Chemistry 360 Final exam April 2005 Smith-Palmer
[4] Why are there many different stationary phases available for glc and HPLC columns?
[8] What are the advantages and disadvantages of capillary columns compared to packed columns? Think GC, HPLC, SCF.
What is a monolithic silica column. How is it designed? What are the advantages of it compared to a typical packed HPLC column.
[2]
[2] The activity of the just-separated uranium increases. Why?
[1] For how long would you expect it to increase?
[5] Willy and Nilly were carrying out GC analysis of a mixture of pesticides. The worst resolution was 1.5. Willy suggested that they should increase the flow rate and Nilly thought they should decrease it. Who was right and why?
What does the 1.5 tell you about the resolution?
What else could they do to optimize the technique?

[20] 1. You are going to take part in a debate. You may choose your side.
The postulate is:
“
You will be the first speaker.
Write
to use for your speech
The debate will be marked on how many “points” are made.
Make everything you say count.
Don’t waffle – use facts and examples.
[20] There are two summer projects to be carried out in a popular analytical laboratory.
It is well equipped and has an example of most analytical instruments.
You are the supervisor. You must decide what instrument will be used for each project - Obviously you cannot use the same instrument for both projects
Answer the questions below to act as an introduction to the students involved.
Project 1: Analyzing K
+
, Ca
2+
, NO
3
- and SO
4
2-
in water samples from local rivers.
Instrument:
Reason for choice:
Principle of Operation:
Notes on experimental design, choice of column, sample preparation.
Project 2: Analyzing cortisone, estradiol and cortisone in drug preparations from rival companies.
Instrument:
Reason for choice:
Principle of operation:
Describe how they should go about method development.

[5] 3. Do either A or B.
A C
5
H O
How many double bond equivalents are indicated by the formula?
From the fragmentations in the mass spectrum, suggest a formula that could account for this.
Note: the peak at 58 is due to protonation of the fragment with mass 57 and thus is not a direct fragment.
B How many double bond equivalents are indicated by the given formula?
What is a tropylium ion?
Which peak does it correspond to and why is it stable?
[20] 5. Describe five of the following:
Supercritical fluid chromatography
Cyclic voltammetry
APCI interface for HPLC-MS
ES interface for GC-HPLC
A detector for γ-ray spectroscopy
The origin of an EOF
[10] 6. Short Snappers – Choose 5 of the following
Head space GC
The molecular ion of a compound containing C,H,O is at mass with height .
The M+1 peak has height . How many carbon atoms in the compound?
How can uranyl ions be separated chromatographically from thorium ions?
Draw the structure of an anion exchange resin.
Name two compounds that could be separated using micellar electrokinetic chromatography.
Problems
Draw the V versus time curve for differential pulse polarography, and the resulting current versus time curve.
Do one of the following: