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VicSoffiantini AnalyticalChemistry Also of Interest AtomicEmissionSpectrometry. AES–Spark,Arc,LaserExcitation DevicePhysics,Fabrication,Simulation Heinz-GerdJoosten,AlfredGolloch,JörgFlock,SusanKillewald, ISBN----,e-ISBN---- Micro-RamanSpectroscopy. TheoryandApplication JürgenPopp,ThomasMayerhöfer(Eds.), ISBN----,e-ISBN---- ElementalAnalysis. AnIntroductiontoModernSpectrometricTechniques GerhardSchlemmer,LieveBalcaen,JoséLuisTodolí, MichaelW.Hinds, Togetherwith:PublishingHouseofElectronicsIndustry ISBN----,e-ISBN---- ElasticLightScatteringSpectrometry ChengZhiHuang,JianLing,JianWang, Togetherwith:ChinaSciencePublishing&MediaLtd. ISBN----,e-ISBN---- Vic Soffiantini Analytical Chemistry Principles and Practice Author VicSoffiantini 4618P.O.Box Durban4000 SouthAfrica [email protected] ISBN978-3-11-072119-5 e-ISBN(PDF)978-3-11-072120-1 e-ISBN(EPUB)978-3-11-072121-8 LibraryofCongressControlNumber:2021947263 BibliographicinformationpublishedbytheDeutscheNationalbibliothek TheDeutscheNationalbibliothekliststhispublicationintheDeutscheNationalbibliografie; detailedbibliographicdataareavailableontheInternetathttp://dnb.dnb.de. ©2022WalterdeGruyterGmbH,Berlin/Boston Coverimage:VicSoffiantini Typesetting:IntegraSoftwareServicesPvt.Ltd. Printingandbinding:CPIbooksGmbH,Leck www.degruyter.com Preface Thisanalyticalchemistrytextbookhasbeencompiledbasedonalaboratoryskillsin- structionmanualformat,toassistanylaboratoryworkerwhohasnothadtheoppor- tunitiestoobtainformaleducationandtraininginsimplelaboratoryproceduresoris readingundergraduatechemistryorasciencecourse.Itcouldalsobeusedasateach- ingaidforlecturersandprofessors,ingeneralanalyticalprinciplesandpractice. Thebookcontains25chapters,manydiagramsandphotographs,aswellas20 appendicesofusefultablesandmaybeconsideredasanintroductiontobasicprin- ciplesandoperationsorprocessesofanalyticalscience,whichisanappliedscience andart,wherebyknowledgeofthescience,laboratoryskillsandtheart,areusedto obtain answers (e.g. for dissertations, laboratory data or test results) to problems suchas: – What test procedure to use for what type of sample composition or research work? – Whatapparatustouseforthatevaluationorinvestigation? – Howtousethatapparatusorinstrumentation? – Is the test result or research data obtained precise, accurate and scientifically credible? – Doestheresultshowthattheproduct,rawmaterial,specimen,testorresearch item, or sample is within quality specifications and standards; or whether the resultsproveordisproveahypothesis? Keywordsarelistedatthebeginningofeachchapter,foreaseofuseandindexing. There are some sections of text that has been repeated throughout the book. The intention of the repetition is to gain the attention of the reader or student to rememberandnotethosesectionsorcomments. Note: whilst every reasonable care has been taken in compiling this technical chemistry book to ensure the accuracy of the information supplied, the author does notacceptanyresponsibilityforanyerrorsoromissionsoranyconsequencesthereof. https://doi.org/10.1515/9783110721201-202 Contents Preface V Introduction 1 Chapter1 Analyticalchemistry 3 Chapter2 Laboratoryoperations 7 Chapter3 Planningtheanalysis 31 Chapter4 Sampling 35 Instrumentalanalysis Chapter5 Calorimetry 51 Chapter6 Chromatography 55 6.1 Columnchromatography 57 6.2 Gas–liquidchromatography 57 6.3 High-performanceliquidchromatography 63 6.4 Ionchromatography 65 6.5 Paperchromatography 66 6.6 Thin-layerchromatography 67 Chapter7 Conductometry 71 Chapter8 Coulometricanalysis 79 Chapter9 Potentiometry 83 VIII Contents Chapter10 Polarimetry 89 Chapter11 Turbidimetryandnephelometry 95 Chapter12 Polarography(voltammetry) 97 Chapter13 Refractometry 99 Chapter14 Spectrophotometry 103 14.1 Colorimetry 107 14.2 Colourscales 108 14.3 Ultravioletandvisiblespectrophotometry 109 14.4 Infraredspectrophotometry 114 14.5 FTIRspectrophotometry 114 14.6 Near-infraredspectrophotometry 117 14.7 Ramanspectrophotometry 118 14.8 Massspectrophotometry 118 14.9 Atomicabsorptionspectrophotometry 119 14.10 Inductivelycoupledspectrophotometry 125 14.11 Reflectancespectrophotometry 127 14.12 Fluorescencespectroscopy 128 14.12.1 Physicalmeasurements 129 Physicalmeasurements Chapter15 Viscosity 133 Chapter16 Density 139 16.1 Hydrometers 141 Chapter17 Particleanalysis 147 17.1 Gelpermeationchromatography 147 17.2 Testsieveanalysis 148 Contents IX 17.3 Particlecounters 151 17.4 Imaging 151 Chapter18 Surfacetension 153 18.1 Chemicalanalysis 154 Chapter19 Chemicalanalysis 157 19.1 Electrochemicalseries 157 19.2 Nomenclatureofacids 158 19.3 Valencies 158 19.4 Chemicalreagents 160 19.4.1 Preparationofsomecommonlaboratorysolutionsor reagents 163 19.4.2 Dilutionformula 164 19.4.3 PreparationofAASstandardaqueoussolutions 164 Chapter20 Gravimetricanalysis 167 20.1 Co-precipitation 168 20.2 Post-precipitation 169 Chapter21 Volumetricanalysis(titrimetric) 171 21.1 Titrations 172 21.2 Indicators 175 21.3 Coulometrictitrations 176 21.4 Argentometrictitrations 177 21.5 Neutralisationtitrations(acidsandbases) 178 21.6 Neutralisationtitrations(acidsandbases) 180 21.7 Redox(reduction–oxidation)titrations 181 21.8 Precipitationtitrations 182 21.9 Complexometrictitrations 183 Chapter22 Reactionswithiodine 185 22.1 Iodimetry 185 22.2 Iodometry 185 X Contents Chapter23 Qualitativechemicalanalysis 187 Data Chapter24 Datainterpretation 197 24.1 Thet-test:(akaStudent’st-test) 199 24.2 TheQ-test(orGrubbs’test) 199 24.3 TheF-test 200 24.4 Ganttcharts 200 24.5 Controlcharts 200 24.6 Regressionanalysis 201 24.7 Calibrationofinstrumentation 202 24.8 Validationofanalyticaltestmethods 203 24.9 Measurementoferrors 207 Chapter25 Laboratoryreports 215 25.1 Whataresignificantfigures? 215 25.2 Thereport 217 Appendices AppendixI Laboratorysafetyandchecklists 223 AppendixII Internationallyacceptedlaboratoryproceduresandtestmethods 233 AppendixIII Strengthsofcommonconcentratedacids 235 AppendixIV Unitsofmeasurementandconcentration 237 AppendixV InternationalSystem(SI)ofUnits 241 AppendixVI Metric(SI)prefixesanddecimalunitmultiples 243