Tutorial 4-CHM260

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TUTORIAL CHM260

CHAPTER 4

1. The following data was obtained when a sample mixture was analyzed by GC on a
column 1.1 m long.

a) Calculate the retention factor, k', for hexanol.


b) Calculate the resolution, Rs, between propanol and butanol peaks. Are the peaks
completely resolved?
c) Calculate N and H using data from the propanol peak.
d) State the probable reason why a fronting peak appears in a chromatogram.

2. State two (2) methods which can improve the efficiency of a chromatographic column.

3. Consider a chromatography experiment in which a mixture of two components, P (k' =


4.00) and Q (k' = 5.00) are injected into a column with N = 1.00 x 103 theoretical
plates. The retention time for the less retained component, P is 10.0 min. Calculate:

a) tM
b) retention time for component Q
c) peak width (at base), W b for component P
d) selectivity factor, α of the column

4. Describe the following terms used in chromatography:

a) Mobile phase
b) Retention time
c) Stationary phase
d) Resolution

5. State whether plate height H, will increase or decrease and also whether the
chromatographic column will be more or less efficient if the following changes were
made during a chromatographic analysis.

a) Increasing the flow rate of the mobile phase,


b) Reducing the particle size of a packed column,
c) Increasing the diameter of a capillary column in GC.
d) Increasing the length of column L, in GC.

6. List two ways to increase the number of theoretical plates in a GC experiment.

yhanani/CHM260/T4
7. The following data was obtained from the chromatogram of species A, B, C and D run
on a GC which used a 30 m column:

a) the number of plates for compounds B and C on this column,


b) the retention factor, k' for peaks B and C.
c) the resolution of peaks B and C.

8. A mixture of organic acids was separated by reversed-phase liquid chromatography.


The data obtained from the chart recorder were as follows:

For acid A, the retention time was 4.4 min with the width at baseline of 1.6 min. For
acid B, the retention time was 6.8 min with the width at baseline of 1.2 min. A non-
retained compound generated a peak that appeared 0.8 min after injection. The mobile
phase flow rate in the column was 20 mL/min. The column was 1.0 m in length.

Calculate:

a) The capacity factor (k') for acid A.


b) The resolution achieved of compounds A and B.
c) The average number of theoretical plates in the column.
d) The average plate height.

9. What observation on a chromatogram would lead you to conclude that sample injected
into a GC column are overloaded/too much.

10. Heptane and toluene were separated with retention times of 15.4 min and 16.5 min,
respectively on a 1.0-meter packed column. An unretained species passed through the
column in 1.8 min. The peak widths measured at the base were 1.15 min for heptane
and 1.20 min for toluene. Calculate:

a) The resolution achieved between the peaks,


b) The average number of plates for the column,
c) The average plate height,
d) Capacity factor, k' for toluene.

11. The following data were obtained in a GC analysis of a sample mixture. The
chromatogram of 200 ppm butyl acetate showed a retention time of 4.4 min and
produced a peak area of 20360.

yhanani/CHM260/T4
a) What is species A?
b) Calculate the concentration of A.
c) Determine the selectivity and resolution factors for peaks A and B.
d) Are peaks A and B well separated? Justify your answer.

12. Trace amounts of phenol can be detected by HPLC. A 20-uL of 25 mg/L of a phenol
standard gives a peak of 140 cm2 and a 20-uL water sample gives a peak of 26 cm2
due to phenol. Using the 'response factor' method, calculate the phenol content in
water, in units of parts per million (ppm). (Refer Laboratory Manual, pg 59)

13. Based on the following chromatogram, name the liquid chromatography technique
which was probably used to separate the mixture.

14. Chromatograms of compounds A and B were obtained at the same flow rate with two
columns at equal length.

a) Which column has more theoretical plates ?


b) Which column has a higher plate height ?
c) Which column gives higher resolution ?

15. Name the specific type of liquid chromatography in which:

a) Different sized solutes penetrate voids in the stationary phase to different extents
and largest solutes are eluted first
b) Ions in mobile phase are attracted to counterions covalently attached to the
stationary phase.

yhanani/CHM260/T4

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