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E-raamat: Quantitative EPR

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  • Formaat: PDF+DRM
  • Ilmumisaeg: 10-Apr-2010
  • Kirjastus: Springer Verlag GmbH
  • Keel: eng
  • ISBN-13: 9783211929483
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Quantitative EPRSuurem pilt
  • Formaat: PDF+DRM
  • Ilmumisaeg: 10-Apr-2010
  • Kirjastus: Springer Verlag GmbH
  • Keel: eng
  • ISBN-13: 9783211929483
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There is a growing need in both industrial and academic research to obtain accurate quantitative results from continuous wave (CW) electron paramagnetic resonance (EPR) experiments. This book describes various sample-related, instrument-related and software-related aspects of obtaining quantitative results from EPR expe- ments. Some speci c items to be discussed include: selection of a reference standard, resonator considerations (Q, B ,B ), power saturation, sample position- 1 m ing, and ?nally, the blending of all the factors together to provide a calculation model for obtaining an accurate spin concentration of a sample. This book might, at ?rst glance, appear to be a step back from some of the more advanced pulsed methods discussed in recent EPR texts, but actually quantitative “routine CW EPR” is a challenging technique, and requires a thorough understa- ing of the spectrometer and the spin system. Quantitation of CW EPR can be subdivided into two main categories: (1) intensity and (2) magnetic ?eld/mic- wave frequency measurement. Intensity is important for spin counting. Both re- tive intensity quantitation of EPR samples and their absolute spin concentration of samples are often of interest. This information is important for kinetics, mechanism elucidation, and commercial applications where EPR serves as a detection system for free radicals produced in an industrial process. It is also important for the study of magnetic properties. Magnetic ?eld/microwave frequency is important for g and nuclear hyper ne coupling measurements that re ect the electronic structure of the radicals or metal ions.
Introduction.- Principles of Quantitative EPR; Why should examples of
applications be quantitative?; Examples of applications.- Introduction to
Quantitative EPR; General expression for CW EPR signal intensity; The EPR
transition; Derivative spectra; The CW EPR line width; Second derivative
operation; What transitions can we observe; Features of transition metal EPR;
Parallel and perpendicular transitions.- Getting started- some practical
matters; Operating the spectrometer-cautionary notes; Sample preparation;
Don´t forget the cooling water!; Detector current; Automatic frequency
control and microwave phase; Searching for a signal; Gain; Effect of scan
rates and time constants on S/N and signal fidelity; bandwidth
considerations; scan rate and filter time constant; selecting a
non-distorting filter and scan rate; A note about comparing noise in CW and
pulsed EPR; Background signals; Integration; Microwave power; Modulation
amplitude; Modulation amplitude calibration; How to select modulation
frequency; Modulation sidebands;Illustration of the effect of modulation
amplitude, Modulation frequency, Microwave power on the spectra of free
radicals; Phase; Automatic frequency control and microwave phase;Sample
considerations; Passage effects; Software; Summary guidance for the operator;
Scaling results for quantitative comparisons; Signal averaging; Number of
data points, Cleanliness; Changing samples; NMR gaussmeter interference.-
What matters, and what can you control? Crucial parameters and how they
affect EPR signal intensity;What accuracy can one aspire to?- A deeper look
at B1 and modulation field distribution in a resonator; Inhomogenity of B1
and modulation amplitude; Flat cells; Double-cavity simultaneous reference
and unknown.-Resonator Q; Conversion efficiancy, C;Contributions to Q;
Measurement of Resonator Q.- Filling factor. Temperature; Intensity vs.
temperature; Practical example; Glass-forming solvents; Practical aspects of
controlling and measuringsample temperature; Operation above room
temperature.-Magnetic field and Microwave frequency;G-values; Microwave
frequency; Magnetic field; Magnetic field homogenity; Coupling constants vs.
hyperfine splittings.-Standard samples; Comparison with a standard sample;
Standard samples for Q-band; Achievable accuracy and precision- g value and
hyperfine splitting.- How good can it get?- Absolute EPR signal intensities;
The spin magnetization M for an arbitrary spin S; Signal voltage; Calculation
of noise; Calculation of S/N; Summary of impact of parameters on S/N; How to
improve the spectrometer-the Friis equation.- Less common measurements with
EPR spectrometers; Multiple resonance methods; Saturation transfer
spectroscopy; Electrical conductivity; Static magnetization.
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