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Analytical studies of oxidants for catalytic oxidation of organic compounds

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C O N T E N T S

Page 1 2 3-9 10-73

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DECLARATION ACKNOWLEDGEMENTS ABSTRACT

PART 1 A NOVEL METHOD FOR DETERMINATION OF ACTIVITY OF A SAMPLE-ADDITIVE REAGENT

IN ORGANIC ELEMENTAL ANALYSIS 1.1 INTRODUCTION

1.1.1 Activity of combustion catalysts

1.1.2 Activity of oxidants as sample-additive reagents

1.1.3

Need for development 1.1.4 Basic requirements

1.1.5 Mechanism of catalysis by solid catalysts

1.1.6 Role of transition metal oxides as oxidants.

1.2 EXPERIMENTAL

1.2.1 Apparatus and Equipment 1.2.2 Materials

1.2.3 Procedure

1.2.4 Condensed volatile products 1.2.5 Nature of the residual material 1.2.6 Mean particle size determination 1.2.7 Surface area determination

1.2.8 XPS of the sample-additive reagents

1.3

RESULTS AND DISCUSSION

1.3.1

Activity of the sample-additive reagents 1.3.2 Dependance of activity

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Page 1.3.3 D.T.A. and T.G.

1.3.4 Mean particle size data 1.3.5 Surface area data

1.3.6 ESCA: X-ray photoelectron spectroscopy of the sample-additive reagents

1.4 CONCLUSION

PART 2 KINETIC STUDIES OF COMBUSTION OF PHENANTHRENE WITH VARIOUS SAMPLE- ADDITIVE REAGENTS

2.1 INTRODUCTION

2.1.1 Methods to study the mechanism of catalytic oxidation

2.1.2 Study of combustion kinetics on microscale

2.1.3 Limitations in the measurements 2.1.4 Present Work

2.1.5 Kinetic study 2.2 EXPERIMENTAL

2.2.1 Apparatus 2.2.2 Materials 2.2.3 Procedure

2.3 RESULTS AND DISCUSSION 2.3.1 Stages of combustion 2.3.2 Data of combustions

2.3.3 Relation of activity with the combustion data

2.4 CONCLUSION

PART 3 CATALYTIC VAPOUR-PHASE OXIDATION OF SOME ALIPHATIC ALCOHOLS ON VANADIUM PENTOXIDE IN A SEMI-MICROREACTOR 3.1 INTRODUCTION

3.1.1 General methods for the preparation of aldehydes

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99 100-146 100

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Page 3.1.2 Liquid-phase oxidation of alcohols

3.1.3 Catalytic vapour-phase oxidation of alcohols

3.2 EXPERIMENTAL

3.2.1 Apparatus and Equipment 3.2.2 Materials

3.2.3 Procedure

3.3 RESULTS AND DISCUSSION

3.3.1 Recoveries of the total oxidation product

3.3.2 Conversion of alcohols to aldehydes 3.3.3 Impurities

3.3.4 Unidentified products

3.3.5 Activity of the regenerated catalyst 3.4 CONCLUSION

REFERENCES

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