Hanna Instruments HI 4107 Manual de usuario

HI 4007HI 4007

HI 4007

HI 4107HI 4107

HI 4107

Chloride Ion

SelectiveElectrode

Instruction Manual

CHLORIDE

HI 4007

HI 410

COMBINATION

CHLORIDE

Half-cell

Combination

HI4007ChlorideHalf-cellHI4007ChlorideHalf-cell

HI4007ChlorideHalf-cell

HI 4107 Chloride Combination ElectrodeHI 4107 Chloride Combination Electrode

HI 4107 Chloride Combination Electrode

I.I.

I. Introduction:Introduction:

Introduction:Introduction:

Introduction:

The Hanna HI 4007and HI 4107 are ion selective elec-

trodes designed for the measurement of chloride ions in

aqueous solutions. The HI 4007 is a solid state half-cell

sensorthatrequiresaseparatereference.TheHI4107isa

combinationionselectiveelectrode.

IIII

II.

SpecificationsSpecifications

Specifications

Type: SolidStateelectrodewith

aSilverChloridepellet.

Ion(s)measured: Chloride(Cl-)

Measurementrange: 1.0Mto5X10-5M

35,500to1.8ppm

Interferingions: Cyanide,andMercuryions

mustbeabsent.RatioofinterferingiontoCl-mustbeless

thanthe ratio indicated below:

1.0 forl-iodide

3.5 forBr-bromide

forCO32- carbonate

1.0 forOH-hydroxide

0.01 forS2O3

2- thiosulfate

Operating Temperature: 0-80°C

Operating pH: 2-11pH

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:::::

TheHI4007orHI4107chlorideelectrodesarepotentio-

metricdevicesusedfortherapiddeterminationoffreechlo-

rideionsingroundwater,boilerwateranddrinkingwater.

Theelectrodefunctionsasasensororionicconductor. The

HI4007requiresaseparatereferenceelectrodetocomplete

itselectrolyticcircuit. TheHI4107hasareferenceelectrode

incorporatedinitsdesign.Thesilverchloridepelletisprac-

tically insoluble in the test solutions being measured and

producesapotentialchangeduetochangesinthesample’s

ionactivity.Whentheionicstrengthofthesampleisfixed

by the addition of ISA, the voltage is proportional to the

concentrationofchlorideionsinsolutionandtheelectrode

followstheNernstequation.

E=Ea +2.3RT/nFlogAion

E=observedpotential

Ea=Referenceandfixedinternalvoltages

R=gasconstant(8.314J/KMol)

n= Chargeonion (-1)

A i=ion activity in sample

T=absolutetemperatureinK

F=Faradayconstant(9.648x104 C/equivalent)

IV.IV.

IV. Design elements of the HI 4007 and HI 4107Design elements of the HI 4007 and HI 4107

Design elements of the HI 4007 and HI 4107Design elements of the HI 4007 and HI 4107

Design elements of the HI 4007 and HI 4107

electrodeselectrodes

electrodes

CHLORIDE

HI 4007

Cap

Sensing

Membrane

Sensor

Handle

UpperCap

Spring

O-Ring

CeramicJunction

onInnerStem

FillHole

O-Ringand

Plug

Sensing

Membrane

OuterSleeve

Upper

Threads

Liquidjunction

V. Equipment required:V. Equipment required:

V. Equipment required:

•HannaHI5315DoubleJunctionReferenceElectrode

withHI7072FillSolutionforHI4007.

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

ionorpH/mVmeter.(Note:log/lineargraphpaperis

usefulif an ISE(ion) meter isnot available.

•Hanna HI 180 Magnetic Stirrer or equivalent with

Tefloncoatedstirringbars(HI731320). (Note:iso-

latebeakersfromstirrermotorheatbyplacinginsu-

latingmaterialsuchasfoamorcorkbetweenthem).

•HannaHI76404ElectrodeHolderorequivalent.

•Plasticbeakers(HI740036P)orothersuitablemea-

surementvessel.

VI.VI.

VI. Solutions RequiredSolutions Required

Solutions RequiredSolutions Required

Solutions Required

for Chloride Measurementsfor Chloride Measurements

for Chloride Measurements

Select appropriate Hanna Instruments standard and ISA

fromthelistbelow:

0.1MSodiumChlorideStandard,500mL HI4007-01

100ppm Chloride standard, 500mL HI4007-02

1000ppmChloridestandard,500mL HI4007-03

ISA,500mL HI4000-00

Usingvolumetricpipettesandglasswaremakedilutionsto

brackettheconcentrationofthesamples. Standardswith

concentrations <10-3 M (35.5 ppm) should be prepared

daily.

TwomLofHanna ISAforHalideelectrodes(HI4000-00)

shouldbeaddedto100mLofsampleorstandard.

A user prepared acetate pH buffer may also be used to

adjustsamplestoapproximately4pH. Add10mLper100

mL sample or standard. Prepare 250 mL by dissolving

19.5 g ammonium acetate and 15.0 mL glacial acetic

acid in 200 mL deionized water and diluting to volume.

Auser supplied oxidizingreagent may be used tosupress

interferences such as hydroxide, sulfide, bromide, ammo-

niaorcyanide. Add10mLto100mLstandardorsample.

Permitsampletomix10minutesbeforemeasurementsare

taken. Discard samples and standards promptly as the

chloridein these will oxidizeuponstanding making them

unrelible.Donotpermit electrodestoremaininthissolu-

tionforlongperiodsoftime. Work in ahoodandprotect

eyesandskin.Prepareoxidizingreagentbydiluting6.25

mL analytical grade concentrated nitic acid into approxi-

mately800mLdeionizedwater.Mixcarefully.Diluteto1

liter.

VIIVII

VII. General GuidelinesGeneral Guidelines

General GuidelinesGeneral Guidelines

General Guidelines

•Calibration standards and sample solutions should

havethesameionicstrength.ISA,acetatebuffer or

oxidizing reagent should be added to both samples

and standards in the same ratio.

•Calibration standards and sample solutions should

beatsametemperature.

•Thermally insulate beaker with standard or sample

frommagneticstirrer.

•Calibration standards and sample solutions should

be stirred at the same rate using identical sized TFE

coatedstirbars.

•Rinseelectrodepairwithdistilledordeionizedwater

between samples and gently dry off using soft dis-

posable absorbent toweling. Do not rub sensor sur-

face.

•Presoaking chloride sensor in a dilute standard will

optimize response. Do not use concentration above

10-3M.

•A scratched, pitted, or tarnished pellet surface can

causedrift,alossoflowlevelresponse,orpoorrepeat-

ability. Optimumresponsecanberestoredbyremov-

ingthedamagedsurfacewiththemicroabrasivestrip

HI4000-70.

HI4007

•Removeprotectivecoverfromsensortip.

•PrepareHI5315referenceelectrodebyfillingelectro-

lytereservoirwithHI7072fillsolution.

•Place sensor and reference electrodes into electrode

holderandconnectcableconnectorstometer.

HI4107

•Remove the protective plastic wrap that covers the

ceramicjunctionbeforeassemblingsensorforthefirst

time.

•HI7072referencefillsolutionshouldbeaddeddaily

toelectrolytereserviorbeforeelectrodeuse.

•During measurement always operate electrode with

thefillhole open.

•Duringnormaluse, fill solution will slowlydrainout

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 refill with freshfillsolution.

•Avoidlarge changes intemperature (thermal shock)

asitmaydamage the sensor.

VIII.VIII.

VIII. Electrode PreparationElectrode Preparation

Electrode PreparationElectrode Preparation

Electrode Preparation

HI4007

1. Removeprotectivecoverfromsensortip.

2. Preparereferenceelectrodebyfillingouterelectrolyte

reservoirwithHI7072.

3. Place sensor and reference electrodes into electrode

holderandconnectcableconnectorstometer.

HI4107

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,addafewdrops

HI7072fill solutiontotheelectrode,wettingtheo-

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-

trodebodyuntilfill solutionvolumeisjustbelowfill

hole.

8. Position electrode in a Hanna HI 76404 electrode

holder (orequivalent)and connect plugtometer.

HI 4107

CHLORIDE

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.

•Placereferenceandmeasuringhalf-cellintoprepared

sample.

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

dard)tobeaker.RecordthemVvaluewhenstable.

•Addanadditional10-mLofstandardtothesolution.

Record the mV when reading has stabilized. This

value should be less than the previous noted (more

negative).

•Determinethedifferencebetweenthetwo-mVvalues.

Anacceptablevalueforthisslopeis-56±4mV.

X.X.

X. Corrective actionCorrective action

Corrective actionCorrective action

Corrective action

•Verifyprotectivecaphasbeenremoved.(HI4007)

•Verify plastic film has been removed from inner

stem.(HI4107)

•Verifyelectrodesareconnectedproperlytometerand

meterispowered.

•Verify dilute standards are freshly made and stored.

Remakesolutionsifappropriate.

•If the sensor slope just misses the suggested slope

window,soakingthesensorinadilutestandardmay

solve the problem. (Choose 10-3 M chloride or 100

ppm 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.

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