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Chemical / Operational
Thus nitrate can be tolerated up to the same concentration as perchlorate (this will cause an approximately 2% enhancement), and chloride can be present up to 100 times more concentrated before it will cause a significant error.Return to top
Procedure for determining the concentration of PERCHLORATE (ClO4-) in WATER
Ion-Selective Electrode for perchlorate ion (ELIT 8061 PVC membrane)
Reference electrode: single junction silver chloride (ELIT 001)
Dual electrode head (ELIT 201)
Standard solution: 1000 ppm ClO4 as NaClO4
Buffer solution (ISAB): 1 Molar CH3COONa .
ELIT Computer Interface/Ion Analyser, or Ion/pH/mV meter.
100 or 150 ml polypropylene beakers, 100ml volumetric flask, 1, 2, 5, 10ml pipettes.
Before use, the electrodes must be calibrated by measuring a series of known standard solutions, made by serial dilution of the 1000ppm standard solution. For a full calibration, prepare 100ml of solutions containing 1000, 100, 10, 1, and 0.1ppm ClO4. If the approximate range of concentrations of the samples is known, and this is within the specified linear range of the ISE, then it is only necessary to make two solutions which span this range: e.g. if samples are known to lie between, say, 30 and 130ppm then you could use standards of 10 and 200ppm or even 20 and 150ppm.
NB: If the samples to be measured are expected to have a total ionic strength of greater than 0.01 Molar, then 2 ml of buffer solution should be added to each 100ml standard and mixed thoroughly to compensate for different activity coefficients between samples and standards.
Follow the instructions in the General Operating Instructions to measure these standard solutions and prepare a calibration graph.
For low ionic strength samples, no sample preparation is necessary. Simply take approximately 50 to 100 mls of sample in a plastic beaker, or even immerse the electrodes directly in a lake or river (but take care to avoid losing the electrodes!). For samples with high ionic strength, take 100mls of sample and add 2 mls of buffer solution and stir well before measurement.
Follow the instructions in the electrode operating instructions to measure a series of samples and record the results. Briefly, it is important to note that, if measuring in beakers, the electrodes must be washed and dried between each sample, to avoid cross contamination, and sufficient time must be allowed (2 or 3 minutes), before taking a reading after immersion, to permit the electrode signal to reach a stable value. For the highest precision, frequent recalibration is recommended (see operating instructions).
The results will be displayed as ppm and mol/l. If buffer solution has been added equally to standards and samples then these figures will not need adjusting because they will all be affected by the same dilution factor.Return to top