Hanna Instruments HI 4102 Manual de usuario

HI 4002HI 4002

HI 4002

HI 4102HI 4102

HI 4102

Bromide Ion

SelectiveElectrode

Instruction Manual

Half-cell

Combination

BROMIDE

HI 4002

HI 4102

BROMIDE

COMBINATION

HI4002BromideHalf-cellHI4002BromideHalf-cell

HI4002BromideHalf-cell

HI 4102 Bromide Combination ElectrodeHI 4102 Bromide Combination Electrode

HI 4102 Bromide Combination Electrode

I.I.

I. Introduction:Introduction:

Introduction:Introduction:

Introduction:

The Hanna HI 4002and HI 4102 are ion selective elec-

trodes designed for the measurement of Bromide ions in

aqueous solutions. The HI 4002 is a solid state half-cell

sensorthatrequiresaseparatereference.TheHI4102isa

combinationionselectiveelectrode.

IIII

II.

SpecificationsSpecifications

Specifications

Type: SolidStateelectrodewith

aSilverBromidepellet.

Ion(s)measured: Bromide(Br--

- )

Measurementrange: 1.0Mto1X10-6M

79,910to0.08ppm

Interferingions: Cyanide, and Mercury

mustbeabsent.Ratioof

interferingiontoBr--

-must

belessthantheratio

indicated below:

0.01 forI--

-iodide

0.01 forCN--

-cyanide

50 forCl--

-Chloride

Operating Temperature: 0-80°C

Operating pH: 2-12.5pH

Dimensions: 12 mm (OD) X 120 mm

nominal insertion

(0.47”X4.72”)

Connection: BNC

III.III.

III. Theory of OperationTheory of Operation

Theory of OperationTheory of Operation

Theory of Operation:::::

TheHI4002orHI4102Bromideelectrodesarepotentio-

metricdevicesusedfortherapiddeterminationoffreeBro-

mideionsinfoodproducts,beverages,plants,soilsandas

anindicatorintitrations.Theelectrodefunctionsasasen-

sor or ionic conductor. The HI 4002 requires a separate

referenceelectrodetocompleteitselectrolyticcircuit. The

HI4102incorporates areferenceelectrode.ThesilverBro-

mide pellet is practically insoluble in the test solutions

being measured and produces a potential change due to

changesinthesample’sionactivity.Whentheionicstrength

ofthesampleisfixedbytheadditionofISA,thevoltageis

proportionalto theconcentration ofbromide ionsinsolu-

tionandtheelectrodefollowstheNernstequation.

E=Ea +2.3RT/nFlogAion

E=observedpotential

Ea=Referenceandfixedinternal voltages

R=gasconstant(8.314J/KMol)

n= Chargeonion(1-)

A i=ion activity in sample

T=absolutetemperature inK

F=Faradayconstant(9.648x104C/equivalent)

IV.IV.

IV. Design elements of the HI 4002 and HI 4102Design elements of the HI 4002 and HI 4102

Design elements of the HI 4002 and HI 4102Design elements of the HI 4002 and HI 4102

Design elements of the HI 4002 and HI 4102

electrodeselectrodes

electrodes

BROMIDE

HI 4002

Cap

Sensing

Membrane

Sensor

Handle

UpperCap

Spring

O-Ring

CeramicJunction

onInnerStem

FillHole

O-Ringand

Plug

Sensing

Membrane

OuterSleeve

Upper

Threads

Liquidjunction

V.V.

V. Equipment required:Equipment required:

Equipment required:Equipment required:

Equipment required:

•HannaHI5315DoubleJunctionReferenceElectrode

withHI7072FillSolutionforHI4002.

•Hanna HI 4222 pH/ISE/mV meter or other suitable

ionorpH/mVmeter.(Note:log/lineargraphpaperis

usefulifan ISE(ion) meteris notavailable).

•HannaHI180MagneticStirrerorequivalentwithTFE

coatedstirringbars(HI731320). Note:isolatebea-

kers from stirrer motor heat by placing insulating

materialsuchasfoamorcorkbetweenthem.

•HannaHI76404ElectrodeHolderorequivalent.

•Plasticbeakers(HI740036P)orothersuitablemea-

surementvessel.

VI.VI.

VI. Solutions RequiredSolutions Required

Solutions RequiredSolutions Required

Solutions Required for Bromide Measurementsfor Bromide Measurements

for Bromide Measurementsfor Bromide Measurements

for Bromide Measurements

0.1M BromideStandard,500mL HI4002-01

ISA,500mL HI4000-00

ForMolarsolutions:

Usingvolumetricpipettesandglasswaremakeserialdilu-

tions to approximately bracket the concentration of the

samples. Standardswithconcentrations <10-3Mshould

be prepared daily.

TwomLofHannaISAforHalideelectrodes (HI4000-00)

shouldbe addedto 100mLof sampleorstandard.

Forppmsolutions:

Prepare 799 ppm bromide standard by diluting HI4002-

01:Pipette100mL standardtoa 1litervolumetric flask.

Adddeionizedwatertovolume.Usingadditionalvolumet-

ricpipettesandglasswaremakeserialdilutionsofthis799

ppm standard to approximately bracket the concentration

ofthesamples. Standardswithconcentrations<80ppm

should be prepared daily.

TwomLofHannaISAforHalideelectrodes (HI4000-00)

shouldbe addedto 100mLof sampleorstandard.

VIIVII

VII. General GuidelinesGeneral Guidelines

General GuidelinesGeneral Guidelines

General Guidelines

•Calibration standards and sample solutions should

havethesameionicstrength.ISAshouldbeaddedto

bothsamplesandstandardsinthesameratio.1part

ISAto50partsstandardisthenormaldosing.

•Concentrated samples (>1 M) should be diluted

beforemeasurement. Multiplythefinalresultbythe

correspondingdilutionfactor.

•For high ionic strength samples, prepare standards

with similar ionic strength by increasing the ISA

addiiton.

•Calibration standards and sample solutions should

beatsametemperature.

•The magnetic stirrer may generate heat. Thermally

insulate beaker containing standard or sample from

magnetic stirrer by placing cork or other insulative

sheetbetweenbeakerandstirrerplate.

•Calibration standards and sample solutions should

be stirred at the same rate using identical sized TFE

coatedstirbars.

•Rinseelectrodepairwithdistilledordeionizedwater

between samples and gently dab dry with soft dis-

posableabsorbenttoweling.Donotrubelectrodes.

•Presoaking bromide sensor in a dilute standard will

optimizeresponse.Useconcentrationsapproximately

10-3Morless.

•A scratched, pitted, or tarnished pellet surface can

causedrift,alossoflowlevelresponse,orpoorrepeat-

ability. Optimumresponsecanberestoredbyremov-

ingthedamagedsurfacewiththemicroabrasivestrip

HI4000-70.

•Avoidlargechanges intemperature (thermalshock)

asit maydamagethesensor.

•Gasbubblesmayformfromsolutionout-gassingdue

totemperaturechange. Gentlytapbodyofsensorto

dislodgethem frommembranesurface.

HI4002

•Removeprotectivecoverfromsensortip.

•PrepareHI5315referenceelectrodebyfillingelectro-

lytereservoirwithHI7072fillsolution.

•Place sensor and reference electrodes into electrode

holderandconnectcableconnectorstometer.

HI4102

•Remove the protective plastic wrap that covers the

ceramicjunctionbeforeassemblingsensorforthefirst

time.

•HI7072referencefillsolutionshouldbeaddeddaily

toelectrolytereserviorbeforeelectrodeuse.

•During measurement always operate electrode with

thefillholeopen.

•Duringnormal use,fill solutionwillslowlydrainout

ofthetaperedconejunctionatthelowerportionofthe

electrode.Excessiveloss(>4cmdropwithin24hours)

isnotnormal.Ifthisoccursverifycapistightenedand

the interface between the internal cone and outer

bodyisfreeofdebris.

•Addfillsolutiondailytomaintainagoodheadpres-

sure.Foroptimumresponse,thislevelshouldbemain-

tainedandnotbeallowedtodropmorethan2-3cm

(1-inch) below fill hole. It must cover the ceramic

foundontheinnerstem.

•Ifanerraticmeasurementoccurs,checktoseeiffor-

eign matter is seen trapped near the internal cone.

Drainand refillwith freshfill solution.

VIII.VIII.

VIII. Electrode PreparationElectrode Preparation

Electrode PreparationElectrode Preparation

Electrode Preparation

HI4002

1. Removeprotectivecoverfromsensortip.

2. Preparereferenceelectrodebyfillingouterelectrolyte

reservoirwithHI7072.

3. Place sensor and reference electrodes into electrode

holderandconnectcableconnectorstometer.

HI4102

1. Unwrapplasticfilmsealfoundoverceramicjunction

oninnerstemanddiscard.Thisisonlyusedforship-

ping and long term storage.

2. Rinseinnerstemwithdeionizedwatermakingcertain

towettheo-ringfoundontheinnerstem.

3. Reassemble electrode by gently pushing the inner

assembly into the outer body, sliding spring down

cable, and screwing cap into place.

4. Removefillholecoverando-ringonfillholespout.

5. Usingthedropperpipetteprovided,addafew drops

HI7072fillsolutionto theelectrode,wetting theo-

ring and rinsing out the fill solution chamber.

Deionized

Water

Remove

Parafilm

6. Holdingthebodyoftheelectrodegentlypress upper

capwithyourthumb.Thispermitsthefillsolutionto

drain out of the body. Release cap and verify elec-

trodereturnstoitsoriginalposition.(Youmayneedto

gentlyassistforthistooccur).

7. Tightentheelectrodecapontothebodyandfillelec-

trodebodyuntilfillsolutionvolume isjustbelowfill

hole.

8. Position electrode in a Hanna HI 76404 electrode

holder (orequivalent)andconnect plugto meter.

HI 4102

BROMIDE

COMBINATION

IX.IX.

IX. Quick Check of Electrode SlopeQuick Check of Electrode Slope

Quick Check of Electrode SlopeQuick Check of Electrode Slope

Quick Check of Electrode Slope

•ConnectsensorstopH/mV/ISEmeter

•PlacemeterinmVmode.

•Place100mLofDIWintoabeakerwithstirbar.

•Placeelectrodesintopreparedsample.

•Add 1 mL of a standard (0.1 M or 1000 ppm stan-

dard)tobeaker.RecordthemVvaluewhenstable.

•Addanadditional10mLofstandardtothesolution.

Record the mV when reading has stabilized. This

value should be less than the previous noted (more

negative).

•DeterminethedifferencebetweenthetwomVvalues.

Anacceptablevalueforthisslopeis-56±4mV.

X.X.

X. Corrective actionCorrective action

Corrective actionCorrective action

Corrective action

•Verifyprotectivecaphasbeenremoved(HI4002).

•Verifyplasticfilmhasbeenremovedfrominnerstem

(HI4102).

•Verifyelectrodesareconnectedproperlytometerand

meterispowered.

•Verify dilute standards are freshly made and stored.

Remakesolutionsifappropriate.

•If the sensor slope just misses the suggested slope

window,soakingthesensorinadilutestandardmay

solvethe problem.(<10-3Mbromide or <80ppm

standard).

•A scratched sensing surface can be polished with HI

4000-70 polishing strip. Cut off approximately 1

inchofthemicro-abrasivestrip.Wetthefrostedside

with deionized water and place against damaged

membraneoftheelectrode. Placeyourthumbagainst

the shiny backing and slowly rotate back and forth

while applying gentle pressure. Continue polishing

untilyouaresatisfiedwiththesurface. Ifdarkdepos-

itsappearon polishingstrip movethepaperslightly

and continue polishing.

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