Quantitative EPR:
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| Format: | Book |
|---|---|
| Language: | English |
| Published: |
Wien [u.a.]
Springer
2010
|
| Subjects: | |
| Online Access: | Inhaltsverzeichnis |
| Item Description: | Literaturverz. S. 167 - 178 |
| Physical Description: | XII, 185 S. Ill., graph. Darst. |
| ISBN: | 3211929479 9783211929476 |
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MARC
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Record in the Search Index
| _version_ | 1804142724793761792 |
|---|---|
| adam_text | Titel: Quantitative EPR
Autor: Eaton, Gareth R
Jahr: 2010
Contents
1 Basics of Continuous Wave EPR .......................................... 1
1.1 The Zeeman Effect ..................................................... 1
1.2 Hyperfine Interactions .................................................. 3
1.3 Signal Intensity ......................................................... 5
1.4 Introduction to Typical CW EPR Spectrometers ....................... 5
1.5 The Microwave Bridge ................................................. 6
1.6 The EPR Cavity ......................................................... 8
1.7 The Signal Channel .................................................... 10
1.8 The Magnetic Field Controller ........................................ 13
1.9 TheSpectrum .......................................................... 14
2 Why Should Measurements Be Quantitative? .......................... 15
2.1 Examples of Applications of Quantitative EPR ....................... 16
2.2 Measuring Unstable Radicals by Spin Trapping: Effect
of Resonator Q ......................................................... 18
2.3 Measuring Weak Signals in the Presence of Strong Ones:
Dynamic Range Issues ................................................. 18
2.4 Signals in Mixtures .................................................... 19
2.5 Radiation Dosimetry ................................................... 19
2.6 Use of Accurate Line Width Information ............................. 21
2.7 Catalysis and Mineralogy .............................................. 22
2.8 Free Radical Content in Commercial Materials ....................... 22
2.9 Feasibility of Quantitative EPR ....................................... 23
2.10 Further Reading ...................................................... 24
3 Important Principles for Quantitative EPR ............................. 25
3.1 The EPR Transition and Resulting Signal ............................. 25
3.2 Relaxation and Saturation ............................................. 26
3.3 Why Are EPR Spectra Displayed as the Derivative? ................. 28
3.4 Some Caveats About Modulation and First Derivative Displays ..... 28
3.5 Finding the Signal Area Requires a Double Integration .............. 30
3.6 The CW EPR Line Width ............................................. 31
x Contents
3.7 Transition Metal EPR .................................................. 32
3.8 Spectrometer Field and Frequency May Determine
Which Transitions Are Observed ...................................... 32
3.9 Parallel and Perpendicular Transitions ................................ 34
4 A More in Depth Look at the EPR Signal Response ................... 37
4.1 Sample Preparation .................................................... 37
4.1.1 Capillary Tube Sealant ......................................... 37
4.2 Searching for a Signal (Also See Appendix A) ....................... 38
4.3 Detector Current ....................................................... 38
4.4 Optimize the Receiver Gain ........................................... 39
4.5 Be Aware of Noise Sources ........................................... 39
4.6 Number of Data Points ................................................ 40
4.7 Optimize the Sweep Time and Conversion Time ..................... 41
4.8 Optimize the Time Constant for the Selected Sweep
Time and Conversion Time ............................................ 42
4.9 Background Signals .................................................... 43
4.10 Integration ............................................................ 44
4.11 Microwave Power .................................................... 45
4.12 Modulation Amplitude (Also See Appendix B for More
Details on This Topic) ................................................ 48
4.13 Modulation Amplitude Calibration .................................. 51
4.14 How to Select Modulation Frequency ............................... 54
4.15 Passage Effects ....................................................... 55
4.16 Illustration of the Effect of Modulation Amplitude, Modulation
Frequency, and Microwave Power on the Spectra
of Free Radicals ...................................................... 55
4.17 Phase .................................................................. 56
4.18 Automatic Frequency Control and Microwave Phase ............... 58
4.19 Resonator Design for Specific Samples .............................. 59
4.20 Software .............................................................. 59
4.21 Scaling Results for Quantitative Comparisons ....................... 59
4.22 Signal Averaging ..................................................... 60
4.23 Cleanliness ............................................................ 61
5 Practical Advice About Crucial Parameters ............................ 63
5.1 Crucial Parameters and How They Affect EPR Signal Intensity ..... 63
5.2 What Accuracy Is Achievable? ........................................ 65
5.3 A More In-Depth Look at Adjusting the Coupling to the
Resonator in the Tuning Procedure ................................. 66
6 A Deeper Look at Bi and Modulation Field Distribution
in a Resonator ............................................................. 69
6.1 Separation ofB] and Ei ............................................... 69
Contents xi
6.2 Inhomogeneity of B] and Modulation Amplitude ..................... 70
6.3 Sample Size ............................................................ 73
6.4 AFC Considerations ................................................... 73
6.5 FlatCells ............................................................... 75
6.6 Double-Cavity Simultaneous Reference and Unknown ............... 76
6.7 Summary ............................................................... 76
7 Resonator Q ............................................................... 79
7.1 Conversion Efficiency, C ............................................. 80
7.2 Loaded Q and Unloaded Q ............................................ 81
7.3 Relation of Q to the EPR Signal ...................................... 83
7.4 Contributions to Q ..................................................... 83
7.5 Measurement of Resonator Q ......................................... 84
7.5.1 Estimate Q Using the Bruker Software ......................... 85
7.5.2 Q Measurement Using a Network Analyzer:
By George A. Rinard ........................................... 85
7.5.3 Q by Ring Down Following a Pulse ............................ 86
8 Filling Factor .............................................................. 89
8.1 General Definition ..................................................... 89
8.2 Calculation of Filling Factor .......................................... 89
9 Temperature ............................................................... 91
9.1 Temperature Dependence of Signal Intensity ......................... 91
9.2 Sample Preparation for Cryogenic Temperatures ..................... 92
9.2.1 Selection of Solvent ............................................ 92
9.2.2 Sealed Samples ................................................. 92
9.3 Practical Aspects of Controlling and Measuring
Sample Temperature ................................................... 93
9.3.1 Cavity Resonators .............................................. 94
9.3.2 Flexline Resonators ............................................. 95
9.3.3 Other Components of the Cooling Systems .................... 97
9.4 Operation Above Room Temperature ................................. 98
9.5 Example for S 1/2 .................................................... 98
10 Magnetic Field and Microwave Frequency ............................ 101
10.1 g-Factors ................................................................ 101
10.2 Measurement of Microwave Frequency ............................... 101
10.3 Magnetic Field .......................................................... 102
10.4 Magnetic Field Homogeneity .......................................... 103
10.5 Coupling Constants Vs. Hyperfine Splittings .......................... 104
10.6 Achievable Accuracy and Precision: g Value
and Hyperfine Splitting ................................................. 104
xü Contents
11 Standard Samples ....................................................... 107
11.1 Comparison with a Standard Sample ............................. 107
11.2 Spin Quantitation with a Calibrated Spectrometer ................ 109
Appendix ...................................................................... 115
Appendix A: Acquiring EPR Spectra and Optimizing Parameters ..... 115
Appendix B: Field Modulation and Phase Sensitive Detection ......... 124
Appendix C: Post Processing for Optimal Quantitative Results ........ 132
Appendix D: Quantitation of Organic Radicals Using Tempol ......... 141
Appendix E: Using a Reference Standard for Relative
Intensity Measurements ................................... 146
Appendix F: Example Procedure for Measuring
Signal-to-Noise Ratio ..................................... 151
Appendix G: How Good Can It Get: Absolute EPR Signal Intensity ... 157
References ..................................................................... 167
Index ........................................................................... 179
|
| any_adam_object | 1 |
| building | Verbundindex |
| bvnumber | BV025550959 |
| classification_rvk | VG 9700 |
| ctrlnum | (OCoLC)699323694 (DE-599)BVBBV025550959 |
| dewey-full | 543.67 |
| dewey-hundreds | 500 - Natural sciences and mathematics |
| dewey-ones | 543 - Analytical chemistry |
| dewey-raw | 543.67 |
| dewey-search | 543.67 |
| dewey-sort | 3543.67 |
| dewey-tens | 540 - Chemistry and allied sciences |
| discipline | Chemie / Pharmazie |
| format | Book |
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| id | DE-604.BV025550959 |
| illustrated | Illustrated |
| indexdate | 2024-07-09T22:36:19Z |
| institution | BVB |
| isbn | 3211929479 9783211929476 |
| language | English |
| oai_aleph_id | oai:aleph.bib-bvb.de:BVB01-020151367 |
| oclc_num | 699323694 |
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| owner_facet | DE-11 DE-188 DE-703 |
| physical | XII, 185 S. Ill., graph. Darst. |
| publishDate | 2010 |
| publishDateSearch | 2010 |
| publishDateSort | 2010 |
| publisher | Springer |
| record_format | marc |
| spelling | Quantitative EPR Gareth R. Eaton ... Wien [u.a.] Springer 2010 XII, 185 S. Ill., graph. Darst. txt rdacontent n rdamedia nc rdacarrier Literaturverz. S. 167 - 178 Elektronenspinresonanzspektroskopie (DE-588)4151888-3 gnd rswk-swf Elektronenspinresonanzspektroskopie (DE-588)4151888-3 s DE-604 Eaton, Gareth R. Sonstige oth Erscheint auch als Online-Ausgabe 978-3-211-92948-3 HBZ Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=020151367&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis |
| spellingShingle | Quantitative EPR Elektronenspinresonanzspektroskopie (DE-588)4151888-3 gnd |
| subject_GND | (DE-588)4151888-3 |
| title | Quantitative EPR |
| title_auth | Quantitative EPR |
| title_exact_search | Quantitative EPR |
| title_full | Quantitative EPR Gareth R. Eaton ... |
| title_fullStr | Quantitative EPR Gareth R. Eaton ... |
| title_full_unstemmed | Quantitative EPR Gareth R. Eaton ... |
| title_short | Quantitative EPR |
| title_sort | quantitative epr |
| topic | Elektronenspinresonanzspektroskopie (DE-588)4151888-3 gnd |
| topic_facet | Elektronenspinresonanzspektroskopie |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=020151367&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
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