EXPERIM NT

(-

Synthesis of o Chemicol Compound:

(_
Moking Alum from Aluminum
("_

L melted down, and used to make more cans or other

Purpose
(.-- aluminum metal products. So this experiment repre-
. Apply the principles of synthetic chemistry, the sents another way of recycling scrap aluminum into
process by which one pure substance is something potentially useful. (To be truthful, we
transformed into another. would have to say that if you wanted to make tons of
alum, it would be cheaper to start with natural ore
(- already containing Al3* ions. This is because a lot of
Pre-Lob Preporotion chemical reagents and electrical energy go into mak-
-
Anyone who lives in a modern city surrounded by ing aluminum metal from natural ores. On a large
!_ the necessities that make urban life possible and the scale, making alum from aluminum metal would be
luxuries that make it enjoyable should ponder this uneconomical.)
L question: Where does all this stuff come from? The
answer, of course, is that it comes from the elements
Now let's look at the chemistry involved in trans-
forming an aluminum can into alum. Aluminum cans
L found on earth. The same elements that make up the
mountains and valleys, the seas and the air, and all
are made of fairly pure aluminum, except for the
decorative paint on the outside and the thin coating

t living and nonliving matter can be transformed into

new substances that are used in a variety of ways in
our technological society.
of plastic on the inside, which prevents acidic chem-
icals in the beverage from reacting with the alu-
minum can. The first step in this experiment is to
L The process of making new substances from remove these coatings before the chemical reactions
with aluminum can begin.
other, usually simpler, substances is called chemical
L synthesis. The word synthesis implies the notion of
putting things together. The opposite of synthesis
The next step is to react the clean aluminum with
potassium hydroxide solution:
is analysis, which implies taking things apart, that 2Al(s) + 2 K+(aq) + 2OH (aq) + 6H2O(l) -
\_ is, determining the chemical composition of
2K+(aq) + 2AI(OH)t(aq) + 3Hz(g) (r)
substances.
\* In this experiment, we will transform the alu- This reaction can be classified as an oxidation-
minum from a beverage.can into a substance known reduction reaction, in which aluminum is oxidized
( as alum, more formally designated "aluminum and water is reduced, producing hydrogen gas and
potassium sulfate dodecahydrate," which has the hydroxide ion by transfer of electrons from alu-
chemical composition AIK(SO4)2 . 12 H2O. Alum is a minum to water. The KOH helps to dissolve the thin
\- versatile substance used in dyeing fabrics, tanning oxide coating on the aluminum that normally pro-
leather, and clarifying water in municipal water tects it from further oxidation. The hydroxide ion
treatment plants. Medicinally, it has applications as produced when aluminum replaces hydrogen forms
an astringent and a styptic; for example, if you a complex ion, the tetrahydroxyaluminate ion,
nicked yourself while shaving, you might use a stick Al(oH)4-.
\- of alum to coagulate the blood and stop the bleed- Equation (1) also explains why alkaline products
ing. Derivatives of alum are also widely used in for- like liquid detergents and bleaches are never stored
{
mulating antiperspirants, thus exploiting the astrin- in aluminum containers. The aluminum would slowly
gent properties of Al3+ ions, which bind water dissolve, producing hydrogen gas. In a sealed con-
\- strongly. tainer, a high pressure of hydrogen gas might build
Since aluminum cans have some intrinsic value, up, possibly causing the container to rupture or
t. empty cans are normally recycled, that is, collected, explode if the hydrogen ignited.

6-t
L-
6-2 Synthesis of o Chemicol Compound: Moking Alum from Aluminum
L
\-
Addition of a slight excess of sulfuric acid to the Experimentql Procedure
products produced in Equation (1) neutralizes the
excess KOH from the previous step and neutralizes Special Supplies: Aluminum beverage can; sturdy f
the four OH groups on the tetrahydroxyaluminate scissors or snips; coarse steel wool (or metal pot scrub-
complex ion: ber); smooth board or other material on which the alu- \-
minum metal can be scrubbed; crushed ice; glass filter
Al(OH)i(aq) + 2 H2SO.{(aq) -
I('F(aq) + funnel; Whatman No. 4 filter paper; filter flask; Btichner
filter funnel; filter paper to fit Buchner funnel; aspirator
K*(aq) + Al3 (aq) + 2 SOr2 (aq) + 4 H2o(l) (2)
or house vacuum; hot plate or steam bath; rubber
policeman; container for the alum produced.
This is an acid-base (or neutralization) reaction in
which the H+ ions in H2SOa react with the OH- ions in Chemicals: 1.4 M KOH; 9 M H2SO4; methanol; NaHCOr.
Al(OH)4- to form water, leaving behind Al2(SO4)3. The \-
reaction is strongly driven to the right by the forma-
tion of the very stable HrO molecule.
SAFETY PRECAUTIONS:
The resulting solution contains K+, Al3+, and
SOn2- ions in the proportions in which they are
I WEAR EYE PROTECTION AT ALL
found in alum: AIK(SOa)2. After sufficient cooling, TIMES. Potassium hydroxide, KOH, and
crystals of hydrated potassium aluminum sulfate, or sulfuric acid, HrSOn, are very corrosive.
alum, will form. Both can cause burns if left in contact
There are 12 molecules of water associated with with the skin. If either chemical gets on
each formula unit of the salt, so the formula of the your skin, immediately rinse with plenty
crystalline alum that forms is AIK(SO+)z . 12 H2O. of cool water for several minutes. Your
This is typically true of compounds that contain instructor will discuss emergency
metal ions, but in a beginning chemistry course we measures to follow if your eyes are
often ignore these water molecules as we write affected. If spills occur, notify the
chemical formulas-unless they are critical to the instructor, who will know how to
results of an experiment, as they are here. For neutralize the spill with sodium
example, what you usually see written as FeCl3 is bicarbonate and can advise you on proper i

actually FeCl, . 6 HrO (or [Fe(HzO)o]Cl3 to show that cleanup procedures, Wear gloves if there
the waters surround the metal). X-ray crystallo- is any chance of contact with strong acids
graphic studies show that each K+ ion and each Al3+ or bases.
ion is surrounded by six water molecules. In solu- Methanol vapors are toxic, and liquid
tion, each is also surrounded by a cluster of approx- methanol is toxic if swallowed. Use
imately six water molecules. As you will study later methanol in the hood, and avoid getting it
in greater detail, water is a polar molecule, with the on your skin. If it does contact your skin,
oxygen atom having a slightly negative charge rinse it off immediately with water.
while the hydrogen atoms are slightly positively Because methanol is flammable, no open
charged. So the negative oxygen atoms in the water flames should be allowed in the
molecules are attracted to the positively charged K+ laboratory,
and Al3+ ions, and there is just enough room for
about six water molecules to crowd around each
positive ion.
The solution containing the dissolved alum is
The synthesis of olum
cooled with ice because alum is quite soluble in
water, but its solubility decreases as the temperature To begin the synthesis of alum, cut a piece of alu-
is lowered. So cooling the alum solution increases minum about 5 x 5 cm from an aluminum beverage
the amount of solid alum that can be recovered. can. Be careful with the sharp-edged piece of metal.
To get pure alum, it is necessary only to filter off Place it on a smooth board surface, and scour off the
the crystals and wash them to remove the excess coatings on both sides with coarse steel wool or a t

HrSO, used in the second step. The washing is done metal pot scrubber. When the piece of aluminum is !
with methanol, which does not dissolve the alum or clean and bright, rinse and wipe it with a paper
remove any of the water of crystallization. Methanol towel. Using scissors, cut the clean aluminum into
also has the advantage of evaporating quickly. small squares about 0.5 x 0.5 cm.
I
(__
Synthesis of o Chemicol Compound: Moking Alum from Aluminum 6-3

Tare,l or weigh, an empty I50-mL beaker to the

Fill the funnel with water and let it
( nearest milligram, and record the mass. Add between run until the air is washed out oI
0.5 and 0.6 g of the small pieces of aluminum, and the stem. When the water level
record the mass to the nearest milligram. drops to the top of the stem,
L obtain 25 mL of 1.4 M KoH solution. Fold and crease lightly
add the mixture to be filtered.

CAUTION; KOH will dissolve aluminum and your

( skin! Make certain you are wearing your eye protec-
tion, and immediately rinse off with water any KOH
L that gets on your skin.
Working in the hood, carefully add the 25 mL of
1.4 M KOH to the beaker containing the small pieces
L of aluminum. Use a stirring rod to guide the solution
Fold again.

stream as you pour it.

L Place the beaker on a hot plate set at low heat or
on a steam bath. Warm the solution, but do not allow
it to boil. With occasional stirring, all the aluminum
should react in about 20 min. While the aluminum is
dissolving, set up a glass funnel using a ring stand
a (r
L and iron ring or funnel support. See Figure 6-1 for an
Tear olf the corner
unequally (the torn corner
example of the equipment setup. Place the stem of prevents air {rom leaking
the funnel in a 150-mL beaker. Fold a piece of coarse down the fold). Then open
l'- the filter out like this.
filter paper (Whatman No. 4 or equivalent) into quar-

L ters, and place it in the funnel. Pour a little water into

the filter paper so that it will stay in place. Discard
The weight oI this
column of water
hastens tiltration.
any water that runs through the filter into the beaker.
L When there are no visible pieces of aluminum or
bubbles of hydrogen gas, you will know that all of

t
i
the aluminum has reacted. Remove the beaker from
the hot plate temporarily. Obtainl0 mL of 9 M H2SO4,
and carefully but rapidly pour all of the 9 M H2S04
Place the filter paper in the
funnel and seal the edge
against the funnel wall by
moistening the paper.
Stem

L into the beaker, stirring steadily. If the H,SO, is

added too slowly, you may see the transient forma-
L tion of insoluble AI(OH)3 that will precipitate when
just enough acid has been added to react with one of
The filtrate should
run down the walls
of the beaker.
(- the OH groups of the Al(OH)a complex ion. Because
you are adding a strong acid to a solution of a strong
base, there is an exothermic neutralization reaction,
L making the solution hotter.
Stir the solution thoroughly. If white crystals are
(,., visible, return the beaker to the hot plate or steam FIGURE 6-l $ rhe process of filtration.
bath, and stir until all such material dissolves. Any
tiny black specks may be disregarded. When the beaker can be handled safely, place
\__
your stirring rod against the lip of the beaker to
guide the hot solution into the previously prepared
L tTo "tare" a container is to weigh it on a balance wl-rile adjusting
the balance to read "zero" w'hile the container is on the balance.
glass filter funnel. Do not touch the filter paper with
You can then place an object in the container, and the weight of
the stirring rod or you may puncture the paper. Don't
L the object can be read directly from the balance display. If you
are to use this feature on your balance, your instructor will need
overfill the filter funnel. The level should not
closer than I cm to the top of the filter paper. The fil-
be

to instruct you in the taring process. The alternative is to weigh trate should be clear and colorless.
the container, then weigh the container \,vith the object in it, and
Allow the 150-mL beaker containing the filtrate to
then subtract one weight from the other to determine tl'le weight

I of the object. This method is referred to as "weighing by differ-

ence." Under no circumstances should reagents be rveighed by
placir-rg them directly on the balance pan.
cool. Fill a 600-mL beaker about half full of crushed
ice. Place the 15O-mL beaker in the ice bath for about
20 min, stirring frequently as crystals of alum form.
L
t_
6-4 Synthesis of o Chemicol Compound: Moking Alum from Aluminum

\
transfer the dried alum crystals and filter paper cir-
Moist filter paper cle to the weighed 150-mL beaker. Use a stirring rod
or metal spatula to scrape off any crystals adhering
to the filter paper, and remove the filter paper.
Reweigh the beaker containing the alum crystals, and
record this mass.
Follow the instructor's directions for disposing of
Filter pump the sample of alum that you prepared.
Weigh 10 g of sodium bicarbonate, NaHCOr. Add
about 80% of the NaHCOq to the solution left in the fil-
ter flask. Swirl the flask until the bubbling ceases and
the NaHCO3 has dissolved. Now add the rest of the \-
NaHCO3, and note whether any additional bubbles of
CO2 are produced. If additional bubbles form, add 2 g
more of NaHCO3. When there is no more bubbling
upon further addition of a small amount of NaHCOr,
rinse the solution in the filter flask down the drain.

lj,ll$Sitlll$i coNsIDER THIs lli:illl ,.-.,,,

What does the CRC Handbook of Chemistry and
Physics, the Merck Index, or another reference tell
i1
you about what it takes to remove the 12 water mol-
FIGURE 6-2 li Vacuum filtration technique using a ecules from alum? Why do we often "forget" to
Btichner funnel. To prevent aspirator water from include the ". 12 H2O" when we write the formula of
entering the flask, disconnect the rubber tube
before turning off the aspirator. alum or similar hydrated salts? Would it be better to
write the formula as Al(H,O)ol((H2O)6(SO.r)2? Com \

ment on other ways the formula could be written,

While the solution is cooling, set up a filter flask such as AlH21KO20S2 or All((SOa)2(HzO)iz.
and Btichner filter funnel attached to an aspirator or When we combine salt (NaCl) and water, we don't
house vacuum (see Figure 6-2). describe the process as a synthesis or the product,
When the crystallization is complele, stir care- "salt water," as a compound. What is the difference
fully with a thermometer, and record the tempera- between the synthesis of a compound such as alum
ture when the reading stabilizes. The solution tem- and the production of a mixture or solution such as
perature should be 6'C or less. salt water? As you write your description, suppose
Place a circle of filter paper (preferably Whatman you are an early chemist and cannot use the con-
No. 4, although No. I will do) of the appropriate size cepts of an element or a formula in your explanation.
in the Btichner funnel. Moisten the filter paper to Clean, dry, and weigh an aluminum can. Find the
hold it in place. Turn on the aspirator or house vac- price of aluminum by doing a Google search on
uum. Remove the 15O-mL beaker from the ice bath, "price of aluminum." What is the value of the alu-
and stir the contents of the beaker with a stirring rod minum in a beverage can? Then determine how much
to loosen all of the alum crystals. Transfer all of the a local recycling center is paying for aluminum cans.
suspended crystals to the Btichner funnel. A rubber How does the value of aluminum compare to its
policeman on the end of your stirring rod is helpful "worth" in your community? Why are the two prices
in scraping out as many crystals as practical. so different?
Add two 10-mL portions of methanol in succes- You can find science activities on the Web where
sion to wash the excess H2SOa out of the crystals. alum is used to clarify water, as described in the Pre-
Continue to draw air through the alum for another 10 Lab Preparation section. You can also find directions 1

to 15 min to dry the crystals. for growing large, clear crystals of alum from the
Weigh a clean, dry 150-mL beaker to the nearest powder that you produced in this experiment. With
milligram. Record the mass. Shut off the source of your instructor's permission, explore these uses of alum.
vacuum, and remove the Btichner funnel. Carefully
I RE PO RT 6
Synthesis of a Chemical Compound: Name
Making AIum from Aluminum
Date Section

Locker Instructor_

L
(__
Doto

a i)
l. Weighing the oluminum

L (a) Mass of empty 150-mL beaker o

(b) Mass of I50-mL beaker + aluminum c

L (c) Temperature of cooled alum crystals C

(-
2. Weighing the olum
(.-
(a) Mass of empty 150-mL beaker b

L (b) Mass of 150-mL beaker + alum o

b

f
t_ Colculofions

L Mass of aluminum metal used o

f Mass of alum obtained o

(.- Calculate the number of moles of aluminum that you used. Show your calculations

L moles Al

L Calculate (or look up in a reference such as the CRC Handbook of Chemistry and Physics) the formula mass
(molar mass) of alum, KAI(SOq)z-12 H2O, including its water of crystallization. (You might find it under the

L name potassium aluminum sulfate.)

f g/mole
(.-- Noting that one aluminum atom is in each formula unit of alum, we know that each mole of aluminum will give
rise to one mole of alum. Based on the number of moles of aluminum you used, calculate the maximum num-
(.- ber of grams of alum that you could produce, assuming that aluminum is the limiting reagent:

t g alum

I 6-5
 I

Using the number of grams of alum that you actually obtained, calculate the percentage yield of alum for your
synthesis:
U
galum from experiment y
% vield
' - maxrmum g alum rrom theory
loo% %

Show your calculation \.,

Questions
l. Experiments show that the solubility of alum in 25 mL of 1.4 M KOH plus l0 mL of 9 M HrSO, is about
1.0 g at 1.0 "C and 1.7 g at 6.0'C. Using your measured solution temperature, estimate the amount of alum left
in your chilled solution.
\-
1

Alum left in solution b

2. Does the amount of alum left in solution account for most of the difference between the maximum grams of
alum and your experimental grams of alum? Explain.

ffiffiwffiffiffi& coNsrDER THrs ffi;ffi## !-

What does the CRC Handbook of Chemistry and Physics, Ihe Merck Index, or another reference tell you about
what it takes to remove the I2 water molecules from alum? Why do we often "forget" to include the ''. 12H2O"
when we write the formula of alum or similar hydrated salts? Would it be better to write the formula as
Al(H2O)6K(HzO)o(SO+)z? Comment on other u,ays the formula could be written, such as AlHrrKOroS, or
AIK(S04)2(H2O)12.

6-6
REPORT 6 SHEET 2

Name Date

When we combine salt (NaCl) and water, we don't describe the process as a synthesis or the product, "salt
water," as a compound. What is the difference between the synthesis of a compound such as alum and the pro-
duction of a mixture or solution such as salt water? As you write your description, suppose you are an early
chemist and cannot use the concepts of an element or a formula in your explanation.

Clean, dry, and weigh an aluminum can. Find the price of aluminum by doing a Google search on "price of
aluminum." What is the value of the aluminum in a beverage can? Then determine how much a local recycling
center is paying for aluminum cans. How does the value of aluminum compare to its "worth" in your community?
Why are the two prices so different?

If you explored any of the properties of alum, such as using it to clarify water or to grow alum crystals, describe
the results of your experiments and explorations.

6-7
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