Notifications

Log in to see your notifications.

Chemical Analysis

13 min read

Types of chemical analysis

Chemical analysis finds out what is in a sample (qualitative) and how much (quantitative). Choosing a method depends on the sample, the amount available and the accuracy needed.

MethodPrincipleExample
GravimetricWeigh a pure precipitate of known formulaBarium sulphate for sulphate
Volumetric (titration)Measure the volume of a standard solution that reacts exactlyAcid–base, redox and complexometric titrations
Colorimetry and UV–visible spectroscopyAbsorption of light is proportional to concentrationNitrate or phosphate in water
Atomic absorption spectroscopyAtoms absorb light of characteristic wavelengthsMetals in water and soil
ChromatographyComponents separate between a mobile and a stationary phaseDyes, amino acids, drugs
Infrared spectroscopyBonds absorb characteristic infrared frequenciesIdentifying functional groups
Mass spectrometryIons separate by mass to charge ratioRelative molecular mass and structure
NMR spectroscopyHydrogen nuclei in different environments absorb different radio frequenciesStructure of organic compounds

Chromatography

Chromatography and the Rf valueA chromatography plate after the solvent has risen. The solvent front is marked, and a spot has moved part of the way. The Rf value is the distance moved by the spot divided by the distance moved by the solvent front. In this example the spot moved 3 centimetres and the solvent 5 centimetres, so Rf is 0.6.solvent front 5.0 cmspot 3.0 cmstart lineRf = distance moved by the spot÷ distance moved by the solvent= 3.0 ÷ 5.0 = 0.6
R_f is always between 0 and 1. A compound has a fixed R_f in a given solvent and stationary phase, so it can be identified by comparison with known samples.

In paper or thin-layer chromatography the stationary phase is paper or a thin layer of silica on a plate and the mobile phase is a solvent that rises by capillary action. In gas chromatography (GC) the mobile phase is a gas and the stationary phase is a liquid on a solid in a column; in HPLC a liquid is forced through a column at high pressure. Components that stick more strongly to the stationary phase move more slowly.

Try itCalculating the Rf value

Measure the distances from the start line. Find the Rf value.

Spectroscopy and the Beer–Lambert law

Absorbance A is proportional to concentration c and path length l. ε is the molar absorptivity. A calibration graph of absorbance against known concentrations gives the concentration of an unknown.
  • molar absorptivity (dm³ mol⁻¹ cm⁻¹)
Try itA colorimeter reading

Choose the absorptivity, the concentration and the width of the cell. Find the absorbance and the percentage of light that passes through.

TechniqueWhat it tells you
InfraredO–H (broad, 3200–3600 cm⁻¹), C=O (1680–1750 cm⁻¹), C–H (about 2900 cm⁻¹)
Mass spectrumThe molecular ion peak gives the relative molecular mass; fragments show the structure
¹H NMRThe number of peaks shows the number of different hydrogen environments; the area shows how many hydrogens
Open the acid–base titration lab
Practise a volumetric analysis.
Check yourself What does a high R_f value show?
Check yourself An absorbance of 0.30 was measured for a solution of concentration 0.0002 mol/dm³ in a 1 cm cell. What is ε?
Check yourself Which technique is best to find the relative molecular mass of an unknown organic compound?

Key terms

Qualitative analysis
Finding out which substances are present.
Quantitative analysis
Finding out how much of a substance is present.
Rf value
The distance moved by a spot divided by the distance moved by the solvent front.
Calibration graph
A graph from known standards used to find the concentration of an unknown.

Summary

  • Chemical analysis can be gravimetric, volumetric or instrumental.
  • Chromatography separates mixtures; R_f = distance of spot ÷ distance of solvent.
  • Beer–Lambert: A = ε c l; use a calibration graph.
  • IR, mass spectrometry and NMR identify the structure of compounds.