Qualitative analysis of cations and quantitative

analysis of anion chloride

I. Introduction
The main objective of this experiment was to check the presence of some compounds by using
precipitation reactions and further filtration to separate one ion from others. In this experiment,
we also had to determine the concentration of chloride by volumetric titration.

II. Material
 Erlenmeyer
 (250 ml).
 2 beaker (150 ml and 250 ml)
 Graduated cylinder (20ml-50 ml)
 Funnel
 Burette (50 ml)
 Chemicals: silver nitrate solution (0.1n), HCl solution (0.1n)
 Problem solutions
 Indicator: potassium chromate
 Distilled water
 Wash bottle
 Bunsen
 Wire gauze and tripod stand
 Test tube clamps
 Erlenmeyer clamps

III. Procedure

1. Qualitative analysis of a mixture of silver group cations

1.1. Take 12 ml of the problem solution in a small tube.
1.2. Add drop by drop a small volume of HCl 0,1M to the problem solution.
1.3. Filtrate the mixture and save the residue.
1.4. Pass around 2 ml of boiling water through the filter paper containing the residue
and save the filtrate and the residue. Wash the residue twice with 2 ml of boiling
water and collect.
1.5. Take two different aliquots of around 2-3 ml of the filtrate and perform two
different tests for lead (II) identification.
1.5.1. Add few drops of potassium chromate in the first tube.
1.5.2. Add few drops of potassium iodide in the second tube.
1.6. Pass around 2 ml of NH3 0.1 M through the residue over the filter.
1.6.1. Add some drops of HNO3 to the filtrate and look for a white precipitate to
check the presence of silver.
 1.6.2. Test for mercury cation in the residue looking for a black or grey finely
divided solid and a white solid over the filter paper.
2. Titration of chloride against silver nitrate
2.1. Prepare the titrant solution (accurately measured 20 ml) by adding a few drops of
potassium chromate.
2.2. Perform the titration of the solution with the titrant: silver nitrate by using manual
agitation up to the equivalence point.

IV. Results & Discussion

1. Qualitative analysis of a mixture of silver group cations:
Solution + HCl

ADD HOT
WATER

FILTRATE PRECIPITATE

ADD NH3

FILTRATE PRECIPITATE

Check the
presence of
Pb FILTRATE PRECIPITATE

Check the Check the

presence of presence of
Ag Hg

Following the steps in the charts we found the following components:

- Lead Pb: We took the filtrate after adding hot water and we divided it between two
tubes.
 In the first tube, we added few drops of potassium chromate. The chromate ion,
CrO4 2-, combined with lead (II) and formed a bright yellow, insoluble solid lead
(II) chromate, PbCrO4.
Pb2+ + CrO4 2- → PbCrO4

 In the second tube, we added few drops of potassium iodide. Pb2+ precipitated
as PbI2, lead iodide, a slightly soluble yellow precipitate.
 Pb2+ + 2I-→ PbI2

- Silver Ag: We took the filtrate after adding NH3.

 We added some drops of HNO3 to the filtrate and the H+ from nitric acid reacted
with ammonia to form the very stable NH4+ and the free Ag+ will reacted with the
Cl-1 still in solution and precipitates again as AgCl (white): Ag+ + Cl- → AgCl

2. Titration of chloride against silver nitrate

We perform the titration using tap water, using the potassium chromate indicator K2CrO4.
The titrant is silver nitrate: AgNO3 → Ag+ + NO3-
The tap water has chloride which reacts with the silver ions: Ag+ + Cl- → AgCl (white
precipitate)
→ Find the concentration of chloride:
[AgNO3]∙ VAdded= [Cl-]∙Vinitial
[Cl-]=[AgNO3]∙ VAdded/ Vinitial
[Cl-]=0, 1∙ 50/ 2
[Cl-]=2.5 mol/l
N.B: When we don’t have any chloride left (when we go beyond the equivalence point) the silver
ions will react with the chromate ions and thus the colour of the solution will change to
brown/orange.
3. Discussion
From this experiment we notice that lead, silver and mercury can be precipitated by the addition
of HCl, and this is the reason why we added it to the problem solution.
Silver, lead, and mercury have different solubility. Lead is more soluble as we could get it in the
filtrate just by the addition of boiling water (from the table we can see that it has a solubility of 1).
Mercury and silver are less soluble than lead, in order to dissolve them we need to add ammonia
NH3.
Reactions taking place for identification of the isolated cations:
Lead:
 Pb2+ + CrO4 2- → PbCrO4
 Pb2+ + 2I-→ PbI2
Silver:
 Ag+ + Cl- → AgCl
Mercury:
 Hg2Cl2 + 2 NH3→ HgClNH2(s) + Hg(s) + NH4Cl(aq)
 V. Conclusion
If one has a mixture of a large number of ions, the usual approach is to use a chemical method to
separate the mixture into subgroups that consist of just a few ions. Then it may be possible to
test for one particular ion in the presence of just one or two others. Alternatively, each subgroup
of just a few ions may be separated further so that each ion in the subgroup ends up in a different
test tube where its presence can be confirmed by other chemical tests.