CH332 Instrumental Analysis - Lake Superior State University

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CH332 - Instrumental Analysis Class Syllabus
Spring 2005 Semester
CH332 Instrumental Analysis (4 semester credits)
Required Text:
Quantitative Chemical Analysis, 6th Edition, by Daniel C. Harris
Laboratory Notebook
State Council of State Science Supervisors:
http://www.csss-science.org/safety.shtml
http://www.csss-science.org/downloads/scisafe.pdf
Instructor:
Dr. Barb Keller, CRW 319 (phone: 635-2438)
Office Hours:
9:00- 10:00 MWF
11:00- 12:00 MW
Course Objectives: Upon completion of this course, the student should be able to:
(Chapter emphasizing each outcome is provided.)
Chapter 14:
 Demonstrate an understanding of the basic concepts of electrochemistry by
solving pertinent problems relating to redox reactions, Ohm’s law, voltage,
work and free energy
 analyze and construct galvanic cells and solve problems relating to such a cell
utilizing standard potentials and the Nernst equation
 understand the relationship between standard potentials and chemical
equilibrium constants and demonstrate this understanding through problem
solving
Chapter 15:
 demonstrate an understanding of the workings of various types of electrodes
including reference electrodes, indicator electrodes, pH electrodes, and ionselective electrodes through problem solving and laboratory use
Chapter 16:
 analyze and construct redox titration curves
 solve redox titration problems
 demonstrate an understanding of redox indicators through problem solving
and laboratory work
 demonstrate an understanding of the use of chemical oxidants such as
potassium permanganate, cerium (IV), iodine, and sodium thiosulfate through
problem solving
Chapter 17:

conceptualize the methods of electrogravimetric and coulometric analysis
through laboratory work and problem solving
Chapter 18:
 demonstrate an understanding of the basic concepts of spectophotometry,
including the properties of light and Beer’s Law and basic instrument design,
through problem solving and laboratory work
 describe what can happen (i.e., electronic transitions, fluroescence,
phosphorescence, etc) to a molecules when it absorbs light as demonstrated
through problem solving and in class discussion
Chapter 19:
 apply Beer’s law to complex mixtures as demonstrated through problem
solving
 use a Scatchard plot to measure an equilibrium constant as demonstrated
through problem solving
 demonstrate, through in-class discussion and problem solving, an
understanding of flow injection systems, immunoassay systems, sensors based
on luminescence quenching
Chapter 20:
 demonstrate, through laboratory work and problem solving, an understanding
of the basic components that make up spectrophotometric instrumentation
(including sources of light, monochrometers, detectors, etc.)
 understand the method of Fourier transform spectroscopy and its application
to modern instruments of infrared analysis as demonstrated through problem
solving and in-class discussion and examination
 understand the basic operation of optodes and their application to analytical
chemistry as demonstrated through problem solving and in-class discussion
and examination
Chapter 21:
 demonstrate, through laboratory work and problem solving, an understanding
of the basic components that make up atomic absorption and atomic emission
spectrometric instrumentation, including sources of atomization (flames,
graphite furnace, plasmas), lamps (hallow cathode, deuterium)
monochrometers, detectors, etc.
 understand (as demonstrated through problem solving and laboratory work)
how atomic absorption and atomic emission is affected by temperature,
spectral interference, and chemical interference and how to determine
detection limits for these instruments
Chapter 22:

demonstrate through laboratory work and problem solving, an
understanding of the basic components that make up different types of
mass spectrometers
Chapter 23:
 demonstrate, through problem solving, the analytical process of
chromatography including retention time, resolution, plate height and number,
capacity factor, etc.
 demonstrate an understanding of the different types of chromatographic
separation techniques (adsorption, partition, extraction, ion-exchange, etc)
through problem solving and laboratory work
Chapter 24:
 demonstrate, through laboratory work and problem solving, an understanding
of the basic components that make up gas chromatography instrumentation,
including the various sample injection systems, columns, carrier gases,
detectors (including mass spectrometry), etc.
Grading:
Class:
Lab**:
Total:
10 - homework assignments 100 points
3 - one hour exams
300 points
1 - final exam
200 points
200 points
800 points
Extra Credit: During the semester I will offer extra credit problems totaling 20 points
that may be used to bring up your grade.
All exams MUST be taken during the scheduled time. The will be no makeup for
missed exams. Four exams will be given during the semester. I will drop the lowest
exam.
In compliance with Lake Superior State University policy and equal access laws,
disability-related accommodations or services are available. Students who desire such
services are to meet with the professor in a timely manner, preferably the first week of
class, to discuss their disability-related needs. Students will not receive services until
they register with the Resource Center for Students with Disabilities (RCSD). Proper
registration will enable the RCSD to verify the disability and determine reasonable
academic accommodations. RCSD is located in South Hall Office 206. The telephone
number is (906) 635-2454.
**It is MANDATORY that you attend the laboratory. A failing grade in the
laboratory will result in a failing grade for the class.
Class attendance is the responsibility of the student. Attendance will not be recorded.
However, it is strongly recommended that the student attend all classes as overall student
performance on the exams is usually directly related to the student’s participation in the
class.
Final Grade: You MUST attend the lab. A failing grade in the laboratory will be an
automatic failing grade for the class. The final grade will be based upon the total points
(730 points). The letter grade given will be as follows:
Points
758 to 800
720 to 757
694 to 719
671 to 693
640 to 670
614 to 639
591 to 613
560 to 590
533 to 559
510 to 532
480 to 509
508 or less
Letter Grade
A
AB+
B
BC+
C
CD+
D
DF
CH332 – Tentative Course Schedule*
Week of
Jan. 10, 2005
Chapter/Topic
Chapter 14/Fundamentals of Electrochemistry
Jan. 17, 2005
Chapter 14/Fundamentals of Electrochemistry
Chapter 15/Electrodes and Potentiometry
Chapter 15/Electrodes and Potentiometry
Jan. 24, 2005
Jan. 31, 2005
Chapter 16/Redox Titrations
Exam 1 (Chapters 14 and 15)
Feb.7, 2005
Chapter 16/Redox Titrations
Feb. 14, 2005
Chapter 17/Electroanalytical Techniques
Chapter 18/Fundamentals of Spectrophotometry
Feb. 21, 2005
Chapter 18/Fundamentals of Spectrophotometry
Exam 2 (Chapters 16, 17)
Feb. 28, 2005
Spring Break
Mar. 7, 2005
Chapter 19/Applications of Spectrophotometry
Mar. 14, 2005
Chapter 20/Spectrophotometers
Exam 3 (Chapters 18,19)
Chapter 20/Spectrophotometers
Chapter 21/Atomic Spectroscopy
Mar. 21, 2005
Mar. 28, 2005
Chapter 21/Atomic Spectroscopy
Chapter 22/Mass Spectrometry
Apr. 4, 2005
Exam 4 (Chapters 20,21)
Chapter 22/Mass Spectrometry
Apr. 11, 2005
Chapter 23/Introduction to Analytical Separations
Apr. 18, 2005
Chapter 24/Gas Chromatography
Apr. 25, 2005
Final Exam
* Note: The course syllabus represents the best estimate and projection of course
content, scope, and sequence. The syllabus is subject to change based upon the
discretion of the instructor.
Laboratory:
The laboratory is organized to allow the student experience in practical chemical
instrumental analysis. Whenever possible, the laboratory methods will employ practical
techniques of modern instrumental analysis used in academic and industrial laboratories.
Write ups for the specific laboratories will be handed out one week in advance. The
student is expected to attend the laboratory. Additionally, the student is expected to
maintain a professional laboratory notebook and to prepare type written laboratory reports
for each laboratory activity using the standard format that is provided. The laboratory
reports are due 7 days after the laboratory is completed. Late reports will be accepted
only upon permission from the instructor.
Scheduled Laboratories
Week of:
Lab
Jan 10
No lab
Jan 17
Analysis of Acid-Base Titration Curve (pH meter)
Jan 24
Potentiometric Titration of a Weak Acid (pH meter)
Jan 31
Determination of Calcium using an Ion Selective Electrode
Feb 7
Determination of Nitrate using an Ion Selective Electrode
Feb 14
Electrolytic Determination of Copper
Feb 21
Separation of Copper and Nickel by Electrolysis
Feb 28
Spring Break
Mar 7
Introduction to Spectrophotometry: Spectrophotometric
Determination of Iron
Mar 14
Spectrophotometric Determination of Nitrate Nitrogen in Water
Mar 21
Introduction to Fourier Transform Infrared Spectroscopy (FTIR)
Mar 28
Determination of Calcium by Atomic Absorption Spectrometry
Apr 4
Determination of Lead in Soil by Atomic Absorption Spectrometry
Apr 11
Demonstration of Inductively Coupled Plasma Mass Spectrometry
Apr 18
Introduction to Gas Chromatography Mass Spectrometry
Standard Format for Laboratory Reports:
All reports should be typewritten with the exception of the raw data and calculations
which may be photocopied from your laboratory notebook and legibly written into the
report by hand, respectively. The report should adhere to the general outline below.
Depending upon the nature of the experiment, the laboratory instructor may also ask you
to include additional sections in your report or may ask you to delete a section of the
report.
Outline (Format)
I. Experiment Title, Date, and Your Name
II. Purpose of the Experiment (i.e., what is the experiment designed to do?)
III. Reaction Equations (when appropriate)
IV. General Description of the Experiment and the Observations
V. Raw Data
VI. Calculations (and Graphs if applicable)
VII. Final Results or Conclusions
Safety in the Laboratory
While working in the laboratory you are expected to comply with the safety rules which
follow, any and all rules posted in the laboratory or as established by your instructor.
Violations of the safety rules endanger both yourselves and other in the laboratory.
Students who violate the established rules and procedures may be subject to warnings,
reductions in grade, or expulsion from the lab. Safety rule violations include but are not
limited to the following:
1. Laboratory eye protection is required at all times in the laboratory. Not wearing
appropriate safety goggles for the activities assigned is a violation of the safety rules.
Note: Some activities such as pouring and mixing concentrated reagents require the
used of SPECIAL chemical splash goggles and perhaps other personal protective
equipment. Consult your laboratory instructor and always use the highest level of
protection available and appropriate for the task assigned.
2. Smoking, eating, or drinking in the laboratory is prohibited.
3. Pipetting by mouth or otherwise handling chemicals unsafely is prohibited.
4. Using an open flame to heat flammable liquids is prohibited.
5. Not working under a fume hood when directed to do so is a violation of
laboratory safety and subject to actions mentioned above.
6. Failing to report or clean up chemical spills or broken equipment is a violation
of laboratory safety and subject to actions mentioned above. Special spill kits are
available in the lab to handle a variety of spilled chemicals. Consult the laboratory
instructor for guidance using these kits.
7. Disposing of chemicals improperly. ALWAYS consult the instructor for the proper
handling instructions or location of the designated chemical waste container for the
experiment.
8. Working alone in the laboratory or working outside the regularly scheduled lab
times with the permission of the instructor is prohibited.
9. Performing unauthorized experiments or mixing unknown is prohibited.
10. Engaging in horseplay or other behavior that jeopardizes your safety or the
safety of others in the laboratory is prohibited.
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