ANALYSIS AND CHARACTERIZATION OF ALUM SYNTHESISED FROM WASTE CAN

Abstract.

Alum Potash was synthesized from waste cans and analyzed for its effectiveness in waste water
treatment. The waste can was broken into pieces, and dissolved in 2.5M Potassium hydroxide
followed by the removal of the plastic and color coatings through filtration using Buchner funnel. The
can pieces were later chemically and step wisely converted to alum – a viable double salt. The
synthesized alum was qualitatively and quantitatively analyzed thereafter for the quantity and type
of ions present, coagulation efficiency, acidity/alkalinity were also determined. The synthesized alum
exhibit coagulation property and possesses every other property any alum would possess.

1.0 Introduction

Throughout history and the advancement of Civilization, discovery, development and application of
metals has driven the way people live and how societies are organically shaped (Azom.com, 2012).

Metals, when considered in a broad sense may be divided into two large groups, ferrous and non-
ferrous. Ferrous materials are iron based, and non- ferrous materials have some elements other than
iron as principal constituent. The application of non-ferrous materials in engineering are enormous
this include; corrosion resistance, electrical conduction application, low density and easy to fabricate
(Williams et.al. 2014).

Aluminum has contributed very significantly in this development as a versatile metal. Because of its
unique characteristics, it has substituted much older materials like wood, copper, iron and steel.
Aluminium has achieved this position in spite of the fact that its commercial production began only
towards the end of the 19th century, and thus aluminum was a latecomer to the industry. (Avner,
2000).

Partly to this reasons, the global production of aluminium in 2005 rose to 31.9 million tonnes , and the
world aluminium consumption, which was 45.3Mt in 2006, is estimated to be 59Mt in 2015, 92Mt by
2020, and 120Mt by 2025 ( Menzie et. Al., 2010).

Aluminium is found in combined state in over 270 different minerals (Ugwekar et. al, 2012). The
chief ore being bauxite (Al2O3) requires 780KJ for the production of 1 mole of aluminum (Shakbashir,
2008). This amount is on a high side in terms of energy requirement and on a debt side in terms of
cost for a product that will be eventually be discarded as waste even indiscriminately most of the time.
Another option is to convert the aluminium waste to another aluminum compound
(KAl(SO4)2.12H2O), an important double salt, a process which simultaneously leads to the production
of hydrogen gas.

Alum (as aluminium sulfate is commonly called) is manufactured in a simple two-step process from
aluminium in trihydrate and sulfuric acid according to the following reaction:

2Al(OH)3+3H2SO4 + 8H2O Al2(SO4)3.14H2O ∆H = -156kjmol-1

Alum is one of the major chemical components for the treatment of water which help to reduce
suspended solid particles of the water. It is also used in the pulp and paper industry to control pitch,
prevent foam, and improve the properties of broken, secondary fibers, and the Weija treatment
plant/headwork. About 30% of the treatment cost goes into purchasing of alum thus implying that
alum produced under reliable and cheap technologies can help reduce the unit cost of production.
(Akabzaa, 2004).

Alum is of importance as waterproofing agent and accelerator in concrete, as a clarifier for fats and
oils, foaming agent in fire foams (Kanlayavattanakul, et.al, 2011). It was also used as adjutant to

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increase the efficacy of vaccines as far back as 1920s (Mbow, et.al., 2011: Marrack et.al., 2009).
Alum has also been found to stop bleeding in cases of hemorrhagic cystitis (Christopher et.al., 2009).

However, less emphasis is laid and scanty information is recorded of the synthesis of alum from cheap
and readily available material which can complement the existing waste management process and to
improve the availability and abundance of alum in the various sectors where it is needed. This is what
prompted this study.

Product synthesis studies have shown the justification of such process as the synthesis of alum from
waste especially on a large scale basis (David et. al., 2006) but a common misconception is that
environmental protection and sustainable initiatives must come at the expense of economic
development (El- Haggar, 2007), this is particularly for managing waste. A number of metrics have
been proposed almost a decade ago to make chemists aware of the need to direct research on the
synthesis of chemical product from wastes so that they become less wasteful. David et. al., (2006)
proposed a metric known as effective mass yield, which is defined as the percentage of the mass of
desired product relative to the mass of all non – benign materials used in its synthesis.

mass of Product
Effective mass Yield = x100 ……… (1)
Massof non−benign reagents
Sheldon 1992 also proposed the E-factor metric defined as :

Total Waste(Kg)
E-factor =
Product (Kg)

Curzors et. al,2001. similarly proposed a metric known as :

Total mass used ∈a process∨ process step( Kg)
Mass Intensity =
Mass of product (Kg)
Other metrics developed by Glaxosmithkline both in U.S.A and U.K are

mass of product
Reaction mass efficiency = x 100 ……… (4)
mass of reactant
Molecular weight of desired product
Atom economy = …………… (5)
molecular weights of all the reactants
Wang et.al. , (2011) also described and proposed another concept called real atom economy or
effective atom economy
actual weight of desired product (Kg)
Real atom economy = …………… (6)
total weight of all the reactants(Kg)
2.1 Material and methods

2.1.1 Sample Collection : Aluminum cans of beverages were collected from domestic homes at U.U
drive Ugbor area G.R.A Benin City Nigeria.

2.1.2 Reagents : The following reagents were used in the course of this studies – Distilled water,
KOH, Sulfuric acid, BaCl2, Glycerol, Ethanol, HCl, Isoprene and Ammonia.

2.1.3 Synthesis of alum

The method adopted in the synthesis of alum here is Birni-Yauri, (2014). The can was broken into
smaller pieces. 5.77g of the aluminum was weighed and transferred into 500ml beaker containing
200ml of 2.5M KOH and was placed in a fume cupboard. As the reaction proceeds effervescence

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occurred. During the reaction, the mixture was dark due to the presence of the plastic and color
coatings. The cold black solution formed was filtered using Buchner funnel . The filtrate obtained
was colorless and clear. The filtrate was allowed to cool by placing it gently in a cooling bath of cold
water slowly and gently. 40 ml of 98% Sulfuric acid was measured with measuring cylinder and drop
wisely added to the filtrate. Initially, a thick white gelatinous precipitate was formed , as more acid
was added, the reaction was exothermic and the final solutions containing potassium ions (K +, from
potassium hydroxide), Sulfate ion (SO 4-2 from Sulfuric acid) and Aluminum ion was obtained. The
beaker was left for some times to allow the mixture to cool, as the solution chill solid alum
precipitated out forming alum crystals. Finally, the alum crystal was removed from the solution after
some hours by filtration and washed with a mixture of 20ml aqueous ethanol and 20ml water. This
was placed in filter paper and allowed to dry overnight and then reweighed.

2.2 Qualitative analysis

The following qualitative analyses were carried out on the synthesized alum crystal:

2.2.1 Analysis for potassium ion (K+) in the synthesized alum crystal

Using flame test, the presence of potassium was tested in the synthesized alum, the crystal was held
in flame for 20 seconds until the crystal glows. Potassium was evolved and red flame turned pale
purple.

2.2.2 Analysis for sulfate ion (SO4-2) in the synthesized alum crystal.

Small amount of the pulverized alum crystal was added into a test tube filled halfway with distilled
water and the solution was stirred with a stirring rod until dissolution was complete. Two drops of
aqueous barium chloride (BaCl2) solution was added to the mixture. A white precipitate formed,
which was insoluble in Barium Chloride. This indicate the presence SO 4-2 in the synthesized alum
crystal

2.2.3 Analysis for Aluminum ion (Al3+) in the synthesized alum Crystal

Two drops of diluted 1.4M KOH was added to the dissolved alum solution. Sulfuric acid in drop and
then in excess was also added to the alum solution. A thick white gelatinous precipitate was formed
which was insoluble in drops but soluble in excess sulfuric acid. This indicates the presence of
aluminum ion in the synthesized alum crystal (Birnin – Yurian, 2014).

2.2.4 Melting point of the Synthesized alum crystal

The alum crystal was packed into a melting point capillary tube. The capillary tube was fastened to a
thermometer with a thread. A universal clamp and cork stopper was used to fasten the
thermometer to a ring stand. The bottom of the capillary tube and thermometer was immersed in
the beaker containing paraffin oil which is been heated. The temperature point at which the crystal
melts was recorded.

2.2.5 Acidity/ Alkalinity of the synthesized alum crystal

The pH of the solution was determined with the aid of pH meter (Surgifield SM- pHB4 pH Meter).
2.2.6 Coagulative strength of the synthesized alum in waste water.

Little amount of the alum crystal was dissolved in a waste water. The water was left for 10 minutes
after which the particles settled at the bottom of the container. The waste water was muddy in color
before application of the alum but became clear and colorless after application of the synthesized
alum crystal.

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2.3 Quantitative analysis

The amount of potassium ion (K+) and the sulfate ion (SO 4-2) was determined using flame
photometry and atomic absorption spectroscopy (AAS) respectively.

3. Results and Discussion

Table 1: Qualitative analysis of ions present in the Synthesized alum crystal
Test Observation Inference
Alum solution + White Precipitate SO42-
Aqueous BaCl2 formed, and insoluble Confirmed
Solution (After 20 hours)

Solid Alum Crystal+ heat (10 Red flame turned to K+

minutes) Pale purple flame color Confirmed
Aluminate ion

Solution + H2SO4(aq) Thick, white gelatinous Al3+

in drop and in precipitate formed Confirmed
Excess insoluble in drop but
soluble in excess

Table 1 presents the qualitative analysis of the synthesized alum crystal. The aluminum, Potassium
and sulfate ions were positively tested as expected. This is an indication that the synthesized alum
crystal possesses all necessary chemical properties expected of any alum crystal.

Table 2: Quantitative analysis of the synthesized alum crystal.

Ions Quantity Methods

(gram)
Potassium 12594.82 AAS
ions (K+) Spectroscopy
Sulfate Ions 40.135 Flame
(SO4-2) Photometry

Table 2: presents the quantitative analysis of the synthesized alum crystal to know the quantity of
the various ions of potassium and sulfate.
Atomic spectroscopy was used to determine the quantity of sulfate ion in the crystal while flame
photometry was used for potassium ion. The result of the analysis shows that 12,594.82 ion of
potassium and 40.135 ion of sulfate was found in the synthesized alum. Adejumo et, al., 2016
reported smaller values (K+ - 1524.930 and SO4-2- 16.581). This deviation may be due to the
difference in the source of aluminium used in the synthetic process. The values obtained showed
that the various ions are in considerable quantities in the alum crystal synthesized (Bratby J. (2006).
Table 3: Summary of pH & appearance in waste water before and after coagulation with the
synthesized alum crystal.
Parameters Test tube (Before Coagulation) Test tube (After Coagulation)

Volume of Dirty Water 30ml 30ml

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pH of Muddy Water 10.7 3.5

Appearance in water Muddy Clear and colorless

Solids dissolved (g) 5g 3g

Table 4: Summary of calculated values

Parameters Calculated values

Melting Point 90oC
Mass Of Alum Obtained 50.23g
Number of moles of Aluminum 0.214moles
Theoretical yield of alum 251.08g
Number of moles of alum 0.109moles
Percentage yield of alum 20.01%
Mass Conc (ppm) of SO4 -2 40.135
+
Mass Conc (ppm) of K 12594.82
Table 4 showed the properties of the alum obtained. The melting point is found to be 90 oC. This
method of synthesis was found to be effective because 5.77g of the aluminum was used to produced
52.23g of the alum crystal.

The literature melting point for alum is 92 oC while the melting point of the synthesized alum is 90 oC.
The slight differences might be due to the presence of impurities. This indicates that the synthesized
alum would be equally effective.

Conclusion.

The synthesis of alum from waste cans and aluminium related wastes was effectively achieved.
Making use of these aluminium related wastes makes it possible to rid the environment of such
discarded items, not only that, the constant demands of alum in treating waste water, production of
pulp and paper etc. is being met.

Recommendation for further studies.

1. Determination of Heavy metals in the alum crystal synthesized from waste can.
2. Economic feasibility of the large scale production.

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