CHEM 2106 ANALYTICAL CHEMISTRY I - FALL 2009 3 CREDIT HOURS Dr. Stephen Kariuki H203 Ext. 4430 (office) Office Hours: Mon. 2:30-3:30; Tue. 10:30-11:30; Wed. 11:30-12:30 Or by appointment - minimum 6 hrs required Dr. Joey Patapas – Lab Instructor Office: H242 Office Hours: T.B.A. Class Meetings Lecture: Tue. 12:30 – 3:30 PM (R309) Labs: Thu. 12:30-3:30 PM (H205) Texts - Analytical Chemistry, An Introduction, 7 th ed. [Skoog D.A.; West D.M.; Hollre F.J.; Crouch S.R.] (available in the Campus Shop). - *Quantitative Chemical Analysis by Harris D.C., 6th ed. - *Fundamentals of Analytical Chemistry, 7th ed. [Skoog D.A; West D.M.; Holler F.J.] * These books may be borrowed from the instructor for a maximum of 3 days Lab Resources: - Handouts Prerequisite: CHEM 1005 or the equivalent from another university Course Objectives Providing a strong background in those chemical principles that are particularly important to analytical chemistry. Developing an appreciation for the difficult task of judging the accuracy and precision of experimental data and showing how these judgments can be sharpened by the application of statistical methods. Introducing a wide range of techniques that are useful in modern analytical chemistry Developing the skills needed to solve analytical problems in a quantitative manner, particularly with the aid of the spreadsheet tools. Teaching those laboratory skills that will give students confidence in their ability to obtain high-quality analytical data. Course Description A. The Basic Tools of Analytical Chemistry 1. 2. 3. 4. 5. 6. 7. What Analytical Chemistry is Chemicals and Apparatus: Putting Tools to Work How Quantities and Concentrations are expressed Basic Approach to Equilibrium Errors in Chemical Analyses and Quality of Results Random Error Statistical Evaluation of Data 2 B. Principles and Application of Chemical Equilibrium Systems in Quantitative Analysis 1. 2. 3. 4. 5. 6. 7. 8. Gravimetric Methods of Analysis Electrolyte Effects: Activity or Concentration Application of Equilibrium Calculations to Complex Systems Stoichiometric Reactions Acids, Bases and Buffers Polyfunctional Acids and Bases Application for Neutralization Titrations Complexation and Precipitation Titrations C. Electrochemical Methods 1. Oxidation-Reduction Reactions, Electrochemical Cells, Electrode Potentials 2. Calculating Potentials of Electrochemical Cells and Applications D. Spectroscopic Methods of Analysis 1. Making Measurements with Light 2. Instruments for Measuring Absorption 3. Calculations Involving Absorption E. Separations Based on Chromatographic Techniques 1. Introduction to Analytical Separations: Masking, Precipitation and Filtration, … 2. Gas-Liquid and High-Performance Liquid Chromatography Attendance: Punctual and regular attendance is essential for the successful completion of a course. When the lectures absenteeism exceeds 20%, the student may be excluded from writing the final examination. In case of an absence, the student will be responsible for all announcements and material covered in the class. Disability Services: Students with disabilities are encouraged to contact the Office for Students with Disabilities to discuss and plan for individual accommodations and support. Take Home Problem Sets: These will be mainly from end of chapter questions. Questions from other sources may also be assigned in class. Late problem sets will be penalized 50% the 1st day, 80% the 2nd day, and 100% any other day. Tests/Quizzes: Tests and quizzes will be conducted during the class lecture time. A notice of no less than a week will be given before a test is conducted. No notice will have to be given for quizzes covering the material taught in the same day that the quiz is conducted. Labs: Since no make-up labs can be guaranteed, attendance of all the labs will be expected. When the labs ABSENTEEISM EXCEEDS 20%, the student may be excluded from writing the final examination. Further, a student who fails to get a passing grade in the labs may be awarded a failing grade in the class. Exams/Tests/Quizzes/Take Home P. Sets/Labs Weighting%: Test: Oct. 6 10% Quizzes: 10% (impromptu) Problem Sets: 10% Labs: 20% Mid-term Exam: 17th Nov. 20% Final Exam (3 hours; comprehensive): Venue and schedule to be announced later – 30% 3 Academic Dishonesty: The University takes a very serious view of such offences against academic honesty as plagiarism, cheating, and impersonation. Penalties for dealing with such offences will be strictly enforced. For full details of the policy on academic dishonesty see the appropriate section of the Nipissing Academic Calendar. Special Final Examinations: Students who are unable to write final examinations because of illness or other circumstances beyond their control, or whose performance on the examination has been impaired by such circumstances, may on application, be granted permission to write a special final examination. Such application must: 1. be made in writing to the Dean of Arts and Science not later than one week after the date of the examination; and 2. be fully supported in the cases of illness by a medical certificate or by appropriate documents in other cases. The Dean’s decision on special final examinations is final and may not be appealed to the Student Academic Standing Appeals Committee. Grading Scale: 80 – 100% (A) 70 – 79% (B) 60 - 69% (C) 50-59% (D) 0 – 49% (F) Absences from Quizzes, Tests, and Mid-term Exams: Students must notify the course instructor prior to the test when there are circumstances rendering them unable to attend scheduled quizzes, tests, and mid-term exams. A mark of zero will be given unless alternate arrangements are made with the professor. There will otherwise be no rewrites or supplementals for tests and quizzes Test Protocol: 1. Any questions you may have during the test should be brought to the attention of the test proctor - but quietly and privately. Come to the desk or raise your hand and the proctor will try to come to you. 2. A periodic table will be provided when required. You may have only pencil/pen and calculator at your desk. 3. If possible, sit on every other seat from your adjacent neighbor. 4. Stop work when you are asked to do so. If you finish early, you may leave, but do not disturb others. 5. You may only leave the room during a test with the consent of the proctor. 6. Students wishing to have "extra time" on examinations must have a demonstrated medical condition and permission from the Office for Students with Disabilities 4 Analytical Chemistry 1 Tentative Lab Schedule Fall 2009 Date Experiment Number Experiment Title Sept 10 First Week No Lab Meeting Sept 17 Introduction/Experiment #1 Calibration of Volumetric Glassware Sept 24 Experiment #2 Gravimetric Determination of Nickel in an Unknown Solution Oct 1 Experiment #2 Gravimetric Determination of Nickel in an Unknown Solution Oct 8 Experiment #3 Volumetric Determination of the Purity of KHP Sample Oct 15 Reading week No Lab Meeting Oct 22 Experiment #3 Volumetric Determination of the Purity of KHP Sample Oct 29 Experiment #4 Determination of the Identity of a Weak Acid via Titration with a Strong Base Nov 5 Experiment #5 Colorimetric Determination of Iron Nov 12 Experiment #6 Determination of Total Hardness of Water by EDTA Titration Nov 19 Experiment #6 Determination of Total Hardness of Water by EDTA Titration Nov 26 Spare Week No Lab Meeting (Unless Needed) Dec 3 Lab Exam No Experiment 5 LABORATORY SAFETY AND WORK INSTRUCTIONS The laboratory can be -- but is not necessarily – a dangerous place. When precautions and a proper understanding of techniques are employed, the laboratory is not more dangerous than any other classroom. Most of the precautions are just common-sense practices. These include the following: 1. Wear approved eye protection (including splash guards) at all times while in the laboratory. (No one will be admitted without it.) You may purchase a pair of safety goggles from the Campus Shop. The laboratory has an eyewash fountain available for your use. In the event that a chemical splashes near your eyes, you should use the fountain before the material runs behind your eyeglasses and into your eyes. 2. Know where to find and how to use all safety and first-aid equipment. 3. Consider all chemicals to be hazardous unless you are instructed otherwise. Dispose of chemicals as directed by your instructor. 4. Wear closed shoes at all times. 5. Eating, drinking, and smoking are strictly prohibited in the laboratory. 6. If chemicals come into contact with your skin or eyes, wash immediately with copious amounts of water and then consult your laboratory instructor. 7. Never taste anything. Never directly smell the source of any vapor or gas. Instead, by means of your cupped hand, bring a small sample to your nose. 8. Perform in the fume hood any reactions involving skin-irritating or dangerous chemicals, or unpleasant odors. 9. Never point a test tube that you are heating at yourself or your neighbor – it may erupt dangerously. 10. Do not perform any unauthorized experiments. 11. Clean up all broken glassware immediately. 12. Always pour acids into water, not water into acid, because the heat of solution will cause the water to boil and the acid to spatter. 13. Avoid rubbing your eyes unless you know that your hands are clean. 14. When inserting glass tubing or thermometers into stoppers, lubricate the tubing and the hole in the stopper with glycerol or water. Wrap the rod in a towel and grasp it as close to the end being inserted as possible. Slide the glass into the rubber stopper with a twisting motion. Do not push. Finally, remove the excess lubricant by wiping with a towel. Keep your hand as close together as possible in order to reduce leverage. 15. Do not use flammable reagents such as alcohols, ethers and acetones near a flame. 16. Learn the location and operation of fire-protection devices. 17. Any clothing that has bulky or loose sleeves should not be worn in the lab – this reduces chances for ones clothing to catch fire. Long hair also presents a fire hazard and must be tied back. In case someone’s clothing or hair is on fire, immediately lead the person to the shower and pull the metal ring. 6 RECOMMENDED LAB PRACTICE 1. Read the procedure for each assignment before coming to the laboratory. Attend to any assignment that needs to be done. 2. RECORD YOUR RESULTS DIRECTLY ONTO YOUR REPORT SHEET OR A BOUND NOTEBOOK – and not on a loose piece of paper. 3. Dispose of excess reagents as instructed by your instructor. Never return reagents to the reagent bottle. 4. Leave reagent bottles on the location where you found them. 5. Use only the amount of reagent called for; avoid excesses. 6. Whenever instructed to use water in these experiments, use distilled/deionized water unless instructed to do otherwise. 7. KEEP YOUR WORKING AREA CLEAN. NO ONE SHOULD COME AND CLEAN YOUR AREA AFTER YOU ARE GONE. 8. When weighing, pay extra attention so that you do not pour chemicals on the balance. ANY MESS SHOULD BE CLEANED IMMEDIATELY. 9. Do not weigh hot or warm objects. Objects to be weighed should be at room temperature. 10. Do not put hot objects on the desktop. Place them on a wire gauze or heat-resistant pad.