Chapter 24: Q1TY (page 641)
Where would an unknown with a retention index of 936 be eluted in Figure 23-7?
Short Answer
The eluted unknown with a retention index of 936 would be found after nonane.
Chapter 24: Q1TY (page 641)
Where would an unknown with a retention index of 936 be eluted in Figure 23-7?
The eluted unknown with a retention index of 936 would be found after nonane.
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Get started for free(a) If retention times are 1.0 min for CH4, 12.0 min for octane, 13.0 min for unknown, and 15.0 min for nonane, find the Kovats retention index for the unknown. (b) What would be the Kovats index for the unknown if the phase ratio of the column were doubled? (c) What would be the Kovats index for the unknown if the length of the column were halved
The antitumor drug gimatecan is available as nearly pure (S)-enantiomer. Neither pure (R)-enantiomer nor a racemic (equal) mixture of the two enantiomers is available. To measure small quantities of (R)-enantiomer in nearly pure (S)-gimatecan, a preparation was subjected to normal-phase chromatography on each of the enantiomers of a commercial, chiral stationary phase designated (S,S)- and (R,R)-DACH-DNB. Chromatography on the (R,R)-stationary phase gave a slightly asymmetric peak at tr 5 6.10 min with retention factor k 5 1.22. Chromatography on the (S,S)- stationary phase gave a slightly asymmetric peak at tr 5 6.96 min with k 5 1.50. With the (S,S) stationary phase, a small peak with 0.03% of the area of the main peak was observed at 6.10 min.
Chromatography of gimatecan on each enantiomer of a chiral stationary phase. Lower traces have enlarged vertical scale. [Data from E. Badaloni, W. Cabri, A. Ciogli, R. Deias, F. Gasparrini, F. Giorgi, A. Vigevani, and C. Villani, โCombination of HPLC โInverted Chirality Columns Approachโ and MS/MS Detection for Extreme Enantiomeric Excess Determination Even in Absence of Reference Samples.โ Anal. Chem. 2007, 79, 6013.]
(a) Explain the appearance of the upper chromatograms. Dashed lines are position markers, not part of the chromatogram. What Problems 709 would the chromatogram of pure (R)-gimatecan look like on the same two stationary phases?
(b) Explain the appearance of the two lower chromatograms and why it can be concluded that the gimatecan contained 0.03% of the (R)-enantiomer. Why is the (R)-enantiomer not observed with the (R,R)-stationary phase?
(c) Find the relative retention (a) for the two enantiomers on the (S,S)-stationary phase.
(d) The column provides N 5 6 800 plates. What would be the resolution between the two equal peaks in a racemic (equal) mixture of (R)- and (S)-gimatecan? If the peaks were symmetric, does this resolution provide baseline separation in which signal returns to baseline before the next peak begins?
(a) What are the characteristics of an ideal carrier gas?
(b) Why do
Why is split less injection used with purge and trap sample preparation?
(a) How can you improve the resolution between two closely spaced peaks in gas chromatography?
(b) What approach from (a) would be most cost effective (not involve a purchase)?
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