CURRICULUM FOR HIGER EDUCATION

(KURIKULUM PENDIDIKAN TINGGI 2014)

Instrumental Methods of Analysis & Methods Development

Team Teaching:
Mutakin, Ph.D,
Dr. Jutti Levita, M.Si.,
Danni Ramdhani, MSi

DEPARTEMENT OF PHARMACEUTICAL ANALYSIS AND MEDICINAL CHEMISTRY

FACULTY OF PHARMACY
UNIVERSITAS PADJADJARAN
2015

Instrumental Methods of Analysis & Methods Development- Syllabus

OBJECTIVE
The following outlines general objectives of this course:
1. As a result of this course students should be able to define a problem where the determination
and/or measurement of some chemical species is required. There are a long series of questions
which must be answered about the desired results before one can address the question of what
instrumental technique should be utilized.
2. Students should develop sufficient knowledge about the major instrumental methods of
chemical analysis so that they can determine what technique should be used to solve a
particular problem. The knowledge base includes:
a. the chemical and/or physical basis of the measurement (e.g. what is used to stimulate
the sample, how does the sample interact with the stimulus, how is the interaction
detected)
b. the type of information that can be obtained from the measurement
c. the limitation and/or requirements of the method
d. the advances in instrumentation which have been made, especially those made as a
result of problems encountered with the method.
3. The student should be able to address the problems of analyzing complex samples. This would
include defining the problem, determining any constraints, choosing the best methodology, and
determining how to test the methodology to prove its merits. Where there are alternatives the
student should be able to define the advantages and disadvantages of each.
4. The class will be divided into groups of about four and most of the assignments will be
performed by the group. This exercise in cooperative learning should help students develop
skills in working as a team.
5. To give a better opportunity for the students to understand all aspects of providing analytical
results, a semester long project will focus on the requirements for a developing and testing
methodologies and/or procedures for the rapid analysis of threat substance in the field, and in
the laboratory. This will include the background necessary for a scientific expert witness to
present new techniques in a court of law.
INSTRUCTORS:
Mutakin, PhD.
email: mutakin12@unpad.ac.id
Dr. Jutti Levita, M.Si. email: la_via63@yahoo.com
Danni Rhamdani, M.Si. email ramdhani07@gmail.com
Faculty of Pharmacy-New Building Office Hours: 13.00-14.00 Other times by appointment

TEXTBOOK:
There is no official textbook but any modern Instrumental Analysis text like Instrumental Methods of
Analysis, 7th ed, Willard, Merritt, Dean, Settle, will be of value as a reference.
Any Web Resources are acceptable.
GRADING:
Group Presentations 40%
Final Exam 20%
Group Project 30%
Participation 10%
GROUP PROJECT:
Any analytical approach requires that the problem be defined before making decisions about what type
of instrumentation to utilize. The class will be divided into teams that will work together to define an
analytical problem and develop a proposal for the analysis. The focus will be related to other courses
(especially substances that could be utilized in another interesting cases: crime, forensic, drug abuse) or
environmental or related to an industrial need. The projects may involve looking at rapid field analysis or
accurate laboratory analysis. There will be oral and written presentations as well as periodic progress
reports.
The use of instrumental methods of analysis on evidentiary material from a crime scene means that the
results will be presented in a court of law. Generally a scientist does not understand the requirements
placed on the expert witness (scientist) and the methodology that generated the results which will be
presented (testimony). To give you an example of the analytical approach the various groups will
consider some aspect of the preparation that a scientific expert might have to prepare for and present
in a court of law or before a judge in a Hearing. Each group will choose one of the following aspects
and prepare what they believe would be testimony to present to a judge. The idea is to give a lawyer
enough factual information to explain the process or procedure. You will then be asked the types of
questions that you would likely be asked by a judge (or opposing lawyer). You may need to go back and
get new information to support your claims and add this to you written testimony. Depending upon the
time available, some groups will appear in a mock courtroom setting before a judge to answer
questions posed by the court.
1.
2.
3.
4.

Use of fluorescence to do presumptive tests to identify blood or other body fluids.

Use of presumptive tests for anthrax or cocaine
The collection, preservation, and control of blood evidence being used for DNA testing
The use of capillary electrophoresis with laser fluorescence detection for nuclear DNA (Y
chromosome only or multiple chromosome)

5.
6.
7.
8.
9.
10.

The use of sequencing for the analysis of mitochondrial DNA

Laboratory analysis to confirm cocaine
Detection in the field and confirmation in the laboratory of flammable accelerants or explosives
Detection of illegal drugs or steroids in athletes
Detection of analgesics in traditional medicine
Detection of Formaldehyde residue in Food and beverages

GROUP PRESENTATIONS:
In an effort to be sure that each person is developing an understanding of a technique or the analytical
approach, each group is expected to meet regularly to discuss and prepare for specific topics which they
will be expected to present in class. These topics are specified below and will be used to supplement
presentations made by the instructor. It is expected that there will be class discussions on the topics so
even the groups not actually making presentations are expected to have investigated the topic and thus
be able to contribute to the discussions. There will be questions asked as a part of the presentation and
you will use iClickers to respond. The iClicker response will also be used to take attendance. In the
following schedule some of the specific topics that will be assigned are numbered sequentially for
reference. PowerPoint presentations on some of these topics are available on the class web site
UNPADs elearning.
You will be expected to attend classes and attendance will be recorded using your iClickers. You will be
allowed no more than 3 (three) absences during the semester. You may be sick or on an interview or
whatever reason but if you are absent for more than 3 class sessions you will have to write a 3 page
paper for each class you miss (beyond the 3).
TENTATIVE SCHEDULE:
I.

II.

Understanding the problem: the analytical approach

A. knowing the questions to ask and recognizing connections
B. recognizing strengths and weaknesses of the technique (what results are expected and
where are the errors)
C. knowing statistics is essential for interpretation (detection limits, signal/noise)
D. general philosophy in instrument design
E. special problems with analysis within the criminal justice system
F. issues of quality assurance and quality control
G. special problems for portable instrumentation and rapid detection
Molecular spectroscopy
A. what are the samples and what results are expected
B. infrared spectroscopy - most qualitative
1. what are the interactions with molecules absorption scattering
2. means of excitation (light sources)
3. separation of spectrum (wavelength dispersion, time resolution)
4. detection of the signal (heat, differential detection)

III.

IV.

5. interpretation of spectrum (qualitative, mixtures, resolution)

6. advantages of Fourier Transform (FTIR)
C. UV-Visible - more qualitative.
1. emission
2. absorption
3. fluorescence
4. photoacoustic
5. excitation sources (lasers, time resolution)
6. wavelength dispersion (gratings, prisms, interference filters, laser, placement of
sample relative to dispersion, resolution)
7. detection of signal (photocells, photomultipliers, diode arrays, sensitivity and
S/N)
8. interpretation (quantification, mixtures, absorption vs. fluorescence and the use
of time, photoacoustic, fluorescent tags)
Separation techniques
A. Chromatography
1. gas chromatography, liquid chromatography, supercritical fluids
2. importance of column technology (packing, capillaries)
3. separation based on increasing number of factors (volatility, solubility,
interactions with stationary phase, size, electrical field)
4. detection: simple vs. specific (gas and liquid)
5. detection as a means of further analysis (use of tags and coupling to IR and MS)
6. electrophoresis (plates and capillary) and use with DNA analysis
B. Immunoassays and DNA techniques
C. mass spectroscopy
1. making the gaseous molecule into an ion (electron impact, chemical ionization)
2. making liquids and solids into ions (electrospray, electrical discharge, laser
desorption, fast atom bombardment)
3. separation of ions on basis of mass to charge ratio
magnetic
time of flight
electric quadrupole
4. resolution, time and multiple separations
5. detection and interpretation (how this is linked to excitation)
Elemental analysis
A. mass spectrometry (electrical discharges)
B. atomic spectroscopy
atomic absorption
atomic emission
atomic fluorescence

6. excitation and getting sample into gas phase (flames, electrical discharges,
plasmas)
7. wavelength separation and resolution (dependence on technique)
8. detection of radiation (simultaneous/scanning, signal noise)
9. interpretation (errors due to molecular and ionic species, matrix effects, other
interferences)
D. X-ray analysis and electron spectroscopy (surface analysis)
REFERENCES:
1. http://people.virginia.edu/~jnd/UGCourseEval/syllabus-chem%205570.pdf