A rapid simple method for the measurement of iodide in water in the range of 0.01 ppm - 10,000 ppm.
- pH/ION analyzer or pH meter with millivolt scale
- Iodide combination ion selective electrode
- Iodide standard, 10,000 ppm
- Ionic strength adjustment buffer (ISAB), 5M NaNO3
- Nickel sulfate 1M (dissolve 26.3g of NiSO4. 6H2O in distilled water and dilute to 100 ml.)
Ionic Strength Adjustment Buffer (ISAB) Preparation
Dissolve 42.5g A.R. grade NaNO3 in distilled water and dilute to 100 ml.
Iodide Standard Preparation
Dissolve 11.81g of dried NaI (sodium iodide) in distilled water and dilute to 1000 ml. Prepare 10, 100, 1000, ppm standards by serial dilution of the 10,000 ppm standard.
To any sample containing sulfide or cyanide add 1 molar nickel sulfate. Addition of 0.1 ml of nickel sulfate to 100 ml sample will react with 58 ppm sulfide or 117 ppm cyanide.
To each 100 ml of sample add 2 ml of ISAB and stir thoroughly.
To 100 ml of each standard add 2 ml of ISAB. If any sample requires treatment for interferents prepare standards with the same background.
Immerse the electrodes in each of the standards in increasing concentration steps, rinsing the electrodes between standards and recording the mV response of the electrode.
Plot in graph of mV response against each standard concentration used on semi-log paper.
Immerse the electrodes in the sample solution, record the mV response of the electrodes and plot sample concentration from graph.
This determination may be carried out directly in concentration units by use of the “activity” modes on pH/ION analyzers.
As both, standard and samples have been diluted by the same amount, the result obtained from the graph relates to the concentration of the original sample.
Sulfide and cyanide ion interference is removed by addition of NiSO4. 6H2O.
Bromide does not interfere in concentrations up to 5000 times that of iodide.
Chloride and thiosulfate ions do not interfere when present in excess of iodide by up to 106 and 105 respectively. Mercury should be absent.
Concentration of free metal ions causing 10% error are:
Bismuth 4 ppm
Cadmium 50 ppm
Lead 1000 ppm