Analytical Techniques

First year, Semester 2

Preparation of standard solution, primary standard and secondary standard

Standard solutions are solutions of known concentration used in chemical analysis. They are crucial for quantitative analyses, such as titrations, where they serve as the reference to determine the unknown concentration of an analyte. There are two types of standards: primary and secondary standards.

Preparation of Standard Solutions

Steps for Preparing a Standard Solution

  1. Choosing the Solute:

    • Select the appropriate substance (solute) to prepare the standard solution. This can be a primary standard or a solute that can be standardized against a primary standard.
  2. Weighing the Solute:

    • Accurately weigh the required amount of solute using an analytical balance.
  3. Dissolving the Solute:

    • Dissolve the weighed solute in a small amount of solvent (usually distilled or deionized water) in a beaker.
  4. Transferring to a Volumetric Flask:

    • Transfer the solution to a volumetric flask using a funnel. Rinse the beaker and funnel with the solvent and add these rinsings to the flask to ensure all the solute is transferred.
  5. Diluting to the Mark:

    • Add solvent to the volumetric flask until the bottom of the meniscus is at the calibration mark on the neck of the flask. Ensure thorough mixing by inverting the flask several times.
  6. Labeling:

    • Label the flask with the concentration and the date of preparation.

Primary Standards

Characteristics of Primary Standards

A primary standard is a highly pure, stable, non-hygroscopic compound with a high molar mass, which allows for precise weighing. It should react completely and predictably with the analyte. Examples include sodium carbonate (Na₂CO₃) for acid-base titrations and potassium dichromate (K₂Cr₂O₇) for redox titrations.

Preparation of Primary Standards

  1. Selection:

    • Choose a suitable primary standard compound based on the type of analysis.
  2. Purity Verification:

    • Verify the purity of the primary standard, usually 99.9% or higher.
  3. Weighing:

    • Accurately weigh the primary standard on an analytical balance.
  4. Dissolution:

    • Dissolve the weighed primary standard in a small amount of solvent in a beaker.
  5. Transfer and Dilution:

    • Transfer the solution to a volumetric flask, rinse the beaker and funnel, and dilute to the mark with solvent.
  6. Labeling:

    • Label the flask appropriately.

Secondary Standards

Characteristics of Secondary Standards

A secondary standard is a solution whose concentration is determined by titration against a primary standard. Secondary standards are less pure and stable than primary standards but are used because the primary standard might not be suitable for direct use in all titrations.

Preparation of Secondary Standards

  1. Preparation:

    • Prepare a solution of approximate concentration by weighing the solute and dissolving it in the solvent, similar to the preparation of a standard solution.
  2. Standardization:

    • Standardize the prepared solution by titrating it against a primary standard solution.
    • Calculate the exact concentration of the secondary standard using the titration data.
  3. Labeling:

    • Label the flask with the exact concentration and date of standardization.

Example Procedures

Preparation of a Sodium Carbonate (Na₂CO₃) Primary Standard Solution

  1. Weighing: Weigh accurately 1.325 g of anhydrous sodium carbonate (Na₂CO₃).

  2. Dissolution: Dissolve the Na₂CO₃ in a small amount of distilled water in a beaker.

  3. Transfer and Dilution: Transfer the solution to a 250 mL volumetric flask, rinse the beaker and funnel, and dilute to the mark with distilled water.

  4. Mixing: Mix thoroughly by inverting the flask several times.

  5. Labeling: Label the flask with the concentration and date.

Preparation of a Hydrochloric Acid (HCl) Secondary Standard Solution

  1. Preparation: Prepare approximately 0.1 M HCl by diluting concentrated HCl with distilled water in a volumetric flask.

  2. Standardization: Standardize the HCl solution by titrating it against the primary standard Na₂CO₃ solution.

    • Use the reaction: Na2CO3+2HCl2NaCl+H2O+CO2Na2CO3 +  2HCl  →  2NaCl   +  H2O  +  CO2
  3. Calculation: Calculate the exact concentration of the HCl solution using the titration data.

  4. Labeling: Label the flask with the exact concentration and date of standardization.

The preparation of standard solutions, primary standards, and secondary standards is fundamental in quantitative chemical analysis. Primary standards provide the basis for accurate and precise measurements due to their high purity and stability. Secondary standards, standardized against primary standards, offer practical solutions for routine analysis. Proper preparation, standardization, and labeling ensure the reliability and accuracy of analytical results.

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