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使用紫外可见吸收光谱法测定水性分散液中单壁碳纳米管的浓度。

Determination of the concentration of single-walled carbon nanotubes in aqueous dispersions using UV-visible absorption spectroscopy.

作者信息

Attal S, Thiruvengadathan R, Regev O

机构信息

Department of Chemical Engineering and Ilse Katz Center for Meso- and Nanoscale Science and Technology, Ben-Gurion University of the Negev, Beer Sheva 84105, Israel.

出版信息

Anal Chem. 2006 Dec 1;78(23):8098-104. doi: 10.1021/ac060990s.

Abstract

Stable, homogeneous, aqueous dispersions of single-walled carbon nanotubes (SWNTs) are prepared by nonspecific physical adsorption of surfactants enhanced by sonication. Upon centrifugation, supernatant and precipitate phases are obtained. The initial weights of the SWNTs and the surfactant are divided between these two phases, and the respective SWNT concentration in each phase is unknown. The focus of this work is on the determination of the true concentration of raw, exfoliated HiPCO SWNTs in the supernatant phase. A UV-visible absorption-based approach is suggested for a direct measurement of the SWNT and the surfactant concentration in the supernatant. UV-visible absorbance spectra of SWNTs-surfactant dispersions and surfactants alone reveal that the intensity of a certain peak, attributed to the pi-plasmon resonance absorption, is unaffected by the presence of most surfactants. A calibration plot is then made by monitoring the intensity of the peak as a function of the true concentration of the exfoliated SWNTs. Thus, we are able to determine the unknown concentration of surfactant-dispersed HiPCO SWNTs in the supernatant solution, simply by measuring its optical absorbance. Moreover, we can now calculate the surfactant efficiency in dispersing SWNTs. Cryogenic-transmission electron microscopy and thermogravimetric analysis techniques are used for the characterization of these dispersions and to complement the UV-visible measurements.

摘要

通过超声强化的表面活性剂非特异性物理吸附制备了单壁碳纳米管(SWNTs)的稳定、均匀的水分散体。离心后,得到上清液相和沉淀相。SWNTs和表面活性剂的初始重量在这两个相之间分配,并且每个相中各自的SWNT浓度未知。这项工作的重点是测定上清液相中原始剥落的HiPCO SWNTs的真实浓度。建议采用基于紫外可见吸收的方法直接测量上清液中SWNT和表面活性剂的浓度。SWNTs-表面活性剂分散体和单独表面活性剂的紫外可见吸收光谱表明,归因于π-等离子体共振吸收的某个峰的强度不受大多数表面活性剂存在的影响。然后通过监测该峰的强度作为剥落的SWNTs真实浓度的函数来制作校准曲线。因此,我们能够通过简单地测量其吸光度来确定上清液中表面活性剂分散的HiPCO SWNTs的未知浓度。此外,我们现在可以计算表面活性剂在分散SWNTs方面的效率。低温透射电子显微镜和热重分析技术用于表征这些分散体并补充紫外可见测量。

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