Experimental Confirmation of Overall

and Component Mass Balances in a

Liquid-Liquid Extraction Unit

Anna Welton-Arndt, Emily Condic, Matt Koberstine, Natalia Markiewicz, Lorenzo

Estrada, Aditya Kapoor
Introduction

Liquid-liquid extraction separates

compounds utilizing chemical potential

In this experiment, t-BuOH contaminates

a mineral oil feed and is removed by water
in the column

Ideal goal: To achieve pure mineral oil

raffinate (0% t-BuOH)

2
Introduction

3
Objectives

Main Points:

● Verify overall and component mass balances for LLE column

○ t-BuOH content measured via refractive index (RI)
○ Pump calibration and calibration curve for % t-BuOH in water/mineral oil
versus RI
● Determine how quickly feed can be run while still achieving mineral oil
purification
● Determine to what extent the feed can purified of t-BuOH

4
Approach

1. Two trials ran with varying flow speeds

a. Filled column with 4.5 L water for extraction of t-BuOH
b. Collect raffinate and water phase samples every 10 minutes; determine wt%
t-BuOH via RI
c. Time started once desired flow rate was set and pump was turned on
d. Trial ended upon consumption of feed
2. wt% t-BuOH of raffinate and water plotted versus time
3. Mass balance equation applied:
a. Overall: Feed + Stagnant Phase=Extract + Raffinate
b. Component: xtBuOH,feed *Vfeed*dfeed = xtBuOH,aq*Vaq*daq + xtBuOH,raf*Vraf*draf

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Results - Trial 1 Mass Flow Rate t-BuOH in Raffinate

Trial 1 Conditions
● 4.73% t-butanol in feed
● Flow rate: ~390 mL/min
● 4052 mL H2O in column
● Mass in: 11.7 kg
● Mass out: 11.9 kg

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Results - Trial 2 Mass Flow Rate t-BuOH

Trial 2 Conditions
● 7.48% t-butanol
● Flow rate: ~220 mL/min
● 4052 mL H2O

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Results - Trial 2 Weight Percent in Water

Trial Conditions
● 7.48% t-butanol
● Flow rate: 220 mL/min
● 4052 mL H2O

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Results - Mass Balance

Overall Mass Balance

Component Mass Balance

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Results - Mass Balance
Trial Overall Mass In Overall Mass Difference Percent
(g) out (g) (g) Difference

1 (48 minutes) 11659 - - -

2 (73 minutes) 13714 13720 6 0.04%

Trial Tert-butanol Tert-butanol Difference Percent

Mass In (g) Mass out (g) (g) Difference

1 552 - - -

2 697 534 173 28.33%

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Calibration Curve - wt% tBuOH in Mineral Oil (Refractive
Index)

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Calibration Curve - wt% tBuOH in Water (Refractive Index)

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Calibration Curve - Flow Rate of Mineral Oil Pump

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Equipment

Column

Mineral Oil Raffinate

Mineral Oil Feed Tank Tank

Stainless Steel
Mineral Oil Feed
Water Feed Tank
Pump

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Refractometer

Measures refractive index of liquid

samples

Model: Bausch & Lomb

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Mineral Oil Feed Tank

Feed is a mixture of mineral oil from conical tank 16

Mineral Oil Pump

Pump records in cc H2O/minute, needs to be converted to mL

mineral oil per minute

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Sample Collection

The volume of sample for 10 seconds was

collected in a graduated cylinder
● Every 10 minutes
● Volume recorded for ten
● seconds of flow
● Refractive index

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Error Sources

Possible Source of error:

The outlet stream did not
flow at a constant rate

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Mineral Oil-Water Interface

Blue Arrow: Entrance to water feed tank

Orange Arrow: Phase interface

Yellow Arrow: Initial phase interface

● Mineral Oil/Water interface line was below

the water intake

● Backflow of mineral oil into water feed tank;

likely source of error

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Conclusion

● Difficult to determine if performance is improved at a slower or faster

feed flow rate from collected data
○ Preliminarily appears trial 1 achieved better purification (faster is
better)
● There are discrepancies between the inlet t-BuOH and the outlet of t-
BuOH due to:
○ Backflow of mineral oil feed in water feed tank
■ Contaminated stagnant water with tBuOH
○ Inconsistencies in feed flow rate (not constant)
○ Accumulation of feed in the column over run time
○ Issues with water RI measurements (contaminated with mineral oil)
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Recommendations

● Ensure that the water-oil interface is above the water inlet pipe

○ Edit the SOP guidelines to have more pictures with this problem

● Clean the water feed tank due to where the interface was located

● Determine a method to check for mineral oil contamination in water

samples

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References

[1] Wesley, Sabrina. “Basic Technology and Tools in Chemical Engineering Field.”
2012, www.overdrive.com/media/793707/libraries.

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Questions?
Procedure - Mineral Oil Pump Calibration

● The mineral oil pump was first calibrated

○ Two marks were made at the bottom of the mineral oil column
○ The mineral oil pump was set to a specific flow rate on the flow
meter
○ The time that it took for the oil to fill from the first to second mark
was recorded
○ The volume of mineral oil that drained from the column was
recorded
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Procedure - Trial Process

● Filled the column to the marked line with water using the water pump
○ The volume was 4052 mL
● Started the mineral oil pump and changed the flow rate to the desired
flow rate (this was t=0 min)
○ First trial used 390 mL/min, second used 220 mL/min
● As soon as the raffinate flowed into the tank, a sample was taken of the
mineral oil and
○ Volume of raffinate in ten seconds
○ Refractive index of mineral oil
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Procedure - Sample Collection/Analysis

● Each sample was taken at 10 minutes after the first raffinate flowed
into the tank
● Water sample was taken right after the mineral oil sample was taken
● The refractive index of the the mineral oil and t-butanol mixture was
measured over time to determine purification amount

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