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Chemistry 461W - Experimental Chemistry F '08

The emphasis of this course is for students to apply their problem-solving skills to the analysis of "real-world" samples in a team environment. Much of the emphasis will be environmental in nature. In addition to a series of standard laboratory exercises, students will be given chemical problems to solve, and then after researching the problems by consulting the literature, they will submit a plan of action to the instructor for approval. Since extraction and sampling techniques have not been covered in detail in other courses, students will be taught the basics of solvent extraction, Solid Phase Extraction (SPE), Solid Phase Microextraction (SPME), Soxhlet extraction, and Supercritical Fluid extraction techniques. Since this class is a writing-intensive course, there will be a research proposal (PAH in creosote) and formal lab report required (Au-nanoparticles).

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Instructor
 Dr. Pete Poston
office: NS 110
phone: 838-8218
office hours: M 11, WF 1, TR 10, drop by, or make an appointment.
email questions: postonp@wou.edu
Web page: http://www.wou.edu/poston - click on "Classes" and then Ch 461
Pre-req's Ch 313 Instrumental Analysis, Ch 350 Chemical Literature, Ch 440 Physical Chemistry I, or consent of instructor

Texts & References

 Texts:

We will be borrowing from a variety of sources, including your Ch 312 and Ch 313 texts. Reading materials will be made available.

  • "Exploring Chemical Analysis", 3rd ed. by Daniel C. Harris
  • "Quantitative Chemical Analysis", 5th ed. by Daniel C. Harris
  • "Principles of Instrumental Analysis", 6th ed. by Skoog, Holler, & Nieman
  • "Laboratory Experiments in Environmental Chemistry", D. Neal Boehnke, R. Del Delumyea
  • "Modern Analytical Chemistry", by David Harvey

References:

  • "Standard Methods for the Examination of Water & Wastewater", 19th ed.
  • "Official Methods of Analysis of AOAC International", 16th ed., Vol I & II
  • "The Basics of Technical Communicating", by B. Edward Cain
  • "The ACS Style Guide", 2nd ed, Janet S. Dodd, ed.
Quizzes There are four regularly scheduled quizzes worth 25 pts each. Quizzes will be based on lecture materials, the introduction section of labs, or on assigned reading.
Lab

Lab Notebooks:

A bound notebook is required for the class to record laboratory experiments. For experiments, follow the standard format of Intro, Experimental, Results and Discussion, and Conclusions.

In addition to content, I grade notebooks based upon the following criteria:

  1. pages numbered
  2. table of contents
  3. presence of any loose papers
  4. written in pen, not pencil
  5. errors crossed out, not blacked out
  6. overall organization
  7. usage of significant figures
  8. neatness and legibility
  9. record of each step written down in an analysis

Labs must be turned in on time or else chaos ensues! The following "late fees" will be assessed starting at 8 AM the day following the due date:

1 day late = 1/4 off, 2 days late = 1/2 off, 3 days late = 3/4 off

You will receive a zero for all labs more than 3 days late. No labs will be accepted past the last day of classes. If you receive two unexcused zeros, on any two labs, you fail the course.
Writing Assignments You will write a formal lab report for the Au-nanoparticle project in the same format as taught in Ch 313. You will also write a research proposal for the analysis of PAH's in creosote. The lab notebook is considered to be the informal writing component of a writing intensive class. If you fail to turn in any of these assignments, you fail the class.
Make-ups Make-ups are always problematic in a course like this. Illnesses, family-related emergencies, and other emergencies must be communicated through the Office of Student Affairs (838-8221) and broadcast to all your professors. Under this condition, you can make-up a lab if available that week. Quizzes can be made up if not already handed back to the class. Otherwise, I will replace the missing lab or quiz with your average scores in those areas. Only one lab or quiz can be replaced this way - otherwise an incomplete can be given (see below).
Grading
200 pts (50%) Writing exercises/Research Results: PAH proposal (60 pts), Nanoparticle formal lab report (100 pts), Lab notebook (40 pts)
100 pts (25%) Lab Handouts: 5 Lab handouts (20 pts each)
100 pts (25%) 4 Quizzes (25 pts each)
400 pts Total

Grading will be no harder than:

A = 90% and higher
B = 80-89%
C = 70-79%
D = 60-69%
F less than 60%
Incompletes Incompletes are given under special circumstances such as medical reasons, family emergencies, etc. In order to receive an incomplete, you must sign a contract with me outlining the steps you must take to finish the course. Usually this means there will be a time deadline for completion of the course.
Academic Dishonesty

The Code of Student Responsibility defines cheating as "intentional use, or attempted use of artifice, deception, fraud, and/or misrepresentation of one's academic work". For this class, which involves taking exams, quizzes, and perform labs, cheating is usually but not limited to talking or writing to other students, using crib sheets (prepared notes), or looking at another student's paper. The penalty for cheating will be a zero grade for the test or quiz or assignment in question.

Students have the right to appeal this action as described in the Code of Student Responsibility
Students with Disabilities It is your right to request special accommodations under the Americans with Disabilities Act. For questions, call the Office for Disability Services at (503) 838-8250 V/TTY, or email them at ods@wou.edu.

TENTATIVE SYLLABUS (updated as we go)

Week of Lecture Topics and Quizzes Reading Lab
Sept 29
  • Liquid-Liquid Extraction
 Harris 5th ed:
  • liquid-liquid extraction:
    Ch 23 "Introduction to Analytical Separations", p. 641-644
  • Solid-Phase Microextraction (SPME):
    Ch 24 "Gas Chromatography", p. 694-696
  • Solid Phase Extraction (SPE) and Supercritical Fluid Extraction:
    Ch 28 "Sample Preparation", p. 831-834
  • Soxhlet Extraction:
    Quicktime Movie: James Hardy Animation
  • Lab Handout #1 (20 pts):
    Determination of the Octanol/Water Partition Coefficient Coefficients for Organic Pollutants
Oct 6

Quiz #1 - Liquid-Liquid Extraction (25 pts)

  • Solid Phase Extraction (SPE) and Solid Phase Microextraction (SPME)

  • Soxhlet Extraction

  • Supercritical Fluid Extraction (SFE)

---
  • Continued

 
Oct 13

Quiz #2 - SPE, SPME, Soxhlet and SFE (25 pts)

  • Surface Enhanced Raman Spectroscopy (SERS)

 

SERS:

  • Formal Lab Report (100 pts):
    The Development of a Chemical Sensor Using Au Nanoparticles and SERS

  • Lab Handout #2 (20 pts):
    Introduction to Raman Spectroscopy - written by DeltaNu, manufacturers of Infrared and Raman spectrometers

  • Lab Handout #3 (20 pts)
    Preparation and Characterization of Au Nanoparticles as a Chemical Sensor for Methamphetamine
Oct 20 --- ---
  • Continued
Oct 27 Quiz #3 - Raman Spectroscopy and SERS (25 pts) ---
  • Continued
Nov 3* --- ---
  • Writing Exercise - Proposal (60 pts):
    Proposal for the analysis of PAHs and chlorinated phenols in creosote, a common wood preservative
Nov 10
  • Quality Assurance-Quality Control (QA/QC) Techniques

 

 ---
  • Lab Handout #4 (20 pts):
    Photodegradation of Methylene Blue
Nov 17
  • Photolysis
 ---
  • Continued
Nov 24 Quiz #4 - QA/QC Techniques (25 pts) ---
  • Lab Handout #5 (20 pts):
    The Photolysis of Pentachlorophenol
Dec 1 catch-up ---
  • Continued
*Last day to drop without being responsible for a grade is Fri, Nov 7

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