Hanna Instruments HI 4101 Manual de usuario

HI 4101HI 4101

HI 4101

Ammonia

Ion

Selective Electrode

Instruction Manual

AMMONIA

HI 4101

HI 4101 Ammonia ElectrodeHI 4101 Ammonia Electrode

HI 4101 Ammonia Electrode

I.I.

I. Introduction:Introduction:

Introduction:Introduction:

Introduction:

TheHannaHI4101Ammonia gasselectiveelectrodeisa

combination electrode designed for the measurement of

ammoniainaqueoussolutionssuchaswastewatersamples,

wine,beer. Ammoniumionsarealsomeasuredbyconver-

sion to ammonia gas upon ISA addition.

II.II.

II. SpecificationsSpecifications

SpecificationsSpecifications

Specifications

Type: NH3gas sensing

electrodewithglasspH

internal, Ag/ AgCl

referenceand gas

permeable PTFE

membrane.

SpeciesMeasured: NH4+, NH3

Measurement Range: 1.0Mto1x10-6M

17000to0.02ppm

Interferingions: Surfactants,wetting

agents, volatile amines.

Operating Temperature: 0to40°C

Operating pH: >11pH

Dimensions: 12mm(OD)X120

mm (insertion)

0.47”x4.72”

Wettedmaterials: Delrin®, body and cap

PTFE gas membrane

Connection: BNC

III.III.

III. Theory of OperationTheory of Operation

Theory of OperationTheory of Operation

Theory of Operation:::::

The ammonia electrode is a complete potentiometric cell

thatcontainsboth asilver/silver chloride(Ag/AgCl)refer-

enceandapHmeasurementelement. Theseelementsare

housedwithinathermoplasticbodyinachlorideion-con-

tainingelectrolyte,andareisolatedfromthesample bya

gaspermeablemembranemadeofpolytetrafluoroethylene

(PTFE).

Dissolvedgasinthesamplesolutiondiffusesintothemem-

braneandchangesthepHinthethinfilmofelectrolyteon

the surface of the pH glass. Diffusion continues until the

partialpressuresofthegasinthesampleandthinfilmare

equal.The changeinpHis proportionalto theconcentra-

tionofdissolved gasinthesample solution.

TheNernstexpressionforanammoniasensorisexpressed

intheequationbelow.Notethatthepotentialisafunction

oftheammoniagas,whichinturnisrelatedtothehydroxyl

ion concentration. The glass internal, Ag/AgCl reference,

and Henry’s law constant are rolled into the E’and Eo

constants.TheNernstequationforthesensorbecomesthe

equationnotedbelow:

E=E’–2.3RT/nFlog[A]=Eo–0.059log[OH-]

E=observedpotential

E’=Reference andfixedinternal voltages

R=gasconstant(8.314J/KMol)

n=Chargeon ion(equivalents/mol)

A ion=ion activityin sample

T=absolutetemperaturein K

F=Faradayconstant(9.648x104C/equivalent)

ThemV shoulddecrease ina Nernstianmanner asthe

ammonia partial pressure increases in the sample.

IV.IV.

IV. Design ElementsDesign Elements

Design ElementsDesign Elements

Design Elements

The Hanna HI 4101 ammonia gas sensor has 3 main

parts.Thesearethemembrane/membranecap,outerprobe

bodywithantirotationkeyandthepH/referenceassembly

which includes the outer electrode cap, spring, inner cap

andpH/referenceelectrodeassembly.

Outerprobebody

antirotationkey innercap

pH/referenceelectrodeassembly

spring

outerelectrode

cap

sensitive

membrane

reference

electrode

cable

membrane/membrane cap

V.V.

Equipment Required:Equipment Required:

Equipment Required:

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

ionorpH/mVmeter.(Note:log/lineargraphpaperis

useful if an ISE meter is not available).

•Hanna HI 180 magnetic stirrer or equivalent with

stirringbars.(Note:Isolatebeakersfromstirrermotor

heat by placing insulating material such as foam or

corkbetweenthem).

•HannaHI4000-71gassensortestvessel or

•HannaHI76404electrodeholderorequivalentwith

Beakers or other suitable measurement vessel with

plasticsealingfilm orwrap.

VI.VI.

VI. Solutions Required for Calibration:Solutions Required for Calibration:

Solutions Required for Calibration:Solutions Required for Calibration:

Solutions Required for Calibration:

IonicStrengthAdjuster(ISA): HI4001-00

Hanna 0.1 M standard: HI4001-01

Hanna 100 ppm N standard: HI4001-02*

Hanna 1000 ppm N standard: HI4001-03*

*Please Note: These calibration standards are ppm as

NH3-N.

SeeSectionXVIIfor additionalsolutionsusedformainte-

nance.

Usingvolumetricpipettesandglasswaremakedilutionsof

the standard to bracket the concentration of the samples.

Standardswithconcentrationsless than10-3M should be

prepared fresh daily. Store solution in a tightly sealed

bottlewithoutISAadded.2mLofHI4001-00ISAshould

beaddedtoeach100mLsampleofstandardandsamples

justpriortomeasurement. ISAadjuststhepHofthesample

orstandardtoaboutpH11thusconvertingammoniumion

to ammonia. It also provides samples and standards a

constantionicstrengthbackgroundthatstabilizesthesolu-

tions activity coefficient and permits concentration to be

measureddirectly.TheISAprovidescolorindicationto verify

ithasbeenaddedtothesolutionandacomplexingagent

toremove metalions(i.ecopper,zinc)fromsolution.These

VIIVII

VII. General GuidelinesGeneral Guidelines

General GuidelinesGeneral Guidelines

General Guidelines

•Calibration standards and sample solutions should

havethesameionicstrength.ISAshouldbeaddedto

bothsamplesandstandardsimmediatelybeforetak-

ing measurements.

• Calibrationstandardsandsamplesolutionsshouldbe

atthesametemperature.Thermallyinsulatesolution

vesselfrommagneticstirrerwithcorkorotherinsulat-

ing medium.

•Calibration standards and sample solutions should

be stirred at the same rate using identical sized stir

bars.

•Surfacecoatingor“wetting“thePTFEmembranewill

effecttheresponse. Inspectsensorbeforeusing.Re-

place PTFE membrane if damage is evident.

•Rinse electrode with distilled or deionized water be-

tweensamplesanddabdrywithlabwipeorothersoft

disposable absorbent toweling.

•Checkcalibrationevery1-2hours.

•Position sensorsatanangleofapproximately20°to

lessen bubble adherence from solution out-gassing

dueto temperaturechange.

•Closecontainerwithplasticwraporuse

HI4000-71gassensortestvesseltopreventgas

fromleaving.

•Gently pulling cable will permit an exchange of fill

solution at membrane surface. Re-Calibration is re-

quired.

ionsarecapableofreducingthe ammoniaconcentration.

Ifothervolumesofsample/standardareused,addISAat2

partsper100 partsstandard/sample.

VIII.VIII.

VIII. Inner Electrode CheckInner Electrode Check

Inner Electrode CheckInner Electrode Check

Inner Electrode Check

Before assembling the electrode for the first timefirst time

first timefirst time

first time or if

reactivating it after storage, the inner electrode assembly

shouldbeconditioned andthentestedas apHelectrode.

PreparepHtestsolutions HI4000-47-4andHI4000-47-

7bymixinganddissolvingeachbufferpacketinseparate

containerswith50mLdeionizedwater.ThesepHsolutions

containchlorideionsandpHbuffersthatareusedtoverify

the inner electrode (pH internal) is operational. See

SectionXVIIforreplacementaccessoriesandmaintenance

items.

Foranewsensor:

Remove the protective shipping cap from the glass inner

electrode.

Forexistingsensor:

Unscrew the upper cap on the top of the electrode and

carefullywithdrawtheinternalpH/referenceassembly.

Usetest

tubeor

graduated

cylinder

(weighed

Bottom)when

testingor

conditioning

pHinternal

Testbuffer

canbe

usedasa

conditioning

solution

forthe

pHinternal

Protectiveshippingcap

Forstable readings,glassshould becovered tothe

bottomof thelongblack band.

•Ifsensorhasbeenstoredorshippeddry,itshouldbe

“conditioned”by soaking the pH/reference assem-

bly1hourormoreinoneofthepHtestsolutions.

•AvoidtouchingthepHglasswithyourfingers.

•Attention:ThepH/referenceassemblyisfragile!

Support the upper portion of the internal cell while

immersing the glass and reference assembly. A tall

narrowcontainer withweightedbottom isbest.The

pHtestsolutionshouldcoverthebottomofthelarge

black ban.

Test:ConnecttheBNCconnectorontheelectrodecable toa

pH/mV(mVorORPmode)meter.Carefullyimmerse

thesensorassemblyintooneofthebuffers.Whenthe

measurmentstabilizesrecordthemVgenerated.Rinse

sensor tip in deionized water and dab dry between

bufferstopreventsolutioncarry-over.Donotrubthe

glass.Takeameasurementinthesecondbufferand

recordmV. Payattentiontominussignifpresent.

CalculatethedifferenceinmVbetweenthetwosolutions.

Example of typical values:

HI4000-47-7 -90.2mV

HI4000-47-4 80.66mV

Difference 170.8mV=80.6-(-90.2)

A calculated value equal or greater than 160 mV is ac-

ceptableforambienttemperaturesbetween20°and25°C.

1) Removeglassinternalfromsensorbodyandperform

innerelectrodecheck.(SeesectionVIII).

2) Installmembraneontheouterprobebody.Usetwee-

zers provided and avoid touching working area of

membranewith yourfingers asskin oilwill change

thehydrophobicproperties.Discardthepaperback-

ing (blue) found between white PTFE membranes.

Hold membrane at corner with tweezers and drape

overloweropeningofouterprobebody.

IX.IX.

IX. Electrode PreparationElectrode Preparation

Electrode PreparationElectrode Preparation

Electrode Preparation

3) Holdonecorneragainstthethreadswiththumbwhile

gently stretching membrane over opening and cap-

turing opposite membrane corner against threads .

Smoothexcessmembranematerialaroundthethreads.

4) Screwoutermembranecapontobody

thus capturing the membrane between the cap and

outerbodythreads.

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