USGS-NWQL: I-2546-91:  Nitrate and Nitrite in Low Ionic-Strength Water by Colorimetry

  • Summary
  • Analytes
  • Revision
  • Data and Sites
Official Method Name
Nitrogen, Nitrate Plus Nitrite, Low-Ionic Strength Water, Colorimetry, Cadmium Reduction - Diazotization, Automated-Segmented Flow
Current Revision
1993
Media
WATER
Instrumentation
Spectroscopy (Colorimetry; Photometry)
Method Subcategory
Inorganic
Method Source
  USGS-NWQL
Citation
M.J. Fishman, 1993, Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of inorganic and organic constituents in water and fluvial sediments: U.S. Geological Survey Open-File Report 93-125
Brief Method Summary
Nitrate is reduced to nitrite by cadmium metal. The sample stream then is treated with sulfanilamide under acidic conditions to yield a diazo compound, which couples with N-1-naphthylethylenediamine dihydrochloride to form an azo dye, the absorbance of which is measured colorimetrically. The result is the sum of the nitrite originally present plus that formed by the reduction of the nitrate (Morris and Riley, 1963; Brewer and Riley, 1965; Wood and others, 1967; Strickland and Parsons, 1972; Nydahl, 1976; Sherwood and Johnson, 1981; Patton, 1982; U.S. Environmental Protection Agency, 1983).
Scope and Application
This method is used to analyze samples of precipitation or natural water, containing from 0.005 to 1.0 mg/L of nitrite- plus nitrate-nitrogen. Concentrations greater than 1.0 mg/L must be diluted. This method was implemented in the National Water Quality Laboratory in March 1986 and modified in May 1989. See OFR 93-125 for additional modifications to the method.
Applicable Concentration Range
0.005 - 1.0 (undiluted)
Interferences
Concentrations of potentially interfering substances generally are negligible in unpolluted surface and ground water. For specific details of inorganic and organic compounds that interfere, see Norwitz and Keliher (1985, 1986) as well as more general information from the American Society for Testing and Materials (1991).
Sulfides, often present in anoxic water, rapidly deactivate cadmium reactors by forming an insoluble layer of cadmium sulfide on the active metal surface (Strickland and Parsons, 1972).
The buffer capacity of the imidazole solution and the approximate 10:1 volume ratio of buffer to sample eliminate the possibility of erroneous results for moderately acidic (pH greater than or equal to 1).
Quality Control Requirements
Quality-control samples area analyzed at a minimum of one in every ten samples. These QC samples include at least one of each of the following: blanks, quality control samples, third party check solutions, replicates, and spikes. Correlation coefficients for calibration curves must be at least 0.99. QC samples must fall within 1.5 standard deviations of the mean value. If all of the data-acceptance criteria in the SOPs are met, then the analytical data are acceptable.
Sample Handling
Description: 125 mL Brown polyethylene bottle. Treatment and Preservation: Filter through 0.45-um filter, use filtered sample to rinse containers, chill and maintain at 4oC, ship immediately.
Maximum Holding Time
30 days from sampling
Relative Cost
Less than $50
Sample Preparation Methods