DISTILLATION.ppt has been provided for the details

DISTILLATION.ppt has been provided for the details discussion

1. 1
LAB DISTILLATION
AND SIGNIFICANCE
BY
S.K. CHHIBBER

2. 2
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

3. 3
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

4. 4
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.

5. 5
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.

6. 6
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.

7. 7

8. 8
OUT LINES OF THE METHOD
100 ml sample is taken in RB distillation flask.
Heated under controlled conditions, the
temperature at which 1
st
. 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.

9. 9
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.

10. 10
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.

11. 11
ASTM DISTILLATION-D1160
Used for heavy petroleum products
Having max. temp.400°C@1mm
Hg.pressure
Conditions provide one theoretical
plate

12. 12
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.

13. 13
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

14. 14
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

15. 15
TYPICAL TBP,ASTM,EFV CURVES
te
m
p
e
r
at
u
r
e

16. 16
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

17. 17
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.

18. 18
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
INJECTOR
DECETOR
INTIGRATOR
COLUMN
OV –101
SE –30
UCW -982
CARRIER GAS

19. 19
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

20. 20
SIMULATED DISTILATON-D2887
Typical conditions
Column length 1.2m
Liquid phase OV-1 SE 30, UC-W 98
Def Temp. 350°C
Inf.( FID) Temp. 350°C
Oven Temp. Int. -30°C
Final 350°C
Oven temp.
program rate 10
B
O
I
L
I
N
G
P
O
I
N
T
°
C

21. 21
SHORT PATH DISTILLATION
Used to distill petroleum products up to
750°C

22. 22
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.

23. 23
Hot POT Distillation apparatus

24. 24