The main distinction of our method for particle size distribution characterization is ability to treat concentrated systems as is, with no dilution. We achieve this by using Acoustic spectroscopy, which is described in the
International Standard ISO 20998-1:2006 “Measurement and characterization of particles by acoustic methods — Part 1: Concepts and procedures in ultrasonic attenuation spectroscopy”
There are four models having this capability: DT-1202 and DT-1210 (size and zeta potential) and DT-100 and DT-110 (size only). Models DT-1210 and DT-110 have disposable sample cell with small sample volume.
Particle size range is from 5 nm up to 1 mm. Particles content must be above 1 % with practically no upper limit.
Ability of Acoustic spectroscopy for characterizing concentrated dispersions and emulsions with no dilution and no sample preparation is critical in many cases when dilution affects particle size distribution. In addition, this method can be applied for structured dispersions. Structure contributes to ultrasound attenuation by itself, but this contribution can be subtracted using appropriate existing theory (see Newsletter #8). Acoustic spectroscopy could also resolve particle size distributions of different particles species in mixed dispersions, assuming that they have different densities (see Newsletter #6).
This method can be used for continuous monitoring of particle size during milling (see Newsletter #18), crystallization, and other industrial processes. One of the most important applications is particle sizing of nano-dispersions and other nano-particulates. Acoustics can monitor presence of nano-particles with precision of 1%, (see Newsletter #21). Nano-particles can be masked by larger particles if other methods are involved.
Accuracy test for nano-particles.
Results of this accuracy test are published in the paper: “Particle sizing and zeta potential of silica Koestrosol (Basis for Certified reference material ERM-FD100 for nano-particles) by Acoustics and Electroacoustics”, Part.Part. Syst. Charact., 27, pp.165-171 (2012). Here is the Abstract of this paper:
“….Precipitated silica Koestrosol 1530 is the basis for the recently adopted certified reference material ERM-FD100 used for nanotechnology. A similar reference material based on another precipitated silica (silica LudoxTM) has been used for testing ultrasound based instruments for particle sizing and zeta potential in concentrated dispersions and emulsions for the past two decades. In this study we test silica Koestrosol as a potential replacement for the silica LudoxTM since the latter has not been certified.
The measurements were performed using ultrasound based instruments, which were suitable for concentrated systems. Two laboratories (USA and Germany) with 3 different instruments were involved. Samples mass fraction was 5%. The statistically averaged mass-based median particle size was found to be 22.4 ±0.5 nm, which is within range of certified values obtained for more diluted samples.”
Accuracy test for micron size particles.
Accuracy test for micron size particles was conducted with a well known standard Silica Quartz BCR-70. Results are published in our book . Here we present a table from this book with median particle sizes for several materials having known reported particle size:
|Sample Material||Median Size (manufacturer data), microns||Median Size (acoustics), microns|
|Silica Ludox TM||0.022||0.028|
|Silica Geltech 1.5||1.5||1.55|
|Silica Geltech 0.5||0.5||0.53|
|Silica quartz BCR 70||2.9||2.85|
|Silica Cabot SS25||0.1||0.087|
|Rutile Dupont R746||0.3||0.31|
|Alumina Sumitiomo AKP-15||0.7||0.67|
|Alumina Sumitomo AKP-30||0.3||0.33|
|Zirconia TOSO TZ-3YS||0.3||0.34|
|Silicon Nitride Ube E-10||0.5||0.47|
Independence of the particle size on the weight fraction of solids.
When comparing our instrument with competing technologies / instruments claiming the same functionality, PLEASE be aware of necessity of having verification tests. Equilibrium dilution test is the most appropriate for characterizing concentrated systems. The tested instrument should provide the same value of the particle size and zeta potential for various volume fraction of the same concentrated system, IF dilution performed with the equilibrium supernate. Failure to provide such tests from the highest to the lowest limit of the claimed concentration range, means that such instrument is not validated.
Importance of the equilibrium dilution test has been stressed by International Standard ISO 13099-1 published in 2012.
We have conducted such tests with variety of dispersions. Results for concentrated TiO2 at 45.9% vl and Silica Ludox TM at 31.2% vl are presented in our book Dukhin, A.S. and Goetz, J.P. “Characterization of Liquids, Nano- and Microparticulates, and Porous Bodies using Ultrasound”, Edition 3, Elsevier, 571 pages, 765 references, (2017).