An approach to improve the accuracy of sub-micron particle size distribution measurement using the Horiba CAPA-700

Bowen, Paul; Dirksen, James A.; Humphrey-Baker, Robin; Jelinek, L.

doi:10.1016/0032-5910(93)80009-y

Cited by 8 publications

(5 citation statements)

References 9 publications

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“…In order to apply the light scattering correction [7,11] it is required to have absorbance data with a good plateau of constant absorbance values at the beginning and an end point of zero. In none of the cases was it possible to collect all the data in one size range.…”

Section: Methodsmentioning

confidence: 99%

Particle Size Distribution Measurement and Assessment of Agglomeration of Commercial Nanosized Ceramic Particles

Staiger¹,

Bowen²,

Ketterer³

et al. 2002

Journal of Dispersion Science and Technology

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Commercially available powders with primary particle sizes of 10-100 nm (transition aluminas, Boehmites, and a commercially available silica dispersion) have been studied using three different instruments, a photocentrifuge (Horiba CAPA 700), photon correlation spectroscopy (PCS, Malvern Zetasizer 4), and an x-ray disc centrifuge (XDC, Brookhaven X-ray Disc Centrifuge BI-XDC). Particle size distributions for five powders were collected with each instrument and in conjunction with nitrogen adsorption measurements an agglomeration factor calculated. An example is given to show the importance of using a light scattering correction when measuring particle size distributions with a photocentrifuge for a gamma alumina powder where the uncorrected data can overestimate the D V50 by up to a factor of 10 depending on the powder. The importance of the assessment of agglomeration and how different treatments such as milling modifies the agglomeration factor F AG is illustrated for an ''as received'' and attrition milled gamma alumina. Results are discussed with respect to the assumptions and limitations of the different instruments. Results are presented after consideration of the hydrodynamic density in the sedimentation methods, and light scattering for the optical based methods. For narrow size distributions in the 15-25 nm range all three instruments show very a good correlation. When the size range approaches the 40-100 nm regime PCS is very sensitivity to small populations of agglomerates. The instrument giving the best resolution in the 10-100 nm range was found to be the XDC. The speed of measurement should also be born in mind and varies enormously from several minutes for the PCS to several hours for the sedimentation techniques. To assess the accuracy of the measured sizes a model spherical silica powder was analyzed on all the instruments as well as by image analysis. The results with the silica powder showed how the accuracy of the sedimentation methods depends strongly on a knowledge of the suspended particles hydrodynamic density. This can be effected greatly by particle or agglomerate porosity and the thickness of the electrical double layer in the aqueous dispersions investigated. The results with the silica suggest accuracy's on the size better than AE20% is difficult without an accurate hydrodynamic density whereas consistency between methods for narrow size distributions can be better than 5% for median volume diameters.

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Section: Methodsmentioning

confidence: 99%

Particle Size Distribution Measurement and Assessment of Agglomeration of Commercial Nanosized Ceramic Particles

Staiger¹,

Bowen²,

Ketterer³

et al. 2002

Journal of Dispersion Science and Technology

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“…The particle size distributions (PSD) of the precursor and ceramic powders were measured using a Horiba Capa 700 photo-centrifuge (without light scattering correction which will underestimate the finer fraction of the PSD [8]). The powders were dispersed in 2-propanol (Merck 818766) and treated for 5 min in an ultrasonic bath (Telsonic TUC 150).…”

Section: Characterisationmentioning

confidence: 99%

Preparation and analysis of aluminate sodalite ceramics from solution spray-dried precursors

Bowen

Daglish

Frenzer

et al. 1997

Journal of Thermal Analysis

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Aluminate sodalite ceramics, (Sre,(Al12024)(CrO4)2) -SACR, have been prepared from solution spray-dried precursors. The spray drying of a mixed aqueous nitrate solution gave an anhydrous powder which was thermally decomposed in air at 1350~ to give a crystalline SACR powder with a median volume diameter of 4-6 lam. The SACR powder was dry pressed and sintered to >90% density. The yellow SACR powder showed two phase transitions between 10 and 45~ with a 25 ~ intermediate phase region indicative of a low defect concentration in the crystalline structure. A colour change observed in the sintered ceramic (changing to a mixed green/yellow) and a narrowing of the phase transition region (15-40~ are discussed. Dielectric measurements were consistent with the presence of two extrinsic ferroelectric transitions at 17 and 35~

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“…Combining Eqs. (2) and (3), the flux can be written as or (5) This partial differential equation can be solved with the Lagrange charac te ristics [ 13], which yields the following equation:…”

Section: Theoretical Considerationsmentioning

confidence: 99%

“…As can be seen in Figure I, there is a dec rement that is not due to sedimentati on of parti cles, bu t to rad ial and tange nti al dilution effects because of th e speed gradi ent and tan genti al di spl ace ment, res pectively. Hence in the traditi onal approaches th e latter decrement is th ought to be due to sed imentati on of particles of give n size past th e detec ti on poin t. As a furth er result, the particle size di stri buti ons obtained by thi s erroneo us approach are always ta iling [5] . If Figure I is traditi onall y approached, the fracti on of parti cles th at are considered to be larger than 2 IJ.…”

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confidence: 95%

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A CONTIN‐Based Approach Towards the Data Analysis of Particle Sizing Experiments by Centrifugal Photosedimentometry

Putman¹,

Meeren²,

Vanderdeelen³

1997

Part & Part Syst Charact

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In order to analyse the output data of centrifugal photosedimentation experiments using CONTIN software, a mathematical model has been derived. This model is based on Fick's second law and describes the sedimentation behaviour of monomodal particles in a centrifugal field: it predicts that the extinction at the detection point decays exponentially until the particles are sedimented past the detection point, which gives a sharp drop of the curves to the baseline. In practice, however, a more fluently decaying profile was obtained. Simulations revealed that the polydispersity of the sample was responsible for this behaviour. When centrifugal photosedimentation data for effective monomodal and bimodal samples of fairly monodispersed PMMA lattices were analysed with CONTIN, using the model proposed, accurate particle size distributions were obtained, provided that the sample cell was completely filled. This was imperative in order to minimize the deviations of the practical application as compared with the theoretical model.

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An approach to improve the accuracy of sub-micron particle size distribution measurement using the Horiba CAPA-700

Cited by 8 publications

References 9 publications

Particle Size Distribution Measurement and Assessment of Agglomeration of Commercial Nanosized Ceramic Particles

Particle Size Distribution Measurement and Assessment of Agglomeration of Commercial Nanosized Ceramic Particles

Preparation and analysis of aluminate sodalite ceramics from solution spray-dried precursors

A CONTIN‐Based Approach Towards the Data Analysis of Particle Sizing Experiments by Centrifugal Photosedimentometry

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