Thermal methods of analysis:
Gespeichert in:
| Beteilige Person: | |
|---|---|
| Format: | Buch |
| Sprache: | Englisch |
| Veröffentlicht: |
New York [u.a.]
Wiley
1974
|
| Ausgabe: | 2. ed. |
| Schriftenreihe: | Chemical analysis
19 |
| Schlagwörter: | |
| Links: | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=001498529&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| Umfang: | XVII, 505 S. Illustrationen, Diagramme 24 cm |
Internformat
MARC
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| 100 | 1 | |a Wendlandt, Wesley William |e Verfasser |4 aut | |
| 245 | 1 | 0 | |a Thermal methods of analysis |c Wesley Wm. Wendtlandt |
| 250 | |a 2. ed. | ||
| 264 | 1 | |a New York [u.a.] |b Wiley |c 1974 | |
| 300 | |a XVII, 505 S. |b Illustrationen, Diagramme |c 24 cm | ||
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Datensatz im Suchindex
| _version_ | 1819310989621854208 |
|---|---|
| adam_text | CONTENTS
CHAPTER I. GENERAL INTRODUCTION
CHAPTER n. THERMOGRAVIMETRY 6
A. Introduction 6
B. Some Factors Affecting Thermogravimetric
Curves 8
1. Instrumental (Thermobalance) Factors 9
a. Heating Rate 9
b. Recording or Chart Speed 13
c. Effect of Furnace Atmosphere 14
d. Sample Holder 19
e. Conditions for Optimum Sensitivity 24
2. Sample Characteristics 25
a. Sample Mass 25
b. Sample Particle Size 27
c. Miscellaneous Sample Effects 28
C. Sources of Error in Thermogravimetry 29
1. Sample-Container Buoyancy 29
2. Furnace Convection Currents and Turbulence 31
3. Temperature Measurement 33
4. Other Errors 36
D. Self-Generated Atmosphere Thermogravimetry 37
E. Derivative Thermogravimetry (DTG) 42
F. Reaction Kinetics 45
1. Nonisothermal Methods 45
a. Newkirk Method 47
b. Freeman and Carroll Method 47
c. Horowitz and Metzger Method 48
d. Coats and Redfern Method 48
e. Doyle Method 48
f. Ingraham and Marier Method 50
g. Vachuska and Voboril Method 51
h. Miscellaneous Methods 51
2. Comparison of Different Methods 53
3. Mechanism of Reaction from Nonisothermal
Kinetics 56
XI
Xii CONTENTS
CHAPTER ffl. THERMOBALANCES 62
A. Introduction 62
1. Recording Balances 64
a. Cahn Balances 67
2. Sample Holders 67
3. Furnaces and Furnace Temperature Pro-
grammers 72
4. Temperature Detection and Recording Systems 74
B. Thermobalances 79
1. Introduction 79
2. Chevenard Thermobalance 82
3. Helical-Spring Thermobalances 84
4. DuPont Thermobalance 85
5. Derivatograph 87
6. Mettler Thermoanalyzer 89
7. Miscellaneous Thermobalances 91
8. Quartz Balances 91
9. Automated Thermobalances 93
CHAPTER IV. APPLICATIONS OF THERMOGRAVIMETRY 99
A. Introduction 99
B. Applications to Analytical Chemistry 100
1. Automatic Gravimetric Analysis 101
C. Analytical Determinations Using TG 104
1. Drying of Analytical Precipitates 104
2. Drying and Decomposition of Sodium Car-
bonate 105
3. Ignition Temperature of Aluminum Oxide 107
4. Complex Mixtures of Hydrates 108
5. Analysis of Clays and Soils 109
6. Analysis of Calcium Silicate Hydrates for Free
Lime and Carbonate 111
7. Determination of Magnesium, Calcium, Stron-
tium, and Barium 113
8. Potassium Hydrogen Phthalate 116
9. Some Amine Molybdophosphates 117
D. Polymers 119
1. Introduction 119
2. Relative Thermal Stability 122
3. Additive Content 123
4. Comparison of Polymer Blends and Copoly-
mers 124
CONTENTS Xiii
5. Miscellaneous 125
E. Miscellaneous Inorganic Applications 125
F. Applications to Vapor Pressure and Sublimation
Determinations 127
G. Miscellaneous Applications 129
CHAPTER V. DIFFERENTIAL THERMAL ANALYSIS
AND DIFFERENTIAL SCANNING
CALORIMETRY 134
A. Differential Thermal Analysis 134
1. Introduction 134
2. Historical Aspects 137
3. Theoretical Aspects 139
4. Factors Affecting the DTA Curve 146
a. Heating Rate 148
b. Furnace Atmosphere 150
c. Sample Holders 157
d. Thermocouple Location 163
e. Thermocouples 169
5. Sample Characteristics 172
a. Sample Mass 172
b. Sample Particle Size and Packing 172
c. Effect of Diluent 175
6. Critique of Operational Parameters 176
B. Quantitative Differential Thermal Analysis 178
1. Introduction 178
2. Calibration 179
3. Calibration Standards 183
4. Calculation of AH 183
5. Precision and Accuracy of A//Measurements 183
C. Reaction Kinetics 187
D. Differential Scanning Calorimetry 193
1. Introduction 193
2. Theory 194
CHAPTER VI. DIFFERENTIAL THERMAL ANALYSIS
AND DIFFERENTIAL SCANNING
CALORIMETRY INSTRUMENTATION 202
A. Differential Thermal Analysis 202
1. Introduction 202
2. Sample Holders 202
iv CONTENTS
3. Ar and T Detection Systems 208
4. Furnaces and Furnace Temperature Pro-
grammers 212
5. Low-Level Voltage Amplifier and Recording
Systems 219
6. DTA Instruments 219
a. Introduction 219
b. Sealed-tube DTA Techniques 220
c. High Pressure DTA Instruments 223
d. High Temperature DTA Instruments 225
e. Micro DTA Instruments 229
f. Automation of DTA Instrumentation 229
g. Miscellaneous DTA Instruments 233
B. Differential Scanning Calorimetry 241
CHAPTER VH. APPLICATIONS OF DIFFERENTIAL
THERMAL ANALYSIS AND
DIFFERENTIAL SCANNING
CALORIMETRY 251
A. Introduction 251
B. DTA Card Indexes 255
C. Organic Compounds 256
D. Inorganic Compounds 271
E. Clays and Minerals 283
F. Biological Materials 289
G. Polymers 294
H. Miscellaneous Applications 308
CHAPTER Vffl. EVOLVED GAS DETECTION AND EVOLVED
GAS ANALYSIS 319
A. Introduction 319
B. Evolved Gas Detection 319
C. Evolved Gas Analysis 331
1. Gas Chromatography 332
2. Titrimetric Methods 335
3. Infrared Spectroscopy 338
4. Thermoparticulate Analysis (TPA) 339
5. Thin Layer Chromatography (TLC) 339
6. Flame Ionization Detection 343
7. Mass Spectrometry 345
a. EGA-MS 347
CONTENTS XV
b. Simultaneous EGD-MS 347
c. Simultaneous DTA-EGD-MS 350
d. Simultaneous TG-EGD-MS or TG-
DTA-EGD-MS 350
8. Thermobarogravimetry (TBG) 352
CHAPTER IX. SPECTROSCOPIC, PHOTOMETRIC, AND
OPTICAL THERMAL TECHNIQUES 360
A. High-Temperature Reflectance Spectroscopy and
Dynamic Reflectance Spectroscopy 360
1. Introduction 360
2. High-Temperature Reflectance Spectroscopy 362
3. Instrumentation 364
4. Applications of HTRS and DRS to Inorganic
Compounds 368
a. The Octahedral —*¦ Tetrahedral Transition
in Co(py)2Cl2 368
b. [Cu(en)(H2O)2]SO4 370
c. CuSO4-5H2O 373
d. CoCl2-6H2O 374
e. Ni(py)4Cl2 377
f. Thermochromism of Ag2[HgI4] 379
g. Thermal Matrix Reactions 381
B. Photometric Methods 382
C. High-Temperature Infrared Spectroscopy 385
D. Thermal Optical Microscopy Techniques 386
1. Fusion Microscopy 386
2. Depolarized Light Intensity and Photometric
Thermal Microscopy 388
CHAPTER X. CRYOSCOPIC PURITY DETERMINATION 397
A. Introduction 397
B. Theory 398
C. Experimental Techniques 405
D. Errors, Limitations, and Other Factors Affecting
Results 409
1. Limitations of Dynamic Method 410
a. Solid-Liquid Transitions 410
b. Solid-Phase Transitions 411
c. Rates of Diffusion 411
d. Effect of Stirring 411
xvi CONTENTS
e. Rate of Heat Transport 411
f. Temperature Differences During Melting 412
g. Influence of Contact Between Layers 412
2. Limitations of the Static Method 412
a. Uncertainty of Impurity Values 412
b. Evidence of Solid-Solution Formation 412
c. Application of Solid-Solution Theory 413
3. Comparison of Results Obtained by the Static
and Dynamic Methods 413
4. Recommendations 413
E. Applications to Impurity Determinations and
Other Problems 415
F. Purity Determinations by Differential Scanning
Calorimetry 421
1. Introduction 421
2. Theory 421
3. Instrumental Considerations 422
4. Applications 425
5. Assessment 426
CHAPTER XI. MISCELLANEOUS THERMAL ANALYSIS
TECHNIQUES 428
A. Introduction 428
B. Dilatometry (Thermomechanical Analysis) 428
1. Introduction 428
2. Instrumentation 429
3. Applications 433
C. Electrical Conductivity 437
D. Emanation Thermal Analysis (ETA) 445
E. Thermoluminescence 449
F. Thermomagnetic Analysis 459
G. Torsional Braid Analysis 461
H. Oxyluminescence 465
CHAPTER XH. APPLICATION OF DIGITAL AND ANALOG
COMPUTERS TO THERMAL ANALYSIS 469
A. Introduction 469
B. Thermogravimetry (TG) 469
C. Differential Thermal Analysis (DTA) and Differ-
ential Scanning Calorimetry (DSC) 479
D. Miscellaneous Thermal Techniques 483
CONTENTS xvii
CHAPTER XIII. THERMAL ANALYSIS NOMENCLATURE 488
A. Introduction 488
B. General Recommendations 489
C. Terminology 490
D. Definitions and Conventions 490
1. General 490
2. Methods Associated with Weight Changes 490
a. Static 490
b. Dynamic 492
E. Methods Associated with Energy Changes 492
F. Methods Associated with Evolved Volatiles 493
G. Methods Associated with Dimensional Change 493
H. Multiple Techniques 493
I. DTA 493
J. TG 494
K. DTA and TG 494
L. DTA 494
M. TG 495
INDEX 499
|
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| dewey-tens | 540 - Chemistry and allied sciences |
| discipline | Chemie / Pharmazie |
| edition | 2. ed. |
| format | Book |
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| genre_facet | Einführung |
| id | DE-604.BV002280474 |
| illustrated | Illustrated |
| indexdate | 2024-12-20T07:48:48Z |
| institution | BVB |
| language | English |
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| publishDate | 1974 |
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| publisher | Wiley |
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| series | Chemical analysis |
| series2 | Chemical analysis |
| spellingShingle | Wendlandt, Wesley William Thermal methods of analysis Chemical analysis Chemistry, Analytical Thermal analysis Analytische Chemie (DE-588)4129906-1 gnd Thermoanalyse (DE-588)4135675-5 gnd Thermochemie (DE-588)4078260-8 gnd |
| subject_GND | (DE-588)4129906-1 (DE-588)4135675-5 (DE-588)4078260-8 (DE-588)4151278-9 |
| title | Thermal methods of analysis |
| title_auth | Thermal methods of analysis |
| title_exact_search | Thermal methods of analysis |
| title_full | Thermal methods of analysis Wesley Wm. Wendtlandt |
| title_fullStr | Thermal methods of analysis Wesley Wm. Wendtlandt |
| title_full_unstemmed | Thermal methods of analysis Wesley Wm. Wendtlandt |
| title_short | Thermal methods of analysis |
| title_sort | thermal methods of analysis |
| topic | Chemistry, Analytical Thermal analysis Analytische Chemie (DE-588)4129906-1 gnd Thermoanalyse (DE-588)4135675-5 gnd Thermochemie (DE-588)4078260-8 gnd |
| topic_facet | Chemistry, Analytical Thermal analysis Analytische Chemie Thermoanalyse Thermochemie Einführung |
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