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INTRODUCTION:

Ferrous sulfate (FeSO4.7H2O), traditionally known as "green vitriol" or


"copperas", forms beautiful blue-green crystals of the monoclinic system. Ferrous
sulfate is useful in chemistry as a reducing agent and a source of ferrous ions. It can
also act as a catalyst; an example is Fenton's Reagent, which is used to destroy organic
chemical wastes.
Ferrous Sulfate is an essential body mineral. Ferrous sulfate is used to treat iron
deficiency anemia (a lack of red blood cells caused by having too little iron in the body).
Less serious ferrous sulfate side effects may include: constipation, upset
stomach, black or dark-colored stools, or temporary staining of the teeth.

MATERIALS:

Sulfuric Acid (H2SO4), about 30-40% concentration


Acetone
Steel wool, #00 or 000 fineness
Safety goggles
Rubber or vinyl gloves
Lab apron & lab coat
Beaker, glass
Steel pan or glass dish, reserved only for chemistry
Petri dish or crystallizing dish, glass
Droppers
Laboratory oven or sealed-element hot plate
Ice, crushed, in a shallow container
Funnel and filter paper; better yet, a vacuum filtration setup
pH paper or pH meter
Desiccator with calcium chloride drying pellets (optional)

METHODOLOGY:

Again, keep those safety goggles on at all times. During the acetone step,
exclude all possible sources of spark, flame, or live heating element.
The size of beaker selected depends on how much ferrous sulfate you wish to make. A
good, all-around beaker size is 100 or 250 mL.

I. Preparation of FeSO4 solution.


For best results the lab temperature should be kept below 25C. Avoid
temperature fluctuations as much as possible, except where indicated in this procedure.
Degrease the steel wool by immersing it in acetone for half an hour. Remove it
from the acetone and let it dry in a well-ventilated lab where nobody can disturb it.
During this whole time there must be no ignition sources nearby. Do not attempt to
evaporate the acetone with a heat source. Even an electric lamp could cause ignition.
Place the glass beaker in the center of a metal pan or wide glass dish that's
reserved just for lab use. The reaction can produce minor spattering as hydrogen
bubbles to the surface of the acid.
Place the degreased, dry steel wool in the glass beaker and pour in enough 3040% sulfuric acid to cover it completely. Don't use concentrated acid. If the steel wool
is not fully submerged, carefully push it down with a glass rod.
The sulfuric acid will begin to dissolve the steel, producing hydrogen gas. Over
the course of several hours the steel wool will gradually disappear. Carefully add more
steel wool. Repeat this a few times. Reddish-brown, insoluble ferric compounds will
form if you add too much steel wool; just add some dilute sulfuric acid if this happens.
The pH of the solution should be acidic at any given time, otherwise the ferrous ions will
oxidize to the ferric state.

II. Filtering
Green crystals should have started forming in the solution and settling to the
bottom after just a few hours. They may become tangled up in any steel wool that's still
left; don't bother trying to free these.
When you're satisfied with the amount of ferrous sulfate that has formed, add
excess water that's been acidified to a pH between 2 and 4 using sulfuric acid. Add
enough of this acidified water to re-dissolve all the green crystals that have settled out.
If the solution turns brown, add just enough sulfuric acid to make it green again.

Filter this solution through filter paper. Discard the solids and the paper;
neutralize their acidity with some dilute sodium carbonate solution. Save the filtrate. It
should now be free of steel wool pieces, carbon (from the steel), rust, and other solids.
Keep the solution in a covered container to minimize contact with atmospheric oxygen.
If the pH is not kept low enough, ferrous sulfate will oxidize to ferric sulfate on
standing. Normally, atmospheric oxygen changes Fe2+ to Fe3+ quite readily. This
reaction is reversible, however, by lowering the pH. Below 4 or so, ferrous ion is heavily
favored over ferric, with the concentration of Fe3+ becoming vanishingly small at pH 12. Aqueous FeSO4 in this pH range is stable for days, even with much air contact.

III. Evaporation
The filtered solution is put in a shallow, glass container such as a petri dish or
crystallizing dish. Place this on the hot plate and turn it to the lowest setting; even
better, use a small, laboratory oven. Don't use a household-type oven; these are not
safe for general lab use.
Slowly heat the solution to about 80 to 90 C; do not boil it. Hold it at this
temperature until about half the liquid has evaporated. Don't breathe the vapors given
off; although they will be mostly water, they will contain some sulfuric acid. The color of
the solution may change to yellowish, but don't let this discourage you. On cooling it
becomes green again.
Allow the solution to cool to room temperature and place the shallow dish on
crushed ice. Leave it there for at least an hour. Don't let it sink into the water as the ice
melts.
Remove the dish from the cold and place it on the lab bench in your locked
laboratory (remember, the liquid contains sulfuric acid!). Let it stand for 24 hours.
Green crystals should form. If not, the cause is probably one of the following:
1. You didn't evaporate the solution down far enough.
2. The pH was too high.
3. The ambient temperature was too high.
4. Your sulfuric acid was contaminated with something that oxidized Fe2+.

Decant or pipette off the yellowish liquid that remains after the crystals have
formed. It is strong sulfuric acid, so be careful with it. Use a dropper to add it slowly
into a cold, dilute solution of NaOH, sodium carbonate, or ammonia.
Do not handle ferrous sulfate with your fingers. Use a plastic or steel spatula.

IV. Washing
If possible, have a previously-prepared batch of ferrous sulfate crystals which are
dissolved to saturation in cold (1 to 4 C) distilled water. Use this solution, prepared and
chilled shortly before use, to wash the crystals you've grown.
If you've prepared FeSO4 for the first time and don't have another batch, just use
distilled water cooled to just above freezing. There will be some minor losses as some
of the crystals go into solution.
As the washing removes the strong sulfuric acid from the surface of the crystals,
the atmosphere will unfortunately oxidize them more readily. Larger crystals are more
desirable; less FeSO4 will oxidize. Conversely, don't crush or powder the crystals,
since it will increase the surface area.

V. Drying; Final steps


If no desiccator is available, dry the ferrous sulfate crystals in air at the lowest
relative humidity available (e.g., not outside on a foggy day). It's preferable to do the
drying in a desiccator having a some calcium chloride drying pellets in the bottom.
Obviously, the ferrous sulfate shouldn't contact the desiccant material. Let them dry
just enough to get the excess water off the crystals, then put them in a tightly-sealed
container where moisture can't get to them.
The washed and air-dried crystals of ferrous sulfate can be saved for future
experiments as they are, or some / all of the moisture in the crystals can be driven off.
Placing them in a vacuum desiccator containing some calcium chloride can
dehydrate the crystals, depending on time and on vacuum strength. It's uncertain what
state of hydration this treatment leaves; evidently, predicting this is more involved than it
would seem. The dried compound may be the monohydrate (FeSO4.H2O) or the
tetrahydrate (FeSO4.4H2O), or even a mixture containing both. Mitchell (1984)
explores the subject in depth.

If ferrous sulfate is heated to dehydrate it, the heat mustn't be too strong, or they
will decompose to make the toxic and corrosive sulfur trioxide (SO3).
According to The Merck Index (1983), heating FeSO4.7H2O to 90C will leave
ferrous sulfate monohydrate. The same source (1983) lists the synonym "exsiccated
ferrous sulfate" for the monohydrate; the term appears in older texts and formularies,
especially with the spelling "sulphate". Some sulfuric acid remnants from solution may
also begin to come off during heating to the monohydrate, so there must be adequate
ventilation.
The monohydrate will give up its last H2O by heating to 300C, preferably with as
little air contacting the sulfate as is practical. (Never heat anything in a completely
sealed vessel.) Much of the remaining sulfuric acid bound to the crystals will also come
off, so the heating must be done under a laboratory fume cupboard or outdoors. In the
latter case, wear a respirator that's rated by the manufacturer for sulfuric acid vapors,
just in case the wind shifts your way.
FeSO4 decomposes at around 480C to give off SO3 (dangerous!!). To ensure a
healthy margin of safety, avoid heating it above 350C.

DATA AND OBSERVATION:

DISCUSSION:
Now that we've prepared ferrous sulfate, it can be used as a reducing agent, a
catalyst, an ingredient for Fenton's reagent, or a reactant for preparing a number of
other compounds. For example, mixing equimolar solutions of FeSO4 and ammonium
sulfate will yield ferrous ammonium sulfate, also known as Mohr's salt. This can be
crystallized out and is much more resistant to air oxidation than FeSO4 (McGraw-Hill
Encyclopedia of Chemistry, 1993). Of course, Mohr's salt is not interchangeable with
FeSO4 for every application.
Since so much of chemistry hinges directly on oxidation and reduction, it's easy
to imagine how useful a reducing agent would be. For example, ferrous ion will reduce
Ag+ to metallic silver in the following manner:
Fe2+ (aq) + Ag+ (aq) = Fe3+ (aq) + Ag (s)
Some experiments will call for a solution of ferrous sulfate at a pH where there's
not enough acid to stabilize it. In other words, the FeSO4 is simply dissolved in water
without adding the sulfuric acid. This kind of solution won't last long in the presence of
air, but it's a more effective reducing agent than acidic FeSO4. If an experiment calls for
the non-acidic variety, it should be prepared immediately prior to use. Use de-gassed
water, keep the solution in a closed container with very little air space, and keep it on
ice.
Ferrous sulfate is incompatible with certain compounds; see the Merck Index
entry or MSDS for it. You may read about some experiments here and there which, in
apparent contradiction, call for mixing these same compounds together. It's often a
matter of the conditions. For instance, there are well-established experiments that
involve iron and silver salts together in dilute solution. Under other circumstances,
though, the resulting silver particles might pose a combustion or reactivity hazard.
Ferrous sulfate is also incompatible with lead acetate, so keep these compounds
separate if you've prepared both. Whenever there's any doubt about chemical
compatibility, just stay with the established procedures.

CONCLUSION: