TABLE OF CONTENTS

Title Abstract/Summary Introduction Objectives Theory Procedures Apparatus Results Calculation Discussions Conclusions Recommendations References Appendices

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ABSTRACT AND SUMMARY Experiment A Experiment A is the experiment to determine the distribution coefficient for the system organics solvents Propionic acidWater. The concentration values depends on the distribution value. In this Page 1 of 11

experiment, absorber has been used. The reason is because the extract(organic solvent)flow throw pallet ring to raffinate(Propionic acid). It will compromise with water to separate the organic solvent and propionic acid. This experiment is to be to titrated and measured completely. Hence, when the volume of propionic acid that added to the mixture decreases, the value of the distribution coefficient, K also decreases. Experiment C Experiment C is the experiment to measure the coefficient without equipment of the machine. This experiment is more accurate because no equipments were exposed. It is similar with experiment A to determine the distribution coefficient. This experiment does not need to be titrated, but the separation of separate the extract and raffinate substances are needed. Then Phenolphthalein can be used as an indicator. Introduction Objectives Experiment A To determine the distribution coefficient for the system organic solvent-Proponic Acid-Water and to show its dependence on concentration. Experiment C To demonstrate how a mass balance is performed on the extraction column, and to measure the mass transfer coefficient with the aqueous phase as the continuous medium.

Theory Experiment A Page 2 of 11

The solvent (water) and solution (organic solvent / propionic acid) are mixed together and then allowed to separate into the extract phase and the raffinate phase. The extract phase will be water and propionic acid and the raffinate,organic solvent with a trace of propionic acid. The distribution coeffient, K, is defined as the ratio, Concentration of solute in the extract phase, Y Concentration of solute in the raffinate phase, X It is assumed that equilibrium exists between the two phases. At low concentrations, the distribution coefficient is dependent on the concentration and thus Y=KX. Experiment C Let VW V0 X Y Subscripts:
1 2

= = = = = =

Water flow rate (l/s) Organic solvent flow rate (l/s) Propionic Acid concentration in the organic phase (kg/l) Propionic Acid concentration in the aqueous phase (kg/l) Top of column Bottom of column

1. Mass Balance Propionic Acid extracted from the organic phase (raffinate) = V0 (X1-X2) Propionic Acid extracted from the aqueous phase (extract) Page 3 of 11

=VW (Y1-0) Therefore V0 (X1-X2) = VW (Y1-0) 2. Extraction Efficiency Mass transfer coefficient (based on the raffinate phase) = Rate of Acid Transfer Volume of Packing x Mean Driving Force Log mean driving force = x1 - x2 Ln x1/x2 Where x1 x2 = = Driving force at the top of column = (X2-0) Driving force at the bottom of the column = (X1-X1*)

Where X1* is the concentration in the organic phase which would be in the equilibrium with concentration Y1 in the aqueous phase. The equilibrium values can be found using the distribution coefficient found in the first experiment.

Apparatus and Procedures Apparatus Experiment A Page 4 of 11

1. 250ml Conical stoppered flask 2. 250ml Measuring cylinder 3. 250ml Separating Funnel 4. Pipette with rubber bulb 5. Sodium Hydroxide Solution (0.1M) 6. Phenolphthalein 7. Propionic acid Experiment C

The solvent matering pump is calibrated in percentage of maximum flow which varies slightly from pump to pump. The pump should be calibrated initially by setting F2 to 100%, setting valve V8 to the calibrate position and measuring the flow from the pump, using the measuring cylinder and stopwatch.

Procedures
Experiments A 1. A mixture of 50ml organic solvent and 50ml of de-mineralised water were makeup in a conical flask. Page 5 of 11

2. 5ml of propionic acid were added. It can be pipetted into the flask using a pipette with a rubber bulb. 3. A stopper was placed into the flask and was shaked for a minimum of 5 minutes. 4. The mixture were poured into a separating funnel, and then leaved for 5 minutes and the lower aqueous layer was removed. 5.10ml sample of this layer were taken and 0.1M sodium hydroxide was titrated using phenolphthalein as indicator 6. The experiment for two further concentrations of propionic acid were repeated for initial additions of 3ml and 1ml of propionic acid. Experiment C 1. 100ml of propionic acid was added to 10 liters of the organic phase. The solution were mixed well to ensure an even concentration and then the organic phase feed tank (bottom tank) is filled with the mixture. 2. The level control was switched to the bottom of the column (electrode switch S2) 3. The water feed tank was filled with 15 liters of clean de-mineralised water. The water feed pump started and the column was filled with water at a high flow rate. 4. As soon as the water was above the top of the packing, the flow rate was reduced to 0.21/min. 5. The metering pump was started and the flow rate of 0.21/min was set. 6. 15-20 minutes were needed to run until steady conditions were achieved. The flow rates during this period must be monitored to ensure that they remain constant. 7. 15ml samples were taken from the feed, raffinate and extract streams. DO NOT use the calibration valve V8 for taking feed samples. 8. 10ml of each sample were titrated against 0.1 M NaOH using phenolphthalein as the indicator. (To titrate the feed and raffinate they may need continuous stirring using magnetic stirrer. Alternatively: 0.025 M NaOH may be used which will lead to phase inversion of the raffinate and feed streams so that aqueous phase is the continuous phase) WARNING: Ensure that diluted Sodium Hydroxide (NaOH) is used when performing this experiment.

8.0 Calculations
Experiments A 5 mL Propionic Acid M1V1 = M2V2 Page 6 of 11

M2

= M1V1 V2 M2 = (0.1)( 73.3) 10 So, X = 0.733 MOLE Propionic Acid Concentration in Organic Layer, Y = (0.1)(46) 10 So, Y = 0.46 K = Y X = 0.46 0.733 = 0.628 MOLE M1

3 ML of Propionic Acid Propionic Acid Concentration in aqueous Layer, X M2 = (0.1)(54.5) 10 So, X = 0.545 MOLE Propionic Acid Concentration in Organic Layer, Y M1 = (0.1)(24.8) 10 So, Y = 0.248 MOLE K = 0.248 0.545 = 0.455

1 ML of Propionic Acid Propionic Acid Concentration in Organic Layer, X

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M2

= (0.1)(45.0) 10 So, X = 0.45 MOLE Propionic Acid Concentration in Organic Layer, Y M1 = (0.1)(19.3) 10 So, Y = 0.193 MOLE K = 0.193 0.45 = 0.429

Experiment C The concentration of feed sample, M1V1= M2V2 M = (0.025) (46.0) (10)(1000) = 1.15X10-4 MOLE The concentration of raffinate sample, M1V1= M2V2 M = (0.025)(2.8) (10)(1000) = 7X10-7 MOLE The concentration of extract sample, M1V1= M2V2 M = (0.1)(2.1) (10)(1000) = 2.1X10-5 MOLE Mass balance Propionic acid extracted from the organic phase (raffinate) Page 8 of 11

= V0(X1-X2) Propionic acid extracted from the aqueous phase = Vw (Y1 0) V0= = ( 0.2 lit/min)x(1min/60s) = 3.33 x 10-3 lit/s Vw = = (200 cm3 / min) x (1 min/ 60 s) x (1litre/ 1000 cm3 ) = 3.33 x 10-3 lit/s Propionic acid extracted from the organic phase = V0(X1X2) = (3.33x10-3 lit/s) (6.75X10-6 1.00X10-6) kg/l = 1.92X10-8 kg/s Propionic acid extracted from the aqueous phase = Vw (Y10) = ( 3.33x10-3) x (9.00X10-6 0 )kg/l = 2.997X10-8 kg/s To conclude Propionic acid extracted from the organic phase Propionic acid extracted from the aqueous phase

9.0 Result And Discussion Result

Experiment A

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Propionic acid added (ml)

Titre of M/10 NaOH X Y 46.0 24.8 19.3 73.3 54.5 45.0

Propionic acid concentration in aqueous layer ,X 0.733 0.545 0.45

Propionic acid concentration in organic layer ,Y 0.46 0.248 0.193

K=Y X 0.628 0.455 0.429

5 3 1 Experiment C

Flow rate of Aqueous Phase Flow rate of Organic Phase Titre of M/10 NaOH Feed Raffinate Extract Propionic acid extracted from the organic phase Propionic acid extracted from the aqueous phase 46.0 2.8 2.0 1.92X10-8 kg/s 2.33X10-8 kg/s Concentration of Propionic Acid kg/L 0.0115 7.5X10-6 9.00X10-6

Propionic Acid concentration in the organic phase (kg/L) for feed, for 0.025M NaOH 46.0/1000 =0.046 so, 0.046x0.025 =0.0115 kg/L 10 x10-3 Propionic Acid concentration in the aqueous phase (kg/L) for raffinate, for 0.025M NaOH 2.8/1000 = 0.0028 so, 0.0028x0.025 10 x10-3 Propionic Acid concentration in the aqueous phase (kg/L) for extract, For 0.1M NaOH Page 10 of 11 =0.0007 kg/L

2.0/1000 = 0.002 so, 0.002x0.1 =

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