Environmental Sciences 528

Analysis of Environmental Contaminants

Southern Illinois University Edwardsville

Spring 2004

Monday 6:20 - 8:00 pm (SL2224)

 

Course Instructor      

                                                                       

Dr. Kevin A. Johnson, SL 3316                                    650-5934, kevjohn@siue.edu

 

Office Hours

 

Monday after class or by Appointment.

 

Course Description

 

The course will focus on the theory and application of procedures used in the separation, detection, identification, and quantitation of toxicants in environmental samples.  Discussion of the laboratory instrumentation, procedures, and experimental methods used for identification and quantitation of toxic substances, as well as their transformation products in environmental and biological samples.

 

Course Objectives 

 

This course will emphasize the practical aspects of toxicant analysis.  In the lecture portion of the course, students will be exposed to the theories and fundamentals of chromatographic behavior, selective detection, and identification of unknown chemicals through spectroscopic characteristics and partitioning behavior.

 

Text

Kenkel, John.  2003.  Analytical Chemistry for Technicians.  3rd Ed., CRC, New York, NY.

 

There will be additional handouts as needed throughout the semester.

 

Exams and Homework

 

There will be three exams during the course of the semester.  The third exam will take place during the scheduled final exam.  There will be approximately 4 homework assignments throughout the semester.

 

Grading

 

The course grade will be weighted as follows:

                        Homework                                                       25 %

                        Exams                                                              75 %

Policy Statement: Academic Misconduct by Students

 

Faculty members retain their traditional authority to take disciplinary action in the event of academic misconduct.  Acts of academic misconduct for which students are subject to sanctions include, without limitation, plagiarism, cheating, failure or refusal to follow clinical practice standards, falsifying or manufacturing scientific or scholarly experiments or research, and soliciting, aiding, abetting, concealing, or attempting such acts.

 

Plagiarism is defined as including, without limitation, the act of representing the work of another as one’s own.  Plagiarism may consist of copying, paraphrasing, or otherwise using written or oral work of another without proper acknowledgment of the source or presenting oral or written material prepared by another as one’s own.

 

In the event of academic misconduct, the instructor may request the Student Assessments and Standards Committee of the Environmental Sciences Program to impose on a student the sanction of a failing grade on an individual assignment or on the course as a whole.  The Director of the Program may recommend to the dean of Students other sanctions, such as dismissal from a major or from the University.

 

Students with disabilities:

 

Persons with documented disabilities should visit the Disability Support Services Office, located in Peck Hall, room 1311, at their earliest convenience to meet the director and discuss available services.  The student should also, make an appointment with the instructor as soon as possible to discuss any special arrangements.
Tentative Lecture Schedule

 

Date

Topic

Suggested Reading

January

 

 

12

Course overview, Risk Assessment, QA-QC

S-0, S-1

19

NO CLASS, ML King day

 

26

Physical properties: (polarity, solubility, Kow, volatility, vapor pressure, Henry’s)

S-2, S-3

February

 

 

2

Extraction & cleanup methods, Principles of chromatography

B-2,6,11, S-4

 

Methods of Separation

 

09

Gas chromatography: Analyte/analytical requirements, measures of efficiency, modes

S-5, B-12

16

Gas chromatography: columns and stationary phases, detectors

 

23

Exam I,  Liquid chromatography: Comparison to GC, measures of efficiency, packing material

 

March

 

 

1

Liquid chromatography

B-13

08

NO CLASS, Spring Break

 

15

Liquid chromatography: Modes, stationary phases, instrumentation, Detectors

 

 

Methods of Detection

 

22

Mass spectrometry: Theory & ionization techniques

S-7

19

Exam II, Mass Spectrometry  

 

April

 

 

05

Mass spectrometry: Common fragments & isotopic ratios

S-6

12

Atomic spectroscopy: Atomic absorbance

B-7,9

19

Atomic spectroscopy: Atomic absorbance instrumentation

 

26

Enzyme-Linked Immunosorbent Assays

S-9

May 03

Final

 

 

S = Supplementary Reading

B = Course Book

 

The following will be helpful for lecture performance

 

Unit conversions

 

Many conversions of units will be necessary throughout the course.  Recall the metric prefixes.  Some of you may not be familiar with the low end: pico- (10-12) and femto- (10-15).  Concentrations of solutions used in instrumental analysis are frequently expressed in ng/µl (nanograms per microliter), which is also, though somewhat inaccurately, expressed as ppm.  Strictly speaking, ppm is weight to weight or volume to volume, and our solutions are actually weight to volume.  Solutions expressed as a percent of one compound in another should indicate if the proportions are weight to weight (W/W), or weight to volume (W/V).  For accuracy in reports, use the proper units for the reported data.

 

Calculations

 

Make sure you are able to calculate, for example, a 0.2 mg/ml solution of a chemical in a solvent (what is a practical weight and volume to use?), and how much of this solution should be added in fortification of a 25 ml water sample to yield, after extraction and solvent reduction to a 2 ml final volume, a final concentration of 3 ng/µl.  Also, what is the concentration in the water itself after it is fortified?  If you find a 0.8 ng/µl concentration of a pesticide by gas chromatography, and it was from the analysis of a 5 ml final volume extract from a 3 g avian GI sample, what was the concentration in the GI tissue?  If the whole bird weighed 500 g, what was the dose to the bird, assuming the entire dose was represented by the GI contents?  Make sure you aren't going to have any trouble with these kinds of calculations and conversions before you need to use them in the laboratory or in reports.

 

 

 

 

 

 

 

Key for the Calculations

 

Weights should be at least 10 mg for the balances we ordinarily use.  This allows concentrations with 3 significant figures.  For a 0.2 mg/ml solution, this would require a volume of 50 ml for a 10 mg weight.  You generally want to generate the minimum volume of solution possible, as the excess must be disposed of as hazardous waste.

 

At 3 ng/µl, 2 ml of solution will contain 6 µg.  You will need to add 30 µl of a 0.2 mg/ml solution to the water to obtain this final concentration.  The water itself upon fortification will be at a concentration of 6 µg/25 ml, which would be 0.24 µg/ml.

 

At 0.8 ng/µl, the final 5 ml solution contains 4 µg of the compound.  The concentration in 3 g tissue would be 4 µg/3 g, which would be 1.33 µg/g or 1.33 ppm.  The dose for the whole bird would be 4 µg/500 g, which would be 8 ng/g or 8 ppb.