A sample of waste water contains calcium ions, copper(II) ions and lead(II) ions. You are to plan an experimental procedure to separate the metal ions in the waste water sample by forming precipitates of the metal ions. The table shows the numerical values of the solubility products, Ksp, of some compounds. For example, the solubility product of calcium chloride, Ksp = [Ca²⁺][Cl⁻]² = 2 × 10¹ mol³ dm⁻⁹. The smaller the solubility product, the easier it is for a precipitate to form. Ksp values | | Cl⁻ | CO₃²⁻ | S²⁻ | |:---|:---|:---|:---| | Ca²⁺ | 2 × 10¹ | 5 × 10⁻⁹ | 3 × 10⁻¹⁰ | | Cu²⁺ | 1 × 10¹ | 3 × 10⁻¹⁰ | 6 × 10⁻³⁶ | | Pb²⁺ | 2 × 10⁻⁵ | 7 × 10⁻¹⁴ | 3 × 10⁻²⁸ | You are provided with * a sample of waste water containing Ca²⁺(aq), Cu²⁺(aq) and Pb²⁺(aq), * HCl(aq), * (NH₄)₂CO₃(aq), * (NH₄)₂S(aq). No other reagents should be used. Standard laboratory equipment is available.
- (a)The flowchart below is provided to plan the order of steps for the separation by filtration of the precipitates from the sample of waste water. Complete the flowchart. For each step state the reagent added and the substance(s) removed by filtration. [Figure 1.0 - Flowchart showing step 1, step 2, step 3 with reagent added and substance(s) removed by filtration][3]
- (b)After the substances formed in each step in (a) have been removed by filtration, a further drop of the reagent used for that step is added to the waste water sample. Suggest why this is necessary.[1]
- (c)Between steps 1 and 2, the waste water sample is neutralised. This is so that steps 2 and 3 will work. Suggest a reagent that should be added to neutralise the waste water sample. State how you could test that the waste water sample had been neutralised. reagent test[2]
- (d)(i)The student plans to calculate the concentration of X²⁺ ions present in this sample of waste water by measuring the mass loss on heating the freshly filtered sample of XCO₃(s). Draw and label a diagram of the experimental set-up the student should use. Your diagram should show how loss of solid during heating would be prevented.[2]
- (d)(ii)The student weighs the XCO₃ precipitate and records its mass. The student then heats the precipitate strongly for five minutes and weighs it again. The student records the difference in mass and from this calculates [X²⁺]. The precipitate thermally decomposes according to the following equation. heat XCO₃(s) ––––→ XO(s) + CO₂(g) Identify two problems with this method. Explain the effect that each problem has on the calculated concentration of X²⁺. problem 1 effect 1 problem 2 effect 2[4]
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Mark scheme
Marking points from the official mark scheme (Oct/Nov 2018). The mark or mark type is shown in brackets.
- [3] M1 = PbCl2
- [3] M2 Step 2 (NH4)2S and Step 3 (NH4)2CO3
- [3] M3 Step 2 CuS removed by (NH4)2S and step 3 CaCO3 removed by (NH4)2CO3
- [1] To remove any unreacted (cat)ions
- [2] M1 Any group 1 hydroxide or NH4OH
- [2] M2 pH meter and pH 7 OR Suitable indicator (which changes colour) and when solution is neutral
- [2] M1 (Solid in a) crucible and heat source
- [2] M2 lid and suitable label for lid
- [4] M1 Precipitate not dry
- [4] M2 (Too much mass loss so) higher calculated [X²+]
- [4] M3 Decomposition incomplete
- [4] M4 (Too little mass loss so) lower calculated [X2+]
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