Hanna Instruments HI 4003 Manuel utilisateur

HI 4003HI 4003

HI 4003

HI 4103HI 4103

HI 4103

Instruction Manual

Half-cell

Combination

COMBINATION

CADMIUM

HI 4103

CADMIUM

HI 4003

Cadmium Ion

Selective Electrode

HI 4003 Cadmium Half-cellHI 4003 Cadmium Half-cell

HI 4003 Cadmium Half-cell

HI 4103 Cadmium Combination ElectrodeHI 4103 Cadmium Combination Electrode

HI 4103 Cadmium Combination Electrode

I.I.

I. Introduction:Introduction:

Introduction:Introduction:

Introduction:

The Hanna HI 4003 and HI 4103 are ion selective elec-

trodes designed for the measurement of cadmium ions in

aqueous solutions. The HI 4003 is a solid state half-cell

sensor that requires a separate reference. The HI 4103 is a

combination ion selective electrode.

IIII

II.

SpecificationsSpecifications

Specifications

Type: Solid State electrode with

a Cadmium sulfide/ silver

sulfide membrane.

Ion(s) measured: Cadmium (Cd 2++

Measurement range: 0.1M to 1X 10-7 M

11,200 to 0.01 ppm

Interfering ions: Silver and mercury must

be absent. Any ion that forms a more insoluble sulfide than

cadmium sulfide will interfere with the electrode response.

These include lead (Pb2+)and cupric ions (Cu2+). Oxidation

of the cadmium surface by ferric ion( Fe3+) will severely

poison the electrode. Ions that can form complexes with

cadmium ions will reduce the measured concentration.

Examples include bromide, chloride and EDTA.

Operating Temperature: 0-80°C

Operating pH: 2 to12 pH

concentration dependant

(4.5-7.5 recommended)

Dimensions: 12 mm (OD) X 120 mm

nominal insertion

(0.47” X 4.72”)

Connection: BNC

III.III.

III. Theory of OperationTheory of Operation

Theory of OperationTheory of Operation

Theory of Operation:::::

The HI 4103 or HI 4103 cadmium electrodes are potentio-

metric devices used for the rapid determination of free cad-

mium ions in samples and as a detector for the titration of

cadmium with EDTA. Cadmium sensors are “electrodes of

the third kind”because they detect cations which also form

low-solubility salts with sulfide anions that also form low-

solubility salts with silver.

The electrode functions as a sensor or ionic conductor. The

HI 4003 requires a separate reference electrode to complete

its electrolytic circuit. The HI 4103 incorporates a reference

electrode. The mixed cadmium sulfide/ silver sulfide mem-

brane produces a potential change due to changes in the

sample’s cadmium ion activity. When the ionic strength of

the sample is fixed by the addition of ISA, the voltage is

proportional to the concentration of cadmium ions in solu-

tion and the electrode follows the Nernst equation.

E= Ea + 2.3 RT/nF log A ion

E= observed potential

Ea= Reference and fixed internal voltages

R= gas constant (8.314 volt coulomb/K Mole)

n= Charge on cadmium ion (2+)

A i=ion activity in sample

T= absolute temperature in K

F= Faraday constant (9.648 x 104 coulomb/mole)

IV.IV.

IV. Design elements of the HI 4003 and HI 4103Design elements of the HI 4003 and HI 4103

Design elements of the HI 4003 and HI 4103Design elements of the HI 4003 and HI 4103

Design elements of the HI 4003 and HI 4103

electrodeselectrodes

electrodes

Upper Cap

Spring

O-Ring

Ceramic Junction

on Inner Stem

Fill Hole

O-Ring and

Plug

Sensing

Membrane

Outer Sleeve

Upper

Threads

Liquid junction

Cap

Sensing

Membrane

Sensor

Handle

CADMIUM

HI 4003

V.V.

V. Equipment required:Equipment required:

Equipment required:Equipment required:

Equipment required:

•Hanna HI 5315 Double Junction Reference Electrode

with HI 7072 Fill Solution for use with HI 4003 half-

cell.

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

ion or pH/mV meter. (Note: log/linear graph paper is

useful if an ISE (ion) meter is not available).

•Hanna HI 180 Magnetic Stirrer or equivalent with TFE

coated stirring bars (HI 731320). Note: isolate bea-

kers from stirrer motor heat by placing insulating

material such as foam or cork between them.

•Hanna HI 76404 Electrode Holder or equivalent.

•Plastic beakers (HI 740036P) or other suitable mea-

surement vessel.

VI.VI.

VI. Solutions RequiredSolutions Required

Solutions RequiredSolutions Required

Solutions Required

For Cadmium Measurements

0.1 M cadmium standard, (500 mL) HI 4003-01

ISA, (500 mL) HI 4000-00

For direct cadmium measurements- Using volumetric pi-

pettes and glassware, make dilutions of HI 4003-01 to

bracket the concentration of the samples. Note: 0.1M cad-

mium standard is equivalent to 11,200 ppm. Standards

with concentrations <10-3 M (112 ppm) should be pre-

pared daily. Store in tightly closed plastic bottle. To 100

parts standard or sample add 2 parts of ISA.

Please note: cadmium compounds are toxic by ingestion or

skin contact. Take appropriate precautions.

VIIVII

VII. General GuidelinesGeneral Guidelines

General GuidelinesGeneral Guidelines

General Guidelines

•Concentrated samples (>0.10 M) should be diluted

before measurement. Multiply the final result by the

corresponding dilution factor.

•Calibration standards and sample solutions should

have the same ionic strength.

•For high ionic strength samples, use standard addi-

tion or titration methods.

•Calibration standards and sample solutions should

be at same temperature.

•The magnetic stirrer may generate heat. Thermally

insulate beaker containing standard or sample from

magnetic stirrer by placing cork or other insulative

sheet between beaker and stirrer plate.

•Calibration standards and sample solutions should

be stirred at the same rate using identical sized TFE

coated stir bars.

•Rinse electrode pair with distilled or deionized water

between samples and gently dab dry with soft dis-

posable absorbent toweling. Do not rub electrodes.

•Avoid Cd(OH)2

precipitation or hydrogen ion interfer-

ence by maintaining pH of samples between 4.5 and

7.5 pH. Use Nitric acid or sodium hydroxide to adjust

pH.

•Presoaking the cadmium sensor tip in a dilute stan-

dard will optimize response. Use concentrations ap-

proximately10-3M.

•Presoaking the cadmium tip in a mild reducing solu-

tion such as ascorbic acid for a few minutes may be

helpful when oxidation of the membrane surface is

an issue between sample measurments.

•A scratched, pitted, or oxidized pellet surface can cause

drift, a loss of low level response, or poor repeatability.

Optimum response can be restored by removing the

damaged surface with the microabrasive strip HI 4000-

70. Use gloves to protect skin. Cadmium dust is toxic.

•Avoid large changes in temperature (thermal shock)

as it may damage the sensor.

•Gas bubbles may form from solution out-gassing due

to temperature change. Gently tap body of sensor to

dislodge them from sensing membrane.

HI 4003

•Remove protective cover from sensor tip.

HI 4103

•Remove the protective plastic wrap that covers the

ceramic junction before assembling sensor for the first

time.

•HI 7072 reference fill solution should be added daily

to electrolyte reservoir before electrode use.

•During measurement always operate electrode with

the fill hole open.

•During normal use, fill solution will slowly drain out

of the tapered cone junction at the lower portion of the

electrode. Excessive loss (>4 cm drop within 24 hours)

is not normal. If this occurs verify cap is tightened and

the interface between the internal cone and outer

body is free of debris.

•Add fill solution daily to maintain a good head pres-

sure. For optimum response, this level should be main-

tained and not be allowed to drop more than 2-3 cm

(1-inch) below fill hole. Fill solution must cover the

ceramic found on the inner stem.

•If an erratic measurement occurs, check to see if for-

eign matter is seen trapped near the internal cone.

Drain, wipe off outer cone while depressing cap, re-

lease cap and refill with fresh fill solution.

VIII.VIII.

VIII. Electrode PreparationElectrode Preparation

Electrode PreparationElectrode Preparation

Electrode Preparation

HI 4003

1. Remove protective cover from sensor tip.

2. Prepare reference electrode by filling outer electrolyte

reservoir with HI 7072.

3. Place sensor and reference electrodes into electrode

holder and connect cable connectors to meter.

HI 4103

1. Unwrap plastic film seal found over ceramic junction

on inner stem and discard. This is only used for ship-

ping and long term storage.

2. Rinse inner stem with deionized water making certain

to wet the o-ring found on the inner stem.

3. Reassemble electrode by gently pushing the inner

assembly into the outer body, sliding spring down

cable, and screwing cap into place.

4. Remove fill hole cover and o-ring on fill hole spout.

5. Using the dropper pipette provided, add a few drops

HI 7072 fill solution to the electrode, wetting the o-

ring and rinsing out the fill solution chamber.

Deionized

Water

Remove

Parafilm

6. Holding the body of the electrode gently press upper

cap with your thumb. This permits the fill solution to

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

trode returns to its original position. (You may need to

gently assist for this to occur).

7. Tighten the electrode cap onto the body and fill elec-

trode body until fill solution volume is just below fill

hole.

8. Position electrode in a Hanna HI 76404 electrode

holder (or equivalent) and connect plug to meter.

HI 4103

CADMIUM

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

•Connect sensors to pH/mV/ISE meter

•Place meter in mV mode.

•Place 100 mL of deionized water into a beaker with

stir bar and 2 mL of HI 4000-00 ISA. Add stir bar and

place on magnetic stirrer.

•Place electrodes into prepared sample.

•Add 1 mL of the stock standard HI 4003-01 (or .01 M

or .001 M standard by dilution) to the beaker.

Record the mV value when reading has stabilized.

•Add an additional 10 mL of standard HI 4003-01 (or

same dilute standard) to the solution. Record the mV

when reading has stabilized. This value should be

more positive than the previous noted.

•Determine the difference between the two mV values.

An acceptable value for this slope is +27 ± 4 mV

near 25°C.

X.X.

X. Corrective actionCorrective action

Corrective actionCorrective action

Corrective action

•Verify protective cap has been removed (HI 4003).

•Verify plastic film has been removed from inner stem

(HI 4103).

•Verify electrodes are connected properly to meter and

meter is powered.

•Verify standard has been properly stored. Remake

standards if appropriate.

•If the sensor slope just misses the suggested slope

window, soaking the sensor in a dilute standard may

solve the problem. (<10-3 M standard).

•A scratched, pitted or oxidized sensing surface can be

polished with HI 4000-70 polishing strip. Cut off

approximately 1 inch of the micro-abrasive strip. Wear

protective gloves. Wet the frosted side with deionized

water and place against damaged membrane of the

electrode. Place your gloved thumb against the shiny

backing and slowly rotate back and forth while

applying gentle pressure. Continue polishing until

you are satisfied with the surface. If dark deposits

Ce manuel convient aux modèles suivants

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