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

Image result for damp red litmus
Image result for ammonia and hydrogen chloride fumes

Transition Metal ions

As previously discussed Transition Metal solutions exist as hexaqua complexes

Image result for hexaaquairon ii iii
Image result for hexaaquairon ii doc b

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.

Image result for transition metal precipitates

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.

Image result for halide ion tests

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)

Image result for barium sulfate precipitate

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.