World Journal of Chemical Education, 2022, Vol. 10, No.

4, 131-136
Available online at http://pubs.sciepub.com/wjce/10/4/2
Published by Science and Education Publishing
DOI:10.12691/wjce-10-4-2

Improvement of Accuracy and Precision during Simple

Distillation of Ethanol-Water Mixtures
Kyeongseok Oh1, Byoung-Un Kang1, Joo-Il Park2,*
1
Department od Chemical and Biological Engineering, Inha Technical College, Incheon, Republic of Korea
2
Department od Chemical & Biological Engineering, Hanbat National University, Daejeon, Republic of Korea
*Corresponding author:

Received September 17, 2022; Revised October 21, 2022; Accepted October 30, 2022
Abstract The simple distillation of ethanol-water mixture is a well-known experimental subject in either general
chemistry laboratory or organic chemistry laboratory. The objective is to provide a reliable guidance for college
students who are major in chemistry or chemical engineering to obtain repeatable results during the simple
distillation of ethanol-water mixture. The liquid-vapor phase diagram of ethanol-water mixtures was introduced
before experiment. As similar to a tradition distillation assembly, Liebig condenser, specific gravity hydrometer set,
and heating mantle were mainly employed to perform the experiment of a simple distillation with minor but critical
changes. The examination of diverse results in distillate amounts and distillate ethanol concentrations were analyzed
by Rayleigh equation. The simple distillation was evaluated at the assigned temperature that was selected from
liquid-vapor phase diagram. Even though the first evaporation started at a temperature below the theoretical bubble
point shown in liquid-vapor phase diagram in most cases, the set temperature was gradually adjusted and maintained
until no more vapor generated. In fact, this work motivates students to design their simple distillation plans through
changing initial ethanol concentration and set temperature. The experimental data from 23 groups suggest that the
accuracy and the precision were dependent upon how to control heating rates and to sustain set temperature in this
work.
Keywords: simple distillation, ethanol-water mixture, liquid-vapor phase diagram, two temperature measurements,
Rayleigh equation
Cite This Article: Kyeongseok Oh, Byoung-Un Kang, and Joo-Il Park, “Improvement of Accuracy and
Precision during Simple Distillation of Ethanol-Water Mixtures.” World Journal of Chemical Education, vol. 10,
no. 4 (2022): 131-136. doi: 10.12691/wjce-10-4-2.

a hydrometer [5], a device working on the principle of

buoyancy. If it exceeds the measurement limit of the
1. Introduction hydrometer, recommended is to use a hydrometer in
different range of measurement. For example, one
The practice of a simple distillation of ethanol-water hydrometer has specified measurement ranges, such as
mixture is often included in freshmen laboratory courses 0.940 to 1.000. The hydrometer measurement has
in chemistry or chemical engineering major [1,2]. The advantages when strong acid or strong alkali solutions are
similar experiment called a simulated distillation was determined. Listed below are considerations that students
performed in petrochemical laboratory for mainly refinery often brought during a simple distillation experiment of
purpose [3,4]. In brief comparison, while a simulated binary ethanol-water mixtures.
distillation uses a temperature program that keeps • Can we determine when a simple distillation ends?
increasing temperatures and collects fractions based on • Is the experiment always predictable?
their boiling points, a simple distillation focuses on a • How to operate the distillation experiment when we
specific collection at a certain temperature, such as change ethanol concentrations?
distillate collection at a bubble point. If a simple In order to response the considerations above, we
distillation proceeds without heating control, the system focused on accuracy and precision of experiment in this
temperature will keep increasing and the characteristic paper. And the phase diagram of ethanol-water mixtures
analysis of distillates would be similar to the analysis in was essentially needed to explain the overall phenomena
simulated distillation. In practice, the simple distillation of of simple distillation [6,7,8]. The objectives are to
ethanol-water mixtures often uses the assigned motivate students to design the simple distillation of
temperatures that were selected between 80~89°C, slightly ethanol-water mixtures by changing ethanol concentration
higher temperature than ethanol boiling point. In a and temperature set by their own plan and to examine the
traditional practice, specific gravity measurement is used results by comparison with their prediction. As
to determine the ethanol concentration of distillates using background skills, students are encouraged to have several
 World Journal of Chemical Education 132

capabilities to measure the mass, density, and specific is performed in a traditional glassware assembly. Figure 1
gravity of a liquid, to convert and calculate the weight and shows the typical assembly of a simple distillation. The
molar ratios of liquids, to assemble distillation parts, and schematic diagram was drawn by ChemSketch software
to interpret liquid-vapor phase diagram. [9]. In many cases, thermometer can be installed in two
different locations. One is placed in near the entrance to a
Liebig condenser and the other case is installed inside the
2. New Protocol liquid in still pot. If one thermometer is placed in the
entrance of Liebig condenser, no significant temperature
2.1. Installation of Two Thermometers increases are observed until vapor starts to generate.
It will be advantageous only if the distillation adapts the
In a laboratory practice, the simple distillation of simulated distillation that requires the continuous heating for
ethanol-water mixtures is often performed in one of first fraction cuts [3,4]. Therefore, it seems to be reasonable
stage of task subjects. A faculty and lab assistant (if when the thermometer placed inside the liquid, which is
available) should examine whether hydrometers work easy to monitor the temperature of liquid mixture in heating
properly. The simple distillation of ethanol-water mixtures process.

Figure 1. Schematic diagrams of a typical simple distillation

Figure 2. Current assembly of ethanol simple distillation in this work

133 World Journal of Chemical Education

In this work, we installed two thermometers in both Evaporation and slow heating harmonizes to reach the
places mentioned above. That is, one thermometer is target temperature for minutes. If the temperature did not
installed in front of inlet of Liebig condenser and the other reach to a target temperature, the control of heating can be
is placed inside the mixture liquid. The current employed applicable through heating application in a short period of
assembly is presented in Figure 2. Here, the temperatures time. The temperature differences between thermometer 1
of liquid mixture and vapor can be comparatively and 2 were recorded by 5 degrees in most cases. As vapor
monitored. The monitoring of two temperatures has been generation becomes slow, the decrease of temperature in
reported elsewhere [10]. Temperature monitoring from thermometer 1 is noticeable. The sudden decrease of
two locations is suggested for quality control as well [11]. temperature in thermometer 1 suggest us the termination
However, a sensor monitoring needs more sophisticated of distillation at a certain temperature. After evaporation
equipment system. It should be noted that this work stops, the weight measurement of distillate is followed by
focused on the utilization of traditional assembly system the determination of specific gravity. The temperature of
with minor modification. distillate is also measured at the same time.

2.2. Distillation at a Bubble Point

3. Results and Discussion
The overall procedure of simple distillation is enlisted
below, when a heating mantle is used. The phenomenon of distillation is simple, and it can be
1) Turn on the power switch of the heating mantle, said that a boiling liquid comes out when the temperature
then turn the analog switch to a position and adjust rises. However, a distillation has the ultimate purpose of
levels during heating. separating one component from liquid mixture. If one
2) After operating the cooling water in Liebig component in binary mixture is separated completely from
condenser to flow, examine whether an ethanol- their initial state, a distillation will be a very useful
water mixture in 2-neck round flask placed on the method. However, one component is not completely
heating mantle starts to boil. separated from one another in ethanol-water binary
3) As evaporation begins, the condensed sample is mixtures. It is general concept that vapor composition is
collected through the cooling tube within Liebig quite different from liquid mixtures in binary system.
condenser. Regarding simple distillation of ethanol-water mixtures,
4) While reading the scale of the thermometer, if the boiling point and liquid-vapor compositions were
necessary, turn the analog switch left and right to published long ago and has been widely used [6,7,8]. In
adjust the temperature of heating mantle. addition, azeotropic concept in ethanol-water system is
5) Keep the liquid mixture in 2-neck round flask at well-known [12]. It refers that the composition in liquid
85°C as best as we operate (in case of ethanol phase and vapor phase are same, which explains the
30% w/w). Here, a set temperature can vary difficulty of distillation method to obtain high purity of
depending upon the ethanol concentrations. ethanol. And, it is also popular concept to use multiple
6) Continue to collect the condensed sample, and distillations in order to produce high purity ethanol instead
when there is no more effluent, stop the experiment of simple distillation [13,14]. These azeotropic and
and turn off the heating mantle. multiple distillations are beyond the scope of this paper
7) After waiting for the heating mantle to cool, and are not discussed in detail here.
dismantle the device For our simple distillation, 400 grams of 30% (w/w)
8) Measure the specific gravity of the distillate and the ethanol-water mixture (126 g of 95% ethanol and 274 g
residues using hydrometers after moved proper of distilled water) were placed in a 1000 mL 2-neck
amount to a 100mL mass cylinder. round flask. The end part of Liebig condenser connected
Apart from monitoring two thermometers shown in a 200mL Erlenmeyer flask using a connecting tube.
Figure 2, the performance of heating mantle is also For better sealing, each joint is secured with joint
critically important. When fast heating was applied, clips made of polymer material. The boiling point of
early evaporation is easy to occur. It may occur because ethanol-water mixtures varies depending on ethanol
the two-neck round flask can be heated up to higher contents. In general, liquid-vapor phase diagram at certain
temperatures than we originally planned for a distillation pressure condition is useful to understand the distillation
schedule. Nevertheless, evaporation also affects to slow process. Liquid-vapor phase diagram of ethanol-water
increase of temperature in overheated liquid mixtures mixtures were presented in Figure 3. The diagram was
during distillation operation. For instance, if the target plotted by the data provided in references [7,8]. The curve
temperature was 85°C in case of 30% w/w (0.144 mole in liquid composition represents the bubble points of
fraction), we can easily detect the evaporation start as low ethanol-water mixtures. And the curve in vapor
as 80°C. As vapor generates, we can also easily detect composition provides the composition of distillate after
temperature increases of thermometer 1. Interestingly, the condensed during simple distillation. In Figure 3, the
temperature increase of mixture was not accelerated capital letters F, D, and R represent the feed, the distillate
when vapor generates because evaporation is endothermic. and the residue, respectively. Initial concentration of
However, evaporation proceeds for approximately 20 ethanol was 30% w/w (0.144 mole fraction). For the
minutes, which helps us to control the slow heating convenience for students, weight percentage was used for
up to 85°C from 80°C by manual adjustment. Manual mixture preparation. However, liquid-vapor phase
adjustment can be successful when turning off heating diagram was presented with respect to mole fraction of
before reaching 1 degree below, here, at 84°C. ethanol in Figure 3.
 World Journal of Chemical Education 134

Figure 3. Experimental procedure for simple distillation

If a distillation starts, we expect the distillation generate. Then, the rapid decrease of temperature is
temperature would be near 85°C and ethanol concentration observed when no vapor generates from liquid mixture.
of distillate would be 70% w/w (0.475 mole fraction). Meanwhile, temperature of thermometer 2 kept increasing
However, the evaporation easily started at the temperature until vapor starts to come out. Once vapor comes out, the
below 85°C, such as 80°C. This may be the effect of fast temperature of liquid stays for minutes and slowly climbs
heating rates that affect to the temperature increase in up to target temperature, here, the temperature at F point
glassware flask in advance. When glassware was carefully in Figure 3. In our case with 30% w/w ethanol-water
heated, the evaporation may begin as close as 85°C. In mixture (0.144 mole fraction), vapor starts to generate at
practice, the temperature of liquid mixture is slow increase 80°C, and stays for minutes and increases slowly up to
during evaporation process. It can be interpreted that 85°C. It should be reminded that the bubble point of 30%
endothermic evaporation regulates the fast heating of w/w of ethanol-water mixture is near 85°C. Here, we need
liquid mixture. The mixture temperature was slowly to operate carefully not to overheat as mentioned above. It
reached to 85°C during evaporation process. The sounds little arbitrary but it could be persuasive as long as
evaporation proceeded for 20 to 30 minutes and then no accuracy and precision are concerned. Without
more vapor generated. The amount and specific gravity of thermometer 1, accuracy and precision of simple
distillate were determined and recorded [15]. distillation could be hardly achieved. In order to examine
Return to Figure 3, the short length of error bars in F the validity of our current simple distillation, Rayleigh
(feed) represents the initially well-prepared ethanol equation was used to examine the distillation process. In
concentration. Other longer error bars in D (distillate) and equation (1) and (2), Rayleigh equations were presented.
R(residue) present the deviation of experimental data form Here, x and y are the ethanol mole fractions in liquid
students. The boiling point of ethanol-water mixture phase and vapor phase in equilibrium state. In our
(0.144 mole fraction) is near 85°C. If this temperature is experiment, since we measured the feed amount (F) and
maintained steadily, the evaporation process will proceed distillate amount (D), the left-hand side of Rayleigh
and vapor concentration would be the concentration at D equation became constant.
point (0.475 mole fraction). The longer error bars in D is
W final dW x dx
not statistically represented but conceptually presented
∫Winitial = ∫ final (1)
W xinitial y − x
that the results were occurred in certain deviation. After
distillation is over, the specific gravity of the collected
R x dx
distillate was determined by the hydrometer (0.82-0.88). ln   = ∫ final (2)
The specific gravity data of distillates were converted to  F  xinitial y − x
the ethanol concentration. If thermometer 2 works
The right-hand side of Rayleigh equation is often
properly, the question will be raised why we still need
calculated by integration of experimental data. In general,
thermometer 1. Someone will claim that we may need one
a simple distillation in temperature ranges of equilibrium
thermometer instead of two thermometers installation. In
state use the average value of (y-x) that is also counted by
our experience, thermometer 1, located near the inlet of
the values shown in Figure 3. The value, 0.331 was used
Liebig condenser, is still important to install because it
in this work. The hypothesis is that current distillation
provides the right time about when evaporation starts and
proceeds in narrow temperature gradients, which assumes
when no more evaporation comes. In brief, the
dx is as small as 0.1 or less. The experimental data and
temperature of thermometer 1 rises when vapor starts to
calculated data from 23 groups were presented in Table 1.
come out and stays at a certain temperature (slightly lower
The subscripts 1, 2 represent ethanol and water,
temperature than bubble point) until no more vapor
respectively. Equations were represented by mole fraction,
135 World Journal of Chemical Education

xi. The values of dx were at the ranges between 0.037 and distillate amount and mole fraction as expected. As the
0.086. The value of dx is dependent upon the temperature distillate amount is becoming less, ethanol concentration
control at near the bubble point. This suggest that the will be higher. The advantages in this work are to help
lower value of dx can be obtained by well-controlled students to choose ethanol concentrations for their future
heating at setting temperature. As reminded, the set experiments, such as 20wt.%, 40wt.%, and so on. If
temperature was 85°C. The overheating may be possible students design their distillation schedules, they can
in a heating mantle and overheating may generate more predict the bubble point and distillate concentration. This
fraction of ethanol-water vapor with less concentration of work suggests that well-control heating can be achieved
ethanol. The bigger in dx value leads the larger amount of by two thermometers monitoring and also improved in the
distillate with less concentration of ethanol in general. prediction of ethanol concentration in distillates even in
In Figure 4, total moles of distillate were presented by the variances of ethanol concentrations and set
mole fraction as well as weight fraction. The data of 23 temperatures. The accuracy and precision will be also
results showed more or less inverse relations between expected.
Table 1. Experimental data of ethanol simple distillation collected from students in 2022
No. F(g) F(mol) D(g) D(mol) D1(w.f.) D1(m.f.) R(g) R1(g) R1(m.f.) R(mol) ln(R/F) (mol/mol) y-x dx
1 400 18.16 103.2 3.29 0.70 0.477 296.8 47.8 0.0698 14.87 -0.200 0.331 -0.066
2 400 18.16 116.1 3.78 0.68 0.454 283.9 41.1 0.0621 14.38 -0.233 0.331 -0.077
3 400 18.16 60.9 1.90 0.72 0.502 339.2 76.2 0.1018 16.27 -0.110 0.331 -0.037
4 400 18.16 79.6 2.46 0.73 0.514 320.4 61.9 0.0857 15.71 -0.145 0.331 -0.048
5 400 18.16 129.3 4.17 0.69 0.466 270.7 30.8 0.0478 14.00 -0.261 0.331 -0.086
6 400 18.16 74.6 2.35 0.71 0.489 325.4 67.0 0.0921 15.81 -0.139 0.331 -0.046
7 400 18.16 76.5 2.36 0.73 0.514 323.5 64.2 0.0883 15.80 -0.139 0.331 -0.046
8 400 18.16 86.6 2.76 0.70 0.477 313.4 59.4 0.0838 15.40 -0.165 0.331 -0.055
9 400 18.16 86.4 2.76 0.70 0.477 313.6 59.5 0.0840 15.41 -0.165 0.331 -0.054
10 400 18.16 98.7 3.18 0.69 0.466 301.3 51.9 0.0753 14.98 -0.193 0.331 -0.064
11 400 18.16 75.8 2.34 0.73 0.514 324.3 64.7 0.0889 15.83 -0.138 0.331 -0.046
12 400 18.16 117.4 3.74 0.70 0.477 282.6 37.8 0.0570 14.42 -0.231 0.331 -0.076
13 400 18.16 83.3 2.68 0.69 0.466 316.7 62.5 0.0878 15.48 -0.160 0.331 -0.053
14 400 18.16 87.6 2.79 0.70 0.477 312.4 58.7 0.0830 15.37 -0.167 0.331 -0.055
15 400 18.16 73.1 2.28 0.72 0.502 326.9 67.3 0.0922 15.88 -0.134 0.331 -0.044
16 400 18.16 85.5 2.67 0.72 0.502 314.6 58.5 0.0820 15.50 -0.159 0.331 -0.053
17 400 18.16 84.8 2.73 0.69 0.466 315.2 61.5 0.0866 15.43 -0.163 0.331 -0.054
18 400 18.16 85.2 2.75 0.69 0.466 314.8 61.2 0.0863 15.42 -0.164 0.331 -0.054
19 400 18.16 121.1 3.90 0.69 0.466 278.9 36.5 0.0556 14.26 -0.242 0.331 -0.080
20 400 18.16 81.4 2.60 0.70 0.477 318.6 63.0 0.0880 15.57 -0.154 0.331 -0.051
21 400 18.16 126.0 4.06 0.69 0.466 274.0 33.0 0.0509 14.10 -0.253 0.331 -0.084
22 400 18.16 124.7 4.10 0.67 0.443 275.3 36.4 0.0563 14.06 -0.256 0.331 -0.085
23 400 18.16 123.8 3.99 0.69 0.466 276.2 34.6 0.0530 14.17 -0.248 0.331 -0.082
Here, w.f. and m.f. represent weight fraction and mole fraction, respectively. And, subscript 1 represents ethanol.

Figure 4. Total moles of distillate amount according to weight fractions and mole fractions of ethanol
 World Journal of Chemical Education 136

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