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Gas Chromatography

1. Make a table of retention times, peak widths and peak areas for each mixture on
each column.

Retention Time (min) Peak Width Peak Area
Air 1.260 0.115 8899
Hexane 1.840 0.260 80772
Toluene 6.468 0.130 11233
T-butylbenzene 8.125 0.150 2804
P-xylene 9.793 0.180 9051
Noise peak 9.314 0.110 989
Table 1 Hydrocarbon mixture.

Retention time (min) Peak Width Peak Area
Benzene 1.222 0.219 841
Chlorobenzene 1.325 0.019 14656
Dichlorobenzene 6.896 0.017 2438
Nitrobenzene 7.765 0.051 14340
Trichlorobenzene 8.616 0.017 5730
Noise peak 1.880 0.073 1010
Table 2 Halocarbon Mixture.
2. Calculate the selectivity for toluene and p-xylene in each column. Do they differ?
Why do you expect this result?
R1 = toluene
R2 = p-xylene
= 1.540
3. Calculate N for the first and last analyte peak in each chromatogram. Report your
results in a table, and then discuss the results. Are they the same for the different
columns? For the different mixtures on the same column? Why or why not? Should N
change for different components?
Column Efficiency
Hexane 79.621
P-xylene 35956.587
Table 3 Column efficiency of hydrocarbon FID.

Column Efficiency
Chlorobenzene 426752.754
Trichlorobenzene 3026781.232
Table 4 Column efficiency of halocarbon ECD.

4. Calculate the average height of an equivalent theoretical plate (HETP) or plate
height (H) for each of the 4 chromatograms using the equation H=L/N, where L is
the column length (polar FID column 15 meters; nonpolar ECD column 30
meters) and N is the number of theoretical plates. Use the average of the two N values
from the first and last analyte measured for each chromatogram to get the average
HETP for the particular mixture on the particular column.
Average HETP
Hydrocarbon - FID 18018.104 0.0008332 m
Halocarbon - ECD 1726766.993 0.0000174 m
Table 5 HETP of FID and ECD.
5. What is the resolution, R, of the last two analyte peaks in the ECD mixture
chromatogram? What is R for the toluene and p-xylene peaks?

Resolution
Nitrobenzene / trichlorobenzene
25.029
Toluene / p-xylene
31.667
Table 6 Resolution for ECD and FID peaks.




High Performance Liquid Chromatograpy

6. Make a table of retention time, peak height, peak width and peak area for each
solvent composition at 245 and 263 nm.


Figure 1 Absorbance of 50/50 mixture.

Name Retention Time
(min)
Peak Height Peak Width Peak Area
245
nm
263
nm
245 nm 263 nm 245
nm
263
nm
245 nm 263 nm
Phenol 1.497 1.514 424125 1364625 0.333 0.482 70616.812 328874.265
Nitrobenzene 2.263 2.279 477057 588555 0.449 0.449 107099.296 132130.597
Toluene 3.810 3.844 36678 988294 0.283 0.549 5189.937 271286.703
o-xylene 5.158 5.208 20838 805763 0.299 0.499 3115.281 201037.868
p-xylene 5.657 5.707 9955 581074 0.299 0.532 1488.272 154565.684
Table 7 Properties of 50/50 Mixture.



-200000
0
200000
400000
600000
800000
1000000
1200000
1400000
1600000
0.9 1.9 2.9 3.9 4.9 5.9 6.9
A
b
s
o
r
b
a
n
c
e

(
m
A
U
)

Time (min)
Absorbance of 50/50 Acetronitrile and
water mixture

Figure 2 Absorbance of 80/20 mixture.

Name Retention Time
(min)
Peak Height Peak Width Peak Area
245 nm 263 nm 245 nm 263 nm 245 nm 263
nm
245 nm 263
nm
Phenol 1.017 1.017 23703 23.703 0.050 0.050 592.575 0.592
Nitrobenzene 1.300 1.300 262042 262.042 0.200 0.200 26204.200 26.204
Toluene 1.433 1.433 183134 183.134 0.133 0.133 12178.411 12.178
o-xylene 1.600 1.600 23166 23.166 0.150 0.150 1737.450 1.737
p-xylene 1.767 1.767 20823 20.823 0.150 0.150 1561.725 1.562
Table 8 Properties of 80/20 Mixture.



-50000
0
50000
100000
150000
200000
250000
300000
0.9 1.1 1.3 1.5 1.7 1.9 2.1 2.3
A
b
s
o
r
p
t
i
o
n

(
m
A
U
)

Time (min)
Absorbance of 80/20 Acetonitrile and
water mixture

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