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Analysis of Ammonium Sulphate ((NH₄)₂SO₄)

Class 12 Chemistry Practical

Aim

To analyse the given inorganic salt for one acidic and one basic radical.

Preliminary Test

ExperimentObservationInference
Physical examinationWhite crystalline solid; ammoniacal smellAmmonium salt, not odourless
SolubilitySoluble in waterUnlike BaSO₄ / PbSO₄
Dry heatingMay give NH₃; residue can leave sulphateAmmonium sulphate
Dilute H₂SO₄No CO₂ / H₂S / SO₂Not carbonate / sulphide / sulphite
Conc. H₂SO₄No halide fumesNot Cl⁻ / Br⁻ / I⁻
Flame testNo characteristic colourNot Ba / Ca / Sr

Test of Anion (SO₄²⁻)

ExperimentObservationInference
Confirmatory Tests
Barium chloride
Acidify the water / soda extract with dilute HCl and add BaCl₂
White ppt of BaSO₄, insoluble in conc. HCl and conc. HNO₃SO₄²⁻ is confirmed
Lead acetate
Acidify with acetic acid and add lead acetate
White ppt of PbSO₄SO₄²⁻ is confirmed

Ionic equations

  • Ba²⁺ + SO₄²⁻ → BaSO₄ ↓ (white, insoluble in acids)
  • Pb²⁺ + SO₄²⁻ → PbSO₄ ↓

Test of Cation (NH₄⁺)

ExperimentObservationInference
Heat the salt with NaOH solutionAmmoniacal smell; gas turns red litmus blueNH₄⁺ may be present (Group 0)
Bring a glass rod dipped in conc. HCl near the mouth of the tubeDense white fumes of NH₄ClNH₄⁺ may be present
Confirmatory Test
Nessler’s reagent
Pass the gas into Nessler’s reagent (K₂[HgI₄] in KOH)
Brown colouration or brown ppt of basic mercury(II) amidoiodideNH₄⁺ is confirmed. Stop cation analysis here for ammonium salts.

Ionic equations

  • NH₄⁺ + OH⁻ → NH₃ ↑ + H₂O
  • NH₃ + HCl → NH₄Cl (white fumes)
  • 2K₂[HgI₄] + 3KOH + NH₃ → H₂N–Hg–O–Hg–I ↓ + 7KI + 2H₂O

Result

The given salt contains NH₄⁺ as the cation (basic radical) and SO₄²⁻ as the anion (acidic radical). The salt is Ammonium Sulphate ((NH₄)₂SO₄).

Precautions

  1. Use small quantities of salt and reagents; do not use excess.
  2. Keep the mouth of the test tube away from the face while heating.
  3. Use freshly prepared FeSO₄ for the brown ring test.
  4. Nessler’s reagent is toxic (mercury); handle with care and do not pipette by mouth.

Viva voce

  1. Why is BaSO₄ insoluble in conc. HCl while BaSO₃ dissolves?

    BaSO₄ is a highly insoluble sulphate; sulphite ppt dissolves with evolution of SO₂.

  2. Why acidify before adding BaCl₂?

    To destroy carbonate / sulphite which would also give a white barium ppt.

  3. Why Nessler for this salt?

    To confirm the ammonium cation after NaOH liberates NH₃.

  4. Why no brown ring?

    The anion is sulphate, not nitrate.

  5. Why Group 0 before sulphate tests?

    Anion tests can be done on soda extract; ammonium is still tested on the original salt with NaOH.

  6. Why scratch not needed here unlike Mg?

    Sulphate ppt with BaCl₂ comes at once; MgNH₄PO₄ is slow and needs scratching.

  7. Is (NH₄)₂SO₄ used in Group IV?

    No. Group IV uses (NH₄)₂S / H₂S in ammoniacal medium. Different salt.

  8. Why white ppt with lead acetate?

    PbSO₄ is insoluble.