You are on page 1of 3

Experiment 3

AIM/OBJECTIVE: Preparation of a) Tetrammine copper (II) Sulfate and b) estimation of


copper as CuCNS gravimetrically in the complex.
Safety Notes
a) Concentrated ammoniatoxic, corrosive and irritating. Prevent contact with your eyes, skin,
and clothing. Permanent fogging of soft contact lenses may result from NH 3 vapors. Avoid
inhaling vapors and ingesting the solution. If you spill any NH3 solution on yourself,
immediately rinse with a large amount of running water. If you spill any solution on the
laboratory bench, add water and wipe up immediately with a damp paper towel. Immediately
notify your laboratory instructor of any NH3 spills.
b) Copper(II) sulfate pentahydratetoxic and irritant
c) Ethanoltoxic and flammable, it is highly flammable. Be sure that the gas flow to your
Bunsen burner is shut off, and that there are no other open flames nearby when you bring the
ethanol container to your work area.
Apparatus/glassware required:
Part A: Conical flask, stoppers, filter flask, filter paper, Buchner funnel and flask, beaker, glass
rod etc
Chemicals Required: Concentrated ammonia, Copper(II) sulfate pentahydrate, ethanol
Part B:
Apparatus/glassware required: Filter flask, filter paper, Buchner funnel and flask, beaker, glass
rod G-4 Sintered glass crucible heated to constant weight, Suction pump, Electric oven
maintained at 110C.
Chemicals Required:10% aqueous solution of Sodium bisulphite, H2SO4, Ammonium or
potassium thiocynate : 2N solution, Alcohol 20% aqueous solution
Introduction and Theory: a) In this experiment, you will prepare tetraamminecopper(II) sulfate
monohydrate, [Cu(NH3)4]SO4 H2O, from a reaction of CuSO4 5 H2O and NH3 in aqueous
solution. Although we usually write the formula of the reactant compound as CuSO 4 5 H2O, in
the crystalline state this compound is composed of tetraaquacopper(II) complex ions,
[Cu(H2O)4]2+. Therefore, we might better represent the compound as [Cu(H2O)4]SO4 H2O. The
fifth water molecule is not part of the complex ion, but is hydrogen bonded to the sulfate ion
(SO42) in the solid.
The chemical reaction described above is shown in Equation.

This is a single replacement reaction in which NH3 molecules replace the water molecules
originally bonded to the copper(II) ion. The strategy you will employ in this synthesis is to add a
large excess of NH3 solution to an aqueous solution of [Cu(H 2O)4]2+ ion in order to achieve a
complete replacement of H2O by NH3. At this point, you will have the product in solution, where
it exists as discrete tetraamminecopper(II) ions, [Cu(NH3)4]2+, and SO42 ions.
To isolate the product as a solid, you must crystallize it. To do this, you will evaporate a portion
of the water, add some ethanol, and cool the solution in an ice bath. Each of these steps reduces
the solubility of the product and is therefore important in maximizing your yield. Because
ethanol is less polar than water, ethanol is a poor solvent for ionic compounds.
Addition of ethanol to the solution reduces the solubility of [Cu(NH 3)4]SO4 H2O in the mixture,
causing the product to crystallize. Very little, if any, solid [Cu(NH3)4]SO4 H2O will form if you
do not add ethanol.

If you fail to reduce the water volume or to cool the solution sufficiently, your yield will also be
reduced, because some of the [Cu(NH3)4]SO4 H2O will remain dissolved in solution. You can
also help maximize your yield by using proper experimental technique. You must be particularly
careful to prevent loss of product during certain steps in the synthesis. First, when evaporating
the water, you must heat the CuSO4NH3 solution gently.
Some of the [Cu(NH3)4]SO4 H2O may decompose if you heat the reaction mixture too
vigorously. If some decomposition does occur, you will see a brown film on the bottom of your
beaker and a blackish brown tinge in the solid product.
Second, you must be careful when you filter the crystallized product from the supernatant liquid.
The filtration process involves three steps: decanting the supernatant liquid, transferring the solid
product, and washing the solid product.
Decantation is the process of pouring the supernatant liquid into the funnel without disturbing
the solid at the bottom of the beaker.The filtration takes longer if you do not transfer most of the
liquid to the funnel before you begin to transfer the solid. Once this is done, you can pour the
wet solid into the funnel and use a rubber policeman attached to a glass stirring rod to scrape the
remaining solid out of the beaker.
Clearly, you want to transfer all of the product from the beaker into the funnel. To assist in
getting the last remaining product out of the beaker, you will add asmall amount of ice-cold
NH3ethanol solution to the beaker, swirl, and immediately transfer the mixture to
the funnel. Then you will wash the solid with the remainder of this ice-cold solution as well as
with a portion of ice-cold ethanol. It is important that the washing solutions be very cold and free
of water so you do not redissolve any of the product.
Finally, you will dry and weigh your product. You will then calculate the theoretical and percent
yields for your synthesis.
b) Gravimetric Estimation of Copper as copper thiocynate in the tetrammine complex prepared as
CuCNS. When Copper (II) ions arc treated with potassium thiocynate in a solution containing
sulphurous acid white copper(l) thiocynate is precipitated which is fairly insoluble.
In this reaction an excess of KCNS must be added to decrease the solubility of CuCNS.
However, a very large excess of KCNS may dissolve the ppt. as K3[Cu(CNS)4].
Procedure:
Part A:
1. Prepare these items:
a hot water bath
6 ml of ethanol in a 20 ml test tube (use a graduated pipette)
2. Weigh between ~1.5 g of copper(II) sulphate using a balance. Weigh a test tube using a 0.01g
balance and record its mass. Add your copper (II) sulphate to the test tube, re-weigh using the
0.01g balance and record its mass.
3. Add 4 ml of water using a graduated pipette and place the test tube in the water bath. Stir
gently to dissolve the copper(II) sulphate.
4. Remove the test tube of copper(II) sulphate solution from the water bath. Do the next step in
the fume cupboard while wearing gloves. Add, with stirring, 4 ml of concentrated ammonia
solution to the copper(II) sulphate solution.
5. Pour the contents of the test tube into the conical, add alcohol (6 ml) dropwise with constant
stirring when dark blue precipitate of [Cu(NH3)4]SO4 H2O is obtained, warm it on water bath
for 10 minutes, mix to dissolve the content with stopper on conical flask, then cool the mixture
to crystallize the product.
6. Using a Buchner funnel and flask, filter the crystals. Wash out your test tube with cold ethanol
and add the washings to the Buchner funnel. Finally, rinse the crystals with cold ethanol.
7. Carefully scrape the crystals off the filter paper and onto a fresh piece of filter paper. Cover
the crystals with a second piece of filter paper and pat to dry the crystals. Note that, to get the

crystals completed dry, you may need to repeatedly move the crystals to dry parts of the filter
paper.
8. Weigh a sample bottle and record its mass using a 0.01g balance. Carefully transfer your
crystals to the sample bottle. Re-weigh the sample bottle and record its mass.
Analysis:
1. Calculate the relative formula masses of CuSO4.5H2O and Cu(NH3)4SO4.H2O.
2. Calculate the amount of copper(II) sulphate you used. Use your answer to calculate the
theoretical yield (mass) of tetraamminecopper(II) sulphate-1-water your reaction should have
produced.
3. Use your recorded masses to calculate the mass of copper(II) sulphate and the actual yield of
product.
4. Calculate the % yield you obtained
Comment on your % yield, and explain any loss or gain in mass compared with the theoretical
yield.

Part B:
1) Weigh 08 to 09 g of the dry complex and transfer to 250 ml beaker.
2) Acidify the solution with 25 ml of H 2S04 and add to it 25 ml of 10% Sodium bisulphite
solution and dilute to 100 ml with distilled water and boil the solution.
3) Add about 5 ml of ammonium thiocyanate drop-wise with constant stirring. Cover the beaker
with a watch glass and boil it. Remove the burner and allow the contents to stand for six hours.
4) Filter the precipitate on a G-4 sintered glass crucible. Wash the white ppt. with dilute
ammonium thiocyanate solution and then with alcohol.
5) Dry the ppt. at 110C in oven, cool till constant weight and weigh the precipitate
Analysis:
Calculate the amount of copper or Tetra ammonium coppcr(II) sulphate by using the following
stoichiometric factor.

Wt. of Cu in the given complex= 052243x wt. of ppt


Wt. of complex in the given sample = 21639x wt. of ppt.
Result: Report the yield, % yield and % purity of the complex

You might also like