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Midwest Grape and Wine Industry Institute

Preparing Standard Sodium Hydroxide Solution*


By Dr. Murli Dharmadhikari and Tavis Harris
Note:Thisarticlehasbeenwrittenattherequestoftheindustry.Itis
writtenforwinelabworkerswithnobackgroundinchemistry.

Inawinelaboratory,analyzingwineforTA,VAandS02involvestheuseofasodium
hydroxide(NaOH)reagent.Winemakersusuallybuysodiumhydroxidesolutionofa
knownconcentration(usually0.1Normal).Thisreagentisrelativelyunstableandits
concentrationchangesovertime.Toensuretheaccuracyofanalyticalresultsitis
importanttoperiodicallychecktheconcentration(Normality)ofsodiumhydroxide.If
theconcentrationhaschangedthenitmustbereadjustedtotheoriginalconcentration
orthenewconcentration(Normality)valueneedstobeusedincalculations.

Sometimesawinemakermaywishtomakehis/herownNaOHsolutioninsteadof
buyingit.Whethermakinganewsolutionorcheckingthenormalityofanoldsolution
itisimportanttoknowtheprocedureformakingastandard(knownconcentration)
solutionofNaOHreagent.Inthepresentarticlethestandardizationprocedurealong
withthebasicconceptbehindthetitrationprocedureareexplained.
Expressing concentration in solution

Asolutionconsistsofasoluteandthesolvent.Soluteisthedissolvedsubstanceand
solventisthesubstanceinwhichthesoluteisdissolved.Asolutecanbeasolidora
liquid.InNaOHsolution,sodiumhydroxide(solid)isthesoluteandwater(liquid)is
thesolvent.Notethatthesolutebeingasolidismeasuredintermsofweight(in
grams)andthesolventwaterismeasuredintermsofvolume.Thisisanexampleof
expressingsolutioninweightpervolume(w/v)basis.

Inasolutionconsistingoftwoliquidstheconcentrationisexpressedinavolumesper
volumesbasis.Forexampletheconcentrationofalcoholinwineisexpressedas
volumepervolume.A12%alcoholwinemeansitcontains12mlofalcoholper100ml
ofwine.

Generally,inmanysolutions,theweightisgiveningramsandvolumeisgivenin
millilitersorliters.Atthispoint,itisimportanttoestablishtherelationbetweenthe
unitsofweightandvolume.Onekilogram(weight)ofwateratatemperatureof
maximumdensityandundernormalatmosphericpressurehasthevolumeofoneliter.
Thismeansthatonekilogram(weight)ofwaterequalsoneliterofvolume,andone
gramofwaterbyweightequalsonemilliliterofwaterbyvolume.Thustheunitsof
weight(gram)andvolume(ml)aresimilarandinterchangeable.

Thechemistexpressestheconcentrationofasolutioninvariousways.Thecommon
expressionsincludePercent,Partspermillion(ppm),MolarandNormal.Itis
importanttohaveaclearunderstandingoftheseterms.
Percent

Oneofthesimplestformsofconcentrationisthepercent.Thissimplymeansunitsper
100units,orpartsper100parts.Thepercentconcentrationcanbeusedinthreeways.
Itcanbeweightperweight,volumepervolumeorweightpervolumebasis.

WhenwinemakersuseBrixhydrometertomeasuresugarsingrapejuicetheyare
essentiallymeasuringgramsofsugarper100gramsofjuice.Ajuicesampleof18Brix
means18gramsofsugarper100gramsofjuiceorcommonlyreferredas18%.In
describingthealcoholcontentofawine,percentalcoholcontentisexpressedinterms
ofavolumepervolumebasis.Inmanycases,includinginalaboratory,asolutionis
madebydissolvingasolidinaliquid,usuallywater.Insuchacasetheconcentrationis
expressedinaweightpervolumebasis.
Parts per million

Whendealingwithaverysmallamountofasubstanceinsolution,theconcentrationis
oftenexpressedintermsofpartspermillion.A20ppmconcentrationmeans20parts
ofsolutedissolvedforevery1,000,000partsofsolution.Theunitofmeasurementcan
beweightorvolume.Generallytheppmconcentrationisusedtoindicatemilligramsof
soluteperliterofsolution.
Molar solution

Amolarsolutionimpliesconcentrationintermsofmoles/liter.Onemolar(IM)
solutionmeansonemoleofasubstance(solute)perliterofsolution.Amolemeans
grammolecularweightormolecularweightofasubstanceingrams.Sothemolecular
weightofachemicalisalsoitsmolarweight.Tocalculatethemolecularweightone
needstoaddtheatomicweightsofalltheatomsinthemolecularformulaunit.For
examplethemoleculeofNaOHconsistsofoneatomeachofsodium(Na),oxygen(0),
andhydrogen(H).Theirrespectiveatomicweightsare:Na23,016andH1,sothe
molecularweight,is23+16+I=40.Thus40gramsofNaOHequalsonemoleof
NaOH,anda1molarsolutionofNaOHwillcontain40gramsofNaOHchemical.
Normal solution/Normality

Theotherformofconcentrationusedrelativelyfrequentlyisnormality,orN.
Normalityisexpressedintermsofequivalentsperliter,whichmeansthenumberof
equivalentweightsofasoluteperliterofasolution.Thetermnormalityisoftenused
inacidbasechemistry.Theequivalentweightofanacidisdefinedasthemolecular
weightdividedbythenumberofreactinghydrogensofonemoleculeofacidinthe
reaction.
Understandingequivalentsrequiresknowingsomethingabouthowareactionworks,
solet'sstartthere.Belowisabasicequationforanacidandabase.

HCI+NaOH>NaCl+H20
or
Acid+base>salt+water

Inoursimpleequationaboveyoucanseewehavetheacidandbasereactingtoforma
saltandwater,andthattheyreactequally.Theacidgives1H+foreveryOHgivenby
thebase.SoforeverymoleofH+oneneedsamoleof

OH.Thisreactionisonetoonereactiononamolarbasis.Onemoleofacidhasone
reactingunitandonemoleofbasealsohasonereactingunitthusbothacidandbase
has,intheaboveexample,equal1:1reactingunits.Asstatedabove,foracidswedefine
anequivalentweightasthemolecularweightdividedbythenumberofH+donated
permolecule.Above,theHCIgaveup1H+(proton)tothereaction.

MolecularweightofH2SO4=98.08g=49.04gramsperequivalent
#ofprotonsgiven2protons

Normalityisthemolecularweightdividedbythegramsperequivalent(allthisresults
inthenumberofequivalents)inagivenvolume.Foran1Nsolutionweneed1
equivalent/liter.Forhydrochloricacid(HCl)theequivalentweightis36.46grams.
Therefore,formakingan1Normalsolution,36.46g/literofHC1isneeded.Notethata
1Msolutionisalso36.46g/L.Formoleculesthatcangiveofforacceptonlyone
protonpermolecule,theNormalityisequaltotheMolarity.

Table1.MolecularandEquivalentweightsofsomecommoncompounds.

Inthecasewhereamoleculecangiveofforacceptmorethanoneproton,youneedto
adjustyourcalculation.Forexample,sulfuricacidwithaformulaofH2SO4donates2
separateprotons.Usingthemolarmassofsulfuricacid,andknowingthatone
moleculecandonate2protonswecanfindtheequivalentweight.
Withamolarmassof98.08grams,asolutioncontaining98.08gin1literwouldhave
aMolarityof1MandaNormalityof2N.ThisisbecauseeveryImoleofsulfuricacid
(H2SO4)has2molesofH+atoms.

Table1liststhemolecularweightsandequivalentweightsofimportantacidsand
basesusedinawinelaboratory.
Making 1 N solution of NaOH

Fromthediscussionabove,itshouldbeclearthattomake1Normalsolutionweneed
toknowthe,equivalentofNaOH,whichiscalculatedbydividingMolecularweightby
1,thatis40dividedby1=40.SotheequivalentweightofNaOHis40.Tomake1N
solution,dissolve40.00gofsodiumhydroxideinwatertomakevolume1liter.Fora
0.1Nsolution(usedforwineanalysis)4.00gofNaOHperliterisneeded.
Standardization

Beforewebegintitratingthatwinesamplewehaveonemoreimportantstep,
standardizationofNaOHsolution.Standardizationsimplyisawayofcheckingour
work,anddeterminingtheexactconcentrationofourNaOH(orother)reagent.Maybe
ourdilutionwasinaccurate,ormaybethebalancewasnotcalibratedandasaresult
thenormalityofoursodiumhydroxidesolutionisnotexactly1Nasweintended.So
weneedtocheckit.ThisisachievedbytitratingtheNaOHsolutionwithanacidof
knownstrength(Normality).Generally0.1NHCIisusedtotitratethebase.The
reagent,0.1NHCIsolutionispurchasedfromachemicalsupplierthatiscertifiedin
concentration.Thatmeansitwasstandardizedtoabaseofknownconcentration."But
isn'tthatgoingincircles?"youask.No,becauseacidsarestandardizedtoapowdered
basecalledKHP,orpotassiumhydrogenphthalate.Thiscanbeveryaccurately
weighedoutbecauseitisafinepowder,andthenistitratedwiththeacid.

TostandardizeNaOH,startbypipetting10.0mlof0.1Nhydrochloricacid(HC1)into
aflask.Addapproximately50mlofwater(remember,nottapwater)andthreedrops
ofmethylredindicator.Filla25mlburetwiththe0.1Nsodiumhydroxidesolution
andrecordtheinitialvolume.Titratethehydrochloricacidtothepointatwhicha
lemonyellowcolorappearsandstaysconstant.Recordthefinalvolume.

SubtracttheinitialvolumefromthefinaltoyieldthevolumeofNaOHused,andplug
thatintotheequationbelow.

NormalityofNaOH=VolumeofHCIxNormalityofHCI
VolumeofNaOHused
Titration Techniques

Beforeconqueringvolumetricanalysistotally,weneedtodiscusssometitration
techniques.Firstofall,handletheburetwithcare.Avoiddamagingthetipandpetcock
assemblybecausedamageandleaksintheseareascanandwillalterperformance.
Also,besuretoalwaysrecordyourfinalandinitialvolumereadingsaccuratelyby
readingthebottomofthemeniscusofthesolution.Don'ttrytosqueezeinthatlast
sampleanddraintheburetpastitslowestmarktakethetimetorefillitproperly.For
helpinreadingaburet,takeawhiteindexcardandcolorablacksquareonitas
shown.Holdthisbehindtheburetscalewhentakingreadingstoaidinseeingthe
meniscus.Someburetsactuallycomewithastripepaintedonthemforthisreason.

Next,remembertostiryoursampleasyoutitrate.Whetherusingastirplate
(recommended)orstirringbyswirlingtheflaskmanually,itisimperativethatthe
solutionbemixed.Besurenottosloshthesampleoutsideofthebeaker/flaskand
don'tallowtheburet'scontentstofalloutsideofthebeaker.Also,loweryourburet
enoughsothatsplatterfromthesampledoesnotexittheflaskasyoutitrate.Thisis
notonlybadlabpracticebutcanalsobedangerous.

Safetyisanimportantconsiderationwhenworkingwithburets,acidsandbases.
Realizethatyouarehandlingcorrosivechemicalsanddelicateglassware,treatitlike
anirreplaceablewineinthedaintiestglass.Thatmeansdeliberatelyandwithrespect.
Wearsafetyglassesandalabcoatatleast,andglovesarealsorecommended.When
fillingaburet,takeitoutofthestandandholditatananglewiththetipabovethe
sink.Thatwayanyspillswilldrainintothesinkandyoucanstandsafelyonthefloor,
notastool.Leaningovertheburetwhileitisonthebenchtopisdangerous.

Besuretohaveaccesstoaneyewashstationorsomethingthatcansupplyastreamof
watertoyourbodyand/oreyesfor15minutes,theOSHArecommendedtreatmentfor
chemicalspillstotheeyesandbody.Rememberyouwillhavesodiumhydroxideinthe
buretatandaboveeyelevelsomakesureyourequipmentisattachedtoasteadybase.

Goodlaboratorypracticescanhelpyoumonitorthequalityofyourwinesmore
accuratelyandefficiently.Volumetricanalysisbytitrationisoneofthemostcommon
techniquesthewinemakeremploystoanalyzehisproduct.Improvingyourskillsin
thisareaisimportantinthequestforexcellentwinesonaconsistentbasis.

*PreviouslypublishedinVineyardandVintageView,MountainGrove,MO.

Category: Enology
Tags: wine,winemaking,chemistry

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