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SANDRA IBRAHIM Practicum Report

A. Title : Synthesis of Alum KAl(SO4)2.12H2O


B. Objectives : Understand some of the chemical aspects of Aluminium and alum
production
C. Literature Review

Until the late nineteenth century, aluminum metal was more precious than gold
because no one knew how to purify it in large quantities. In 1886, 22-year-old Charles Martin
Hall (1863–1914) developed a process to produce aluminum by electrolysis.

He used heat from a blacksmith forge, electricity from homemade batteries, and his
mother’s iron skillets as electrodes. At almost the same time, one of Le Châtelier’s students,
Paul L. T. Héroult (1863–1914), also 22 years old, discovered the same process [5].

Aluminum that has a protective coating of aluminum oxide is less reactive than
elemental aluminum. Aluminum forms only tripositive ions. It reacts with hydrochloric acid as
follows:

2Al(s) + 6H+(aq) 2Al3+(aq) + 3H2(g)

Aluminum sulfate [Al2(SO4)3] is sometimes used in municipal water treatment plants to


remove undesirable particles. Explain how this process works.

Another problem with paper made from wood pulp is that it is porous. Tiny holes in the
surface of the paper soak up ink from a printing press, spreading it over a larger area than is
intended. To prevent ink creep, a coating of aluminum sulfate [Al2(SO4)3] and rosin is applied
to some paper to seal the holes. This process, called sizing, results in a smooth surface. You
can readily tell the difference between papers with and without sizing by feeling the surface of
a newspaper and this page. (Or try to write on them with a felt-tip pen.) Aluminum sulfate was
chosen for the treatment because it is colorless and cheap. Because paper without sizing
does not crumble, aluminum sulfate must be responsible for the slow decay [4].

Industri uses :

 Aluminum is the most abundant metal in Earth’s crust. However, it is found in nature
only in compounds and never as the pure metal.
 The most important source of aluminum is the mineral bauxite. Bauxite consists
mostly of hydrated aluminum oxide.
 Recycling aluminum by melting and reusing it is considerably cheaper than producing
new aluminum.
 Aluminum is light, weather-resistant, and easily worked. These properties make
aluminum ideal for use in aircraft, cars, cans, window frames, screens, gutters, wire,
food packaging, hardware, and tools.
[8].

Aluminum, the most abundant metal in the Earth’s crust at 8.23%, takes its name from
alum, KAl(SO4)2·12H2O, a salt that has been used medicinally since Roman times. In spite of

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its abundance, the metal nevertheless proved difficult to isolate in pure form. It was such a
precious substance in the mid-nineteenth century, in fact, that aluminum cutlery was
sometimes used for elegant dinners and the Washington Monument was originally capped by
a pyramid of pure aluminum. Not until 1886 did an economical manufacturing process
become available [7].

The Alum Shale’s kerogen underwent catagenesis in the main petroleum kitchen area
420 to 340 Ma bp. Our calculations suggest the kerogen was much more aliphatic and oil-
prone after deposition than that after extensive exposure to radiation. In addition, the gas
sorption capacity of the organic matter in the Alum Shale can be assumed to have been less
developed during Palaeozoic times, in contrast to results gained by sorption experiments
performed at the present day, for the same reason. The kerogen reconstruction method
developed here precludes overestimations of gas generation and gas retention in the Alum
Shale by taking irradiation exposure into account and can thus significantly mitigate charge
risk when applied in the explorations for both conventional and unconventional
hydrocarbons.

[KAl(SO4)2·12H2O], the Alum Shale Formation is an informal name for Middle


Cambrian, Upper Cambrian (Furongian) and Lower Ordovician (Tremadocian) shale in and
around the Baltic Basin (Andersson, 1985; Thickpenny, 1984). This shale can be as thick as
180 metres in offshore Denmark (Nielsen and Schovsbo, 2006) and 90 metres in southern
Sweden (Pool et al., 2012). The TOC content [1].

Potassium sulfate (K2SO4) is a very important compound, mostly used as nutrient for
plant growth. Potassium sulfate production can be accomplished through the Mannheim pro-
cess. For potassium bearing silicate minerals, such as glauconite, one alternative is acid
leaching followed by selective precipitation and thermal decomposition of potassium alum
(KAl(SO4)2). This chemical process is responsible for the formation of soluble K2SO4 and
insoluble Al2O3, which can be later separated after solubilization in water and filtration. In this
pyrometallurgical reaction, the temperature control is very important. Through the addition of
a reducing agent, the decomposition temperature could be significantly reduced. In the
present work, the thermal behavior of synthetic samples of hydrated potassium alum
(KAl(SO4)2·12H2O) is appreciated through thermogravimetric analysis (TGA), both in the
absence as well as in the presence of a reducing agent (charcoal) under inert atmosphere
(nitrogen) and dynamic analysis. The addition of a stoichiometric amount of the reducing
agent stimulated considerably the decomposition, which started at a lower temperature in
comparison with the pure alum sample. Based on the XRD characterization of selected sam-
ples, it is suggested that the decomposition process should happen in at least two stages,
with Al2(SO4)3as one of the intermediate reagents. After full decomposition, only Al2O3 and
K2SO4 have been identified, as expected based on thermodynamic simulations. Finally, it was
demonstrated that the K2SO4 formed could be totally transferred to aqueous solution after a
solubilization carried out at 363 K for two hours; the remaining solid was characterized as
pure aluminum oxide (Al2O3) [2].

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In this study, the SWI test was used to assess the effect of alum on the swelling
characteristics of highly expansive bentonite clay and the saturation of the clay surfaces with
Al species to improve the phosphorus retention characteristics of clays. The experiments
included varying the pH and alum dosages and measuring the resulting SWI. When alum was
not present, varying the pH was seen to have a profound impact on the swelling
characteristics of the clay. Below pH 2 and above pH 11, the SWI was low because of an
abundance of Hþ at low pH values and an abundance of NaOH at high pH values. Alum was
effective below pH 5 in reducing the SWI from 20 mL/g without alum down to 5 mL/g using
increasing quantities of alum up to 1 g of alum per 2 g of clay in 100 mL of water. Within the
pH range of 5–9, alum was not effective in controlling the SWI. Above pH 11, aluminum
precipitated and the SWI was low [3].

As an inescapable by-product from waterworks, alum and ferric sludge are produced
in the flocculation process where aluminum and iron salt are used as the primary coagulant.
Alum sludge has long been treated as waste for landfill despite the high cost and the lack of
available land for this process[5]. In recent years, the research on alum sludge has attracted
much attention due to its high capability of P adsorption[6,7]. Most studies has focused on the
effects of alum on P-adsorption[8,9], but less work has been done on the effects of alum with
other components, and the forms of phosphorus retained in the sludge. The phosphorus
adsorption capacity of sludge is affected by various factors, such as the nature of the alum
sludge, the characteristics of the raw water, and dosage of coagulation [6,10]. It is necessary
to carry the relationship between the characters of alum sludge and phosphorus adsorption
capacity [4].

Alum [KAl(SO4)2.12H2O] is used in food preparation, dye fixation, and water


purification. To prepare alum, aluminum is reacted with potassium hydroxide and the product
with sulfuric acid. Upon cooling, alum crystallizes from the solution

Aluminum sulfate (cake alum), Al2(SO4)3. Used in purifying water, tanning leather, and
sizing paper; as a fixative for dyeing cloth (see photo); and as an antiperspirant. Aluminum
oxide, Al2O3. Major compound in natural source (bauxite) of Al metal. Used as abrasive in
sandpaper, sanding and cutting tools, and toothpaste. Large crystals with metal ion impurities
often of gemstone quality (see photo). Inert support for chromatography. In fibrous forms,
woven into heatresistant fabrics; also used to strengthen ceramics and metals [6].

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D. Methods
1. Experimental tools and materials
1.1. Tools
No Tools name Tools picture Function Category
1. Beaker glass As the container is aquades 1
(100)

2. measuring cup To measure the volume of 1


cylinder NaOH, H2O, AlCl3, Mg (OH)
2, HCl.

3. A Watch Glass Container for weighing the 1


powder of aluminum powder,
magnesium, Al2O3 and MgO

4. Analytical To measure the weight of 2


Balance aluminum powder, magnesium
powder, Al2O3 and MgO

5.. Spatula To take a solid aluminum 1


powder, magnesium powder,
Al2O3 and MgO

6. Stirring Rod To stir the solution 1

7. Bath To heat the solution 2

8. Mouthipiece To pour the solution so that it 1


does not spiil

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9. Oven As place to dry solution 2

10. Filter paper To filter crystal 1

11. Evaporation dish As a container of solution that 1


will be in the form of crystals

1.2. Material
No Physical
Name Of Material Chemical Properties Material Category
Properties
1. Aquadest (H2O) - Universal - Odorless, General
solvent tasteless
- pH neutral - Boiling point 100
ºC
- Freezing point 0
ºC
2. Potassium - Slightly - Molecular weight: Specific
sulphate (K2SO4) soluble in 174,259 gr / mol
glycerol and - Melting point:
insoluble in 1,069 ºC
acetone, - Boiling point:
alcohol, CS2. 1,689 ºC
- Substances - Solid white matter
that can
irritate
3. Aluminum sulfate - Easy to - Solid form Specific
(Al2(SO4)3) dissolve in hot - Odorless
water - Molecular mass:
- Aluminum 342.14 g / mol
sulfate will be - White
hydrolyzed in
water to form
sulfuric acid
- not soluble in
alcohol

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2. Experimental work scheme

Star

- Dissolve 16.7 gr Al (SO ) 18H O in 12.5 ml water


2 4 3. 2

80 C
o

- Dissolve 4.35 gr K SO in 25 ml of water


2 4

- Mix the two solutions, transfer this mixture to the


evaporation dish
- Cool on room temperature to form crystals
- Considering empty filter paper
- Filtering crystal deposits using filter paper and
buchner funnel
- Drying in an oven at 80 C o

- Weighing filter paper and crystals Kal (SO ) 12H O


4 2. 2

Crystal weight =
10.7939 gram

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E. Result and Discussion


1. Result

No. Treatment Observations


1. Weigh 16,7 gr Al2(SO4)3 and 4,35 gr Both materials in the form of solids (powder) are
K2SO4 white
2. Add 25 ml of distilled water to Soluble material in the form of white solid
Al2(SO4)3 and heated at 800C
3. Add 25 ml of distilled water to Ingredients that are less soluble
K2SO4
4. Mix the two ingredients that have Both solutions mix with white solution
been dissolved with distilled water
on the evaporation cup
5. Shut up until the precipitate forms White deposition
and filter using filter paper
6. Deposits dry the deposits obtained Weght sedimen = (weight of filter paper +
and weigh them sediment ) - (empty filter paper weight)
= 11.6942 gr – 0.9003 gr
= 10.7939 gr

2. Discussion

At this time, namely teaching about the manufacture of alum KAl (SO 4)2.12H2O, aims
to understand some aspects of the chemistry of elemental aluminum and make alum. Alum
who formed a double salt meruapakan comes from two salts, namely K2SO4 and Al2(SO4)3.
H2O. the reaction that occurs is:

K2SO4 + Al(SO4)3 + 24H2O → K2SO4.Al2(SO4)3.24H2O

In this experiment the first step undertaken was to dissolve 16.7 grams of Al2(SO4)3 in
hot water with the temperature of hydrolysis will occur because of 800C, meaning water will
decompose into H+ and OH- so there will be a corresponding hydrates formed with formulae
of laughter. From the observations, Al2(SO4)3.18H2O insoluble perfect be homogeny. The
reaction that occurs is:

Al3+ + 6H2O → Al(H2O)63+

Figure 1.1 dissolve Al2(SO4)3 at a temperature

Next dissolve 4.35 g K2SO4 in plain water, K2SO4 is difficult to dissolve in plain water,
so to do a longer stirring until clear it, a reaction occurs:

K2SO4 + H2O → H2SO4 + H2O

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Figure 1.2 dissolve K2SO4

Then added the second solution in vials of evaporation to crystallize. The reaction that
occurs is:

Al2(SO4)3.18H2O (aq) + K2SO4 (aq) → 2Al(SO4)2.12H2O (s) + 6H2O (aq)

Figure 1.3 mix Al2(SO4)3 and K2SO4

After the dissolving process is complete, the screening process is done, the process
aimed to peyaringan meyaring penganggu ions, and left only a filtratnya. And there is a
sludge that is colored white. The weight of sediment obtained is 11.6942 grams

Picture of a 1.4 screening process Figure 1.5 the weight of sediment

From the observations note that alum can purify water, aluminium formed deposits of
almunium hydroxide. This fits with the theory that alum is very much of its usefulness.

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F. Conclusions

From the experiment results it can be concluded that the warming warming alum
cannot be more than 80oC due to undergo hydrolysis.

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G. Bibliography

Journals

[1] Yang, S., Schulz, H. M., Horsfield, B., Schovsbo, N. H., Noah, M., Panova, E., … Hahne,
K. (2018). On the changing petroleum generation properties of Alum Shale over
geological time caused by uranium irradiation. Geochimica et Cosmochimica Acta, 229,
20–35. https://doi.org/10.1016/j.gca.2018.02.049

[2] Souza, R., Navarro, R., Grillo, A. V., & Brocchi, E. (2018). Potassium alum thermal
decomposition study under non-reductive and reductive conditions. Journal of Materials
Research and Technology, (x x), 1–7. https://doi.org/10.1016/j.jmrt.2018.05.017

[3] Omar, M., Shanableh, A., & Al Zaylaie, M. (2016). Modification of the swelling
characteristics and phosphorus retention of bentonite clay using alum. Soils and
Foundations, 56(5), 861–868. https://doi.org/10.1016/j.sandf.2016.08.010

[4] Hou, Q., Meng, P., Pei, H., Hu, W., & Chen, Y. (2018). Phosphorus adsorption
characteristics of alum sludge: Adsorption capacity and the forms of phosphorus
retained in alum sludge. Materials Letters, 229, 31–35.
https://doi.org/10.1016/j.matlet.2018.06.102

Book

[7]. Actinides, L. (n.d.). No Title.


[4]. Chang, R. (2010). Chemistry 10e. In Chemistry (pp. 1062–1084).
[5]. Malloy, B. C., & Flores, C. (2005). Nteractive Tudent Dition. Teacher (Vol. 86).
Retrieved from http://www.ias.ac.in/currsci/may252004/1355.pdf
[6]. Silberberg, M. S. (2012). The Molecular Nature of Matter and Change.
[8]. Wilcocks, L. P., & Management, I. (1993). About the authors (p. 1980).
https://doi.org/10.1016/B978-0-7506-4821-9.50002-7

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