Chapter 15 – Chemical Analysis

‘O’ Level Chemistry

Chapter 15 – Chemical Analysis

Qualitative Analysis
 Physical Tests
- Colour: some substances have distinctive colours

Compounds of Colour
White solid.
Ammonium, Group I and II elements
Colourless solution when dissolved.
Copper (II) Blue or green. (except CuO – black)
Iron (II) Pale green / dirty green
Iron (III) Red / brownish / yellowish

- Smell

Odourless Characteristic smells

H2, O2, CO2 Cl2, NH3, SO2

- Solubility in water: a useful criterion to eliminate substances. Refer to the table on

solubility of bases and salts
- pH in previous chapter.

 Chemical Tests
- Test for Cations: uses aqueous sodium hydroxide and aqueous ammonia

1 Add NaOH (aq) Na+ / K+

No

ppt formed? No On warming produces Yes

pungent gas that turns NH4+
moist red litmus blue
Yes

White ppt Blue ppt Green ppt Reddish brown ppt

Cu2+ Fe2+ Fe3+

ppt dissolves in
excess NaOH? No
Ca2+

Yes

Al3+ / Pb2+ / Zn2+

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 Chapter 15 – Chemical Analysis

2 Add NH3 (aq)

No
ppt formed? NH4+ / Ca2+

Yes

White ppt Blue ppt Green ppt Reddish brown ppt

Cu2+ Fe2+ Fe3+

No Forms yellow ppt No Al3+

ppt dissolves in Al3+ / Pb2+
with KI (aq)
excess NH3 ?
Yes
Yes

Zn2+ Pb2+

- Test for Anions

Anion Test Observations

Add NaOH (aq), then add a little aluminium A colourless, pungent gas that turns damp red litmus paper
NO3-
powder. Warm. blue is formed. The gas is NH3.
A colourless, odourless gas which forms a white ppt with
CO32- Add HCl (aq)
limewater is formed. The gas is CO2.
Cl- Add dil HNO3 (aq), then AgNO3 (aq) A white ppt of AgCl is formed.
I- Add dil HNO3 (aq), then Pb(NO3)2 (aq) A yellow ppt of PbI2 is formed.
SO42- Add dil HNO3 (aq), then Ba(NO3)2 (aq) A white ppt of BaSO4 is formed.
*Dilute nitric acid is added to remove other anions (carbonate ions) which might also give a ppt with the reagent.

- Test for Gases

Gas Test Observations

NH3 Damp red litmus paper. Damp red litmus paper turns blue.
CO2 Bubble gas through limewater. A white ppt is formed in limewater.
Cl2 Damp blue litmus paper. Blue litmus paper is bleached.
H2 Put a lighted wooden splint near the gas. Lighted splint extinguishes with a ‘pop’ sound.
O2 Put a glowing splint near the gas. Glowing splint is relighted.
Place a drop of aq. acidified potassium
Acidified orange potassium dichromate (VI) paper turns
SO2 dichromate (VI) on a piece of filter paper, and
green.
then place it in the gas.

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 Chapter 15 – Chemical Analysis

- Test for Water

Substance Test Observations

Water Blue cobalt (II) chloride paper. Blue paper turns pink.

Quantitative Analysis (Volumetric Analysis)

 Acid-Alkali Titrations
- An alkali is added to a fixed volume of acid. (or vice versa)
- One of these solutions is a standard solution.
- Standard solution: a solution of known concentration.
- End point: the point at which neutralisation is complete.
 Using indicators to detect end point.
 Phenolphthalein and methyl orange give a sharp change in colour at the end point.
 Litmus and universal indicator are not used as the colour change at the end point is not sharp (i.e. not distinct).

Exercise 1
20 cm3 of an unknown concentration of sulfuric acid is titrated with 24 cm 3 of 0.05 mol/dm3 sodium hydroxide.
Phenolphthalein is used as the indicator.
(a) Describe the apparatus and steps used for this titration. State the changes in the colour of the solution
during the titration.
(b) Calculate the concentration of sulfuric acid.
Solution:
(a) 1. Draw 20 cm3 of sulfuric acid into a pipette with pipette filler. Place the acid into a titration flask.
2. Add 2 to 3 drops of phenolphthalein indicator. The colour of the solution remains colourless.
3. Fill the burette with the 0.05 mol/dm3 sodium hydroxide solution.
4. Run the alkali into the titration flask until the indicator changes from colourless to pink. Record the volume of the
sodium hydroxide used.
(b) Step 1: Write a balanced chemical equation for the reaction.
H2SO4 + 2NaOH  Na2SO4 + 2H2O
Step 2: Start your calculation with the standard solution.
No. of moles of NaOH used = 0.05 mol/dm3 x 0.024 dm3 = 0.0012 mol
Step 3: From the equation, find the ratio of the no. of moles of the acid: no. of moles of alkali
Ratio of H2SO4 to NaOH = 1 : 2
Step 4: Find the no. of moles of acid used using the ratio in step 3
Thus, no. of moles of H2SO4 used = ½ x no. of moles of NaOH = 0.0006 mol
Step 5: Calculate the concentration of H2SO4 used
Concentration of H2SO4 used = 0.0006 mol / 0.02 dm3 = 0.03 mol/dm3

 Other Titrations
- Titration can also be carried out with solutions other than acid and alkali.
- Example: To find the concentration of iodine using a standard solution of sodium thiosulfate solution,
Na2S2O3 (aq)
- Example: To find the concentration of iron (II) sulfate solution using a standard solution of potassium
manganate (VII).

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Exercise 2
An unknown concentration of iron (II) sulfate solution required 25 cm 3 of 0.01 mol/dm3 acidified potassium
manganate (VII) for reaction in a titration. Given that 20 cm 3 of iron (II) sulfate is used, calculate the
concentration of the iron (II) sulfate solution. (5 mol of iron (II) sulfate solution react with 1 mol of acidified
potassium manganate (VII) solution.)
Solution:
No. of moles of KMnO4 = 0.025 dm3 x 0.01 mol/dm3 = 0.00025 mol
Ratio of FeSO4 to KMnO4 = 5 : 1
No. of moles of FeSO4 = 5 x 0.00025 mol = 0.00125 mol
Concentration of FeSO4 = 0.00125 mol / 0.02 dm3 = 0.0625 mol/dm3

 Uses of Titrations in Analysis

- Identification of Acids and Alkalis
 when known concentrations of both solutions are titrated
- Determine Percentage Purity of Compounds
 when an impure sold is dissolved in a solution and titrated with a standard solution
- Determine Formulae of Compounds
- Calculate the Number of Reacting Moles in an Equation

Exercise 3
An unknown solution of an alkali, MOH, is neutralised with sulfuric acid in a titration.
Given that 20 cm3 of 3.5 g/dm3 MOH is titrated with 25 cm3 of 0.025 mol/dm3 sulfuric acid,
(a) Calculate the relative molecular mass of MOH.
(b) Suggest the identity of the unknown alkali, MOH.
Solution:
(a) H2SO4 + 2MOH  M2SO4 + 2H2O
No. of moles of H2SO4 reacted = 0.025 dm3 x 0.025 mol/dm3 = 0.000625 mol
Ratio of MOH to H2SO4 = 2 : 1
No. of moles of MOH reacted = 2 x 0.000625 mol = 0.00125 mol
Mass of MOH reacted = 0.02 dm3 x 3.5 g/dm3 = 0.07 g
Molar mass of MOH = 0.07 g / 0.00125 mol = 56 g mol-1
Thus, Mr of MOH = 56
(b) Let x be Ar of M, x + 16 +1 = 56
x = 39 (potassium has Ar of 39)
Thus, MOH is potassium hydroxide.

Exercise 4
10.0 g of an impure nitric acid is dissolved in 500 cm3 of water. 15 cm3 of this acid solution required 20 cm3 of
0.125 mol/dm3 sodium hydroxide for neutralisation. Calculate the percentage purity of the nitric acid.
Solution:
HNO3 + NaOH  NaNO3 + H2O Mass of HNO3 reacted = 0.0025 x 63 = 0.1575 g
No. of moles of NaOH reacted Concentration of the impure acid = 10 g / 0.5 dm3
= 0.02 dm3 x 0.125 mol/dm3 = 0.0025 mol = 20 g/dm3
No. of moles of HNO3 used in the neutralisation Mass of impure HNO3 in 15 cm3 of the acid solution
= 0.0025 mol = 20 g/dm3 x 0.015 dm3 = 0.3 g
Mr of HNO3 = 1 + 14 + 3(16) = 63 % purity of HNO3 = (0.1575 / 0.3) x 100 % = 52.5 %

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Exercise 5
A dibasic acid has the formula, H2C2O4.nH2O. 6.48 g of this acid dissolves in 0.8 dm 3 of water to give
solution X. 20 cm3 of solution X required 25 cm3 of 0.01 mol/dm3 sodium hydroxide in a titration.
(a) Calculate the concentration of the dibasic acid in mol/dm3.
(b) Find the value of n.
Solution:
(a) Ratio of dibasic acid : NaOH = 1 : 2.
No. of moles of NaOH = 0.025 dm3 x 0.01 mol/dm3 = 0.00025 mol
No. of moles of dibasic acid = 0.00025 mol x 2 = 0.0005 mol
Concentration of dibasic acid in mol/dm3= 0.0005 mol / 0.02 dm3 = 0.025 mol/dm3
(b) Concentration of dibasic acid in solution X in g/dm3 = 6.48 g / 0.8 dm3 = 8.1 g/dm3
Molar mass of H2C2O4.nH2O = 8.1 g / 0.025 mol = 324 g mol-1
[2(1) + 2(12) + 4(16)] + n (2 + 16) = 324
90 + 18n = 324
n = 13

Exercise 6
In a titration, 25 cm3 of 5.1 g/dm3 iodine solution reacted with 29 cm3 of 0.036 mol/dm3 sodium
thiosulfate solution. The chemical equation of the reaction is: x I 2 (aq) + y Na2S2O3 (aq)  products
Find the values of x and y.
Solution:
Mr of I2 = 2 x 127 = 254
Concentration of I2 in mol/dm3 = 5.1 g/dm3 ÷ 254 = 0.02008 mol/dm3
No. of moles of I2 reacted = 0.02008 mol/dm3 x 0.025 dm3 = 0.000502 mol
No. of moles of Na2S2O3 reacted = 0.029 dm3 x 0.036 mol/dm3 = 0.001044 mol
Ratio of I2 : Na2S2O3 = 0.000502 : 0.001044 ≈ 1 : 2
Therefore, x = 1 and y = 2.

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