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Text: Skoog, West, and Holler, Analytical Chemistry--An Introduction, 6th edition
Supplies: Bound laboratory notebook, calculator with scientific and statistical functions, Safety Glasses. Optional: white cotton gloves, available at camera stores and cosmetics counters.
Grading: Three hour exams (100 points each) and one Final Exam (200 pts.) 50%
Seven Lab Experiments (100 pts each) and report (25 pts) 50%
You must pass both lecture (about 40% of possible lecture points) and lab (about 60% of possible lab points) to pass the course. Grades are computed separately from the lecture and lab scores and are then combined to generate your course grade. Homework will be collected and examined. The amount and quality of the homework will be used to decide borderline grades at the end of the semester. History has shown that homework has decided grades for three or four people each semester. Another historical lesson is that students who are nearest failure in the course are those who do not do the homework.
If you find yourself struggling with the problems, please see your instructor for additional help.
Explanation of the Schedule Given Below:
LAB covers what is happening in lab on that day.
LECTURE tells what is probably being discussed on that day.
HAVE READ TEXT tells what you were to have read before coming to class on that day. The same section of text may be assigned several times, with different sections emphasized in lecture.
UNDERSTAND tells you what to concentrate on during your reading, and gives a rough outline of the lecture for that day.
PROBLEMS gives you a problem assignment to do after the material for the day has been presented. Problems are usually due the period following the day under which they are assigned in this schedule. In the event that the lecturer has not yet covered the material assigned, the homework should be delayed until the material is covered. Note that pages A-30 to A-45, have the answers to the asterisked problems. If by some chance you have obtained a solutions manual, don't use it to learn the material without first working on the problem yourself . Trying to memorize solutions (many of which are poorly done) rather than working through them is the Kiss of Death on exams.
Period 1 Week 1 8/27/96 Tuesday
LAB: Check in and Balance Instruction. Also read SWH Ch. 28, Lab Procedures
LECTURE: Introduction to course. Measurement of mass. What "dry" means.
HAVE READ TEXT: Ch. 1 (Intro); Ch. 28 (Basic Tools, desiccators, ovens and hood, volumetric glassware, electronic balances); Read techniques on the balance and on the use of pipets and burets. Memorize the molarities of standard reagents found in the lab.
UNDERSTAND: Diagram of electronic balance; mass, weight; standard weights; calibration of electronic balance; sensitivity; sources of error , general rules, weighing by difference; direct weighing, tare, weighing of liquids; rough vs. accurate weighing. desiccators and desiccants. Drying to constant weight.
PROBLEMS: None
Period 2 Week 1 8/29/96 Thursday
LAB: Complete balance instruction. Get chloride solid unknown and silver nitrate for the gravimetric chloride experiment. Assume unknowns are 60% by weight of chloride and digest precipitate for one week, during which the glassware calibration is done. Prepare 500 ml of 0.1M Silver Nitrate. Use the remainder for Volumetric Chloride. Begin drying unknown and silver nitrate. Clean crucibles, begin drying to constant weight. Practice pipet and buret techniques.
LECTURE: Introduce Grav. Chloride experiment and calibration of glassware.
HAVE READ TEXT: Ch. 6, Gravimetric Methods of Analysis; Ch. 28, pages 533-551(Unit Operations in gravimetry). Pages 550-560, use of pipet and buret. Ch. 29 Pages 566-568 (Gravimetric Chloride Experiment--we will use different concentrations than in SWH).
UNDERSTAND: Sintered glass crucibles; how to transfer precipitates; calibration of pipet and buret: note especially instructions on cleaning and use. Rubber policemen; experimental procedure with solid unknown and sintered glass crucibles; supersaturation, nucleation, optimum conditions, digestion; impurities and how to get rid of them.
PROBLEMS: None
Period 3 Week 2 9/3/96 Tuesday
LAB: Grav. Chloride: precipitate chloride in unknown samples, store in dark in desk; begin glassware calibrations. (SWH pages 557-560). Do buret, 10 ml pipet, and 25 ml pipet. Report results in laboratory notebook.
LECTURE: Gravimetric Calculations. Grams, moles, wt./wt. expressions, and stoichiometry.
HAVE READ TEXT: Survival Guide on Grav Calcs; Ch.2 (A Review of Some Basic Concepts); Ch. 6, pages 109-111 (Gravimetric Calculations).
UNDERSTAND: Metric mass units, %, ppm, ppb, mg%. How to do calculations in a gravimetric analysis. Warning: Many texts tend to do gravimetric calculations by setting up one all-inclusive formula. While this provides a compact explanation in a text, it does not reflect how real people solve problems. In lecture you will be shown how to break up a problem into small, understandable steps. Be sure you listen to the lecture before you do the assigned problems.
PROBLEMS (1): Page 25 #7, 11, 13; page 116 #12, 26, 32. Remember, these are due next period.
Period 4 Week 2 9/5/96 Thursday
LAB: Calibrate Glassware
LECTURE: Error Analysis. How to express an analytical result.
HAVE READ TEXT: See Survival Guide on error analysis. Text Ch. 4 Errors in Chemical Analysis; Ch. 5 Statistical Evaluation of Analytical Data
UNDERSTAND: Significant Figures, rounding off, accuracy and precision; determinant errors (or bias), indeterminate errors (or scatter); absolute error, relative error, standard deviation; standard deviation of the mean; student t applied to 95% confidence limits; rejection of a result. Introduction to linear least squares. We will not master all of these techniques at this time. We will return as needed during later experiments.
PROBLEMS (2): Begin these tonight. Complete the rest following tomorrow's lecture. p. 75, #4, 5 (* only); p.94, #6, 13.
Period 5 Week 3 9/10/96 Tuesday
LAB: Grav. Chloride--wash precipitate and transfer to constant weight sintered glass crucibles. Begin final drying operations.
LECTURE: Complete statistics; Volumetric Calculations; Molarity; Normality; ppm (mg/l); how to prepare solutions of known concentration.
HAVE READ TEXT: Ch. 2, sect. 2B, Solutions and their concentrations; Ch. 9 (Titrimetric Methods of Analysis).
UNDERSTAND: Ch. 2: Analytical vs. Equilibrium Molarity; calc of M, "how to prepare" calculations, ppm, ppb, calcs. Ch.9: more examples, a bit on Normality (see Appendix 7), Standard materials and solutions, titration calculations and stoichiometry. From lecture distinguish concentration from amount and understand the "work backwards" method for M, N, and mg/liter calculations.
PROBLEMS (3): (Remember: only * problems are required.) page 25, #21, 23, 27, 29, 33; p. 165, #11, 16.
Period 6 Week 3 9/12/96 Thursday
LAB: End Gravimetric Chloride/glassware calibration
LECTURE: The Precipitation Titration -- Introduction to Equilibrium Effects
HAVE READ TEXT: Ch. 3 (Chemical Equilibrium) esp. read 38-42 on solubility. Also read the Survival Guide.
UNDERSTAND: Solubility, solubility product (Ksp), example 3.3(pure solid), example 3.4 (common ion), example 3.5 (mixture problem); conditions to initiate precipitation.
PROBLEMS (4): (*only) p. 50, #7, 9, 10, 11
Period 7 Week 4 9/17/96 Tuesday
LAB: Begin Volumetric Chloride Using Adsorption Indicator. Same Solid Unknown used above for Grav Cl. Procedure SWH pages 579-580.
LECTURE: Ksp and Solubility (cont'd)
HAVE READ TEXT: Ch. 7 Systematic Solving of Equilibrium Problems
UNDERSTAND: Analytical concentration, equilibrium concentration, charge balance, mass balance, solving equilibrium problems using mathematical models. Read Ch. 7 for general concepts. We will do only a few of the simpler problems at this time.
PROBLEMS (5): Page 51, #12, 14
Period 8 Week 4 9/19/96 Thursday
LAB: Vol. Chloride
LECTURE: Ksp and solubility (conclusion)
HAVE READ TEXT: Ch. 13 Precipitation Titrations
UNDERSTAND: The precipitation titration curve, the end point, adsorption indicators, use of chromate as indicator (Mohr titration), Volhard titration (as an example of a back titration).
PROBLEMS (6): Page 234, #7, 11, 29c
Period 9 Week 5 9/24/96 Tuesday
LAB: End Volumetric Chloride
LECTURE: Intro Acid/Base and use of indicators. Titration Curves. Preparation of 0.1M NaOH.
HAVE READ TEXT: Ch. 10(A/B Titrations--read for concepts. We will do calculations later.); Ch. 18, pages 328-338 (measurement of pH)(Skim for content--this subject will be done in detail later in the course.): Ch. 12 Applications of Neutralization Titrations (esp. section 12A-3 on Standard NaOH)
UNDERSTAND: Preparation of 0.1M NaOH, carbonate error procedure for KHP; lecturer will do problem of 1/4 aliquot from 100 ml vol. flask, given that the unknown is 40-70% KHP. Glass electrode, reference electrode, use of pH meter, standard buffers, plotting titration curves.
PROBLEMS: None
Period 10 Week 5 9/26/96 Thursday
LAB: Begin acid/base titration of KHP. See the 105 Laboratory handout. Procedure as in SHW p. 571-573, except prepare standard KHP solution (12 millimoles in 100 ml) and do standardization with aliquots. Evaluate two indicators (methyl red and phenolphthalien) by doing a titration curve of some KHP with a pH meter. A critical evaluation of the endpoints will be required (25 points)(see handout) in addition to the usual unknown results.
LECTURE: Definition of pH -- Calculation of pH for strong acids and bases.
HAVE READ TEXT: Ch. 2, p. 20 (p functions); Ch. 3, pages 28-38, Acid/Base Equilibria. Read the Survival Guide on A/B calculations.
UNDERSTAND: Strong and Weak acids and bases; pH; Kw; pH of strong acids and bases.
PROBLEMS (7): page 25, #18, 19(*parts and H+ and OH- only).
Period 11 Week 6 10/1/96 Tuesday
LAB: KHP
LECTURE: *** HOUR EXAM I *** Covers gravimetry, error analysis, and Ksp. Bring your text (for tables), a calculator, and a 3X5 inch card with anything you wish written on it.
Period 12 Week 6 10/3/96 Thursday
LAB: KHP
LECTURE: Weak Acids and Bases
HAVE READ TEXT: Ch. 3, pages 42-50
UNDERSTAND: Ka, pH of weak acids, how to do approximations and successive approximations. Kb, pH of weak bases and salts of weak acids.
PROBLEMS (8): page 51, #19, 20. page 193, #26, 28, 32.
Period 13 Week 7 10/8/96 Tuesday
LAB: End KHP Titration
LECTURE: Buffers and Titration Curves
HAVE READ TEXT: Ch. 10, Theory of Neutralization Titrations. Read Survival Guide.
UNDERSTAND: Buffer, Henderson equation, pH given composition, composition given pH, buffer capacity.
PROBLEMS(9): page 193, #34, 37, 40g, 43, 50a (as always, *only).
Period 14 Week 7 10/10/96 Thursday
LAB: Begin Ca by EDTA. Solid Unknown. Directions on handout.
LECTURE: Introduce Ca by EDTA
HAVE READ TEXT: Ch. 14 Complex-Formation Titrations
UNDERSTAND: Preparation and standardization of EDTA. Preparation of unknown solution. The Mg-EDTA "spike."
PROBLEMS (10): page 255, #10, 12, 18.
Period 15 Week 8 10/15/96 Tuesday
LAB: EDTA
LECTURE: EDTA as a polyprotic acid
HAVE READ TEXT: Ch. 11 Titration Curves for Polyfunctional Acids and Bases (skim over the math), Ch. 14, figure 14-2, figure 14-6, figure14-8, Effect of pH on EDTA
UNDERSTAND: How to sketch a polyprotic titration curve; location of multiple end points, location of multiple buffer regions. Principal species present at various pH's.
PROBLEMS (11): page 210, #8, 12, 16, 28a (sketch the curve only--no detailed calc).
Period 16 Week 8 10/17/96 Thursday
LAB: EDTA
LECTURE: Review Acid/Base calculations
HAVE READ TEXT: Review acid/base and complex formation in preparation for the next hour exam.
UNDERSTAND: Be prepared to ask any questions you may have had while doing the homework.
PROBLEMS: None.
LECTURE: Introduce Spectrophotometric Iron Experiment.
HAVE READ TEXT: Ch. 21 Theory of Molecular Absorption
UNDERSTAND: Beer's Law, P, Po, T, %T, a, b, C, absorbance, molar absorptivity; from lecture get working curve, standard solutions, color formation reaction.
PROBLEMS (12): page 419, #9, 10, 11.
Period 18 Week 9 10/24/96 Thursday
LAB: Begin determination of Fe in an ore by Spectrophotometry. You will need to use the 50 ml volumetric flasks in your lockers and calculate your own dilutions. You will also need to prepare your own unknown solution by dissolving some of your Fe ore unknown as described in the Redox Fe experiment.
LECTURE: Use of Spectrophotometric Instrumentation
HAVE READ TEXT: Ch. 20 Spectro Instrumentation; Ch. 22 Applications of Molecular-Absorption Spectroscopy
UNDERSTAND: Spectrophotometer, source, monochromator, detector, readout, sources for UV and VIS, prisms and gratings, cells, detectors for UV-VIS and IR, diagram of Spectronic 20, single beam and double beam spectrophotometers. Errors shown in fig. 22-11, p. 438.
PROBLEMS (13): page 441, #27, 28 (calculate concentrations only. Skip the statistics).
Period 19 Week 10 10/29/96 Tuesday
LAB: Spectro Iron
LECTURE: *** HOUR EXAM II *** on Acid/Base and Complex Formation. Don't forget your calculator, your text, and your 3x5 inch card.
Period 20 Week 10 10/31/96 Thursday
LAB: Spectro Iron
LECTURE: Introduction to Atomic Spectroscopy
HAVE READ TEXT: Ch. 24, Atomic Spectroscopy Based upon Flames
UNDERSTAND: Emission vs. absorption spectrometry, instrumentation for atomic absorption, hollow cathode lamps, burners, sample introduction, flames, interferences, sensitivity, detection limit, flameless methods.
PROBLEMS : None
Period 21 Week 11 11/5/96 Tuesday
LAB: Spectro Iron/AA
LECTURE: Oxidizing and Reducing Agents. Introduce Iron redox experiment.
HAVE READ TEXT: Ch. 15, An Introduction to Electrochemistry (skim for concepts).
UNDERSTAND: Oxidizing agent as electron acceptor; reducing agent as electron donor; how to use the table of standard reduction potentials to determine which species will donate electrons to which other species; know that good acceptors are on the upper left of the table, while good electron donors are on the lower right. Half reactions from the Fe experiment will be used as examples.
PROBLEMS: None
Period 22 Week 11 11/7/96 Thursday
LAB: End Spectro Fe/AA
LECTURE: Half reactions and equation balancing. Homogeneous charge transfer in solution.
HAVE READ TEXT: Ch. 17, Applications of Oxidation/Reduction Titrations (esp. note reactions involving Iodine, dichromate and other important reagents). Also read the handout on the Glucose Experiment as an example of several redox reactions and calculations.
UNDERSTAND: Glucose experiment as an exercise in half reactions and equation balancing; Normality vs. Molarity, and equivalents/mole used in making calculations; examples of mole method and of equivalent method.
PROBLEMS (14): Page 281, #7, 8, 9; page 325, #28, 30, 32, 35.
Period 23 Week 12 11/12/96 Tuesday
LAB: Begin Iron in Ore by Redox Titration.
LECTURE: Electrochemical Cells
HAVE READ TEXT: Ch. 15, pages 260-281, Electrochemical Cells and the Nernst Equation. (There is a lot of confusing material here. Let the lecture be your guide to the important stuff.)
UNDERSTAND: Cells, what happens at each side; what happens in the salt bridge; anode, cathode, electrolytic, galvanic, direction of current flow; effect of concentration (Nernst Equation).
PROBLEMS (15): page 282, #16, 18.
Period 24 Week 12 11/14/96 Thursday
LAB: Redox Fe
LECTURE: Redox Titration Curves
HAVE READ TEXT: Ch. 16 Theory of Oxidaton/Reduction Titrations (but the lecture will be more useful)
UNDERSTAND: How to sketch a redox titration curve, E vs. SCE reference, E at equivalence point; redox indicators.
PROBLEMS (16): page 304 #14.
Period 25 Week 13 11/19/96 Tuesday
LAB: Redox Fe
LECTURE: Glucose Procedures and Calculations Revisited
Period 26 Week 13 11/21/96 Thursday
LAB: End Redox Fe
LECTURE: Potentiometry, pH, and Ion Selective Electrodes
HAVE READ TEXT: Ch. 18 Potentiometric Methods
UNDERSTAND: Electrode types, reference electrodes, liquid junction, E(meas), measurement of concentration by direct potentiometry, measurement of pH. Glass electrode, limitations and interferences in ion selective electrodes.
PROBLEMS: None
Period 27 Week 14 11/26/96 Tuesday
LAB: Begin Glucose. Procedure on handout.
LECTURE: *** HOUR EXAM III *** on Oxidation/Reduction and Spectrophotometry. Be sure and bring text, calculator, and 3x5 card.
Period 28 Week 14 11/28/96 Thursday
Holiday --- Thanksgiving
Period 29 Week 15 12/3/96 Tuesday
LAB: Glucose
LECTURE: Chapters25, 26, 27 -- Analytical Separations -- skim these chapters for basic concepts about extractions, ion-exchange, column chromatography, gas/liquid chromatography (GLC), High Performance Liquid Chromatography (HPLC)
Period 30 Week 15 12/5/96 Thursday
LAB: End Glucose
LECTURE: Continue Analytical Separations
Period 31 Week 16 12/10/96 Tuesday
LAB: Clean up and check out. Glucose results due.
LECTURE: Review
Period 32 Week 16 12/12/96 Thursday
No classes Thursday or Friday. Final exam preparation and faculty consultation days.
Final Exam: Comprehensive.
Morning Section: 0845-1045, Thursday, Dec 19, 1996
Afternoon Section: 1315-1515, Tuesday, Dec 17, 1996