Inorganic Porous Material for Remediation

of Texas Environment
Date: 17 October 2018
Deepansh Bhatia*1, Kaicey Pritts
Section 520

Abstract
The efficacy of three adsorbents were measured using spectrophotometry, namely, charcoal,
zeolite, and magnetic zeolite, by calculating the difference in concentration of the solute before
and after the addition of adsorbent. Zeolite was found to be the most effective sequestration agent
to adsorb the model dye Procion Red MX-5B.

Introduction
Polycyclic Aromatic Hydrocarbons (PAHs) are a group of organic compounds that are major
carcinogenic water pollutants.1 To counter the pollutant, an attempt was made to develop
economically viable method to remove PAHs from water. Three sequestration agents were
considered: activated charcoal, zeolite, and magnetic zeolite. Activated charcoal is used in
industries to adsorb pollutants.2 Zeolites, belonging to a class known as Molecular Sieves, are a
cost-effective alternative to charcoal.3 The efficacy of zeolite and non-magnetized zeolite were
compared to that of charcoal by calculating the difference in concentration of the model pollutant
Procion Red MX-5B using spectrophotometry and Beer’s Law before and after reacting with the
adsorbing agents.

Materials and Methods

The zeolites were first synthesized. A volume of 50 mL of 3.0 M NaOH solution was obtained and
placed on a hot plate/stirrer. 3.75 g of sodium aluminate was added to the solution, and the resulting
mixture was heated and stirred. Meanwhile, 50 mL of distilled water was heated, and 2.65 g of

*-Primary author
sodium silicate was added after the water came to a boil. Both solutions were then brought to a
gentle boil, and sodium silicate solution was added to the other one. The resulting solution was
heated at 90°C for 60 minutes. After being allowed to cool, the solution was centrifuged and
decanted. Then deionized water was added to the tubes and the solution was centrifuged again.
The zeolite had settled at bottom and was then removed.

A similar procedure was adopted for the preparation of magnetized zeolite. After heating the
solution for 60 minutes at 90°C, 0.78 g of FeCl3 and 0.39 g of FeSO4  7H2O was added. Rest of
the procedure was the same.

To measure the absorptivity constant of the model dye, four clean cuvettes were obtained and one
of them was filled with deionized water, which was then labelled as a blank solution. Another was
filled with 0.05 mM red dye solution. Then, using a 5 mL serological pipet and a 10 mL volumetric
flask, three successive dilutions were performed, yielding three solutions of 50%, 25%, and 12.5%
concentration of the undiluted solution. The solvent used was deionized water.

Approximately 0.2 g of the three adsorbing agents were obtained. The agents were placed into a
mortar and grinded with a pestle. Their mass was recorded. The contents were transferred to three
vials containing 10 mL the stock solution and allowed to react. The contents of the vials were then
centrifuged for five minutes.

While the solutions were being centrifuged, the absorbance of the prepared solutions using
dilutions were measured. After the spectrophotometer was calibrated, the undiluted sample was
placed inside the device and the spectra was collected. λmax was selected from the wavelength of
495 – 570 nm. At the selected λmax, the absorbance of all four samples was measured. The
centrifuged samples were then filtered out and their absorbances were recorded at λmax.
Results and Discussions

Results

Maximum absorption wavelength = 527.8 nm

Absorbance Spectra
0.8
λmax= 537.8 nm
0.7

0.6
Absorbance

0.5

0.4

0.3

0.2

0.1

0
350 400 450 500 550 600 650 700 750
Wavelength (nm)

Figure 1. Absorbance spectra for undiluted Model Dye Procion Red MX-5B.

Solution Concentration Absorbance @ λmax

Stock solution 5 × 10−3 M 0.685
Dilution 1 (50% conc.) 2.5 × 10−3 M 0.328
Dilution 2 (25% conc.) 1.25 × 10−3 M 0.134
Dilution 3 (12.5% conc.) 6.25 × 10−4 M 0.086

Table 1. The concentrations and absorbances of the three solutions prepared with successive dilutions and
the undiluted sample.
Regression line equation: y = 140.3x – 0.0206
R2 value: 0.9962
⸫ Molar absorptivity = 140.3 L mol-1 cm-1

Absorbance vs Concentration
0.8

0.7
y = 140.3x - 0.0206
R² = 0.9962
0.6
Absorbance @ λmax

0.5

0.4

0.3

0.2

0.1

0
0 0.001 0.002 0.003 0.004 0.005 0.006
Concentration (mol/L)

Figure 2. Plot of absorbance vs. concentration for the three solutions prepared with successive dilutions
and the undiluted sample.

Concentration of stock solution = 5.03 × 10−3 M

Moles adsorbed
Absorbance of Concentration
Adsorbing agent Mass added per gram of
solution of solution
agent
Activated
0.2179 g 0.362 2.73 × 10−3 M 1.05 × 10−4 mol/g
charcoal
Zeolite 0.2116 g 0.240 1.86 × 10−3 M 1.50 × 10−4 mol/g

Magnetic zeolite 0.2170 g 0.612 4.51 × 10−3 M 2.39 × 10−5 mol/g

Table 2. Various properties of the samples of model dye for three different sequestration agents.
Discussion
Some parameters through which we can compare zeolites and charcoal are efficiency, cost, and
mass-producibility. In the experiment, the efficiencies of the sequestration agents were compared.

Zeolite was shown to have the best efficacy out of all sequestration agents, followed by activated
charcoal and magnetic zeolite as the least effective method to remove the model dye Procion Red
MX-5B. Zeolite removed 41.8% more pollutant per gram than activated charcoal, making it an
excellent adsorbing agent, as the porous molecular structure of zeolite lets it adsorb materials
readily. Zeolite is also cost-effective to produce. The salts used to prepare zeolites are readily
available, thereby making it mass producible.4

Zeolites, with their microporous aluminosilicate structures, more effectively adsorb model dye
because of larger surface area as compared to activated charcoal. Since neither the model dye nor
PAHs are magnetic, magnetic zeolite is ineffective at adsorbing the pollutants.

It is important to note the model dye Procion Red MX-5B used has dissimilar structure to
Polycyclic Aromatic Hydrocarbons as shown below. The structure is much larger and has more
branches than PAH. As such, the model dye is harder to be adsorbed through intercalation for
zeolites since it is harder for the molecules to be inserted in the pores, which makes zeolites less
effective at adsorbing model dye.

(a.) (b.)

Figure 3. Structures of (a.) Procion Red MX-5B and (b.) Benzo (a) Pyrene
There are several sources of error for this experiment, including but not limited to improper
measurements while preparing the solutions, foreign particles and impurities entering the solutions
and affecting the absorbance values, unclean cuvettes affecting absorbance, et cetera. The errors
could also include manufacturing errors, like the volumetric flasks having inexact measurements
or spectrophotometer recording inexact absorbance. All of these affects the quality of data and
could yield incorrect results to some extent.

Conclusion
Through this experiment, an attempt was made to develop an economically viable method to
remove PAHs from water sources. The three sequestration agents considered were activated
charcoal, zeolite, and magnetic zeolite. It was found that zeolite was the most effective at removing
model dye. Considering zeolites are economically viable to produce, the desired results were
achieved.

References
1. Manoli, E. & Samara, C. (2009). Polycyclic aromatic hydrocarbons in natural waters: sources,
occurrence and analysis. TrAC Trends in analytical Chemistry, 18(6), 417-428. Retrieved from URL:
https://www.sciencedirect.com/science/article/pii/S0165993699001119.
2. Ryan Bethel & Edward Lee (Eds.). (2018). Laboratory Manual Chemistry 111/112 (8). 2018.
3. Shaobin, W. & Peng, Y. (2010). Natural zeolites as effective adsorbents in water and wastewater
treatment. Chemical Engineering Journal, 156(1), 11-24. Retrieved from URL:
https://www.sciencedirect.com/science/article/pii/S1385894709007219.
4. Virta, R. L. (1997). Zeolites. U.S. Geological Survey. Retrieved from URL:
https://minerals.usgs.gov/minerals/pubs/commodity/zeolites/zeomyb97.pdf.