Vandenbruwane Jeroen, Neve Stefaan De, Qualls Robert G, Salomez Joost, Hofman Georges
Department of Soil Management and Soil Care, Division of Soil Fertility and Nutrient Management, Ghent University, Coupure Links 653, 9000 Ghent, Belgium.
Sci Total Environ. 2007 Nov 1;386(1-3):103-13. doi: 10.1016/j.scitotenv.2007.06.025. Epub 2007 Jul 20.
Since dissolved organic nitrogen (DON) concentrations in aqueous samples can only be determined by the subtraction of three independently measured concentrations (total dissolved nitrogen (TDN), nitrate and ammonium), analytical errors are compounded in the calculation of DON concentration. Several methods were tested to increase the recovery and precision of the DON determinations in aqueous samples with high inorganic nitrogen concentrations. The first step was the objective selection of the most accurate TDN analysis method. The persulfate oxidation (PO) method had a significantly higher recovery than the high-temperature catalytic oxidation (HTCO) method. The second step involved the lowering of the DIN (dissolved inorganic N)/TDN ratio by applying three sample pretreatment procedures: conventional dialysis, dialysis against a buffered acceptor solution and concentration of the samples combined with the buffered dialysis. Despite the fact that DIN was only partially removed, conventional dialysis pretreatment resulted in higher precision and recovery of the DON determination compared to analysis of untreated samples. Dialysis of the samples against a buffered acceptor solution gave additional improvements in precision, recovery, and reproducibility. The concentration of aqueous samples by lyophilization, however, did not lead to higher recovery rates in the DON measurements.
由于水样中溶解有机氮(DON)的浓度只能通过减去三个独立测量的浓度(总溶解氮(TDN)、硝酸盐和铵)来确定,因此在计算DON浓度时分析误差会叠加。测试了几种方法以提高高无机氮浓度水样中DON测定的回收率和精密度。第一步是客观选择最准确的TDN分析方法。过硫酸盐氧化(PO)法的回收率明显高于高温催化氧化(HTCO)法。第二步是通过应用三种样品预处理程序来降低溶解无机氮(DIN)/TDN比值:传统透析、用缓冲受体溶液透析以及将样品浓缩与缓冲透析相结合。尽管DIN只是部分被去除,但与未处理样品的分析相比,传统透析预处理提高了DON测定的精密度和回收率。用缓冲受体溶液对样品进行透析在精密度、回收率和重现性方面有进一步改善。然而,通过冻干对水样进行浓缩并没有提高DON测量的回收率。