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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

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R-COOH + R2-OH ⇌ (conc. H₂SO₄) R-COO-R2 + H₂O
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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.
IonTest with NaOH(aq)Observation
Fe2+Add NaOHGreen precipitate that darkens in air
Fe3+Add NaOHOrange-brown precipitate
Cu2+Add NaOH, then excess NH3Blue precipitate dissolving to a deep blue solution

Part 4 of 9Core Practical 15: tests for negative ions

IonTestPositive result
Cl−, Br−, I−Add dilute HNO3, then AgNO3White, cream and yellow precipitates; dilute or concentrated ammonia then distinguishes them
OH−Red litmus or universal indicator paperLitmus turns blue, clearly alkaline pH
CO32−Add dilute HCl and pass the gas into limewaterGas 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

GroupReagentPositive result
C=CBromine waterOrange solution decolourises
–OHPCl5Steamy fumes of HCl at room temperature
Primary or secondary alcoholAcidified K2Cr2O7 or KMnO4Orange to green, or purple to colourless
Carbonyl C=O2,4-DNPHDeep orange precipitate
AldehydeTollens' reagent, warmedSilver mirror
AldehydeFehling's or Benedict's solution, warmedBrick-red precipitate of Cu2O
Carboxylic acidNa2CO3(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

TermMeaning
RecrystallisationPurifying a solid by dissolving it in the minimum hot solvent, cooling to crystallise and filtering.
Complex ionA central metal ion with ligands bonded by dative covalent bonds.
Buchner filtrationFiltration under reduced pressure for speed.
Qualitative analysisTests that identify which ions or functional groups are present.
Tollens' reagentAmmoniacal silver nitrate, which gives a silver mirror with aldehydes.
Melting point rangeThe 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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