6.2Unit 6. Practical Skills in Chemistry II
Advanced Inorganic & Organic Chemistry Core Practicals — IAL Edexcel Linear (Chemistry) Revision Notes & Topical Questions
5 min read 7 parts Lesson 4 of 14 Unit quiz
Curriculum Equation Key Esterification Reaction EquationFast Exam Solution
R-COOH + R2-OH ⇌ (conc. H₂SO₄) R-COO-R2 + H₂O
Lesson summary
6.2 Advanced Inorganic & Organic Chemistry Core Practicals: Complex Preparation, Qualitative Analysis and Aspirin — IAL EDEXCEL LINEAR (CHEMISTRY) notes: Carry out and evaluate the core practicals on preparing a transition metal complex, qualitative analysis of inorganic and orga…
- Cold ethanol wash
- Yield above 100%
- Group 2 ions
- Ammonium ions
- Order for sulfate
- Tollens' reagent
Part 1 of 9Core Practical 12: preparing a copper complex
Product
- Product dark blue crystals of Cu(NH3)4SO4·H2O.
Equation
- CuSO4·5H2O + 4NH3 → Cu(NH3)4SO4·H2O + 4H2O.
1
Weigh 1.4–1.6 g of copper(II) sulfate by difference using a test tube.
2
Add 4 cm3 of water and dissolve it in a hot-water bath.
3
In a fume cupboard wearing gloves, add 2 cm3 concentrated ammonia while stirring, giving deep blue [Cu(NH3)4(H2O)2]2+.
4
Pour into 6 cm3 ethanol and cool in an ice bath.
5
Filter under reduced pressure with a Buchner funnel and wash with cold ethanol.
6
Dry between two filter papers and weigh the crystals.
Part 2 of 9Explaining the complex preparation
Ethanol
- Ethanol is less polar than water, so the ionic complex is less soluble and crystallises.
Cold ethanol wash
- Cold ethanol wash removes impurities without dissolving the product, which a hot wash would.
Yield above 100%
- Yield above 100% shows the crystals are wet or impure.
Losses
- Losses come from incomplete reaction and product remaining in solution.
Hazards
- Hazards concentrated ammonia is corrosive, toxic and environmentally harmful;
- copper salts are harmful;
- ethanol is flammable.
Part 3 of 9Core Practical 15: tests for positive ions
Core Practical 15: tests for positive ions
Preparation
- Preparation a solid sample is first dissolved in deionised water.
Group 2 ions
- Group 2 ions add NaOH dropwise to the chloride solutions of Ba, Ca, Mg and Sr, then in excess, and compare the precipitates.
Ammonium ions
- Ammonium ions warm the sample gently with NaOH(aq) and hold damp red litmus paper at the mouth of the tube, which turns blue in ammonia gas.
| Ion | Test with NaOH(aq) | Observation |
|---|---|---|
| Fe2+ | Add NaOH | Green precipitate that darkens in air |
| Fe3+ | Add NaOH | Orange-brown precipitate |
| Cu2+ | Add NaOH, then excess NH3 | Blue precipitate dissolving to a deep blue solution |
Part 4 of 9Core Practical 15: tests for negative ions
| Ion | Test | Positive result |
|---|---|---|
| Cl−, Br−, I− | Add dilute HNO3, then AgNO3 | White, cream and yellow precipitates; dilute or concentrated ammonia then distinguishes them |
| OH− | Red litmus or universal indicator paper | Litmus turns blue, clearly alkaline pH |
| CO32− | Add dilute HCl and pass the gas into limewater | Gas turns limewater milky |
| SO42− | Add dilute HCl, then BaCl2(aq) | White precipitate of BaSO4 |
- Order for sulfate
- HCl is added first to remove carbonate, which would also give a precipitate.
Part 5 of 9Core Practical 15: tests for organic functional groups
| Group | Reagent | Positive result |
|---|---|---|
| C=C | Bromine water | Orange solution decolourises |
| –OH | PCl5 | Steamy fumes of HCl at room temperature |
| Primary or secondary alcohol | Acidified K2Cr2O7 or KMnO4 | Orange to green, or purple to colourless |
| Carbonyl C=O | 2,4-DNPH | Deep orange precipitate |
| Aldehyde | Tollens' reagent, warmed | Silver mirror |
| Aldehyde | Fehling's or Benedict's solution, warmed | Brick-red precipitate of Cu2O |
| Carboxylic acid | Na2CO3(s) or NaHCO3(aq) | Effervescence of CO2 |
| CH3CO– or CH3CH(OH)– | Iodine and NaOH (iodoform) | Yellow precipitate |
Part 6 of 9Interpreting the carbonyl tests
2,4-DNPH
- 2,4-DNPH the C=O group condenses with it, and the precipitate is purified by recrystallisation and identified from its melting point.
Tollens' reagent
- Ag+ oxidises an aldehyde to a carboxylic acid and is reduced to silver.
Fehling's solution
- Cu2+ oxidises an aldehyde to a carboxylic acid and is reduced to Cu+ in Cu2O.
Ketones
- Ketones give no reaction with Tollens' or Fehling's because they cannot be oxidised.
Alcohol oxidation
- Alcohol oxidation primary and secondary alcohols are oxidised to aldehydes and ketones,
- which can be tested further,
- whereas tertiary alcohols are not oxidised.
Part 7 of 9Core Practical 16: preparing aspirin
- Skills
- measuring, heating in a water bath, recrystallising a solid and using melting-point apparatus.
1
Mix 6.0 g salicylic acid, 10 cm3 ethanoic anhydride and 5 drops of concentrated sulfuric acid catalyst in a conical flask.
2
Warm in a water bath at about 60 °C for 20 minutes.
3
Cool and pour into 75 cm3 cold water so aspirin crystallises.
4
Filter under reduced pressure with a Buchner funnel.
5
Recrystallise: dissolve in the minimum hot ethanol, pour over 40 cm3 cold water, filter and dry.
6
Take the melting point of the dry product.
Part 8 of 9Recrystallisation and melting point of aspirin
Recrystallisation
- Recrystallisation uses the minimum hot solvent, a hot filtration for insoluble impurities, slow cooling for large crystals and a wash with cold solvent.
Repeating
- Repeating gives a purer product but lowers the yield each time.
Purity
- Purity pure aspirin melts sharply at 135 °C, whereas impurities lower and broaden the melting range.
Technique
- Technique use a dry, finely powdered sample, heat slowly, repeat three times and quote a range.
Part 9 of 9More from the specification
More from the specification
Principles of Redox Titrations
- A redox titration determines the concentration of an unknown oxidising or reducing agent by measuring the precise volume of standard titrant required to complete electron transfer.
Potassium Manganate(VII) Titrations
- Self-indicating potassium manganate(VII) (KMnO₄) acts as a powerful oxidising agent under acidic conditions, turning from deep purple to a permanent pale pink end-point.
- (MnO₄⁻ + 8H⁺ + 5e⁻ → Mn²⁺ + 4H₂O)
Iodine-Thiosulfate Titrations
- In indirect redox titrations, an oxidising analyte liberates iodine (I₂) from excess iodide ions,
- which is then titrated against standard sodium thiosulfate using starch indicator.
- (2S₂O₃²⁻ + I₂ → S₄O₆²⁻ + 2I⁻)
Calculating Moles and Percentage Purity
- By calculating the stoichiometric moles of titrant consumed, chemists determine the moles and mass of active analyte present in a sample to establish its percentage purity.
Principles of Redox Titrations
- A redox titration determines the concentration of an unknown oxidising or reducing agent by measuring the precise volume of standard titrant required to complete electron transfer.
Potassium Manganate(VII) Titrations
- Self-indicating potassium manganate(VII) (KMnO₄) acts as a powerful oxidising agent under acidic conditions, turning from deep purple to a permanent pale pink end-point.
- (MnO₄⁻ + 8H⁺ + 5e⁻ → Mn²⁺ + 4H₂O)
Iodine-Thiosulfate Titrations
- In indirect redox titrations, an oxidising analyte liberates iodine (I₂) from excess iodide ions,
- which is then titrated against standard sodium thiosulfate using starch indicator.
- (2S₂O₃²⁻ + I₂ → S₄O₆²⁻ + 2I⁻)
Calculating Moles and Percentage Purity
- By calculating the stoichiometric moles of titrant consumed, chemists determine the moles and mass of active analyte present in a sample to establish its percentage purity.
Carbon dioxide
- A gas that turns limewater cloudy.
Percentage yield
- Actual yield divided by theoretical yield, times 100.
Titration
- Method for finding the volume of one solution that reacts exactly with another.
Hydroxide
- A compound containing the OH− ion, formed by Group I metals with water.
Redox titration
- A titration using electron transfer to find a concentration.
Key terms
| Term | Meaning |
|---|---|
| Recrystallisation | Purifying a solid by dissolving it in the minimum hot solvent, cooling to crystallise and filtering. |
| Complex ion | A central metal ion with ligands bonded by dative covalent bonds. |
| Buchner filtration | Filtration under reduced pressure for speed. |
| Qualitative analysis | Tests that identify which ions or functional groups are present. |
| Tollens' reagent | Ammoniacal silver nitrate, which gives a silver mirror with aldehydes. |
| Melting point range | The interval over which a solid melts, which shows purity. |
Avoid these mistakes
1
Using hot solvent to wash crystals — the product dissolves, so use cold solvent.
2
Adding BaCl2 before HCl in the sulfate test — carbonate would give a false precipitate.
3
Quoting a melting point as a single number — give a range and compare it with the data book.
4
Saying ketones give a silver mirror — only aldehydes react with Tollens' reagent.
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