Acedemic Notes: Experimental Chemistry and Analysis

Principles of Experimental Design

  • Stepwise Planning: Involves suggesting a hypothesis, identifying variables (independent, dependent, controlled), choosing apparatus, carrying out tests, and drawing conclusions.
  • Apparatus Choice: Selection depends on required accuracy. Digital probes (pH, temperature) offer higher resolution than manual indicators or liquid thermometers.
  • Measuring Volume: For high precision, use volumetric pipettes (fixed volume) or burettes (variable volume). Measuring cylinders are for general use.
  • Accuracy vs. Precision: Accuracy refers to how close a result is to the true value; precision refers to the consistency of repeated results.
  • Errors: Random errors are reduced by repetitions and averaging. Systematic errors (like zero errors) require apparatus calibration or adjustment.

Separation and Purification Techniques

  • Filtration: Separates insoluble solids from liquids (residue stays in paper, filtrate passes through).
  • Crystallisation: Recovers a soluble solid from a solution by evaporating the solvent.
  • Simple Distillation: Separates a solvent from a solution (e.g., pure water from seawater).
  • Fractional Distillation: Separates miscible liquids with close boiling points (e.g., ethanol and water) using a fractionating column.
  • Magnetic Separation: Used for mixtures containing magnetic metals like iron.
  • Assessing Purity: Pure substances have sharp, specific melting and boiling points (0C0\,^{\circ}\text{C} and 100C100\,^{\circ}\text{C} for water). Impurities lower the melting point and raise the boiling point, often causing melting over a range of temperatures.

Chromatography

  • Mechanism: Separates substances based on their different solubilities in a solvent and attraction to the paper.
  • Procedure: Samples are placed on a pencil baseline. The solvent must start below this line. The resulting dried paper is a chromatogram.
  • Rf Value: A ratio used to identify substances: Rf=distance moved by substancedistance moved by solvent frontR_{f} = \frac{\text{distance moved by substance}}{\text{distance moved by solvent front}}.
  • Locating Agents: Necessary for separating colourless substances (like amino acids) to make them visible under UV light or via chemical reaction.

Standard Chemical Tests

  • Cations (Metal Ions):
    • Flame Tests: Li+Li^{+} (red), Na+Na^{+} (yellow), K+K^{+} (lilac), Ca2+Ca^{2+} (orange-red), Ba2+Ba^{2+} (light green), Cu2+Cu^{2+} (blue-green).
    • Aqueous Precipitates: Adding NaOH(aq)NaOH(aq) or NH3(aq)NH_{3}(aq) forms characteristic hydroxide precipitates (Fe2+Fe^{2+} is green, Fe3+Fe^{3+} is red-brown, Cu2+Cu^{2+} is blue).
    • Ammonium (NH4+NH_{4}^{+}): Heating with NaOH(aq)NaOH(aq) releases ammonia gas.
  • Anions:
    • Carbonate (CO32CO_{3}^{2-}): Reaction with acid produces CO2CO_{2} gas (test with limewater).
    • Halides (ClCl^{-}, BrBr^{-}, II^{-}): Reaction with acidified silver nitrate forms white (AgClAgCl), cream (AgBrAgBr), or yellow (AgIAgI) precipitates.
    • Sulfate (SO42SO_{4}^{2-}): Reaction with acidified barium nitrate forms a white precipitate.
  • Gases:
    • Hydrogen (H2H_{2}): 'Squeaky pop' with a lighted splint.
    • Oxygen (O2O_{2}): Relights a glowing splint.
    • Carbon Dioxide (CO2CO_{2}): Turns limewater cloudy.
    • Chlorine (Cl2Cl_{2}): Bleaches damp litmus paper.
    • Ammonia (NH3NH_{3}): Turns damp red litmus paper blue.

Quantitative Analysis: Titration

  • Purpose: Used to determine the exact concentration of a substance.
  • Method: An acid is added from a burette to a measured volume of alkali (measured by pipette) until the indicator (e.g., methyl orange) changes colour.
  • Reliability: Titrations are repeated until 'concordant' results (within ±0.10cm3\pm 0.10\,cm^{3}) are achieved.