simple distillation (dis) · simple distillation is one of the distillation methods that can be...

EXPERIMENT MODULE

CHEMICAL ENGINEERING EDUCATION LABORATORY

SIMPLE DISTILLATION

(DIS)

CHEMICAL ENGINEERING DEPARTMENT

FACULTY OF INDUSTRIAL TECHNOLOGY

INSTITUT TEKNOLOGI BANDUNG

2018

INSTRUCTIONAL LABORATORY CHEMICAL ENGINEERING DEPT.

FTI - ITB

SIMPLE DISTILLATION MODULE (DIS)

DIS – 2016/PW i

Contributor:

Dr. Danu Ariono, Dr. Dianika Lestari, Dr. Ardiyan Harimawan, Fardhila Rochman,

Alexander Armyn, Dr. Pramujo Widiatmoko


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DIS – 2016/PW ii

TABLE OF CONTENT

TABLE OF CONTENT .......................................................................................................................... ii

LIST OF FIGURES ............................................................................................................................... iii

LIST OF TABLE ................................................................................................................................... iv

CHAPTER I INTRODUCTION ............................................................................................................. 1

CHAPTER II PURPOSE AND TARGET OF EXPERIMENT ............................................................. 2

CHAPTER III EXPERIMENTAL DESIGN .......................................................................................... 3

III. 1. Experiments and Measurements ........................................................................................... 3

III.2. Materials / Chemicals............................................................................................................. 4

CHAPTER IV WORK PROCEDURE ................................................................................................... 5

IV.1. Work Procedures.................................................................................................................... 5

IV.2. Experimental Flow Diagram .................................................................................................. 7

BIBLIOGRAPHY ................................................................................................................................... 8

APPENDIX ............................................................................................................................................. 9

A. Raw Data ..................................................................................................................................... 9

B. Examples of Data Processing .................................................................................................... 13

B.1. Determination of ethanol density .............................................................................................. 13

B.2. Determination of the volume of ethanol needed to make the feed solution .......................... 13

B.3. Calibrate refractive index of ethanol solution with refractometer ......................................... 14

B.4. Determination of heating rate ................................................................................................ 15

B.5. The relationship of distillate concentration to time ............................................................... 16

B.6. The relationship of distillate volume to time ......................................................................... 17

B.7. Mass balance of distillation ................................................................................................... 18

C. Specification and Literature Data ............................................................................................. 19

Tablel C.1. Water density at various temperatures ........................................................................... 19

JOB SAFETY ANALYSIS CONTROL SHEET ................................................................................. 21


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DIS – 2016/PW iii

LIST OF FIGURES

Figure IV.1. Experimental flow diagram ................................................................................................ 7

Figure B.1. Refractometer calibration curve ......................................................................................... 15

Figure B. 2. Relationship curve of distillate concentration to distillation time .................................... 17

Figure B. 3. Distillate volume relation curve to distillation time .......................................................... 18

Figure B. 4. Cumulative distalate volume relation curve to distillation time ....................................... 18

Figure C.1. T-x-y diagram of water ethanol mixture at 1 atm .............................................................. 20


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DIS – 2016/PW iv

LIST OF TABLE

Table A.1. Laboratory condition ............................................................................................................. 9

Table A.2. Thermometer calibration ....................................................................................................... 9

Table A.3. Determination of pure ethanol density .................................................................................. 9

Table A.4. Refractometer calibration ...................................................................................................... 9

Table A.5. Calibration heating rate ....................................................................................................... 10

Table A.6. Distillation ........................................................................................................................... 10

Table B.1. Raw experimental data for ethanol density determination .................................................. 13

Table B.2. Physical data of ethanol used .............................................................................................. 13

Table B.3. Refractometer calibration result data .................................................................................. 14

Table B.4. Measurement data of heating rate ....................................................................................... 15

Table B.5. The measurement data of the refractive index of distillate ................................................ 16

Table B.6. Data of distillate volume measurement ............................................................................... 17

Table B.7. Data table for the calculation of the distillate mass balance ............................................... 19

Tablel C.1. Water density at various temperatures ............................................................................... 19


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DIS – 2016/PW 1

CHAPTER I

INTRODUCTION

Separation is one of the most important process especially in the downstream part of a

chemical process. The principle of separation is to determine the nature difference between

the components to be separated so as to determine the proper separation process to use. The

properties of components can be physical or chemical. One of the physical properties of a

component is its boiling point or temperature when it has the same vapor pressure as the

environmental pressure.

Simple distillation is one of the distillation methods that can be used to separate the mixture

in the liquid form which one component with the other components has a much difference in

boiling point. The mixture will be heated until the temperature exceeds the boiling point of

the lower component but does not exceed the boiling point of the higher component. The

mixture having a liquid phase, some of the more volatile components will be in the gas phase

due to heating so that the two components are separated.

In this experiment a simple distillation process will be carried out to separate the ethanol-

water solution and review the aspects that affect this separation process. The purpose of the

distillation is to obtain a distillate product with higher purity than the feed so that the aspect

under consideration is the aspect affecting the concentration and the quantity of distillate.

Some of the influencing aspects are the feed concentration and feed heating rate which then

reviewed the results by looking at the distillate concentration over time.


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DIS – 2016/PW 2

CHAPTER II

PURPOSE AND TARGET OF EXPERIMENT

The purpose of implementing this experimental module is to study the process of separating

binary mixtures and acquiring skills in performing simple distillation experiments. After

doing the experiment, practition expected:

1. Create a mass balance for ethanol-water distillation experiments.

2. Determine the relationship between the time distillate concentration and the variation

of the ethanol concentration in the feed or the variation in the rate of heating the feed.

3. Compare the results and discuss the experiments with different variations.

4. Determine the relationship between distillate volume to distillation time.


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DIS – 2016/PW 3

CHAPTER III

EXPERIMENTAL DESIGN

III. 1. Experiments and Measurements

1. A set of simple distillation apparatus consisting of:

1 piece of three-necks boiling flask

1 electric heater and heating mantle

1 condenser for counter-current distillation

1 piece adapter to connect three-necks flask with condenser

3 rubber plugs equipped with a hole in the middle (2 pieces fitted with a

three-neck flask and 1 piece fitted with a condenser adapter)

2 pieces of thermometer to measure distillate and bottom

1 sampling device

2 water hoses

2 pairs of stative and clamps

1 piece of adapter to drain the condensed distillate

2. Refractometer

3. Pycnometer

4. Beaker

5. Erlenmeyer flask

6. Vial

7. Drop pipette

8. Filler

9. Stopwatch

10. Measuring cylinder

11. Digital balance

12. Label

13. Cotton

14. Gloves

15. Cloth

16. Aluminium foil

17. Boiling stone


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III.2. Materials / Chemicals

1. Ethanol

2. Aqua dm

3. Acetone

4. Vaselin or silica grease

5. Soap water

6. Ice cube


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DIS – 2016/PW 5

CHAPTER IV

WORK PROCEDURE

IV.1. Work Procedures

a. Checking Tools

1. A glassware removed from cabinet

2. The glassware is checked, if any is broken or cracked please return it. If

something is not clean, clean it first.

3. If any equipment is incomplete, immediately equipped with a report to the

officers and assistants.

4. Once the equipment is ascertained in perfect condition, the lab can proceed.

b. Thermometer Calibration

1. Thermometer that has been confirmed in good condition is prepared.

2. Ice cube is melted in a beaker and then measured melting temperatures of ice

cubes with both thermometers. Temperatures read by both thermometers are

recorded after indicating a constant number.

3. Aqua dm is boiled in a beaker and then the temperature is measured with both

thermometers. Temperatures read by both thermometers are recorded after

indicating a constant number.

c. Refractometer Calibration

1. The standard ethanol-water solution with 8 variations of concentration is made,

the concentration variation include the range of the distillation feed concentration

in order to avoid extrapolation.

2. The refractive index of each is measured using a refractometer

3. The refractive index of each standard solution is recorded.

d. Measurement of Ethanol Density

1. An empty pycnometer mass is weighed and recorded.

2. The pycnometer is filled with aqua dm and its mass is weighed and recorded.

3. The pycnometer is emptied and then cleaned with acetone and dried.

4. The pycnometer is filled with ethanol and its mass is weighed and its measured

results are recorded.


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e. Making feed solution

1. The feed solution was prepared by mixing the ethanol and aqua dm mixtures with

a predetermined amount.

2. Cover the container with aluminum foil.

f. Determination of Heating Rate

1. Water is put into three-necks boiling flask.

2. Flask is placed on top of heater with heating mantle.

3. The thermometer is inserted into one of the necks.

4. The heater is turned on.

5. When boiling, the temperature at each time is recorded.

6. Heating rate is calculated.

g. Distillation

1. The feed solution is fed into the distillation flask together with the boiling stone.

2. Trial tools are strung together and ensured to keep all tools straight.

3. Water to the condenser is flowed.

4. The heater is turned on with a predetermined heating scale.

5. The tool set is checked so that no leakage by dripping the soapy water in the

circuit junctions.

6. The first drop of distillate is awaited. After the first drops drip, the stopwatch is

turned on.

7. Every 3 minutes, the distillate container is replaced with a new one until 8

distillates (24 minutes) are obtained. The volume of each distillate is recorded.

8. Bottom and steam temperatures of distillates formed, the thermometer read are

recorded at each change of the distillate reservoir.

9. After the data is obtained, the heater is turned off and the equipment is kept to

cool.

10. Mass of the distillation flask with the residue is measured. Next, the distillation

flask is emptied and its mass is weighed.

11. All equipment is cleaned up. Steps 1 to 10 are repeated with varying

concentrations or heating rates.


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DIS – 2016/PW 7

IV.2. Experimental Flow Diagram

Start

checking and preparation of module tools

feasible and completecompleteness,

replacement, and repair tool

No

Thermometer calibration

Yes

the actual T calibration equation against actual

theoretical T

determination of ethanol density

using pycnometerEthanol density

Refractometer calibration

Set of distillation devices

the calibration curve of the refractive index against the

ethanol fraction

variation of feed concentration

Variation of heating scale

Distillation

No

Yes

determination of heating rate

Distillation

repeat for 3 different scales

repeat up to 3 variations

Finish

Finish

repeat up to 3 variations

the relationship of distillate concentration

to time

the distillate volume relationship with

time

Figure IV.1. Experimental flow diagram


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BIBLIOGRAPHY

McCabe, W.L., Unit Operation of Chemical Engineering, 3rd

Edition, McGraw-Hill Book

Co., New York, 1978, Chapter 19.

Treybal, R.E., Mass Transfer Operations, McGraw-Hill, 1981 Chapter 9.

Perry, R., Green, D.W., Maloney, J.O., Perry’s Chemical Engineers’ Handbook, 6th

Edition, McGraw-Hill, Japan, 1984.

Veazey, W.R., Hodgman, C.D., Handbook of Chemistry and Physics, 64th Edition, CRC press,

1984.


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DIS – 2016/PW 9

APPENDIX

A. Raw Data

Table A.1. Laboratory condition

Time Pressure (mmHg) Temperature (oC)

09.00 …. ± 0,05 …. ± 0,5

13.00 …. ± 0,05 …. ± 0,5

17.00 …. ± 0,05 …. ± 0,5

Table A.2. Thermometer calibration

T literature Thermometer 1 Thermometer 2

Water freezing point (oC)

Water boiling point (oC)

Table A.3. Determination of pure ethanol density

Thermometer used (Thermometer 1/Thermometer 2)

Aqua dm temperature (oC)

Empty pycnometer mass (g)

Pycnometer mass contains aqua dm (g)

Pycnometer mass contains ethanol (g)

Table A.4. Refractometer calibration

No. Composition of

ethanol

Ethanol

volume

aqua dm

volume

Refractive

index 1

Refractive

index 2

Average refractive

index

1.

2.

3.

4.

5.

6.

7.


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DIS – 2016/PW 10

Table A.5. Calibration heating rate

Heating scale :

Time (s) 30 60 90 120 150 180 210 240

Temperature (oC)

Heating scale :

Time (s) 30 60 90 120 150 180 210 240

Temperature (oC)

Heating scale :

Time (s) 30 60 90 120 150 180 210 240

Temperature (oC)

Table A.6. Distillation

Feed compotition (%-mol etanol) / Heating scale

Thermometer for distillate

Thermometer for bottom

Run to- 1


Feed mass (g)

Bottom mass (g)

Ethanol volume (mL)

Aqua dm volume (mL)

Distillate mass (g)


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DIS – 2016/PW 11

No. Time

(menit)

Distilate

volume

(mL)

Cumulative

volume (mL)

Refractive

index

Bottom

temperature

(oC)

Distillate

temperature

(oC)

1.

2.

3.

4.

5.

6.

7.

8.

Run to- 2


Feed mass (g)

Bottom mass (g)

Ethanol volume (mL)

Aqua dm volume (mL)

Distillate mass (g)

No. Time

(menit)

Distilate

volume

(mL)

Cumulative

volume

(mL)

Refractive

index

Bottom

temperature

(oC)

Distillate

temperature (oC)

1.

2.

3.

4.

5.

6.

7.

8.


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DIS – 2016/PW 12

Run to- 3


Feed mass (g)

Bottom mass (g)

Ethanol volume (mL)

Aqua dm volume (mL)

Distillate mass (g)

No. Time

(menit)

Distilate

volume

(mL)

Cumulative

volume

(mL)

Refractive

index

Bottom

temperature

(oC)

Distillate

temperature (oC)

1.

2.

3.

4.

5.

6.

7.

8.

Distillation Bottom data

No. Time Refractive index

(variaton 1)

Refractive index

(variation 2)

Refractive index

(variation 3)

1.

2.

3.

4.

5.

Bottom mass for variation 1 (g)




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DIS – 2016/PW 13

B. Examples of Data Processing

B.1. Determination of ethanol density

For example data obtained from experiment:

Table B.1. Raw experimental data for ethanol density determination

Temperature of aqua dm (oC) 26

Empty pycometer mass (g) 8,907

Pycnometer mass contains aqua dm (g) 13,708

Pycnometer mass contains ethanol (g) 12,704

Ρwaater at aqua dm temperature (g/cm3) 0,99678

The equation used to obtain pure ethanol density is

The data obtained from the experiment is entered into the equation.

So obtained pure ethanol density.

B.2. Determination of the volume of ethanol needed to make the feed solution

For example data bait solution to be made:

Table B.2. Physical data of ethanol used

Feed total volume (mL) 100

Ρwater at room temperature 26oC (g/cm

3) 0,99678

ρethanol at room temperature 26oC (g/cm

3) 33

Ethanol fraction(%-mole etanol) 10

Available ethanol concentrations (% -v / v) 95

Mr ethanol (g/mole) 46

Mr aqua dm (g/mole) 18

The equations used to calculate the volume of ethanol required to prepare the feed solution

are:


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DIS – 2016/PW 14

Entered data to make the feed solution.

From the calculation, the required ethanol volume is obtained to obtain the aqua dm volume

required to prepare the feed solution which is the difference between the total volume of the

desired feed and the required ethanol volume. The above equation can also be used to

calculate the volume of ethanol and aqua dm required to prepare ethanol solution at the

refractometer calibration.

B.3. Calibrate refractive index of ethanol solution with refractometer

Example data obtained from the experiment:

Table B.3. Refractometer calibration result data

Each sample volume is 20 mL

No.

The composition of

ethanol (mol

ethanol / mol aqua

dm)

Ethanol

volume

(mL)

Aqua dm

volume

(mL)

Refractive

index 1

Refractive

index 2

Average

Refractive

index

1. 0 0 20,00 1,3326 1,3325 1,33255

2. 0,03 1,83 18,17 1,3363 1,3362 1,33625

3. 0,06 3,44 16,56 1,3405 1,3416 1,34105

4. 0,09 4,87 15,13 1,3458 1,3448 1,3453

5. 0,12 6,15 13,85 1,3480 1,3491 1,34855

6. 0,15 7,30 12,70 1,3522 1,3512 1,3517


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7. 0,18 8,34 11,66 1,3543 1,3544 1,35435

8. 0,21 9,30 10,70 1,3565 1,3559 1,3562

The measurement data of refractive index of ethanol solution with various concentrations

using refractometer was plotted and linear regression was done so that it is become

calibration curve. The calibration curve was used to determine the ethanol fraction for the

distillate sample taken during the distillation experiment.

Figure B.1. Refractometer calibration curve

From the calibration curve obtained equation

or

B.4. Determination of heating rate

Suppose the data obtained from the experiment is

Table B.4. Measurement data of heating rate

y = 0.0035x + 1.3301

1.33000

1.33500

1.34000

1.34500

1.35000

1.35500

1.36000

0 2 4 6 8 10

Ref

ract

ive

ind

ex

Ethanol fraction(%-mol etanol)


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DIS – 2016/PW 16

Heating scale : 7

Time (s) 30 60 90 120 150 180 210 240

Temperature (oC) 78 81 82,5 84 86 87,5 89 91

From the data in Table B.4 we can calculate the rate of heating by the equation

With an average increase in temperature every 30 seconds ie 1,86oC the rate of heating is

obtained. For aqua dm as much as 300 mL, its mass is 299,1 gram and from literature

obtained data of Cp aqua dm at 26oC that is equal to 4,179 kJ/kg.K.

B.5. The relationship of distillate concentration to time


Table B.5. The measurement data of the refractive index of distillate

No. Time (minute) Refractive index

Ethanol

fraction (% -

mol ethanol)

1. 3 1,3617 9,03

2. 6 1,3616 9,00

3. 9 1,3609 8,80

4. 12 1,3606 8,71

5. 15 1,3605 8,68

6. 18 1,3594 8,37

7. 21 1,3583 8,05

8. 24 1,3571 7,71

The mole fraction of ethanol in the sample was obtained from the previous calibration of

refractometer so that the curve of the relationship between the distillate concentration and the

distillation time was obtained.


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DIS – 2016/PW 17

Figure B. 2. Relationship curve of distillate concentration to distillation time

B.6. The relationship of distillate volume to time


Table B.6. Data of distillate volume measurement

No. Time (minute) Distillate volume (mL) Cumulative volume (mL)

1. 3 14,5 14,5

2. 6 13,7 28,2

3. 9 12,6 40,8

4. 12 11,3 52,1

5. 15 11,1 63,2

6. 18 10,0 73,2

7. 21 9,5 82,7

8. 24 9,0 91,7

By diverting the distillate volume data to the distillation time, there is a

relationship of volume at each time or cumulative volume to the distillation time

and a graphic tendency can be seen.

7.6

7.8

8

8.2

8.4

8.6

8.8

9

9.2

0 5 10 15 20 25 30

Eth

an

ol

fra

ctio

n (

%-m

ole

)

Time (menit)


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DIS – 2016/PW 18

Figure B. 3. Distillate volume relation curve to distillation time

Figure B. 4. Cumulative distalate volume relation curve to distillation time

B.7. Mass balance of distillation

In accordance with the law of conservation of mass for system without

reaction then

For example experimental data for distillation with 10% feed solution -mol ethanol

0

2

4

6

8

10

12

14

16

0 5 10 15 20 25 30

Vo

lum

e (m

L)

Time (menit)

0

10

20

30

40

50

60

70

80

90

100

0 5 10 15 20 25 30

Vo

lum

e (m

L)

Time (minute)


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Table B.7. Data table for the calculation of the distillate mass balance

Feed mass (g) 278,4

Final bottom mass (g) 180,6

Bottom sample mass (g) 19,6

The distillate mass (g) 77

gram

Loss of mass as much as 1.2 gram can be explained when done by calculation of mass

balance more detail by involving ethanol fraction of experiment analysis result so that can

know whether mass loss of water or ethanol and can be analyzed why mass balance

calculation is deviated as 0,43%.

C. Specification and Literature Data

Tablel C.1. Water density at various temperatures

(Source : Handbook of Chemistry and Physics, CRC press, 64th Ed.)


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(Source : Dortmund Data Bank)

Figure C.1. T-x-y diagram of water ethanol mixture at 1 atm


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JOB SAFETY ANALYSIS CONTROL SHEET

No. Material Material properties Repressive act

1. Water

- Colorless

- No smell

- Non-toxic

- Boiling point: 100oC

- Melting point: 0oC

- Stable

- Delivers electricity

- No need special handling

because it is not harmful to the

body.

- Avoid substances scattered near

the power source.

2. Ethanol

-Liquid

-Colorless

-Easy to evaporate

-Flammable in both liquid and gas

form

-Smell light

-Boiling point: 78oC

- Melting point: -114oC

- Soluble in water

-Make sure the substance

container is closed when not

in use.

-Store in a place with good

ventilation.

-Avoid from the fire.

-Avoid contact with eyes and

mouth.

3. Acetone

-Liquid

-Colorless

- Smells strongly fragrant

- Soluble in water

- Good solvent

-Stable

- Not corrosive

- Boiling point: 58.02oC

- Melting point: -95.35oC

- Make sure the substance

container is closed when not

in use.

-Store in a place with good

ventilation.

- Avoid from the fire.

Avoid contact with eyes and

mouth.

4. Vaselin

- Shaped white gel

- Not reactive

- Melting point: 48oC-52

oC

- Flash point: 190oC

- Avoid contact with eyes

and mouth.


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Accidents that may occur Repressive act

Equipment breaks and fractions exposed to

body parts.

- Put the broken equipment in a stable

place so it is not easy to fall.

- The hot glass equipment is not directly

cooled with water.

- When fractions exposed to body parts

immediately contact the assistant to

provide first aid.

The vapors of the substance are exposed to

the eye resulting in irritation.

Rinse eyes with running water, seek medical

help.

Substances inhaled in large quantities. Immediately move to the open, breathe fresh

air, seek medical help.

Substances ignite fire and cause fire. Substances ignite fire and cause Fire

extinguisher with a damp cloth or fire

extinguishers, keep the fire away from

potentially flammable items, away from fire.

Shorting due to the entry of water to the

power source.

- Keep water from a power source.

- Clean and dry the stagnant water.

- If electrocuted, a non-stuck practitioner

should unplug an electrical connection

with rubber gloves, contact the assistant

and the clerk.

Safety equipment

Gloves Laboratory coat Goggle

Safety Procedures

Preparation of materials

- Acetone and alcohol are always placed

in a closed container so that the vapor is

not harmful.

- Keep acetone and alcohol from the fire.

- Keep acetone from soluble ingredients.

Tools preparation

- Put the equipment tightly and neatly,

attach the clamps in a prone area.

- Apply vaseline on each tool joint.

Post distillation

- Turn off the heater before discharging

the condenser water flow.

- Be careful on equipment that is still hot.

- Unplug the electricity and dry the work

Distillation

- Use boiling rocks during

distillation for homogeneous

heating.

- Flow the condenser water before


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DIS – 2016/PW 23

area. turning on the heater.

- Observe the distillation feed,

warm up to the exhausted feed can

be harmful to the distillation flask.

Assistant Advisor Lab TK Coordinator

simple distillation (dis) · simple distillation is one of the distillation methods that can be...

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