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Beschreibung

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.

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Seitenzahl: 187

Veröffentlichungsjahr: 2022

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Table of Contents
BENTHAM SCIENCE PUBLISHERS LTD.
End User License Agreement (for non-institutional, personal use)
Usage Rules:
Disclaimer:
Limitation of Liability:
General:
FOREWORD
Preface
List of Contributors
Introduction to Analytical Chemistry
Abstract
INTRODUCTION
INTRODUCTION TO VOLUMETRIC TITRATIONS
Advantages And Disadvantages Of Volumetric Analysis
What is Titration?
Simple Titrations
Types of Volumetric Titrations
Acid-Base Titrations
Acid-Base Indicators
Redox Titrations
Oxidation-Reduction Indicators
Precipitation Titration
Complexometric Titration
Back Titration
Double Titrations
Steps Involved in Titrimetric Analysis
Primary Standard Solution
Methods of Expressing Concentrations in Volumetric Analysis
Calculation of Equivalent Weights
Equivalent Weight in Neutralization Reactions
Equivalent Weight in Oxidation -reduction Reactions
Equivalent Weight of Complex Formation and Precipitation Reactions
CONSENT FOR PUBLICATION
CONFLICT OF INTEREST
ACKNOWLEDGEMENTS
REFERENCES
Recent Advances and Future Perspectives in Volumetric Analysis
Abstract
Introduction
Types of Volumetric Titrations
Acid-Base Titration
Redox Titrations
Permanganate Titrations
Dichromate Titrations
Iodometric and Iodometric Titrations
Precipitation Titrations
Complexometric Titrations
Procedure for Volumetric Analysis
Basic principles of volumetric analysis
Importance of volumetric analysis
Applications and future perspectives of Volumetric Analysis
Conclusion
CONSENT FOR PUBLICATION
CONFLICT OF INTEREST
ACKNOWLEDGEMENTS
References
Aqueous Acid-Base Titrations
Abstract
INTRODUCTION
THEORIES OF ACIDS AND BASES
Arrhenius Concept
Bronsted-Lowry
Lewis Acids
Law of Mass Action
Ion Product Constant of Water
COMMON ION EFFECT
ACID BASE EQUILIBRIUM
INDICATOR
Neutralisation Indicator
Ostwald Theory
Mixed Indicators
Universal Indicator
NEUTRALISATION CURVES
Titration of a Strong Acid with a Strong Base
Titration of a Weak Acid with a Strong Base
Titration of a Strong Acid with a Weak Base
Titration of a Weak Base with a Weak Acid
CONSENT FOR PUBLICATION
CONFLICT OF INTEREST
ACKNOWLEDGEMENTS
REFERENCES
Non-Aqueous Titrations
Abstract
INTRODUCTION
Solvent System for Non-Aqueous Titrations
Factors Affecting Selection of Solvent
Solvents Employed In Non-Aqueous Titration
Glacial Acetic Acid
Acetonitrile
Alcohols
Dioxane
Dimethylformamide
Indicators In Non-Aqueous Titrations
Crystal Violet
1-Naphtholbenzein
Nile Blue A
Oracet Blue B
Quinaldine Red
Thymol Blue
Azovoilet
Alkalimetry
Estimation of Acids
Assay of Ethosuximide
Assay of Chlorthalidone
Acidimetry
Estimation of Amines and Amine Salts of Organic Acids
Assay of Methyldopa
Assay of Nitrazepam
Estimation of Halogen Acid Salts of Bases
Assay of Amitriptyline Hydrochloride
Advantages of Non-Aqueous Titrations
Limitations of Non-Aqueous Titrations
Conclusion
CONSENT FOR PUBLICATION
CONFLICT OF INTEREST
ACKNOWLEDGEMENTS
REFERENCES
Redox Titrations
Abstract
INTRODUCTION
History And Development Of Redox Titration Method
Principle and Theory
Oxidizing and Reducing Agents
Oxidizing Agents
KMnO4 (Potassium Permanganate)
K2Cr2O7 (Potassium Dichromate)
Iodine Solution
Potassium Iodate
Bromate-bromide Mixture
Reducing Agents
Equivalent weight of oxidizing and reducing agents
Oxidation number (O.N.)
Rules of Assigning Oxidation Number
Primary Standard
Factors affecting redox titrations
Redox Indicators
Types of Redox Indicators
Based on the Addition of Indicator
Based on the Nature of the Indicator
Based on the Dependence on pH
Potentiometric Method (Redox Indicators)
Types of Redox Titrations
Based on the Titrant Used
Permanganate Titration
Dichromate Titration
Iodine Titration
Direct Method
Indirect Method
Based on the Method
Direct Titration
Back Titration
Redox Titration Curve
Calculating Titration Curve
Determining End Point
Use of Visual Indicator
Use of Potentiometric Method
Applications of the Redox Titrations
Use of Redox Titrimetry in the Inorganic Analysis
Chlorination of Public Water Supply
Determining Dissolved Oxygen in Water
Determination of Water in Nonaqueous Solvents
Use of Redox Titrations in Organic Analysis
Quantification of Lithium
Conclusion
CONSENT FOR PUBLICATION
CONFLICT OF INTEREST
ACKNOWLEDGEMENTS
REFERENCES
Complexometric Titrations
Abstract
INTRODUCTION
Complexation
Chelate
Ligands
Classification of Ligands
Monodentate Ligand
Bidentate and Multidentate Ligands
Co-ordinate Covalent Bonds or Dative Bonds
Covalent Bond
Werner’s Coordinate Number (WCN)
Stability Constant
Stability
Types of Complexometric Titrations
Types of Titrations:
Masking and Demasking Agents
Masking Agents
Need
Examples of Masking Agents
Demasking Agents
Metal ion Indicators Used in Complexometric Titrations
Common Examples
Mordant Black-II
Murexide (Ammonium Purpurate)
Xylenol orange (lemon to yellow)
Solochrome Dark Blue or Mordant Black-17 or Calcon
Alizarin Fluorine Complex or Alizarine Fluorine Blue or Alizarine Complex One
Assay of Magnesium Sulphate
Preparation and Standardization of 0.05M EDTA Solution
Standardisation
Assay of Aluminium Hydroxide Gel
Assay of Calcium Gluconate
Conclusion
CONSENT FOR PUBLICATION
CONFLICT OF INTEREST
ACKNOWLEDGEMENTS
REFERENCES
Diazotization Method
Abstract
INTRODUCTION
Principle
Theory
End Point Detection
Preparation and Standardization of the Sodium Nitrite Solution
Factors Affecting the Diazotization
Diazotization Titrations Methods
1. Direct Method
2. Indirect Method
3. Other Method
Procedure
Applications
Conclusion
CONSENT FOR PUBLICATION
CONFLICT OF INTEREST
ACKNOWLEDGEMENTS
REFERENCES
Kjeldahl Method
Abstract
INTRODUCTION
Principles
Digestion
Neutralization
Titration
Procedure
Step One: Digestion of the Sample
Digestion is Accomplished by
Step Two: Distillation
Step Three: Titration
Applications
Recent Developments
Conclusion
CONSENT FOR PUBLICATION
CONFLICT OF INTEREST
ACKNOWLEDGEMENTS
REFERENCES
Oxygen Flask Combustion Method
Abstract
INTRODUCTION
Apparatus
Preparation of Test Solution and Blank Solution
Preparation of Sample
Method of Combustion
Procedure of Determination
1. Chlorine and Bromine
2. Iodine
3. Fluorine
Standard Fluorine Solution
4. Sulfur
Applications
Conclusion
CONSENT FOR PUBLICATION
CONFLICT OF INTEREST
ACKNOWLEDGEMENTS
REFERENCES
Precipitation Titration
Abstract
INTRODUCTION
Precipitation Titration Example
Principle of Precipitation
Factors Influencing the Solubility of Precipitate
a) Effect of Temperature
b) Effect of Solvent
c) Effect of Corrosive
d) Formation of Complex Particles
Methods for Precipitation Titration
Mohr's Method
Precautions
Limitations
Preparation of 0.1 M Silver Nitrate
Volhard Method: Jacob Volhard (1834-1910)
Fajan's Strategy: Karl Kazimierz Fajan (1887-1975)
Limits of Precipitation Titration
How to Conquer the Issues of Precipitation Titration
APPLICATIONS
Conclusion
CONSENT FOR PUBLICATION
CONFLICT OF INTEREST
ACKNOWLEDGEMENTS
REFERENCES
Advanced Techniques of Analytical Chemistry
(Volume 1)
Edited by
Anju Goyal
Department of Pharmaceutical Chemistry,
Chitkara College of Pharmacy,
Chitkara University
Punjab
India
&
Harish Kumar
Govt. College of Pharmacy,
Rohru, Shimla,
Himachal Pradesh
India

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FOREWORD

Dr. Prabhakar Kumar Verma
M.Pharm, Ph.D. (UDPS Nagpur) Associate Professor of Pharmaceutical Chemistry Department of Pharmaceutical Sciences, M.D. University,
Rohtak-124001, Haryana, India

The classical analytical techniques include gravimetric, volumetric, and titrimetric methods; on the other hand, instrumental techniques involve ultraviolet-visible (UV-Vis), infrared (IR), and near-infrared (NIR) spectrophotometry fluorimetry, atomic spectroscopy (absorption/emission), electroanalytical chromatography.

The current volume of a book titled “Advance Techniques of Analytical Chemistry-Volume-1” is about techniques depending on the nature of reactions such as Acid-Base titrations which involve the reaction of an acid and a base. Redox titrations include redox reaction between analyte and titrant as the key reaction, Non-aqueous titrations, Complexometric titration which involves the formation of a colored complex compound, and some miscellaneous methods like Diazotisation Titrations, Kjeldahl Method and Oxygen flask combustion method, etc.

Advance Techniques of Analytical Chemistry-Volume-1 covers a number of important analytical chemistry topics. It does not, however, cover spectroscopic such as mass spectroscopy, IR or NMR as well as chromatographical techniques such as TLC, HPLC, HPTLC and other advanced techniques because these qualitative applications will be covered adequately incoming volumes i.e. Volume-II and Volume-III.

We are happy to recommend this book to students and researchers as there is more material than anyone can cover in one semester; I hope that the diversity of topics will meet the needs of different instructors.

Prabhakar Kumar Verma M.Pharm, Ph.D. (UDPS Nagpur) Associate Professor of Pharmaceutical Chemistry Department of Pharmaceutical Sciences, M.D. University, Rohtak-124001 Haryana India

Preface

Dr. Anju GoyalMr. Harish Kumar
Department of Pharmaceutical Chemistry, Chitkara College of Pharmacy,
Chitkara University, Punjab, India.
Govt. College of Pharmacy, Rohru, Shimla, Himachal Pradesh. India

The main purpose of this book is to cover the basic concept of volumetric titrations. Modern Advance Techniques of Analytical Chemistry essentially involves, as a necessary integral component, even greater horizons than the actual prevalent critical analysis of not only the active pharmaceutical substances but also the secondary pharmaceutical product(s) i.e., the dosage forms having the either single or multi-component formulated product. The fundamental reasons for this sudden legitimate surge in the newer evolving methodologies in the ‘analysis of drug substances’ are perhaps due to the tremendous growth in the progress of ‘medicinal chemistry’ towards achieving one ultimate objective which is to obtain ‘better drugs for a better world’. With the advent of computer-aided-drug modeling (CADM) the critical, scientific, and faster approach to newer drug entities based on the biologically active prototypes, combinatorial chemistry, chiral chemistry, and biotechnology has paved the way towards more specific, potent, and above all, less toxic ‘drugs’ to improve the ultimate quality of life in humans.

Keeping in view the above astronomical growth in the design of complicated, specific, and highly active drug molecules, equally viable, rigorous, accurate, and precise analytical methods have been evolved with the time which has now occupied pivotal and vital positions in most of the Official Compendia viz., USP, BP, Int.P., Eur. P, IP, etc., for the analysis of such compounds both in pure and dosage forms.

The present book on ‘Advance Techniques of Analytical Chemistry’ caters for the much-needed handbook and reference book, which is current about the esteemed philosophy of analytical chemistry, obvious solid support towards drug discovery, development, stability studies, bioavailability, and pharmacokinetic studies, and above all the quality assurance of pure drugs together with their respective dosage forms.

The textbook on ‘Advance Techniques of Analytical Chemistry’ would enormously serve the undergraduates, postgraduates, researchers, analytical chemists working in the Quality Assurance Laboratories, new drug development, production and control, teaching, or regulatory authorities.

Anju Goyal Chitkara College of Pharmacy Chitkara University Rajpura, Punjab India&Harish Kumar Govt. College of Pharmacy

List of Contributors

Astha SharmaLaureate Institute of Pharmacy, Jawalamukhi, Himachal Pradesh, IndiaAnju GoyalChitkara College of Pharmacy, Chitkara University, Punjab, IndiaHarish VermaGovt College of Pharmacy, Rohru, Shimla, Himachal Pradesh, IndiaKomalpreet KaurG.H.G Khalsa College of Pharmacy, Gurusar Sadhar, Ludhiana, IndiaMadhukar GargChitkara College of Pharmacy, Chitkara University, Punjab, IndiaMonika GuptaA.S.B.A.S.J.S. Memorial College of Pharmacy, Bela Punjab, IndiaNavdeep SinghLaureate Institute of Pharmacy, Jawalamukhi, Himachal Pradesh, IndiaNidhi GargChitkara College of Pharmacy, Chitkara University, Punjab, IndiaPayal DasChitkara College of Pharmacy, Chitkara University, Punjab, IndiaRajendra AwasthiAmity Institute of Pharmacy, Amity University Uttar Pradesh, Noida, Uttar Pradesh, IndiaRajwinder KaurChitkara College of Pharmacy, Chitkara University, Punjab, IndiaRamninder KaurChitkara College of Pharmacy, Chitkara University, Punjab, IndiaSandeep AroraChitkara College of Pharmacy, Chitkara University, Punjab, IndiaSapna KumariChitkara College of Pharmacy, Chitkara University, Punjab, IndiaShammy JindalLaureate Institute of Pharmacy, Jawalamukhi, Himachal Pradesh, IndiaShivani SharmaRKSD College of Pharmacy, Kaithal-136027, Haryana, IndiaSunaina AggarwalRKSD College of Pharmacy, Kaithal-136027, Haryana, IndiaUpasna KaushikRKSD College of Pharmacy, Kaithal-136027, Haryana, India

Introduction to Analytical Chemistry

Sapna Kumari1,*,Anju Goyal1,Madhukar Garg1,Harish Verma2
1 Chitkara College of Pharmacy, Chitkara University, Punjab, India
2 Govt College of Pharmacy, Rohru, Shimla, Himachal Pradesh, India

Abstract

Analytical chemistry, a branch of chemistry, deals with the analysis of substances. Identification of the constituents from the mixture or substance is called qualitative analysis while Quantitative Analysis deals with determining the purity of the constituents present in the mixture. This is also known as assay method. Various methods like volumetric analysis, gravimetric analysis, polarimetry, refractometry, photometry, fluorimetry, electrochemical methods, chromatographic methods and biological methods comes under the category of quantitative analysis. Volumetric titrations are the elementary procedures applied in the life sciences, pharmaceutics, industrial analysis, water pollution and clinical chemistry and are used to determine the amount of analyte with the standard solution. Main advantages of these methods are cost-effective, rapid and simple, while disadvantages include pH, temperature, and humidity sensitivity, indicator requirement, occurrence of human error, etc.

Keywords: Analytical chemistry, Endpoint, Indicator, Quantitative analysis, Volumetric titration.
*Corresponding Author Sapna Kumari: Chitkara College of Pharmacy, Chitkara University, Punjab, India; Email: [email protected]