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Introduction

Cement can be a problematic material in the application of particle size analysis. First, the size distribution itself is extremely broad, extending in most cases over two to three orders of magnitude, from about 100 µm down to below micrometer size. In general, sizing techniques work best over a limited size range. The optimum range of particle size analysis varies according to a number of factors, including detector sensitivity and the assumptions associated with the underlying principle of measurement. Second, cement particles are highly agglomerated in the dry state, and therefore must be properly dispersed in order to determine the "true" particle size distribution (PSD). Standard protocols for dispersing cement particles prior to analysis by wet methods are nonexistent, and the degree of dispersion achieved in dry dispersion (air) methods will likely vary depending on the method used, the geometry of the dispersing device, the residence time in the sensing zone and the applied shear force employed to separate physically agglomerated particles. This introduces a potentially large source of variation at the sample preparation stage. Third, cement particles are typically irregular in shape and inhomogeneous in composition. Most commercial methods (see Table 1) are designed specifically for, or work best with, homogeneous spheres. The degree to which irregularity affects the results vary with technique, and is generally not well understood or accounted for properly n in many methods.

A universally recognized standard method for characterizing the complete PSD of cement particles does not currently exist [2]. The only standard test, ASTM C115 [1] (also known as the Wagner test), is really designed to measure the "fineness" of a cement powder and it is limited to a minimum particle size of 7.5 µm. As there is no standard procedure covering the whole range of cement PSD, the implementation of different measurement methods varies widely within the industry. Therefore, there is the necessity of having a method in which cement is used as a standard. Other potential sources of variability in sizing methods include adjustable instrument parameters or material property data required as inputs, and fundamental differences due to the nature of the technique itself. In the latter case, it must be acknowledged that different methods may "sense" a different aspect of the size distribution. For instance, a given method may be sensitive to either particle mass, particle number or projected surface area. As a result, for a polydisperse system, each method produces a distribution with a slightly different weighting. Thus the "mean" particle diameter values are expected to differ.

ASTM committee C01.25.01 sponsored a round-robin test to measure the PSD of cement. The scope of this report is to analyze the data generated during those tests and to summarize various methodologies available. The analysis of the data is conducted in two parts:

 

Table 1: Particle size measurement methods commonly used in characterizing fine inorganic powders.
Method1 Abbrev. Underlying Principle Applicable
Size Range2
(µm)
LASER Diffraction
[Fraunhofer Diffraction, Mie Scattering, LASER Light Scattering, Elastic Light Scattering]
Dry method (-D)
Wet method (-W)
LAS electromagnetic wave
interaction
0.1 - >100
Quasi-Elastic Light Scattering
[Dynamic Light Scattering, Photon Correlation
Spectroscopy, Optical Beating Spectroscopy]
Heterodyne method
Homodyne method
QELS electromagnetic wave
interaction
0.005-2
Small Angle Neutron Scattering
Ultra-Small Angle Neutron Scattering
SANS

USANS

wave interaction 0.001 - 10
Small Angle X-Ray Scattering
Ultra-Small Angle X-Ray Scattering
SAXS
USAXS
electromagnetic wave
interaction
0.001 - 31
LASER Doppler Velocimetry
[LASER Doppler Anemometry]
LDV aerodynamics &
electromagnetic scattering
0.5 - 10
[Coulter Principle, Coulter Counter] EZS volume displacement 0.4 - >100
Differential Mobility Analysis DMA electrostatic
classification
0.005 - 1
Scanning Electron Microscopy
Field Emission SEM
SEM
FE-SEM
imaging 0.02 - 10
Transmission Electron Spectroscopy TEM imaging 0.01 - 0.5
X-Ray Gravitational Sedimentation XGS sedimentation 0.5 - 100
Optical Centrifugal Sedimentation OCS sedimentation 0.01 - >5
X-Ray Centrifugal Sedimentation XCS sedimentation 0.01 - >5
Sedimentation Field Flow Fractionation SdFFF sedimentation classification 0.03 - >1
Sieving - size exclusion 2 - >100
Gas Adsorption Surface Area Analysis
[Brunauer-Emmet-Teller]
BET surface area no limit
Acoustic Attenuation Spectroscopy
[Ultrasonic Attenuation Spectroscopy, Ultrasonic
Spectroscopy]
Coupled phase theory
Scattering theory
Multiple scattering theory
AAS acoustic wave interaction 0.025 - >100
Electroacoustic Spectroscopy
[Electrokinetic Sonic Amplitude]
ESA electroacoustic response 0.1 - 10

1Terms in brackets represent other names by which the method is commonly known and/or closely related techniques that have been grouped together under a single general method. Indented terms represent specific variants, implementations or theoretical constructs used to analyze measurement results.

2Size ranges are approximate and provide the extreme limits attainable, given access to all commercially available adaptations of that method. Actual size ranges may vary significantly between instruments and may depend on the test material.


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