EXPERIMENTS IN ANALYTICAL CHEMISTRY - AEACI
EXPERIMENTS INANALYTICAL CHEMISTRYA.V.R. ReddyK.K. SwainK. VenkateshASSOCIATION OF ENVIRONMENTALANALYTICAL CHEMISTRY OF INDIA
Printed by Mr. Vilas SangurdekaratPerfect Prints22/23, Jyoti Industrial EstateNooribaba Darga RoadThane 400 601, INDIATel. 022-2534 1291Copyright 2012byASSOCIATION OF ENVIRONMENTALANALYTICAL CHEMISTRY OF INDIAFor copies and other information, please write to:Secretary,Association of Environmental Analytical Chemistry of IndiaC/o Analytical Chemistry DivisionBhabha Atomic Research CentreTrombay, Mumbai 400 085INDIAFAX : 91 22 25505151
Association of Environmental Analytical Chemistry ofIndia (AEACI)Association of Environmental Analytical Chemistry of India (AEACI ) wasfounded on 30th November, 2010 during a meeting held at Analytical ChemistryDivision (ACD) in Bhabha Atomic Research Centre (BARC), Trombay, Mumbai toprovide a common platform to all the Indian scientists and scholars working in thefield of Analytical & Environmental Chemistry within the country from variousUniversities or Institutes or Industries. AEACI is a non-profit-making organizationwith its Head-Quarters at Analytical Chemistry Division, BARC, Mumbai. AEACIaims to promote the analytical environmental sciences and technology in India, todisseminate scientific and technological knowledge within the country and toadvance both national and international cooperation (in particular south Asianscountries) in the area of analytical and environmental Chemistry. The motivationto commence a national forum like AEACI came from the discussion in theSchool of Analytical Chemistry held at BARC, Mumbai during November 19th to26th November in 2011. Since its inception, the Association has evolvedmagnificently to represent a truly National Organization and at present, itcomprises about 155 life-members from different parts of India. The Executivecommittee of AEACI , which manages all the activities of AEACI, is being electedtriennially by the members of AEACI. The scientific and technological foraprovided by AEACI comprise the following. Symposia – that address environmental issues in a broad sense, butalways include analytical environmental chemistry as a central topicWorkshops – that are dedicated to specific topical areas of analyticalenvironmental researchShort courses – that are intended to familiarize scientists or engineerswith new techniques applicable in carrying our environmentally relevantinvestigations.To provide partial financial assistance to Indian Scientist (AEACI,members) to South Asian Countries.AEACI plans to have biannual Bulletins with guest editors from differentfields in the area of analytical environmental chemistry.To encourage scientists & technologists AEACI will institute a few awards torecognize and honour valuable contributions of Indian Scientists or scholars inthe area of analytical environmental Chemistry. Please visit the “Awards” sectionin the AEACI website (www.aeaci.org) to know details about these awards and tonominate for awards.R.K. SinghalGeneral Secretary, AEACI
About School on Analytical ChemistryAnalytical chemistry an interdisciplinary science and often is called centralscience that contributes to every branch of science. Analytical chemistry findsapplication in all the branches of science like chemistry, physics, biology, geology,materials science, nuclear science and technology, medicine, environment and industry.Analytical measurements are aimed at obtaining qualitative and quantitative informationabout the composition and structure of various materials that have relevance to bothfundamental understanding as well as applications towards improving the quality of life.Obtaining precise and reliable data is the prime requirement in the studies involvingmedical products, clinical evaluations, Environment impact and remediation, and hightech products. These data may be used in decision making. In view of this, a host ofinstrumental methods have been developed. The pace of development compares withthat of electronics industry. It is also essential to evaluate essence of the problem andchoose the right method that is fit for the purpose. Therefore analytical scientists need agood working knowledge of the available techniques, awareness about theadvancements made in instrumentation and methodologies, and have to adapt“continued education” approach for keeping abreast with the advancements intheoretical and experimental knowledge associated with the state-of-the-art analyticalmethodologies. One of the major requirements is understanding the underlying principleof the chosen method for a particular analysis. During the last century with the advent ofelectronics, rapid improvements in computer technology and automation of instrumentalmethods of analysis, a large number of instrumental methods are made available toanalytical chemists. Veracity of analytical data not only depends on choosing the correctinstrumental method, materials, procedures and evaluating the measured results intoconcentrations of the analytes but more on understanding the phenomenon of signalgeneration and deciphering reliably signal from background.It was thought that this could be achieved through organizing a 7 day School ofAnalytical Chemistry with an objective of providing a forum for revisiting fundamentals ofanalytical chemistry and exchanging with experts, the latest developments in analyticalchemistry and its applications. In addition to regular lectures on various aspects ofanalytical chemistry, laboratory experiments were included in this School to providehands on experience to the participants. It is expected that the participants will takeadvantage of the presence of experts and interact with them in a manner that facilitatescollective growth in the field of analytical chemistry. While formulating the syllabus forthe first school, some topics to impart the essence of work-culture, safe practices andgood laboratory practices, besides theoretical and experimental aspects were included.I am very happy that Analytical Chemistry Division has taken lead in organizingthis School in a Works-shop mode. It was planned for 50-60 participants, mainlycomprising of research scholars, young academics and young scientists from researchinstitutions like BARC, with Chemistry and Physics background. An examination isincluded on the last day of the Second School and the performance of the participantswas very good. Feedback from the first School encouraged us to make this School aregular feature and for the first time, the third School will be organized in a university (S.K. University, Ananatapur) during February 24 - March 01, 2012. It is heartening thata fledgling Association, AEACI has come forward to extend cooperation to organize thisSchool and thanks are due to all the members of EC, AEACI, particularly Dr. T.
Mukherjee, President, AEACI and director, Chemistry Group for all the support andguidance provided. Dr. R. Sinha, Director, BARC has been a source of inspiration in allour endeavours and his patronage to this School is gratefully acknowledged.Dr. S. Banerjee, Chairman, Atomic Energy Commission and Secretary, Department ofAtomic Energy for his continued guidance and encouragement.Organising such a School is not possible without the generous funds from theBoard of Research in Nuclear Sciences (BRNS). I take this opportunity to thank Prof. P.Rama Rao, Chairman, BRNS, Shri S.G. Markandeya, Scientific Secretary, BRNS,Members of the Board and Dr. S. Kailas, Chairman, Basic Sciences Committee, BRNSfor their support. I thank the cooperation extended by all the members of AnalyticalChemistry Division and administrative colleagues.A.V.R. ReddyHead, Analytical Chemistry Division
Presidential MessageGreetings to each one of you from AEACI and from all the members of ManagingCommittee of AEACI. Hope that all of you have also received the hard copy of thepamphlet for the School on Analytical Chemistry to be held at S.K. University,Anantapur, during February 24 - March 01, 2012. If not, please download the same fromthe website http://www.aeaci.org . This School consists of lectures in the morningsessions and laboratory experiments in the evening sessions. The target participants willbe young academics, research scholars, industrial personnel and budding scientistsfrom research centres. A total of 50 applicants will be selected as participants for thisSchool on all India basis. I am glad that my colleagues made efforts to publish a book on‘Experiments in Analytical Chemistry’ which will serve as a laboratory manual not only inSAC 2012 but also to M.Sc. students in Analytical Chemistry.Delegates and colleagues from India and overseas working in the area ofenvironmental and analytical chemistry are welcome to join hands with us, by becominglife-members of AEACI, to promote the growth of environmental and analytical chemistryworld-wide. We propose to work synergistically with other Societies in India and abroad,working in the field of environmental and analytical chemistry, to make use of themultifaceted applications of environmental analytical chemistry for the benefit ofmankind. Let us all work together to take the discipline of Environmental and AnalyticalChemistry to newer heights and make India as one of the internationally known leadersin this branch of science.My best wishes to each one of you in this challenging endeavour and lookforward to discuss at length scientifically during the upcoming events.You are welcome to suggest the names of reputed scientists and academiciansfrom India and abroad in this field who can deliver lucid and inspiring lectures in theupcoming events as well as in the continuous educational programmes of AEACI.Dr. T. MukherjeeDistinguished ScientistDirector, Chemistry GroupBhabha Atomic Research CentreTrombay, Mumbai 400 085
PrefaceAnalytical Chemistry is useful in all the branches of science like chemistry,physics, biology, geology, materials science, nuclear science and technology, medicine,environment and industry. Analytical measurements are aimed at obtaining qualitativeand quantitative information about the composition and structure of various materialsthat have relevance to both fundamental understanding as well as applications towardsimproving the quality of life. Analytical scientists need a good working knowledge of theavailable techniques, awareness about the advancements made in instrumentation andmethodologies. In view of this Analytical Chemistry Division, BARC has initiated toorganize a series of School on Analytical Chemistry for the benefit of young scientists,academics and research scholars with chemistry background and those who usechemical instrumentation of analysis in their work. In this School lectures are planned inthe morning hours, laboratory experiments in the afternoon hours to provide hands onexperience to the participants and specialized plenary lectures in the evening hours toprovide an insight into the frontiers of Analytical Chemistry. Although many good textbooks in the subject analytical chemistry are available, there is a paucity of books onexperiments in Analytical Chemistry. This book on experiments in Analytical Chemistryis an effort to provide a simple introduction to about 25 experiments covering variousaspects of instrumental methods of analysis. A few of the experiments are chosen ineach school and therefore this book is written as a manual with a provision to note theobservations and perform calculations. In addition a brief introduction is provided on afew relevant topics to inculcate laboratory work-culture, safe practices in the laboratoryand good laboratory practices, besides theoretical and experimental aspects. This bookis modeled on an IANCAS publication of Experiments in Radiochemistry: Theory andpractice.We thank all the authors who contributed to various experiments. We also thankother colleagues who have gone through the book critically.Association ofEnvironmental Analytical Chemistry of India (AEACI) has come forward to publish thisbook and we record our gratitude to the members of executive committee, AEACI led byDr. T. Mukherjee, President, AEACI and Director, Chemistry Group. Dr. R. Sinha,Director, BARC has been a source of inspiration in all our endeavors and his patronageto this School is gratefully acknowledged. We record our gratitude to Dr. S. Banerjee,Chairman, Atomic Energy Commission and Secretary, Department of Atomic Energy forhis continued guidance and encouragement. We thank Prof. P. Rama Rao, Chairman,Board of Research in Nuclear Sciences (BRNS) for his encouragement and support.This book is composed meticulously by Shri Sharad Nalavade and Shri Vishal N.Koli and we thank them for their whole hearted efforts. Our office colleagues SmtVaishali Wade and Smt S D. Shinde deserve appreciation for their cooperation andcontribution.A.V.R. ReddyK.K SwainK. VenkateshAnalytical Chemistry DivisionFebruary 18, 2012
Table of ContentsAssociation of Environmental Analytical Chemistry of India (AEACI)About School on Analytical Chemistry Presidential MessagePresidential MessagePrefaceChapter 1General Analytical Chemistry.1Basic Tools in Analytical Chemistry .4Safety Practices in a Chemical Laboratory . 6Sampling and Sample Preparation .9Analysis Methods .12Instrumental Methods of Analysis.13Basic Function of Instrumentation .16Signal generation, blank corrections, Calibration and Standardisation .17Treatment of Analytical Data . 19Some Aspects of Quality in Analytical Chemistry. 22LABORATORY EXPERIMENTSChapter 2ANALYTICAL SPECTROSCOPY .29Experiment 1Spectrophotometric Determination of Fe in WaterSample using Standard Addition Method .30Experiment 2Determination of Complex Ion Composition byJob’s Method of Continuous Variation .32Experiment 3Determination of Fe in Copper Metal by FlameAtomic Absorption Spectrometry (FAAS) .34Experiment 4Determination of Trace Metals (Fe, Ni, Cu, Cr andZn) in Environment Water Samples by FlameAtomic Absorption Spectrometry (FAAS) .36Experiment 5Determination of Cadmium (Cd) in BiologicalReference Material using Graphite Furnace Atomic
Experiment 6Absorption Spectrometry (GFAAS).39Determination of Arsenic in Ground Water usingHigh Resolution Continuum Source HydrideGeneration Atomic Absorption Spectrometry (HG-AAS) .41Experiment 7Determination of Cu, Ni and Zn in soil by ICP-OES.43Experiment 8Determination of Uranium in Ground Water by ICP- MS.45Chapter 3Chromatographic Methods.47Experiment 9Determination of Pesticides (Organophosphate) in SoilSample using HPLC .48Experiment 10Determination of Anions in Aqueous Samples usingIon Chromatography .50Experiment 11Determination of Hydrogen in the Gaseous Sampleusing Gas Chromatography .52Experiment 12Determination of Hydrocarbons in a Sample by GasChromatography (GC) .53Experiment 13Determination of Organics in Ground Water using GasChromatography / Mass Spectrometry .55Chapter 4Nuclear Analytical Techniques .57Experiment 14Determination of Absolute Activity by High ResolutionGamma ray Spectrometry using High PurityGermanium (HPGe) Detector .59Experiment 15Determination of Radioactivity in Surface Soil, Cementand Fly Ash .62Experiment 16Determination of Manganese in Steel by NeutronActivation Analysis .64Experiment 17Multielement Determination in Soil by SingleComparator NAA .66Experiment 18Determination of Thickness of Films by RutherfordBackscattering Spectrometry (RBS) .67Chapter 5Thermal And Electrochemical Methods Of Analysis .69Experiment 19Determination of ΔHmelting of Indium using DTA Technique .71
Experiment 20TG and DTA Techniques to Study of ReactionMechanism of Potassium Tetraoxalate atElevated Temperatures .72Experiment 21Determination of the Solubility ProductConstant of AgCl .73Experiment 22Determination of Toxic Elements by ElectrochemicalMethod .76Experiment 23Determination of Cu, Pb and Cd in Water Sampleby Differential Pulse Anodic StrippingVoltammetry (DPASV) .79Chapter 6Environmental Analytical Chemistry .81Experiment 24Estimation of Ammonia in Water using Kjeldahl Method .81Experiment 25Estimation of Mass Concentration of Aerosols .83Experiment 26Effect of Synoptic Meteorology on Aerosols .85Experiment 27Analysis of BOD and DO in Waste Water Sample .88Experiment 28Determination of Chemical Oxygen Demand (COD) .91Experiment 29Analysis of Fluoride in Ground Water and Potable Water .93Annex IFundamental Constants .95Annex IIConversion factors .96
1Experiments in Analytical ChemistryChapter 1GENERAL ANALYTICAL CHEMISTRYA.V.R. Reddy, K. Venkatesh, Sanjukta A. Kumar, K.K. Swain and R. VermaINTRODUCTION0BAnalytical Chemistry is the science of measurement based on a set of ideas andmethods employing state-of-the-art technology. Analytical chemistry is useful in all the branchesof science like chemistry, physics, biology, geology, materials science, nuclear science andtechnology, medicine, environment and industry. Analytical measurements are aimed atobtainingqualitative and quantitative information about the composition and structure ofvarious materials that have relevance to both fundamental understanding as well as applicationstowards improving the quality of life. Analytical chemistry is of interdisciplinary nature and oftenis called central science that contributes to every branch of science. Today, analyticalchemistry has a range of powerful tools to obtain the needed information. Obtaining preciseand reliable data is the prime requirement in any analytical method for obvious reasons. Thisaspect is pertinent to nuclear industry and contributes significantly in various stages of nuclearfuel cycle. It is also essential to evaluate essence of the problem and choose the right methodthat is fit for the purpose. Therefore analytical scientists need a good working knowledge of theavailable tec
Association of Environmental Analytical Chemistry of India (AEACI ) was founded on 30th November, 2010 during a meeting held at Analytical Chemistry Division (ACD) in Bhabha Atomic Research Centre (BARC), Trombay, Mumbai to provide a common platform to all the Indian scientists and scholars working in the field of Analytical & Environmental .
Stage / Analytical Chemistry Lecture - 1 Introduction to Analytical Chemistry 1.1 Types of analytical chemistry & their uses . 1.2 Classifying Analytical Techniques. 1.3 Quantitative Analysis Methods. 1.4 Applications of Analytical Chemistry. 1.5 Units For Expressing Concentration of Solutions. 1.6 P Functions. 1.7 Stoichiometric Calculation.
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Everything is made of chemicals. Analytical chemistry determine what and how much. In other words analytical chemistry is concerned with the separation, identification, and determination of the relative amounts of the components making up a sample. Analytical chemistry is concerned with the chemical characterization of matter and the
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Fundamentals of Analytical Chemistry (9thEd, 2014) Skoog-West-Holler-Crouch 7 8 9. 4 Chapter 1 Introduction of Analytical Chemistry What is Analytical Chemistry? An unknown sample solution The sample could contain: (1) Ca2 , Na , or K ions OR (2) A urine sample from a potentially pregnant woman
Chemistry is the science that describes matter, its properties, the changes it undergoes, and the energy changes that accompany those processes. Inorganic chemistry Organic chemistry Physical chemistry Biochemistry Applied Chemistry: Analytical chemistry, Pharmaceutical Chemistry, . Istv an Szalai (E otv os University) Lecture 1 6 / 45
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