Instrument Notes

 
                                                                                               

                                                                                               

 

   Light blue boxes are active links to my own notes. 

   You should also read the assigned material from the lecture text.

 

        

Technique

Equipment Available

Sample Prep

Text Box: E-Chem

Cyclic voltammetry

pp 190 – 191 of our lecture text

 

EG&G Princeton Applied Research Model 362 Scanning Potentiostat

DATAQ A to D interface for data collection

Supporting electrolyte solution, prepare 10 mL

   in organic solvents: 0.1 M [NBu4][BF4]

   in water: 0.1 M KCl

Need about 5 mg of sample

Text Box: EPR

Electron paramagnetic resonance
(ESR, electron spin resonance)
     pp 181 – 183 of lecture text

·    H. A. Farach and C. P. Poole, Jr. provides an overview of the technique.

·    On-line EPR help from Natl. Inst. of Environmental Health Sciences (NIEHS) EPR research groups

 

Resonance Instruments Model 8400

Approximately 0.05 M solutions.

 

Less polar solutions can be recorded in cylindrical quartz EPR tubes.

 

More polar solutions must use flat quartz EPR cell.

Text Box: NMR

Nuclear magnetic resonance

pp 177 – 181

 

Jeol ECX-300 FT-NMR

0.1 M solutions

Can be run in protio solvents, although deuterated

give good lock and shim.

Text Box: IR

Infrared 

pp 175 – 177

 

Thermo Nicolet FTIR 100

as KBr pellets

 

ATR attachment: allows direct spectra collection on bulk powders

Text Box: UV-vis

Electronic spectroscopy

Ch 19 of the lecture text

 

Varian Cary 50

1 cm quartz cuvettes

Text Box: Magnetic Susceptibility

pp 463 – 465 of lecture text

Johnson-Matthey MSB-1 magnetic susceptibility balance

 

finely ground powder packed in glass tube about the same diameter as an NMR tube

Text Box: GCMS

pp 185 – 187 of lecture text

Varian CP-3800 GC, Saturn 2200 MS