Determination of cyanide in cyanide slag from gold smelting by nitrogen blowing bath and ion chromatography
SHI Yanhua1, ZHANG Ruoxuan2, WU Zanhua*1,3, WU Xiaolu1
1. Experimental Testing Team of Jiangxi Geological Bureau,Nanchang 330002,China; 2. School of Nuclear Science and Engineering,East China University of Technology,Nanchang 330003,China; 3. Jiangxi Bureau of Geology,Nanchang 330001,China
Abstract：The accurate determination of CN- content in cyanide slag from gold smelting is of great significance for judging the harm of CN-. In this study, the nitrogen blowing-water bath heated distillation was used to extract CN-, avoiding the danger of flammability and explosion in heating. The sulfur in the sample was adsorbed by installing a desulfurization device in series in front of the absorption bottle, eliminating the interference of S2- on the determination of CN-. Finally, the determination of CN- in the cyanide slag of gold smelting product by ion chromatography was realized. The type, concentration, and flow rate of the eluent were optimized: the eluent was 0.10 mol/L sodium hydroxide -0.05 mol/L sodium acetate-0.5% (volume fraction) ethylenediamine mixture; the flow rate was 1.0 min/mL. The mass concentration of CN- had a good linear relationship with the corresponding spectral peak area in the range of 1-30 μg/L with the correlation coefficient of 0.999 3. The minimum detection concentration was 0.15 μg/L, the limit of detection was 2.9 μg/kg, and the limit of quantification was 9.6 μg/kg. Three cyanide slag samples with different content levels were determined according to the experimental method, and the standard addition recovery tests were conducted. The relative standard deviations (RSD, n=6) of the measurement results were between 2.7% and 6.5%, and the spiked recoveries were between 94% and 111%. The quality control samples of total CN- in solid waste with high, medium, and low content were selected and determined according to the experimental method and spectrophotometry. The results showed that the measurement results of both methods were relatively close to the reference values, which could meet the requirement that the measurement error of the quality control standard sample should not exceed 10%. The obtained t values were all less than t0.05 (5)=2.571, and there was no significant difference between the two methods. The cyanide slag samples of SPL2 and SPL5 from gold smelting products were selected and determined according to the experimental method. Meanwhile, the gas chromatography method was used for the comparison. The results showed that the results obtained by two methods were basically consistent. The obtained t values were all less than t0.05 (5)=2.571, indicating that there was no significant difference between the experimental method and the gas chromatography method.
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