EXPERIMENT NO.

7
PREPARATION OF POTASSIUM ALUMINUM SULFATE, KAl(SO4)2·12 H2O
(ALUM)
Castil, J.*, Alegre, J. L., Almorado, M. J., Andaya, J., Beluan, A. J.
Bachelor of Science in Chemistry – 1, College of Arts and Sciences, Department of Pure
and Applied Chemistry, Visayas State University, Visca, Baybay City, Leyte, Philippines

Abstract

This experiment was conducted to prepare a “double salt” potassium aluminum

sulphate or alum, study and explain chemical reactions involved in the preparation and
determine the theoretical yield and percent yield in the preparation. Small piece of
aluminium, 50 mL of 1.5 M KOH, 30 mL of 6 M H2SO4, 250-mL beaker, sand paper, wire
gauze, hot plate, stirring rod, tripod, triangle clay, short stem funnel, filter paper, watch
glass and water bath was used in the experiment. The aluminum metal with KOH was
heated to dissolve the aluminum metal, the solution was filtered then was added with
H2SO4 after. To dissolve the precipitates formed the solution was heated, the solution has
been cooled in an ice bath after. A week after crystals formed, the crystals were placed in
the watch glass for air drying. The alum was weighed and the actual yield was 12.18 g, the
actual yield did not match to the theoretical yield which was 17.56 g, because of some error
which include the incomplete or competing reactions and loss of sample during recovery.
The actual yield was smaller than the theoretical yield which implied that the percent yield
was also small that was 69.36%. Though the theoretical yield did not match to the actual
yield still, potassium aluminum sulfate was able to prepare and chemical reactions involved
were able to observed and explained.

Introduction

One goal of chemistry is to be able to transform substances (reactant) to another

substances (product) through chemical reaction, the preparation of alum is a process of one.
Alum refers to potassium alum, which is the hydrated form of potassium aluminum
sulphate and has the chemical formula KAl(SO4)2·12H2O (Helmenstine, 2019). It have a
cubic crystal structure and grow easily from aqueous solution, usually in the form of
octahedral and is colourless (Quevedo, 2019). Alum is prepared through recycling
aluminum metal which also help the environment, during the process of recycling only
around 5% of carbon dioxide is produced (Aliyu & Yauri, 2014). Alum has many practical
uses; it has long been used in paper sizing to improve durability, ink receptivity, in water
treatment, as clarifier for fats and oils and as foaming agent in fire foams (Aliyu & Yauri,
2014). Many tripositive cations yield crystals of the same stoichiometry and structure;
chrome alum KCr(SO4)2·12H2O for example (Quevedo, 2019).

In the preparation of potassium aluminum, chemical reactions have occured and

theoretical (the quantity of a product obtained from the complete conversion of the
limiting reactant in a chemical reaction) and percentage yield (the percent ratio of actual
yield to the theoretical yield) can be acquired which is important to be studied by the
chemistry students.

Experimental Procedure

The method used in this experiment was based on the laboratory manual
“Chemistry 117.1 – Inorganic Chemistry I – Lab” (Quevedo, 2019). The material used in
this experiment were as follows: small piece of aluminium, 50 mL of 1.5 M KOH, 30 mL
of 6 M H2SO4, 250-mL beaker, sand paper, wire gauze, hot plate, stirring rod, tripod,
triangle clay, short stem funnel, filter paper, watch glass and water bath. An aluminum
metal was scraped with sandpaper to removed impurities then was weighed about 1 g. The
scrap was cut into small pieces and was placed in a 250-mL beaker. Using stirring rod, 50
mL of 1.5 M KOH was added carefully and was heated while stirring up to 30 minutes
until the aluminum metal dissolve. As the evolution of gas came to completion the beaker
was then removed from the hot plate. After that, filter the solution using filter paper with
funnel into the beaker. Next, 30-mL of 6M H2SO4 was added while stirring and was heated
again to dissolve the white precipitate. The solution was cooled in an ice bath, keeping it
motionless. An octahedral crystals were formed after a week, the crystals were collected
and was washed with 15 mL 50:50 water-alcohol. Crystals were placed in a watch glass
for air drying. When the crystals were dry it was weighed to determine the mass.
Results and Discussion

The preparation of potassium alum involved chemical reactions. The first chemical
reaction was: 2Al (s) + 2KOH (aq) + 6H2O (l) → 2KAl(OH)4 (aq) + 3H2 (g)
The reaction of aluminum with KOH produced a potassium salt of tetrahydroxoaluminate
complex ion. KOH was a strong base so it readily ionized in water into K+ and OH-.
Furthermore, aluminum was very active metal and readily reacts with water (Wiberg,
2001). The free OH- formed complex with Al forming the tetrahydroxoaluminate ion. This
ion bound with K+ forming salt. The product H2 gas was emitted in the reaction which
caused the unpleasant fumes in the process. The reactivity of Al with water reduced water
to Al(OH)3 and released H2 gas. Therefore the reaction of aluminum metal and water
brought the gas. The chemical reaction above was an example of oxidation-reduction
reaction. The aluminum metal was oxidized to Al+3 and the H atom from KOH or the water
molecules was reduced from +1 oxidation number to 0 oxidation state hydrogen gas. Also,
OH- came in excess in the reaction.

The second reaction was acidification of KAI(OH)4 with 6 M 50:50 H2SO4:

2KAl(OH)4 (aq) + H2SO4 (aq) → 2Al(OH)3 (s) + K2SO4 (aq) + 2H2O (l)
There was an acid-base reaction that occurred. KAI(OH)4 was converted to aluminum
hydrate Al(OH)3 and a salt (K2SO4) plus the water. Al(OH)4- complex was neutralized by
the H+ in the acid and freed Al3+ ions. Excess OH- were also neutralized by the acid to form
water. The neutralization of the complex ion resulted to the formation of a thick gelatinous
substance Al(OH)3. At this point, Al(OH)3 came from two sources: reaction of aluminium
with water and the acid-base reaction with H2SO4. Simultaneously, K2SO4 and Al(OH)3
reacted to form the alum. Al(OH)3 precipitated out in the reaction but redissolve again as
more and more H2SO4 was added. Heating enhanced the dissolution of Al(OH)3 and the
effective crystallization of the alum after. It also aided in the vaporization of some of the
water molecules in the solution to increase better crystallization (McCurdy, Pultz, &
McCormick, 2014). After complete dissolution, cooling of the solution in the water bath
hastened crystallization to observe the formation of the octahedral crystals of the alum
since potassium alum hydrate were soluble in water at room. The crystals were the alum
with dodecahydrate water of hydration (KAl(SO4)2·12H2O). Like any other synthesis,
crystals of potassium alum underwent washing with 50:50 water-alcohol. Potassium alum
had a very limited solubility in ethanol compared to water. This action prevented greater
loss of the alum during filtration. Table 1 represents all the data or masses gathered after
crystallization, filtration, and drying to account for the percent yield of the synthesis of the
alum.

Figure 1. Potassium alum crystal.

Table 1. Data gathered in the preparation of alum.
Mass of clean weighing paper 2.36 g
Mass of weighing paper plus aluminium 3.36 g
Mass of aluminium 1.00 g
Mass of watch glass plus aluminium 43.53 g
Mass of clean watch glass 42.53 g
Mass of alum 12.18 g

The table shows the actual yield of alum which is 3.7095 g. Initially, only 1 g of
aluminium metal was used. Series of chemical reactions took place before the alum was
produced. This stoichiometric relationship was used to account for the theoretical yield of
alum.

Theoretical yield of alum

1 mol Al 1 mol alum 474 g alum

1 g Al x x x = 17.56 g alum
27.0 g Al 1 mol Al 1 mol alum
 By this, theoretically, 17.56 g of alum must be obtained from 1 g aluminum metal.
However, due to the fact that chemical reactions are not always 100% due to transferring
or losses during reaction, the actual yield always came in less amount than expected. Only
12.18 g of alum was created.

Percentage yield alum

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑎𝑙𝑢𝑚 𝑜𝑏𝑡𝑎𝑖𝑛𝑒𝑑 12.18 g alum

= x 100 = 𝟔𝟗. 𝟑𝟔%
𝑡ℎ𝑒𝑜𝑟𝑖𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑 𝑜𝑓 𝑎𝑙𝑢𝑚 17.56 g alum

By the formula, the percent yield was found to be 69.36%. As observed, the actual
yield was a little smaller as compared to theoretical yield. This implied that the percent
yield was small.

Conclusion
At the end of the experiment potassium aluminum sulfate KAl(SO4)2·12
H2O was able to prepared and chemical reactions were observed and explained. Moreover,
theoretical yield and percent yield were determined. The theoretical yield was 17.56 g
which did not match to the actual yield that was 12.18 g because of some error which
include the incomplete or competing reactions and loss of sample during recovery. And as
observed, the actual yield was a little smaller as compared to theoretical yield which
implied that the percent yield was small that was 69.36%.

Acknowledgement

The fulfilment of this activity could not be possible without the help and
participation of many people; their contributions are greatly appreciated. The student
would like to express deepest gratitude to Almighty God, for his guidance, enlightenment
and protection for the completion of this activity. Dr. Elizabeth S. Quevedo for sharing her
knowledge, suggestions, guidance and teachings for the success of this activity. Also, to
the group mates, classmates, dorm mates, for the ideas and participation. Thank you so
much and God bless!
References

Aliyu, M. and Yauri, A. U. 2014. Synthesis and Analysis of Potassium Aluminum Sulphate
(Alum) from Waste Aluminum Can. Kebbi State University of Science and
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https://www.thoughtco.com/definition-of-percent-yield-605899. (accessed on 20
April 2019).
Helmenstine, A. M. (2019, January 17). What is Alum. Retrieved from Thought.Co:
https://www.thoughtco.com/what-is-alum-608508. (accessed on 20 April 2019).
McCurdy, D. L., Pultz, V. M., & McCormick, J. (2014, August 21). Preparation and
Analysis of Alum. Retrieved from Truman State University:
http://chemlab.truman.edu/chemical-principles/chem130labsalum/. (accessed on
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Wiberg, E. (2001). Preaparation of Potassium Alum. Retrieved from Academia.edu:
https://www.academia.edu/10989753/Preparation_of_Potassium_Alum. (accessed
on 20 April 2019).
Quevedo, E. S. 2019. Laboratory Manual in Chem 117.1 – Inorganic Chemistry I Lab.
Baybay, Leyte, Philippines: Department of Pure and Applied Chemistry.