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37. Analytical techniques

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  1. 37.1 Thin-layer chromatography

    1. • Describe and understand the terms: (a) stationary phase, e.g. aluminium oxide (on a solid support); (b) mobile phase; a polar or non-polar solvent; (c) Rf value; (d) solvent front and baseline

    2. • Interpret Rf values

    3. • Explain the differences in Rf values in terms of interaction with the stationary phase and of relative solubility in the mobile phase

  2. 37.2 Gas / liquid chromatography

    1. • Describe and understand the terms: (a) stationary phase; a high boiling point non-polar liquid (on a solid support); (b) mobile phase; an unreactive gas; (c) retention time

    2. • Interpret gas / liquid chromatograms in terms of the percentage composition of a mixture

    3. • Explain retention times in terms of interaction with the stationary phase

  3. 37.3 Carbon-13 NMR spectroscopy

    1. • Analyse and interpret a carbon-13 NMR spectrum of a simple molecule to deduce:: (a) the different environments of the carbon atoms present; (b) the possible structures for the molecule

    2. • Predict or explain the number of peaks in a carbon-13 NMR spectrum for a given molecule

  4. 37.4 Proton NMR spectroscopy

    1. 37.4.1Proton NMR interpretation

      • Interpret proton NMR to deduce proton environments, relative proton numbers, n + 1 splitting (singlet to multiplet), and possible structures.

    2. 37.4.2The chemical shifts and splitting patterns

      • Predict the chemical shifts and splitting patterns of the protons in a given molecule

    3. 37.4.3Of tetramethylsilane, TMS, as the standard

      • Describe the use of tetramethylsilane, TMS, as the standard for chemical shift measurements

    4. 37.4.4Need for deuterated solvents, e.g. CDCl ₃,

      • State the need for deuterated solvents, e.g. CDCl ₃, when obtaining a proton NMR spectrum

    5. 37.4.5O-H and N-H proton exchange with D2O

      • Describe the identification of O–H and N–H protons by proton exchange using D₂O