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首页> 外文期刊>Journal of Analytical Atomic Spectrometry >Characterization of solid magnetic nanoparticles by means of solid sampling high resolution continuum source electrothermal atomic absorption spectrometry
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Characterization of solid magnetic nanoparticles by means of solid sampling high resolution continuum source electrothermal atomic absorption spectrometry

机译:固体样品高分辨率连续谱源电热原子吸收光谱法表征固体磁性纳米粒子

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摘要

Magnetic nanopartictes (MNPs) are a new kind of nanometer-sized superparamagnetic material with potential applications as magnetic carriers for various biomedical uses, wastewater remediation, preconcentration of various anions and cations, etc. The excellent properties of MNPs are strongly influenced by the size of the nanoparticles. Another important factor is the amount of iron present. In this work, a simple and inexpensive approach was developed for the direct determination of the Fe concentration and particle size of solid MNPs by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). A new strategy of evaluating the area and upslope of the obtained absorbance signals for a line of Fe (352.614 nm) with low sensitivity was developed for both determinations. For this purpose, five furnace program parameters, atomization heating rate, atomization temperature, pyrolysis heating rate, pyrolysis temperature and pyrolysis hold time, were optimized with the employment of two multiple response surface designs. With the optimized furnace parameters, satisfactory calibration curves were obtained with liquid iron standards (for Fe determination) (R ≥ 0.995) and with MNP samples with a certified size of particle (for size particle determination) (R ≥ 0.990). The determinations of the MNPs' size and their iron percentage were validated by transmission electron microscopy (TEM) and scanning electron microscopy (SEM), respectively. This method can be employed in the optimization of the synthesis of MNPs by the coprecipitation method.
机译:磁性纳米颗粒(MNPs)是一种新型的纳米级超顺磁性材料,具有潜在的用途,可作为各种生物医学用途的磁载体,废水修复,各种阴离子和阳离子的预浓缩等。MNPs的优异性能受其大小的强烈影响。纳米粒子。另一个重要因素是铁的含量。在这项工作中,开发了一种简单而廉价的方法,可通过固体采样高分辨率连续谱源石墨炉原子吸收光谱法(HR CS GFAAS)直接测定固体MNP的铁浓度和粒径。对于这两种测定方法,开发了一种新的策略来评估低灵敏度的Fe(352.614 nm)线所获得的吸光度信号的面积和上坡度。为此,利用两个多重响应表面设计优化了五个炉程序参数,雾化加热速率,雾化温度,热解加热速率,热解温度和热解保持时间。通过优化的熔炉参数,使用铁水标准品(用于铁的测定)(R≥0.995)和具有经认证的颗粒尺寸的MNP样品(用于粒径的测定)(R≥0.990)可获得令人满意的校准曲线。 MNP的大小和铁含量的测定分别通过透射电子显微镜(TEM)和扫描电子显微镜(SEM)进行了验证。该方法可用于通过共沉淀法优化MNP的合成。

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  • 来源
    《Journal of Analytical Atomic Spectrometry》 |2016年第12期|2391-2398|共8页
  • 作者单位

    Department of Analytical Chemistry, Faculty of Sciences, University of Malaga, Campus of Teatinos, 29071 Malaga, Spain;

    Department of Analytical Chemistry, Faculty of Sciences, University of Malaga, Campus of Teatinos, 29071 Malaga, Spain;

    Department of Analytical Chemistry, Faculty of Sciences, University of Malaga, Campus of Teatinos, 29071 Malaga, Spain;

    Department of Analytical Chemistry, Faculty of Sciences, University of Malaga, Campus of Teatinos, 29071 Malaga, Spain;

    Department of Analytical Chemistry, Faculty of Sciences, University of Malaga, Campus of Teatinos, 29071 Malaga, Spain;

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