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.