Advanced techniques of analytical chemistry. (volume 1)

Advanced Techniques of Analytical Chemistry explains analytical chemistry in an accessible manner for students. The book provides basic and practical knowledge that helps the learner to understand the methods used in conducting experiments. Readers will understand the key concepts of qualitative and quantitative analysis through easy-to-read chapters written for chemistry students. Volume 1 covers the topic of volumetric analysis in detail. Topic-wise chapters introduce the reader to volumetric titrations and then explain the range of titration techniques which include aqueous acid-base titration, non-aqueous titration, redox titration, complexometric titration and some miscellaneous methods like diazotisation titration, Kjeldahl’s method and the oxygen flask combustion method. The combination of basic and advanced methods makes this an ideal textbook for chemistry students at graduate and undergraduate levels as well as an ideal handbook for the laboratory instructor. Cover 1 Title 2 Copyright 3 End User License Agreement 4 Contents 6 Foreword 12 Preface 13 List of Contributors 14 Introduction to Analytical Chemistry 15 Sapna Kumari1,*, Anju Goyal1, Madhukar Garg1 and Harish Verma2 15 INTRODUCTION 15 INTRODUCTION TO VOLUMETRIC TITRATIONS 16 Advantages And Disadvantages Of Volumetric Analysis 16 WHAT IS TITRATION? 17 Simple Titrations 18 Types of Volumetric Titrations 19 Acid-Base Titrations 19 Redox Titrations 21 Precipitation Titration 22 Complexometric Titration 22 Steps Involved in Titrimetric Analysis 25 Primary Standard Solution 26 Methods of Expressing Concentrations in Volumetric Analysis 27 Calculation of Equivalent Weights 27 Equivalent Weight in Neutralization Reactions 28 Equivalent Weight in Oxidation -reduction Reactions 28 Equivalent Weight of Complex Formation and Precipitation Reactions 28 CONSENT FOR PUBLICATION 29 CONFLICT OF INTEREST 29 ACKNOWLEDGEMENTS 29 REFERENCES 29 Recent Advances and Future Perspectives in Volumetric Analysis 30 Nidhi Garg1,*, Anju Goyal1 and Payal Das1 30 INTRODUCTION 31 TYPES OF VOLUMETRIC TITRATIONS 32 Acid-Base Titration 32 Redox Titrations 33 Permanganate Titrations 33 Dichromate Titrations 33 Iodometric and Iodometric Titrations 33 Precipitation Titrations 34 Complexometric Titrations 34 PROCEDURE FOR VOLUMETRIC ANALYSIS 34 BASIC PRINCIPLES OF VOLUMETRIC ANALYSIS 35 IMPORTANCE OF VOLUMETRIC ANALYSIS 36 APPLICATIONS AND FUTURE PERSPECTIVES OF VOLUMETRIC ANALYSIS 38 CONCLUSION 39 CONSENT FOR PUBLICATION 39 CONFLICT OF INTEREST 39 ACKNOWLEDGEMENTS 39 REFERENCES 40 Aqueous Acid-Base Titrations 41 Astha Sharma1,*, Monika Gupta2 and Anju Goyal3 41 INTRODUCTION 41 THEORIES OF ACIDS AND BASES 42 Arrhenius Concept 42 Bronsted-Lowry 43 Lewis Acids 43 Law of Mass Action 43 Ion Product Constant of Water 44 COMMON ION EFFECT 45 ACID BASE EQUILIBRIUM 45 INDICATOR 47 Neutralisation Indicator 47 Ostwald Theory 47 Mixed Indicators 49 Universal Indicator 50 NEUTRALISATION CURVES 50 Titration of a Strong Acid with a Strong Base 51 Titration of a Weak Acid with a Strong Base 52 Titration of a Strong Acid with a Weak Base 54 Titration of a Weak Base with a Weak Acid 55 CONSENT FOR PUBLICATION 56 CONFLICT OF INTEREST 56 ACKNOWLEDGEMENTS 56 REFERENCES 56 Non-Aqueous Titrations 59 Sunaina Aggarwal1,*, Upasna Kaushik1 and Shivani Sharma1 59 INTRODUCTION 59 SOLVENT SYSTEM FOR NON-AQUEOUS TITRATIONS 60 FACTORS AFFECTING SELECTION OF SOLVENT 61 SOLVENTS EMPLOYED IN NON-AQUEOUS TITRATION 62 Glacial Acetic Acid 62 Acetonitrile 62 Alcohols 62 Dioxane 63 Dimethylformamide 63 INDICATORS IN NON-AQUEOUS TITRATIONS 63 Crystal Violet 63 1-Naphtholbenzein 63 Nile Blue A 63 Oracet Blue B 63 Quinaldine Red 63 Thymol Blue 63 Azovoilet 64 ALKALIMETRY 64 ESTIMATION OF ACIDS 64 ASSAY OF ETHOSUXIMIDE 65 ASSAY OF CHLORTHALIDONE 66 ACIDIMETRY 67 ESTIMATION OF AMINES AND AMINE SALTS OF ORGANIC ACIDS 68 ASSAY OF METHYLDOPA 68 ASSAY OF NITRAZEPAM 69 ESTIMATION OF HALOGEN ACID SALTS OF BASES 69 Assay of Amitriptyline Hydrochloride 69 ADVANTAGES OF NON-AQUEOUS TITRATIONS 70 LIMITATIONS OF NON-AQUEOUS TITRATIONS 70 CONCLUSION 70 CONSENT FOR PUBLICATION 70 CONFLICT OF INTEREST 71 ACKNOWLEDGEMENTS 71 REFERENCES 71 Redox Titrations 72 Sapna Kumari1,*, Anju Goyal1 and Madhukar Garg1 72 INTRODUCTION 72 HISTORY AND DEVELOPMENT OF REDOX TITRATION METHOD 72 Principle and Theory 73 OXIDIZING AND REDUCING AGENTS 74 Oxidizing Agents 74 KMnO4 (Potassium Permanganate) 75 K2Cr2O7 (Potassium Dichromate) 75 Iodine Solution 75 Potassium Iodate 75 Bromate-bromide Mixture 76 REDUCING AGENTS 76 EQUIVALENT WEIGHT OF OXIDIZING AND REDUCING AGENTS 77 OXIDATION NUMBER (O.N.) 77 Rules of Assigning Oxidation Number 78 PRIMARY STANDARD 79 FACTORS AFFECTING REDOX TITRATIONS 79 Redox Indicators 79 Types of Redox Indicators 80 TYPES OF REDOX TITRATIONS 82 1. Based on the Titrant Used 82 Permanganate Titration 82 Dichromate Titration 82 Iodine Titration 82 Based on the Method 83 Direct Titration 83 Back Titration 83 REDOX TITRATION CURVE 83 Calculating Titration Curve 84 Determining End Point 88 Use of Visual Indicator 88 Use of Potentiometric Method 88 Applications of the Redox Titrations 90 Use of Redox Titrimetry in the Inorganic Analysis 90 Use of Redox Titrations in Organic Analysis 92 Quantification of Lithium 92 Conclusion 94 CONSENT FOR PUBLICATION 94 CONFLICT OF INTEREST 94 ACKNOWLEDGEMENTS 94 REFERENCES 94 Complexometric Titrations 96 Anju Goyal1, Ramninder Kaur1,*, Sandeep Arora1 and Komalpreet Kaur2 96 INTRODUCTION 96 COMPLEXATION 96 CHELATE 97 LIGANDS 97 Classification of Ligands 97 Monodentate Ligand 97 Bidentate and Multidentate Ligands 98 CO-ORDINATE COVALENT BONDS OR DATIVE BONDS 99 COVALENT BOND 99 WERNER’S COORDINATE NUMBER (WCN) 99 STABILITY CONSTANT 100 STABILITY 100 TYPES OF COMPLEXOMETRIC TITRATIONS 101 TYPES OF TITRATIONS: 102 MASKING AND DEMASKING AGENTS 103 Masking Agents 103 Need 103 Examples of Masking Agents 104 Demasking Agents 104 METAL ION INDICATORS USED IN COMPLEXOMETRIC TITRATIONS 104 COMMON EXAMPLES 104 Mordant Black-II 104 MUREXIDE (AMMONIUM PURPURATE) 105 XYLENOL ORANGE (LEMON TO YELLOW) 106 SOLOCHROME DARK BLUE OR MORDANT BLACK-17 OR CALCON 106 ALIZARIN FLUORINE COMPLEX OR ALIZARINE FLUORINE BLUE OR ALIZARINE COMPLEX ONE 106 ASSAY OF MAGNESIUM SULPHATE 107 PREPARATION AND STANDARDIZATION OF 0.05M EDTA SOLUTION 107 STANDARDISATION 107 ASSAY OF ALUMINIUM HYDROXIDE GEL 108 ASSAY OF CALCIUM GLUCONATE 109 CONCLUSION 109 CONSENT FOR PUBLICATION 110 CONFLICT OF INTEREST 110 ACKNOWLEDGEMENTS 110 REFERENCES 110 Diazotization Method 111 Kamya Goyal1,2,*, Navdeep Singh1, Shammy Jindal1, Rajwinder Kaur2, Anju Goyal2 and Rajendra Awasthi3 111 INTRODUCTION 111 Principle 112 Theory 113 End Point Detection 114 Preparation and Standardization of the Sodium Nitrite Solution 114 Factors Affecting the Diazotization 114 DIAZOTIZATION TITRATIONS METHODS 115 1. Direct Method 115 2. Indirect Method 115 3. Other Method 115 Procedure 115 Applications 116 CONCLUSION 116 CONSENT FOR PUBLICATION 116 CONFLICT OF INTEREST 116 ACKNOWLEDGEMENTS 117 REFERENCES 117 Kjeldahl Method 119 Kamya Goyal1,2,*, Navdeep Singh1, Shammy Jindal1, Rajwinder Kaur2, Anju Goyal2 and Rajendra Awasthi3 119 INTRODUCTION 120 Principles 120 Digestion 120 Neutralization 121 Titration 121 Procedure 122 Step One: Digestion of the Sample 122 Digestion is Accomplished by 122 Step Two: Distillation 123 Step Three: Titration 123 Applications 124 Recent Developments 124 CONCLUSION 124 CONSENT FOR PUBLICATION 125 CONFLICT OF INTEREST 125 ACKNOWLEDGEMENTS 125 REFERENCES 125 Oxygen Flask Combustion Method 127 Kamya Goyal1,2,*, Navdeep Singh1, Shammy Jindal1, Rajwinder Kaur2, Anju Goyal2 and Rajendra Awasthi3 127 INTRODUCTION 128 Apparatus 128 Preparation of Test Solution and Blank Solution 129 Preparation of Sample 129 Method of Combustion 129 Procedure of Determination 129 Chlorine and Bromine 129 2. Iodine 130 3. Fluorine 130 4. Sulfur 131 Applications 131 CONCLUSION 132 CONSENT FOR PUBLICATION 132 CONFLICT OF INTEREST 132 ACKNOWLEDGEMENTS 132 REFERENCES 132 Precipitation Titration 134 Kamya Goyal1,2,*, Navdeep Singh1, Shammy Jindal1, Rajwinder Kaur2, Anju Goyal2 and Rajendra Awasthi3 134 INTRODUCTION 135 Precipitation Titration Example 135 PRINCIPLE OF PRECIPITATION 135 FACTORS INFLUENCING THE SOLUBILITY OF PRECIPITATE 136 a) Effect of Temperature 136 b) Effect of Solvent 136 c) Effect of Corrosive 136 d) Formation of Complex Particles 136 METHODS FOR PRECIPITATION TITRATION 137 Mohr's Method 137 Precautions 137 Limitations 137 Preparation of 0.1 M Silver Nitrate 138 Volhard Method: Jacob Volhard (1834-1910) 138 Fajan's Strategy: Karl Kazimierz Fajan (1887-1975) 139 LIMITS OF PRECIPITATION TITRATION 139 HOW TO CONQUER THE ISSUES OF PRECIPITATION TITRATION 139 APPLICATIONS 140 CONCLUSION 140 CONSENT FOR PUBLICATION 141 CONFLICT OF INTEREST 141 ACKNOWLEDGEMENTS 141 REFERENCES 141 Subject Index 144 Advanced Techniques of Analytical Chemistry explains analytical chemistry in an accessible manner for students. The book provides basic and practical knowledge that helps the learner to understand the methods used in conducting experiments. Readers will understand the key concepts of qualitative and quantitative analysis through easy-to-read chapters written for chemistry students.Volume 1 covers the topic of volumetric analysis in detail. Topic-wise chapters introduce the reader to volumetric titrations and then explain the range of titration techniques which include aqueous acid-base titration, non-aqueous titration, redox titration, complexometric titration and some miscellaneous methods like diazotisation titration, Kjeldahl s method and the oxygen flask combustion method.The combination of basic and advanced methods makes this an ideal textbook for chemistry students at graduate and undergraduate levels as well as an ideal handbook for the laboratory instructor.