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Text: Skoog, West, and Holler, Analytical Chemistry--An Introduction, Sixth Edition.
1 per. 1. Check-in and Balance Instruction. Also read SWH Ch. 28, pp. 531-563, Lab Procedures
Begin Tu 27 Aug-- End Tu 27 Aug
4 per. 2. Gravimetric Determination of Chloride -- Solid Unknown (also
used for Vol Cl below)
Procedure as in SWH pp. 566-568 except assume
unknowns are 60% by weight of chloride and digest precipitate for one week,
during which the glassware calibration (below) is done. Prepare 500 ml of
0.1M Silver Nitrate, not 0.2 M. Use the remainder for Volumetric Chloride.
Report %Cl.
Begin Th 29 Aug-- End Th 12 Sep (5 periods -- includes
glassware calibration. below)
1 per. 3. Calibrate Volumetric Glassware (SWH pages 557-560). Do
buret, 10 ml pipet, and 25 ml pipet. Report results in laboratory
notebook.
--done during the AgCl digestion period.
3 per. 4. Volumetric Determination of Chloride Using Adsorption
Indicator. Same Solid Unknown used above for Grav Cl. SWH pages 579-580.
Report %Cl.
Begin Tu 17 Sep -- End Tu 24 Sep. Results of %Cl Grav
and Vol due Tue 1 Oct.
4 per. 5. Determination of %KHP in a solid unknown. Procedure as in
SWH 29B-7 and 2B-8, p 573-574; 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. Report
%KHP (100 points, as usual).
Begin Thu 26Sep-- End Tu 8 Oct. %KHP
results due Tue 15 Oct.
4 per. 6. Determination of Calcium with EDTA. Solid Unknown.
Procedure on handout. (See also SWH pp. 580-582) Report %CaO.
Begin Thu 10 Oct-- End Tu 22 Oct. %CaO results due Tue 29 Oct.
5 per. 7. Spectrophotometric Iron. Solid Unknown. Procedure for molecular absorption in SWH, pages 604-605, except 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 Titration experiment. Once standards and unknowns have been prepared for Molecular Absorption Spectrophotometry, we will have you make runs on Atomic Absorption as well. Your instructor will provide directions for AA. Report %Fe in the solid unknown by both methods (50 points each) Begin Thu 24 Oct-- End Th 7 Nov. %Fe results by both methods due Tu 12 Nov.
4 per. 8. Determination of Iron in Ore by Redox Titration. Use the
same unknown issued for Experiment 7. Procedure SWH 29E-1, p. 582 (Prep of
Permanganate); 29E2, p. 582-3 (Stdz. of Permanganate); 29E-4, p. 585-588
(Determination. of Fe in ore.). Report %Fe in the ore.
Begin Tu 12
Nov -- End Thu 21 Nov. %Fe results due Tue, 26 Nov.
3 per. 9. Determination of Glucose. Solid Unknown. Procedure on
Handout. Report mg Glucose per 100 ml per 2 gram sample.
Begin Tu 26
Nov-- End Th 5 Dec. Glucose results due Tu 10Dec.
1 per. 10. Clean up and check out. No experiments on Tuesday, Dec 10 (last lab day).
Laboratory results must be reported during the week following the last day of the experiment. Experiments finished but with unacceptable errors are worth 30 points. Experiments not completed are worth 0 points. A 20 point penalty is exacted for repeated or recalculated experiments, or for a new unknown to replace one you botched. Late penalties of 5 points per period may be assessed at the discretion of your instructor.