USGS-NWQL: I-4515-91:  Ammonium plus organic nitrogen, total

  • Summary
  • Analytes
  • Revision
  • Data and Sites
Official Method Name
Ammonium plus organic nitrogen, total
Current Revision
1991
Media
WATER
Instrumentation
Spectroscopy (Colorimetry; Photometry)
Method Subcategory
Inorganic
Method Source
  USGS-NWQL
Citation
Patton, C.J., and Truitt, E.P., 2000, Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory -- Determination if ammonium plus organic nitrogen by a Kjeldahl digestion method and an automated photometric finish that includes digest cleanup by gas diffusion: U.S. Geological Survey Open-File Report 00-170.
Brief Method Summary
Organic nitrogen is converted to ammonium ions at a temperature of 370oC in a reaction medium of sulfuric acid, potassium sulfate, and mercury (II). In principle, nitrate and nitrite are not reduced to ammonium ions under these conditions; USGS nomenclature refers to Kjeldahl nitrogen as ammonium plus organic nitrogen to emphasize this distinction. In practice, however, nitrate and nitrite might interfere positively or negatively.
An air-segmented continuous flow analyzer is used to automate the photometric determination of ammonium ions in resolvated Kjeldahl digests by the salicylate analog of the Berthelot reaction. Resolvated Kjeldahl digests often contain suspended particulates and ions that interfere with the photometric finish. Both classes of interferents are eliminated by means of an on-line gas diffusion cell, which consists of a continuous-flow, parallel-plate dialyzer assembly that replaces the dialysis membrane with a hydrophobic, microporous, polypropylene membrane. Gases pass through the microporous polypropylene membrane; particles and ions do not. Before passage through the gas diffusion cell, ammonium ions in acidic resolvated Kjeldahl digests mix with the alkaline donor stream and are converted to ammonia: NH4+(aq)plus-OH --> NH3(g) | + H2O.
Inside the diffusion cell, gas-phase ammonia in the donor stream passes through the polypropylene membrane and is trapped in the interferent-free recipient stream.
Scope and Application
This method is used to determine Kjeldahl nitrogen in water, drinking water, wastewater, brines, and water-suspended sediment. The suitability of this method for determination of Kjeldahl nitrogen in bottom materials has not been investigated.
Applicable Concentration Range
0.1 to 10.0
Interferences
In-line digest cleanup by gas diffusion eliminates all particulate and potential ionic interference in the photometric finish. Thus, resolvated digests containing suspended particulates do not require filtration prior to analytical determinations. Likewise, colorimetric reagents do not contain complexing agents, such as citrate, tartrate, or EDTA, that are required to prevent precipitation of calcium (II) and magnesium (II) in the alkaline analytical stream of methods that lack a gas-diffusion cleanup step.
Once samples have been acidified, they are subject to contamination by ammonia in the laboratory atmosphere. The digestion process, therefore, must be performed in a hood that is located in an ammonia-free area of the laboratory. Other analytical or housekeeping procedures with potential to contribute ammonia vapor to the laboratory atmosphere may not be performed in or near this hood. Avoid delays between sample preparation, sample digestion, and digest analyses to minimize the risk of ammonia contamination.
Nitrate can exert both a positive and negative interference in Kjeldahl nitrogen determinations. As stated by the American Public Health Association (1992, p. 4-94): During [Kjeldahl] digestion, nitrate in excess of 10 mg/L can oxidize a portion of the ammonia released from the digested organic nitrogen, producing N2O and resulting in a negative interference. When sufficient organic matter in a low state of oxidation is present, nitrate can be reduced to ammonia, resulting in a positive interference. The conditions under which significant interferences occur are not well defined and there is no proven way to eliminate the interference.
Quality Control Requirements
Calibrate instrument using calibration standards (CAL); quality control samples (QCS); and laboratory blanks (LB) analyzed at a minimum of 1 for every 10 samples.
Sample Handling
125mL WCA
Description: 125 mL Plain (translucent) polyethylene bottle, Use unfiltered sample to rinse bottles
Treatment and Preservation: acidify with 1 mL of 4.5N (4.5 normal) sulfuric acid (H2S04), chill and maintain at 4oC, ship immediately
Maximum Holding Time
30 days
Relative Cost
Less than $50
Sample Preparation Methods