イソニコチン酸-ピラゾロンを用いるシアンイオンの定量
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The pyridine-pyrazolone method for the determination of cyanide ion has been used widely as Testing Method for Industrial Waste Water (JIS K 0102) and Testing Method for Supplying Water, etc., because of the selectivity and high sensitivity. But, as the pyridine-pyrazolone reagent has an unpleasant odor owing to pyridine and the reagent solution is unstable and its preparation is time-consuming, pyridine-pyrazolone method is unsuitable for routine work.<BR>For establishing a simpler analytical procedure without using pyridine, a spectrophotometric method using isonicotinic acid and pyrazolone has been developed and the optimum conditions have been established. This reagent has no unpleasant odor and is stable in <I>N</I>, <I>N</I>-dimethylformamide-water solution. A colored product with cyanide ion has an absorption maximum at 638 nm. The calibration curve followed the Beers law in the range of 02.5 ppm CN<SUP>-</SUP> in samples.<BR>To 1 m<I>l</I> of sample containing 0.052.5 ppm CN<SUP>-</SUP> 2 m<I>l</I> of 0.05 <I>M</I> phosphate buffer solution (pH 6.8) and 0.1 m<I>l</I> of 1% chloramine T solution were added. The mixture was allowed to stand at 1525°C for 5 min. Three m<I>l</I> of isonicotinic acid-pyrazolone reagent was added, and the mixture was kept at 40°C±2°C for 30 min. The amount of CN- was determined from the absorbance at 638 nm.<BR>The presence of 1000 ppm of NH<SUB>4</SUB><SUP>+</SUP>, CNO-, hydroquinone did not interfere, but the presence of 10 ppm of Cu<SUP>2+</SUP>, Zn<SUP>2+</SUP>, or Ni<SUP>2+</SUP>interfered. Thiocyanate ion gave a color similar to that of the cyanide compound.
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