Mulholland G W, Hartman A W, Hembree G G, Marx Egon, Lettieri T R
National Bureau of Standards, Gaithersburg, MD 20899.
J Res Natl Bur Stand (1977). 1985 Jan-Feb;90(1):3-26. doi: 10.6028/jres.090.001.
The average diameter of the first micrometer particle size standard (Standard Reference Material 1690), an aqueous suspension of monosized polystyrene spheres with a nominal 1 μm diameter, was accurately determined by three independent techniques. In one technique the intensity of light scattered by a diluted suspension of polystyrene spheres was measured as a function of scattering angle, using a He-Ne laser polarized in the vertical direction. The second technique consisted of measuring as a function of angle the intensity of light scattered from individual polystyrene spheres suspended in air, using a He-Cd laser with light polarized parallel and perpendicular to the scattering plane. The measurement of row length by optical microscopy for polystyrene spheres arranged in close-packed, two-dimensional hexagonal arrays was the basis of the third technique. The measurement errors for each technique were quantitatively assessed. For the light scattering experiments, this required simulation with numerical experiments. The average diameter determined by each technique agreed within 0.5% with the most accurate value being 0.895±0.007 μm based on light scattering by an aqueous suspension. Transmission electron microscopy, flow through electrical sensing zone counter measurements, and optical microscopy were also used to obtain more detailed information on the size distribution including the standard deviation (0.0095 μm), fraction of off-size particles, and the fraction of agglomerated doublets (1.5%).
通过三种独立技术精确测定了首个微米级粒径标准物质(标准参考物质1690)的平均直径,该标准物质是标称直径为1μm的单分散聚苯乙烯球的水悬浮液。在一种技术中,使用垂直偏振的氦氖激光,测量稀释后的聚苯乙烯球悬浮液散射光的强度,并将其作为散射角的函数。第二种技术是使用氦镉激光,其光在平行和垂直于散射平面的方向上偏振,测量悬浮在空气中的单个聚苯乙烯球散射光的强度,并将其作为角度的函数。通过光学显微镜测量紧密排列的二维六边形阵列中的聚苯乙烯球的行长,是第三种技术的基础。对每种技术的测量误差进行了定量评估。对于光散射实验,这需要通过数值实验进行模拟。每种技术测定的平均直径与最准确值的偏差在0.5%以内,基于水悬浮液光散射的最准确值为0.895±0.007μm。还使用透射电子显微镜、流通式电感应区计数器测量和光学显微镜来获取有关尺寸分布的更详细信息,包括标准偏差(0.0095μm)、尺寸不符颗粒的比例和团聚双峰的比例(1.5%)。