ABSTRACT

The aim of the experiment is to observe the effect on mixing the mass transfer
coefficient of acetic acid diffusing from organic phase to aqueous phase.

,
 ii

TABLE OF CONTENTS

TABLE OF CONTENTS...........................................................................iii
LIST OF FIGURES...............................................................................iv
LIST OF TABLES..................................................................................v
1. INTRODUCTION...............................................................................1
2. THEORETICAL BACKGROUND...............................................................2
3. EXPERIMENTAL SET UP AND CHEMICALS..................................................4
3.1. EQUIPMENTS..............................................................................4
3.2. CHEMICALS...............................................................................4
4. PROCEDURE...................................................................................6
5. CALCULATIONS AND EXPERIMENTAL RESULTS............................................7
5.1. CALCULATIONS........................................................................7
5.2 EXPERIMENTAL RESULTS..............................................................9
6. DISCUSSION..................................................................................10
7.1.CONCLUSION..........................................................................11
7.2. RECOMENDATION....................................................................11
REFERENCES.................................................................................12
APPENDIX.....................................................................................13
APPENDIX A................................................................................13
APPENDIX B................................................................................24
 iii

LIST OF FIGURES

Figure 2.1 Example of Liquid-Liquid Extraction

Figure 3.1 Experimental Set-up...............................................................5
Figure 5.1 Calibration Curve
Figure A.1 Conductivity vs Time for 130 rpm
FigureA.2 Conductivity vs Time for 330 rpm
FigureA.3 ln(C A ∞−C A ¿ vs Time for 130 rpm
Figure A.4 ln(C A ∞−C A ¿ vs Time for 330 rpm
 iv

LIST OF TABLES

Table 5.1 K values for different measurements............................................9

Table A.1 Acid Concentration and Conductivity data....................................13
Table A.2 Calculations for 130 rpm.........................................................13
Table A.3 Calculations for 330 rpm.........................................................20
 1

1. INTRODUCTION
The experiment was mention about the effect of mixing on mass transfer
coefficient. General information about liquid-liquid extraction (solvent extraction)
was given and separation processes and separation methods for some substances
are mentioned and sampled in theoretical part. All chemicals and equipment used
in experiment were listed in experimental set-up part. Acetic acid concentration
versus conductivity graph were plot in calculation part. ln(C A ∞−C A ¿ versus time
graph was plotted for 130 rpm and 330 rpm, showed in Appendix. All other datas
were showed in Appendix part. In discussion part, according to the calculation and
graphs, datas and graphs were discussed. Also the reason of the slopes of different
ka values were discussed. Some conclusion and recommendation about these
experiments were showed in this part.
 2

2. THEORETICAL BACKGROUND
Liquid-liquid extraction which was also known solvent extraction is dispersion of a
substance between two immiscible liquids to a certain extent is called solvent
extraction. Extraction process consists of an aqueous solution and an organic
solvent. One of the most used in solvent extraction process is water. The other
phase is must be immiscible or slightly immiscible with water. Because seperation
process can take place if two substance are immiscible or sligtly immiscible in each
other. [1]

If a foreign substance is not added to an operation, it is called a direct method.

Such as, distillation, evaporation. The other method is indirect method. Solvent
extraction is not include direct method because solvent (foreign substance) is
added into operation. Aborption, adsorption, ion exchange can be given an
example of this operation. [2]

Figure 2.1 Example of Liquid-Liquid Extraction

Acetic acid from organic phase into an aqueous solution can give an example of
solvent extraction. It is non-reacting. This example is physical method and indirect
methods. Exact concentration can not find so, conductivity-meter can be used. In
conductivity-meter, lower phase is organic phase and upper phase is aqueous
phase. The acetic acid transfer rate is considered the first order according to the
 3

difference between the final concentration (C A∞) and actual solute concentration
(CA). Rate of exchange of solute concentration can be expressed by:

dC A (2.1)
VA =k a A(C A ∞−C A )
dt

Which can be integrated as:

CA
dC A k A
t
(2.2)
∫ (C −C = a ∫ dt
VA 0
C Ai
A∞ A)

ka A (2.3)
ln (C A ∞−C A )=(C A ∞−C Ai )− t
VA
 4

3. EXPERIMENTAL SET-UP
3.1 Equipment

 1000 ml Beaker
 50 ml Beaker*4
 Separator funnel
 50 ml Burette
 Conductivity meter
 Mechanical stirrer
 50 ml Erlenmeyer Flask*5,
 20 ml Graduated cylinder*4
 Droppers
 1000 ml Round bottom flask

3.2 Chemicals

 Acetic acid, CH3COOH

 Distilled water, H2O
 Sodium hydroxide, NaOH
 Chloroform, CHCl3
 Phenolphthalein, C20H14O4
 5

Figure 3.1 Experimental Set-up

 6

4. PROCEDURE
1. 0.1 M 500 mL NaOH was prepared. 2 g NaOH was taken and it was put in 500
mL volumetric flask. Then, water was added in 500 mL volumetric flask.
2. 0.1 M 250 mL acetic acid (CH 3COOH) solution was prepared. 1.43 g CH 3COOH
was put in 250 mL volumetric flask. Then, water was added in volumetric
flask.
3. Stock solution was prepared. 1000 mL chloroform was taken and put in round
bottom flask. 20 mL acetic acid solution was added in round bottom flask.
4. 400 mL stock solution was put in 1000 mL beaker and also 400 mL water was
added same beaker.
5. Magnetic stirrer was set 130 rpm.
6. Probe of conductivitymeter was put in solution and datas were taken 20
second intervals by used chronometer. Measurement was continued until
datas were not changed.

5. EXPERIMENTAL RESULTS AND SAMPLE CALCULATION

5.1 Sample Calculations

In calculation part, first of all, calibration curve was plotted which was using
concentration versus conductivity data as Figure 5.1.
 7

Figure 5.1 Calibration Curve

After that, the conductivity of acetic acid was found with the help of different
concentration of acetic acid. Then, ln(C A ∞−C A ¿ versus time graph was plotted.
The slope of this graph was given – k a A /V A . The slope of the calibration curve was

y=0.0003x-0.036

x values shows that the conductivity values according to the equation. All values
were represents in Appendix. Then, ln(C A ∞−C A ¿ versus time graph was plotted for
130 rpm. According to the equation

Slope= – k a A /V A

D=11 cm=0.11 m

V=400 mL=0.0004 m3

For the second part of the experiment, the same calculation was repeated for the
330 rpm and the slope of the graph was found as 8.418x10-6 m/s.

-3 2
-k(9.5033× 10 m )
0.0002=
0.0004 m 3

K= 8.418x10-6 m/s
 8

In the first part of the experiment, the stock solution was prepared. Then, 10 mL
sodium hydroxide was put into the burette. The amount of acetic acid and sodium
hydroxide was calculated.

CH3COOH + NaOH→ H2O + CH3COONa (5.1)

The molecular weight of the acetic acid was 60.05 g/mol.

1L -3
Volume=31.3 mL× =31.3× 10 L
1000 mL

m=(0.1 M) x 31.3× 10-3 L x 60.05 g/mol= 0.188 g

For 400 mL solution

400
n=0.188 g x =7.518 mol
10

For the organic phase

4.1 mL= 4.1× 10-3 L

m= (0.1 M) x 4.1× 10-3 L x 60.05 g/mol= 0.025 g

For 400 mL solution

400
m= 0.025 g x =0.985 g
10

For the aqueous phase

29.2 mL= 29.2× 10-3 L

m= (0.1 M) x 29.2× 10-3 L x 60.05 g/mol= 0.175 g

For 400 mL solution

 9

400
m= 0.175 g x =7.014 g
10

Total mass balance: 7.014 g + 0.985 g = 7.998 g

5.2 Experimental Result

Table 5.1 K values for different measurements

K values for 130 rpm K values for 330 rpm

3.367x10-6 m/s 8.418x10-6 m/s

6. DISCUSSION
This experiment is done to observe how mixing effect the mass transfer coefficient
(ka) of acetic acid diffusing from organic phase (at the beginning it contains
chloroform and acetic acid) to aqueous phase since diffusion is movement from
high concentration to low concentration.This observation done by measuring
conductivity data and concentration data which are found with using conductivity
data. ( calibration curve is used.) ka value is found in calculation part as in lower
mixing speed smaller than in higher mixing speed . If the experiment is done with
longer time until the equilibrium point (where all acetic acid molecule diffuse to
aqueous phase) is reached, the ka value would be equal in both speed since the
amount of acetic acid inside organic phase is not changed. However, the time that
require for completely diffusion of acetic acid to aqueous phase will be longer for
 10

low speed mixing. Chloroform, water and acetic acid forms tertiary system since
chloroform is soluble in water and insoluble in acetic acid and it helps to make easy
to observation, also diffusion of acetic acid in water becomes maximum (Also,
acetic acid soluble in both liquid). Two phase is observed when liquids are mixing;
lower phase is organic phase and upper phase is aqueous phase because of lower
low density of water and solubility difference.When water added to acetic acid,
solution conductivity increases since amount of ion that formed is increases.

Titration made for obtaining amount of acetic acid in different phase and inside
the stock solution. Measured amount of acetic acid is become less precise because
at second part of experiment, dark pink is observed when phenolphthalein is added
into organic phase and this color change is unwanted result for obtaining data.(This
part repeated but same color is observed.)

7. CONCLUSION and RECOMMENDATION

7.1. Conclusions
Liquid extraction method is used to predict mass transfer coefficient of acetic acid
and which factors affect to change mass transfer coefficient.It was experimentally
proved and showed with graph in figure A.1 and in figure A.2 that diffusion will be
faster if magnetic stirrer is used in high speed(in high rpm) and necessary time for
same diffusion of acetic acid will be shorter.Also graphs in figure A.1&A.2 and
tables A.2&A3 show that with increasing time values, conductivity values are also
increasing and that’s why concentration values are also increasing.With help to this
relation, conductivity data is used to obtain related concentration in calculation
part and this result is used to find diffusion mass transfer coefficient for different
speed. Also, titration value is used to confirm overall mass balance and
concentration values that taken from calibration curve.
 11

7.2. Recommendations
To be sure about diffusion of acetic acid from organic phase to aqueous phase
finished, data can be recorded longer so that mass transfer coefficient will be more
realistic and it help to obtain same result for both part of the experiment.In
titration part, phenolphthalein is used for indicating acid concentration and light
pink is observed when equilibrium is achieved.In some part of titration dark pink is
observed as mentioned in discussion part and it is unwanted result for accuracy.To
avoid any unaccuracy, Ph-meter can be used since it gives more accurate result of
acid content in solution.

Also for making comparison and understanding relation of mass transfer coefficient
with different parameter, experiment can be repeated with changing some
parameter in experiment like using bigger beaker or changing temperature.ka value
depends on diffusion area between organic and aqueous phase. If bigger beaker is
used for diffusion of acetic acid to aqueous phase, the diffusion will be faster.

References

1. https://www.researchgate.net/publication/
318561499_Separation_of_Acetic_acid_from_aqueous_solution_using_various
_organic_solvents
2. Analytical Chemistry 1991,63,5, 275A-282A
3. https://www.docsity.com/pt/mass-transfer-operations-robert-treybal/
4740450/
 12

APPENDIX
Appendix A

Table A.1 Acid Concentration and Conductivity data

Acid Concentration (M) Conductivity (µs/cm)

0.01 140

0.025 288

0.05 360

0.075 436

0.1 488
 13

5560 799 0.2037 -1.591106956

5580 800 0.204 -1.589635285
5600 800 0.204 -1.589635285
5620 800 0.204 -1.589635285

Table A.3 Calculations for 330 rpm

Conductivity Concentration
Time (s) (µs/cm) (M) ln(C A ∞−C A )
0 5.6 0.0192 -3.952845
20 506 1.482 0.393392527
40 527 1.545 0.43502391
60 588 1.728 0.54696467
80 622 1.83 0.604315967
100 643 1.893 0.638162872
120 646 1.902 0.642905964
140 648 1.908 0.646055573
160 650 1.914 0.649195293
180 652 1.92 0.652325186
200 653 1.923 0.653886467
220 655 1.929 0.657001734
240 657 1.935 0.660107326
260 659 1.941 0.663203304
280 661 1.947 0.666289726
300 663 1.953 0.669366652
320 664 1.956 0.670901572
340 667 1.965 0.675492245
360 668 1.968 0.677017799
380 670 1.974 0.680061941
400 672 1.98 0.683096845
420 674 1.986 0.686122566
440 675 1.989 0.687632
460 677 1.995 0.69064405
480 679 2.001 0.693647056
500 681 2.007 0.69664107
520 682 2.01 0.698134722
540 684 2.016 0.70111535
560 685 2.019 0.702602339
580 687 2.025 0.705569701
600 689 2.031 0.708528283
 14

620 690 2.034 0.710004298

640 692 2.04 0.712949808
660 694 2.046 0.715886668
680 695 2.049 0.717351869
700 697 2.055 0.720275848
720 698 2.058 0.721734637
740 700 2.064 0.724645848
760 701 2.067 0.726098281
780 703 2.073 0.728996833
800 704 2.076 0.730442965
820 706 2.082 0.73332897
840 707 2.085 0.734768855
860 708 2.088 0.73620667
880 710 2.094 0.739076112
900 711 2.097 0.740507752
920 713 2.103 0.743364897
940 714 2.106 0.744790414
960 716 2.112 0.747635366
980 717 2.115 0.749054812
1000 718 2.118 0.750472247
1020 720 2.124 0.753301103
1040 721 2.127 0.754712536
1060 722 2.13 0.75612198
1080 723 2.133 0.757529439
1100 725 2.139 0.76033843
1120 726 2.142 0.761739972
1140 727 2.145 0.763139552
1160 729 2.151 0.76593285
1180 730 2.154 0.767326579
1200 731 2.157 0.768718367
1220 732 2.16 0.770108222
1240 733 2.163 0.771496147
1260 734 2.166 0.772882149
1280 736 2.172 0.775648402
1300 737 2.175 0.777028665
1320 738 2.178 0.778407025
1340 739 2.18 0.779324877
1360 740 2.184 0.781158058
1380 741 2.187 0.782530742
1400 742 2.19 0.783901544
1420 743 2.193 0.785270469
1440 744 2.196 0.786637524
1460 745 2.199 0.788002712
1480 747 2.205 0.790727509
1500 748 2.208 0.792087128
1520 749 2.211 0.793444902
 15

1540 750 2.214 0.794800834

1560 751 2.217 0.796154931
1580 752 2.22 0.797507196
1600 752 2.22 0.797507196
1620 753 2.223 0.798857635
1640 754 2.226 0.800206253
1660 756 2.232 0.802898045
1680 757 2.235 0.804241228
1700 757 2.235 0.804241228
1720 758 2.238 0.80558261
1740 759 2.241 0.806922195
1760 760 2.244 0.808259988
1780 761 2.247 0.809595993
1800 762 2.25 0.810930216
1820 763 2.253 0.812262661
1840 764 2.256 0.813593334
1860 764 2.256 0.813593334
1880 765 2.259 0.814922237
1900 767 2.265 0.817574759
1520 768 2.268 0.818898386
1540 769 2.271 0.820220263
1560 769 2.271 0.820220263
1580 769 2.271 0.820220263
1600 770 2.274 0.821540395
1620 771 2.277 0.822858787
1640 772 2.28 0.824175443
1660 773 2.283 0.825490368
1680 774 2.286 0.826803565
1700 774 2.286 0.826803565
1720 775 2.289 0.828115041
1740 776 2.292 0.829424799
1760 777 2.295 0.830732844
1780 778 2.298 0.832039179
1800 778 2.298 0.832039179
1820 779 2.301 0.833343811
1840 780 2.304 0.834646743
1860 780 2.304 0.834646743
1880 781 2.307 0.835947979
1900 783 2.313 0.838545383
1920 783 2.313 0.838545383
1940 784 2.316 0.83984156
1960 785 2.319 0.841136058
1980 786 2.322 0.842428883
2000 786 2.322 0.842428883
2020 787 2.325 0.843720039
2040 788 2.328 0.84500953
 16

2060 788 2.328 0.84500953

2080 789 2.331 0.84629736
2100 790 2.334 0.847583534
2120 790 2.334 0.847583534
2140 791 2.337 0.848868056
2160 792 2.34 0.850150929
2180 792 2.34 0.850150929
2200 793 2.343 0.85143216
2220 793 2.343 0.85143216
2240 794 2.346 0.85271175
2260 795 2.349 0.853989706
2280 795 2.349 0.853989706
2300 796 2.352 0.85526603
2320 797 2.355 0.856540727
2340 797 2.355 0.856540727
2360 798 2.358 0.857813802
2380 798 2.358 0.857813802
2400 799 2.361 0.859085258
2420 799 2.361 0.859085258
2440 800 2.364 0.8603551
2460 800 2.364 0.8603551
2480 800 2.364 0.8603551

Appendix B
 17

Figure A.1 Conductivity vs Time for 130 rpm

Figure A.2 Conductivity vs Time for 330 rpm

18