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Home Chemistry Chemistry Class 12 Preparation of a double salt—either ferrous ammonium sulphate (Mohr’s salt) or potash alum
Chemistry Class 12 Lab Experiments

Preparation of a double salt—either ferrous ammonium sulphate (Mohr’s salt) or potash alum



Complete experimental guide for preparing double salts in chemistry laboratory with detailed procedure and observations


Introduction

The preparation of double salts represents a fundamental practical in inorganic chemistry laboratories. This experiment demonstrates the formation of complex salts through the combination of two simple salts, creating compounds with distinct properties and enhanced stability. Two common examples include ferrous ammonium sulfate (Mohr's salt) and potash alum, both essential compounds in analytical and industrial applications.

Aim

To prepare and crystallize double salts:

  • Ferrous ammonium sulfate (Mohr's salt): (NH₄)₂Fe(SO₄)₂·6H₂O
  • Potash alum: K₂SO₄·Al₂(SO₄)₃·24H₂O

And to verify their formation through systematic analysis.

Apparatus Required

Glassware and Equipment

  • Beakers (250 mL and 400 mL)
  • Conical flask (250 mL)
  • Glass rod for stirring
  • Funnel
  • Filter paper
  • Weighing bottle
  • Watch glass
  • Bunsen burner
  • Tripod stand with wire gauze
  • Evaporating dish
  • Buchner funnel (optional)

Chemicals Required

For Mohr's Salt Preparation:

  • Ferrous sulfate heptahydrate (FeSO₄·7H₂O)
  • Ammonium sulfate [(NH₄)₂SO₄]
  • Concentrated sulfuric acid (H₂SO₄)
  • Distilled water

For Potash Alum Preparation:

  • Potassium sulfate (K₂SO₄)
  • Aluminium sulfate [Al₂(SO₄)₄·18H₂O]
  • Distilled water

Theory

Double Salt Formation

Double salts are molecular compounds formed when two simple salts crystallize together in stoichiometric proportions. Unlike complex salts, double salts dissociate completely into simple ions when dissolved in water.

Mohr's Salt Formation:

FeSO₄ + (NH₄)₂SO₄ + 6H₂O → (NH₄)₂Fe(SO₄)₂·6H₂O

Potash Alum Formation:

K₂SO₄ + Al₂(SO₄)₃ + 24H₂O → K₂SO₄·Al₂(SO₄)₃·24H₂O

Chemical Properties

Mohr's Salt:

  • Pale green crystalline solid
  • Contains Fe²⁺, NH₄⁺, and SO₄²⁻ ions
  • Stable against air oxidation due to protective water of crystallization

Potash Alum:

  • Colorless octahedral crystals
  • Contains K⁺, Al³⁺, and SO₄²⁻ ions
  • Exhibits astringent properties

Procedure

Preparation of Mohr's Salt

  1. Solution Preparation:

    • Weigh 15g of FeSO₄·7H₂O in a 250mL beaker
    • Add 5mL of dilute H₂SO₄ to prevent oxidation
    • Dissolve in 100mL of distilled water with gentle heating
  2. Ammonium Sulfate Addition:

    • Weigh 7g of (NH₄)₂SO₄ separately
    • Dissolve in minimum quantity of distilled water
    • Mix both solutions thoroughly
  3. Crystallization:

    • Filter the hot solution through glass wool
    • Concentrate to about half the volume
    • Cool slowly to room temperature
    • Cool further in ice bath for complete crystallization
  4. Product Collection:

    • Filter crystals using Buchner funnel
    • Wash with small amount of cold distilled water
    • Dry between filter papers

Preparation of Potash Alum

  1. Solution Preparation:

    • Weigh 3g of K₂SO₄ and 12g of Al₂(SO₄)₃·18H₂O
    • Dissolve each salt separately in minimum water
    • Mix both solutions and heat to dissolve completely
  2. Crystallization:

    • Filter hot solution to remove impurities
    • Cool solution rapidly with constant stirring
    • Scratch glass rod against beaker wall to induce crystallization
  3. Product Collection:

    • Filter crystals and wash with cold water
    • Dry crystals between filter papers

Observation Table

Parameter Mohr's Salt Potash Alum
Color Pale green Colorless
Shape Small crystals Octahedral crystals
Solubility Soluble in water Soluble in hot water
Weight obtained ___ g ___ g
Percentage yield ___% ___%
Odor Odorless Odorless
Stability Stable in air Efflorescent

Result

The preparation of double salts was successfully accomplished with:

  • Mohr's Salt: Pale green crystals obtained with good yield
  • Potash Alum: Colorless octahedral crystals formed
  • Both compounds showed characteristic properties of double salts
  • The experimental yield was satisfactory for both preparations

Precautions

General Precautions

  1. Handle concentrated H₂SO₄ carefully - Always add acid to water, never vice versa
  2. Maintain proper ventilation during heating processes
  3. Use clean glassware to avoid contamination
  4. Control heating temperature to prevent decomposition
  5. Avoid prolonged exposure to air to prevent oxidation

Specific Precautions

For Mohr's Salt:

  • Add dilute H₂SO₄ to prevent Fe²⁺ oxidation to Fe³⁺
  • Avoid overheating during crystallization
  • Store crystals in airtight containers

For Potash Alum:

  • Ensure complete dissolution of both salts
  • Rapid cooling promotes better crystal formation
  • Handle hot solutions with care

Viva Questions and Answers

Q1: What are double salts? Give examples.

A: Double salts are molecular compounds formed by the combination of two simple salts that retain their individual properties in solid state but dissociate completely in solution. Examples include Mohr's salt [(NH₄)₂Fe(SO₄)₂·6H₂O] and potash alum [K₂SO₄·Al₂(SO₄)₃·24H₂O].

Q2: Why is H₂SO₄ added during Mohr's salt preparation?

A: Concentrated H₂SO₄ prevents the oxidation of Fe²⁺ ions to Fe³⁺ ions and maintains the acidic pH necessary for the stability of the compound.

Q3: What is the difference between double salts and complex salts?

A: Double salts dissociate completely into simple ions in solution, while complex salts contain coordinate covalent bonds and form complex ions that do not dissociate into simple ions.

Q4: Why is slow cooling preferred for Mohr's salt crystallization?

A: Slow cooling allows proper arrangement of ions in crystal lattice, resulting in well-defined crystals with better yield and purity.

Q5: What is the role of scratch crystallization in potash alum preparation?

A: Scratch crystallization provides nucleation sites for crystal formation, promoting rapid and uniform crystal growth.

Q6: Why should the solutions be filtered before crystallization?

A: Filtering removes insoluble impurities and undissolved particles that could interfere with crystal formation and affect the purity of the final product.

Q7: Explain the structure of potash alum.

A: Potash alum crystallizes in octahedral form with a highly symmetrical structure. Each K⁺ ion is surrounded by twelve water molecules, and the compound shows isomorphism with other alums.

Q8: What precautions should be taken to prevent oxidation during Mohr's salt preparation?

A:

  • Use freshly prepared FeSO₄ solution
  • Add dilute H₂SO₄ to maintain acidic medium
  • Avoid prolonged heating
  • Exclude air as much as possible during preparation

Applications

Mohr's Salt:

  • Primary standard in volumetric analysis
  • Preparation of iron compounds
  • Pharmaceutical applications

Potash Alum:

  • Water purification and treatment
  • Leather tanning industry
  • Fire extinguisher preparation
  • Styptic pencils for stopping bleeding

Conclusion

This laboratory experiment successfully demonstrates the preparation of double salts through simple crystallization techniques. The formation of Mohr's salt and potash alum illustrates fundamental principles of inorganic chemistry, including stoichiometry, crystallization, and salt formation. Proper technique and attention to experimental conditions yield high-quality crystals suitable for further analysis and practical applications.

The experiment reinforces theoretical concepts while developing essential laboratory skills in weighing, solution preparation, crystallization, and product characterization. Both double salts prepared show characteristic properties and find extensive use in analytical chemistry and industrial processes.


This comprehensive guide provides all essential information for successfully conducting the double salt preparation experiment in educational laboratory settings. Students should follow all safety protocols and seek instructor guidance when necessary.








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