Analytical Techniques (Chemistry 442) Lecture and Laboratory Syllabus Spring 2016 Lecture Instructor: Dr. E. McJimpsey, Department of Chemistry, Visiting Professor Office: Currens Hall 519D, phone number: 309.298.3271, and e-mail: EL-Mcjimpsey@wiu.edu Office Hours: T & R. 9:00-11:00am Lecture: MWF 12:00-12:50pm, Currens Hall 202 Lab Instructors: Dr. E. McJimpsey (January 19-March 3, 2016) Dr. L. Song, (March 8-April 26, 2016) Currens Hall 324B, office hours: MWF 10-11am, e-mail: L-song@wiu.edu, phone number: 309.298.656 Laboratory: TA: Sangeetha Mylapurapu (s-mylapurapu@wiu.edu) Section 21- Tues. 11:00am-1:50pm, Currens Hall 419 Section 22- Thurs.11:00am-1:50pm, Currens Hall 419 Chem 442G Prerequisite: Completion of Chem 341. Required Materials: • Textbook. “Undergraduate Instrumental Analysis”, 7th edition, by James Robinson, Eileen Frame, and George Frame. CRC Press. ISBN: 978-1-4200-6135-2. • Course Syllabus: PDF file downloadable from Western Online • Official Laboratory Research Notebook-50 pages (Available at the WIU bookstore.) • Material Safety Data Sheets (MSDS) information about all chemicals utilized in the laboratory can be found at the following web site. http://avogadro.chem.iastate.edu/MSDS/. E-copies are free of charge. • Approved safety goggles are required for the Chem 442G laboratory. • Scientific calculator • Laboratory usage fee of $35 Testing and Grading: Three 50 min exams and a comprehensive final will be given. The lowest score of the four exams will be dropped. The final exam can be used as a make-up exam, with an excused absence, for one and only one missed lecture exam. Several in-class assignments that are equally weighted will be given throughout the semester. Quizzes will be given on Fridays at the beginning of each class period. To accommodate absences, the lowest quiz score will be dropped. Make-up quizzes will not be given. Ten laboratory experiments will be conducted; the highest nine scores will be used to determine the final grade. Two laboratory exams will be given. Emerging Techniques and Technologies in Analytical Chemistry Presentation: In groups of two or three, students will give a 20 min oral presentation (5 min questions) on a peer-reviewed research article that focuses on a new and emerging technique or technology in the field of analytical chemistry. An article published within the last 6 months from an analytical chemistry journal (http://www.scimagojr.com/journalrank.php?category=1602) should be selected. A copy (pdf) of the article must be emailed to the instructor for approval a minimum of three weeks prior to the scheduled presentation date. Failure to do so will result in a loss of points. For the presentation, a minimum of 8 power point slides should be composed and include the following: article title, author names, journal name, background on the need for the new technique/technology, application of the technique/technology, description of the testing procedure, and results/discussion for the new technique/technology, as well as, the conclusions drawn. Particular emphasis should be placed on the benefit new technique/technology. Your presentation must include some elements of digital multimedia (images, charts, graphs, diagrams, video, audio) to illustrate your spoken text. Provide references for all multimedia. Each student in the group is expected to present a portion of the presentation. The final grade for the presentation will be a composite score calculated from evaluations performed by your peers (30%) and the instructor (70%). There will be no make-up presentations. An electronic copy of each article will be posted on Western Online. Make sure that any movie files or sound files in your presentation are included in a folder with your presentation file or they will not work. On the day of your presentation, bring the presentation to class on a USB drive. A paper copy of your presentation slides should also be brought as a back-up. Presentations will begin on Friday, February 19, 2016. Some quiz questions will be garnered from the presentations. Best 9 of 10 Quizzes: 15% Classroom Assignments: 5% Best 3 of 4 Exams: 35 % Best 9 Laboratory Reports of 10: 30% 2 Laboratory Exams: 5% Emerging Techniques in Analytical Chemistry Presentation:10% Course Grading Scale: Course Grading Scale Grade Percentage (%) 94-100 A 89-93 A85-88 B+ 80-84 B 77-79 B73-76 C+ 69-72 C 66-68 C63-65 D+ 60-62 D 57-59 D0-56 F Tentative Lecture Schedule Chapter # Chapter Title 1 Concepts of Instrumental Analytical Chemistry 2 Introduction to Spectroscopy 5 Visible and Ultraviolet Molecular Spectroscopy 9 and 10.3.3 Mass Spectrometry I: Principles and Instrumentation Exam #1, Mid/Late February (Chapters 1, 2, 5, and 9/10) 4 Infrared, Near-Infrared, and Raman Spectroscopy 6 Atomic Absorption Spectrometry 11 Principles of Chromatography Exam # 2, Mid/Late March (Chapters 4, 6, and 11) 12 Gas Chromatography 13 Chromatography with Liquid Mobile Phases 15 Electroanalytical Chemistry Exam #3, Late April (Chapters 12, 13, and 15) May. 9-13, 2016, Finals Week, No Class Tentative Laboratory Schedule Date Laboratory Experiments Tues. (Thurs.), Jan. 19 (21), 2016 Check-In & Safety Exp. #1, Comparing Transmittance and Absorbance Tues. (Thurs.), Jan. 26 (28), 2016 of KMnO4 in UV/VIS Spectroscopy (Exp. 2.1 and 2.2, p. 108) Exp. #2, Determination of L-Phenylephrine Tues. (Thurs.), Feb. 2 (4), 2016 Concentration in Dristan Nasal Spray Using UV/VIS Spectroscopy (Exp. 5.10, p. 433) Exp. #3, Proteomics Virtual Laboratory, Currens Hall Tues. (Thurs.), Feb. 9 (11), 2016 529 (handout) Exp. #4, FTIR Absorption Comparison of Hexane Tues. (Thurs.), Feb. 16 (18), 2016 and Heptane (Exp. 4.1 and 4.2, p. 348) Exp. #5, Determination of Sodium Concentration in Tues. (Thurs.), Feb. 23 (25), 2016 Soda Using Atomic Absorption Spectrometry (Exp. 6.3, p. 490) Tues. (Thurs.), March 1 (3), 2016 Laboratory Exam 1 Exp. #6, Quantitative Determination of Limonene Tues. (Thurs.), March 8 (10), 2016 Content Using Gas Chromatography (handout) Exp. #7, Determination of Trace Impurities in Tues. (Thurs.), March 22 (24), 2016 Whiskey Using Gas Chromatography Mass Spectrometry (handout) Exp. #8, Determination of Caffeine Concentration in Tues. (Thurs.), March 29 (31), 2016 Urine Using HPLC (handout) Exp. #9, Determination of Peptide Concentration Tues. (Thurs.), Apr. 5 (7), 2016 Using HPLC (handout) Exp. #10, The Effect of Temperature on pH Tues. (Thurs.), Apr. 12 (14), 2016 Measurements (Exp. 15.7, p. 1131) Tues. (Thurs.), Apr. 19 (21), 2016 Laboratory Exam 2 Tues. (Thurs.), Apr. 26 (28), 2016 Check-out Important Dates: Date (Spring, 2015) January 18, Mon. January 19, Tues. February 12, Fri. February 15, Mon. March 14-18, Mon.-Fri. March 21, Mon. May 9-13, Mon.-Fri. Event Martin Luther King Day - University is closed Classes Begin Lincoln's Birthday - University is closed Classes Resume Spring Break - No Classes Classes Resume Final Exam Week Safety: Safety is of primary concern in the chemistry laboratory. Prior to each laboratory experiment, please review the Material Safety Data Sheets (MSDS) for the hazards of the chemicals being used in each experiment at the website, http://hazard.com/msds/. Additionally, safety goggles must be worn at all times while in the laboratory, as well, as closed-toed shoes and pants covering the entire shin. Shoulders must also be covered. Failure to adhere to these policies will result in a student being asked to leave the lab. The lab will be considered as a missed session. Laboratory Reports: With the exception of one excused absence, each laboratory experiment and report is expected to be completed. Laboratory reports are due one week after the scheduled completion of the experiment. There will be a 12pt loss for each day (including weekends) it is late. The laboratory reports should be submitted to the dropbox on Western Online on or before the scheduled lab date; a paper copy should be submitted to the instructor on your lab day. Laboratory (pre- and post-) reports will be analyzed by the software, TurnitIn, for plagiarism; post-laboratory TurnitIn scores above 35% will result in an 80 % deduction in overall report points. Additionally, please be aware that school policy requires notification of all cheating to the departmental chairperson. If the report is late, place it in your instructor’s mailbox in the chemistry department office. No late materials will be accepted beyond one week after the due date. Missing any scheduled laboratory activities will result in a loss of points. Report Format: Pre- and post-laboratory reports are to be typewritten (Font: 12, Times New Roman and 1 inch margins). Pre-laboratory reports should be done prior to the laboratory and must include a cover page and the following 5 sections: objective of the experiment, experimental theory/background, materials, procedures (in your own words), and reference. The final laboratory report should include the revised pre-laboratory report sections, as well as, the: experimental results (including calculations), discussion and conclusion, and answers to end of lab questions. A copy of the raw data should be included at the end of the final report. Lab reports should represent each student’s individual work. Participation in the laboratory requires completion of pre-laboratory report, including all calculations needed for experimental sample preparation prior to the start of class. Laboratory Report Section Formatting A stand-alone cover page (2 pts) should be the first page of the laboratory report. It must include the title of the experiment, course number, your name (bold type) and the name of your lab partner, the names of your lab instructor and TA (for that experiment), and the date that the lab was performed; the text should be centered in the middle of the page. Two to three sentences about the objective (3 pts) of the experiment should be given. The theory/background section (5 pts) should be no less than ½ of a page and summarize how the objectives will be realized. For example, important reactions, techniques, or instrumental methods can be discussed; all sources utilized used should be cited. The theory should not include a description of the procedure. All chemicals, reagents (including concentrations), instruments, devices, and glassware should be recorded in the materials section (5 pts). The procedure (methods) section (8 pts) should give a description of the laboratory experiment that was performed and should be written in your own words. Arabic numerals should not be used at the beginning of a sentence and the procedure must be written in past tense and a passive voice. The results section (12 pts) should report findings and include all tables, graphs, and calculations. A representative example for each calculation should be labeled with a title, typewritten, and included in the in this section (i.e. mean, standard deviation, etc). All data should be typed and organized in tables. Tables and graphs should have titles and the x/y axis should be labeled. All calculations should include the appropriate units. The discussion and conclusion section (12 pts) should be used to interpret the findings, draw conclusions, and explain erroneous findings from the data that was collected and analyzed. The reference section (3 pts) should be last and the citations should be formatted using the American Chemical Society style. Attendance Policy: Students are expected to punctually attend all lecture and laboratory classes. A total of 3 excused and 1 unexcused absences are allowed. The WIU policy on class attendance can be found at: http://www.wiu.edu/student_services/student_developme nt_office/ current/a bs ence pol icy.php. An OARS report must be filed with each absence. Failure to report the absence will result in a loss of exam points. Any student arriving more than ten minutes late for a quiz, exam, or laboratory exercise will be allowed to take or complete the assigned work at the instructor’s discretion. Any student who receives six or more absences may be dropped from this course without notice. Outside work requirements: Students are expected to read ahead and be prepared for class. Reading the designated chapter before the class and going over the notes after each class is recommended. A daily minimum of two hours of out of class work is needed to do well in this class. Classroom and Course Policies: Any student convicted of academic dishonesty will receive a failing grade and may be subjected to further academic penalty, including expulsion. See the WIU academic dishonesty policy 4 (http://www.wiu.edu/policies/acintegrity.shtml). Emergency Preparedness: The WIU Office of Risk Management and Emergency Preparedness provides resources on how to respond to emergency situations. Please view the video resources at http://www.wiu.edu/rmep/. Students with Disabilities: In accordance with University values and disability law, students with disabilities may request academic accommodations where there are aspects of a course that result in barriers to inclusion or accurate assessment of achievement. To file an official request for disability-related accommodations, please contact the Disability Resource Center at 309-298-2512, disability@wiu.edu or in 143 Memorial Hall. Please notify the instructor as soon as possible to ensure that this course is accessible to you in a timely manner. Students Rights and Responsibilities: The WIU policy on the rights and responsibilities of students can be found at http://www.wiu.edu/provost/students.php.