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通过激光衍射法对亚微米颗粒进行尺寸分析——已发表的测量结果中有90%是错误的。

Size analysis of submicron particles by laser diffractometry--90% of the published measurements are false.

作者信息

Keck Cornelia M, Müller Rainer H

机构信息

Department of Pharmaceutical Technology, Biopharmaceuticals & NutriCosmetics, Free University of Berlin, Kelchstrasse 31, 12161 Berlin, Germany.

出版信息

Int J Pharm. 2008 May 1;355(1-2):150-63. doi: 10.1016/j.ijpharm.2007.12.004. Epub 2007 Dec 15.

Abstract

The first part of this paper gives an easy and understandable introduction into modern laser diffractometry (LD). It explains why modern laser diffractometry is not only the simple detection of a diffraction pattern but a combination of two independent technologies, which is done to extend the measuring range down to several nanometers and incorrectly named LD measurement. In the second part the impact of the optical parameters on the result analysed was investigated. The results show, that changes in optical parameters change the particle size and the size distribution tremendously. For a trimodal mixture of latex particles, having a mean particle size of 845nm, mean particle sizes ranging from 284nm to up to 1.005microm were obtained due to the variation of the optical parameters. The obtained particle size distributions varied from monomodal, bimodal over trimodal to even tetramodal distributions. The results prove that the analysis of submicron particles is meaningless, if incorrect optical models are applied. Another hazard was found to be the use of the additional techniques for the extension to the submicron measuring range. Combining this technology with laser diffraction can fail to detect larger particles besides a small sized main population. This can be overcome by analyzing the samples also without the additional technology, i.e. using laser diffraction only. From the results it is concluded that laser diffractometry for submicron particles is only useful if correct optical parameters are applied and if the presence of larger particles is investigated without the enhanced submicron measuring range.

摘要

本文的第一部分对现代激光衍射技术(LD)进行了通俗易懂的介绍。它解释了为什么现代激光衍射技术不仅仅是简单地检测衍射图案,而是两种独立技术的结合,这样做是为了将测量范围扩展到几纳米,且这种技术被错误地称为LD测量。在第二部分中,研究了光学参数对所分析结果的影响。结果表明,光学参数的变化会极大地改变颗粒尺寸和尺寸分布。对于平均粒径为845nm的乳胶颗粒三峰混合物,由于光学参数的变化,得到的平均粒径范围为284nm至1.005微米。所获得的粒度分布从单峰、双峰、三峰甚至到四峰分布都有。结果证明,如果应用不正确的光学模型,对亚微米颗粒的分析是没有意义的。另一个风险是使用扩展到亚微米测量范围的附加技术。将该技术与激光衍射相结合,除了一小部分主要的小尺寸颗粒外,可能无法检测到较大的颗粒。这可以通过在不使用附加技术的情况下分析样品来克服,即仅使用激光衍射。从结果可以得出结论,对于亚微米颗粒的激光衍射技术,只有在应用正确的光学参数且在不使用增强的亚微米测量范围的情况下研究较大颗粒的存在时才有用。

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