EPA Method 9013A

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EPA Method 9013A:
CYANIDE EXTRACTION PROCEDURE FOR SOLIDS AND OILS

Summary:
The extraction procedure described in this method is designed for the extraction of soluble and insoluble cyanides from solids and oil wastes. The resulting extraction solutions may be analyzed for total cyanide and/or cyanides amenable to chlorination (Methods 9010, 9012 and 9014) as well as analyzed for metal cyanide complexes (Method 9015). The method is applicable to oil, solid, and multiphasic matrices.

Scope:
If the waste sample contains so much solid, or solids of such a size as to interfere with agitation and homogenization of the sample mixture in the distillation flask, or so much oil or grease as to interfere with the formation of a homogeneous emulsion, the sample may be extracted with water at pH 10 or greater, and the extract distilled and analyzed (e.g., by Methods 9010, 9012 and 9014). Samples that contain free water are filtered and separated into an aqueous component and a combined oil and solid component. The nonaqueous component may then be extracted, and an aliquot of the extract combined with an aliquot of the filtrate in proportion to the composition of the sample. Alternatively, the components may be analyzed separately, and cyanide levels reported for each component. However, if the sample solids are known to contain sufficient levels of cyanide (about 50 :g/g) as to be well above the limit of detection, the extraction step may be deleted and the solids distilled directly by the procedure found in Methods 9010 and 9012. This can be accomplished by diluting a small aliquot of the waste solid (1-10 g) in 500 mL of water in the distillation flask and suspending the slurry during distillation with a magnetic stir-bar.