Analytical Chemistry of Zirconium and Hafnium (eBook)

Front Cover 1
Analytical Chemistry of Zirconium and Hafnium 4
Copyright Page 5
Table of Contents 8
Dedication 6
PREFACE 10
PHYSICAL PROPERTIES OF ZIRCONIUM AND HAFNIUM 12
CHAPTER 1. AQUEOUS SOLUTIONS OF ZIRCONIUM AND HAFNIUM 16
EFFECT OF CHLORIDE, NITRATE, AND PERCHLORATE 17
HYDROLYTIC POLYMERIZATION AND THE HYDROUS OXIDES 18
EFFECT OF SULPHATE 20
ZIRCONIUM CHELATES 21
REFERENCES 25
CHAPTER 2. DISSOLUTION OF ORES AND ALLOYS 27
BORAX FUSION 27
SODIUM PEROXIDE FUSION 28
REFERENCES 28
CHAPTER 3. METHODS OF DETECTION AND IDENTIFICATION 29
SPECTROGRAPHIC METHOD 29
CHEMICAL METHODS 29
REFERENCES 32
CHAPTER 4. GRAVIMETRIC DETERMINATIONS 33
INORGANIC PRECIPITANTS 33
FLUOZIRCONATE 33
ORGANIC PRECIPITANTS 37
DETERMINATION OF ZmCONIUM-HAFNIUM RATIOS 54
OTHER SEPARATIONS 55
REFERENCES 56
CHAPTER 5. TITRIMETRIC METHODS 60
NEUTRALIZATION REACTIONS 60
PRECIPITATION REACTIONS 60
OXIDATION OR REDUCTION OF THE PRECIPITANT MOLECULE 61
COMPLEXOMETRIC REACTIONS 62
BACK-TITRATION PROCEDURES 69
BACK-TITRATION WITH IRON (III) AND SALICYLIC ACID AS INDICATOR 69
REFERENCES 74
CHAPTER 6. ELECTROMETRIC METHODS 76
POLAROGRAPHY 76
SINE-WAVE POLAROGRAPHY DETERMINATION OF ZIRCONIUM 79
AMPEROMETRIC TITRATIONS 83
EDTA 83
REFERENCES 88
CHAPTER 7. ABSORPTIOMETRIC METHODS 89
ALIZARIN SULFONATE 89
PHENYLFLUORONE AND ITS DERIVATIVES 92
XYLENOL ORANGE 93
PYROCATECHOL VIOLET 96
l-(2-PYRIDYLAZO)-2-NAPHTHOL 101
CHLORANILIC ACID 104
BROMANILIC ACID 105
REFERENCES 112
CHAPTER 8. SEPARATIONS USING ION-EXCHANGE 115
ION-EXCHANGE SEPARATION AND DETERMINATION OF TRACE AMOUNTS OF ZIRCONIUM, HAFNIUM, CERIUM, AND THORIUM IN SILICATE ROCKS 119
ANION EXCHANGE SEPARATION OF ZIRCONIUM, TITANIUM, NIOBIUM, TANTALUM, TUNGSTEN, AND MOLYBDENUM 120
SEPARATION OF TITANIUM, ZIRCONIUM, AND THORIUM BY CATION EXCHANGE 122
SEPARATION OF ZIRCONIUM FROM TITANIUM, IRON, ALUMINUM, AND OTHER CATIONS 123
ANION EXCHANGE SEPARATION OF THORIUM, ZIRCONIUM, HAFNIUM, AND MOLYBDENUM IN SULPHURIC ACID MEDIA 124
REFERENCES 141
CHAPTER 9. SEPARATIONS USING SOLVENT EXTRACTION 143
EXTRACTION WITH ß-DIKETONES 143
EXTRACTION WITH AMINES 151
EXTRACTION USING 8-HYDROXYQUINOLINE 152
EXTRACTION WITH TRI-N-BUTYL PHOSPHATE 152
EXTRACTION WITH 
155 
EXTRACTION WITH TRI-N-OCTYL PHOSPHINE OXIDE 156
EXTRACTIONS USING CUPFERRON 161
EXTRACTION OF ZIRCONIUM ALIZARIN SULFONATE COMPLEX WITH BUTANOL 163
EXTRACTION WITH MESITYL OXIDE 164
EXTRACTION WITH FATTY ACIDS 165
REFERENCES 169
CHAPTER 10. SEPARATION OF HAFNIUM FROM ZIRCONIUM 172
1. FRACTIONAL CRYSTALLIZATION AND PRECIPITATION 173
2. DISTILLATION 176
3. ELECTROLYSIS 181
4. ADSORPTION SEPARATIONS 181
5. ION-EXCHANGE SEPARATIONS 184
6. LIQUID-LIQUID EXTRACTION 194
COMPARISON OF THE SEPARATION PROCESSES 204
HAFNIUM SEPARATION AND ITS COMPATIBILITY WITH THE TOTAL METALLURGICAL SCHEME 206
REFERENCES 208
CHAPTER 11. SPECTROGRAPHIC ANALYSES 213
POROUS CUP TECHNIQUE 219
PELLET TECHNIQUE USING CONDENSER DISCHARGE 219
ANALYSIS OF ZIRCONIUM METAL AND ALLOYS 227
REFERENCES 238
CHAPTER 12. X-RAY ANALYSES 241
X-RAY EMISSION 241
X-RAY FLUORESCENCE 242
REFERENCES 261
CHAPTER 13. NEUTRON ACTIVATION ANALYSIS AND SEPARATION OF TRACERS 262
DETERMINATION OF ZIRCONIUM IN ZIRCONIUM–HAFNIUM MIXTURES 262
DETERMINATION OF LOW CONCENTRATIONS OF HAFNIUM IN ZIRCONIUM METAL AND ALLOYS 267
REACTOR THERMAL NEUTRONS FOR THE ACTIVATION ANALYSIS OF ZIRCONIUM AND HAFNIUM 271
DETERMINATION OF HAFNIUM IN ZIRCONIUM OXIDE USING LITHIUM-DRIFTED GERMANIUM SOLID-STATE DETECTORS 272
DETERMINATION OF ZIRCONIUM AND HAFNIUM IN STONE METEORITES 273
PHOTONUCLEAR ACTIVATION ANALYSIS 278
DETERMINATION OF Zr95 IN FISSION PRODUCT MIXTURES 278
RAPID RADIOCHEMICAL SEPARATION OF ZIRCONIUM FROM NIOBIUM WITH SALICYLHYDROXAMIC ACID 279
SEPARATION OF Zy95 FROM Nb95 WITH BUTYL PHOSPHORIC ACIDS 280
SEPARATION OF Zr95 FROM Nb95 WITH TRI-N-BUTYL PHOSPHINE OXIDE (TBPO) 281
SEPARATION OF Nb95 FROM Zr95 USING UNFIRED VYCOR GLASS 282
FAST SEPARATION OF Zr95-Nb95 BY THIN LAYER CHROMATOGRAPHY 282
SEPARATION OF Zr95 BY THENOLYTRIFLUOROACETONE (TTA) EXTRACTION 283
SEPARATION OF Nb95 FROM Zr95 IN COMMERCIAL RADIOISOTOPE SOLUTIONS 284
REFERENCES 285
INDEX 288
OTHER TITLES IN THE SERIES IN ANALYTICAL CHEMISTRY 296