Core Practical 12: Preparation of a Transition Metal Complex
Objective: To prepare a transition metal complex: tetraamminecopper(II) sulfate monohydrate, Cu(NH₃)₄SO₄·H₂O.
Reaction Equation
CuSO₄·5H₂O + 4NH₃ → Cu(NH₃)₄SO₄·H₂O + 4H₂O
Safety
- Wear lab coat and eye protection.
- Concentrated ammonia is corrosive and dangerous to the environment – use in a fume cupboard while wearing gloves.
- Copper(II) salts are harmful and environmentally hazardous.
- Ethanol is flammable – keep away from open flames.
Apparatus and Chemicals
Apparatus
- Copper(II) sulfate
- Concentrated ammonia solution (2 cm³)
- Ethanol (10 cm³)
- Graduated pipette (10 cm³) and pipette filler
- Beakers (50 cm³ and 100 cm³)
- Stirring rod, spatula
- Ice bath (crushed ice)
- Büchner funnel and flask (for vacuum filtration)
- Filter paper, gloves, test tube
- Balance (2 d.p.) and weighing boat
- Access to hot water (e.g. kettle)
Chemicals
- Copper(II) sulfate
- Concentrated ammonia solution (2 cm³)
- Ethanol (10 cm³)
- Anhydrous calcium chloride (6 g)
- Sodium hydrogencarbonate solution (20 cm³, 0.1 mol dm⁻³)
- Anhydrous sodium sulfate (1 g)
Procedure
- Weigh between 1.4 g and 1.6 g of copper(II) sulfate.
- Weigh the empty test tube first, then again after adding the solid.
- The difference is the mass of copper(II) sulfate used.
- Dissolve the solid in 4 cm³ of water using a graduated pipette.
- Stand the test tube in a 100 cm³ beaker containing hot water to gently heat it.
- Stir to aid dissolution, then remove from water bath once dissolved.
- In a fume cupboard, add 2 cm³ concentrated ammonia solution slowly while stirring.
- Transfer the contents into 6 cm³ cold ethanol in a beaker. Mix and cool the mixture in an ice bath.
- Filter the blue crystals using a Büchner funnel.
- Rinse the original test tube with cold ethanol and add washings to the funnel.
- Rinse crystals with cold ethanol.
- Dry the product:
- Transfer crystals to dry filter paper, cover with another, and pat dry.
- Repeat with fresh paper until dry.
- Weigh the dried crystals and record the mass.
Calculations
Example based on 1.5 g starting material
- Mr(CuSO₄·5H₂O) = 249.5
- Mr(Cu(NH₃)₄SO₄·H₂O) = 245.5
Moles of CuSO₄·5H₂O used = 1.5 ÷ 249.5 = 0.00601 mol
Theoretical yield = 0.00601 × 245.5 = 1.48 g
Actual yield (example) = 1.2 g
% yield = (1.2 ÷ 1.48) × 100 = 81%
Possible Reasons for Yield Loss or Gain
- Losses: Incomplete reaction, some product remain dissolved in the solution, transfer losses during filtration.
- Gains: Crystals not fully dry, impurities present.