Analytical Atomic Spectrometry with Flames and Plasmas PDF
Preview Analytical Atomic Spectrometry with Flames and Plasmas
AnalyticalAtomicSpectrometrywithFlamesandPlasmas.Jose´A.C.Broekaert Copyright>2002Wiley-VCHVerlagGmbH&Co.KGaA ISBNs:3-527-30146-1(Hardback);3-527-60062-0(Electronic) Jose´A.C.Broekaert AnalyticalAtomic SpectrometrywithFlames andPlasmas AnalyticalAtomicSpectrometrywithFlamesandPlasmas.Jose´A.C.Broekaert Copyright>2002Wiley-VCHVerlagGmbH&Co.KGaA ISBNs:3-527-30146-1(Hardback);3-527-60062-0(Electronic) Analytical Atomic Spectrometry with Flames and Plasmas Valeur,B. Molecular Fluorescence. Principles and Applications 2001.ISBN3-527-29919-X Gu(cid:127)nzler,H.andWilliams,A. Handbook of Analytical Techniques 2001.ISBN3-527-30165-8 Hu(cid:127)bschmann,H.-J. Handbook of GC/MS 2001.ISBN3-527-30170-4 Welz,B.andSperling,M. Atomic Absorption Spectrometry Third,CompletelyRevisedEdition 1998.ISBN3-527-28571-7 AnalyticalAtomicSpectrometrywithFlamesandPlasmas.Jose´A.C.Broekaert Copyright>2002Wiley-VCHVerlagGmbH&Co.KGaA ISBNs:3-527-30146-1(Hardback);3-527-60062-0(Electronic) Jose´ A. C. Broekaert Analytical Atomic Spectrometry with Flames and Plasmas Weinheim –New York – Chichester– Brisbane – Singapore –Toronto AnalyticalAtomicSpectrometrywithFlamesandPlasmas.Jose´A.C.Broekaert Copyright>2002Wiley-VCHVerlagGmbH&Co.KGaA ISBNs:3-527-30146-1(Hardback);3-527-60062-0(Electronic) Prof.Dr.Jose´A.C.Broekaert Typesetting AscoTypesetters,HongKong Universita¨tLeipzig Printing betz-druckgmbH,D-64291 Institutfu¨rAnalytischeChemie Darmstadt Linne´straße3 Bookbinding WilhelmOsswald&Co.,67433 04103Leipzig Neustadt Germany ISBN 3-527-30146-1 9 Thisbookwascarefullyproduced. Nevertheless,authorandpublisherdonot warranttheinformationcontainedtherein tobefreeoferrors.Readersareadvisedto keepinmindthatstatements,data, illustrations,proceduraldetailsorother itemsmayinadvertentlybeinaccurate. LibraryofCongressCardNo.:appliedfor Acataloguerecordforthisbookisavailable fromtheBritishLibrary. DieDeutscheBibliothek–CIP Cataloguing-in-Publication-Data Acataloguerecordforthispublicationis availablefromDieDeutscheBibliothek (WILEY-VCHVerlagGmbH,D-69469 Weinheim(FederalRepublicofGermany). 2002 Allrightsreserved(includingthoseof translationinotherlanguages).Nopartof thisbookmaybereproducedinanyform– byphotoprinting,microfilm,oranyother means–nortransmittedortranslatedinto machinelanguagewithoutwritten permissionfromthepublishers.Registered names,trademarks,etc.usedinthisbook, evenwhennotspecificallymarkedassuch, arenottobeconsideredunprotectedbylaw. PrintedintheFederalRepublicof Germany. Printedonacid-freepaper. AnalyticalAtomicSpectrometrywithFlamesandPlasmas.Jose´A.C.Broekaert Copyright>2002Wiley-VCHVerlagGmbH&Co.KGaA ISBNs:3-527-30146-1(Hardback);3-527-60062-0(Electronic) TomywifePaulaandourdaughtersIlse, SigridandCarmen AnalyticalAtomicSpectrometrywithFlamesandPlasmas.Jose´A.C.Broekaert Copyright>2002Wiley-VCHVerlagGmbH&Co.KGaA ISBNs:3-527-30146-1(Hardback);3-527-60062-0(Electronic) vii Contents Preface xi Introduction 1 1 BasicPrinciples 4 1.1 Atomicstructure 4 1.2 Plasmas 8 1.3 Emissionandabsorptionofradiation 9 1.4 Ionization 18 1.5 Dissociation 23 1.6 Sourcesforatomicspectrometry 27 1.7 Analyticalatomicspectrometry 31 2 SpectrometricInstrumentation 34 2.1 Figuresofmeritofananalyticalmethod 34 2.2 Opticalspectrometers 51 2.2.1 Opticalsystems 52 2.2.2 Radiationdetectors 61 2.2.3 Non-dispersivespectrometers 70 2.3 Massspectrometers 72 2.3.1 Typesofmassspectrometers 73 2.3.2 Iondetection 80 2.3.3 Ionextraction 82 2.3.4 Ionopticsandtransmission 84 2.4 Dataacquisitionandtreatment 84 3 SampleIntroductionDevices 88 3.1 Sampleintroductionbypneumaticnebulization 90 3.2 Ultrasonicnebulization 103 3.3 Hydrideandothervolatilespeciesgeneration 105 3.4 Electrothermalvaporization 109 3.4.1 Thevolatilizationprocess 109 3.4.2 Typesofelectrothermaldevices 111 viii Contents 3.4.3 Temperatureprogramming 114 3.4.4 Analyticalperformance 115 3.5 Directsolidssampling 117 3.5.1 Thermalmethods 117 3.5.2 Slurryatomization 120 3.5.3 Arcandsparkablation 124 3.5.4 Laserablation 131 3.6 Cathodicsputtering 135 4 AtomicAbsorptionSpectrometry 148 4.1 Principles 148 4.2 Atomicabsorptionspectrometers 150 4.2.1 Spectrometers 150 4.2.2 Primaryradiationsources 152 4.3 Flameatomicabsorption 158 4.3.1 Flamesandburners 159 4.3.2 Nebulizers 161 4.3.3 Figuresofmerit 162 4.4 Electrothermalatomicabsorption 164 4.4.1 Atomizers 165 4.4.2 Thermochemistry 168 4.4.3 Figuresofmerit 169 4.5 Specialtechniques 172 4.5.1 Hydrideandcold-vaportechniques 172 4.5.2 Directsolidssampling 174 4.5.3 Indirectdeterminations 175 4.5.4 Flowinjectionanalysis 175 4.5.5 Diodelaseratomicabsorptionspectrometry 176 4.6 Backgroundcorrectiontechniques 177 4.6.1 Correctionforbackgroundabsorptionwiththedeuteriumlamp technique 177 4.6.2 BackgroundcorrectionwiththeaidoftheZeemane(cid:128)ect 179 4.6.3 Smith–Hieftjetechnique 182 4.6.4 Coherentforwardscattering 183 4.7 Fieldsofapplication 184 4.8 Outlook 191 5 AtomicEmissionSpectrometry 192 5.1 Principles 192 5.2 Atomicemissionspectrometers 202 5.3 Flameemission 210 5.4 Arcsandsparks 210 5.4.1 Arcemissionspectrometry 210 5.4.1.1 Arccharacteristics 210 Contents ix 5.4.1.2 Dcarcspectrometry 211 5.4.1.3 Acarcspectrometry 213 5.4.2 Sparkemissionspectrometry 213 5.4.2.1 Sparks 213 5.4.2.2 Analyticalfeatures 215 5.5 PlasmasourceAES 216 5.5.1 Dcplasma-jetAES 217 5.5.1.1 Typesofplasmajets 217 5.5.1.2 Three-electrodeplasmajet 218 5.5.2 InductivelycoupledplasmaAES 219 5.5.2.1 Theinductivelycoupledplasma 219 5.5.2.2 Instrumentation 221 5.5.2.3 Analyticalperformance 223 5.5.2.4 Applications 232 5.5.3 Low-powerhigh-frequencyplasmas 233 5.5.4 Microwaveplasmas 234 5.6 GlowdischargeAES 241 5.6.1 HollowcathodesforAES 242 5.6.2 Furnaceemissionspectrometry 243 5.6.3 Dcglowdischargeswithaflatcathode 244 5.6.4 Rfglowdischarges 248 5.6.5 Newdevelopments 249 5.7 Lasersources 251 6 PlasmaMassSpectrometry 254 6.1 ICPmassspectrometry 255 6.1.1 Instrumentation 255 6.1.2 Analyticalfeatures 257 6.1.3 Applications 268 6.1.4 Outlook 272 6.2 Glowdischargemassspectrometry 275 6.2.1 Instrumentation 277 6.2.2 Analyticalperformance 281 6.2.3 Analyticalapplications 282 7 AtomicFluorescenceSpectrometry 290 7.1 Principles 290 7.2 Instrumentation 293 7.3 Analyticalperformance 295 8 LaserEnhancedIonizationSpectrometry 297 8.1 Principles 297 8.2 Figuesofmerit 300 8.3 Analyticalapplications 301 x Contents 9 SamplePreparationforAtomicSpectrometry 302 9.1 Samplepreparationindirectcompactsampleanalysis 302 9.2 Grinding,sievingandcompactionofpowders 302 9.3 Sampledissolution 304 9.3.1 Wetchemicalmethods 304 9.3.2 Fusionprocedures 304 9.3.3 Microwave-assistedmethods 305 9.3.4 Combustiontechniques 305 9.4 Flowinjectionanalysis 305 9.5 Leachingsamplepreparationmethods 306 10 ComparisonwithOtherMethods 307 10.1 Powerofdetection 307 10.2 Analyticalaccuracy 309 10.3 Economicaspects 310 Literature 312 Index 348 AnalyticalAtomicSpectrometrywithFlamesandPlasmas.Jose´A.C.Broekaert Copyright>2002Wiley-VCHVerlagGmbH&Co.KGaA ISBNs:3-527-30146-1(Hardback);3-527-60062-0(Electronic) xi Preface Spectrochemical analysis is a powerful instrumental principle for the determina- tionofthechemicalelementsandtheirspeciesinavarietyofsampletypesofdif- ferent size, at widely di(cid:128)erent concentration levels and with very di(cid:128)ering cost performanceratiosandtimeconsumption.Inaddition,notonlymonoelementbut alsomultielementdeterminationsarepossible withwidelydi(cid:128)ering precisionand accuracy using the various di(cid:128)erent methods. The basic principles of spectro- chemicalanalysisarerelatedtotheatomicandmolecularstructureandalsotogas dischargephysicsaswellastoinstrumentationandmeasurementsciences.There- fore, research into spectrochemical analysis requires knowledge of the aforemen- tioned disciplines to enable innovative developments of new methodologies to be achieved in terms of the improvement of power of detection, accuracy and cost performance ratios, these being the driving forces in analytical innovation. The developmentofanalyticalproceduresalsorequirestheanalyticalchemisttohavea knowledgeofthetheoryandtheprinciplesoftheabovementioneddisciplines.Itis the aim of this monograph to bring together the theory and principles of todays spectrochemicalmethodsthatmakeuseofflamesandplasmasources.Thisshould enableresearcherstoenterthefieldofspectrochemicalresearch,whereinnovation is through the use and development of new sources and the application of new types of spectrometers, and also to face challenges from emerging fields of appli- cation,whichisasstraightforwardtodayasitwaseveninthetimeofBunsenand Kirchho(cid:128). This work should appeal both to chemists and physicists, the coopera- tion of whom is instrumental for progress to be made in this field of analytical chemistry as well as to users from di(cid:128)erent areas of science, including the life sciences, material sciences, environmental sciences, geochemistry, chemical pro- cess technology, etc. This present work could also be viewed as a resume of the theoretical background, which manufacturers of instrumentation for atomic ab- sorptionspectrometry,arc,sparkandglowdischargeemissionspectrometryaswell as ICP emission spectrometry and plasma mass spectrometry with ICPs or glow dischargesandlaserbasedtechniquescanrecommendtotheirinterestedusersto makethemoste(cid:129)cientuseoftheseanalyticalmethodsintheirrespectivefieldsof application.Alsoresearchassociatesenteringthefieldofatomicspectroscopywith flamesandplasmasshouldfindthenecessarybasicsandreferencestofurtherlitera- tureinthisbook.
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