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Note for ANALYTICAL INSTRUMENTATION - AI by Abhishek Apoorv

  • ANALYTICAL INSTRUMENTATION - AI
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IN THE NAME OF GOD TO JAMARAN

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CONTENTS ACKNOWLEDGEMENTS (i) GLOSSARY OF TERMS USED (ii) ABSTRACT (iv) DECLARATIONS (vi) CHAPTER ONE GENERAL INTRODUCTION TO PESTICIDE ANALYSIS AND SURVEY OF ANALYTICAL METHODS 1.1 GENERAL INTRODUCTION TO PESTICIDE ANALYSIS 1 1.1.1 Introduction 1 1.1.2 History 1 1.1.3 Current use 3 1.1.4 Mechanism of action 3 1.1.4.1 Effects on enzymes of the esterase type 4 1.1.4.2 Effect on other enzymes 6 1.1.5 Pesticide toxicity 7 1.1.5.1 Pesticide used in this project 7 1.2 SURVEY OF ANALYTICAL METHODS 9 1.2.1 Spectrometric methods 9 1.2.1.1 UV-visible spectrometry 9 1.2.1.2 Infrared spectroscopy 9 1.2.1.3 Chemiluminescence spectroscopy 9 1.2.2 Electrochemical methods 10 1.2.2.1 Polarography 10 1.2.2.2 Enzymatic methods 10 1.2.3 CHROMATOGRAPHIC METHODS 11 1.2.3.1 Thin layer chromatography 11 1.2.3.2 Gas chromatography 11

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1.2.3.2.1 Gas chromatography-mass spectrometry 13 1.2.3.3 High performance liquid chromatography (HPLC) 14 1.2.3.3.1 Combined HPLC-MS 16 17 REFERENCES CHAPTER TWO INTRODUCTION TO ANALYTICAL METHODS 2.1 INTRODUCTIRON 23 2.2 Principles of gas chromatography 23 2.3 Gas liquid chromatography 25 2.4 Theory of gas liquid chromatography 25 2.4.1 Partition coefficient 25 2.4.2 Partition ratio 26 2.4.3 Efficiency of column 27 2.4.4 Resolution 27 2.5 Apparatus 28 2.5.1 Carrier gas 28 2.5.2 Flow controller 28 2.5.3 Injection system 29 2.5.4 The column 29 2.5.4.1 The support 30 2.5.4.1.1 Chromosorb W 31 2.6 Detector 31 2.6.1 Detector performance 31 2.6.2 Minimum detection level (MDL) 32 2.6.3 Electron capture detector 32 2.7 GLC of organophosphorus pesticides 35 2.7.1 Packed column analysis 35 2.7.2 Wide-bore capillary column 36 2.8 GC-MS 39 2.9 Gas chromatogram-mass spectrometer system 39 2.9.1 Inlet system 40

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2.9.2 Interface 40 2.9.1 Direct coupling 40 2.9.3 Ion source 41 2.9.4 Mass analyser 42 2.9.5 Quadrupole mass analyser 42 2.9.6 Detector 43 2.9.7 Vacuum system 43 2.9.10 Data system 44 2.9.10.1 Reconstructed ion chromatogram 44 2.9.10.2 Mass chromatogram 45 2.9.10.3 Library search and identification of mass spectra 45 2.9.11 Selected ion monitoring 46 2.10 Quantitative aspects of environmental analysis 47 2.10.1 Internal standardisation 47 57 REFERENCES CHAPTER THREE DETERMINATION OF ORGANOPHOSPHORUS PESTICIDES IN FRUIT AND VEGETABLE MATERIALS BY GAS LIQUID CHROMATOGRAPHYMASS- SPECTROMETRY 3.1 EXPERIMENTAL 61 3.1.1 Introduction 61 3.1.2 Instrumentation 62 3.1.2.1 Gas liquid chromatography-mass spectrometry 62 3.1.2.1.1 The optimum operating conditions 63 3.1.2.1.2 Adjustment of the electrometer zero 64 3.1.2.1.3 Electron multiplier voltage 64 3.1.2.2 Capillary column 65 3.1.3 Reagents 65 3.1.3.1 Acetone 66 3.1.3.2 Hexane 66

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