异烟酸-吡唑啉酮分光光度法测定白酒中氰化物的含量

Determination of cyanide in Chinese liquor by isonicotinic acid-pyrazolone spectrophotometry

探究国标法GB／T5009．48—2003异烟酸-吡唑啉酮分光光度法测定酒中氰化物产生浑浊的原因及消除干扰的方法，并对测定过程进行优化。样品加热碱解后，用乙酸将溶液pH值调节至中性，加入氯胺T将氰化物氧化成氯化氰，再加入异烟酸-吡唑啉酮溶液生成蓝色染料，用分光光度计测量并定量。结果表明，氰化物含量在0～0．2mg／L范围内线性关系良好，相关系数r=0．9994，加标回收率87％～104％，RSD2．85％，测定结果准确、可靠。

Herein, the affecting factors causing turbidity during the determination of cyanide in Chinese liquor by national standard method （ GB/T 5009. 48-2003 Isonicotinic acid-pyrazolone spectrophotometric method） and the way to eliminate interference were investigated. The process was optimized and improved. After the samples were heated and hydrolyzed by alkaline agents, pH of the solution was adjusted to neutral with acetic acid. The cyanide was converted to cyanogen chloride after the addition of chloramine-T. Then isonicotinic acid-pyrazolone was added to generate a blue dye. Finally, the cyanide was detected and quantified through spectrophotometer. The results showed that the correlation coefficient was 0. 9994 within the detectable range of 0 - 0.2 mg/L, and the recovery rate and RSD were 87% - 104% and 2.85% respectively. The results were accurate and reliable.