Accuracy And Precision Of The EPA Reflux Method For Cyanide In Gold-Processing Waste Streaming

The determination of aqueous cyanide is accomplished by either detection in the sample as collected or by removal of the cyanide of the collected sample, followed by detection. The direct determination of the cyanide content of a solution can only be used in the simplest of systems, since many interferences can result in errors. Thus the most widely used method for total cyanide determination involve the reflux distillation of the sample using heat, acid and vacuum or air flow. The basic theory underlying this analytical approach is that by reducing the pH, the quality of molecular hydrogen cyanide will be in- creased and can be removed from the solution by elevating the temperature. The hydrogen cyanide is then collected in a caustic solution and analyzed. The general approach of removing the cyanide from the sample by distillation represented a major advance in this area of analytical chemistry. It enabled the determination of cyanide in many additional types of samples. When it became apparent that the tightly bonded cyanide complexes were not being detected by this approach, many methods fox complex ion destruction were proposed. These methods usually involved low pH adjustment with oxidizing mineral acids, coupled with the catalytic decomposition of the tightly hound complexes. All off the complexes except the strongest could he broken by these methods. The catalytic reflux distillation step has been found to have some negative aspects, since many materials that can be distilled with hydrogen cyanide will interfere with the color development step and result in a false positive reading.