Instrumental Analysis

Instrumental Analysis
Lecture Syllabus, Fall 2014
General Information
Dates and Times
CHEM 4233 31 Instrumental Analysis
CHEM 7733 91 Instrumental Analysis
Tuesday 12:55 PM – 3:25 PM, Science Building, Room 18
Description
The Instrumental Analysis lecture course comprises the fundamentals of modern instrumental analysis. Selected topics in the theory and applications of absorption, emission,
interpretive spectroscopy, electrochemistry, and chromatography are studied. The concepts
of interfacing, data acquisition, and data analysis are introduced. Topics covered are outlined in “Objectives and Expected Learning Outcomes”. If time permits, other topics and
techniques are discussed. The content of this course overlaps many fields, and thus spans
areas that are valuable to students in the fields of chemistry, biology, physics, pharmacy,
medicine, engineering, environmental science, forensics, etc.
Prerequisite: Completion of Physical Chemistry II (CHEM 3242 or CHEM 5242).
Objectives and Expected Learning Outcomes
Each student:
• gains proficiency in the scientific areas
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•
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•
•
•
•
•
•
•
•
calibration methods
electrical components, circuits, digital electronics, and computers
signals and noise
spectrometric methods
optical instruments and methods
atomic absorption and emission spectrometry
fluorescence spectrometry
ultraviolet-visible spectrometry
infrared spectrometry
Raman spectroscopy
nuclear magnetic resonance spectroscopy
atomic and molecular mass spectroscopy
chromatographic separation
gas and liquid chromatographic methods
• enhances his or her
• ability to work independently on detailed scientific problems
• critical and analytical thinking skills, and problem solving ability
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Contact Information
Alexey Teslja, Ph.D., Associate Professor
Office Hours†
Office: Science S21 (second floor)
Tuesday 3:30 PM – 6:30 PM
E-mail: [email protected] (best for contact)
Phone: (973) 443-8783; FAX: (973) 443-8795
Website: http://alpha.fdu.edu/~ateslja
†
A student who cannot attend scheduled office hours due to a class conflict should e-mail
Dr. Teslja to schedule an appointment.
Mrs. Camilla Coniglio, Departmental Administrative Assistant
Office: Science Building Main Office (first floor)
Phone: (973) 443-8778
E-mail: [email protected]
Textbook and Materials
• Principles of Instrumental Analysis (Sixth Edition) by Douglas A. Skoog, F. James
Holler, and Stanley R. Crouch; Thomson Brooks/Cole, 2007 (Hardcover print version;
non-digital).
• Two scientific calculators.
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Guidelines
Academic Integrity Policy
Each student must carefully review the FDU Academic Integrity Policy. The FDU Academic
Integrity Policy is available at: http://www.fdu.edu/academicintegrity
Academic Accommodations
“Syllabus Disability Statement” from the office of the Disability Support Services [DSS] at
FDU:
“Any student with documented disabilities, who feels he/she may need academic
accommodations while taking this course, should first contact the office of Disability Support Services at 973-443-8079 to discuss his/her specific needs. Once
the disability is verified, pick-up your letters from the office of Disability Support
Services, then make an appointment to see the professor.”
A student who receives academic accommodations through DSS must set up an appointment
to meet with the instructor in a confidential environment as soon as possible, and must
provide the DSS accommodation letter. An extended time academic accommodation for one
course is not a valid excuse to show up late for another course; it is the responsibility of the
student to notify all instructors and resolve any potential schedule conflicts well in advance.
Assessment
Depending on the course, a variety of assessment types is used: exams, quizzes, reports,
performance, etc. The assignment of weights to assessment types is shown in “Assessment
Type Weights”, and a description of the application of a curve and numerical score to letter
grade conversion is shown in “Application of a Curve”.
Quizzes and Exams
Quizzes may be specific or cumulative, and quizzes are usually unannounced. Exams are
cumulative, and exam dates are indicated on the Course Calendar. The Final Exam is
cumulative and is given at the time and on the date determined by the University. There
may be no communication between students during quizzes or exams, for it is considered
cheating. If a student has a question when taking a quiz or exam in class, he or she must
raise his or her hand to notify the instructor. Students may not share calculators during a
quiz or exam.
Reports
For each experiment, the instructor indicates whether the laboratory report is to be completed individually, or by the assigned laboratory group.
If the report is to be completed individually, then a student may not collaborate, work together, or discuss his or her report with anyone else except for the course instructor. A
student receives a grade of zero (0) if his or her report is not submitted before the deadline.
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If the report is to be completed by the laboratory group (as a team effort), then the group
may not collaborate, work together, or discuss the report with anyone else outside the group
except for the course instructor. The instructor assigns one group member as the group
representative; the group representative submits the group’s report. The entire group receives
a grade of zero (0) if the report is not submitted before the deadline.
Performance
Laboratory performance assessment is based on the safety, preparation, efficiency, skills,
punctuality (both at the start and end of class), and record keeping (laboratory notebooks
may be inspected and assessed at any time).
Other
Other types of assessments, such as presentations.
Graded material
Graded material is distributed when class is in session. Any questions regarding a possible
grading error on returned material must be addressed to the instructor in person within
three business days after the material is returned.
Absence
A student receives a grade of zero (0) for an unexcused missed quiz or exam. To be excused
from a quiz or exam, a student must provide a letter from the Office of the Dean of Students
at Becton College on official letter-head (or an e-mail sent to the instructor from the Dean’s
office) indicating the specific date or dates for which the Dean has requested the instructor
to excuse the student.
Application of a Curve
A curve may be applied to raw grades of an assessment type population, to a distinct subset
of an assessment type, and/or to cumulative weighted average grades. Application of a curve
is done at the discretion of the instructor. For example, a curve applied to a series of grades
(x1 , x2 , x3 ... xi ) is done in the following way:
The mean (¯
x) and standard deviation (s) of the series of grades are computed, and Equation
1 is used to assign each student a z value.
zi =
xi − x¯
s
(1)
The instructor inspects the z scores and assigns to the class a new value for the mean (µ),
and a new value for the standard deviation (σ). Equation 2 is then used to calculate each
student’s curved numerical grade (ci ).
ci = σzi + µ
(2)
Curved grades are mapped to letter grades using the table shown below. Calculations are
usually performed with a spreadsheet so that rounding does not influence the mapping.
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Numerical
Letter grade
Letter grade
score (ci )
(undergraduates) (graduates)
93 ≤ n
A
A
90 ≤ n < 93
A−
A−
87 ≤ n < 90
B+
B+
83 ≤ n < 87
B
B
80 ≤ n < 83
B−
B−
77 ≤ n < 80
C+
C+
73 ≤ n < 77
C
C
70 ≤ n < 73
C−
C
60 ≤ n < 70
D
F
0 ≤ n < 60
F
F
For courses with a graduate and undergraduate student population, the graduate student
subset is separated from the undergraduate subset prior to the application of a curve. Since
each student’s z value (Equation 1) depends on his or her relative position within the population, the curving process discourages academic unscrupulousness.
Accounts
• Students must set up and maintain their FDU Novell, FDU WebCampus, FDU student
e-mail, and FDU linked Google services accounts. Students unsure about how to do
this must contact FDUTAC.
• FDU University Technical Assistance Center [FDUTAC]
http://view.fdu.edu/default.aspx?id=1513
• Students must use their student.fdu.edu e-mail account to send e-mail to the course
instructor (“[email protected]”); formal style should be used when composing each e-mail.
E-mail sent from a non-FDU address is likely to be tagged as spam resulting in delays
or automatic deletion. The instructor generally replies to an e-mail within one to two
business days.
• Students should ensure that e-mail received from the instructor (“[email protected]”) and
the class mailing list (course-ID#@class-list.fdu.edu) is not marked as spam by their
e-mail client or e-mail server. Students unsure about how to do this must contact
FDUTAC.
• Although FDU students access Google services with a student.fdu.edu e-mail address
and password, this service is not available to faculty members at FDU. Thus, the
instructor uses his own Google account ([email protected]) for distributing some
course items via Google Drive (http://drive.google.com). Students must not send email
to [email protected]; all e-mail to the instructor should be directed to [email protected]
only. The link to the Google Drive folder is maintained on the instructor’s website,
and accessible via the students student.fdu.edu e-mail address and password.
General
• The Syllabus may be revised (or periodically updated) and posted on the instructor’s
website as a PDF file. Students are notified in class or via e-mail, and it is the
responsibility of each student to download and read the updated Syllabus.
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• The Course Calendar may be modified as the course proceeds, and each student is
expected to abide by any modifications.
• For some courses, a list of homework exercises is posted in the Syllabus and may be
updated as the semester proceeds.
• Supplementary material is provided on-line as necessary via the instructor’s website
or via the course folder on Google Drive. Files are usually in text or PDF file format,
most PDF readers are available at no cost.
• The following programs may be useful: GNU Octave (no cost), LibreOffice (no cost),
OpenOffice (no cost), LATEX(no cost), PrimoPDF (no cost), Adobe Acrobat Reader
(no cost), ACD ChemSketch (no cost), Matlab, Maple, Mathematica, Microsoft Office,
and Graphical Analysis. Each program has its own advantages and disadvantages.
• Except for scientific calculators, use of all other electronic devices (cell phones, smart
phones, pads, computers, etc.) is not permitted during class.
• Students must always arrive to class on time. Extra time is not given for a student
who arrives late.
Assessment Type Weights
Type
Quizzes
Final Exam
Updated: December 8, 2014
Weight (%)
70
30
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Course Calendar
Week
1
2
3
4
5
6
7
—
8
9
10
11
12
13
14
—
Date (2014)
Aug. 26
Sep. 2
Sep. 9
Sep. 16
Sep. 23
Sep. 30
Oct. 7
Oct. 14
Oct. 21
Oct. 28
Nov. 4
Nov. 11
Nov. 18
Nov. 25
Dec. 2
Dec. 12
Chapter(s)
A1, 1
1, 2
2, 3, 4, 5
5, 6, 7
7, 8
9
13, 14
—
16, 17
15, 18
19
11, 20
26
27
28
—
Notes
Homework C1 due
Fall Recess
Homework C2, C3, C4, C5, C6, C13 due
Homework C7, C14, C16, C17 due
Homework C8, C9, C15, C18 due
Homework C19 due
Homework C11, C20 due
Homework C26 due
Homework C27 due
Final Exam
Friday 12:30 – 2:30 PM
Homework is handed directly to the instructor at the start of class on the date shown in the
Course Calendar. Complete solutions to the assigned homework problems are hand-written
clearly on standard white “printer paper” using blue or black non-erasable pen; the student’s
name is written on the top of each page, and pages (per chapter) are stapled together.
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Chapter
1
2
3
4
5
6
7
8
9
11
13
14
15
16
17
18
19
20
26
27
28
A1
Chapter title (Skoog, Holler, and Crouch; Sixth Edition)
“Introduction”
“Electrical Components and Circuits”
“Operational Amplifiers in Chemical Instrumentation”
“Digital Electronics and Computers”
“Signals and Noise”
“An Introduction to Spectrometric Methods”
“Components of Optical Instruments”
“An Introduction to Optical Atomic Spectrometry”
“Atomic Absorption and Atomic Fluorescence Spectrometry”
“Atomic Mass Spectrometry”
“An Introduction to Ultraviolet-Visible Molecular Absorption Spectrometry”
“Applications of Ultraviolet-Visible Molecular Absorption Spectrometry”
“Molecular Luminescence Spectrometry”
“An Introduction to Infrared Spectrometry”
“Applications of Infrared Spectrometry”
“Raman Spectroscopy”
“Nuclear Magnetic Resonance Spectroscopy”
“Molecular Mass Spectrometry”
“An Introduction to Chromatographic Separations”
“Gas Chromatography”
“Liquid Chromatography”
“Evaluation of Analytical Data”
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Homework Exercises
A1 a1-1, a1-2, a1-3, a1-4, a1-5, a1-6, a1-7, a1-8, a1-9, a1-10, a1-11, a1-12, a1-13, a1-14,
a1-15, a1-19, a1-20, a1-21, a1-24
C1 1-1, 1-2, 1-3, 1-4, 1-5, 1-6, 1-7, 1-8, 1-9, 1-10, 1-11
C2 2-1, 2-2, 2-3, 2-4, 2-5, 2-6, 2-7, 2-8, 2-9, 2-10, 2-11, 2-12, 2-13, 2-14, 2-15, 2-16, 2-17,
2-18, 2-19, 2-20
C3 3-1, 3-2, 3-3, 3-6, 3-10(a-c), 3-11
C4 4-1, 4-2, 4-3, 4-4, 4-5, 4-6, 4-8, 4-9, 4-11, 4-12
C5 5-1, 5-2, 5-3, 5-4, 5-5, 5-6, 5-7, 5-8, 5-9, 5-10
C6 6-1, 6-2, 6-3, 6-4, 6-5, 6-6, 6-7, 6-8, 6-9, 6-10, 6-11, 6-12, 6-13, 6-14, 6-15, 6-16, 6-17,
6-18, 6-19
C7 7-1, 7-2, 7-3, 7-4, 7-5, 7-6, 7-7, 7-8, 7-9, 7-11, 7-12, 7-13, 7-14, 7-16, 7-17, 7-18, 7-19,
7-20, 7-22, 7-23
C8 8-1, 8-2, 8-3, 8-4, 8-5, 8-6, 8-7, 8-8, 8-9
C9 9-1(a,b,c,d,e,f,g,h,i,j,l), 9-2, 9-3, 9-4, 9-5, 9-6, 9-7, 9-8, 9-9, 9-10, 9-11, 9-12, 9-13, 9-14,
9-19, 9-20
C11 11-1, 11-2, 11-3, 11-4, 11-5, 11-6, 11-7, 11-8
C13 13-1, 13-2, 13-3, 13-4, 13-5, 13-6, 13-7, 13-8, 13-9, 13-10, 13-11, 13-13(a,b,c,d,e,g,h),
13-14, 13-16, 13-17, 13-18, 13-19, 13-20, 13-22, 13-23
C14 14-1, 14-2, 14-6, 14-7, 14-8, 14-9, 14-10, 14-11, 14-12, 14-13, 14-14, 14-15, 14-16, 14-18,
14-23(a)
C15 15-1, 15-2, 15-3, 15-4, 15-5, 15-6, 15-7, 15-9, 15-10, 15-15
C16 16-1, 16-2, 16-3, 16-4, 16-5, 16-6, 16-7, 16-8, 16-9, 16-10, 16-11, 16-13, 16-14
C17 17-1, 17-6, 17-7, 17-9, 17-10
C18 18-1, 18-2, 18-3, 18-4, 18-5, 18-6, 18-7, 18-8
C19 19-1, 19-2, 19-3, 19-4, 19-5, 19-6, 19-7, 19-8, 19-9, 19-10, 19-11, 19-12, 19-13, 19-15,
19-16, 19-17, 19-23, 19-24, 19-25, 19-38, 19-39, 19-40
C20 20-1, 20-2, 20-3, 20-4, 20-5, 20-6, 20-7, 20-8, 20-9, 20-11, 20-12
C26 26-1, 26-2, 26-3, 26-4, 26-5, 26-6, 26-7, 26-8, 26-9, 26-10, 26-11, 26-12, 26-13, 26-14,
26-15, 26-16, 26-17, 26-18, 26-19, 26-20, 26-21
C27 27-1, 27-2, 27-3, 27-4, 27-5, 27-6, 27-8, 27-9, 27-10, 27-11, 27-12, 27-14, 27-15, 27-16,
27-17, 27-18, 27-22(a,b,c,d), 27-23
C28 28-1, 28-2, 28-3, 28-4, 28-5, 28-6, 28-7, 28-8, 28-9, 28-10(a), 28-12, 28-13, 28-14, 28-15,
28-16, 28-17, 28-18, 28-19, 28-20, 28-21, 28-22
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Supplemental Reading
A Complete Introduction to Modern NMR Spectroscopy, Roger S. Macomber, Wiley-Interscience,
2008, ISBN-13: 978-0471157366.
An Introduction to Error Analysis: The Study of Uncertainties in Physical Measurements, John
R. Taylor, University Science Books, 2 ed., 1996, ISBN-13: 978-0935702750.
Atomic Spectra and Atomic Structure, Gerhard Herzberg, Dover Publications; 2 ed., 2010, ISBN13: 978-0486601151.
Basic Gas Chromatography, Harold M. McNair and James M. Miller, Wiley-Interscience; 2 ed.,
2009, ISBN-13: 978-0470439548.
Introduction to Mass Spectrometry: Instrumentation, Applications, and Strategies for Data Interpretation, J. Throck Watson and O. David Sparkman, Wiley, 4 ed., 2007, ISBN-13: 9780470516348.
Introduction to Modern Optics, Grant R. Fowles, Dover Publications, 2 ed., 1989, ISBN-13: 9780486659572.
Introduction to Quantum Mechanics, David J. Griffiths, Benjamin Cummings, 2 ed., 2004, ISBN13: 978-0131118928.
Introduction to Electrodynamics, David J. Griffiths, Benjamin Cummings; 3 ed., 1999, ISBN-13:
978-0138053260.
Microelectronic Circuits (The Oxford Series in Electrical and Computer Engineering), Adel S.
Sedra and Kenneth C. Smith, Oxford University Press, USA, 6 ed., 2009, ISBN-13: 9780195323030.
Modern Raman Spectroscopy: A Practical Approach, Ewen Smith and Geoffrey Dent, Wiley,
2005, ISBN-13: 978-0471497943.
Molecular Spectra and Molecular Structure: Electronic Spectra and Electronic Structure of Polyatomic Molecules (Volume III), Gerhard Herzberg, Krieger Publishing Company, 1991, ISBN13: 978-0894642708.
Molecular Spectra and Molecular Structure: Infrared and Raman of Polyatomic Molecules (Volume II), Gerhard Herzberg, Krieger Pub Company, 1991, ISBN-13: 978-0894642692.
Molecular Spectra and Molecular Structure: Spectra of Diatomic Molecules (Volume I), Gerhard
Herzberg, Krieger Pub Company, 2 ed., 1989, ISBN-13: 978-0894642685.
Physical Chemistry, Ira Levine, McGraw-Hill Science/Engineering/Math; 6 ed., 2008, ISBN-13:
978-0072538625.
Principles of Fluorescence Spectroscopy, Joseph R. Lakowicz, er: Springer, 2nd ed., 1999, ISBN-13:
978-0306460937.
Principles of Lasers, Orazio Svelto, Springer, 5 ed., 2009, ISBN-13: 978-1441913012.
Raman Spectroscopy for Chemical Analysis, Richard L. McCreery, Wiley-Interscience; 1 ed., 2000,
ISBN-13: 978-0471252870.
Most of these references are available at the FDU library. If the library does not have a reference,
please notify the course instructor.
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