Hl. Demedina et al., DETERMINATION OF TOTAL NITROGEN IN WATER SAMPLES BY MEANS OF HIGH-PRESSURE BOMBS AND ION CHROMATOGRAPHY, Journal of chromatography, 671(1-2), 1994, pp. 287-293
The standard method for the determination of organic nitrogen in water
samples in the past has been based on the Kjeldahl digestion techniqu
e that converts organic nitrogen into ammonia, which can then be deter
mined along with any ammonia originally present. However, this method
is time consuming and the accuracy is variable because the effect of i
nterferences causes unreliable results, especially in complex matrices
. An alternative method for the determination of organic nitrogen is t
he alkaline peroxodisulphate digestion technique. This oxidizes all ni
trogen in the sample using potassium peroxodisulphate in a strongly al
kaline environment under high pressure and temperature. Nitrate is the
sole product and can easily be determined by ion chromatography or by
other methods (e.g., cadmium reduction method). A method for total ni
trogen determination was developed using 23-ml high-pressure bombs wit
h potassium peroxodisulphate and sodium hydroxide to oxidize the organ
ic nitrogen to nitrate. Urea and ammonium chloride were used as nitrog
en compounds for calibration. The method was checked with the Kjeldahl
method, showing good agreement (R.S.D. = 4.62%). Studies of digestion
time were carried out to determine the optimum time in the pressure v
essel. The results were checked with the cadmium reduction method (R.S
.D. = 3.62%) for natural water samples. The recoveries with urea and a
mmonium chloride reagents were higher than 90%.