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Problem Set 13 and 14

Retention index (RI) of 1-hexene = 100(t'R of 1-hexene - t'R of n-pentane)/(t'R of n-hexane - t'R of n-pentane) = 100(2.579 - 1.589)/(3.659 - 1.589) = 100(0.99)/(2.07) = 480 Therefore, the retention index of 1-hexene is 480.

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sophia del rosario
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239 views

Problem Set 13 and 14

Retention index (RI) of 1-hexene = 100(t'R of 1-hexene - t'R of n-pentane)/(t'R of n-hexane - t'R of n-pentane) = 100(2.579 - 1.589)/(3.659 - 1.589) = 100(0.99)/(2.07) = 480 Therefore, the retention index of 1-hexene is 480.

Uploaded by

sophia del rosario
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© © All Rights Reserved
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Download as PDF, TXT or read online on Scribd
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Del Rosario, Maria Sophia R.

Chem 2130
Problem Set 13 and 14 (Liquid and Gas Chromatography)

1.) What phenomenon gives rises to band broadening in chromatography and why does band
broadening increase with longer columns?

The occurrence of band broadening in a chromatographic system is mainly caused by four


principal sources: longitudinal diffusion, Eddy diffusion, mass transfer of sample among the phases
(mobile phase and stationary phase), and extra-column diffusion. In longitudinal diffusion, the
concentration of the analyte favors the center rather than the edges of the band, which causes band
broadening as the particles diffuse out from the central region of the column to the edges. Due to the
frictional drag forces that remain throughout the column, the flow is fastest in the central region of the
column, which results in the band broadening upon increasing the column length. In Eddy diffusion of
solutes, wherein solute molecules will take different paths through the stationary phase. Some solute
molecules move straight through the column, while others might encounter deviations from their
directions. This accounts for the band broadening as different paths are of different lengths. The mass
transfer of samples among the phases also contributes to band broadening, wherein if the sample of
interest has a strong affinity for the stationary phase under the condition of high velocity in the mobile
phase, then the sample of interest in the mobile phase will move ahead of the sample of interest in the
stationary phase. In such cases, the band broadening becomes worse as the flow rate of mobile phases
increases. In relation to the aforementioned occurrences and consequences, it can be inferred that all
of them are concerned with the column length, to which as the column length increases, so does the
retention time or the time for these effects to occur, which explains the increase in the band
broadening.

2.) Suggest approaches for helping to improve the resolution between different substances within a
chromatographic separation
There are many practiced approaches that are suggested to increase the resolution between
different substances within a chromatographic separation. This could be done by increasing the column
length, decreasing the particle size, reducing the peak tailing by assessing what mobile phase to use
and its solvent, increasing the temperature, reducing the system extra-column volume, choosing the
best packing and packing material, having appropriate mobile phase pH, having suitable column
stationary phase, changing the mobile phase solvent(s), and by increasing k (retention) through the
use of weaker solvent and stronger stationary phase.
Liquid Chromatography

3.) Alkali metal ions can be determined volumetrically by passing a solution of them through a cation
exchange column in the hydrogen form. They displace an equivalent amount of hydrogen ions that
appear in the effluent and can be titrated. How many millimoles of potassium ion are contained in a
liter of solution if the effluent obtained from a 5.00-mL aliquot run through a cation exchange column
requires 26.7mL of 0.0506 M NaOH for titration?
4.) The standard addition technique was used to analyze a sample component by liquid
chromatography. From the results listed in the following table determine the concentration of the
sample component.
Added concentration, mg/ml Peak Area
0 (pure sample) 3.72
1.23 7.00
3.47 12.70
4.89 16.30
6.24 20.01
7.15 22.25

Solution:

Added Concentration, mg/mL Peak Area


0 3.72
1.23 7.00
3.47 12.70
4.89 16.30
6.24 20.01
7.15 22.25
Gas Chromatography

5.) Gas reduction valves used on gas tanks in gas chromatography usually give the pressure in psig
(pounds per square inch above atmospheric pressure). Given that atmospheric pressure (760 torr) is
14.7 psi, calculate the inlet pressure to the gas chromatograph in torr, for 40.0 psig, if the ambient
pressure is 745 torr.
6.) A water sample is analyzed for traces of benzene using headspace analysis. Samples and standards
are spiked with a fixed amount of toluene as internal standard. The following data are obtained:
ppb Benzene Peak Area Benzene Peak Area Toluene
10.0 252 376
15.0 373 370
25.0 636 371
Sample 533 368

What is the concentration of benzene in the sample?


ppb Benzene Peak Area Benzene Peak Area Tolouene Average
10.0 252 376 314
15.0 373 370 371.5
25.0 636 371 503.5
Sample 533 368 450.5
7.) Use the retention data given in the following table to calculate the retention index of 1 -hexene
Sample Retention time, min
Air 0.571
n-pentane 2.16
n-hexane 4.23
1-hexene 3.15

Solution:

Sample Retention time (tR), min tM t'R


Air 0.571 0.571 0
n-pentane 2.16 0.571 1.589
n-hexane 4.23 0.571 3.659
1-hexene 3.15 0.571 2.579
t’R is the difference between the tR and tM
t’R = tR – tM

For air sample: For n-pentane sample:


t’R = tR – tM t’R = tR – tM
t’R = 0.571 – 0.571 t’R = 2.16 – 0.571
t’R = 0 t’R = 1.589

For n-pentane sample: For 1-hexene sample:


t’R = tR – tM t’R = tR – tM
t’R = 4.23 – 0.571 t’R = 3.15 – 0.571
t’R = 3.659 t’R = 2.579

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