Escolar Documentos
Profissional Documentos
Cultura Documentos
The Course
replaced by water and the second component-the yellow There are a number of standard texts for microscale (2-
fluorescein-is collected in another test tube. 4) and spectroscopic techniques (5, 6)on the market, and
If desired, the concentration of the recovered methylene we maintain copies of each on the laboratory reference
blue can be measured quantitatively from absorbance shelf. A suitable microscale qualitative organic analysis
readings using a W-visible spectrophotometer. In this text is not available so we have adopted references 2 and 5
case the amount of dye applied to the column (0.2-0.3 mL) as course texts and prepared a 15-pagelaboratory handout
must be measured accurately. The entire methylene blue containing information about the course a s well as several
eluate is diluted with 95% ethanol to 100 mL in a volumet- specific procedures, a number of which are described
ric flask. One milliliter of this solution is further diluted below. Students also are provided cross references for the
with 95% ethanol to 50 mL in another volumetric flask. chemical classification tests found in reference 2 and the
From the absorbance of this solution, the concentration of traditional Shriner text (7)available on the laboratory ref-
methvlene icalculated in millimams of methvlene blue oer erence shelf.
milliliter of mixture) can be found by reference to a calibra- The laboratory portion of the course meets twice weekly
tion curve made from suitably diluted samples of a stock for two hours and the students are expected to identify the
solution containing 3.8 x 104 g of methylene blue in 1L of structures of five "unknown&"-three (separate samples of
95% ethanol. All absorbance readings are made a t Lnx= 750 my each and a two-component mixture contain in^ 1.00
663 nm. The quantitative determination of fluoresceinis g of each compound-by the end of the fall semester. While
not as accurate because commercially available fluorescein the identification of these unknowns is based primarily on
contains some impurities and the quantitative analysis of the interpretation of FTIR, NMR, and GCiMS (liquids
these samples is not as precise. only) spectral data, the determination of physical con-
stants, the purification of solids and liquids, the perfor-
Literature Cited mance of selected chemical classification tests and the
1. Lehman, J. W. Operational Organic Chemistry, 2nd ad.; AUyn and Bacon: Boston, preparation ofone derivative out of five unknowns are car-
1988.
2. Fieser, L. F.;WiUiamson, K L.Organic Experiments, 8th ed.; D.C. Heath: Lexington, ried out using microscale techniques and equipment." The
1979. chemical classification tests help students reriolve uncer-
3.Ault.A.Technkes and Experimentsin Organic Chemistry, 4th ed.;Allyn and Bacon: tainties created by unexpected or ambigmous spectral dam.
Boston. 1979.
4, Williaroaon,K L. M m m i f - and MicroscaleOrganic Exaerimerits;D. C. Heath:Lex-
ington. 1989,
-
The 15-nagelaboratory handout contains a microscale ~ r o -
cedure for the separation of a two-component mixture
5. - f a k . D. F.; Hoemer, R. S, J. C k m . Educ. 1991,6873.
6. Rodig,O.R.;Bell,C. E.,Jr.;Clark,A. K OrganicchemistryLabom10ry:Stdrdand
MicroscaleExperiments; Saundem: Philadelphia. 1990. '3910 Timber Ridge Place, Midlothain, VA 23113
7. Roberts. R.M.;Gilbert, J, C.; Rodewald, L. B.; Wingrove, A . S. Modern Experimental %lost, but not all, chemistry majors perform senior thesis research
Organic Chemistry, 5th ed; Philadelphia: Saunders, 1988. or summer research beforegraduating from VMI
8. Nilaitz, J. S. Experiments in Organic Chemistry:From M i c m x ~ kto Macrmde; En.
dewood Cliffs:Prentice-Hall. 1991. = ~ cGlass,
e lnc microscale laboratory equipment.
(Continued on next page)
Volume 70 Number 6 June 1993 A159