Chem 105 Syllabus and Master Schedule Spring 2010

 

Instructor: Dr. Zellmer, S-244, 278-2113, e-mail: david_zellmer@csufresno.edu

 

Text: Skoog, West, Holler and Crouch, Analytical Chemistry--An Introduction, 7th edition

 

Course Web Site: http://zimmer.csufresno.edu/~davidz/Chem105/

 

Blackboard: This course is web assisted through Blackboard. Most course information will be available on the public website given above. Blackboard will be used mainly to post your grades and to serve as a means of electronic communication.

 

Supplies: Bound laboratory notebook, calculator with scientific and statistical functions, Safety Glasses. Optional: white cotton gloves, available at camera stores and cosmetics counters.

 

Computers: There will be a few computer spreadsheet assignments in this class. Your textbook contains substantial information on using computers for statistics and other analytical uses. The course web site contains additional material to help the student. You will need web access to use Blackboard. E-mail is also useful for asking questions, and for me to get information out to the class.

 

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 50-60% of possible lab points) to pass the course. Please check with your instructor if you feel you may be failing a given part of the course. Percentage scores are computed separately from the lecture and lab scores and are then combined to generate your course score and grade. The scale generally used is 85% A, 70% B, 50% C, 40% D, and < 40% F. 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 in a class of 18 students, 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.

 

Cheating and Plagiarism: This course conforms to university guidelines on cheating and plagiarism. Be especially careful on computer-generated assignments that you do not use the files of others as your own work. Example: Two spreadsheet data analyses are turned in as part of two laboratory reports. It is evident that they are virtual duplicates of each other. Penalty: Both reports receive zero points.

 

Per

Wk

Date

Day

Lab

Lecture Topics and Assignments

 

 

 

 

 

Unless otherwise stated, do the * problems only. Problems are generally due the period after the date they are assigned.

1

0

1/21/

2010

Th

Safety,

Balance

Intro to Course. Mass. Dryness

Read: Ch. 1 What is Analytical Chemistry, Ch. 2: Tools of Analytical Chemistry

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.

 

2

1

1/26

Tu

Check In

Grav Cl

Intro Grav Cl. Calibration of Glassware

Read: Ch. 8 Gravimetric Methods of Analysis

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.

 

3

1

1/28

Th

Grav Cl

Gravimetric and Solution Calculations

Read: Ch. 3 Expressing Quantities and Concentrations; Also read relevant sections of the Survival Guide. If you don't have a hard copy, the Survival Guide is available at the Chem 105 web site.

Understand: Metric mass units, %, ppm, ppb, mg%. Moles, millimoles. Stoichiometry. How to do calculations in a gravimetric analysis. Computing solution concentrations. Computing the volume of 0.1M AgNO3 required for quantitative precipitation.

Problems: Ch. 3, p. 76: 7, 9, 11, 14, and 37. Remember, do only the starred (*) portions of the problems. These are due next period.

 

4

2

2/2

Tu

Grav Cl

Error Analysis

Read: Ch. 5 Errors in Chemical Analyses; Ch. 6 Random Error; Ch. 7 Statistical Analysis (We won't cover all of this!)

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: Ch. 5, p. 116: 6, 10 (spreadsheet); Ch. 6 p. 146: 5 (spreadsheet).

5

2

2/4

Th

Grav Cl

Continue Statistics. Begin Volumetric Calcs.

Problems: Ch. 7, p. 173: 1, 19 (LLS by spreadsheet)

6

3

2/9

Tu

Cal. Glass-ware

Volumetric Calculations and Titrations. Begin Ksp.

Read: Ch. 11 Titrations

Understand: Basic volumetric calculations (review Ch. 3), how to make solutions of known concentration; use of primary standard materials; end points and equivalence points; the standardization titration calculation; the calculation of the unknown from a titration.

Problems: Ch. 11, p. 261: 13, 17, 19, 28

7

3

2/11

Th

Vol. Cl

Ksp and Solubility

Read: Ch. 4, pp. 88-91; Survival Guide on Ksp

Understand: solubility, solubility product, charge balance, calculation of solubility in pure water, calculation of solubility with a common ion using the Initial/Final SS method, Ion Product and when precipitation can happen. (see next period for problems)

8

4

2/16

Tu

Vol. Cl

Ksp and Solubility (continued)

Problems: Ch. 4, p. 101: 8, 9, 13, 15.

9

4

2/18

Th

Vol. Cl

Intro Acid/Base Titrations

Read: Ch. 4, pp. 79-88; Survival Guide on Acids, Bases and pH

Read: Ch. 12: Determining Acids, Bases, and the pH of Buffers. (Skim for now. We will cover each part in turn as scheduled below.)

In Lecture: 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

10

5

2/23

Tu

KHP

Hour Exam I (through Ksp)

11

5

2/25

Th

KHP

Meas. of pH. Strong Acids and Bases

Understand: Strong and Weak acids and bases; pH; Kw; pH of strong acids and bases. Initial/Final approach to mixtures of SA and SB.

Problems: (due the period after the exam): Ch. 12, p. 300: 23 a, c, e.

12

6

3/2

Tu

KHP

Weak Acids and Bases

Understand: Ka, pH of weak acids, how to do approximations and successive approximations. Kb, pH of weak bases and salts of weak acids.

Problems: Ch. 12, p. 300: 26. 28, 32.

13

6

3/4

Th

KHP

Buffers and Titration Curves

Read: Go back over the examples in the Survival Guide, then look at Ch. 12 again.

Understand: Buffer, Henderson equation, pH given composition, composition given pH, buffer capacity. Calculating pH during a titration. Sketching a titration curve.

Problems: Ch. 12, p. 300: 34, 40, 43, 51(titration curve). Ch. 14, p. 342: 25 (messy acid base titration calculation).

14

7

3/9

Tu

EDTA

Intro Ca by EDTA

Read: Ch. 15: Complexation and Precipitation Titrations.

Understand: Preparation and standardization of EDTA. Preparation of unknown solution. The Mg-EDTA "spike."

Problems: Ch. 15, p. 383: 14, 16 (real-world calculations).

15

7

3/11

Th

EDTA

EDTA as a Polyprotic Acid

Read: Ch. 13: Polyfunctional Acids and Bases. (Skim the math. Listen in lecture.)

Understand: Polyprotic acids and bases. Amphiprotic substances. How to sketch a polyprotic titration curve; location of multiple end points, location of multiple buffer regions. Principal species present at various pH's. EDTA complexing power at a given pH.

Problems: Ch. 13, p. 324: 8, 12 (pH in polyprotic systems)

16

8

3/16

Tu

EDTA

Review Acid/Base Calculations

17

8

3/18

Th

EDTA

Intro Spectro Fe Experiment

Read: Ch. 21: Spectroscopic Methods of Analysis; Handout on spectro experiment working curves. Ch. 23, pp. 595-601 (spectra and working curves)

Understand: Beer's Law, P, Po, T, %T, a, b, C, absorbance, molar absorptivity; from lecture get working curve, standard solutions, color formation reaction. Determining best wavelength from absorption spectrum.

Problems: Ch. 21, p. 569: 18, 28 (spreadsheet working curve).

18

9

3/23

Tu

Spectro Fe

Hour Exam II (Acid/ Base, and Cmplx)

19

9

3/25

Th

Spectro Fe

Use of Spectro Instrumentation

Read: Ch. 22: Instruments for Measuring Absorption

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.

Problems: None

20

10

3/30

Tu

SB

Spring Break

21

10

4/1

Th

SB

Spring Break

22

sb

4/6

Tu

Spectro Fe

Intro Atomic Spectroscopy

Read: Ch. 23, pp. 626-631.

Understand: Emission vs. absorption spectrometry, instrumentation for atomic absorption, hollow cathode lamps, burners, sample introduction, flames, interferences, sensitivity, detection limit, flameless methods.

Problems: None.

23

sb

4/8

Th

Spectro Fe/AA

Redox Agents. Intro Redox Fe

Read: Ch. 16: Elements of Electrochemistry (Skim for concepts. There is a lot of confusing material here. All will be made clear in lecture.)

Ch. 18: Applying Oxidation/Reduction Titrations. (Concentrate on iron and permanganate chemistry.)

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: Ch. 18, p. 467: 28, 30, 32 (redox titration calculations)

24

11

4/13

Tu

Spectro Fe/AA

Half Reactions; Eqn Balancing; Homogeneous Charge Transfer

Understand: Balancing half reactions by adding water, hydrogen ions and electrons. Writing complete balanced redox reactions. Other oxidizing and reducing reagents, including those involving iodine.

Problems: Ch. 16, p. 416: 7, 8. (balancing and half reactions)

25

11

4/15

Th

Redox Fe

Electrochemical Cells

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: Ch. 16, p. 417: 16 (Nernst Eqn), 18 (cell anode & cathode).

26

12

4/20

Tu

Redox Fe

Redox Titration Curves

Read: Ch. 17, pp. 428-441: Constructing Redox Titration Curves.

Understand: How to sketch a redox titration curve, E vs. SCE reference, E at equivalence point; redox indicators.

Problems: Ch. 17, p. 443: 15a (titration curve; spreadsheet optional)

27

12

4/22

Th

Redox Fe

Conc. from E; Ion Selective Electrodes

Read: Ch. 19 Potentiometry

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: Ch. 19, p. 506: 29 a and b (E vs log C working curve)

28

13

4/27

Tu

Redox Fe

Introduce GLC Experiment

Read: Ch. 24: An Introduction to Analytical Separations, Ch. 25: Gas-Liquid and High Performance Liquid Chromatography. (Skim these chapters for now. We will address the details in lecture.)

Understand (for the GLC experiment): The basic layout of the GLC, including the carrier gas, the injection port, selection of the proper column, care and feeding of the detector, how to record your data and how to make samples and standards using an internal standard. A more detailed coverage of the concepts and instrumentation involved will follow in subsequent lectures.

Problems: None.

29

13

4/29

Th

Quant GLC

Hour Exam III (Spectro and Redox Pt. 1)

30

14

5/4

Tu

Quant GLC

Analytical Separations

Understand: Extraction, partitioning, how chromatographic separation happens. How to choose the correct column and running conditions.

Problems: Ch. 25, p. 699: 15 (This is an internal standard spreadsheet. First reproduce the spreadsheet on page 684, then plot it out without using the IS method to see how bad it gets. This is not a starred problem.)

31

14

5/6

Th

Quant GLC

Analytical Separations

Understand: Separations instrumentation, basic layout of the GLC and HPLC. Flow controllers, injectors, column ovens, and several detectors, including TCD, FID, and Mass Spectroscopy.

32

15

5/11

Tu

Check Out

Last Day of Instruction. Review.

 

15

5/13

Th

Lab is closed

Faculty Consultation Day

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Final Exam is Thursday, May 20, 2010, 0845-1045