SOUTHERN CONNECTICUT STATE UNIVERSITY
CHE 440 ‚ Instrumental Methods of Analysis
Spring Semester 2005
Tuesday, Thursday 9:35 – 10:50 am (lecture)
Tuesday 2:00 – 6:00 pm (laboratory)
Name: Robert
J Snyder
Office Hours:
Office: 305 Jennings Hall Tuesday, Wednesday, Thursday 11-12 pm
Phone: 203-392-6263 Wednesday 1-3 pm
E-mail: snyderr1@southernct.edu or at other times by appointment
COURSE NUMBER CHE 440 CREDIT HOURS 4 PREREQUISITES:
CHE 240, 260,261
COURSE TITLE: Instrumental Methods of Analysis
COURSE DESCRIPTION:
Chemistry 440, Instrumental Methods of Analysis, is an introduction to
the theoretical background and practical use of modern instruments in the
analytical laboratory. After a
brief introduction to the use of instrumentation for chemical analysis, the
properties of electromagnetic radiation will be discussed. Spectroscopic techniques that will be
covered include:
Ultraviolet/Visible Spectrophotometry, Fluorescence and Phosphorescence,
Atomic Absorption (Flame and Graphite Furnace) Spectroscopy, Infrared
Spectroscopy and Nuclear Magnetic Resonance Spectroscopy. After an introduction to
chromatographic separations, Gas Chromatography and High-Performance Liquid
Chromatography will be discussed.
Students will conduct experiments during the laboratory portion of the
course that will demonstrate the scientific method and illustrate basic
concepts presented in the lecture portion of the course. The experiments chosen will demonstrate
the practical use of modern instrumentation in solving real-world problems,
such as determining the amount of lead in Southerní drinking water by
Graphite Furnace Atomic Absorption Spectrometry; the amount of calcium, iron
and copper in Total K breakfast cereal by Flame Atomic Absorption Spectrometry;
the amount of aspirin and caffeine in Anacin tablets by Nuclear Magnetic
Resonance Spectroscopy; and the amount of caffeine in cola drinks by
High-Performance Liquid Chromatography.
COURSEíS CONTRIBUTION:
CHE 440 is a junior/senior level course in Analytical Chemistry. It is generally considered to be the
second half of a year of Analytical Chemistry that began with CHE 240,
Quantitative Analysis. This course
is a requirement for students pursuing the science education degree in
chemistry. The lecture portion of
the course concentrates on the theoretical aspects of the modern instrumentation
that todayís chemists are using in the analytical laboratory. The laboratory portion emphasizes the
practical use of those instruments that the American Chemical Society (ACS,
chemistryís external accrediting agency) has designated as required for an
ACS-certified degree in chemistry.
The course emphasizes analytical thinking and problem solving using
both quantitative and qualitative methods of analysis. Students are expected to learn how to
operate the various spectroscopic and chromatographic instruments as well as
learn the best way to prepare their samples for analysis.
The laboratory experiments offer the students an inquiry-based approach
to solving problems. The
instructor provides the students with detailed instructions on the operation of
the instruments, but he students are left on their own as to designing the
experiment. The students also
learn proper laboratory conduct, good laboratory practice, concern for the
environment and instructions on safety in science.
LEARNER OUTCOMES AND ASSESSMENT
1. Understand
the methods and techniques of Analytical Chemistry. (INTASC 1; NSTA 1 ,3, 4; CCCT
1.4, 2.6)
2. Differentiate
between qualitative analysis and quantitative analysis and learn which
instrumental
techniques are bested suited for each task. (INTASC 1, 4; NSTA 1, 3, 4; CCCT 1.1, 1.3, 1.4, 2.6)
3. Learn
the difference between classical methods of analysis and instrumental methods
of analysis.
(INTASC
1, 4 ; NSTA 1, 2, 3 ; CCCT 1.1, 1.3, 1.5, 2.6 )
4. Define
analyte and analytical signal. (INTASC 1, 4 ; NSTA 1, 2, 3 ;
CCCT 1.1, 1.3, 1.4, 2.6 )
5. Identify
the four basic components of any instrument. (INTASC 1,4 ; NSTA 1, 2, 3 ; CCCT 1.1, 1.3,
1.4, 2.6 )
6. Evaluate
instrumental techniques by determining the six performance characteristics of
analytical
instruments. (INSTAC 1, 4 ;
NSTA 1, 2, 3, 4 ; CCCT 1.4,
1.6 )
7. Use
the method of least squares (linear regression) to determine calibration curves
for quantitative
analysis. (INTASC 1, 4 ;
NSTA 1, 2, 3, 4 ; CCCT 1.4,
1.6 )
8. Understand
the difference between signals and noise. (INTASC 1, 4; NSTA 1,2,3,7 ; CCCT 1.4 )
9. Learn
the difference between noise reduction and signal enhancement. (INTASC 1; NSTA 1, 2, 3 ;
CCCT 1.2, 1.3, 1.4, 2.2, 2.6 )
10. Identify
chemical noise, instrumental noise, and environmental noise. (INTASC 1, 4
; NSTA 1, 2, 3, 4 ;
CCCT 1.2, 1.3, 1.4, 1,6, 2.1, 2.6 )
11. Differentiate
between hardware devices to reduce noise and software methods to enhance
signals.
(INSTAC
1, 4 ; NSTA 1, 2, 3, 4, 7 ; CCCT 1.2, 1.4, 2.2, 2.6 )
12. Identify
the various regions of the electromagnetic spectrum and what information instrumental
techniques tell us about each region. (INSTAC 1, 4 ; NSTA 1, 2, 3, 4 ; CCCT 1.2, 1.3, 1.4, 1.6, 2.2 )
13. Discuss
the wave-particle duality of matter and energy. (INSTAC 1, 4 ; NSTA 1, 2, 3 ; CCCT 1.3, 1.4 )
14. Calculate
wavelength, frequency and wavenumber for the different regions of the
electromagnetic
spectrum. (INSTAC 1, 4;
NSTA 1, 2, 3 ; CCCT 1.2,
1.4 )
15. Differentiate
among diffraction, refraction, reflection and scattering of radiation.
(INSTAC
1, 4 ; NSTA 1, 2, 3 ; CCCT 1.2, 1.3, 1.4, 2.2 )
16. Use
the Planck equation to calculate energy for the various regions of the
electromagnetic spectrum.
(INSTAC
1, 4 ; NSTA 1, 2, 3, ; CCCT 1.4 )
17. Discuss
the impact of the Heisenberg Uncertainty principle on spectroscopy.
(INSTAC
1, 4 ; NSTA 1, 2, 3 ; CCCT 1.2, 1.4, 2.2 )
18. Learn
the Born-Oppenheimer approximation and why it makes spectroscopy possible.
(INSTAC
1,4 ; NSTA 1, 2, 3, 7 ; CCCT 1.4 )
19. Understand
the various processes ( radiative and nonradiative) by which atoms or molecules
emit
energy
upon absorption of radiation.
(INSTAC 1, 4 ; NSTA 1, 2, 3
; CCCT 1.3, 1.4 )
20. Identify
the various components (radiation sources, wavelength selectors, entrance and
exit slits,
sample containers, radiation detectors) of optical instruments. (INSTAC 1, 4 ; NSTA 1, 2, 3, 4 ;
CCCT 1.3, 1.4, 2.2 )
21. Use
ultraviolet/visible spectroscopy for quantitative analysis. (INSTAC 1, 4 ; NSTA 1, 2, 3, 4 ; CCCT
1.4 )
22. Identify
the various forms of atomic spectroscopy and their uses. (INSTAC 1, 4 ; NSTA 1, 2, 3, 4, 7 ;
CCCT 1.2, 1.4, 1.6, 2.2 )
23. Calculate
the sensitivity (characteristic concentration) of a Flame Atomic Absorption
Spectrophotometer and the sensitivity (characteristic mass) of a
Graphite Furnace instrument.
(INSTAC
1 ; NSTA 1, 3, 4 ; CCCT 1.4, 2.6 )
24. Understand
what is happening to the sample in the graphite tube during each of the five
steps of a
Graphite Furnace method. (INSTAC 1, 4 ; NSTA 1, 3, 4 ;
CCCT 1.1, 1.3, 1.4, 2.6 )
25. Identify
the various components ( nebulizers, atomizers, radiation sources, monochromators,
radiation detectors) of
flame atomic absorption and graphite furnace atomic absorption
instruments.
(INSTAC
1, 4 ; NSTA 1, 2, 3, 4 ; CCCT 1.1, 1.3, 1.4, 2.6 )
26. Identify
the infrared region of the electromagnetic spectrum and understand what
information is
obtained from it. (INSTAC 1, 4 ;
NSTA 1, 2, 3 ; CCCT 1.1, 1.3,
2.6 )
27. Connect
the theoretical ideas of the classical model and quantum mechanical model of
infrared
spectroscopy with molecular structure. (INSTAC 1,4 ; NSTA 1, 2, 3, 4, 5, 7 ; CCCT 1.3, 1.5, 2.6 )
28. List
the two necessary conditions for infrared absorbance. (INSTAC 1,4 ; NSTA 1, 2, 3 ; CCCT 1.1,
1.3, 2.6 )
29. Predict
which infrared sample handling technique is best suited for the analysis.
(INSTAC
1, 4 ; NSTA 1, 2, 3, 4, 7 ; CCCT 1.1, 1.3, 1.5, 2.6 )
30. Describe
a modern Fourier-Transform Infrared Spectrometer, including the interferometer,
and how it
collects data. (INSTAC 1, 4
; NSTA 1, 2, 3, ; CCCT 1.1, 1.3, 2.6 )
31. Recognize
how nuclear magnetic resonance spectroscopy differs from the other
spectroscopic
techniques. (INSTAC 1, 4 ;
NSTA 1, 2, 3, 4, 7 ; CCCT
1.1, 1.3, 1.4, 2.6 )
32. Calculate
the resonance frequency, the number of magnetic energy states and the magnetic
quantum
number for each state of a particular isotope. (INSTAC 1, 4 ; NSTA 1, 2, 3, ; CCCT 1.1, 1.3, 1.4, 2.6 )
33. Describe
the function of each component of a Nuclear Magnetic Resonance Spectrometer.
(INSTAC
1,4 ; NSTA 1, 2, 3, 4 ; CCCT 1.1, 1.3, 1.4, 2.2 )
34. Use
chemical shifts and multiplets from spin-spin splitting to predict molecular
structure of
compounds from Nuclear Magnetic Resonance spectra. (INSTAC 1, 4 ; NSTA 1,
2, 3 ; CCCT 1.2, 1.4,
1.6, 2.2 )
35. Classify
the various chromatographic techniques by their mobile phases and mode of
separation.
(INSTAC
1, 4 ; NSTA 1, 2, 3, 4 ; CCCT 1.2, 1.4, 1.5, 2.5, 2.6 )
36. Understand
the difference between gas chromatography and liquid chromatography and what
kind of
samples are best analyzed by each technique. (INSTAC 1, 4 ; NSTA 1, 2, 3, 4 ; CCCT 1.2, 1.3, 1.4, 1.6,
2.2, 2.6 )
37. Calculate
linear velocity of the mobile phase, the number of theoretical plates, the
plate height and the
resolution for a chromatographic column. (INSTAC 1, 4 ; NSTA 1, 2, 3, 4 ; CCCT 1.2, 1.3, 1.4, 1.6, 2.2,
2.6
)
38. Interpret
van Deemter plots and how they illustrate column processes and band broadening.
(INSTAC
1,4 ; NSTA 1, 2, 3, 4 ; CCCT 1.2, 1.3, 1.4, 2.2 , 2.3, 2.6 )
MODES OF LEARNING:
Class lecture and discussion; problem solving; analytical
troubleshooting; experiment design; acquisition and both quantitative and
qualitative interpretation of spectroscopic and chromatographic data.
COURSE CONTENT OUTLINE:
|
CHAPTER |
TOPIC |
NUMBER OF LECTURES |
|
|
|
|
|
|
INTRODUCTION |
|
|
1 |
Introduction to
instrumental methods, classification of instrumental techniques, basic
functions of instrumentation, performance characteristics of instruments |
3.5 lectures |
|
5 |
Signals and noise, sources
of noise in Instrumental Analysis, Signal to Noise enhancement, software
methods for signal to noise enhancement |
1.5 lectures |
|
|
|
|
|
|
SPECTROSCOPIC TECHNIQUES |
|
|
|
|
|
|
6 |
Properties of
electromagnetic radiation, the wave-particle duality of nature, absorption
and emission of radiation |
2.75 lectures |
|
7 |
Components of instruments
for Optical Spectroscopy |
3 lectures |
|
13 |
An introduction to
Molecular ultraviolet/visible and near-infrared absorption spectroscopy,
fundamental laws of photometry |
1 lecture |
|
14 |
Applications of
ultraviolet/visible molecular absorption spectrometry, single component
analysis, multicomponent analysis, method of standard additions |
1.25 lectures |
|
|
|
|
|
|
MIDTERM EXAMINATION |
|
|
|
|
|
|
16 and 17 |
Infrared Absorption
Spectroscopy, theory, models, sample handling techniques, instrumentation,
classical dispersive and modern Fourier-Transform |
5.25 lectures |
|
8 and 9 |
Atomic Spectroscopy based
upon Flame and Electrothermal Atomization, atomic line widths, atomization,
nebulization, sensitivity, interferences, components of instruments,
interpretation of infrared spectra |
4.25 lectures |
|
19 |
Nuclear Magnetic Resonance
Spectroscopy, theory,relaxation, continuous wave and pulsed
(Fourier-Transform) instruments, NMR spectra and molecular structure, the
chemical shift, spin spin splitting, identification of compounds by NMR
spectroscopy |
3.75 lectures |
|
|
|
|
|
|
CHROMATOGRAPHIC
TECHNIQUES |
|
|
|
|
|
|
26 |
Introduction to Chromatographic
techniques, classification of chromatographic methods, qualitative and
quantitative aspects of chromatography, plate theory and rate theory, the van
Deemter equations |
2.25 lectures |
|
27 |
Gas Chromatography |
If time allows |
|
28 |
High Performance Liquid Chromatography |
If time allows |
|
|
|
|
|
|
FINAL EXAMINATION |
|
REQUIRED TEXT:
Principles of Instrumental Analysis, Fifth Edition, D.A. Skoog, F.J. Holler, T.A. Nieman, Saunders
College Publishing (1998) ISBN: 0-03-002078-6
Chemistry Experiments for Instrumental Methods, D.T.Sawyer, W.R. Heineman, J.M. Beebe, J. Wiley (1984)
ISBN: 0-471-89303-X
COURSE REQUIREMENTS:
Students will be expected to read the assigned chapters in the textbook
prior to classroom lecture and to attempt the suggested problems for each
chapter listed on the syllabus.
The suggested problems are found at the end of each chapter in the
textbook and are representative of the material in that chapter that the
professor believes is most important for the student to understand. It of course follows that these are
also the types of questions and problems that will appear on the midterm and
final examinations.
There will be two examinations in the course; a midterm and a final
examination. The examination
questions will be taken directly from the material covered in class. There will be both questions requiring
short answers or descriptions of instrumental techniques and quantitative
problems similar to the suggested problems in the textbook. Both exams will be two hours long; the
midterm will cover the first half of the course and the final examination will
cover only material from the midterm to the end of the course.
Students are required to complete all laboratory experiments. The students normally work in teams in
the laboratory but the laboratory reports must be done by the individual
students alone. The reports are
due two weeks after completion of the laboratory experiment. It is the policy of the Chemistry
Department at Southern Connecticut State University that, to receive a passing
grade in any chemistry course with a laboratory component, the student must
pass the laboratory section of the course. A passing grade for the laboratory portion of CHE 440 is
sixty (60%) per-cent.
EVALUATION CRITERIA:
Mid-Term
Examination 30
%
Final
Examination 30%
Laboratory
Reports 40%
Total 100%
The actual letter grade will be based on the grading scale listed below
with the possible adjustment for class average at the end of the semester (if
necessary).
>95 % A+
87 – 94 % A
82 – 86 % A-
75 – 81 % B+
70 – 74 % B
66 – 69 % C+
61 – 65 % C
58 – 60 % C-
55 – 57 % D+
52 – 54 % D
50 – 51 % D-
<50 % F
|
STANDARDS
GUIDELINES |
||
|
INTASC
[Interstate New Teachers' Assessment & Support Consortium] Scholarship 1. Knowledge of
subject matter 3. Instruction adapted
to meet diverse learners 4. Use of multiple
instructional strategies & resources
Attitudes 5. Effective learning
environment created 7. Lesson planning Integrity 8. Reflection and
professional development Leadership Service
|
Professional Standards National
Science Teacher's Association 1. Content -
Structure and interpret the concepts, ideas and relationships in science 2. Nature of Science -
Define the values, beliefs and assumptions inherent to the creation of
scientific knowledge within the scientific community 3. Inquiry -
Formulating solvable problems, constructing knowledge from data, exchanging
information for seeking solutions, developing relationships from empirical
data 4. Context of Science
- Relate science to daily life: technological, personal, social and cultural
values. 5. Skills of Teaching
- Science teaching actions, strategies and methodologies, interaction with
students, effective organization and use of technology. 6. Curriculum -
Extended framework of goals, plans, materials and resources for instruction. 7. Social Context -
Social and community support network, relationship of science to needs and
values of the community, involvement of people in the teaching of science. 8. Assessment -
Alignment of goals, instruction and outcomes, evaluation of student learning. 9. Environment for
Learning - Physical spaces for learning, psychological and social
environment, safety in science instruction. 10. Professional
Practice - Knowledge and participation in the professional community, ethical
behavior, high quality of science instruction, working with new colleagues as
they enter the profession. |
CCCT {CONNECTICUT
COMMON CORE OF TEACHING] DEMONSTRATIONS OF KNOWLEDGE 1.1 understanding of
student learning & development
1.2 understanding of
need for different learning approaches
1.3 proficiency in reading, writing and mathematics 1.4 understanding of central concepts & skills,
tools of inquiry and structures of discipline(s) 1.5 knowledge of how to design and deliver
instruction 1.6 recognition of need to vary instructional
methods APPLICATION OF KNOWLEDGE THROUGH 2.1 instructional
planning based upon knowledge of subject, students, curriculum &
community 2.2 selection and/or
creation of learning tasks that make subject meaningful for students 2.3 establishment and
maintenance of appropriate behavior standards and creation of positive
learning environment 2.4 creation of
instructional opportunities supporting studentsÌ academic, social and
personal development 2.5 use of verbal,
nonverbal and media communication fostering individual and collaborative
inquiry 2.6 employment of
various instructional strategies in support of critical thinking, problem
solving and skills demonstration
2.7 use of various
assessment techniques to evaluate student learning & modify
instruction DEMONSTRATION OF PROFESSIONAL RESPONSIBILITY
THROUGH: 3.1 professional
conduct in accordance with the Code of Professional Responsibilities for
Teachers 3.2 shared
responsibility for student achievement and well-being 3.3 continuous
self-evaluation regarding choices & actions on students and school
community 3.4 commitment to
professional growth 3.5 leadership in the school community 3.6 demonstrations of
a commitment to students and a passion for improving the profession |
If any student has a particular disability-related need in order to
participate in this course, such as, special seating, note-taking assistance,
use of tape-recorders, or modified examination conditions, please let me know
as soon as possible so that appropriate accommodations can be made. The student will need to make an
appointment with the Disability Resource Center located in EN B 222 to arrange
for approved accommodations However, if you have other information you wish to
speak to me about, if you have emergency medical information to share with me,
or if you need special arrangements in case the building must be evacuated,
please make an appointment with me as soon as possible. My office is located in Jennings Hall
(JE 305) and my office hours are listed on the first page. Every effort will be made to
accommodate students in this course.
Missed/Late Work:
The formal written laboratory reports are due two (2) weeks after the experiment has been completed. Late laboratory reports will have five (5) points taken off for each day late, the first time. The second time a laboratory report is late, ten (10) points a day will be taken off, etc. Remember that, it is SCSU ës Chemistry Department policy that the student must pass the laboratory portion of a course, to pass the course.
Make-up examinations will only be given in the case of substantiated illness (a doctorís note is required). In this case, the student must inform the professor of his/her illness BEFORE the exam.
Inclement Weather:
When inclement weather threatens, call the Universityís WeatherChek voice mail system at 203-392-SNOW to hear the latest official information on possible delayed openings, class cancellations or the closing of the University. If a scheduled examination is postponed due to inclement weather (or for any reason), that examination will be given the next time that the class meets. If a laboratory session is cancelled for any reason, it will be made-up the following Tuesday.
Attendance:
Regular and prompt attendance of scheduled classes and laboratory sessions is necessary for the student to derive the intended benefit of the learning experience the college strives to provide and for the optimization of the studentís academic progress. This especially impacts itself in a course like chemistry, where every dayís lecture requires that the student has given consideration and attempted to come to grips with the material discussed in the preceding class session.
Cell Phones:
All cell phones and pagers must be turned off during the lecture. Students who ignore this policy will be asked to leave the classroom. If you are on call for work related emergencies or personal reasons, please switch to a mode that will not disturb the class (i.e. vibrate mode) and inform the professor prior to class.
Academic Dishonesty:
The student is challenged to put forth a maximum effort while preparing for this class. As with any worthwhile endeavor, the more the student puts in, the more that they will get out, i.e., learn from the actual experience. The professor will, concurrently, be putting forth a maximum effort to bridge any gaps between preparation and performance, so that the studentís maturity, creativity and curiosity as students of Analytical Chemistry may be developed, encouraged and stimulated.
In this vain, cheating in any form will not be tolerated Academic dishonesty is defined in the SCSU Student Handbook and other University publications and includes either giving or receiving information on homework assignments, mid-term or final examinations and laboratory reports. As a minimum, a grade of zero will be given as a result of cheating on any one assignment. Continued evidence of academic dishonesty may result in expulsion from the course.
The studentís cooperation and consideration of these
guidelines is essential for maximum fruition of the learning experience.