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通过电感耦合等离子体发射光谱法测定铵态氮和有机结合态氮。

Determination of ammonium and organic bound nitrogen by inductively coupled plasma emission spectroscopy.

作者信息

Jaber A M Y, Mehanna N A, Sultan S M

机构信息

King Fahd University of Petroleum & Minerals, Chemistry Department, Dhahran 31261, Saudi Arabia.

出版信息

Talanta. 2009 Jun 15;78(4-5):1298-302. doi: 10.1016/j.talanta.2009.01.060. Epub 2009 Feb 10.

Abstract

The continuous flow sample introduction technique with a hydride generator system in conjunction with an inductively coupled plasma emission spectrometer (ICP-AES-HG), is used in this study for quantitative determination of ammonium and organic bound nitrogen in aqueous and solid samples. Ammonia vapor released from ammonium salt after treatment with concentrated NaOH is transferred by argon to plasma for detection at 174.273 nm using axial argon plasma mode. The calibration curves were linear within a range of 25-1000 mg L(-1)N as ammonium molybdate with correlation coefficients of better than 0.99 and limits of detection of about 10-25mg L(-1)N. The percent recovery of N (25-500 mg L(-1)N) in soft (distilled) water and high salt content (1.7 mol L(-1) NaCl) matrices was found to be in the range of about 97-102% with %RSD in the range of 4.6-0.62. The sensitivity, limit of detection, and blank contribution from the atmospheric nitrogen, were tremendously improved in this method compared with the available ICP-AES spray chamber counterpart. Furthermore, the ICP-AES-HG method gave results for real samples (soil, fertilizer, waste water) containing about 50-1800 mg L(-1)N in good agreement with those obtained by the standard Kjeldahl method. No statistical differences at the 95% confidence level on applying the t-test were observed between the values obtained by the two methods. Thus, the ICP-AES-HG method is reliable and faster than the conventional tedious Kjeldahl method, superior to the ICP-AES spray chamber method, and almost free from matrix interference which is usually a critical factor in atomic emission spectroscopic techniques.

摘要

本研究采用连续流动进样技术结合氢化物发生器系统与电感耦合等离子体发射光谱仪(ICP-AES-HG),对水相和固体样品中的铵态氮和有机结合氮进行定量测定。用浓氢氧化钠处理铵盐后释放出的氨气,由氩气转移至等离子体中,采用轴向氩等离子体模式在174.273nm处进行检测。以钼酸铵为标准物,在25 - 1000mg L⁻¹N范围内校准曲线呈线性,相关系数优于0.99,检测限约为10 - 25mg L⁻¹N。在软水(蒸馏水)和高盐含量(1.7mol L⁻¹NaCl)基质中,氮(25 - 500mg L⁻¹N)的回收率约为97 - 102%,相对标准偏差(%RSD)在4.6 - 0.62范围内。与现有的ICP-AES雾化室方法相比,该方法在灵敏度、检测限以及大气氮的空白贡献方面都有极大提高。此外,ICP-AES-HG方法对含氮量约为50 - 1800mg L⁻¹N的实际样品(土壤、肥料、废水)的测定结果与标准凯氏定氮法所得结果高度一致。两种方法所得值在95%置信水平下进行t检验时,未观察到统计学差异。因此,ICP-AES-HG方法可靠,比传统繁琐的凯氏定氮法更快,优于ICP-AES雾化室方法,且几乎不受基质干扰,而基质干扰通常是原子发射光谱技术中的关键因素。

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