education for chemical engineers 1 2 ( 2 0 1 5 ) 2026

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Education for Chemical Engineers

journal homepage: www.elsevier.com/locate/ece

Short communication

A homogeneous chemical reactor analysis and

design laboratory: The reaction kinetics of dye
and bleach

Jason C. Ganley
Department of Chemical and Biological Engineering, Colorado School of Mines, 1613 Illinois Street, Golden, CO, USA

a r t i c l e i n f o a b s t r a c t

Article history: An experimental module for senior-level reaction engineering/reactor design students is
Received 4 April 2015 described. The module is used to characterize the kinetics of dye (food coloring) neutral-
Received in revised form 28 May ization by household bleach, and the reactor system is congurable for use in either batch
2015 reactor or continuous-stirred tank reactor (CSTR) modes. The reactor temperature, volume,
Accepted 22 June 2015 reactant feed rates, and reactant concentrations may be adjusted to enable students to
Available online 2 July 2015 obtain a wide range of kinetic data. Dye concentrations in the reactor are monitored by
absorbance spectroscopy, and the kinetic rate law is determined directly from the batch
Keywords: reactor performance data. Students use the completed kinetic rate law to compare exper-
Reaction kinetics imental steady-state CSTR performance data to the mathematical models derived from
Batch reactor reactor design equations. Finally, the students use the kinetic behavior of the system to
CSTR design a hypothetical plug-ow reactor for the same chemical reaction and a set of stated
Reaction engineering operational goals.
Reactor design 2015 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

1. Introduction interested in adding a low-cost, and easily maintained, mod-

In recent years, the teaching faculty of the Chemical and Bio-
logical Engineering (CBE) department at the Colorado School
of Mines (CSM) have endeavored to make a greater number of
high quality, hands-on experiments available to undergrad-
uate students enrolled in senior-level courses. The delivery
of such laboratory modules are not always required along-
side the lecture material normally covered in such courses,
but the incorporation of a closely associated experimental
project enhances the content in such a way that positive feed-
back is generated from both the students (who enjoy seeing
instructional principles in action) and by those involved in the
departments internal and external accreditation reviews. The
reaction kinetics experiment described here may serve as a
useful example for chemical engineering departments that are
ular experiment to accompany undergraduate reactor design
lectures.
One of the rst published examples involving colorimet-
ric methods for determining the kinetics of dye oxidation was
the reaction of aqueous solutions of crystal violet and sodium
hydroxide (Corsaro, 1964). The reaction of chemical dyes with
commercial bleach to form colorless products (neutralizing or
altering the dyes normal color) involves common household
materials without any exceptional restrictions on handling or
disposal. The fact that the reaction may occur visibly in an
aqueous solution for a variety of dyes and food colorings has
made it a very popular example for the instructors of chem-
istry and chemical engineering (Pickering and Heiler, 1987;
Arce et al., 1998; Henary and Russell, 2007; Kalmatsky, 2013).
Nearly every embodiment of the dye/bleach experiment, even

Tel.: +1 303 384 2163.
E-mail address: jganley@mines.edu
http://dx.doi.org/10.1016/j.ece.2015.06.005
1749-7728/ 2015 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
 education for chemical engineers 1 2 ( 2 0 1 5 ) 2026
those developed for chemical engineering students, involves
simple batch reaction rather than reaction within a contin-
uous reactor with feed and exit ows. One reason for this
limitation is the difculty in measuring dye or bleach con-
centrations (and thus reaction extent) in owing streams,
or within agitated reactors that have continuous reactant
entrance and product exit ow streams.
Dye concentrations in the reaction solutions are con-
veniently measured by monitoring the absorption of the
appropriate wavelengths of light passing through the solution
both before and during reaction. For example, aqueous solu-
tions of the food coloring FD&C Blue #1 (erioglaucine) absorbs
visible light most strongly at about 628 nm. The absorption
(or transmission) of this red-orange light through solutions
of Blue #1 is typically measured using commercial visible
light spectrophotometers, which are generally intended for
use with samples contained in a glass or plastic cuvette.
Further, optical scanning of the sample is typically carried
out in a chamber that is shielded from external light. Light
absorbance or transmittance may also be measured with a
laser/photodiode combination for the wavelength of interest
(Delgado et al., 1998), however this type of system introduces
a potential hazard (laser radiation) and requires signal calibra-
tion, manipulation, and translation for the photodiode/media
interface selected for data acquisition and recording.
In the present communication, a method for arranging a
combination of inexpensive benchtop devices for measuring
dye concentrations in batch and ow reactors is described.
The model reactor designs are created for use with a visible
light spectrophotometer, a ber optic probe, and an electronic
data logger. Students are provided with a choice of two food
coloring dyes: FD&C Blue #1 (peak absorbance 628 nm) and
FD&C Red #40 (peak absorbance 502 nm) for the experiment.
2. Experimental apparatus and operation
methods
All dye and bleach solutions are prepared by laboratory teach-
ing assistants prior to the start of student section laboratory
sessions. The dye solutions are prepared from powdered dye
sources (SigmaAldrich) and tap water. The bleach used is
a concentrated commercial grade solution (Clorox Company;
8.25 wt% NaOCl), which is used both directly and in dilutions
with tap water as required for the creation of reactor feed
solutions.
The specic design features of the experimental appara-
tus for each reactor type (batch and CSTR) were developed
over the course of three semesters of student use, leading to
the nal (unied) apparatus described here. A schematic illus-
trating the combined batch reactor/CSTR vessel is shown in
Fig. 1.
The reactor body consists of a square berglass-reinforced
plastic (FRP) tube section, closed at one end (the reactor bot-
tom) by edge-joining a square aluminum (alloy 5052) plate
with a two-part, waterproof epoxy adhesive (J-B Weld Com-
pany; JB-KWIK). Both the aluminum plate and FRP tube have
edge lengths of 7.62 cm. The FRP tube section is approximately
20 cm in length, with a wall thickness of 6 mm. This cre-
ates a maximum functional reactor volume of approximately
750 mL. The aluminum plate has an approximate thickness of
3 mm. Aluminum alloy 5052 was chosen for its high thermal
conductivity and for its generally high resistance to corrosion
by bleach solutions.
21
The reactor was used above a heating/cooling plate and a
magnetic stirring assembly. The heating/cooling plate consists
of an aluminum (alloy 1100) base with an integrated copper
uid tube. The plate is approximately 13 mm in thickness,
and is supplied with water from a circulating heater/chiller
with digital temperature control. The reactors are agitated
with a Teon -sheathed magnetic stir bar 5 cm in length.
Agitation of the solution within the reactor assists in main-
taining the temperature of the reactor contents (the FRP is
an excellent thermal insulator), and also generates sufcient
solution blending to maintain well-mixed conditions in the
case of CSTR operation. The square cross section of the FRP
tube simplies the placement and gasket sealing of the tubing
and optical ports, and also enables enhanced mixing versus a
cylindrical geometry; the sharp corners naturally bafe the
stirred reactor (Meyers et al., 2002), mixing the contents while
reducing vortex formation in comparison to a cylindrical tank
without bafing (Kresta et al., 2006).
A total of ve ports exist in the reactors sidewalls. Two
of these are tubing connections for the dye and bleach feed
solutions, located above the free liquid surface. The plastic
feed lines connected to both of the feed ports each include a
small (ca. 40 cm) upstream segment, designed with stainless
steel tubing and compression ttings as a double-pipe heat
exchanger. This segment also shares a uid connection to the
circulating heater/chiller which enables simultaneous control
of the reactor and feed temperatures. Two aligned ports near
the bottom of the reactor sides are tted with watertight brass
glass sights. These sights serve as the mounting points for
ber optic connections from both the halogen light source
(Dolan-Jenner Industries; Fiber-Lite MI-152) and the ber optic
detector probe (Vernier Software & Technology; SVIS-FIBER).
The nal port, centered near the bottom of the front side of
the reactor, serves as the drain tubing connection. This drain
connection includes an isolation valve attached to a segment
of exible plastic tubing. The end of the exible drain tubing
may be xed at various elevations with a ring stand clamp,
enabling hydrostatic control of the reactor volume. Feed and
drain connections are only used during CSTR operation, and
the illumination and detection ports are used for every experi-
mental run. Solution absorbance is measured by incorporating
the ber optic probe into the detection port of the miniature
spectrophotometer (Vernier Software & Technology; SVIS-PL).
All absorbance data is collected and recorded with a hand-held
electronic logger (Vernier Software & Technology; LABQ2).
2.1. Batch reactor operation
When testing the reactor in batch mode, students rst ll
the reactor partway with tap water, covering the glass sights
within. The spectrophotometer is set to monitor absorbance
at the wavelength of interest (628 nm or 502 nm), and the
intensity of the light source is manually adjusted so that the
absorbance reported on the logger display is very nearly zero.
This value is recorded as the dye-free absorbance reference,
representing the absorbance of water and the ber optic detec-
tion cable at the selected wavelength. At this point, students
may add a small dose of commercial bleach solution to the
water in order to observe that there is no absorbance caused
by the bleach itself. The reactor is then drained.
Dye solutions are made available to the students at pre-
mixed concentrations (26 M for FD&C Blue #1, and 2060 M
for FD&C Red #40) in insulated 18 L dispensers. Typically, two
different dye solution concentrations are available for each dye
22 education for chemical engineers 1 2 ( 2 0 1 5 ) 2026
Fig. 1 Isometric (left) and front-view (right) schematics of the reactor vessel used for both batch reaction and CSTR
operation: FRP housing (a), dye feed port (b), bleach feed port (c), light source port (d), ber optic detector port (e), drain
connection (f), and aluminum alloy base (g).
color in a given lab session. The dye dispensers labeled with
the dye concentrations within, and are cooled or heated with
immersed coiled copper tubing connected to the circulating
heater/chiller. Sufcient (500 mL) dye solution is measured
by graduated cylinder and added to the empty reactor vessel.
Students once again record the measured absorbance at the
wavelength of interest, which represents the absorptivity of
the solution and optical system at full dye strength.
The students then begin agitation of the solution with
the magnetic stirrer, and start the time-based acquisition
of absorbance data. A pre-measured dose of concentrated
commercial bleach (8.25 wt% NaOCl, specic gravity = 1.09) of
between 2 and 8 g is then added to the solution. This small
dose of bleach does not signicantly impact the temperature
of the solution, but its volume is used to determine the total
solution volume within the reactor vessel. As the dye and
bleach react, students observe a gradual reduction in solution
absorbance, which is plotted in real time on the data logger
display. Reactor temperature is continuously monitored with
an immersion thermocouple. When the absorbance has nearly
returned to its dye-free value, the data logging is manually
halted, and the data is saved. After draining the reactor once
again, students carry out further trials using various combina-
tions of the other available bleach doses and the dye solution
of alternate concentration. Between six and eight batch reac-
tor trials are typically accomplished in about an hours time.
The number of completed trials depends both on when stu-
dents decide to terminate data collection, and on the reaction
rate as inuenced by the reactors temperature. Fig. 2 illus-
trates the raw data from three batch reactor experiments with
identical initial reactant concentrations and differing reactor
temperatures.
2.2. CSTR operation
Operation of the reactor in CSTR mode involves the use of
additional laboratory equipment and slightly alters the gen-
eral experimental technique. As in the case for batch reactor
operation, students use tap water to adjust the illumination
intensity and to determine and record the absorbance of dye-
free water. Once the tap water is drained from the reactor,
exactly 300 mL of dye solution with double the typical concen-
tration ranges as in the batch reactor experiments (412 M for
FD&C Blue #1, and 40120 M for FD&C Red #40) is added to the
reactor, and the absorbance for full-strength dye is recorded.
Students measure the solution depth at this point as well, so
that the volume of reactor internals (ttings, stir bar) may be
calculated using Archimedes method. Magnetic stirring is ini-
tiated, time-based data acquisition commences, and exactly
300 mL of a pre-mixed bleach solution (between 10 and 40 mM
in NaOCl) is added to the dye solution.
At this time, two diaphragm feed pumps (ChemTech,
Pulsafeeder) are switched on to deliver dye and bleach solu-
tions continuously to the reactor. The pumping rates of dye
and bleach solutions are independently adjustable up to
80 mL min1 , although in practice these rates are kept identi-
cal during laboratory experiments in order to best match over
time the initial state of equal parts dye and bleach solutions
within the reactor. The reactor drain is opened, and the exible
drain tubing is suspended at a xed height with a ring stand
clamp. The reactor is gravity (siphon) drained, so a higher
drain tubing exit leads to a larger steady-state reactor volume
and a longer solution residence time. Liquid level is measured
with a thin stainless steel rule, and the reactor temperature is
measured with an immersion thermocouple as before. When
the reactor contents reach a steady-state conversion, as indi-
cated by an unchanging absorption reading, students simply
change the vertical position of the drain tubing to achieve a
new reactor volume and associated solution residence time.
Alternatively, students may adjust the feed ows for dye and
bleach solution to new (identical) rates without adjusting the
elevation of the drain tubing. Between four and six CSTR tri-
als are typically accomplished in about an hours time; mostly
depending on the magnitude of changes to the reactor volume
or feed ows from one experimental trial to the next. Fig. 3
illustrates the raw data from a typical 1-h CSTR experiment;
 education for chemical engineers 1 2 ( 2 0 1 5 ) 2026 23

Fig. 2 Raw batch reactor absorbance data at () 12.0 C, () 25.4 C, and () 38.1 C. For each trial, dye is FD&C Blue #1,
reactor volume is 500 mL, initial dye concentration is 3 M, bleach dose is 4 g.

both a reactor volume change as well as a reactant feed ow by the students in characterizing the reactor, as well as how
rate change are sequentially examined in this particular case. the experimentally determined reaction kinetic information
is used for further reactor design.

3. Data analysis methods and reactor

characterization 3.1. Batch reactor

Students perform the batch reactor and CSTR experiments in
laboratory sessions taking place over the course of 2 h. Each
group spends equal time operating the reactor in the batch
and CSTR modes. The following subsections describe the basic
background theory and the methods of data analysis used
Experiments involving the batch reactor conguration are
designed to allow the students to elucidate the overall
dye/bleach reaction kinetics, including the temperature-
dependence of the reaction. The rate law which describes the
rate of the disappearance of dye (rD ) is presented with four

Fig. 3 Raw CSTR absorbance data for three sequential trials using FD&C Blue #1. Dye feed concentration is 12 M, bleach
feed concentration is 20 mM, reactor temperature is 23.5 C. Vertical dashed lines indicate the operating regions: 600 mL
reactor volume and 78.4 mL min1 total feed rate (a), 350 mL reactor volume and 78.4 mL min1 total feed rate (b), and 350 mL
reactor volume and 27.4 mL min1 total feed rate (c).
24 education for chemical engineers 1 2 ( 2 0 1 5 ) 2026
Table 1 Summary of rate law parameters as dened in
Eq. (1) for FD&C Blue #1 and FD&C Red #40 as
determined from collectively analyzed experimental
batch reactor trials.
Rate law parameter FD&C Blue #1 FD&C Red #40
A (M1 s1 ) 1.50E6 7.91E4 6.82E7 6.21E6
EA (kJ mol1 ) 37.37 1.72 40.41 4.36
(dimensionless) 1 1
(dimensionless) 1.02 0.04 0.97 0.07
Notes: Values for were determined as integers from graphical com-
parison of integrated rate law plots. Values for were determined
by comparing apparent rate constants across trials with bleach con-
centration changes (method details appear in Section 3.1).
parameters that are each to be determined from the analysis
of experimental data: the Arrhenius frequency factor (A), the
reaction activation energy (EA ), and the concentration reaction
orders (, ) for dye (D) and bleach (B), respectively.
d[D]
rD = = k[D] [B] = (AeEA /RT )[D] [B] (1)
dt
Here, bracketed terms indicate concentrations of the respec-
tive species, and k represents the reaction rate constant. The
rate parameters appearing in Eq. (1) may be found using
traditional differential or integral rate law analysis of the
changing dye concentration, as related to the dynamic solu-
tion absorbance at the wavelength of interest. These methods
are discussed in sufcient detail elsewhere (Arce et al., 1998;
Delgado et al., 1998), and are not repeated here.
Fig. 4 shows two linearized batch reactor absorbance versus
time data sets obtained at 22.3 C with identical initial dye con-
centrations but with different amounts of bleach added. The
reaction orders with respect to both dye and bleach are easily
obtained ( = 1, = 1). The effects of temperature upon the rate
of reaction are readily examined by using base heater/chiller
and solution storage temperatures of below, above, and near
to room temperature. In practice, students may observe batch
solution temperatures ranging over a span from as low as
6 C to as high as 45 C. Arrhenius plot [T1 vs. ln(k)] analysis
provides a simple means to obtain values for the Arrhenius
frequency factor (A) and the reaction activation energy (EA )
for each dye color. Table 1 below summarizes each set of
four rate law parameters for FD&C Blue #1 and FD&C Red
#40 as determined from numerous combined experimental
trials.
Although all student groups in each laboratory section
perform experimental trials with the heater/chillers set to a
given temperature, all data is summarily shared among all
of the student groups in all sections. In addition to allow-
ing temperature-based examination of the associated reaction
rates, this sharing of information creates a large bank of data
which students may analyze for quality thus enabling them
to (with reported reasoning) accept or reject data sets and
increase the statistical condence in subsequent regression
operations.
3.2. CSTR
The continuous supply and withdrawal of reactants and
reactor products allows students to observe the various
steady-state conditions (per efuent dye concentration) that
may be achieved with the adjustment of feed ows and/or
reactor volume. Dye and bleach solution feed ows may be
adjusted very quickly using the controls on each of the two
feed pumps. To ensure that students do not choose new ow
settings that create conditions for either a very slow reac-
tion (e.g., by greatly limiting bleach feed ow relative to dye
ow) or those requiring absorbance measurement very near
to the lower threshold of the detector (e.g., insufcient dye
feed ow versus bleach solution ow), ows are set to iden-
tical values for all trials. Generally, students varied the feed
ows between 25% and 75% of the maximum pumping rate
(2060 mL min1 ). The exible drain tubing allowed for adjust-
ment of the solution depth, and for student experimental trials
this depth typically varies from a low of about 6 cm (ca. 300 mL)
up to slightly over 15 cm (ca. 750 mL).
The reactions kinetic rate law parameters, as determined
using batch reactor data, allow students to fully construct and
analyze a dynamic material balance on the CSTR. In addition,
the fully solved reactor material balance for dye can allow stu-
dents to predict the steady-state concentration of dye in the
reactor for various feed concentrations and ows. Students
may also simulate reactor behavior for different reactor vol-
umes and species residence times over a range of operating
temperatures. Performing a material balance on the dye (D)
reactant, while assuming perfect reactor mixing (bulk reactor
conditions identical to exit conditions):
d(nD )
= n D,o n D k[D] [B] V (2)
dt
Here, n and n refer to moles and mole ow rates, respectively,
while V represents the steady-state reactor volume. The sub-
script o refers to inlet conditions.
As discussed previously, the bleach concentration is sev-
eral orders of magnitude greater than the dye, and so [B] may
be treated as having a constant value. With this constraint, Eq.
(2) is easily analyzed by the students as a rst order, linear dif-
ferential equation with constant coefcients. The time-based
concentration model may be used in direct comparison with
transient data such as that shown in Fig. 3.
3.3. Design of plug ow reactor
Experimental data from batch reactor trials is used to gener-
ate a complete kinetic rate law, and this rate data is used to
create a mathematical model for the prediction of CSTR per-
formance. As a nal exercise, students are asked to design
a plug ow reactor (PFR) in which the dye and bleach would
react with no back-mixing or reactant dispersion. Students
are asked to design the PFR to achieve one or more operational
goals. Students may consider a range of reactor variables, such
as reactor volume, conversion, total volumetric ow rate, tem-
perature, and the initial concentrations of each reactant. Some
example design problems include:
Calculation of the minimum PFR volume required to achieve
a specic dye conversion with xed reactant ow rates, tem-
peratures, and feed concentrations.
Determination of the required maximum (dye) or minimum
(bleach) solution feed rate required to achieve a given dye
conversion, with the opposite feed rate xed and all other
reactor conditions (temperature, volume, feed concentra-
tions) known.
 education for chemical engineers 1 2 ( 2 0 1 5 ) 2026
Fig. 4 Linearized absorbance plots for batch reactor operation with identical initial FD&C Blue #1 concentrations and
different bleach doses. Reactor volume is 500 mL, initial dye concentration is 3 M. Bleach doses for each trial are () 3 g and
() 6 g. The apparent reaction rate constants (k ) are displayed next to each linear t.
Finding the range of reactor dye conversion resulting from
the adjustment of the temperature of one or both reactant
feed streams over a specied range.
The PFR model is developed in a straightforward manner.
Beginning with the differential PFR design equation in terms
of dye (D) and bleach (B) concentration, the constant volume
and reactor conversion (X),
ow (V),
dX
o]
V[D = k[D] [B] (3)
dV
This equation may be easily integrated to obtain an algebraic
formula for the reactor conversion as a function of reactor
volume.
4. Observations of student work and
module feedback
As is the case with most hands-on experimental projects
that also require data analysis and a formal report, students
divide their efforts between hands-on laboratory work and
time spent carrying out computational analyses. Prior to per-
forming the laboratory, students are provided with a detailed
electronic document which includes a basic explanation of the
nature of the experiment, sequential operating instructions
for the illumination/sensor and data acquisition systems, and
a short discussion of the signicance of the collected data for
both batch and CSTR modes of operation. In the execution
of laboratory experiments, the number of procedural ques-
tions and clarications requested by the students is by far the
greatest at the very beginning of the lab. These inquiries are
mostly students ensuring that the plan for carrying out the
lab work is properly understood. Students receive immedi-
ate feedback by seeing the response of each reactor system
in real-time via the data acquisition interface. As a result,
the subsequent experimental trials (or implemented reaction
25
condition changes) are generally carried out with condence.
Teams of students are also observed to be actively assist-
ing other teams within the laboratory session for example,
those teams beginning the lab period with CSTR experiments
advise teams that switch to the CSTR in the middle of the
lab period. This results in a very productive and cooper-
ative environment that does not overstress the laboratory
supervisors.
The laboratory module is executed very near the end of
the semester, and long after the lectures introducing such
chemical reaction engineering topics as rate law determina-
tion, the implementation of reactor design equations, and
the use of numerical methods for reactor simulation. The
overall quality of the resulting student work is very good,
and the students generally do not struggle to discuss the
results of their experimental investigations. The extension
of fully analyzed batch reactor and CSTR data to the design
of a hypothetical PFR is accomplished with similar success.
Senior-level students apply the various writing and repor-
ting techniques used in the junior-level thermodynamics
and unit operations laboratories to produce concise reports
of signicant analytical depth to satisfy the learning objec-
tives and course outcomes that are related to the laboratory
module.
Student feedback regarding the homogeneous kinetics lab-
oratory module has been generally very positive. Student
attitudes and responses toward the module and its deliv-
ery indicated greater student satisfaction as the experimental
hardware and the instructional documentation were each suc-
cessively rened over the three semesters that the experiment
has been in use. Faculty instructors appreciate the exible
application of the reactor units (as either batch reactors or
CSTRs) and the integration of data acquisition into the experi-
ment. From an administrative point of view, the dye and bleach
reactors have received good reviews by offering a low opera-
tional cost.
26 education for chemical engineers 1 2 ( 2 0 1 5 ) 2026
5. Conclusions
While the incorporation of laboratory modules into senior-
level chemical engineering courses is by no means universal,
the faculty in the CBE department at CSM recognize the
benets of providing students with practical, hands-on exper-
iments that demonstrate the concepts learned in the lecture
and literature-study aspects of these courses. The present
communication details an inexpensive, reliable, and safe
experimental system that may be provided to chemical engi-
neering undergraduate students enrolled in kinetics and
reactor design courses. The dye and bleach reaction system is
exible in its operation serving as a batch reactor or as a CSTR
with very little required adjustment between modes. The
laboratory module was well-received by the undergraduate
students, instructional supervisors, and course faculty. Mod-
ule planning and execution ensured that the experimental
trials and any associated data analysis exemplied core reac-
tion engineering principles. Student reporting was expanded
beyond simple data reduction so that students also design a
PFR reaction system to accomplish a stated set of operational
goals.
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