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大气湿沉降和干沉降样品中总氮的测定

Determination of total nitrogen in atmospheric wet and dry deposition samples.

作者信息

Karthikeyan Sathrugnan, He Jun, Palani Sundarambal, Balasubramanian Rajasekhar, Burger David

机构信息

Division of Environmental Science and Engineering, National University of Singapore, Singapore.

出版信息

Talanta. 2009 Jan 15;77(3):979-84. doi: 10.1016/j.talanta.2008.07.053. Epub 2008 Aug 5.

Abstract

A microwave-assisted persulfate oxidation method followed by ion chromatographic determination of nitrate was developed for total nitrogen determination in atmospheric wet and dry deposition samples. Various operating parameters such as oxidation reagent concentrations, microwave power, and extraction time were optimized to maximize the conversion of total nitrogen to nitrate for subsequent chemical analysis. Under optimized conditions, 0.012 M K(2)S(2)O(8) and 0.024 M NaOH were found to be necessary for complete digestion of wet and dry deposition samples at 400 W for 7 min using microwave. The optimized extraction method was then validated by testing different forms of organic nitrogen loaded to pre-baked filter substrates and NIST SRM 1648 (urban particulate matter), and satisfactory results were obtained. In the case of wet deposition samples, standard addition experiments were performed. The suitability of the method for real-world application was assessed by analyzing a number of wet and dry deposition samples collected in Singapore during the period of March-April 2007. The organic nitrogen content was 15% (wet) and 30% (dry) of the total nitrogen. During the study period, the estimated wet fluxes for nitrate (NO(3)(-)), ammonium (NH(4)(+)), organic nitrogen (ON), and total nitrogen (TN) were 16.1+/-6.5 kg ha(-1)year(-1), 11.5+/-5.7 kg ha(-1)year(-1), 3.8+/-1.5 kg ha(-1)year(-1)and 31.5+/-13.2 kg ha(-1)year(-1), respectively, while the dry fluxes were 2.5+/-0.8 kg ha(-1)year(-1), 1.4+/-0.9 kg ha(-1)year(-1), 2.3+/-1.4 kg ha(-1)year(-1) and 7.5+/-2.6 kg ha(-1)year(-1), respectively.

摘要

建立了一种微波辅助过硫酸盐氧化法,随后采用离子色谱法测定硝酸盐,用于大气湿沉降和干沉降样品中的总氮测定。对氧化试剂浓度、微波功率和萃取时间等各种操作参数进行了优化,以最大限度地将总氮转化为硝酸盐,便于后续化学分析。在优化条件下,发现使用微波在400W功率下处理7分钟时,0.012M的K₂S₂O₈和0.024M的NaOH对于完全消解湿沉降和干沉降样品是必要的。然后通过测试加载到预烘烤滤膜基质上的不同形式的有机氮和NIST SRM 1648(城市颗粒物)对优化后的萃取方法进行验证,获得了满意的结果。对于湿沉降样品,进行了标准加入实验。通过分析2007年3月至4月期间在新加坡采集的一些湿沉降和干沉降样品,评估了该方法在实际应用中的适用性。有机氮含量分别占总氮的15%(湿沉降)和30%(干沉降)。在研究期间,硝酸盐(NO₃⁻)、铵(NH₄⁺)、有机氮(ON)和总氮(TN)的估计湿沉降通量分别为16.1±6.5 kg ha⁻¹年⁻¹、11.5±5.7 kg ha⁻¹年⁻¹、3.8±1.5 kg ha⁻¹年⁻¹和31.5±13.2 kg ha⁻¹年⁻¹,而干沉降通量分别为2.5±0.8 kg ha⁻¹年⁻¹、1.4±0.9 kg ha⁻¹年⁻¹、2.3±1.4 kg ha⁻¹年⁻¹和7.5±2.6 kg ha⁻¹年⁻¹。

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