Laboratory Techniques in Organic Chemistry
Laboratory Techniques in Organic Chemistry
4th Edition
ISBN: 9781464134227
Author: Jerry R. Mohrig, David Alberg, Gretchen Hofmeister, Paul F. Schatz, Christina Noring Hammond
Publisher: W. H. Freeman
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Chapter 20, Problem 6Q
Interpretation Introduction

Interpretation:

The two adjustments that have to be made to improve resolutions should be determined.

Concept introduction:

Gas chromatography is efficiently used for the compounds that have high vapor pressures which allow them to pass through a GC column.

A gas chromatography does not identify compounds if unknown samples are loaded into the column. GC is one of type of partition chromatography, where the sample that has to be analyzed get adsorbed on the stationary phase.

The stationary phase is formed by high boiling nonvolatile liquid, usually a polymer. An inert gas like helium or nitrogen is utilized to form mobile phase. In GC, no interaction of compound with mobile phase occurs, unlike LC and TLC. The inert gas that makes the mobile phase carries the compound down the column when it is in vapor state. The compounds present in the mixture divide themselves between the gas phase and the liquid phase in the column in an equilibrium.

The components of gas-liquid chromatography are as follows:

  • High-pressure pure carrier gas source
  • Flow controller
  • Heated injection port
  • Column and column oven
  • Detector
  • Recording device or data station

Gas-liquid chromatography is very useful for the quantitative determinations of the components in volatile mixtures. The comparison of peak areas on the chromatogram results in the determination of amounts of the compounds. The area under the chromatographic peak is proportional to the concentration of the sample responsible for it denoted by response factor given as follow:

  A=fC

Where,

  • A is area under chromatographic peak.
  • f is response factor.
  • C is concentration of sample.

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Why does the efficiency (decreased plate height) of liquid chromatography increase as the stationary phase particle size is reduced?
One method for the quantitative determination of the concentration of constituents in a sample analyzed by gas chromatography is area normalization. Here, complete elution of all the sample constituents is necessary. The area of each peak is then measured and corrected for differences in detector response to the different eluates. This correction involves dividing the area by an empirically determined correction factor. The concentration of the analyte is found from the ratio of its corrected area to the total corrected area of all peaks. For a chromatogram containing three peaks, the relative areas were found to be 16.4, 45.2 and 30.2, in order of increasing retention time. Calculate the percentage of each compound if the relative detector responses were 0.60, 0.78 and 0.88, respectively.
A chromatogram of a mixture of species A, B, and C provided the following data:               a) Define "Retention time".     b)  Calculate the resolution between species A and B.      c) Calculate the retention time of species B necessary to separate it from species A with a resolution of 1.5.
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