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Laboratory Experiment

pubs.acs.org/jchemeduc

Rapid Production of a Porous Cellulose Acetate Membrane for Water

Filtration using Readily Available Chemicals
Adrian Kaiser, Wendelin J. Stark, and Robert N. Grass*
Institute for Chemical and Bioengineering, ETH Zurich, Vladimir-Prelog-Weg 1, CH-8093 Zurich, Switzerland
*
S Supporting Information

ABSTRACT: A chemistry laboratory experiment using every-

day items and readily available chemicals is described to
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introduce advanced high school students and undergraduate

college students to porous polymer membranes. In a three-step
manufacturing process, a membrane is produced at room tem-
perature. The filtration principle of the membrane is then
illustrated by filtering solutions containing pigmentary water-
Downloaded via 152.58.227.254 on March 26, 2024 at 04:14:17 (UTC).

color or food coloring. A comparison of the filtration results

shows that insoluble watercolor pigments are too large to pass the pores of the membrane and are successfully rejected by the
membrane, whereas the food coloring is completely soluble in water and easily passes the membrane. The laboratory experiment
can be performed in a 2 h activity and serves the purpose of (1) exposing students to a new and interesting field of material science.
It (2) makes them familiar with porous membranes for the production of safe drinking water and (3) introduces them to a template-
removal technique utilizing acid/base theory. There were 52 advanced high school students and 55 high school teachers in
Switzerland who already successfully performed the laboratory experiment and found the activity engaging and motivating.
KEYWORDS: Membranes, Materials Science, Precipitation/Solubility, High School/Introductory Chemistry,
Environmental Chemistry, Laboratory Instruction, Nanotechnology, First-Year Undergraduate/General,
Interdisciplinary/Multidisciplinary, Hands-On Learning/Manipulatives

■ INTRODUCTION
Importance of Safe Drinking Water
Access to safe and clean drinking water is still a global problem.
In developing countries, about 80% of illnesses are linked
to poor water and sanitation conditions.1 Among the most
common health risks of impure drinking water are waterborne
diseases caused by pathogenic bacteria, viruses, and protozoan
parasites. In a comprehensive study, Bain and co-workers
reviewed the microbial quality of drinking water, and estimated
that around 1.8 billion people globally use a source of drinking
water that is contaminated with E. coli or other thermotolerant
coliform (TTC) bacteria.2
Various approaches, with their inherent advantages and
disadvantages, have been studied to remove microorganisms
related to waterborne diseases.3,4 Portable water purification
devices currently in use include systems based on ultra- and
microfiltration membranes, ceramic filters, activated carbon filters,
or chemical disinfection with halogens.5 The drawbacks of the
best performing systems are usually their complex instal-
lation and periodic maintenance, resulting in high operational
costs and thus rendering these systems unsuitable for developing
countries. Additionally, many point-of-use treatment devices are
not effective against all possible contaminants. Therefore, novel
water treatment technologies are currently being investigated.6,7
Water quality issues are an integral part of many high school
chemical courses, and several experiments have been devel-
oped as educational laboratory procedures.8 Water filtration
© 2017 American Chemical Society and
Division of Chemical Education, Inc.
experiments for the removal of nanomaterials have been
previously described,9 and a laboratory experiment comparing
various biochemical separation technologies (including filtra-
tion) has been presented.10 The experiment presented here
differs from previous approaches, as the filtration device itself
(a porous membrane) is fabricated by the students from standard
materials, and then tested for its separation performance.
Microfiltration Membranes
Solutions to improve the sanitary conditions in developing
countries should preferentially be easy to handle, low-cost,
durable, and environmentally sustainable.11 Microfiltration
membrane technology represents an effective alternative to
obtaining safe drinking water due to its high efficiency in
removing microbiological contaminants.4,12 Moreover, the tech-
nology benefits from its ease of operation, relatively low energy
consumption, and high water flux at low operating pressure.13
A procedure for the production of mesoporous micro-
filtration membranes by removing a nanoparticle pore template
was developed by Kellenberger et al.14 In their method,
calcium carbonate nanoparticles were used as pore templates
to fabricate polymeric membranes with tunable pore sizes.
This technique was upscaled to an industrial level and resulted
in the development of the commercially available DrinkPure
Received: October 26, 2016
Revised: February 24, 2017
Published: March 30, 2017
483 DOI: 10.1021/acs.jchemed.6b00776
J. Chem. Educ. 2017, 94, 483−487
Journal of Chemical Education
water filter.15,16 The key part of this water filter is a micro-
filtration membrane that is produced via pore templation using
calcium carbonate nanoparticles. The industrial production of
this membrane is easy and cheap, but it relies heavily on
sophisticated machinery for processes such as ball-milling,
dispersion coating, and solvent evaporation.
Cellulose Acetate Membrane for Water Filtration
In this paper, we describe a laboratory experiment to produce a
drinking water membrane filter that, in its production stages,
resembles the commercially available drinking filter, but is
accomplished using everyday items such as a kitchen blender,
glass plates, rulers, and readily available chemicals. The whole
experiment can be performed in a 2 h laboratory exercise.
The Supporting Information for this article includes a student
handout and instructor notes for the performance of the
experiment in a class (ca. 20−40 students). Production of the
membrane is based on the addition of calcium carbonate to a
solution of cellulose acetate dissolved in acetone. Glycerol is
also added to the reaction mixture and acts as a pore forming
spacer.17 The polymer solution is then mixed using a kitchen
blender, and the resulting dispersion is spread on a glass plate
using a stainless-steel ruler. After evaporation of the solvent in
ambient air, the calcium carbonate particles and glycerol are
washed out of the polymeric matrix in an acid bath and
subsequently rinsed with a water bath (Figure 1).
Figure 1. Production of polymeric membranes using a kitchen
blender. A calcium carbonate particle−polymer dispersion is cast on a
glass support and the solvent evaporated in ambient air. Acid bath
incubation of the membrane dissolves the calcium carbonate particles
and yields a porous membrane.
Functional Testing of Membrane Using Watercolor and
Food Coloring
Students test the performance of the resultant membrane with a
solution of watercolor and food coloring. While, upon mixing
with water, both result in colored water, the used food color
is a water-soluble dye, and the watercolor is a pigmentary disper-
sion, with particles in the size range 40−80 μm. The pigment-
based watercolor solution is first passed through the membrane.
The filtration is then repeated with the food coloring solution.
In both cases the students are asked to record their observations.
The experiments with both solutions are subsequently repeated
with a standard filter for a Buchner funnel.
■
PROCEDURE
Equipment and Chemicals
The experiment utilizes infrastructure and materials available in
a an undergraduate level chemistry laboratory (see Supporting
Information Instructor and Student Notes) as well as some
additions, which can easily be obtained:
• Kitchen blender with at least 800 W power (e.g., Philips
HR 2195/04)
484
Laboratory Experiment
• Mirror or glass plate (148 × 210 mm2 or larger area)
• Scotch tape
• Ruler with stainless-steel cutting edge or aluminum
profile
• Two plastic basins for diluted hydrochloric acid and
water bath
• Cellulose acetate (Sigma-Aldrich No. 180955)
• Calcium carbonate (Sigma-Aldrich No. 21069)
• Watercolor (e.g., Artists Loft Fundamentals Watercolor
Pan Set from amazon.com)
• Food coloring (e.g., Brilliant Blue FCF E133)
Preparation of Cellulose Acetate Polymer Solution
The cellulose acetate polymer solution was prepared by mixing
20 g of cellulose acetate with 200 g of acetone in a 250 mL
Schott flask. A magnet was added to the flask, the flask was
closed (to limit solvent evaporation), and the polymer solution
was stirred over a period of 1 h using a magnetic stirrer.
The mixing of the polymer solution was finished when the
solution became clear.
Preparation of Cellulose Acetate Dispersion
The whole cellulose acetate polymer solution was transferred into
a kitchen blender. Next, 41 g of calcium carbonate and 17.6 g of
glycerol were added, and the suspension was stirred for
3 min at the highest setting of the kitchen blender. The dis-
persion was put into a fresh 250 mL Schott flask and closed to
limit solvent evaporation. The kitchen blender was immediately
filled with water to precipitate the remaining dispersion, and the
polymer waste was disposed into the household refuse.
Production of Membrane Sheet
Two parallel edges of a mirror or glass plate were plastered
with four consecutive layers of Scotch tape, which will define
the thickness of the membrane (Figure 2a). Subsequently, the
Figure 2. (a) Preparation of mirror plate for dispersion-casting,
(b) acid bath incubation of cellulose acetate membrane, and (c) final
product, removed from the washing bath.
surface was rinsed with a towel and small amount of ethanol.
Approximately 10 g of the cellulose−acetate polymer dispersion
was transferred from the Schott flask to a smaller beaker glass
to facilitate the pouring process. This amount of dispersion
was then poured onto the mirror as an ∼1 in. wide stripe.
The stripe of dispersion was then distributed from the top to the
bottom of the glass plate using the edge of a stainless-steel ruler.
The final membrane sheet was dried in ambient air for 5 min.
Removal of Calcium Carbonate Particles
For the removal of the calcium carbonate particles, one plastic
basin was filled with 5 L of water, and another basin was filled
DOI: 10.1021/acs.jchemed.6b00776
J. Chem. Educ. 2017, 94, 483−487
Journal of Chemical Education
Figure 3. Scanning electron microscopy (FEI nova NanoSEM 450, 3 kV, spot size 2.5) images of cellulose acetate membrane cross sections at
various magnifications. Images on the top row show the membrane cross sections prior to removal of the calcium carbonate pore template; images
on the bottom row show the membrane cross sections after the calcium carbonate pore template has been removed.
with 5 L of hydrochloric acid (0.24 M). The mirror plate con-
taining the membrane sheet was then submerged into the hydro-
chloric acid bath (Figure 2b). The membrane sheet loosened
itself from the mirror plate, and gas bubbles indicated the removal
of calcium carbonate particles. After 10 min, the membrane sheet
was transferred into the basin containing only water and washed
for another 5 min. Finally, the membrane sheet was pulled out of
the water bath (Figure 2c) and placed onto a kitchen towel.
Another kitchen towel was used to dry the membrane.
Functional Testing of Membrane
A standard filter for a Buchner funnel was placed onto the dried
membrane sheet and the shape of the filter copied using a
permanent marker and then cut out of the membrane. The cut
out membrane was placed cautiously onto a Buchner funnel on
top of a suction flask. A 20 mL portion of a blue watercolor
dispersion was prepared in a small beaker glass and transferred
onto the same membrane. The watercolor solution was filtered
by applying vacuum. Next, a 20 mL portion of an aqueous food
coloring solution was prepared and also filtered by means of the
membrane. The suction flask and Buchner funnel were then
washed, and the two filtration experiments were repeated with a
standard Buchner funnel filter.
■
HAZARDS
Safety goggles must be worn at all times. Nitrile safety gloves
must be worn while working with hydrochloric acid. Hydro-
chloric acid is corrosive. Acetone and ethanol are flammable.
Handle all chemicals employed with care, and in the case of
skin contact, wash immediately with water and soap, and rinse
for at least 15 min. In the case of eye contact, rinse with water
for at least 15 min.
■
RESULTS AND DISCUSSION
The method outlined above usually produced enough material
for the production of 25 membrane sheets, each having the
485
Laboratory Experiment
surface area of about 1/2 page. Removal of the calcium
carbonate particles using hydrochloric acid left behind pores
with a diameter of approximately 1−5 μm as shown in the
scanning electron microscope images (Figure 3). Hydrochloric
acid dissolves the calcium carbonate particles, and carbon
dioxide escapes as gas according to the following chemical
equation:
CaCO3(s) + 2H+(aq)
→ Ca 2 +(aq) + H 2O(aq) + CO2 (g) (1)
Consequently, holes in the membrane are formed, which
have the same size as the calcium carbonate particles. For
achievement of a good particle size (and resulting pore size),
the blending step is important. This step not only is required
for the formation of a homogeneous particle dispersion in the
polymer solution, but also decreases the size of the particles.
The chosen blending time (3 min) ensures a good dispersion,
and a significant decrease in the particle size. Longer blending
times, however, do not result in significantly smaller particles
(and pore sizes) because as the particles get smaller the
shear stress acting on the individual particles decreases as well,
resulting in a minimal achievable particle size (to achieve
smaller particles more energy intensive mixing methods are
required, e.g., ball-milling).
Cross-section images of the membranes (Figure 3b,d,f) show
highly inhomogeneous cavity sizes as well as an asymmetric
membrane morphology: the size of the cavities increases from
the top side of the membrane (air side) to the bottom side
(side facing the glass substrate). This can be explained by the
asymmetry of the drying process, where solvent evaporation
only occurs on one side (the air side) of the membrane
and results in a polymer solubility gradient within the material.
On a similarly produced membrane based on poly(ether sulfone)
(PES), Hess et al. showed that glycerol and the template (in this
instance, zinc oxide nanoparticles) are the key parameters in
DOI: 10.1021/acs.jchemed.6b00776
J. Chem. Educ. 2017, 94, 483−487
Journal of Chemical Education
controlling the pore size and pore gradient along the cross
section of the membrane.17
The performance of the membrane was tested with a filter
setup consisting out of a suction flask and Buchner funnel.
A watercolor dispersion and food coloring solution were
filtered, and both filtration results were compared. Watercolor
paints are pigments (10−100 μm particle size) held together by
a water-soluble binder. The pigments are insoluble, colored
particles and are rejected by the membrane. Food coloring
(e.g., Brilliant Blue FCF E133) is completely soluble in water
and therefore passes through the pores of the membrane.
The pores of standard filter paper used in school laboratories
usually have a wider diameter (>20 μm), and therefore, the
pigments can pass the membrane relatively easily.
This laboratory experiment was performed by 52 advanced
high school students during a 2 h laboratory experiment at a
high school in Winterthur, Switzerland, and by 55 high school
teachers at the “Future of Chemical Education” workshop
during the fall meeting of the Swiss Chemical Society (SCS).
The experiment was performed in two different variants. In one
the cellulose acetate membrane was prepared in advance, and
the filtration experiments were presented as an in-class demon-
stration. The other students and teachers followed the whole
procedure for the fabrication of the cellulose acetate membrane
and produced everything themselves.
The feedback from the students and teachers was very
favorable. From the survey conducted after the laboratory
experiment, it was found that most people liked the hands-on
approach of using readily available chemicals and everyday
items to produce a porous membrane. Many participants
found it attractive that the experiment has a direct link to
the solution of the ever-present problem of producing safe
drinking water. Additionally, many teachers welcomed the
fact that the costs for the experiment are relatively low. For a
class of 25 students the cost for chemicals accounts for approxi-
mately 10 USD.
■
CONCLUSION
In this paper we present a new laboratory experiment that
introduces advanced high school students to the production of
porous membrane materials for water purification. In a three-
step process, membranes are produced at room temperature
and tested with a solution of watercolor and food coloring.
The experiment was initially designed for the “Future of
Chemical Education” workshop during the fall meeting of the
Swiss Chemical Society (SCS). Furthermore, the experiment
was performed with 52 advanced high school students.
Both groups (teachers and students) found the activity
engaging and motivating, because it allowed them to gain
exposure to the modern field of functional materials for the
production of safe drinking water. Production of the membrane
is feasible at a relatively low material cost (10 USD for 25
students). The activity can be performed within 2 h and is also
suitable for first year undergraduate college students.
■
ASSOCIATED CONTENT
*
S Supporting Information
The Supporting Information is available on the ACS
Publications website at DOI: 10.1021/acs.jchemed.6b00776.
Student handout (PDF, DOCX)
Instructor notes (PDF, DOCX)
486
■
Laboratory Experiment
AUTHOR INFORMATION
Corresponding Author
*E-mail: robert.grass@chem.ethz.ch.
ORCID
Robert N. Grass: 0000-0001-6968-0823
Notes
The authors declare no competing financial interest.
■
ACKNOWLEDGMENTS
The authors thank ETH Zurich and the Swiss Federal
Department of Economic Affairs, Education and Research
kindly for their financial support. We gratefully acknowledge
the generous assistance and valuable information provided to us
by Christoph Kellenberger and Michael Loepfe from Novamem
Ltd. Special thanks also to Amadeus Baertsch, Raphael Sigrist,
and Jonas Halter for their tremendous help in reviewing the
manuscript and verifying the school laboratory suitability of the
laboratory experiment.
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487 DOI: 10.1021/acs.jchemed.6b00776

J. Chem. Educ. 2017, 94, 483−487