Chemistry 55 Lecture and Lab Quantitative Analysis Fall 2003

Transcription

1 Instructor: Dr. Roger Terrill Duncan Hall 4B (408) Prerequisite: Text: Office Hours: MW 09:30-10:30 DH 4B TR 16:30-17:30 DH-4B & appointment Lecture Hours: TR 07:30-08:20 DH-416 Lab Hours: MW 13:30-16:20 DH-413 TR 10:30-13:20 DH-413 Chem 1B with a C or better (C- not accepted). Quantitative Chemical Analysis; 6 th ed. By Daniel Harris, required available in Spartan Bookstore. Supplementary material at Lab Manual: Quantitative Analysis Laboratory; S.P. Perone required available in the lab or via SAACS, DH 504, during business hours the first two weeks of the semester. Lab Notebook: An acceptable laboratory notebook, with carbon copy pages, will be required for all students. Notebook carbons will be due at the conclusion of each day of lab. All primary data must be taken in the notebook in ink. In many industry or research situations, the lab notebook can be used as a legal document, so good notebook habits are essential for success in science! Notebooks can be purchased in Spartan or Robert s bookstore on 10 th street. It is fine with me if you use part of an old notebook or one in use for another class. Exercises: In this course we will: a. discuss quantitative chemical analysis, statistics and error analysis, chemical equilibria, acid-base and buffer chemistry, basic spectrophotometry and chromatography b. conduct lab experiments in acid/base and EDTA titrimetry, flame and solution photometry, electrochemistry and high performance liquid chromatography. Content: Exams: The lecture will cover material from chapters, the latter time permitting: 0,1,2, 3, 4, 6, 7, 8, 10, 11, 12, 14, 15, 18, 21, 22, 23, 24, 25. The pace and timing of the lecture, including suggested homework problems will be determined during the semester. Anticipate about 1 week per chapter. Tuesday Thursday Tuesday Thursday 8/26 Intro 8/28 10/21 10/23 9/2 9/4 Quiz 1 10/28 10/30 Quiz 3 9/8 9/8 11/4 11/6 9/16 9/18 Exam 1 11/11 11/13 Exam 4 9/23 9/25 11/18 11/20 9/29 10/1 Quiz 2 11/25 Quiz 4 11/27 Holiday 10/7 10/9 12/2 12/4 10/14 10/16 Exam 3 12/9 12/11 Finals Page 1 of 5

2 Grading: A single letter grade will be assigned for CHEM 55. The lecture and the laboratory portions of the course carry roughly equal weights. A passing grade in CHEM 55 requires a passing grade in both the lecture and the laboratory portions of the course. Chemistry 55 Lecture and Laboratory Points Maximum Laboratory *Chloride, w/w % gravimetry 100 *ppm Total Hardness, by EDTA titration 100 *Ca and Mg, w/v % 100 Certification of either Mn, Zn, or Co solution 30 Calibration of ph electrode 20 *H 3 PO 4 and NaH 2 PO 4, w/v %, by titrimetry 200 Directions for preparing 500 ml of ph 7.0 buffer solution 20 Mn in steel, w/w %, by photometry (Spec 20) 50 By AAS, calibration curve 50 By AAS, standard addition 50 Calibration of Cl - electrode 20 Chloride, w/w %, in KCl and NaCl mixture by ISE 100 Polyaromatic hydrocarbons, mg/ml in a mixture by HPLC 100 Calibration of an instrument (Spec 20, AAS, or HPLC) 30 Total Possible 970 Multiply above by Notebook 50 Quizzes Total possible points times a factor equal to 125 Technique, etc. 25 Lab total possible 650 Lecture 3 Hour exams 300 Final Quizzes 100 Lecture total possible 650 Grand Total 1300 Page 2 of 5

3 Laboratory Activities for Fall Check-in and preliminary operations a) View film concerning laboratory safety: safety quiz. b) Become proficient in the use of analytical balances. c) Quiz on basic algebra, logarithms, and chemistry. 2. Gravimetric determination of chloride in a solid sample. SILVER IS COSTLY. Put excess 5% AgNO 3 solution as well as solid AgCl in bottles provided. Do not save wash solutions. Report results by September 18 th. 3. Preparation of standard EDTA solution. 4. EDTA determination of total hardness, calcium and magnesium in a brine sample. 5. Certification of a reagent solution (Mn, Zn, or Co) by EDTA titration. 6. Preparation and standardization of 0.1 M NaOH. 7. Calibration of ph electrode. 8. Potentiometric titration of a mixture of phosphoric acid and sodium dihydrogen phosphate. 9. Submit explicit directions for the preparation of 500 ml of M ph 7.0 phosphate buffer solution. Use activity coefficients. Report by October 19 th. 10. Spectrophotometric determination of manganese in steel. 11. Manganese determination by atomic absorption spectroscopy using both calibration curve and standard addition procedures. 12. Calibration of chloride ion selective electrode. 13. Determination of chloride in a mixture by direct potentiometry. 14. Determination of components of a mixture of polyaromatic hydrocarbons by high performance liquid chromatography. 15. Checkout of locker by Dec. 10. Students failing to check out officially will be charged a fee for the service center to check out the lockers. Page 3 of 5

4 Your lab notebook table of contents should have at least the following entries: EXPERIMENT Page Gravimetric Chloride Determination Preparation of Standard EDTA Solution Hardness by EDTA Titration Ca and Mg by EDTA Titration. Certification of a Solution Concentration by EDTA Titration. Preparation and Standardization of NaOH Solution Calibration of ph Electrode Determination of H 3 PO 4 and NaH 2 PO 4 in a Mixture Directions for preparing ph 7.00 Buffer solution Determination of Manganese in Steel by: Photometry AAS, Calibration Curve AAS, Standard Addition Instrument Calibration Record Calibration of Cl- Electrode. Potentiometric Determination of Chloride by ISE Analysis of a Polyaromatic Hydrocarbon Mixture by HPLC Please note: you must also record the data for: 1) Certification of Solution, 2) ph Electrode Calibration, 3) Cl Electrode Calibration, and 4) Major Instrument Calibration in the appropriate record book, as well as in your notebook. Page 4 of 5

5 ADDENDUM TO ALL CHEMISTRY DEPARTMENT GREENSHEETS (Except Chem 291 Sections) Revised August 2002 CHEMICAL SAFETY all courses Chem 120S is a required course for all chemistry majors and minors and a prerequisite for all Chem 180/298 research. EMERGENCIES AND EVACUATIONS all courses If you hear a continuously sounding alarm, or are told to evacuate by Emergency Coordinators (colored badge identification), walk quickly to the nearest stairway (end of each hall). Take your personal belongings, as you may not be allowed to immediately return. Follow instructions of Emergency Coordinators. Be quiet so you can hear. Once outside, move away from the building. Do no return to the building unless the Police or Emergency Coordinators announce that you may. DISABLED STUDENTS all courses Any student with a pre-existing disability requiring an accommodation (as documented by the Disability Resource Center) should make this need known to the instructor during the first two weeks of classes. Every effort will be made to accommodate your needs. ACADEMIC DISHONESTY all courses Academic dishonesty of any sort will subject the involved person(s) to university mandated consequences. You should be familiar with the section of the SJSU Catalog entitled Policy of Academic Dishonesty (pp in the 2002/04 Catalog). Incidents of academic dishonesty may be referred to the Chief Judicial Affairs Officer of the University and reports may be placed in Department and /or University files. For courses with written assignments include: Note in particular that plagiarism, word-for-word copy of another person s words without proper attribution (quotation marks and a clear literature reference), is a particularly serious form of academic dishonesty. LABORATORY SAFETY all laboratory courses You should read the safety section of the SJSU Catalog under Chemistry Department (page 136 of current 2002/04 Catalog). Note in particular: Failure to comply with proper procedures and prescribed safety cautions shall subject the student to disciplinary action. 1) Any student who engages in unauthorized experimentation, or who seriously disregards safety, thereby endangering self or others shall be withdrawn immediately from the class with a grade of F. 2) Any student who show persistent disregard for safety may have his/her grade lowered, and may risk being withdrawn with a final grade of F. Page 5 of 5