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Combining submerged membrane technology with anaerobic and ...

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N-NO 3-(mg·L -1 )Chapter 2interfere. The determination should be promptly made on fresh samples in order to avoidbacterial conversions of NO 2- . At least filtration of the samples should be done immediatelyafter collection. For longer storage of unchlorinated samples (more than two days),preserve <strong>with</strong> 2 mL conc. H 2SO 4·L -1 <strong>and</strong> store at 4 ºC. When sample is preserved <strong>with</strong>acid, NO 3-<strong>and</strong> NO 2-cannot be determined as single species.543y = 5.04xR² = 1.002100.0 0.2 0.4 0.6 0.8 1.0absorbance 220nm- 2·absorbance 275nmFigure 2.5. Example of a calibration curve for nitrate concentration determination.2.1.2.4. Dissolved total nitrogen (DTN), dissolved organic nitrogen (DON) <strong>and</strong>dissolved inorganic nitrogen (DIN)DTN was determined in a total organic nitrogen analyzer (Rosemount-DohrmannDN-1900) equipped <strong>with</strong> a quimioluminiscence detector <strong>with</strong> two channels. One channeldetermines the DTN, by oxidation at high temperature, <strong>and</strong> the other determines the DIN,by a chemical reduction. DON is determined as the difference between DTN <strong>and</strong> DIN.All the nitrogen present in the water is catalytically oxidised to nitrous oxide (NO).The process for DTN determination occurs in two steps. The first step is a catalytic (Cu ascatalyst) oxidation in the combustion tube at 850°C <strong>and</strong> <strong>with</strong> pure oxygen (1 atm) ascarrier gas. The second one is the chemical reduction of residual NO 2 <strong>with</strong> H 2SO 4 at 80ºC<strong>and</strong> catalyzed by VaCl 3. For the DIN determination, only the second step (chemicalreduction) is used. The NO obtained in the two steps is dried <strong>and</strong> forced to react <strong>with</strong> O 3producing an unstable excited state NO 2*. The change back of this oxide to itsfundamental state releases a proton, from which the determination of DTN <strong>and</strong> DIN iscarried out by quimioluminiscence, using a multiplicator tube. The instrument is calibrated<strong>with</strong> a certified st<strong>and</strong>ard solution (KNO 3, 20 mg N·L -1 ) using a response factor method.70

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