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Home Chemistry Chemistry Class 11 Preparation of a standard solution of oxalic acid
Chemistry Class 11

Preparation of a standard solution of oxalic acid



Preparing a standard solution is a fundamental skill in analytical chemistry that every student must master. This comprehensive guide covers the preparation of a standard solution of oxalic acid through a detailed laboratory experiment verification.

Aim

To prepare a standard solution of oxalic acid (0.1M) and verify its concentration through titration with standardized sodium hydroxide solution.

Apparatus Required

Glassware and Equipment:

  • Weighing bottle or watch glass
  • 250 mL volumetric flask
  • Funnel (small)
  • Glass rod
  • Wash bottle
  • Dropper
  • 100 mL measuring cylinder
  • Burette (50 mL)
  • Pipette (25 mL)
  • Conical flask (250 mL) - 3 pieces
  • White tile or white background sheet
  • Analytical balance

Chemicals Required:

  • Oxalic acid dihydrate (H₂C₂O₄·2H₂O) - A.R. grade
  • Standardized sodium hydroxide solution (0.1M)
  • Phenolphthalein indicator

Theory

What is a Standard Solution?

A standard solution is a solution whose concentration is precisely known. It serves as a reference for quantitative analysis in titrations and other analytical procedures.

Why Oxalic Acid?

Oxalic acid dihydrate is chosen for standard solution preparation because:

  • It is a primary standard substance
  • Available in pure crystalline form
  • Stable in air and does not absorb moisture
  • Has a high equivalent weight, reducing weighing errors
  • Reacts stoichiometrically with bases

Chemical Reaction:

H₂C₂O₄ + 2NaOH → Na₂C₂O₄ + 2H₂O

The reaction shows that one mole of oxalic acid reacts with two moles of sodium hydroxide.

Calculation Formula:

Molarity (M) = (Weight of solute × 1000) / (Molecular weight × Volume in mL)

For oxalic acid dihydrate: Molecular weight = 126 g/mol

Procedure

Part A: Preparation of Standard Oxalic Acid Solution

  1. Weighing: Accurately weigh about 1.575 g of oxalic acid dihydrate crystals in a clean, dry weighing bottle using an analytical balance.

  2. Transfer: Transfer the weighed crystals carefully into a clean 250 mL volumetric flask through a funnel.

  3. Washing: Wash the weighing bottle and funnel with distilled water, ensuring all crystals are transferred to the flask.

  4. Dissolution: Add about 150 mL of distilled water to the flask and shake well to dissolve the crystals completely.

  5. Volume Adjustment: Add more distilled water slowly up to the calibration mark of the volumetric flask. The bottom of the meniscus should touch the mark.

  6. Mixing: Stopper the flask and invert it several times to ensure uniform mixing.

Part B: Verification by Titration

  1. Pipette: Using a pipette, transfer exactly 25 mL of the prepared oxalic acid solution into a clean conical flask.

  2. Indicator: Add 2-3 drops of phenolphthalein indicator to the solution.

  3. Burette Setup: Fill the burette with standardized 0.1M NaOH solution and record the initial reading.

  4. Titration: Slowly add NaOH solution from the burette to the conical flask while constantly swirling. Continue until a permanent pink color appears.

  5. End Point: The endpoint is reached when the pink color persists for at least 30 seconds.

  6. Repeat: Perform the titration three times and record the readings.

Observation Table

Titration No. Initial Burette Reading (mL) Final Burette Reading (mL) Volume of NaOH used (mL)
1 0.00 24.80 24.80
2 0.00 24.85 24.85
3 0.00 24.82 24.82

Concordant Reading: 24.82 mL (average of three readings)

Result

Calculations:

  1. Expected Molarity of Oxalic Acid Solution:

    • Weight taken = 1.575 g
    • Volume = 250 mL
    • Molecular weight of H₂C₂O₄·2H₂O = 126 g/mol
    • Molarity = (1.575 × 1000) / (126 × 250) = 0.05M
  2. Verification using Titration Data:

    • Volume of oxalic acid taken = 25 mL
    • Volume of NaOH used = 24.82 mL
    • Molarity of NaOH = 0.1M
    • Using formula: M₁V₁ = M₂V₂ (considering n-factor)
    • For oxalic acid: n-factor = 2
    • 0.1 × 24.82 = 2 × M₂ × 25
    • M₂ = (0.1 × 24.82) / (2 × 25) = 0.0496M (≈ 0.05M)

Conclusion: The prepared oxalic acid solution has a molarity of 0.05M, confirming successful preparation of standard solution.

Precautions

  1. Accurate Weighing: Use analytical balance for precise weighing of oxalic acid crystals.

  2. Proper Transfer: Ensure complete transfer of crystals to avoid concentration errors.

  3. Meniscus Reading: Always read the burette at eye level, taking the bottom of the meniscus.

  4. End Point Detection: Add NaOH drop by drop near the endpoint for accurate results.

  5. Clean Glassware: Use clean and dry glassware to prevent contamination.

  6. Proper Mixing: Mix the final solution thoroughly by inverting the volumetric flask multiple times.

  7. Storage: Store the prepared solution in a properly labeled bottle.

Viva Voce Questions and Answers

Q1: Why is oxalic acid dihydrate preferred for standard solution preparation?

A: It is a primary standard substance, available in pure form, stable in air, and has high molecular weight reducing weighing errors.

Q2: What is the molecular weight of oxalic acid dihydrate?

A: The molecular weight is 126 g/mol (H₂C₂O₄·2H₂O).

Q3: Why is the solution mixed thoroughly before final volume adjustment?

A: Thorough mixing ensures uniform concentration throughout the solution.

Q4: What is the significance of the meniscus in volumetric measurements?

A: Meniscus provides accurate volume measurement as liquids form a curved surface in glass containers.

Q5: Why should the funnel be removed before making up to the mark?

A: To prevent any additional liquid from the funnel from affecting the final volume measurement.

Q6: How do you calculate the molarity of prepared solution?

A: Molarity = (Weight × 1000) / (Molecular weight × Volume in mL)

Q7: What is the role of phenolphthalein indicator?

A: It changes color from colorless to pink at the endpoint, indicating completion of neutralization reaction.

Q8: Why is distilled water used instead of tap water?

A: Distilled water is free from impurities that could interfere with the analysis or affect solution concentration.


This comprehensive guide provides everything needed for successful preparation and verification of a standard oxalic acid solution. The experiment demonstrates fundamental principles of analytical chemistry while developing essential laboratory skills for chemistry students.






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