ADVANCED INSTRUMENTAL ANALYSIS
1008-621-85 (031)
Fall 2003
Thursdays: 8 AM to 2 PM
Instructor: L. Paul Rosenberg
Office: A256
Phone:475-6159
e-mail: lprsch@rit.edu
OUTLINE:
This instrumental analysis laboratory is aimed at giving orientation towards the
use of sophisticated modern instruments that are relevant to the growth of the modern
science and technology. It is intended to give an opportunity to developing your
innovative skills. The approach adopted here is to give you relevant background materials
on selected topics. The topics are enclosed herewith for guidance. This list contains
instrumental analysis by AA, GC/MS, HPLC, UV-VIS, IR, cyclic voltammetry and Ionselective electrode. The analysis is to be carried out following the procedures given in
“Chemistry Experiments for Instrumental Methods.”
by D.T. Sawyer et al. The
procedure can be modified in appropriate cases to suit the analysis requirements.
SCHEDULE-DATES
Week 1 (9/11)
Week 2 (9/18)
Week 3 (9/23)
Week 4 (10/2)
Week 5 (10/9)
Week 6 (10/16)
Week 7 (10/23)
Week 8 (10/30)
Week 9 (11/6)
Week 10 (11/13)
Week (Finals)
EXPERIMENT NO.
Orientation-overview
EXPERIMENT-1
EXPERIMENT-1
EXPERIMENT-2
EXPERIMENT-2
EXPERIMENT-3
EXPERIMENT-3
EXPERIMENT-4
EXPERIMENT-4
EXPERIMENT-5
No Lab.
REPORT DUE DATES
Report 1
Report 2
Report 3
Report 4
Report 5
The laboratory report is due one week following its completion.
The following experiments are suggested from the above book.
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Experiment 4-1: Cyclic Voltammetry
Experiment 4-2: Study of Electrode Mechanism by Cyclic Voltammetry
Experiment 9-3: Det. Of Ca,Fe,Cu in Food by AAS
Experiment 12-3: Qualitative Identification of hydrocarbons by GC/MS
Experiment 13-5: Separation of carbohydrates by HPLC
Experiment 6-1: Spectroscopy in Visible Region::Two component mixtures
Experiment 8-2: IR spectra of Aldehydes and Ketones.
Experiment
: Ion selective electrode-Fluoride ion determination
GRADING SCHEME:
Lab. report 1 : 20%
Lab. report 2 : 20%
Lab. report 3 : 20%
Lab. report 4 : 20%
Lab. report 5 : 20%
LABORATORY REPORT WRITING STYLE:
The report should be written in the style of a journal article. It should have
a)
Title
b)
Abstract
c)
Introduction
d)
Experimental
e)
Results
f)
Discussion of results
g)
Conclusions
h)
Acknowledgment
i)
References
If you wish to have a look at the format, consult any article in the
Analytical Chemistry journal; it is easily available in the library. It may also be useful to
have a look at the Journal of American Chemical Society as a general reference. to the
style. Alternatively, you can follow the style given in the book on “Instrumental
Analysis” by D.T. Sawyer et al.
The following description will give what is generally expected in the
above areas.
a)
Title: It should be appropriate to the experiment and the results. It should carry
key words by which the article could be identified.
b)
Abstract: Brief summary of the results focusing on the outcome of the analysis.
c)
Introduction: It should give an outline of the analytical problem being solved
with references to the earlier literature. A short description of the technique used
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and the theoretical principles involved should be given. Don’t discuss the theory
extensively.
d)
Experimental: Discuss the experimental procedures including the
instrumentation used. It generally can be divided into chemicals used in the
preparation of the reagents (include the purity of the grades of chemicals). Any
standardization procedure used should be discussed here. If the solution
preparation involved precipitation or coagulation etc., it should be detailed out in
the this section.. Instrumentation used in the analysis should be given with
procedural details. Overall by reading the experimental section an analytical
chemist must be able to reproduce the reported results to a great degree of
accuracy.
e)
Results and discussion: The data collected should be reported in a tabular form.
The degree of precision of measurements should be reflected in the data. The
units of measurements should be SI units. Figures are appropriate way of showing
the nature of the data sampled and the associated trend. Orient discussions of the
results with reference to the tables and figures.
The data obtained should be discussed with respect to the literature reports by
giving appropriate references.
f)
Conclusions: It should be a short paragraph giving information on the final
conclusions drawn from the experiment. If the conclusions warrant future work,
it should also be discussed.
g)
Acknowledgment: In carrying out the experiment if you have sought the help of
others, you should acknowledge here.
h)
References: Follow the journal pattern- look into Analytical chemistry or Journal
of the American Chemical Society.
GRADING SCHEME:
(Total 100 points)
1.
Title page
2.
Abstract
3.
Introduction & Theory
4.
Experimental
5.
Results and discussion
6.
Conclusions
7.
References
5 points
10 points
15 points
10 points
35 points (10 points for Questions)
15 ponts
10 points
Guidelines:
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Prepare to carry out the standard analysis on the instrument before starting
on the problem.
Wear safety glasses all the time in the lab.
Do not do the experiments alone.
Do the experiments within the scheduled period.
Manuals for the use of the instruments are available and
read them before starting the experiment.
Instrumental failures or trouble should be reported immediately.
Feel free to ask questions.
Available instruments:
UV/Vis spectrometer
High performance liquid chromatography (HPLC)
Gas Chromatography (GC)
Gas Chromatography/mass spectrometer (GC/MS)
Atomic absorption spectrometer (AA)
Fourier Transform Infrared Spectrometer (FT-IR)
Nuclear Magnetic Resonance Spectrometer (NMR)
Cyclic Voltammetry (CV)
Ion-Selective Electrode: Fluoride and Lead Ion Selective Electrodes
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