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LAB DISTILLATION LAB DISTILLATION AND SIGNIFICANCEAND SIGNIFICANCE

BYBY

S.K. CHHIBBERS.K. CHHIBBER

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DISTILLATIONDISTILLATION

IT is the main criteria for separating and IT is the main criteria for separating and refining of hydrocarbons.refining of hydrocarbons.

Used for the preparation of feed stockUsed for the preparation of feed stock Controlling the quality of the productControlling the quality of the product Preparation of pure hydrocarbons as per the Preparation of pure hydrocarbons as per the

requirementsrequirements

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TYPES OF DISTILLATIONTYPES OF DISTILLATION

Non fractionating distillation (Raleigh Non fractionating distillation (Raleigh vaporisation )vaporisation )

ASTM/IP distillationASTM/IP distillation Equilibrium flash evaporation.Equilibrium flash evaporation. Semi fractionating (Hempels,Sarina still Semi fractionating (Hempels,Sarina still

distillation )Fractionating distillation (True distillation )Fractionating distillation (True boiling point )boiling point )

Spinning band columnSpinning band column

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NON FRACTAING DISTILLATIONNON FRACTAING DISTILLATION

Liquid mixture is partially vapourised Liquid mixture is partially vapourised and the vapour and liquid are allowed to and the vapour and liquid are allowed to separate. There is an increase of separate. There is an increase of concentration of the more volatile concentration of the more volatile components in the vapour phase and the components in the vapour phase and the less volatile components in the liquid less volatile components in the liquid phase.phase.

Vapourization effected by heating the Vapourization effected by heating the liquid or reducing the pressure.liquid or reducing the pressure.

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RAYLEIGH`S VAPORIZATIONRAYLEIGH`S VAPORIZATION

Though ideal but practiced rarelyThough ideal but practiced rarelyFlask contain sample is dipped in the Flask contain sample is dipped in the

thermostatic bath, the vapors formed thermostatic bath, the vapors formed leave the flask without coming in leave the flask without coming in contact with the liquid. i.e. number of contact with the liquid. i.e. number of contact is just one.contact is just one.

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ASTM DISTILLATION-D86ASTM DISTILLATION-D86

IT is a std. distillationIT is a std. distillation Has good repeatability/reproducibilityHas good repeatability/reproducibility Simple & consume less timeSimple & consume less time It is used to know the boiling range of motor It is used to know the boiling range of motor

gasoline, aviation gasoline, special boiling gasoline, aviation gasoline, special boiling point sprit, naptha,kerosene, ATF, &diesel point sprit, naptha,kerosene, ATF, &diesel cuts etc. cuts etc.

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OUT LINES OF THE METHODOUT LINES OF THE METHOD

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

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ATMOSPHERIC DISTILLATION ATMOSPHERIC DISTILLATION ASTM D86 / IP 123 / P18ASTM D86 / IP 123 / P18

Apparatus and operating conditions Apparatus and operating conditions Flask capacity : 125 ml Flask capacity : 125 ml Sample quantity : 100 ml Sample quantity : 100 ml Condenser temp. Depends on fuelCondenser temp. Depends on fuel Time for application heat IBP: 5-15 minTime for application heat IBP: 5-15 min Av. Rate of recovery : 4-5ml / minAv. Rate of recovery : 4-5ml / min Time for 95 rec , to FBP : 3-5 minTime for 95 rec , to FBP : 3-5 min No refluxNo reflux for gasoline, kerosene and diesel.for gasoline, kerosene and diesel.

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EQUILIBRIUM FLASH EQUILIBRIUM FLASH VAPORISATIONVAPORISATION

To obtain EFV curve sample is heated to certain To obtain EFV curve sample is heated to certain temperature and pressure to get percentage vaporized. temperature and pressure to get percentage vaporized. This will give one point on EFV curve.This will give one point on EFV curve.

To get other points experiments are repeated with same To get other points experiments are repeated with same sample heated to different temperature but at same sample heated to different temperature but at same pressure.pressure.

EFV is plotted corresponding to percentage recovered v/s EFV is plotted corresponding to percentage recovered v/s temperature.temperature.

Very useful design data for distillation.Very useful design data for distillation. Co-relations to relate EFV curves with TBP & ASTM Co-relations to relate EFV curves with TBP & ASTM

curves have been developed as it is time consuming.curves have been developed as it is time consuming.

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ASTM DISTILLATION-D1160ASTM DISTILLATION-D1160

Used for heavy petroleum productsUsed for heavy petroleum productsHaving max. temp.400Having max. temp.400°C@1mm °C@1mm

Hg.pressureHg.pressureConditions provide one theoretical Conditions provide one theoretical

plateplate

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OUT LINES OF THE METHODSOUT LINES OF THE METHODS

Weight sample corresponding to 200ml. Is Weight sample corresponding to 200ml. Is taken in 500ml,RB flask, while heating taken in 500ml,RB flask, while heating vacuum between 0.5 to 10mm is vacuum between 0.5 to 10mm is maintained. Heat input is increased to get maintained. Heat input is increased to get the distillation rate 4to 8 ml/min. Reading the distillation rate 4to 8 ml/min. Reading from IBP to every 10% recovery collected. from IBP to every 10% recovery collected. FBP is recorded. These boiling ranges are FBP is recorded. These boiling ranges are converted to atmospheric equivalent tem. converted to atmospheric equivalent tem. By Cox chart.By Cox chart.

% Recovery= %(Recovery +residue )% Recovery= %(Recovery +residue ) % Loss=100-total recovery.% Loss=100-total recovery.

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TBP DISTILLATION, D-2892TBP DISTILLATION, D-2892 It is highly fractionating distillation in which It is highly fractionating distillation in which

fractionating column and controlled reflux is usedfractionating column and controlled reflux is used Equilibrium between vapors rising upwards and Equilibrium between vapors rising upwards and

liquid coming downwards in a column is liquid coming downwards in a column is established.established.

Product of better quality is obtainedProduct of better quality is obtained TBP curve establish the product pattern of various TBP curve establish the product pattern of various

commercial products.commercial products. Curve is plotted commulated%wt./vol.recovered Curve is plotted commulated%wt./vol.recovered

v/s temp.v/s temp. For crude oil curve is normally smoothFor crude oil curve is normally smooth

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OUT LINES OF THE METHODOUT LINES OF THE METHOD Wt. sample 1-30 liters is distilled to 400Wt. sample 1-30 liters is distilled to 400°C max °C max

under vacuum having 14-18 theoretical plate under vacuum having 14-18 theoretical plate fractionating column. Reflux ratio of 5:1 through out fractionating column. Reflux ratio of 5:1 through out the distillation is kept at all the operating the distillation is kept at all the operating pressure.Temp. pressure & other variables are pressure.Temp. pressure & other variables are recorded at an intervals at the end of each cut. recorded at an intervals at the end of each cut. Density & mass of each cut is obtained &yield is Density & mass of each cut is obtained &yield is calculated on vol. basis as followscalculated on vol. basis as follows

Vol.%= Density of feed Vol.%= Density of feed --------------------- x% wt.--------------------- x% wt. Density of fractionDensity of fraction

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TYPICAL TBP,ASTM,EFV TYPICAL TBP,ASTM,EFV CURVESCURVES

temperature

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INTERCONVERSION OF INTERCONVERSION OF DISTILLATION DATADISTILLATION DATA

Reliability of resultsReliability of resultsMaxwell method (Data book on hydrocarbons)Maxwell method (Data book on hydrocarbons) Avg. deviation of converted to experimental 10 to 15Avg. deviation of converted to experimental 10 to 15°F°FAd mister method ( Applied hydrocarbon Ad mister method ( Applied hydrocarbon

thermodynamics)thermodynamics)At atmospheric & higher pressureAt atmospheric & higher pressure ASTM TO TBP, Avg. Deviation : 7ASTM TO TBP, Avg. Deviation : 7°F°F TBP TO EFV : 6°FTBP TO EFV : 6°F ASTM to EFV : 9°FASTM to EFV : 9°FUnder sub atmospheric pressureUnder sub atmospheric pressure ASTM to TBP : 5°FASTM to TBP : 5°F TBP to EFV : 6°FTBP to EFV : 6°F ASTM to EFV : 6°F ASTM to EFV : 6°F

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BOILING RANGE DISTRIBUTION BOILING RANGE DISTRIBUTION BY G.CBY G.C

It is simulated by GCIt is simulated by GC IT is quick & less quantity of sample IT is quick & less quantity of sample

is requiredis required Open pack/ tubular (capillary ) GC Open pack/ tubular (capillary ) GC

column is used to elute the column is used to elute the hydrocarbon components of the hydrocarbon components of the sample in the order of increasing sample in the order of increasing boiling point.boiling point.

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BOILING RANGE DISTRIBUTION BY GAS BOILING RANGE DISTRIBUTION BY GAS CHRONMATORAGRAPHYCHRONMATORAGRAPHY

ASTM 3710-97 –Boiling range distribution of gasoline & ASTM 3710-97 –Boiling range distribution of gasoline & gasoline fraction by G>Cgasoline fraction by G>C

ASTM D2887-97 – Boiling range distribution of petroleum ASTM D2887-97 – Boiling range distribution of petroleum fraction up to 538fraction up to 538°C°C by GC by GC

ASTM D2887 Extended –High Temperature up to 615ASTM D2887 Extended –High Temperature up to 615°C°C ASTM D5307-97 Determination of boiling range distribution ASTM D5307-97 Determination of boiling range distribution

of crude petroleum up to 750of crude petroleum up to 750°C°C by GC by GCSAMPLE

INJECTOR DECETOR

INTIGRATORCOLUMN

OV – 101

SE – 30

UCW - 982

CARRIER GAS

1919

OUT LINES OF THE METHODOUT LINES OF THE METHOD Known calibration mixture contain 20 Known calibration mixture contain 20

components between C5-C42 is allowed to components between C5-C42 is allowed to run in GC and retention time of each run in GC and retention time of each component is printed out. Retention time component is printed out. Retention time v/s boiling point is recorded into the v/s boiling point is recorded into the microprocessor unit automatically. microprocessor unit automatically. Unknown sample is injected & the Unknown sample is injected & the chromatogram of area v/s retention time is chromatogram of area v/s retention time is printed out. The unit prints out % vol. printed out. The unit prints out % vol. recovery corresponding to the boiling recovery corresponding to the boiling points. If desired unit automatically convert points. If desired unit automatically convert the TBP &ASTM data toothe TBP &ASTM data too

2020

SIMULATED DISTILATON-D2887SIMULATED DISTILATON-D2887

Typical conditionsTypical conditions

Column length 1.2mColumn length 1.2m

Liquid phase OV-1 SE 30, UC-W 98Liquid phase OV-1 SE 30, UC-W 98

Detector Temp. 350Detector Temp. 350°C/430°C/430°C°C

Injection port Temp. 350°CInjection port Temp. 350°C

Detector (FID )Detector (FID )

Oven Temp. Int. -30°COven Temp. Int. -30°C

Final 350°CFinal 350°C

Oven temp.Oven temp.

program rate 10program rate 10°C/ min.°C/ min.

Carrier gas Nitrogen/HeliumCarrier gas Nitrogen/Helium

Detector gas HydrogenDetector gas Hydrogen

Sample size 1um Sample size 1um

BOILING POINT°C

2121

SHORT PATH DISTILLATIONSHORT PATH DISTILLATION

Used to distill petroleum products up Used to distill petroleum products up to 750to 750°C°C

2222

OUT LINES OF THE METHODSOUT LINES OF THE METHODS

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

Use to distill petroleum products upto 750Use to distill petroleum products upto 750°C.°C.

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Hot POT Distillation apparatusHot POT Distillation apparatus

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