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 (0∘C and 100∘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 solvent frontdistance moved by substance.
- 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+ (red), Na+ (yellow), K+ (lilac), Ca2+ (orange-red), Ba2+ (light green), Cu2+ (blue-green).
- Aqueous Precipitates: Adding NaOH(aq) or NH3(aq) forms characteristic hydroxide precipitates (Fe2+ is green, Fe3+ is red-brown, Cu2+ is blue).
- Ammonium (NH4+): Heating with NaOH(aq) releases ammonia gas.
- Anions:
- Carbonate (CO32−): Reaction with acid produces CO2 gas (test with limewater).
- Halides (Cl−, Br−, I−): Reaction with acidified silver nitrate forms white (AgCl), cream (AgBr), or yellow (AgI) precipitates.
- Sulfate (SO42−): Reaction with acidified barium nitrate forms a white precipitate.
- Gases:
- Hydrogen (H2): 'Squeaky pop' with a lighted splint.
- Oxygen (O2): Relights a glowing splint.
- Carbon Dioxide (CO2): Turns limewater cloudy.
- Chlorine (Cl2): Bleaches damp litmus paper.
- Ammonia (NH3): 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) are achieved.