EPA-RCA: 7470A:  Mercury by Manual Cold-Vapor Technique

  • Summary
  • Analytes
  • Revision
  • Data and Sites
Official Method Name
Mercury in Liquid Waste (Manual Cold-Vapor Technique)
Current Revision
Revision 1, September 1994
Media
VARIOUS
Instrumentation
Cold Vapor Atomic Absorption
Method Subcategory
Organic+Inorganic
Method Source
  EPA-RCA
Citation
  SW-846 Online: Test Methods for Evaluating Solid Waste, Physical/Chemical Methods
Brief Method Summary
Aqueous samples are digested with sulfuric acid, nitric acid, potassium permanganate, and potassium persulfate in order to oxidize the organo-mercury compounds to the mercuric ion. Once the digested samples have cooled, sodium chloride-hydroxylamine sulfate is added to reduce excess permanganate. Stannous sulfate is then added to the samples for the reduction to elemental mercury which is immediately measured by a cold-vapor atomic absorption spectrophotometer (or equivalent instrument).
Scope and Application
This method determines the concentration of mercury in aqueous wastes, mobility-procedure abstracts, and ground water. It can also be used for analyzing certain solid and sludge-type wastes, however, Method 7471 is recommended for these matrices.
Applicable Concentration Range
Not Available.
Interferences
(A) Matrix interferences: Sulfide as sodium sulfide may possibly interfere with mercury, however, potassium permanganate is added to eliminate interferences from concentrations as high as 20 mg/L. Copper is also known to cause interference, however, concentrations as high as 10 mg/L have shown to have no effect on mercury recovery. Seawaters, brines, and industrial effluents high in chlorides require additional amounts of permanganate and hydroxylamine sulfate to ensure the absence of free chlorine which interfere with mercury detection. In addition, air space in the BOD bottle must be purged before adding stannous chloride. Certain volatile organic compounds may also cause interference. A preliminary run without reagents should determine their presence.
Quality Control Requirements
Refer to section 8.0 of Method 7000.
Sample Handling
Aqueous samples must be acidified to a pH < 2 with nitric acid. Non-aqueous samples shall be refrigerated and analyzed as soon as possible.
Maximum Holding Time
Preserved samples: 28 days.
Relative Cost
$51 to $200
Sample Preparation Methods
Method 7470A