A food scientist is investigating whether a batch of fruit juice has been adulterated with an artificial sweetener. She uses two analytical techniques: thin-layer chromatography (TLC) and nuclear magnetic resonance (NMR) spectroscopy. Explain how each technique could be used to identify whether the artificial sweetener is present in the fruit juice sample, and state one advantage of using NMR spectroscopy over TLC for this analysis.

Edexcel A-Level Chemistry (9CH0) — 19.1 NMR and chromatography · Explain · 5 marks · View as Markdown

Written & reviewed by James Millett — Biology (Imperial College London), PGCE Science (University of Cambridge).

Thin-layer chromatography separates components of a mixture based on how strongly they adsorb to a stationary phase compared to how well they dissolve in a mobile phase. NMR spectroscopy provides information about the number and chemical environment of hydrogen atoms in a molecule.

Model answer (5 marks)

Thin‑layer chromatography (TLC) is first used to separate the components of the juice. The sample is spotted on a silica gel plate and developed in a suitable solvent system. After drying, the plate is examined under UV or by staining and the position of each spot is measured.

The Rf value of any spot that appears in the sample is calculated as the distance travelled by the spot divided by the distance travelled by the solvent front. The Rf value of the spot that is suspected to be the artificial sweetener is then compared with the Rf value of a reference sample of the pure sweetener that has been run on the same plate under identical conditions. A match of Rf values indicates that the sweetener is present in the juice.

Nuclear magnetic resonance (NMR) spectroscopy is then applied to the juice sample. The spectrum is recorded, giving the number of distinct proton environments as a series of peaks with characteristic chemical shifts and multiplicities.

The pattern of peaks in the juice spectrum is compared with the known ^1H‑NMR spectrum of the artificial sweetener. If the chemical shifts, integration and splitting patterns agree, the sweetener can be confirmed to be present.

An advantage of NMR over TLC is that NMR provides detailed structural information about the molecule, allowing unambiguous identification, whereas TLC only gives an Rf value which can be coincident for different compounds.

Examiner tips

  • Use the word ‘calculate’ for Rf, not ‘measure’ alone. Mention that the reference must be run under the same conditions. State that NMR gives chemical‑shift information, not just a Rf value. Highlight that NMR does not need a reference standard to be run alongside for identification.

Common mistakes

  • Saying TLC gives the exact identity of the compound. Forgetting to compare Rf values under identical conditions. Claiming NMR requires a reference standard to be run with the sample.

Mark scheme (5 marks)

  1. TLC separates the components of the fruit juice sample; the Rf value of any spot from the sample is calculated/measured
  2. The Rf value of the sample spot is compared to the Rf value of a known reference/standard sample of the artificial sweetener run under the same conditions; a match indicates the sweetener is present
  3. NMR spectroscopy identifies the number of distinct hydrogen (proton) environments in the molecule
  4. The NMR spectrum of the sample is compared to the known NMR spectrum of the artificial sweetener; if the patterns of peaks match, the sweetener is confirmed as present
  5. One advantage of NMR over TLC: NMR gives structural/molecular information about the compound (can confirm the identity of the molecule unambiguously), whereas TLC only gives Rf values which may coincide for different compounds / NMR does not require a reference standard to be run alongside

Key terms in this question

thin-layer chromatography (TLC) · NMR spectroscopy

Related

More NMR and chromatography questions

▶ Try answering this question with AI marking (free) →