Demonstration

Cite This: J. Chem. Educ. 2019, 96, 518−521 pubs.acs.org/jchemeduc

Demonstration of Composition Changes in a Distillation Column by

Use of Bromophenol Blue Indicator
Sigvart Evjen,*,† Coralie Petit,‡ Mikael Hammer,§ Arne Lindbråthen,§ Gøril Flatberg,§ Sigve Karolius,§
Heinz Presig,§ and Anne Fiksdahl†
†
Department of Chemistry, Norwegian University of Science and Technology, Høgskoleringen 5, 7034 Trondheim, Norway
‡
INSA Rouen-Normandie, 685 Avenue de I’Universitè, 76801 Saint-È tienne-du-Rouvray, France
§
Department of Chemical Engineering, Norwegian University of Science and Technology, Sem Sælands vei 4, 7034 Trondheim,
Norway
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*
S Supporting Information
Downloaded via UNIV DE SANTIAGO DE CHILE on December 26, 2021 at 19:42:18 (UTC).

ABSTRACT: In demonstrations of column distillation for

the general public or in other demonstration settings, the
audience often lacks the equipment or knowledge to access
the distillation process. Distillation of solvents usually gives
colorless solution. By adding bromophenol blue (BPB) to the
distillation of water and ethanol, the authors have developed a
setup sensitive to different ethanol concentrations, allowing
direct visualization of the distillation process. The color in the
distillation column changes from blue to yellow in the
distillation column as ethanol concentration changes.
Bromophenol blue indicator can also be used to quickly and
semiquantitatively determine the ethanol concentration in binary ethanol−water mixtures in laboratory settings.
KEYWORDS: General Public, Demonstrations, Public Understanding/Outreach, Equilibrium, Separation Science,
Testing/Assessment

■ INTRODUCTION
Distillation of liquid mixtures is an important industrial
separation process and a natural part of the laboratory
curriculum for chemical engineers. While simple distillations
can be demonstrated by distilling a liquid out of a colored
solution, fractional distillation cannot as readily be visualized.
In undergraduate courses, the progression of the process and
the influence of different process conditions on the resulting
concentration of the distillate can be examined in great detail
yellow to blue at pH 3.0−4.6 in aqueous solution.4 Out of the
pH indicators, BPB exhibits one of the most visible color
changes, from yellow to blue, improving color change
visualization.
In the following paper, the authors describe a demonstration
setup where BPB indicator is used to visually display the
concentration changes in a distillation column. Our setup has
been used on multiple occasions for both undergraduate
students and for the general public, and it has been a very
popular attraction.

■
by means of advanced scientific methods such as gas
chromatography (GC), specific gravity, refractive indices, or MATERIALS AND DEMONSTRATION
chemical titration.1−3 However, when performing public
The following materials are required for this demonstration:
demonstrations or in class, such methods are not readily
available and direct representation is required. To address the • Deionized water
issue, the authors have developed a setup applying a colored • Ethanol
indicator that is sensitive to differences in ethanol concen- • Bromophenol blue (BPB, CAS no.: 76-59-5)
tration. For the distillation setup, the following items are required:
Indicators are used to observe the state or changes in the
properties of a solution. Different indicators typically are • Multiple tray distillation column, preferable Oldershaw
dichromatic or trichromatic, and the indicator color can be or other types of flat-tray column,
used to determine a variety of properties, such as presence of • Boiler
functional groups in a molecule, pH, or metal content in a • Reflux condenser
solution. pH indicators are widely used both in scientific
laboratories and in schools as an integral part of chemical Received: September 11, 2018
education, primarily for acid−base chemistry. Bromophenol Revised: December 16, 2018
blue (BPB) is a common pH indicator, changing color from Published: January 22, 2019
© 2019 American Chemical Society and
Division of Chemical Education, Inc. 518 DOI: 10.1021/acs.jchemed.8b00736
J. Chem. Educ. 2019, 96, 518−521
Journal of Chemical Education
• Hot plate/heating elements
• Septum
This demonstration is best suited for events where it is
possible to start up the demonstration before the event.
Providing sufficient heat to produce distillate can take between
10 and 30 min depending on the amount of liquid, effect of
heating elements, and number of column trays.
A schematic of the demonstration equipment is shown in
Figure 1. For this setup, a boiler with an injection port on top
Figure 1. Schematic of a small scale distillation setup: (1) boiler, (2)
distillation column, (3) condenser, (4) distillate, and (5) inlet for
indicator injection.
of a heater or connected to heating elements is fitted with a
column containing at least five trays. More trays will give better
separation, until an azeotropic mixture is obtained.5 A column
containing horizontal trays, such as an Oldershaw column, is
strongly recommended, as this will give slower leaching of the
indicator during the demonstration. At the top of the column,
there is a reservoir for collecting distillate. The reservoir must
allow the distillate to run back down the column when filled. A
reflux condenser is fitted over the distillate, together with a
septum. Due to the apparatus size, our reflux condenser was
519
Demonstration
below the distillate outlet and distillate was transferred to the
top of the column with a pump, Figure 2. The system operates
Figure 2. Distillation column setup with BPB indicator injected: (1)
boiler; (2) distillation column; (3) condenser; (4) pump; (5)
distillate inlet, from pump; and (6) syringe with indicator solution.
at atmospheric pressure. Additional equipment which can be
used includes a temperature control unit for power supply,
liquid level, and temperature detector for the distillate.
The distillation setup used in our demonstrations consists of
a glass boiler of 4.8 L with four encapsulated 1 kW heating
elements. Power to the heating elements was controlled by a
Normag USG Leistungsteller 3 temperature control unit based
on a Siemens LOGO 25 temperature controller and a PT100
temperature sensor immersed in the boiler liquid. The distillate
reservoir could contain 100 mL. A complete description of the
setup applied in our demonstration is given in Supporting
Information.
Running the Experiment
The reboiler is filled with a 9 vol % ethanol solution and 2 mL
of BPB solution (1 vol % BPB in 96 vol % ethanol) per L of
total solution and boiled until condensation is observed at the
cooler on top of the column. The BPB solution (1 mL, 1 vol %
in 96 vol % ethanol) is added to the top of the column through
the septum. As BPB slowly runs down the column, the color of
the indicator will change from yellow to blue according to the
ethanol concentration at each level, see Figure 2. After a few
minutes, much of the BPB will have leached down to the lower
levels of the column. To maintain the color at the top of the
column, more BPB in ethanol can be added. Because the BPB
is added in solution with ethanol, the total amount of ethanol
will increase as time passes, giving greater ethanol concen-
tration throughout the column. As the ethanol concentration
increases, the color shift from blue to yellow will occur at lower
trays than at the start of the demonstration. Eventually, all
DOI: 10.1021/acs.jchemed.8b00736
J. Chem. Educ. 2019, 96, 518−521
Journal of Chemical Education
levels of the column will be yellow, after roughly 100 min,
using an Oldershaw column with six trays. By removing
distillate (20 mL/L in boiler) and adding the same amount of
deionized water to the boiler, the color gradient was restored.
■ HAZARDS
The main risks associated with this demonstration are the
following: (i) ethanol is a flammable liquid, even in solutions
with water,6 and (ii) the apparatus and heating elements will
be hot during the demonstration. The demonstration setup
should always be kept away from any open flames or ignition
sources. The setup and heating elements should be placed on a
nonflammable surface. Ethanol should be stored separately in a
closed container, away from any heat or ignition sources.
Appropriate firefighting equipment (suitable for ethanol or
liquid hydrocarbon fuels) should be available, and if perform-
ing the demonstration at a public venue, the fire risks and
precautions necessary should be discussed in advance with the
venue manager. During the demonstration, proper protective
equipment including safety glasses and chemically or heat
resistant gloves should be worn. The equipment should be
checked for leakages before demonstration to minimize risks. If
the equipment is not properly fitted with a pressure release
valve or opening to release pressure during experimental start-
up, the glass may break or shatter.
Bromophenol blue is an irritant by exposure to skin, eyes,
inhalation, or ingestion, but it is present in low concentrations
in the apparatus during the demonstration. The demonstrator
should be familiar with the MSDS of ethanol and bromophenol
blue.
■
RESULTS AND DISCUSSION
The color change is induced by changes in the degree of self-
dissociation of the BPB indicator. BPB is a dichromatic
compound, as deprotonation, or dissociation, of BPB gives a
highly conjugated system. Dissociation of BPB is shown in
Figure 3. In pure water, the pKa of BPB is 3.85, and BPB is
Figure 3. Dissociation of BPB, explaining the color change of BPB
solutions with ethanol/water composition.
practically completely dissociated, as the solution is blue.4
However, in ethanol, which has a weaker dipole and does not
stabilize charges as well as water, BPB does not dissociate,
giving a yellow solution.7 The color of BPB solutions will
change with variation in the concentration of ethanol in pure
water, as shown in Figure 4. The demonstration utilizes the
change in dissociation with ethanol concentration to display
how ethanol and water are separated through distillation. The
lower boiling point compound, ethanol, is distilled off first, and
the indicator color becomes increasingly yellow toward the top
of the column. BPB was chosen as an indicator for this
520
Demonstration
Figure 4. Color scale with BPB in ethanol diluted (0−96 vol %) in
deionized water.
demonstration as bromothymol blue (BTB) was found to be
too unreliable. Even small concentrations of ethanol gave
yellow solutions. Other indicators, such as thymol blue (pKa =
1.65) and eriochrome black (pKa = 6.3), did not give a
sufficiently visible color change for ethanol−water mixtures.
Other solvent mixtures, such as methanol−water, could also be
used. However, all such solvent mixtures are more hazardous
than ethanol−water and were discarded.
For safe running of the setup, monitoring of the operations
is required, e.g., on stands. Our demonstration experiment has
been presented for the past two years at our university at a
series of stands, aimed both at the general public and at first
year and undergraduate students. The demonstration is very
popular, and it often gets many visitors, both of whom are
interested in the principles or just the colors. The visual cue of
the colors makes it easier for students to understand the
principles of how distillation works. For younger students, we
suggest simplifying the part concerning the indicators and
focus instead on the concentration change in the column. For
more advanced practices, addition of temperature sensors at
each tray would allow for a second visual aid. Lower
temperatures would be observed upward in the column
because of higher ethanol concentration.
As shown in Figure 4, BPB allows for quick, semiquantitative
assessment of the ethanol concentration in aqueous solution in
the range from 20 to 90 vol % ethanol. In laboratory
experiments or demonstrations, the ethanol content in solution
can quickly be determined by simple addition of 1 drop of
concentrated BPB in 96 vol % ethanol. BPB analysis of binary
ethanol−water mixtures allows both for a visual cue in
demonstration setups, but also for laboratory exercises.
Hence, BPB analysis can readily be applied as a part of all
ethanol−water distillation exercises.
■ CONCLUSION
The described demonstration allows for an easy visual
observation of a distillation process by the use of bromophenol
blue (BPB) indicator. Changes in the equilibrium for the self-
dissociation of BPB in solutions of water and ethanol give a
clear color change from blue to yellow in a distillation column.
The demonstration is easy to perform and can be run for
several hours without interruption. The equipment can be
reused multiple times, and cheap, nontoxic solvents are used.
The demonstration has been very popular among students of
all ages as it is eye-catching, and the audience more readily
understands the principles of distillation. BPB addition to
ethanol−water mixtures allows for quick, semiquantitative
determination of the ethanol concentration.
DOI: 10.1021/acs.jchemed.8b00736
J. Chem. Educ. 2019, 96, 518−521
Journal of Chemical Education

■
Demonstration

ASSOCIATED CONTENT
*
S Supporting Information

The Supporting Information is available on the ACS

Publications website at DOI: 10.1021/acs.jchemed.8b00736.
Notes for instructors (PDF, DOCX)
Video of running experiment (AVI)

■ AUTHOR INFORMATION
Corresponding Author
*E-mail: sigvart.evjen@ntnu.no.
ORCID
Sigvart Evjen: 0000-0003-2662-5861
Anne Fiksdahl: 0000-0003-2577-2421
Notes
The authors declare no competing financial interest.

■ ACKNOWLEDGMENTS
The authors would like to acknowledge the financial support of
the Research Council of Norway, through CLIMIT grant
233776.

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(4) Meites, L. Handbook of Analytical Chemistry, 1st ed.; McGraw-
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(5) Moore, W. J. Physical Chemistry, 3rd ed.; Prentice-Hall: London,
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(6) Ha, D.-M.; Park, S. H.; Lee, S. The Measurement of Flash Point
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(7) Dangui, A. Z.; Santos, V. M. S.; Gomes, B. S.; de Castilho, T. S.;
Nicolini, K. P.; Nicolini, J. Preferential solvation bromophenol blue in
water-alcohol binary mixture. Spectrochim. Acta, Part A 2018, 203,
333−341.

521 DOI: 10.1021/acs.jchemed.8b00736

J. Chem. Educ. 2019, 96, 518−521