Standard Test Method for Free Cyanide and Aquatic Free Cyanide with Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection
5.1 Cyanide and hydrogen cyanide are highly toxic. Regulations have been established to require the monitoring of cyanide in industrial and domestic wastes and surface waters.4
5.2 It is useful to determine the aquatic free cyanide to establish an index of toxicity when a wastewater is introduced into the natural environment at a given pH and temperature.
5.3 This test method is applicable for natural water, saline waters, and wastewater effluent.
5.4 Free cyanide measured using this test method is applicable for implementation of the International Cyanide Code Guidance in accordance with Guide D7728.
1.1 This test method is used to establish the concentration of free cyanide in an aqueous wastewater, effluent and in-stream free cyanide concentrations after mixing treated water with receiving water. The test conditions of this test method are used to measure free cyanide (HCN and CN-) and cyanide bound in the metal-cyanide complexes that are easily dissociated into free cyanide ions at the pH of 6. Free cyanide is determined at pH 6 at room temperature. The aquatic free cyanide can be determined by matching the pH to the water in the receiving environment in the range of pH 6 to 8. The extent of HCN formation is less dependent on temperature than the pH; however, the temperature can be regulated if deemed necessary for aquatic free cyanide to further simulate the actual aquatic environment.
1.2 The free cyanide test method is based on the same instrumentation and technology that is described in Test Method D6888, but employs milder conditions (pH 6–8 buffer versus HCl or H2SO4 in the reagent stream), and does not utilize ligand displacement reagents.
1.3 The aquatic free cyanide measured by this procedure should be similar to actual levels of HCN in the original aquatic environment. This in turn may give a reliable index of toxicity to aquatic organisms.
1.4 This procedure is applicable over a range of approximately 5 to 500 μg/L (parts per billion) free cyanide. Sample dilution may increase cyanide recoveries depending on the cyanide speciation; therefore, it is not recommended to dilute samples. Higher concentrations can be analyzed by increasing the range of calibration standards or with a lower injection volume. In accordance with Guide E1763 and Practice D6512 the lower scope limit was determined to be 9 μg/L for chlorinated gold leaching barren effluent water and the IQE10 % is 12 µg/L in the gold processing detoxified reverse osmosis permeate waste water sample matrix.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in 8.6 and Section 9.
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