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Dr. Jose G.

Tamayo Medical University

PREPARATION OF POTASSIUM
ALUM FROM ALUMINUM CANS

Final Coverage
Post-Lab
UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

Learning Objectives:
1. Know the process involved in the preparation of potassium
alum from aluminum cans.
2. Evaluate product preparation qualitatively and quantitatively.
3. Research on the different uses of potassium alum.

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

What is alum?
• An alum is a hydrated double sulfate salt of a monovalent cation
and a trivalent cation. The general formula of alum is:

M+1M+3(SO4)2.12H2O

Where M+1 is commonly Na+1, K+1, Ti+1, NH4+1, or Ag+1

M+3 is commonly Al3+, Fe3+, Cr3+, Ti3+, or Co3+

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

The most common alums:


a) sodium aluminum sulfate dodecahydrate (sodium, alum,
NaAl(SO4)2.12H2O), used in baking powders because upon hydrolysis, an
acid is produced that reacts with the baking soda;
b) potassium aluminum sulfate dodecahydrate (alum or potassium alum,
KAl(SO4)2.12H2O), used in water purification, on sewage treatment, and in
fire extinguishers;
c) ammonium aluminum sulfate dodecahydrate (ammonium alum,
NH4Al(SO4)2.12H2O), used in pickling cucumbers, etc. The various alums
crystallize from solution as octahedrally-shaped crystals that are all
isomorphous, i.e., that all have the same crystal structure.

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

Chemical Equations:

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

Related Video
• Preparation of Alum from Aluminum cans
https://www.youtube.com/watch?v=WAjrjY-JQ3o

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

Schematic Diagram in the Preparation of Alum


10g Aluminum scrap After 10min Al Add H2O to Filter the solution
cut into small pieces scrap will be bring back the while hot
+ dissolved and original volume
500mL KOH Allow solution
the fizzing stops of solution to cool

Acidify w/
9MH2SO4

only if the solid is


present (Al(OH)3) Filter

Dry, weigh the


crystals and filtrate
compute the
% yield Ice bath
Potassium
alum
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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

identification tests:
1. Sodium bitartrate TS and a little ethanol
2. Ammonia TS, a few drops, then in excess
3. Sodium hydroxide TS, a little, then in excess
4. Barium chloride TS. Divide the precipitate obtained in
two portions:
a. One portion, add HCl
b. Second portion, add HNO3

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

Sodium bitartrate test:


KAl(SO4)2•12H2O + NaHC4H4O6 KNaC4H4O6 + Al2(SO4)3 + 12 H2O
Rochelle salt

*Addition of a little ethanol enhanced the pptation of Rochelle salt

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

b. KAl(SO4)2•12H2O + NH3 soluble

c. KAl(SO4)2•12H2O + NaOH soluble

d. KAl(SO4)2•12H2O + BaCl2 BaSO4 + AlCl3 + KCl + 2H2O


1. BaSO4 + HCl insoluble
2. BaSO4 + HNO3 insoluble

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

Questions:
1) What is a “true alum?”
Ans.: True alums crystallize in well-defined octahedral shapes and
are beautifully colored, particularly those containing d – transition
metals. E.g. Potassium alum

2) What are two official alums? Give their uses?


• sodium aluminum sulfate dodecahydrate (sodium, alum,
NaAl(SO4)2.12H2O), used in baking powders because upon
hydrolysis, an acid is produced that reacts with the baking soda;
• potassium aluminum sulfate dodecahydrate (alum or potassium
alum, KAl(SO4)2.12H2O), used in water purification, on sewage
treatment, and in fire extinguishers
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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

Significance of this experiment


• This experiment illustrates a chemical recovery process in
which waste aluminum is converted chemically into an
aluminum compound, hydrated potassium aluminum sulfate,
KAl(SO4) •12H2O, or common alum.
• The experiment illustrated an interesting example of the
reduction of environmental waste.

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

Properties of Alum:
1. Potassium alum is a colorless substance that forms large octahedral or cubic
crystals when potassium sulfate and aluminum sulfate are dissolved together
and the solution is cooled. The solutions of potassium alum are acidic.
2. Potassium alum is soluble in seven times its weight of water at room
temperature and is very soluble in hot water. When crystalline potassium
alum is heated, some of the water of hydration becomes chemically
separated, and the partly dehydrated salt dissolves in this water, so that the
alum appears to melt at about 90°C (about 194°F). When heated to about
200°C (about 392°F), potassium alum swells up, loses all the water and
some sulfur trioxide, and becomes a basic salt called burnt alum. Potassium
alum has a density of 1.725.
3. Other types of alums made with aluminum sulfate include sodium alum,
ammonium alum, and silver alum.

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

Uses:
1. Slightly antiseptic; due to basteriostasis through liberation of
acid on hydrolysis.
2. Used as local styptic; and frequently employed in making
astringent lotions in 0.5 to 5% conc. and douches
3. Styptic pencils are made by fusing Potassium alum with the
addition of potassium nitrate and pouring into suitable mold.
(Caustic pencil contains silver nitrate)
4. Alums are used for flame proofing textiles and in baking
powders, mordants for delicate dyeing operations, and
medicines.
5. Potassium alum is a powerful astringent and deodorant.
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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

Principle involved in its deodorant property:


• potassium alum acts by virtue of interaction with odorous fatty
acids liberated or produced by action of bacteria on lipids in
sweat, and by an action suppressing bacterial growth because
of a decrease in pH.

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

PREPARATION OF CUPRIC SULFATE (CuSO4.5H2O)


Procedure:
1. Add the weighed CuO to the diluted H2SO4 contained in a weighed
250mL Erlenmeyer flask.
2. Place a funnel (not inverted) on the mouth of the flask.
3. Heat the mixture gradually to boiling until the reaction is complete.
4. Filter while hot and concentrate to 1/3 its volume.
5. Crystallize in an ice bath.
6. Weigh the undissolved CuO and get the weight of the CuO which
reacted.
7. Compute for the theoretical yield based on this amount.

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

REACTIONS OF COPPER SALTS


1. KI T.S. Filter and divide the filtrate into two (2) portions and
dilute with water. To one portion, add starch TS, to the other
portion, add a few mL of chloroform and shake.

CuSO4 + KI CuI + K2SO4


with starch TS blue color
with CHCl3 violet color in CHCl3 layer due to the
liberation of I2

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

REACTIONS OF COPPER SALTS


2. Add a little HCl to acidify the solution, then place an
untarnished piece of iron wire or nail. Observe.

CuSO4 + Fe FeSO4 + Cu

3. NaOH solution, a little, then in excess.

CuSO4 + 2NaOH Cu(OH)2 + Na2SO4


[the copper hydroxide forms as a blue
precipitate]
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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

REACTIONS OF COPPER SALTS


4. NH4OH solution, a little, then in excess.

CuSO4 + NH4OH Cu(NH3)4SO4


very deep blue color w/c turns black
when copperamine structure was
decomposed
5. Na2CO3 TS

CuSO4 + Na2CO3 → CuCO3 + Na2SO4

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

REACTIONS OF COPPER SALTS


6. Using 0.5mL of CuSO4 TS, slowly add conc. HCl.

CuSO4 + HCl CuCl2 + H2SO4

7. K4Fe(CN)6 TS
Potassium ferrocyanide precipitates red-brown copper(II)
ferrocyanide from Cu2+ solutions:

2Cu2+ + [Fe(CN)6]4- <==> Cu2[Fe(CN)6]

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

QUESTIONS:
1) Which is more stable Cu+ or Cu+2 ? Explain.
a. Salts of monovalent Cu is unstable in a medium that permits
ionization.
b. Cu+2 is more stable
2) What is the difference between the reaction of ammonia TS
and NaOH TS towards cupric ion? Explain.
a. Cupric ion with ammonia TS forms copperamine structure w/c
is blue in color, but when decomposes turns into black;
b. Cupric ion with NaOH TS forms blue ppt of Cu(OH)2

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

QUESTIONS:
3. Explain the results obtained in reaction no. 1.
CuSO4 + KI CuI + K2SO4
with starch TS blue color
with CHCl3 violet color (CHCl3 – oxid. agent)

*Formation of CuI w/c when treated with starch forms blue color
of solution, then turns to violet when treated with CHCl3 due to
oxidation of Cu+2 to Cu+1.

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

QUESTIONS:
4. In reaction no. 4,
a. what complex ion is responsible for the original blue color?

Cu(NH3)4SO4 very deep blue color

b. What complex ion is present after the reaction? What is its


color?
Cu(NH3)4+2 blue solu’n. w/c turns black when the complex ion
was decomposed

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UNIVERSITY OF PERPETUAL HELP – DR. JOSE G. TAMAYO MEDICAL UNIVERSITY

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