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outlines criteria for selection of measurement systems. In addition, results are given for the measurement of particle-size distribution of a typical hydraulic cement in aqueous and nonaqueous liquid environment. A light diffraction technique was
used in these studies since it is not affected by density differences
of the particles.
~Group leader, Ceramics Division, and chemical engineer, respectively, National Institute of Standards and Technology, Gaithersburg,
MD.
1991 by the American Society for Testing and Materials
115
116
I Homogenization of Cement
I
I Sampllngfrom a LargeLot I
1
Preparationand
Dispersion ]
[ CalibratlonofInstrument]
l
1.-=-= I
I
Interpretationand
Conversion of Data
The potential for determining the particle-size distribution accurately depends on the ease with which the cement particles
Techniques
Measurement
Diameter
Nominal Range,
Ixm
Image
Optical
Electron
Image
Mechanical sieving
Dry
Wet
Sieve/mechnical
Sedimentation
Elutriation
Gravity
Centrifugal
Dynamic/
Stoke's
1-100
0.1-130
0.05-100
Zone sensing
Optical
Resistivity
Geometric
0.01 - 500
0,05-500
Hydrodynamic
chromatography
Geometric
0.0t-1.0
Brownian motion
Geometric
Equivalent
spherical
0.01-I
Other
Gas adsorption
Gas permeability
Mercury intrusion
0,5-1000
0.01 - 10
>10
>2
0.05-50
O.1-40
O.1- 200
-r.=-.-oo
[ ,,Presentationof Data [
FIG. 2--Sequence of steps involved in the measurement of particlesize distribution by wetting the cement.
terial consisting of chemical components of various sizes and
densities, segregation is a serious issue. Therefore, care should
be exercised in the division of a bulk lot of cement sample into
subsamples. Each type of instrument requires a different weight
of the sample. Errors in sampling can be minimized by using the
largest possible subsample for analysis consistent with the sample
requirement. For fine-size cements, wet samples of higher than
the required particle concentration can be prepared, and the final
sample for size determination can be taken from this parent
sample. When dilution of the parent sample is involved, the
surfactant concentration in the final dispersion should be maintained at the same level as in the parent sample.
Wetting and mixing of the powder requires the selection of a
proper combination of the solvent and a surfactant. Organic or
inorganic surfactants [6] can be used; however, organic dispersants provide higher flexibility and more definite dispersion in
complex chemical systems. Water is a preferred solvent, though
it has certain disadvantages, such as surface dissolution, swelling,
and setting. In dilute suspensions (less than 1% by weight), the
effects of these interactions are considered to be minimum.
The selection of an appropriate dispersant requires the knowledge of surface charge and isoelectric point, pH~ep (the pH at
which the particles carry a net zero charge) of the cement particles in a given solvent. Since cement has a highly complex
chemical composition, accurate determination of pHie p by traditional electrokinetic techniques is somewhat tedious and difficult. However, based on relative weight ratios of silicates, aluminates, and other components, the pHiep can be estimated.
Also, experimental determination of the pH~ep is possible by the
application of a relatively new technique in which electrokinetic
sonic amplitude is measured [7] as a function of pH.
Ultrasonication of the slurry containing the cement particles
is an essential step in the preparation of well-dispersed suspensions. During ultrasonication, the particles are subjected to cavitation which dislodges loosely held particles [8]. Two primary
devices of ultrasonication are baths and probes. The probe is a
preferred device because it allows the application of a specific
quantity of ultrasonic power localized to the sample. Ultrasonication by the probe is completed in just a few minutes since the
power intensity is high.
The size distribution of a well-dispersed slurry is determined
by following the recommended procedure of a particular equipment. If the suspension has to be diluted, the solvent chemistry
117
118
11
10
Cement in H20
9
rItc(3n
,m
0)
>
-)
c
Cement in IPA
-.-
Cement in A - 1 2
6
5
2
1
.'
.,;s"
0 ,-
1.0
0.1
10.0
100.0
different dgo. The overall differences in the entire size range are
presented in Fig. 4. These data, in terms of cumulative size
fraction, show that IPA is by far a superior solvent. The dg0, ds0,
and d25 data summarized in Table 2 show specific differences in
the size distributions. The size distribution data are presented in
terms of weight fraction by assuming that density variation between the particles is negligible.
tO0
Cement in H20
90
-
Q)
.E
ta_
.Cn
, m
Q)
80
70
"'"
." t/~/t
b,'
---- Cement in A - 1 2
." t~,/
60
." .i/1P
50
:;7
>
-.a,.,a
/ ~
/ Y
..' / /
20
- f~
jQ
1"
10
O,
0.1
1
1
1.0
10.0
Porticle Diometer, microns
I
100.0
FIG. 4--Size distribution data of Fig. 3 presented in the form of cumulative weight fraction to highlight
differences in the entire size distribution,
IPA
d9o
dso
dz5
19.0
9.0
3.6
Water
26.0
12.0
7.5
Water + Darvan C
30.0
13.0
7.5
A-12
30.0
it.0
5.0
CEMENT IN IPA
1
0
Sample I
9
C
cD
I,
cljn
{D
Sample
--'- S a m p l e 3
6
,5
.//
>
-
0
O.
1.0
119
'ii,
10.0
100.0
120
CEMENT IN A - 1 2
11
10
Sample
- Sample
c-
- - . - S a m p l e .3
b..
o~
,!
f.
/Z
3~
"
>
-{3
c"
~
~
O.1
1.0
10.0
100.0
References
[1] Allen, T. and Davies, R., "Modern Aspects of Particle Size Analysis," Advances in Ceramics, Vol. 21: Ceramic Powder Science,
G. L. Messing et at., Eds., American Ceramic Society, pp. 721746.
[2] Allen, T., Particle Size Measurement, 3rd ed., Chapman and Hall,
New York, 1981.
[3] Modern Methods of Particle Size Analysis, H. G. Barth, Ed., Wiley
Interscience, New York, 1984.
[4] Pohl, M., "Selecting a Particle Size Analyzer: Factors to Consider,"
Powder and Bulk Engineering, Vol. 4, No. 2, February 1990, pp.
26-29.
[5] Napper, D. H., Polymeric Stabilization of Colloidal Dispersions,
Academic Press, Inc., London, 1983, pp. 18-30.