SAHAN SATHARASINGHE

Sulphatesolubility
Ifasolutionofanysulphateisaddedtoasolutionofagroup2metalcompoundthenaprecipitateislikely.
Group2ioninsolution Effectofaddingasulphatesolution
Mg2+

Noprecipitate,MgSO4issoluble

Ca2+

WhiteprecipitateofCaSO4

Sr2+

WhiteprecipitateofSrSO4

Ba2+

WhiteprecipitateofBaSO4

Hydroxidesolubility
Ifsodiumhydroxideisaddedtoasolutionofagroup2compoundthenaprecipitateislikely.
Group2ioninsolution Effectofaddingahydroxidesolution
Mg2+

FaintwhiteprecipitateofMg(OH) 2

Ca2+

FaintwhiteprecipitateofCa(OH)2

Sr2+

FaintwhiteprecipitateofSr(OH) 2onstanding

Ba2+

Noprecipitate,Ba(OH)2issoluble

Heatingcarbonatesandnitrates
Substance

Effectofheat

Lithiumandallgroup2carbonates Carbondioxidedetected
Sodiumandpotassiumcarbonates

Noeffect(exceptwaterofcrystallisationmaybegiven
off)

Sodiumandpotassiumnitrates

Oxygenonlygasevolved

Lithiumandallgroup2nitrates

Nitrogendioxideandoxygenevolved

Actionofheatoncompounds

CarbonatesCarbondioxideisgivenoff.

HydrogencarbonatesCarbondioxideandwaterformed.

Group1nitratesNitriteandoxygenformed.

Group2nitratesOxide,brownfumesofnitrogendioxideandoxygenformed.

Distinguishingbetweenhydrocarbons
Alkane:Burn/oxidise/combustthem.TheywillburnwithayellowflameandformCO 2 andH2O(limited

supplyofCO).
Alkene:Ayellow,sootierflameisproduced(duetotheextracarbonandhigherratioofcarbon:hydrogen).

Identifyingsomefunctionalgroups
AlkeneAddtoorangebrominewater.Thealkenewilldecolouriseit.
HalogenalkaneHeatwithsodiumhydroxidesolution.Acidifywithdilutenitricacidandthentestwithsilver

nitratesolutionaswithinorganichalides.
AlcoholsorcarboxylicacidscontainingCOHInadrytesttube(i.e.dryalcohol),addPCl 5.Mistyfumesof

HClareproduced,whichturnsbluelitmuspaperred.
Distinguishingbetweendifferentclassesofalcohol
PrimaryAddPCl5.Warmitwithaqueouspotassiumdichromate(K 2Cr2O7)anddiluteH2SO4.Mistyfumesaregiven
offandthecolourchangedfromorangetogreenaldehyde.
SecondaryMistyfumes,changestogreenketone.
TertiaryMistyfumes,nocolourchange.
Specification
f)interpretquantitativeandqualitativeresults

g)deviseandplansimpleexperimentsbasedonthechemistryandtechniquessummarisedinatoeaboveNormally
thelastquestiononthepaper.Itwillaskyoutoidentifycertaincompoundsfromfour.
E.g.titrations,howtomakeastandardsolution,howtotitrate,identifyQCO3whenheatingitwhereQisagroup2
metalion.

h)evaluateerrorinquantitativeexperiments

j)Commentonsafetyaspectsofexperimentsbasedonsupplieddataorrecallofthechemistryofthecompounds
listedinUnitsland2.Safetyconsiderationsshouldrelatetospecificexperimentsnotbeofageneralnatureitwillbe
assumedthatstudentsweareyeprotectionduringallpracticalwork.

Halogensaretoxicandharmfulbyinhalation,althoughiodineismuchlesssothanchlorineorbromine,becauseitisa
solid.Chlorineandbrominemustalwaysbeusedinafumecupboard.Liquidbrominecausesseriousburnsanmustbe
handledwithgloves.
Ammoniaistoxic.Concentratedammoniasolutionsshouldbehandledinthefumecupboard.
Concentratedmineralacidsarecorrosive.Ifspiltonthehands,washingwithplentyofwaterisusuallyenough,but
advicemustbesought.Acidintheeyerequiresimmediateattentionandpromptprofessionalmedicalattention.
Bariumchloridesolutionandchromatesanddichromatesareextremelypoisonousandsoshouldbeusedinthefume
cupboard/shouldnotbeinhaled.
Sodiumorpotassiumhydroxideorconcentratedammoniaintheeyeisextremelyseriousandmustalwaysreceive
professionalandimmediateattention.Sodiumhydroxideandotheralkalimetalhydroxidesareamongstthemost
damagingofallcommonsubstancestoskinandothertissue.Weargloves,gogglesandanapronwhenhandlingthese
solutionsinhighconcentrations.
Generalsafety

Toxic/carcinogenicusegloves,fumecupboard

FlammableWaterbaths,nonakedfumes.

HarmfulgasesUsefumecupboard

Corrosiveweargoggles/gloves

Spillageofconcentratedacidwashwithplentyofwater.

TESTS
Ion
Carbonate

Formula

Test

CO32

Test1
Heatthesolidinatesttubewitha
Bunsenburner.

Observations
Limewatershouldturnfrom
colourlesstocloudyinthepresence
ofcarbondioxidedueto
precipitationofcalciumcarbonate.

Itshoulddecomposeproducingthe
oxideandcarbondioxide.E.g.
CuCO3(s)=CuO(s)+CO2(g)
Testforthegasusinglimewater
solution.
Test2
AdddiluteHCltothesolid.
Testforthegasevolvedusing

Vigorouseffervescence.
Limewatershouldturnfrom
colourlesstocloudyinthepresence

limewatersolution.

ofcarbondioxidedueto
precipitationofcalciumcarbonate.

Hydrogencarbonate

HCO3

Test
Addcalciumchloridetoa
hydrogencarbonatesolution.

Noprecipitateformssincecalcium
hydrogencarbonateissoluble.

Sulphate(VI)

SO42

Test
Addbariumchloridesolution
acidifiedwithdiluteHCltothetest
solution.

Whiteprecipitateofbariumsulphate
forms.

Sulphite

SO32

Test
WarmthesulphitewithdiluteHCl.
Testforgasesusingacidified
potassiumdichromate(VI)solution
(orpaper)

Thesolutionturnsgreen.

Chloride

Cl

Test1
Addconcentratedsulphuricacidto
thesolidchloride.

Whitesteamyacidicfumesareseen
HClfumes.

Test2
Adddilutenitricacidtoasolutionof
achloridetoacidifythesolution.
Thiseliminatesanycarbonatesor
sulphites.
Addsilverchloridetothesolution.
Adddiluteammoniasolution.
Bromide

Br

Test1
Addconcentratedsulphuricacidto
thesolidbromide.
Test2'
Adddilutenitricacidtoasolutionof
abromidetoacidifythesolution.
Thiseliminatesanycarbonatesor
sulphites.
Addsilverchloridetothesolution.
Addconcentratedammoniasolution.

Iodide

WhiteprecipitateofAgClforms.
Soliddissolves.

Steamybrownishacidicfumesare
seen.

CreamprecipitateofAgBrforms.
Soliddissolves.

Test1
Addconcentratedsulphuricacidto
thesolidiodide.

Purpleacidicfumesareseen.The
mixtureturnstoabrownslurry.

Test2
Adddilutenitricacidtoasolutionof
aiodidetoacidifythesolution.This
eliminatesanycarbonatesor
sulphites.

YellowprecipitateofAgIforms.

Addsilverchloridetothesolution.

Solidisinsoluble.

Addconcentratedammoniasolution.
Nitrate

NO3

Test1
Heatsolidnitrate.
Ifgroup1solid(notLi)thenwill
decomposetogivethenitriteand
oxygen.
Allothersolidnitratesdecomposeto
givethemetaloxide,nitrogen
dioxideandoxygen.
Test2
Boilnitratesolutionwith
aluminium/Devardasalloy,in
sodiumhydroxidesolution.
Testvapourwithredlitmuspaper.

Ammonium

Lithium

NH4+

Li+

Test
Warm ammonium compound with
NaOH.
Test vapours immediately using
dampredlitmuspaper.

Oxygengasisevolvedthatwill
relightaglowingsplint.
Browngasisseen(NO2).Oxygen
gasisalsoevolvedandwillrelight
aglowingsplint.

Litmuspaperturnsblueinthe
presenceofammonia.

NH3
turnsthelitmuspaperblue.

Test
DipnichromewireinHCl.
Acarmineredflameisseen.

Dipwireinsolid.
Heatwireincentreofflame.
Observecolourofflame.
Sodium

Na+

Test
DipnichromewireinHCl.
Dipwireinsolid.

Ayellowflameisseen.

Heatwireincentreofflame.
Observecolourofflame.
Potassium

K+

Test
DipnichromewireinHCl.

Alilacflameisseen.

Dipwireinsolid.
Heatwireincentreofflame.
Observecolourofflame.
Magnesium

Mg2+

Test
AddNaOHsolutiontothe

Awhitesolidformswhichis
insolubleinexcessNaOH(aq).This

Ca2+

Calcium

magnesiumsolid.

isMg(OH)2(s)

Test
DipnichromewireinHCl.

Abrickredflameisseen.

Dipwireinsolid.
Heatwireincentreofflame.
Observecolourofflame.
Sr2+

Strontium

Test
DipnichromewireinHCl.

Acrimsonredflameisseen.

Dipwireinsolid.
Heatwireincentreofflame.
Observecolourofflame.

Ba2+

Barium

Test
DipnichromewireinHCl.

Aapplegreenflameisseen.

Dipwireinsolid.
Heatwireincentreofflame.
Observecolourofflame.
TESTS
Name

Formula

Test

Observations

Hydrogen

H2

Ignitegas.

Squeakypopisheard.

Oxygen

O2

Placeaglowingsplintinasampleof
thegas.

Theglowingsplintrelights.

Carbon
dioxide

CO2

Bubblegasthroughlimewater
(saturatedsolutionofcalcium
hydroxide)

Asolutionturnsfromcolourlesstocloudy.A
white(milky)precipitateofcalcium
carbonateformswhichissparinglysoluble.

Ammonia

NH3

Testforgasusingdampredlitmus
paper.

Litmuspaperturnsblue.

Chlorine

Cl2

Test1
Testforgasusingdamplitmuspaper
(redorblue)

Chlorinebleachesthelitmuspapervery
quickly.

Test2
Testforgasusingmoiststarch
iodidepaper.

Thepaperturnsblueblack.

Test3
Passgasthroughasolutionofa
bromide.

Thesolutionturnsfromcolourlesstoorange.

Test4
Passgasthroughasolutionofan
iodide.

Thesolutionturnsfromcolourlesstobrown
(possiblywithablackprecipitate,iodine).

Nitrogen
dioxide

NO2

Notmanytestsforthisgas.

Thegasisbrown.

Sulphur
dioxide

SO2

Test1
Bubblegasthroughasolutionof
potassiumdichromate(VI)dissolved
insulphuricacid.

Thesolutionturnsfromorangetogreen.

Test2
Bubblegasthroughasolutionof
potassiummanganate(VII)dissolved
insulphuricacid.

Thesolutionturnsfrompurpletocolourless.

Volumetricanalysis
Volumetricanalysis(titration)involvesthereactionbetweentwosolutions.Foronesolution,boththevolumeandthe
concentrationareknown;fortheother,thevolumeonlyisknown.Apparatususedincludesaburette,apipetteanda
volumetricflask.
Whatisastandardsolution?
Asolutionforwhichconcentrationisaccuratelyknown.Theconcentrationmayhavebeenfoundbyaprevious
titrationorbyweighingthesoluteandmakingasolutionofknownvolume.Suchasolutionisaprimarystandard
solution.
Howisa250cm3standardsolutionprepared?

Makesurethatthebalanceiscleananddry.Wipeitwithadampcloth.

Placetheweighingbottleonthepanandtarethebalance(i.e.rezeroit)

Takethebottleoffthebalanceandaddsolidtoit.Thisensuresthatnospillagesfallonthepan.

Whenyouhavetherequiredamount,writeitsvaluedownimmediately.

Replaceonbalance,andiftherequiredamountisadded,withdrawthemass.

Washouta250cm3volumetricflaskthreetimesusingpurewater.

Transferthesolidtoa250cm3volumetricflaskusingafunnel,andwashouttheweighingbottleintotheflask
throughthefunnel.

Addabout100cm3ofdistilledwatertotheflask.

Stirthesolutionusingaglassrod.

Washallremainingapparatusincludingtheglassrod,funnelandtransfertherestofthistotheflask.

10

Makeupto250cm3withdistilledwatersothatthebottomofthemeniscusjusttouchesthe250cm3mark.

Stoppertheflask.

Shaketheflaskvigorouslyand/orinverttheflask5or6timestodissolvethesolid.

Concentrationofsolution=massofsolidused/molarmassofsolidx1000/250(unitsmoldm3)

Usingthepipette

Aglassbulbpipettewilldeliverthevolumestatedonitwithinacceptablelimitsonly.

Usingapipettefiller,drawalittleofthesolutiontobeusedintothepipetteandusethistorinsethepipette.

Fillthepipettetoabout23cm3abovethemark.Pipettefillersaredifficulttoadjustaccurately,soquickly
removethefillerandclosethepipettewithyourforefinger(notthumb).Releasethesolutionuntilthebottom
ofthemeniscusisonthemark.

Immediatelytransferthepipettetotheconicalflaskinwhichyouwilldothetitration,andallowthesolution
todispenseundergravity.

Usingtheburette

Makingsurethatthetapisshut,addabout1015cm3oftheappropriatesolutiontotheburetteandrinseitout,
notforgettingtoopenthetapandrinsethejet.

Closethetapandfilltheburette.Asmallfunnelshouldbeusedtoaddthesolutionbutbecarefulnotto
overfillthefunnel.

Removethefunnel,becausetitratingwithafunnelintheburettecanleadtoseriouserrorifadropofliquidin
thefunnelstemfallsintotheburetteduringthetitration.

11

Bringthemeniscusontothescalebyopeningthetaptoallowsolutiontopassthroughtheburette.Thereisno
particularreasontobringthemeniscusexactlytothezeromark.

Makesurethattheburetteisfulltothetipofthejet.

Afterasuitableindicatorhasbeenaddedtothesolutionintheconicalflask,swirltheflaskundertheburette
withonehandwhilstadjustingtheburettetapwithyourotherhand.

Addthesolutionintheburettetotheconicalflaskslowly,swirlingtheflaskallthetime.

Astheendpointisapproached,theindicatorwillchangecolourmoreslowly.Thetitrantshouldbeaddeddrop
bydropneartotheendpoint.

Repeatthetitrationuntilyouhavethreeconcordanttitres,i.e.volumesthataresimilar.Thismeanswithin
0.2cm3orbetterifyouhavebeencareful.Takingthemeanofthreetiresthatdifferby1cm3ormoreisno
guaranteeofanaccurateanswer.

12

Commonindicators

Methylorangeyellowinalkali,redinacid(orangeatendpoint)

Phenolphthaleinpinkinalkali,colourlessinacid.

Enthalpychangemeasurements

Weighaspiritlamp(containingaliquidalcohol)usingabalanceaccurateto3decimalplaces.Recordthe
massmeasured.

Useameasuringcylindertoput100cm3ofdistilledwaterintoasmallbeakerandclampsthisatafixed
heightabovethespiritlamp(about2cm).

Recordtheinitialtemperatureofthewaterusingathermometer.

Lightthelampusingaburningsplint.

Heatthewaterusingthespiritlampuntilthetemperaturehasgoneupbyabout10C.Stirthewaterwiththe
thermometerthewholetime.

Putacaponthespirittostopthealcoholburning.Thelidstopsalsostopsfurtherevaporationoftheliquid
alcohol.

Reweighthespiritlampandrecordthemass.

Calculatetheenthalpychange

Possiblesourcesoferror

13

Theremaybeheatlossduetotheapparatususedandheatmayhavedissipatedthroughtheinsulatingmaterial
shoulduseapolystyrenecupandinsulationlikealid.

Thespecificheatcapacityanddensityofwaterareused(andnotofHCl).

Themassesofsolidaddedtotheacidareignored.

Itisassumedthatthespecificheatcapacityofthepolystyrenecupisnegligible.

Someheatislostwhenthehydrogenorcarbondioxideareevolvedinthereactions.

Manyorganicreactionsareslowandrequireprolongedheating

Toachievethiswithoutlossofliquid,reactionmixturesareheatedinaflaskcarryingaverticalcondenser.

Thisisheatingunderreflux;thesolventiscondensedandreturnedtotheflask,sothemixturecanbeheated
aslongasdesired.

Toheattheroundbottomedflask,eitheruseawaterbath,anoilbathoraheatedplatemantle.ABunsen
burnerisntreallysuitable.

Simpledistillation
Toseparateavolatilesolventfromamixture

Simpledistillationisusedwhereavolatilecomponenthastobeseparatedfromamixture,theother
componentsofthemixturebeingverymuchvolatileornonvolatile.

Themixtureisheated.

Thefractionthatboilsiscollectedwithinthetemperaturerangeofthefraction.(normally1or2degrees
beforetheboilingtemperature)

Thecondensercoolsthefractionsoitdistilsandiscollectedinthereceivingflask.

14

Fractionaldistillation
Toseparatemixturesofvolatileliquids.

RecrystallisationUsedtopurifyasolidmaterialbyremovingbothsolubleandinsolubleimpurities.The
choiceofsolventisimportant.Thesubstancemustbeeasilysolubleintheboilingsolventandmuchless
soluble at room temperature. This ensures the smallest possible loss of material, although some loss is
inevitablewiththistechnique.

Recrystallisationmethod
1. Dissolvethesolidintheminimumamountofboilingsolvent.Thisensuresthatthesolutionissaturatedwith
respecttothemainsolutebutnotwithrespecttotheimpurities,whicharepresentinmuchsmalleramounts.
2. Filterthehotmixturethroughapreheatedfilterfunnel.Thisremovesinsolubleimpurities.Thehotfunnelis
necessarytopreventthesolutecrystallisingandblockingthefunnel.Filtrationundervacuumusinga
Buchnerfunnelisoftenpreferred,becauseitisfast.
3. Coolthehotfiltrate,eithertoroomtemperatureor,ifnecessary,inabathoficedwater.Rapidcoolinggives
smallcrystals,slowcoolinglargeones.Thelargecrystalsareoftenlesspure.
4. FilterthecoldmixtureusingaBuchnerfunnel.
5. Washthecrystalswithasmallamountofcoldsolvent.Thisremovesanyimpurityremainingonthesurfaceof
thecrystals.Asmallamountofcoldsolventisusedsothatthecrystalsarentwashedaway/dontdissolve.
6. Suckthecrystalsasdryaspossibleonthefilter.
7. Transferthecrystalstoadesiccatortodry.Dryingbetweenfilterpaperissometimesrecommended,butitisa
verypoormethod.

15

16

Meltingpointdetermination
Thisisusedtodeterminethepurityoftherecrystallisationsolid.Placesmallamountofthesolidinthesealedendof
acapillarytube.Placeinthemeltingpointapparatus.Asharpmeltingpointoverasmallrangeshowspurity,when
comparedwiththesetbookvalueofahighermeltingpoint,thatindicatesanimpuresolid.

17

Organictests
Collect10cmofthesamples.
Testthesamplesinthefollowingorder
Alkenesbrominewaterdecolourisesalkene
AlcoholsSpatulaofsolidPCl5.Testfumeswithdamplitmuspaperlitmusred?Whitefumesnear

ammonia?alcohol
HalogenoalkaneAddNaOH,ethanolassolvent.Shakeandwarmfor3minutes.Coolandaddnitricacid+

silvernitrate.white=chloride;cream=bromide;yellow=iodide.Confirmwithammonia
Alkane,thesubstanceleftisthealkane.

18