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Instruction Manual 

 

Cadmium Electrode

 

 

13

A drifting potential reading or a decrease in electrode slope may mean that the electrode membrane 
needs polishing. 
 
To polish the membrane: 
 

1. 

If using polishing paper, cut off a 1-2" piece and place it face up on the lab bench. 

 
2. 

Put a few drops of distilled or deionized water in the center of the paper. 

 
3. 

Holding the paper (cotton) steady with one hand, bring the membrane of the electrode 
down perpendicular to the paper and, with a slight swirling motion, gently polish the tip of 
the electrode against the surface of the polishing paper (cotton) for a few seconds. 

 
4. 

Rinse the electrode surface with distilled or deionized water and soak the electrode tip in 
standard solution for about five minutes before use. 

 
5. 

If using jeweller's rouge, place a cotton ball on the table top and flatten it using the bottom 
of a beaker. 

 
6. 

Put 1-2 drops of distilled or deionized water in the center of the cotton pad. 

 
7. 

Add a small amount of jeweller's rouge to the damp cotton. 

 
8. 

Continue with Steps 3 and 4 above. 

 
 

Limits of Detection 

 
The upper limit of detection in pure cadmium nitrate solutions is 0.1M. In the presence of other 
ions, the upper limit of detection is above 1.0x10

-2

M cadmium, but the possibility of a liquid 

junction potential developing at the reference electrode and the "salt extraction effect" are two 
limiting factors.  Some salts may infuse into the electrode membrane at high salt concentrations 
causing deviation from the theoretical response. Either dilute samples between 0.1M and 1.0x10

-2

or calibrate the electrode at 4 or 5 intermediate points. 
 
The lower limit of detection is influenced by the slight water solubility of the electrode pellet. Refer 
to Figure 1 for a comparison of the theoretical response to the actual response at low levels of 
cadmium. Neutral solutions containing free cadmium ions can be measured down to 1.0X10

-7

(0.01 ppm). Extreme care must be taken with measurements below 1.0X10

-5

M (1.1 ppm) to avoid 

contamination of samples. 
 

pH Effects 

 
Figure 4 shows how the electrode responds to cadmium ion in solution at various pH levels.  
Hydrogen ion interferes with low cadmium ion measurements. The minimum pH at which cadmium 
ion concentrations can be measured without interference is given by the solid line 

"limit of 

detection"

 above the shaded area in Figure 4. 

 
At a high pH, free cadmium ion precipitates with hydroxide ion, thereby reducing the cadmium ion 
concentration. The maximum pH at which cadmium concentration can be measured without 

Summary of Contents for CADMIUM EPOXY

Page 1: ...Instruction Manual Cadmium Electrode 1 EUTECH INSTRUMENTS PTE LTD INSTRUCTION MANUAL CADMIUM ION ELECTRODE ...

Page 2: ...6 Direct Measurement of Cadmium using an ion meter 7 Low Level Cadmium Determination using a pH mV meter 8 Low Level Cadmium Determination using an ion meter 9 Titration 9 Titration of Cadmium 10 ELECTRODE CHARACTERISTICS 11 Reproducibility 11 Interferences 11 Precipitation and Complexation 11 Temperature Influences 12 Electrode Response 12 Limits of Detection 13 pH Effects 13 Electrode Life 14 El...

Page 3: ...d add 425 grams reagent grade sodium nitrate NaNO3 Swirl the flask gently to dissolve the solid Fill to the mark with distilled water cap and upend several times to mix the solution 3 Cadmium Nitrate Standard Solution 0 1M To prepare this solution from your own laboratory stock half fill a one liter volumetric flask with distilled water and add 30 85 grams of reagent grade Cd NO3 2 4H2O Swirl the ...

Page 4: ...d to the beaker When the reading has stabilized record the mV reading 3 Using a pipet add 10 ml of the standard used above to the beaker When the reading has stabilized record the mV reading 4 Determine the difference between the two readings The electrode is operating correctly if the mV potential has changed 27 2 mV assuming the temperature is between 20o and 25o C See the TROUBLESHOOTING sectio...

Page 5: ...stilled water and blot dry Use a clean dry tissue to prevent cross contamination For samples with high ionic strength prepare standards whose composition is similar to the sample Use fresh standards for calibration Use 2 ml of ISA for each 100 ml of sample or standard Always check to see that the membrane is free from air bubbles after immersion into the standard or sample Dilute concentrated samp...

Page 6: ...pare standards with a composition similar to the samples if the samples have an ionic strength above 0 1M 2 Place 100 ml of the most dilute solution 1 0X10 4 M or 10 ppm in a 150 ml beaker on the magnetic stirrer and begin stirring at a constant rate After assuring that the meter is in the mV mode lower the electrode tips into the solution After the reading has stabilized record the mV reading 3 P...

Page 7: ... After the reading has stabilized record the mV reading Using the calibration curve determine the sample concentration 7 The calibration should be checked every two hours Assuming no change in ambient temperature immerse the electrode tips in the mid range standard After the reading has stabilized compare it to the original reading recorded in Step 3 above A reading differing by more than 0 5 mV o...

Page 8: ...change in ambient temperature will necessitate the repetition of Steps 2 6 above The meter should be re calibrated daily Low Level Cadmium Determination using a pH mV meter This procedure is recommended for solutions with cadmium concentrations of less than 1 0X10 5 M 1 1 ppm If the solution is high in ionic strength but low in cadmium ion use the same procedure but prepare a calibration solution ...

Page 9: ... low level calibration curve daily Check the calibration curve every two hours by repeating Steps 3 7 above Low Level Cadmium Determination using an ion meter 1 Using 20 ml of standard ISA dilute to 100 ml with distilled water This low level ISA 1 0M NaNO3 is added at the rate of 1ml low level ISA to each 100 ml of solution The background ionic strength will be 1 0X10 2 M 2 Follow the steps given ...

Page 10: ...le into a 150 ml beaker place the beaker on the magnetic stirrer and begin stirring at a constant rate Adjust the sample to pH 10 by adding ammonia 3 Position the burette tip in the beaker slightly above the liquid level in the beaker and slightly off center Position the electrode tips in the solution about halfway between the center of the beaker and the beaker wall 4 Begin adding the EDTA in 0 5...

Page 11: ...lishing procedure The cadmium ion electrodes do not respond to anions or most cations The electrode membrane is poisoned by solutions containing copper mercury and silver These ions must be absent from the solution If the level of ferric ion or lead ion exceeds the level of cadmium ion in the sample the measurement will be affected Sodium fluoride added to the sample will eliminate ferric ion Prec...

Page 12: ...lope Temp oC S 0 27 10 10 28 10 20 29 08 25 29 58 30 30 07 40 31 07 50 32 06 If changes in temperature occur the electrodes should be re calibrated The temperature range for the Eutech Cadmium Ion Electrode is 0o 80o C provided that temperature equilibrium has occurred If the temperature varies substantially from room temperature equilibrium times up to one hour are recommended Electrode Response ...

Page 13: ...ns the upper limit of detection is above 1 0x10 2 M cadmium but the possibility of a liquid junction potential developing at the reference electrode and the salt extraction effect are two limiting factors Some salts may infuse into the electrode membrane at high salt concentrations causing deviation from the theoretical response Either dilute samples between 0 1M and 1 0x10 2 M or calibrate the el...

Page 14: ...ution if refillable and the rubber insert placed over the filling hole ELECTRODE THEORY Electrode Operation The electrode consists of sulfides of cadmium and other metals bonded into an epoxy or glass body When an electrode potential develops across the membrane the membrane is in contact with a solution containing cadmium ions The electrode potential is measured against a constant reference poten...

Page 15: ... of ions in the two solutions Electrode charge will be carried unequally across the solution boundary resulting in a potential difference between the two solutions since ions diffuse at different rates When making measurements it is important to remember that this potential be the same when the reference is in the standardizing solution as well as in the sample solution or the change in liquid jun...

Page 16: ...ed substitute another cadmium ion electrode that is known to be in good working order for the questionable electrode If the problem persists and you are using an electrode pair try the same routine with a working reference electrode 4 If the problem persists the reagent may be of poor quality interferences in the sample may be present or the technique may be faulty See Standards and Reagents Sampl...

Page 17: ...the samples prior to testing to eliminate a problem before it starts See Measuring Hints Sample Requirements and Interferences Technique Be sure that the electrode s limit of detection has not been exceeded Be sure that the analysis method is clearly understood and is compatible with the sample Refer to the instruction manual again Reread sections GENERAL PREPARATION and ELECTRODE CHARACTERISTICS ...

Page 18: ...ctrodes in solution in solution Noisy or Unstable defective meter check meter with Readings readings shorting strap continuously or rapidly changing air bubble on remove bubble by membrane re dipping electrode electrode exposed soak electrode in to interferences cadmium standard defective electrode replace electrode ISA not used use recommended ISA meter or stirrer ground meter or not grounded sti...

Page 19: ... bubble on remove bubble by membrane redipping probe Incorrect Answer incorrect scaling plot millivolts on but calibration of semi log paper the linear axis On curve is good the log axis be sure concentration numbers within each decade are increasing with increasing concentration incorrect sign be sure to note sign of millivolt number correctly incorrect standards prepare fresh standards wrong uni...

Page 20: ...tance 1 Mohm Reproducibility 2 Samples Aqueous solutions only no organic solvents Size 110 mm length 12 mm diameter 1 m cable length Storage Store in cadmium solution ORDERING INFORMATION CODE NO DESCRIPTION EC CD 03 Cadmium Ion Combination Electrode epoxy body EC ISA CD1 BT Ionic Strength Adjuster ISA 5M NaNO3 EC MIS PP Polishing Paper for the Cadmium Ion Electrodes ...

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