Mc. Devargas et al., DETERMINATION OF TOTAL NITROGEN IN SEDIMENTS BY USING HIGH-PRESSURE BOMBS AND ION CHROMATOGRAPHY, Analyst, 120(3), 1995, pp. 761-763
The standard method for the determination of organic nitrogen in water
samples has in the past been based on Kjeldahl's digestion technique
which determines nitrogen in the triply negative state. In the presenc
e of sulfuric acid, potassium sulfate, mercuric sulfate and a catalyst
, amino nitrogen is converted to ammonium sulfate. Free ammonia and am
moniacal nitrogen are also converted to ammonium sulfate which can be
determined spectrophotometrically, or by titration with a standard min
eral acid. However, this method is time consuming and the accuracy is
variable. An alternative method for the determination of organic nitro
gen is the alkaline persulfate digestion technique which oxidizes all
the nitrogen in the sample to nitrate as the sole product using potass
ium persulfate in a strongly alkaline environment under high pressure
and temperature. In this paper, a methodology for total nitrogen deter
mination in sediments is developed using 23 ml high-pressure bombs wit
h potassium persulfate and sodium hydroxide. The determination of nitr
ogen as nitrate was made by using ion chromatography. Urea was used as
the nitrogenous compound to calibrate the methodology, which was chec
ked using the Kjeldahl method and showed good agreement.