This paper describes the use of fullerene molecules, also known as buckyballs, as a stationary phase for liquid chromatography. The performance of the fullerene-modified stationary phase (FMS) is compared to that of a more common C18 stationary phase and to two other carbon-based stationary phases, PGC and COZ. A. 10A OM B. - Figure 1. Idealized drawing of the cross-section of a pore inside a silica particle, showing the relative densities of aminopropylsilyl (red/green) and fullerene (blue) groups: (A) full cross- section; (B) detailed view of covalent bonding of fullerene to the silica surface. Surface densities of silyl and fullerene groups were inferred from elemental composition results obtained at each stage of the synthesis (see Table 1). Absorbance (mAU, 220 nm) 700 600 500 400 300 200 100 a. Define selectivity, a, with words and an equation. b. Explain how the choice of stationary phase affects selectivity. c. Calculate the resolution of the nitrobenzene and toluene peaks in the top trace of Figure 2. (Estimate any values you need from the graph, and show your work.) Nitrobenzene FMS, 50 mm x 4.6 mm i.d., 5 μm Toluene C18, 100 mm x 4.6 mm i.d., 3 μm COZ, 100 mm x 4.6 mm i.d., 3 μm PGC, 50 mm x 4.6 mm i.d., 5 μm Figure 2. Normalized retention of toluene and nitrobenzene on a conventional C18 bonded phase compared to FMS, PGC, and COZ. Eluent compositions [acetonitrile/water (A/W) v/v] were adjusted to obtain a retention factor of about 6.0 for nitrobenzene in each case: FMS (23.5/76.5 A/W), C18 (35/65 A/W), COZ (43/57 A/W), and PGC (54/46 A/W). All other conditions were constant: flow rate 2 mL/min, column temperature 40 °C, and injection volume 1 μL 0 0 5 10 Normalized Time (t/tm) 15 20
This paper describes the use of fullerene molecules, also known as buckyballs, as a stationary phase for liquid chromatography. The performance of the fullerene-modified stationary phase (FMS) is compared to that of a more common C18 stationary phase and to two other carbon-based stationary phases, PGC and COZ. A. 10A OM B. - Figure 1. Idealized drawing of the cross-section of a pore inside a silica particle, showing the relative densities of aminopropylsilyl (red/green) and fullerene (blue) groups: (A) full cross- section; (B) detailed view of covalent bonding of fullerene to the silica surface. Surface densities of silyl and fullerene groups were inferred from elemental composition results obtained at each stage of the synthesis (see Table 1). Absorbance (mAU, 220 nm) 700 600 500 400 300 200 100 a. Define selectivity, a, with words and an equation. b. Explain how the choice of stationary phase affects selectivity. c. Calculate the resolution of the nitrobenzene and toluene peaks in the top trace of Figure 2. (Estimate any values you need from the graph, and show your work.) Nitrobenzene FMS, 50 mm x 4.6 mm i.d., 5 μm Toluene C18, 100 mm x 4.6 mm i.d., 3 μm COZ, 100 mm x 4.6 mm i.d., 3 μm PGC, 50 mm x 4.6 mm i.d., 5 μm Figure 2. Normalized retention of toluene and nitrobenzene on a conventional C18 bonded phase compared to FMS, PGC, and COZ. Eluent compositions [acetonitrile/water (A/W) v/v] were adjusted to obtain a retention factor of about 6.0 for nitrobenzene in each case: FMS (23.5/76.5 A/W), C18 (35/65 A/W), COZ (43/57 A/W), and PGC (54/46 A/W). All other conditions were constant: flow rate 2 mL/min, column temperature 40 °C, and injection volume 1 μL 0 0 5 10 Normalized Time (t/tm) 15 20
Principles of Instrumental Analysis
7th Edition
ISBN:9781305577213
Author:Douglas A. Skoog, F. James Holler, Stanley R. Crouch
Publisher:Douglas A. Skoog, F. James Holler, Stanley R. Crouch
Chapter28: High-performance Liquid Chromatography
Section: Chapter Questions
Problem 28.7QAP
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Question
![This paper describes the use of fullerene molecules, also known as buckyballs, as a stationary phase for
liquid chromatography. The performance of the fullerene-modified stationary phase (FMS) is compared to
that of a more common C18 stationary phase and to two other carbon-based stationary phases, PGC and
COZ.
A.
10A
OM
B.
-
Figure 1. Idealized drawing of the
cross-section of a pore inside a silica
particle, showing the relative densities
of aminopropylsilyl (red/green) and
fullerene (blue) groups: (A) full cross-
section; (B) detailed view of covalent
bonding of fullerene to the silica
surface. Surface densities of silyl and
fullerene groups were inferred from
elemental composition results obtained
at each stage of the synthesis (see Table
1).
Absorbance (mAU, 220 nm)
700
600
500
400
300
200
100
a. Define selectivity, a, with words and an equation.
b. Explain how the choice of stationary phase affects selectivity.
c. Calculate the resolution of the nitrobenzene and toluene peaks in the top trace of Figure 2.
(Estimate any values you need from the graph, and show your work.)
Nitrobenzene
FMS, 50 mm x 4.6 mm i.d., 5 μm
Toluene
C18, 100 mm x 4.6 mm i.d., 3 μm
COZ, 100 mm x 4.6 mm i.d., 3 μm
PGC, 50 mm x 4.6 mm i.d., 5 μm
Figure 2. Normalized retention of toluene and
nitrobenzene on a conventional C18 bonded phase
compared to FMS, PGC, and COZ. Eluent compositions
[acetonitrile/water (A/W) v/v] were adjusted to obtain a
retention factor of about 6.0 for nitrobenzene in each
case: FMS (23.5/76.5 A/W), C18 (35/65 A/W), COZ
(43/57 A/W), and PGC (54/46 A/W). All other
conditions were constant: flow rate 2 mL/min, column
temperature 40 °C, and injection volume 1 μL
0
0
5
10
Normalized Time (t/tm)
15
20](/v2/_next/image?url=https%3A%2F%2Fcontent.bartleby.com%2Fqna-images%2Fquestion%2F5a600697-f443-4c2b-86e3-dc55cb10171e%2F8cf9cc55-f2fa-43d4-9328-66e3c4845526%2Fu0cnth7_processed.png&w=3840&q=75)
Transcribed Image Text:This paper describes the use of fullerene molecules, also known as buckyballs, as a stationary phase for
liquid chromatography. The performance of the fullerene-modified stationary phase (FMS) is compared to
that of a more common C18 stationary phase and to two other carbon-based stationary phases, PGC and
COZ.
A.
10A
OM
B.
-
Figure 1. Idealized drawing of the
cross-section of a pore inside a silica
particle, showing the relative densities
of aminopropylsilyl (red/green) and
fullerene (blue) groups: (A) full cross-
section; (B) detailed view of covalent
bonding of fullerene to the silica
surface. Surface densities of silyl and
fullerene groups were inferred from
elemental composition results obtained
at each stage of the synthesis (see Table
1).
Absorbance (mAU, 220 nm)
700
600
500
400
300
200
100
a. Define selectivity, a, with words and an equation.
b. Explain how the choice of stationary phase affects selectivity.
c. Calculate the resolution of the nitrobenzene and toluene peaks in the top trace of Figure 2.
(Estimate any values you need from the graph, and show your work.)
Nitrobenzene
FMS, 50 mm x 4.6 mm i.d., 5 μm
Toluene
C18, 100 mm x 4.6 mm i.d., 3 μm
COZ, 100 mm x 4.6 mm i.d., 3 μm
PGC, 50 mm x 4.6 mm i.d., 5 μm
Figure 2. Normalized retention of toluene and
nitrobenzene on a conventional C18 bonded phase
compared to FMS, PGC, and COZ. Eluent compositions
[acetonitrile/water (A/W) v/v] were adjusted to obtain a
retention factor of about 6.0 for nitrobenzene in each
case: FMS (23.5/76.5 A/W), C18 (35/65 A/W), COZ
(43/57 A/W), and PGC (54/46 A/W). All other
conditions were constant: flow rate 2 mL/min, column
temperature 40 °C, and injection volume 1 μL
0
0
5
10
Normalized Time (t/tm)
15
20
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