Optional Area Examination

Analytical Chemistry

Department of Biological, Chemical, and Physical Sciences

Illinois Institute of Technology

October 16, 2009

Instructions: There are three (3) parts to this examination. Place all of your answers in
a blue book. Begin each part with a new blue book. When you have completed this
examination give this examination and your blue books to the proctor.

Part I – Chromatography
Part II – Instrumentation
Part III – Spectroscopy
Part I: Chromatography

1. Briefly describe High Pressure Liquid Chromatography. What are the molecular
mechanisms that drive separation?

2. Explain the basics of Gas Chromatography. How do the mechanisms and

experimental parameters differ from HPLC?

3. Consider the following chromatogram obtained with a column (150 mm long,

0.46 mm diameter). An expanded view of Peak B and Peak C is shown in the
insert.
a. Define tm, tr, and tr’ and identify tr’ for Peak A, Peak B, Peak C. What
is the significance of tr’?
b. What is the resolution between Peak B and Peak C?
c. Using Peak C, calculate N (number of plates).

Peak B and C
(expanded)
 a. Part II: Instrumentation

1. NMR 3 3
a) Label the components of the FT-NMR block diagram in Fig.
1.
b) If the magnet operates at 9.4 Tesla what is the proton
resonant frequency? 4
c) Name 3 NMR active nuclei.
d) How would you increase the signal to noise?
2 5

2) UV-Vis spectroscopy
a) Define each term in the following equation: 1 6
A = -log T = log (Po/P) = εbc
What is the name of this equation?
b) Can this be applied to mixtures, if so how? Fig. 1 NMR Block diagram
c) What is a good range of values for A?
d) Name two lamps that are generally used for your source.
Part III: Spectroscopy

1.) Describe in detail the principle mechanisms, including the type of transitions, and the
advantages and disadvantages for each of the following spectroscopic methods:
a. Infrared spectroscopy
b. Mass Spectrometry
c. UV-Vis spectroscopy
d. NMR

2.) Either benzonitrile or phenylacetonitrile shows a band of medium intensity at 2940

cm-1; the other compound shows nothing in the range 3000 – 2500 cm-1. Explain.

3.) Sketch the 1H NMR spectrum for each of the following compounds. Assume first
order multiplets where possible.
O

OH

a.

b. Br
O

c.