Characterization of particles made by desolvation of monodisperse microdroplets of analyte solutions and particle suspensions for nanoparticle calibration in inductively coupled plasma spectrometry
Characterization of particles made by desolvation of monodisperse microdroplets of analyte solutions and particle suspensions for nanoparticle calibration in inductively coupled plasma spectrometry
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DOI：
10.1016/j.sab.2009.11.002
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发表时间：
2010-01-01
影响因子：
3.3
通讯作者：
Niemax, Kay
中科院分区：
文献类型：
--
作者：
Garcia, Carmen C.;Murtazin, Ayrat;Niemax, Kay
在硅片上收集了分析物标准溶液的单分散微滴低温解溶产生的粒子和纳米粒子悬浮液，并用扫描电子显微镜和X射线微探针技术对其进行了研究。在150摄氏度左右的去溶温度下，来自标准溶液的颗粒通常是球形和固体的，具有良好的重现性，分析元素以及来自微量污染的不可避免的伴随元素似乎均匀地分布在颗粒中。然而，也有令人惊讶的例外，特别是在较高的温度下，分析元素通过还原或结晶在颗粒中分离，如金和钙标准溶液分别显示的那样。在200摄氏度下干燥250纳米金颗粒的稀释悬浮液液滴，发现了另一个有趣的结果，即产生了直径类似于3微米的相对稳定的凹形气球，其中包括金颗粒。气球护套是由悬浮液中的污染元素组成的化合物形成的。在考虑Peclet数、蒸发速率与分析物扩散系数之比的情况下，讨论了颗粒的形态。讨论了在用电感耦合等离子体光谱仪进行纳米颗粒表征时，用于校准目的的颗粒大小和形貌的影响。(C)2009爱思唯尔B.V.保留所有权利。
Particles produced by low-temperature desolvation of monodisperse microdroplets of analyte standard Solution and nanoparticle suspensions in argon were collected on Si-wafers and studied applying scanning electron microscopy and X-ray microprobe techniques. At desolvation temperatures of about 150 degrees C, the particles from standard solutions are most often spherical and solid with good reproducibility and the analyte elements together with the unavoidable accompanying elements from trace contamination seem to be homogeneously distributed in the particles. However, there are surprising exceptions, particularly at higher temperatures, where analyte elements are separated in the particle by reduction or crystallization, as shown with Au and Ca standard solutions, respectively. Drying droplets of a diluted suspension of 250 nm gold particles at 200 degrees C revealed another interesting result, the production of relatively stable concave balloons of similar to 3 mu m in diameter including the Au particles. The balloon sheath was formed of compounds made of the contaminant elements in the suspension. The morphology of the particles is discussed in consideration of the Peclet number, the ratio of evaporation rate to analyte diffusion coefficient. The consequences of particle size and morphology for calibration purposes in nanoparticle characterization by ICP spectrometry are discussed. (C) 2009 Elsevier B.V. All rights reserved.