氰渣中总氰化物的测定

Determination of total cyanide in cyanide residual

氰渣中总氰化物的测定没有标准,研究建立了氰渣中总氰化物的测定方法。氰化物质量分数较高的样品采用硝酸银滴定法测定,质量分数较低的样品采用异烟酸-吡唑啉酮或异烟酸-巴比妥酸分光光度法测定。通过条件实验对预蒸馏试剂、酸种类、分散剂、称样量和分光光度法吸收液分取体积等影响因素进行了优化。该方法测定结果的相对标准偏差为1. 3%～3. 4%,加入标准物质回收率为89. 9%～113. 3%,其精密度和准确度良好,适合氰渣中总氰化物的测定。

There are no standards for the determination of total cyanide in cyanide residual. The research set up methods for the determination of total cyanide in cyanide residual. For samples with high cyanide mass fraction, silver nitrite titration is used for determination. For samples with low cyanide mass fraction, isonicotinic acid - pyrazolone or isonicotinic acid - barbituric acid spectrophotometry is used for determination. By condition experiment, the positive factors are optimized such as pie-distillation agent, acid type, dispersing agent, sample weight and spectrophotometry absorption solution extraction volume. The determination results of the method has RSD of 1.3 % - 3.4 %. The recovery rate of reference material is 89.9 % - 113.3 %. The precision and accuracy are both good. The method is suitable for the determination of total cyanide in cyanide residual.