EXPERIMENT 4
Synthesis of Alum
CHEM 103
Before we start
Safety check
Notebook
Attention
Lab Housekeeping
Outcomes/Objectives
1. Demonstrate synthesis of a new material.
2. Write balanced chemical equations for their synthetic
reactions.
3. Determine and report percent yield of their product.
Al AlK(SO4)212H2O
Aluminum metal Hydrated Aluminum
Potassium Sulfate
Introduction
Synthesis:
Making new substance from other simpler substances
In this experiment;
used beverage can/aluminum foil
Alum
AlK(SO4)2.12H2O Hydrate aluminum potassium sulfate
Double salt of Al+3 & K+ Total +4 charge Balance with
2 SO42- ions
Uses of Alum
Hydrate aluminum potassium sulfate Potash Alum
As a flocculent in Water Purification
As ingredient in aftershave
A treatment in Fireproof textile In Leather tanning
Uses of Alum
It is used for purifying water. The smell particles of pollutants, present in water, tend to
stick with the alum to form colloid particles. Since colloid particles are heavy, they
easily get settled down at the bottom of the container.
Powdered alum can also be used for treating canker sores. It is being used as an
aftershave for centuries. It control bleeding from small shaving cut and thus, prevent
infection.
It controls body odor. It can be applied directly on the perspiring areas of the body. As it
is soluble in water, it mixes up with the sweat and stop the growth of bacteria that
causes body odor.
Alum powder is used as the acidic component in certain brands of baking powder
which gives a metallic taste to the baking powder.
Alum is ingredient in mouthwash and toothpaste as it can fight against oral bacteria.
Alum is used as cosmetics and fire extinguishers
From: http://www.buzzle.com/articles/alum-powder-uses.html
Chemical Preparation of Alum
Chemical reactions
2Al(s) + 2KOH + 6H2O 2KAl(OH)4 + 3H2(g)
2 KAl(OH)4 + 4H2SO4 Al2(SO4)3 + K2SO4 + 8H2O
2 Al(s) + 2KOH + 4 H2SO4 2 AlK(SO4)2·12H2O + 3H2(g)
Alum
Sample Calculation (1 of 2)
Let us suppose you used 0.325 g of Al and produced 2.17 g of alum
Then following steps can be used to calculate % yield of your synthesis
(m2 – m1)
Moles Al = mass / molar mass = 0.325 g/ 27.0 g/mol = 0.0120 moles Al
According to the overall reaction: Al : Alum = 1 : 1
Moles of Alum expected = 0.0120 moles
Molar mass of AlK(SO4)2.12H2O = 474.390 g/mol
Sample Calculation (2 of 2)
Mass of AlK(SO4)2.12H2O expected= Number of moles x molar mass
(theoretical yield)
= 0.0120 moles x 474.390 g/mol
= 5.69 g
Mass of AlK(SO4)2.12H2O produced = 2.17 g (m4 – m3)
(actual yield)
% yield of Alum = x 100 % = = 38.1% yield
Chemical Preparation of Alum
Theory
First Step; Addition of excess KOH to Aluminum
2Al(s) + 2K+OH-(aq) + 6H2O(l) 2K++2[Al3+(OH-)4]- + 3H2(g)
Tetrahydroxyaluminate ion Charge of Al is +3
+1 0
Reduced
H2O H2
0
Oxidized
Al Al+3
Chemical Preparation of Alum
Theory
Second Step; Addition of H2SO4 acid : 2 reactions occur
According to the
1) Removal of excess KOH; overall reaction:
2KOH + H2SO4 K2SO4 + 2H2O
Al : Alum
2) Reaction with aluminate ion; 1:1
2K++2Al(OH)4- + 4H2SO4 Al2(SO4)3 + K2SO4 + 8H2O
Overall: 2Al(s) + 2KOH + 4H2SO4 + 10H2O 2AlK(SO4)2.12H2O + 3H2
Soluble in hot water Insoluble in cold water & methanol:
Cool then wash with Methanol
Safety Precautions
Will use Concentrated KOH & H2SO4 are “corrosive”
Methanol:
Toxic if swallowed – even in small quantities
Avoid skin contact and inhalation
Highly flammable
Wear safety gloves and goggles all the time.
Avoid skin contact with methanol.
Everyone in the lab must wear goggles!!
Must clean the common areas and your bench.
Safety check
Lab Housekeeping
Procedure (1 of 5)
Weigh a piece of aluminum foil
Cut the piece of metal from the aluminum can (or foil).
Cut into smaller piece and measure its weight in the beaker. It should be 0.5-0.6 g
Dry the 150 mL beaker and record the weight
React with KOH (25 mL of 1.5M KOH): In the fume hood, carefully add 25 mL of
1.5M KOH to the beaker containing the aluminum
Place the beaker on hot plate (low heat) (Al should dissolve in about 10-15 minutes)
Warm the solution (not boil) till all the Al have been dissolved while stirring occasionally
Add 25 mL
KOH (1.5M)
(10-15 mins) KAl(OH)4
Al (0.5-0.6 g) Hot plate
2Al(s) + 2KOH + 6H2O 2KAl(OH)4 + 3H2(g) Record the
mass
Procedure (2 of 5)
(Gravity Filtration)
While the Al is dissolving, set up the glass filter with fluted filter paper using
a ring stand for “gravity filtration”
Place a clean and dry 150 mL beaker under the funnel
When all Al has dissolved, remove the beaker from the hot plate
Stir the solution with a stirring rod, and do the “gravity filtration” while still
hot
The filtrate should be clear and colorless
Procedure (3 of 5)
Filter while still hot
Neutralize with H2SO4 (Slowly add 10 mL of 9M H2SO4). Stir steadily.
2 KAl(OH)4 + 4H2SO4 Al2(SO4)3 + K2SO4 + 8H2O
2 AlK(SO4)2·12H2O
Filter the solution KAl(OH)4
Filter paper
9M H2SO4 (10 mL)
Careful! The solution will get hot!
KAl(OH)4
Filtrate (clear and colorless)
Procedure (4 of 5)
Fill a 600 mL beaker with crushed ice (to about half full)
Crushed ice
Place above beaker with the filtrate in this ice bath while stirring
frequently
Cool to below 5 C and stir frequently. Alum will crystallize.
Filter the cold solution on the Büchner funnel
Wash any excess H2SO4 or KOH with methanol.
Add two portions of 10 mL methanol (Alum crystals are not soluble in
methanol).
Transfer the crystal collected on the filter paper
Measure the mass of Alum Actual Yield 100 produced mass of Alum
100
% Yield
Theoratical Yield Expected mass of Alum
Procedure (5 of 5)
Vacuum Filtration
While cooling, set up the Büchner funnel and connect to the aspirator
Filter the cold solution on the Büchner funnel, collecting the alum crystals on
the filter paper.
Add two 10 mL portions of methanol one at a time to wash off any excess
H2SO4
Continue to draw air through the filter until the alum crystals are dry
Remember, your %yield will not be correct if the crystals are not dry
Transfer the crystals collected on the filter paper to a dry, pre-weighed 150 mL
beaker and weigh them and record the weight in the data sheet
Disposal
The filtrate from the Büchner funnel contains excess
concentrated sulfuric acid
Neutralize this with approximately 10g (3-spoons) of NaHCO 3
(the sodium bicarbonate does not need to be weighed carefully,
all that is needed is an excess of this base to neutralize all
sulfuric acid)
The solution can now be poured down the drain
Laboratory Housekeeping
A well kept lab coincides with safe work environment. Work areas have to
be always clean and tidy
20
Thank you for attention
