Identification of ions by chemical and spectroscopic means

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Apuntes de la lección

Flame Tests

  • Metal ions produce a characteristic colour when heated strongly in a flame, so flame tests identify metal cations.
  • Clean the wire by dipping it in dilute acid and holding it in a blue Bunsen flame until no colour is seen; this prevents contamination.
  • Dip the clean wire into the sample, then place it in the edge of the blue flame and note the colour.
  • Flame colours: lithium crimson, sodium yellow, potassium lilac, calcium orange-red, copper green.
  • If a mixture of ions is present, colours can mask each other, making identification unreliable.
  • Use a blue flame because the sample must be heated strongly; avoid overheating the wire until it glows red.

Diagram showing the technique for carrying out a flame test

Diagram showing the technique for carrying out a flame test

Metal Hydroxides

  • Adding sodium hydroxide solution to metal cations forms coloured precipitates of metal hydroxides.
  • Add a few drops of NaOH first, then add excess, because some precipitates dissolve in excess NaOH.
  • Copper(II) gives a blue precipitate; iron(II) gives a green precipitate; iron(III) gives a brown precipitate.
  • Calcium, magnesium and aluminium ions form white precipitates with NaOH.
  • Aluminium hydroxide dissolves in excess NaOH to give a colourless solution, but calcium and magnesium hydroxides do not dissolve.
  • A flame test can distinguish between calcium and magnesium ions.

Testing for Ammonium Ions

  • Test for ammonium ions (NH₄⁺) by adding sodium hydroxide solution and gently heating.
  • If ammonium ions are present, ammonia gas is produced.
  • Ammonia gas turns damp red litmus paper blue; hold the paper near the mouth of the test tube without touching the sides.
  • Ammonia also reacts with hydrogen chloride gas to form a white smoke of ammonium chloride.
  • The ionic equation is: NH₄⁺(aq) + OH⁻(aq) → NH₃(g) + H₂O(l).
  • Ammonium (NH₄⁺) is the aqueous cation; ammonia (NH₃) is the gas.

Testing for ammonium ions

Testing for ammonium ions

Test for Carbonates

  • Carbonates contain the carbonate ion, CO₃²⁻.
  • Add dilute acid to the sample; if a carbonate is present, effervescence occurs and carbon dioxide gas is released.
  • Bubble the gas through limewater; carbon dioxide turns limewater cloudy/milky due to formation of insoluble calcium carbonate.
  • Equation: CO₃²⁻(aq) + 2H⁺(aq) → CO₂(g) + H₂O(l).
  • Equation: CO₂(g) + Ca(OH)₂(aq) → CaCO₃(s) + H₂O(l).
  • Connect the test tube to the limewater quickly so no carbon dioxide escapes.

Test for Halides

  • Halide ions are the negative ions formed by Group 7 elements: Cl⁻, Br⁻, I⁻.
  • Acidify the sample with dilute nitric acid, then add silver nitrate solution.
  • A silver halide precipitate forms: silver chloride white, silver bromide cream, silver iodide yellow.
  • Ionic equation: Ag⁺(aq) + X⁻(aq) → AgX(s).
  • Use nitric acid, not hydrochloric acid, because HCl contains chloride ions that would interfere.
  • Example: KCl(aq) + AgNO₃(aq) → KNO₃(aq) + AgCl(s).

Test for Sulfates

  • Acidify the sample with dilute hydrochloric acid, then add barium chloride solution.
  • A white precipitate of barium sulfate is a positive result for sulfate ions.
  • Ionic equation: Ba²⁺(aq) + SO₄²⁻(aq) → BaSO₄(s).
  • The test can also be carried out using barium nitrate solution.
  • HCl is added first to remove any carbonates, which would also produce a precipitate and interfere.
  • State symbols for the reaction are aq, aq, s.

Core Practical: Identifying Ions

  • The aim is to use chemical tests to identify the ions in unknown single ionic compounds.
  • Common tests include flame tests and tests for sulfate, carbonate and halide ions.
  • Tests can be carried out in any order; you may not need to do all tests on one sample.
  • Use only small amounts of sample and reagent; dissolve solid samples in distilled water if needed.
  • Record observations carefully in a results table and repeat any tests that give unclear results.
  • Identify the salt from the cation and anion present, balancing charges in the formula.
  • Example: a positive test for Fe²⁺ and sulfate ions means the salt is FeSO₄.
  • Hazards: limewater, dilute nitric acid and sodium hydroxide are harmful; ammonia gas is toxic if inhaled.

Instrumental Methods of Analysis

  • Instrumental methods include X-ray, infra-red and mass spectroscopy, gas chromatography and flame photometry.
  • They are more accurate, faster and easier to use, and more sensitive than traditional chemical tests.
  • They can be automated and can perform multiple simultaneous sampling and testing.
  • Modern instruments can work with very small sample sizes.
  • Advantages should be described in terms of sensitivity, speed and accuracy.

Flame Emission Spectroscopy

  • Flame emission spectroscopy is an instrumental method used to analyse metal ions in solution.
  • The sample is put into a flame and the light emitted is passed through a spectroscope.
  • The output is a line spectrum; different elements produce lines in different parts of the spectrum.
  • The spectrum identifies the metal ions present and can measure their concentrations.
  • The intensity of light is proportional to the number of ions vaporised, so a calibration curve can determine concentration.
  • It works for mixtures of ions, unlike a flame test which can only analyse one ion at a time.
  • Unknown samples are identified by comparing their spectrum to reference spectra.

Diapositivas

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Preguntas de práctica

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  1. 1.What colour flame is produced by potassium ions in a flame test?

    Easy
    • AYellow
    • BLilac
    • CCrimson
    • DOrange-red
  2. 2.A student adds sodium hydroxide solution to a solution containing iron(II) ions. What is observed?

    Easy
    • AA blue precipitate
    • BA green precipitate
    • CA brown precipitate
    • DA white precipitate that dissolves in excess
  3. 3.Which reagent is used to test for sulfate ions in solution?

    Easy
    • ASilver nitrate
    • BBarium chloride
    • CSodium hydroxide
    • DLimewater
  4. 4.What is the correct test for ammonium ions?

    Easy
    • AAdd sodium hydroxide and warm gently; test the gas with damp red litmus
    • BAdd silver nitrate; look for a white precipitate
    • CAdd barium chloride; look for a white precipitate
    • DAdd dilute acid; test the gas with limewater
  5. 5.Which instrumental method is used to analyse metal ions in solution by measuring the intensity and wavelength of light emitted?

    Medium
    • AGas chromatography
    • BFlame emission spectroscopy
    • CMass spectrometry
    • DInfra-red spectroscopy
  6. 6.Which statements about testing for halide ions are correct? (select all that apply)

    Medium
    • ADilute nitric acid is added before silver nitrate solution
    • BSilver chloride forms a white precipitate
    • CSilver bromide forms a yellow precipitate
    • DSilver iodide forms a yellow precipitate
    • EDilute hydrochloric acid is used to acidify the solution
  7. 7.Sodium ions produce a yellow flame in a flame test.

    Easy

    True or false?

  8. 8.Instrumental methods are less accurate than traditional chemical tests.

    Easy

    True or false?

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