleum products

 Having max. temp.400°C@1mm
Hg.pressure
 Conditions provide one theoretical
plate

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 OUT LINES OF THE METHODS
 Weight sample corresponding to 200ml. Is
taken in 500ml,RB flask, while heating
vacuum between 0.5 to 10mm is
maintained. Heat input is increased to get
the distillation rate 4to 8 ml/min. Reading
from IBP to every 10% fraction collected
up to FBPis recorded. These boiling ranges
are converted to atmospheric equivalent
tem. By Cox chart.
 % Recovery= %(Recovery +residue )
 % Loss=100-total recovery.
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 TBP DISTILLATION, D-2892
 It is highly fractionating distillation in which
fractionating column and controlled reflux is used
 Equilibrium between vapors rising upwards and
liquid coming downwards in a column is
established.
 Product of better quality is obtained
 TBP curve establish the product pattern of various
commercial products.
 Curve is plotted commulated%wt./vol.recovered
v/s temp.
 For crude oil curve is normally smooth

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OUT LINES OF THE METHOD
 Wt. sample 1-30 liters is distilled to 400 °Cmax
under vacuum having 14-18 theoretical plate
fractionating column. Reflux ratio of 5:1 through out
all the operating pressure.Temp. pressure & other
variables are recorded at an intervals at the end of
each cut. Density & mass of each cut is obtained
&yield is calculated on vol. basis as follows

Vol.%= Density of feed x% Wt.

---------------------
Density of fraction

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TYPICAL TBP,ASTM,EFV
CURVES

te
m
p
e
r
at
u
r
e

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 INTERCONVERSION OF
DISTILLATION DATA
Reliability of results
Maxwell method (Data book on hydrocarbons)
 Avg. deviation of converted to experimental 10 to 15°F
Ad mister method ( Applied hydrocarbon
thermodynamics)
At atmospheric & higher pressure
 ASTM TO TBP, Avg. Deviation : 7°F
 TBP TO EFV : 6°F
 ASTM to EFV : 9°F
Under sub atmospheric pressure
 ASTM to TBP : 5°F
 TBP to EFV : 6°F
 ASTM to EFV : 6°F

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BOILING RANGE DISTRIBUTION
BY G.C
 It is simulated by GC
 IT is quick & less quantity of sample
is required
 Open pack/ tubular (capillary ) GC
column is used to elute the
hydrocarbon components of the
sample in the order of increasing
boiling point.

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BOILING RANGE DISTRIBUTION BY GAS
CHRONMATORAGRAPHY

 ASTM 3710-97 –Boiling range distribution of gasoline &

gasoline fraction by G>C
 ASTM D2887-97 – Boiling range distribution of petroleum
fraction by G>C
 ASTM D2887 Extended –High Temperature
 ASTM D5307-97 Determination of boiling range distribution
of crude petroleum by G>C
SAMPLE

CARRIER GAS INTIGRATOR

COLUMN
INJECTOR DECETOR
OV – 101
SE – 30
UCW - 982 18
OUT LINES OF THE METHOD
 Known calibration mixture contain 20
components between C5-C42 is allowed to
run in GC and retention time of each
component is printed out. Retention time
v/s boiling point is recorded into the
microprocessor unit automatically.
Unknown sample is injected & the
chromatogram of area v/s rent ion time is
printed out. The unit prints out % vol.
recovery corresponding to the boiling
points. If desired unit automatically convert
the TBP &ASTM data too
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SIMULATED DISTILATON-D2887
Typical conditions
Column length 1.2m
Liquid phase OV-1 SE 30, UC-W 98
B
O
I

Def Temp. 350°C L

I
N

Inf.( FID) Temp. 350°C

G

P
O

Oven Temp. Int. -30°C I

N
T
°

Final 350°C C

Oven temp.
program rate 10

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SHORT PATH DISTILLATION

 Usedto distill petroleum products up

to 750°C

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 OUT LINES OF THE METHODS
 Product 370+ is fed into the distillator with a
constant feed rate by gear pump. It is distributed to
the evaporator surface by the distribution plate at
the top of the wiper basket. Forced by the gravity,
the product film flows down and thereby continuous
homogenized by the roller of the wiper basket. The
high volatile components of the mixture are
evaporated on the heated surface and afterwards
condense at the internal condenser. The distillate
flows down on the condenser surface to the
distillate out let nozzle. The low volatile component
of the mixture are not evaporated and are flowing
to the residue outlet nozzle. Very high volatile
component s of the mixture as well as dissolved
gases are not condensed at the internal condenser.
 Use to distill petroleum products upto 750 °C.

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Hot POT Distillation apparatus

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