Solution Manual For Quantitative Chemical Analysis Eighth Edition

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iguy7I,04:AGofWYEDTOiAresPN|af{0WD1)y=pa|:URCWaaa|||eighthEdition/i)SOLUTIONS||||MANUALFOR|49rraRATEDQuantitative_¥oriChemicalANGE|,enST.aTONAnalysis¥enREAR"Z\FSS)=aaADanielC.HarrisyyBRNp$5f\+StudyXy-=:E3§J=)

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DownloadedfromStudyXY.com®+StudyXYSdYe.o>\|iF’prE\3SStudyAnythingThisContentHasbeenPostedOnStudyXY.comassupplementarylearningmaterial.StudyXYdoesnotendroseanyuniversity,collegeorpublisher.Allmaterialspostedareundertheliabilityofthecontributors.wv8)www.studyxy.com

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SolutionsManualforHarris’QuantitativeChemicalAnalysisEighthEditionDanielC.HarrisMichelsonLaboratory

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ContentsChapter0TheAnalyticalProcess1Chapter1Measurements3Chapter2ToolsoftheTrade12Chapter3ExperimentalError17Chapter4Statistics24Chapter5QualityAssuranceandCalibrationMethods38Chapter6ChemicalEquilibrium53Chapter7ActivityandSystematicTreatmentofEquilibrium61Chapter8MonoproticAcid-BaseEquilibria71Chapter9PolyproticAcid-BaseEquilibria82Chapter10Acid-BaseTitrations97Chapter11EDTATitrations126Chapter12AdvancedTopicsinEquilibrium142Chapter13FundamentalsofElectrochemistry175Chapter14ElectrodesandPotentiometry189Chapter15RedoxTitrations202Chapter16~~ElectroanalyticalTechniques217Chapter17FundamentalsofSpectrophotometry230Chapter18ApplicationsofSpectrophotometry238Chapter19Spectrophotometers251Chapter20AtomicSpectroscopy260Chapter21~~MassSpectrometry269Chapter22IntroductiontoAnalyticalSeparations284Chapter23~~GasChromatography298Chapter24High-PerformanceLiquidChromatography311Chapter25ChromatographicMethodsandCapillaryElectrophoresis327Chapter26~~GravimetricAnalysis,PrecipitationTitrations,345andCombustionAnalysisChapter27~~SamplePreparation360

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CHAPTER0THEANALYTICALPROCESS0-1.Qualitativeanalysisfindsoutwhatisinasample.Quantitativeanalysismeasureshowmuchisinasample.0-2.Stepsinachemicalanalysis:(1)Formulatethequestion:Convertageneralquestionintoaspecificonethatcanbeansweredbyachemicalmeasurement.(2)Selecttheappropriateanalyticalprocedure.(3)Obtainarepresentativesample.(4)Samplepreparation:Converttherepresentativesampleintoasamplesuitableforanalysis.Ifnecessary,concentratetheanalyteandremoveormaskinterferingspecies.(5)Analysis:Measuretheunknownconcentrationinreplicateanalyses.(6)Produceaclearreportofresults,includingestimatesofuncertainty.(7)Drawconclusions:Basedontheanalyticalresults,decidewhatactionstotake.0-3.Maskingconvertsaninterferingspeciestoanoninterferingspecies.0-4.Acalibrationcurveshowstheresponseofananalyticalmethodasafunctionoftheknownconcentrationofanalyteinstandardsolutions.Oncethecalibrationcurveisknown,thentheconcentrationofanunknowncanbededucedfromameasuredresponse.0-5.(a)Ahomogeneousmaterialhasthesamecompositioneverywhere.Inaheterogeneousmaterial,thecompositionisnotthesameeverywhere.(b)Inasegregatedheterogeneousmaterial,thecompositionvariesonalargescale.Therecouldbelargepatcheswithonecompositionandlargepatcheswithanothercomposition.Thedifferencesaresegregatedintodifferentregions.Inarandomheterogeneousmaterial,thedifferencesoccuronafinescale.Ifwecollecta“reasonable-size”portion,wewillcaptureeachofthedifferentcompositionsthatarepresent.(c)Tosampleasegregatedheterogeneousmaterial,wetakerepresentativeamountsfromeachoftheobviouslydifferentregions.InpanelbinBox0-1,66%oftheareahascompositionA,14%isB,and20%isC.Toconstructa1

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2Chapter0’representativebulksample,wecouldtake66randomlyselectedsamplesfromregionA,14fromregionB,and20fromregionC.Tosamplearandomheterogeneousmaterial,wedividethematerialintoimaginarysegmentsandcollectrandomsegmentswiththehelpofatableofrandomnumbers.0-6.WeareapparentlyobservinginterferencebyMn2*intheI-analysisbymethodA.TheresultoftheIanalysisisaffectedbythepresenceofMn2*.ThegreatertheconcentrationofMn2*inthemineralwater,thegreateristheapparentconcentrationofI-foundbymethodA.MethodBisnotsubjecttothesameinterference,sotheconcentrationofI-islowandindependentofadditionofMn2*,TheremustbesomeMn2+intheoriginalmineralwater,whichcausesmethodAtogiveahigherresultthanmethodBevenwhennoMn2*isdeliberatelyadded.

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CHAPTER1MEASUREMENTSAnotefromDan:Don’tworryifyournumericalanswersareslightlydifferentfromthoseintheSolutionsManual.YouorImayhaveroundedintermediateresults.Ingeneral,retainmanyextradigitsforintermediateanswersandsaveourroundoffuntiltheend.We'llstudythisprocessinChapter3.1-1.(a)meter(m),kilogram(kg),second(s),ampere(A),kelvin(K),mole(mol)(b)hertz(Hz),newton(N),pascal(Pa),joule(J),watt(W)1-2.Abbreviationsabovekiloarecapitalized:M(mega,106),G(giga,109),T(tera,1012),P(peta,1015),E(exa,1018),Z(zetta,102!)andY(yotta,1024).1-3.(@mW=milliwatt=10-3watt(b)pm=picometer~~=10-12meter(c)kQ=kiloohm=103ohm(d)uF=microfarad~~=10-6farad(e)TJ=terajoule=1012joule(f)ns=nanosecond=10-9second(g)fg=femtogram~~=10-15gram(h)dPa=decipascal=10-!pascal1-4.(a)100{Jor0.1pJ(d)0.1nmor100pm(b)43.1728nF(e)21TW(c)299.79THzor0.29979PHz (f)0.483amolor483zmol1-5.(a)5.4Pg=54x1015g 54x1015£xi=5.4x1012kgofC(b)TheformulamassofCOis12.0107+2(15.9994)=44.0095.0095kg5.4%1012kgexHIa=2.01013kgCO,1ton2.0x1013COyx————=2.0x1010¢fCO(c)K2)To0074ons02)2.0x10"tons~———5———"=4tonsperperson5x10"people3Study

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4Chapter11-6.Table1-4tellsusthat|horsepower=745.700W=745.700J/s.100.0horsepower=(100.0horsepower(raze)=7.457x104J/s.0)er7457x10%4{——ix3600£—6416x10741844hhcal12.2x10°ol4.1841dagnydaywal)\24|3600s7,@)2ATT20(skg)(120pound[oss65]=2.0WikgSimilarly,3.4x103rel3.0J/(s'kg)=3.0W/kg.ay(b)Theofficeworker’spoweroutputis12210624(41801)\(_K“1x12—ix102wdagwlJ24K)(3600s5Theperson’spoweroutputisgreaterthanthatofthe100Wlightbulb.1-8.5.00x103BE1055.061K=1.47x103La1.47x103WxBt)(3600ssm\(ljnch|1fost1milemile1-9.a)11000—||——|——||————|=0.621377—®(i)re|me)km®)100kn(re37miles)(3.785410)_|miles4.68kmgallongallona(c)Thedieselengineproduces223gCO,/km,whichwewillconvertintog/mile:(23B22=)Un)aECDkrfiJ0.62137milemieIn15000miles,CO,=(15000mites)(359g/mite)=5.38x10°gor5.38x10°kg=5.38metrictons.Thegasolineengineproduces266gCO,/km,

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Measurements5whichweconvertinto428g/mileor6.42metrictonsin15000miles.1-10.Newton=force=massxacceleration=(3)smm?Joule=energy=forcexdistance=kg!—|m=kg—ssmkgPascal=pressure=force/area=kg=/m2=—=sms211-11.003FE|[10002(535Jari)1),#2.gaJatt1000pg571tondayton—=|"OR3652>|=6——1000£100074yearyear1-12.(a)molarity=molesofsolute/literofsolution(b)molality=molesofsolute/kilogramofsolvent(c)density=gramsofsubstance/milliliterofsubstance(d)weightpercent=100x(massofsubstance/massofsolutionormixture)(e)volumepercent=100x(volumeofsubstance/volumeofsolutionormixture)(f)partspermillion=106x(gramsofsubstance/gramsofsample)(2)partsperbillion=109x(gramsofsubstance/gramsofsample)(h)formalconcentration=molesofformula/literofsolution1-13.Aceticacid(CH3CO,H)isaweakelectrolytethatispartiallydissociated.Whenwedissolve0.01molinaliter,theconcentrationsofCH3CO2HplusCH3CO;addto0.01M.TheconcentrationofCH3CO2Haloneislessthan0.01M.1-14.32.0g/[(22.990+35.453)g/mol]=0.548molNaCl0.548mol/0.500L=1.10M.1-15,[1mCHOooLsokution)=0.171molCH30HonStudy

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6Chapter10171cine)20)=548gmi1bar1-16.(2)19mPa=19x103Pa.19x103P§x——=1.9x107bar10°p§(b)T7(K)=273.15+°C=273.15-70=203K7rECoed=L1x108M=110M0.08314—=°x203Kmol.X1gsolute...1-17.1ppm=7662solution’Since1Lofdilutesolution=103g,1ppm=10-3gsolute/L.(=10-3gsolute/103gsolution).’Since103g=103pg,1ppm=103pg/Lor1pg/mL.Since10-3g=1mg,1ppm=1mg/L.1-18.0.2ppbmeans0.2x10-9gofCy9HyzpergofrainwaterBN_8CyHy0.2x106gCyoHgp=02x101000grainwater~Lrainwater~~°-602x10°4/L_7x10-10]282.55¢/mol1-19.[os88901|rgsolition)=26.5gHCIO4on37.6gsolution—26.5gHCIO4=11.1gHy0igsolutionol.1-20.(a)|1.67=———|1000—|=1.67x103lution©[toom)<1gHCIO43b)|0.705=———|(1.67x100]=1.18x103gHCIO,(b)polation(1.67x10°gsolution)gHCIO4(©)(1.18%103¢)/(100.46¢/mol)=11.7mol.__molKI1-21.molality=Kgsolventsolvent___200gKI_200gKI20.0wt%KI=7600gsolution~800gH0TofindthegramsofKIin1kgofH20,wesetupaproportion:Study

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Measurements7200gKIxgKI_800gH,0~1000gH0=X~250gKlBut250gKI=1.51molKI,sothemolalityis1.51m.150x10°15mol/eettamol1-22.@25107vesicles/cett~0Vessicle:(b)(6.0x107'8i)5.2«10%—=3.6x106moleculesa6(c)Volume=2x(200x109m)3=3.35x10-20m3;203oddheA335k1017L107°6°/L~18@10x10ol~030M335x107'L3480x101-23.80x10%=4.4x104mol;44x10"mol_44%103M;180.2¢/mol100x107LSimilarly,120mg/100L=6.7x10-3M.aol”1-24.(a)Massof1.000L=1.046x1000x1000¥=1046¢sal)4aolg2GramsofCaHgO3perliter=6.067——x62.07——=376.62Hg02pLprsL(b)1.000Lcontains376.6gofCoHgO2and1046—376.6=669gofH,0=0.669kg6.067molCoHgO2BnmolCoHgO2BMolality=T0660keHhOkg09.07TkgH009.07m1-25.Shreddedwheat:1.000gcontains0.099gprotein+0.799gcarbohydrate0.099¢xw+0799¢xwg=3.6CalDoughnut:1.000gcontains0.046gprotein+0.514gcarbohydrate+0.186gfat0.046£x0+05144xwg+0.186¢x207=3.9CalCInasimilarmanner,wefind2.8-forhamburgerand0.48orapple.Thereare16ouncesin|pound,whichTable1-4saysisequalto453.59237gStudy

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8Chapter18=28.35prToconvertCal/gtoCal/ounce,multiplyby28.35:ShreddedWheat~~DoughnutHamburgerAppleCal/g3.6392.80.48Cal/ounce10211179141-26.Massofwater=7(225pi)2(10.0A)5a)=1.59x109kg_16x103gFL6ppm=“0H0MassofF~required=[1e-1073SosawkgH70)=2.5%106gF~.(Ifweretainthreedigitsforthenextcalculation,thislastnumberis2.54x106.)TheatomicmassofFis18.998andtheformulamassofHySiFgis144.09.OnemoleofHySiFgcontains6molesofF.massof©6x18.9982.54x106gF_5.massofHoSiFg~144.00~xgHoSiFg=%=3:2100gHaSiFe’1-27.(a)PV=nRT(1.000bar)(5.24x10-6)=n|0.083jgLeshan(298.15K)mol-K=n=211%107mol=2.11x107M(b)Ar:0.934%means0.00934LofArperLofair(1.000bar)(0.00934L)=n[08sater)(298.15K)mol+K|=n=3.77x104mol=3.77x104MKr:1.14ppm=1.14pLKrperLofair=4.60x10-8MXe:87ppb=>87nLXeperLofair=3.5x109M1-28.2.00¥0.05002,6153-8—618gina?2Lvolumetricflaskxpat1-29.Weighout2x0.0500mol=0.100mol=6.18gB(OH)3anddissolvein2.00’kgHy0.Study

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Measurements91-30.Mcon*Yeon=MailVail0.80%1.00¥)=(0252)Vai=Vail=32L}4L1-31.Weneed1.00¥x010%=0.10molNaOH=4.0gNaOH40gNaOHSon=8.0gsolution0.50=———gsolutionMail1.00M132.(@)Veon=Vailjg,=1000mLbr)=55.6mL(b)Oneliterof98.0%H,SO4contains(18.0yw6l)(98.079/mel)=1.77x103gofHpSO4.Sincethesolutioncontains98.0wt%HS04,andthemassofH,S04permLis1.77g,themassofsolutionpermilliliter(thedensity)is1.77gHp804/mL_TERRATE80gsolution/mL0.980gH25807/gsolution1-33.2.00Lof0.169MNaOH=0.338molNaOH=13.5gNaOH.__gsolutiondensity={solution135gNaOTl=EEa.i1nE(16.7mLion)0524E00gsolution1-34.FMofBa(NO3);=261.344.35gofsolidwith23.2wt%Ba(NO3),contains(0.232)(4.35g)=1.01gBa(NO3)2-(1.01gBagNO3)2)molBa2t=————=—~~~=3.86x10-3mol(261.34gBagNO73);/mol)molHSO4=molBa2t=3.86x10-3mol(3.86x10-3mol)volumeofHySO4=(3.00mol/L)=1.29mL1-35.25.0mLof0.0236MTh**contains(0.0250L)(0.0236M)=5.90x10-4molTh4+molHFrequiredforstoichiometricreaction=4xmolTh#*=2.36x10-3mol50%excess=1.50(2.36x10-3mol)=3.54x10-3molHF-Study

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10Chapter|RequiredmassofpureHF=(3.54x10-3mol)(20.01g/mol)=0.0708g0.0708gHFMassof0.491wt%HFsolution=—CCOSHE)(0.00491gHF/gsolution)1-36.Concentrationsofreagentsusedinananalysisaredeterminedeitherbyweighingoutsupposedlypureprimarystandardsorbyreactionwithsuchstandards.Ifthestandardsarenotpure,noneoftheconcentrationswillbecorrect.1-37.Theequivalencepointoccurswhentheexactstoichiometricquantitiesofreagentshavebeenmixed.Theendpoint,whichcomesneartheequivalencepoint,ismarkedbyasuddenchangeinaphysicalpropertybroughtaboutbythedisappearanceofareactantorappearanceofaproduct.1-38.Inablanktitration,thequantityoftitrantrequiredtoreachtheendpointintheabsenceofanalyteismeasured.Bysubtractingthisquantityfromtheamountoftitrantneededinthepresenceofanalyte,wereducethesystematicerror.1-39.Inadirecttitration,titrantreactsdirectlywithanalyte.Inabacktitration,aknownexcessofreagentthatreactswithanalyteisused.Theexcessisthenmeasuredwithasecondtitrant.1-40.Primarystandardsarepurerthanreagent-gradechemicals.Theassayofaprimarystandardmustbeveryclosetothenominalvalue(suchas99.95100.05%),whereastheassayonareagentchemicalmightbeonly99%.Primarystandardsmusthaveverylongshelflives.1-41.Sincearelativelylargeamountofacidmightberequiredtodissolveasmallamountofsample,wecannottolerateevenmodestamountsofimpuritiesintheacidfortraceanalysis.Otherwise,thequantityofimpuritycouldbegreaterthanquantityofanalyteinthesample.1-42.40.0mLof0.0400MHga(NO3)>=1.60mmolofHg",whichwillrequire3.20nPY3.201mmolofKI.Thisiscontainedinvolume=5100mmol=32.0mL.1-43.108.0mLof0.1650Moxalicacid=17.82mmol,whichrequires2molMnO,iSmolHhCa0uH2C105(17.82molHyC204)=7.128mmolofMnO,.Study

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Measurements117.128mmol/(0.1650mmol/mL)=43.20mLofKMnOy4.Anotherwaytoseethisistonotethatthereagentsareboth0.1650M.Therefore,volumeofMnO};=(volumeofoxalicacid).Forsecondquestion,volumeofoxalicacid=3(volumeofMnO)=270.0mL.1-44.1.69mgofNH3=0.0992mmolofNH3.Thiswillreactwith20.0992)=0.149mmolofOBr™.ThemolarityofOBr™is0.149mmol/1.00mL=0.149M.1-45.molsulfamicacid=Sa=3.4369mmol._3.4369mmolmolarityofNaOH=“3426mL0.1003M1-46.HCladdedtopowder=(10.00mL)(1.396M)=13.96mmolNaOHrequired=(39.96mL)(0.1004M)=4.012mmolHCIconsumedbycarbonate=13.96—4.012=9.94gmmolmolCaCO3=3molHCIconsumed=4.974mmol=0.497ggCaCO3N_0.497ggCaCO3B5wt%CaCO3=(75413glimestoneglimestonex100=92.0wt%Study

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CHAPTER2-TOOLSOFTHETRADE2-1.Theprimaryruleistofamiliarizeyourselfwiththehazardsofwhatyouareabouttodoandnottodosomethingyouconsidertobedangerous.2-3.Dichromate(Cr,0%)issolubleinwaterandcontainscarcinogenicCr(VI).ReducingCr(VI)toCr(IlI)decreasesthetoxicityofthemetal.ConvertingaqueousCr(III)tosolidCr(OH);decreasesthesolubilityofthemetalandthereforedecreasesitsabilitytobespreadbywater.Evaporationproducestheminimumvolumeofwaste.2-4.Theupper“0”meansthatthereagenthasnofirehazard.Therighthand“0”indicatesthatthereagentisstable.The“3”tellsusthatthereagentiscorrosiveortoxicandweshouldavoidskincontactorinhalation.2-5.Thelabnotebookmust:(1)statewhatwasdone;(2)statewhatwasobserved;and(3)beunderstandabletoastranger.i2-6.SeeSection2.3.2-7.Thebuoyancycorrectionis1whenthesubstancebeingweighedhasthesamedensityastheweightsusedtocalibratethebalance.0.0012g/mL(14.82g)(1~~8.0g/mL)2-8.m=(0.0012ul}=1485¢g~0.626g/mL2-9.ThesmallestcorrectionwillbeforPbO»,whosedensityisclosestto8.0g/mL.Thelargestcorrectionwillbefortheleastdensesubstance,lithium.42366e(10.0012Sal_8.0g/mL)2-10.m=TC(-AEAmn0.0012BE)=42391g“71.636g/mLWithoutcorrectingforbuoyancy,wewouldthinkthemassofprimarystandardislessthantheactualmassandwewouldthinkthemolarityofbasereactingwiththestandardisalsolessthantheactualmolarity.Thepercentageerrorwouldbetruemass—measuredmass4.2391-4.2366truemass=100=4.2391*100=0.06%.12!Study

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