5.3.2 Tests for ions
Syllabus
(a) qualitative analysis of ions on a test-tube scale: processes and techniques needed to identify the following ions in an unknown compound:
(i) anions: CO32–, Cl –, Br–, I–, SO42–
(ii) cations: NH4 +; Cu2+, Fe2+, Fe3+, Mn2+, Cr3+
What does this mean?
If you haven't worked it out yet, quantitative analysis involves "amounts of stuff" (quantities) - in other words mole calculations (yay!)
Qualitative analysis doesn't involve amounts, it investigates what is in substance by looking at how it reacts (its qualities, if you like)
A lot of these twests will be familiar from GCSE and AS and some from the earlier part of this Module.
I'm going to repeat them anyway, because I'm like that.
Anions
Ammonium (NH4+)
The key to identifying Ammonium ions is that they easily break down into Ammonia gas and we can then test for that.
Add Sodium Hydroxide
Warm the mixture
Ammonium ions + Hydroxide ions → Ammonia + Water
NH4+ (aq) + OH- (aq) → NH3 (g) + H2O (l)
Ammonia gas makes damp red litmus paper turn blue
If you still were uncertain you could hold a bottle of Concentrated HCl over the mixture and look for white smoke
NH3 (g) + HCl (g) → NH4Cl(s)
On a reasonably warm day and with a solution containing concentrated Ammonium ions you wouldn't even need the first few steps
Transition Metal ions
As previously discussed Transition Metal solutions exist as hexaqua complexes
Here the overall charge is the charge of the central ion because the ligands are neutral water molecules.
For the purposes of qualitative testing, however, the examiners are usually be prepared to accept Fe2+(aq) or Fe2+(aq).
Again, the previous chapters explain that the OH- ions remove H+ ions from water ligands in an acid-base reaction.
And that they do this until the complex becomes neutral, at which point it will precipitate.
[Fe(H2O)6]2+ (aq) + 2 OH-(aq) --> [Fe(H2O)4(OH)2] (s) + 2 H2O (l)
and
[Fe(H2O)6]3+ (aq) + 3 OH-(aq) --> [Fe(H2O)3(OH)3] (s) + 3 H2O (l)
But, again, the examiner will accept;
Fe2+(aq) + 2 OH-(aq) --> Fe(OH)2 (s) Fe3+(aq) + 3 OH-(aq) --> Fe(OH)3 (s)
So all we really need to do is substitute the symbol for the metal ion under consideration and try to recall the likely colours of the solution we start with and the precipitates we will make.
(*) Colours of solutions are dependent on concentration.
Note: details of behaviour with excess OH- /NH3 may be required and are covered in the previous chapter.
Cations
Halide ions (Cl-,Br-,I-)
Add dilute Nitric Acid
Add Silver Nitrate solution
Note colour of precipitate:Chloride = White, Bromide = Cream, Iodide = Yellow
Ag+ (aq) + X- (aq)--> AgX(s)
Add dilute Ammonia solution, Chloride precipitate will dissolve
Add concentrated Ammonia solution, Bromide precipitate will dissolve
Note: The Nitric acid removes and CO2 that has dissolved to form Carbonate ions which would also precipitate
If you were sure you had a halide solution and it didn't precipitate then you can assume that it is a Fluoride solution.
The ammonia re-dissolving is a chance to confirm your suspicions if the colour of precipitates are not absolutely clear.
Sulphate ions (SO42-)
You may remember that Barium Sulphate is insoluble.
So if you mix a solution of Barium Nitrate (all nitrates being soluble) with an unknown solution a white precipitate of Barium Sulphate may form.
Ba2+(aq) + SO42-(aq) --> BaSO4 (s)
Carbonate ions (CO32-)
Carbonates react with acids to produce Carbon Dioxide
Carbonate + Acid --> Salt + Water + Carbon Dioxide.
So, if you suspected that your unknown substance was a Carbonate (it would most likely be a solid, although Sodium, Potassium and ammonium Carbonates can be solutions) you could add a dilute acid like Nitric Acid.
Any bubbles would suggest that you were correct (although the unknown might still have been a Hydrogen Carbonate)
The ionic equitation for this would be:
2H+ (aq) + CO32-(aq/s) --> H2O(l) + CO2(g)
Note: A level examinmaers don't want your observations to be that "CO2 will form".
They want you to say "bubbles/effervescence or even fizzing will be observed" - because you don't know that it is CO2 unless you prove it but you can see that they are bubbles.