Instrument Notes                                                                                       

                                                                                   

You should also read the assigned material from the lecture text (Shriver, et al. Inorganic Chemistry, 6e, 2014 Freeman).

 

        

Technique

Equipment Available at UCA

Typical Sample Preparations

Electrochemistry

Cyclic voltammetry (CV)

p 264 of lecture text

my CV notes

 

EG&G Princeton Applied Research Model 362

Scanning Potentiostat

DATAQ AtoD 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

EPR

Electron paramagnetic resonance
(ESR, electron spin resonance)
     pp 253,772 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.

NMR

Nuclear magnetic resonance

pp 247-249

 

Jeol ECX-300 FT-NMR

0.1 M solutions

Can be run in protio solvents, although deuterated

give good lock and shim.

IR

Infrared 

p 244-5

 

Thermo Nicolet FTIR 100

as KBr pellets     my notes on IR sample prep

 

ATR attachment: allows direct spectra collection on bulk powders

UVvis

Electronic spectroscopy

·         Ch 20 of the lecture text

·         Ch 22 W. L. Jolly 1991

 

Diffuse reflectance (solid samples)

Varian Cary 50

 

 

Video Barrelino Diffuse Reflectance attachment
(Harrick Sci.)

1 cm quartz cuvettes

 

 

solid between microscope slides, MgO as reference

Luminescence

Fluorescence

p 243

Perkin Elmer LS45 Luminescence Spectrometer

as solutions using special fluorescence cuvettes

or

as solids using a special powder cell holder

Magnetic Susceptibility

p 264,544 of lecture text

my mag. suscept. notes

·         Ch 25 W. L. Jolly 1991

·         MSB1 brochure

 

Johnson-Matthey MSB-1 magnetic susceptibility balance

 

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

GC/MS

Gas chromatography/mass spectrometry

Varian CP-3800 GC, Saturn 2200 MS