Note: Some of the links on this page are accessible only from computers that have a Gustavus address.

All procedures are in Adobe Acrobat portable document format (.PDF). They can be read and printed off via Acrobat Reader. If you do not have Acrobat Reader, it can be downloaded free of charge from: http://www.adobe.com/products/acrobat/readermain.html.


Preparation and Analysis of Transition Metal Hexanitritometallates - Background and Procedures, including pre-lab and report sheets

pre-lab sheet only
report sheet only

IR spectra
K2BaNi(NO2)6 - entire spectrum
K2BaNi(NO2)6 - nitrite region
K2BaCo(NO2)6 - nitrite region
K2SrCo(NO2)6 - nitrite region
K2SrCu(NO2)6 - nitrite region
K2SrNi(NO2)6 - nitrite region




Acylation of Ferrocene or n-Butylferrocene - see your organic laboratory manual for the procedure for acetylferrocene.

Lab Report Instructions
1. Answer the questions from the end of the experiment in the laboratory manual.
2. Further instructions:

Assign the 13C NMR signals of acetylferrocene. Provide a brief description of the reasoning that you used to make your assignments.

Assign the DEPT spectrum of acetylferrocene.

The 1H NMR spectrum available below has some interesting features of which you should be aware, but it is not necessary to include an analysis of it in your report, since the assignments are made in the laboratory text.

13C NMR spectrum of acetylferrocene (CDCl3, Boyum/McDevitt/Groth/Huseby combined sample)
DEPT (90 and 135) NMR spectra of acetylferrocene (same sample)
1H NMR spectrum of acetylferrocene (same sample)



Preparation and Analysis of an Ester of Phosphorous Acid
Experimental Procedures

report sheet

Product A

NMR Spectra
1H
1H with integrals
31P, non-decoupled
31P, 1H-decoupled
13C

GC/MS

IR

Product B
1H
1H with integrals
13C

IR

Product C
1H
1H with integrals
1H with expansion
31P, 1H-coupled
31P, 1H-decoupled
13C

IR

Product D
1H NMR


Reference Items
tables of IR absorptions and NMR coupling constants for organophosphorus compounds

EtPH2 1H NMR
EtPH2 IR

CH2(PH2)2 1H and 13C NMR

benzylamine 1H NMR
benzylamine 13C NMR
benzylamine IR


Preparation of a Macrocyclic Complex of Cu(III)
Background and Procedures

report sheet only


Tetraamminecopper(II) Sulfate Monohydrate and Diethylammonium Tetrachlorocuprate(II)
Background and Procedures

pre-lab sheet
report sheet - Spring 2004

IR and Visible spectra
Cu(NH3)4SO4.H2O - IR
Cu(NH3)4SO4.H2O - visible
(Et2NH2)2CuCl4 room temperature
(Et2NH2)2CuCl4 room temperature - expansion
(Et2NH2)2CuCl4 65 C - expansion
visible and IR spectra of (Et2NH2)2.CuCl4 from the literature

Et2NH2.Cl
Na2SO4


Preparation and Analysis of Ammine Complexes of Co(III)
Experimental Procedures
pre-lab for the first week
pre-lab for the second week
report sheet

IR spectra
Co.NH3.5.Cl.Cl2
Co.NH3.6.Cl3
Co.NH3.5.H2O.Cl3
Co.NH3.5.NO2.Cl2.isomer.A
Co.NH3.5.NO2.Cl2.isomer.B

Visible spectra - use the spectra that were recorded with the Ocean Optics spectrophotometer:
four superimposed visible spectra (note: isomer A is unstable in solution, so only the visible spectrum of isomer B was recorded)


Preparation and Analysis of Chiral Tris(1,10-phenanthroline)cobalt(III)
Background and Procedures, including pre-lab and report sheets

Flow Chart


Preparation and Analysis of Tris(2,4-pentanedionato) and Tris(1,1,1-trifluoro-2,4-pentanedionato) Complexes of Cobalt(III)
Background and Procedures, including lab report instructions, report sheet, and pre-lab sheet

spectra


Preparation and Analysis of a Peculiar and Poorly Understood Oxide of Tungsten
background, experimental procedures, report instructions, and pre-lab sheet


Preparation of Salen

Lab Report Instructions

Salen Spectra
1H NMR spectrum
integrated 1H NMR, 10 second pulse delay (use this version for your analysis)
integrated 1H NMR, 1 second pulse delay (compare the integrals for the aromatic hydrogens to those with
higher-field aromatic signals - expansion
lower-field aromatic signals - expansion
lowest-field signals - expansion

13C NMR spectrum - to be linked later
DEPT spectra - to be linked later

infrared spectrum

Preparation and Analysis of a Cross-Linked Silicone Polymer
background, experimental procedures, report instructions, and pre-lab sheet

IR spectra
poly(dimethylsiloxane)
poly(methylhydrosiloxane) (for comparison - analysis is not required for your report)