X-ray microanalysis for biologists:
Gespeichert in:
| 1. Verfasser: | |
|---|---|
| Format: | Buch |
| Sprache: | English |
| Veröffentlicht: |
London [u.a.]
Portland Press
1997
|
| Schriftenreihe: | Practical methods in electron microscopy
16 |
| Schlagworte: | |
| Online-Zugang: | Inhaltsverzeichnis |
| Beschreibung: | XXIII, 276 S. Ill., graph. Darst. |
| ISBN: | 1855780542 1855780550 |
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Datensatz im Suchindex
| _version_ | 1804126033319821312 |
|---|---|
| adam_text | PRACTICAL METHODS IN ELECTRON MICROSCOPY VOLUME 16 SERIES EDITOR: AUDREY
M. GLAUERT GORE HALL UNIVERSITY OF CAMBRIDGE U.K. PORTLAND PRESS LONDON
AND MIAMI CONTENTS XVII CONTENTS EDITOR S PREFACE VII AUTHOR S PREFACE
AND ACKNOWLEDGEMENTS IX SYMBOLS AND ABBREVIATIONS XIII I 2 5 6 7 8 9 10
10 10 12 12 13 2 PRODUCTION OF X-RAYS 15 2.1 EXCITATION OF X-RAYS . 15
2.2 CHARACTERISTIC X-RAYS 18 2.3 CONTINUUM X-RAYS 22 2.4 FACTORS
AFFECTING THE PRODUCTION OF X-RAYS 23 2.4.1 CRITICAL EXCITATION
POTENTIAL 23 2.4.2 LONIZATION CROSS-SECTION AND FLUORESCENT YIELD 24 2.5
FACTORS AFFECTING EMERGENCE OF X-RAYS FROM THE SPECIMEN 26 2.5.1 X-RAY
FLUORESCENCE 2B 2.5.2 ABSORPTION OF X-RAYS 27 1 I.I 1.2 1.3 1.4 1.5
INTRODUCTION WHAT IS ELECTRON-PROBE X-RAY MICROANALYSIS? INTERACTIONS OF
THE ELECTRON BEAM WITH THE SPECIMEN ANALYSISOF BIOLOGICAL SPECIMENS
CAPABILITIES OF ELECTRON-PROBE X-RAY MICROANALYSIS SAFETY 1.5.1 1.5.2
1.5.3 1.5.4 THE SPECIMEN HAZARDOUS CHEMICALS GLASS KNIVES LOW
TEMPERATURE WORK 1.5.4A LIQUID NITROGEN 1.5.4B LIQUID CRYOGENS 1.5.4C
COOLED APPARATUS L.5.4D CONTAINERS XVIII CONTENTS 3 INTERACTION OF THE
ELECTRON BEAM WITH THE SPECIMEN 29 3.1 THE INTERACTION VOLUME 29 3.1.1
EFFECT OF ACCELERATING VOLTAGE ON THE INTERACTION VOLUME 29 3.1.2
EFFECTS OF SPECIMEN MASS AND THICKNESS ON THE INTERACTION VOLUME 30
3.1.3 X-RAY PRODUCTION FROM THIN SPECIMENS 31 3.1.4 X-RAY PRODUCTION
FROM SEMI-THICK SPECIMENS 32 3.1.5 X-RAY PRODUCTION FROM THICK SPECIMENS
33 3.2 DAMAGE TO THE SPECIMEN DURING THE PRODUCTION OF X-RAYS 36 3.2.1
MECHANISMS BY WHICH BEAM DAMAGE OCCURS 36 3.2.2 ACCELERATING VOLTAGE AND
ELECTRON DOSE 3 7 3.2.3 SPECIMEN COMPOSITION AND BEAM DAMAGE 38 3.2.4
RELEVANCE OF BEAM DAMAGE TO X-RAY MICROANALYSIS 38 3.2.4A LOSS OF
ELEMENTS 38 3.2.4B LOSS OF MASS FROM DRY SPECIMENS 38 3.2.4C LOSS OF
MASS FROM HYDRATED SPECIMENS 40 3.2.4D LOSS OF MASS FROM BULK SPECIMENS
42 4 THE GENERATION AND COLLECTION OF X-RAYS 45 4.1 ELECTRON MICROSCOPES
FOR X-RAY MICROANALYSIS 45 4.1.1 THE PROBE CURRENT 48 4.1.1A THE EFFECT
OF THE ELECTRON EMITTER ON PROBE CURRENT 49 4.1.1B MEASUREMENT OF THE
PROBE CURRENT 51 4.1.2 THE VACUUM SYSTEM AND CONTAMINATION 52 4.1.3
PRODUCTION OF EXTRANEOUS X-RAYS 54 4.1.4 SPECIMEN HOLDERS 56 4.2 ENERGY
DISPERSIVE X-RAY DETECTORS 57 4.2.1 THE SILI DETECTOR CRYSTAL 59 4.2.2
STRUCTURE OF THE EDS DETECTOR 61 4.2.3 X-RAY DETECTION IN AN EDS SYSTEM
63 4.3 SPECTRAL MODIFICATIONS 70 4.3.1 DETECTOR EFFICIENCY 70 4.3.1A
EFFICIENCY FOR X-RAYS FROM ELEMENTS OF LOW ATOMIC NUMBER 7 / 4.3.1B
EFFICIENCY FOR X-RAYS FROM ELEMENTS OF HIGH ATOMIC NUMBER 73 4.4 4.5 4.6
4.3.2 4.3.3 4.3.4 4.3.5 4.3.6 4.3.7 DETECTOI PEAK BROADENING AND PEAK
OVERLAP SUM PEAKS DEAD-TIME CORRECTION LOW ENERGY TAILING ESCAPE PEAKS
SILICON PEAKS R PERFORMANCE BEAM-SPECIMEN-DETECTOR GEOMETRY 4.5.1 4.5.2
4.5.3 SOLID ANGLE TAKE-OFF ANGLE EFFECTS OF TILTING THE SPECIMEN
INTERCEPTION OF BACKSCATTERED ELECTRONS. CONTENTS XIX 73 76 77 78 79 80
80 82 82 84 85 88 5 SPECTRUM PROCESSING AND METHODS FOR QUANTIFICATION
91 5.1 BACKGROUND SUBTRACTION AND ESTIMATION OF NET PEAK INTEGRALS 91 93
95 97 99 100 100 102 102 5.2 QUANTIFICATION 103 5.3 QUANTIFICATION OF
ELEMENTS IN THIN SECTIONS 103 5.3.1 MEASUREMENT OF CONCENTRATIONS AS
ELEMENTAL RATIOS 103 5.3.2 MEASUREMENT OF CONCENTRATION AS MASS PER UNIT
VOLUME 106 5.3.3 CONTINUUM NORMALIZATION 109 5.3.3A THE ENERGY BAND FOR
THE ESTIMATION OF THE CONTINUUM 111 5.3.3B CORRECTIONS TO THE
MEASUREMENT OF THE CONTINUUM . 112 5.3.3C ESTIMATION OF THE G-FACTOR 116
5.3.3D EFFECTS OF CHANGE OF MASS 118 5.3.3E ADVANTAGES AND DISADVANTAGES
OF CONTINUUM NORMALIZATION 119 5.1.1 5.1.2 5.1.3 5.1.4 5.1.5 LINEAR
INTERPOLATION BACKGROUND MODELLING DIGITAL FILTERING FILTERED LEAST
SQUARES (FLS) FITTING DECONVOLUTION OF OVERLAPPING PEAKS 5.1.5A OVERLAP
COEFFICIENTS 5.1.5B DECONVOLUTION USING REFERENCE SPECTRA 5.1.5C
PRACTICAL PROBLEMS ENCOUNTERED IN PEAK DECONVOLUTION QUANTIFICATION
QUANTIFICATION OF ELEMENTS IN THIN SECTIONS XX CONTENTS 5.4
QUANTIFICATION OF ELEMENTS IN SEMI-THICK SECTIONS 120 5.4.1 THE
CONTINUUM NORMALIZATION METHOD 120 5.4.2 PEAK-TO-BACKGROUND RATIOS 120
5.5 QUANTIFICATION OF ELEMENTS IN BULK SPECIMENS 122 5.5.1 DIRECT
COMPARISON OF NET PEAK INTENSITIES 122 5.5.2 PEAK-TO-BACKGROUND RATIOS
123 5.5.3 LONIZATION FUNCTION CURVES 123 6 SPECIMEN PREPARATION 127 6.1
GUIDELINES FOR CHOOSING A METHOD FOR SPECIMEN PREPARATION 128 6.2
SPECIMEN SUPPORTS FOR X-RAY MICROANALYSIS 129 6.3 AIR-DRYING 132 6.4
STANDARD CHEMICAL FIXATION AND EMBEDDING 133 6.4.1 LOSS OF ELEMENTS
DURING STANDARD PROCEDURES 133 6.4.2 ADDITION OF ELEMENTS DURING
STANDARD PROCEDURES 135 6.4.3 EXAMPLES OF X-RAY MICROANALYSIS OF
SPECIMENS PREPARED BY STANDARD METHODS 137 6.4.3A IDENTIFICATION OF
PANICULATE MATERIALS 137 6.4.3B PRECIPITATION METHODS FOR THE
LOCALIZATION OF ELEMENTS 140 6.4.3C VALIDATION OF HISTOCHEMICAL
PROCEDURES 141 6.5 LOW TEMPERATURE METHODS FOR SPECIMEN PREPARATION 142
6.5.1 TREATMENT OF THE SPECIMEN BEFORE CRYOFIXATION 144 6.5.1A THE
EFFECTS OF DISSECTION 144 6.5.1B THE EFFECTS OF DESICCATION 145 6.5.1C
THE EFFECTS OF CRYOPROTECTANTS 146 6.5.2 CRYOFIXATION 148 6.5.2A
CRYOFIXATION OF SPECIMENS IN VIVO 150 6.5.2B CRYOFIXATION OF ISOLATED
FUNCTIONING PREPARATIONS 151 6.5.2C CRYOFIXATION OF ISOLATED OR CULTURED
CELLS 152 6.5.2D CRYOFIXATION OF BULK SPECIMENS 154 6.5.3 STORAGE AFTER
CRYOFIXATION 155 6.5.4 O TREATMENT OF THE SPECIMEN AFTER CRYOFIXATION
157 6.5.5 THIN CRYOSECTIONS FOR EPXMA 158 6.5.5A PREPARATION OF THIN
CRYOSECTIONS 159 6.5.5B FREEZE-DRYING OFCRYOSECTIONS 162 6.5.5C STORAGE
OF FREEZE-DRIED CRYOSECTIONS 167 CONTENTS XXI 6.5.6 METHODS FOR
EMBEDDING CRYOFIXED SPECIMENS 167 6.5.6A FREEZE-DRYING AND
RESIN-EMBEDDING 168 6.5.6B FREEZE-SUBSTITUTION AND RESIN-EMBEDDING 170
6.5.7 PREPARATION OF SEMI-THICK CRYOSECTIONS 172 6.5.8 PREPARATION OF
BULK SPECIMENS 173 6.6 THE PREPARATION OF FLUIDS FOR ANALYSIS 174 6.6.1
DIRECT DEPOSITION OF DROPLETS 174 6.6.2 PREPARATION OF DROPLETS BY
SPRAYING 175 6.6.3 PROBLEMS DURING PREPARATION AND ANALYSIS OF FLUIDS
176 7 QUALITATIVE ANALYSIS OF THE SPECIMEN 185 7.1 PREPARING FOR
ANALYSIS 185 7.1.1 GENERAL CLEANLINESS 185 7.1.2 SELECTING OPERATING
CONDITIONS FOR THE ELECTRON MICROSCOPE 186 7.1.2A GENERAL OPERATING
CONDITIONS 187 7.1.2B CHOICE OF ACCELERATING VOLTAGE 187 7.1.2C CHOICE
OF APERTURES 189 7.L.2D CHOICE OF PROBE CURRENT 190 7.L.2E DURATION OF
ANALYSIS 191 1.1.IF CHOICE OF MAGNIFICATION 191 L.L.2G MINIMIZING
EXTRANEOUS CONTRIBUTION 192 7.L.2H MINIMIZING BEAM DAMAGE 194 7.2 THE
STEPS IN AN ANALYSIS 194 7.2.1 CALIBRATING THE DETECTOR 194 7.2.2
ANALYSIS OF THIN OR SEMI-THICK DRY SECTIONS 195 7.2.3 ANALYSIS OF BULK
SPECIMENS 196 7.3 QUALITATIVE IDENTIFICATION OF PEAKS PRESENT IN THE
SPECTRUM 198 7.4 WHAT MIGHT GO WRONG? 200 7.4.1 NO COUNTS COLLECTED IN
THE SPECTRUM 200 7.4.2 LOW COUNT RATE 200 7.4.3 COUNT RATE TOO HIGH 201
7.4.4 PRESENCE OR ABSENCE OF PEAKS IN THE SPECTRUM 201 8 QUANTITATIVE
ANALYSIS OF THE SPECIMEN 203 8.1 PREPARING FOR QUANTITATIVE ANALYSIS 203
8.1.1 PREPARING PEAK PROFILES FOR FLS FITTING 203 8.1.2 DETERMINATION OF
RELATIVE DETECTOR EFFICIENCY 206 XXII CONTENTS 8.2 STANDT 8.2.1 8.2.2
8.2.3 8.2.4 R OR QUANTITATIVE ANALYSIS MINERAL SALTS STANDARDS BASED ON
PROTEINS STANDARDS BASED ON EMBEDDING RESINS PREPARATION OF STANDARDS
FOR QUANTITATIVE ANALYSIS 8.2.4A GENERAL CONSIDERATIONS IN THE
PREPARATION OF STANDARDS 8.2.4B THIN PROTEIN FILMS 8.2.4C CRYOSECTIONED
STANDARDS 8.2.4D PERIPHERAL STANDARDS 8.2.4E STANDARDS BASED ON EPOXY
RESINS 8.2.4F STANDARDS BASED ON AMINOPLASTIC RESINS 209 209 210 211 212
212 213 214 217 2/7 218 8.2.5 STANDARDS FOR THE ANALYSIS OF SEMI-THICK
AND BULK SPECIMENS 220 8.2.6 ANALYSIS OF THE STANDARD AND DETERMINATION
OF CALIBRATION CONSTANTS 221 8.3 QUANTITATIVE ANALYSIS OF THE SPECIMEN
223 8.3.1 QUANTITATIVE ANALYSIS OF THIN SECTIONS 223 8.3.1A MEASUREMENT
OF CONCENTRATIONS AS ELEMENTAL RATIOS OR AS MASS PER UNIT VOLUME 223
8.3.1B CONTINUUM NORMALIZATION 225 8.3.1C WHAT MIGHT GO WRONG? 227 8.3.2
QUANTITATIVE ANALYSIS OF SEMI-THICK AND BULK SPECIMENS 229 8.3.3
INTERPRETATION OF RESULTS 231 8.3.3A ACCURACY 231 8.3.3B PRECISION 232
8.3.3C MINIMUM DETECTABLE CONCENTRATIONS 233 8.3.3D USE OF THE TERM
RELATIVE MASS FRACTION 235 8.3.3E RESIN-EMBEDDED SPECIMENS 235 8.4
MEASUREMENT OF WATER CONTENT 236 8.4.1 MEASUREMENT OF DRY MASS 237
8.4.1B MEASUREMENT OF WATER CONTENT IN SEMI-THICK, FROZEN-HYDRATED
SECTIONS 239 8.4.2 MEASUREMENT OF WATER CONTENT IN BULK HYDRATED
SPECIMENS 241 8.4.3 CONVERSION TO MILLIMOLAR CONCENTRATIONS 243 CONTENTS
XXIII MAPPING TECHNIQUES 247 9.1 9.2 9.3 DOT MAPPING DIGITAL MAPPING
9.2.1 ADVANTAGES OF DIGITAL MAPPING 9.2.2 QUALITATIVE DIGITAL MAPPING
9.2.3 QUANTITATIVE DIGITAL MAPPING 9.2.3A ADVANTAGES OF QUANTITATIVE
MAPPING 9.2.3B DISADVANTAGES OF QUANTITATIVE MAPPING CONCLUSIONS 247 248
249 250 251 253 255 256 APPENDIX I: SOURCES OF INFORMATION 259 APPENDIX
2: LIST OF MANUFACTURERS AND SUPPLIERS 261 APPENDIX 3: ADDRESSES OF
MANUFACTURERS AND SUPPLIERS 267 SUBJECT INDEX 271
|
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| id | DE-604.BV011511763 |
| illustrated | Illustrated |
| indexdate | 2024-07-09T18:11:01Z |
| institution | BVB |
| isbn | 1855780542 1855780550 |
| language | English |
| oai_aleph_id | oai:aleph.bib-bvb.de:BVB01-007747471 |
| oclc_num | 37465025 |
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| owner_facet | DE-355 DE-BY-UBR DE-20 DE-M49 DE-BY-TUM |
| physical | XXIII, 276 S. Ill., graph. Darst. |
| publishDate | 1997 |
| publishDateSearch | 1997 |
| publishDateSort | 1997 |
| publisher | Portland Press |
| record_format | marc |
| series | Practical methods in electron microscopy |
| series2 | Practical methods in electron microscopy |
| spelling | Warley, Alice Verfasser aut X-ray microanalysis for biologists Alice Warley London [u.a.] Portland Press 1997 XXIII, 276 S. Ill., graph. Darst. txt rdacontent n rdamedia nc rdacarrier Practical methods in electron microscopy 16 Elektronenmicroscopie gtt Röntgen-microanalyse gtt Wetenschappelijke technieken gtt Wissenschaftliches Arbeiten Electron microscopy Technique Mounting of microscope specimens X-ray microanalysis Elektronenmikroskopie (DE-588)4014327-2 gnd rswk-swf Röntgenstrukturanalyse (DE-588)4137203-7 gnd rswk-swf Elektronenstrahlmikroanalyse (DE-588)4151898-6 gnd rswk-swf Elektronenstrahlmikroanalyse (DE-588)4151898-6 s Elektronenmikroskopie (DE-588)4014327-2 s DE-604 Röntgenstrukturanalyse (DE-588)4137203-7 s Practical methods in electron microscopy 16 (DE-604)BV001891054 16 GBV Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=007747471&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis |
| spellingShingle | Warley, Alice X-ray microanalysis for biologists Practical methods in electron microscopy Elektronenmicroscopie gtt Röntgen-microanalyse gtt Wetenschappelijke technieken gtt Wissenschaftliches Arbeiten Electron microscopy Technique Mounting of microscope specimens X-ray microanalysis Elektronenmikroskopie (DE-588)4014327-2 gnd Röntgenstrukturanalyse (DE-588)4137203-7 gnd Elektronenstrahlmikroanalyse (DE-588)4151898-6 gnd |
| subject_GND | (DE-588)4014327-2 (DE-588)4137203-7 (DE-588)4151898-6 |
| title | X-ray microanalysis for biologists |
| title_auth | X-ray microanalysis for biologists |
| title_exact_search | X-ray microanalysis for biologists |
| title_full | X-ray microanalysis for biologists Alice Warley |
| title_fullStr | X-ray microanalysis for biologists Alice Warley |
| title_full_unstemmed | X-ray microanalysis for biologists Alice Warley |
| title_short | X-ray microanalysis for biologists |
| title_sort | x ray microanalysis for biologists |
| topic | Elektronenmicroscopie gtt Röntgen-microanalyse gtt Wetenschappelijke technieken gtt Wissenschaftliches Arbeiten Electron microscopy Technique Mounting of microscope specimens X-ray microanalysis Elektronenmikroskopie (DE-588)4014327-2 gnd Röntgenstrukturanalyse (DE-588)4137203-7 gnd Elektronenstrahlmikroanalyse (DE-588)4151898-6 gnd |
| topic_facet | Elektronenmicroscopie Röntgen-microanalyse Wetenschappelijke technieken Wissenschaftliches Arbeiten Electron microscopy Technique Mounting of microscope specimens X-ray microanalysis Elektronenmikroskopie Röntgenstrukturanalyse Elektronenstrahlmikroanalyse |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=007747471&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| volume_link | (DE-604)BV001891054 |
| work_keys_str_mv | AT warleyalice xraymicroanalysisforbiologists |