EPA-NERL: 353.3:  Nitrate-Nitrite by Cadmium Reduction and Colorimetry

  • Summary
  • Analytes
  • Revision
  • Data and Sites
Official Method Name
Nitrogen, Nitrate-Nitrite (Spectrophotometric, Cadmium Reduction)
Current Revision
Issued 1974
Media
WATER
Instrumentation
Spectroscopy (Colorimetry; Photometry)
Method Subcategory
Inorganic
Method Source
  EPA-NERL
Citation
  Methods for the Chemical Analysis of Water and Wastes (MCAWW) (EPA/600/4-79/020)
Brief Method Summary
Nitrate and nitrite: A filtered sample is passed through a column containing granulated copper-cadmium to reduce nitrate to nitrite. The nitrite (originally in the sample and reduced nitrate) is determined by diazotizing with sulfanilamide and coupling with N-(1-naphthyl)-ethylenediamine dihydrochloride to form a highly colored azo dye, which is measured with a spectrometer.
Nitrite alone: The procedure is the same except that the cadmium column is bypassed.
Scope and Application
This method determines nitrite singly or nitrate and nitrite combined in drinking, surface, and saline waters, domestic and industrial wastes.
Applicable Concentration Range
0.01 to 1.0 mg/L Nitrate-nitrite nitrogen.
Interferences
(A) Suspended matter: Suspended materials will fowl the reduction column and restrict sample flow. Pretreat by filtering the sample through a 0.45 um filter or (for highly turbid samples) pretreating with zinc sulfate before filtration.
(B) Metals: Metals like iron or copper can produce low results. Treat samples with EDTA to remove this interference.
(C) Oil and grease: Oil and grease, that can coat the column and reduce efficiency should be removed by pre-extracting the sample with an organic solvent.
Quality Control Requirements
None.
Sample Handling
If analysis can be made within 24 hours, refrigerating samples at 4oC is sufficient. If samples are kept more than 24 hours, preserve with 2 mL of sulfuric acid per liter of sample and refrigerate.
Do not preserve sample with mercuric chloride if they will be run through the reduction column.
Maximum Holding Time
28 Days (nitrate+nitrite)
48 hours (nitrate or nitrite, singly)
(MCAWW, Table 1).
Relative Cost
Less than $50
Sample Preparation Methods
None.