Characterization of Powder Flowability Using Measurement of Angle of Repose

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CHINA PARTICUOLOGY Vol. 4, Nos.

3-4, 104-107, 2006

CHARACTERIZATION OF POWDER FLOWABILITY USING


MEASUREMENT OF ANGLE OF REPOSE
D. Geldart1,*, E. C. Abdullah2, A. Hassanpour3, L. C. Nwoke3 and I. Wouters4
1
Department of Chemical engineering, Bradford, Leeds, Birmingham, Herriot-Watt Universities, & Powder Research Ltd., HG3 1LU, UK
2
Department of Chemical engineering University of Malaya, 50603Kuala Lumpur, Malaysia
3
Department of Chemical engineering University of LeedsLS29JT, UK
4
Total Petroleum, Fr
*Author to whom correspondence should be addressed. E-mail: prfgeldart@aol.com

Abstract In response to the need in industry for a quick and reproducible method of measuring the flowability of
powders in processes involving transport and storage, the apparently simple idea of measuring angle of repose has been
revived. The simple tester first used has evolved over a number of years into the present version which is shown to be
capable of handling quite small samples of powders that are even slightly cohesive. Experimental data are presented and
results shown to compare consistently with the better known Hausner ratio.
Keywords flowability, characterization, industrial powder testing

1. Introduction low cost and robust testing device. It has been thoroughly
tested in co-operation with industry, and found to be reli-
There are many pieces of equipment and methods able even when the tests were performed outside a formal
available that may be used to measure particle properties laboratory, without the need for highly trained technicians.
such as particle size distribution (PSD), particle density It can also be used as an experimental apparatus in un-
and shape. However it is still not possible to use basic dergraduate laboratories to stimulate in students an inter-
particle properties such as these to predict the behaviour of est in powders and to enable them to gain hands-on ex-
bulk powders except in a very generalized way, and spe- perience of the peculiarities and fascination of this impor-
cific test methods have to be used in order to obtain reli- tant form of matter.
able data that can be used for designing equipment such
as storage hoppers that will not block. Many of these 2. Definitions of AOR
methods involve laboratory equipment having a high capi-
tal cost and/or require skilled technicians to get consistent It is widely agreed that there are two main types of angle
reliable results. Small changes in formulation or raw mate- of repose, i.e. the static and dynamic angles. However, there
rials that result in different particle shapes or surface are at least eight methods of measuring these angles of
properties can often affect the performance of processing repose, and each method will give somewhat different val-
plant, but for trouble-free production of powders it is often ues. Therefore the published values of the angle of repose
only necessary to know whether the powder being pro- are seldom comparable (Brown & Richards, 1970).
duced today has better or worse flow properties than that In establishing a relation between flowability of powders
produced yesterday; that is, will the plant units still perform and some simple physical measures, Carr (1965 & 1970)
as designed, or will blockage, attrition, segregation be and Raymus (1985) suggested that angles of repose below
more or less likely. These tendencies are often covered by 30o indicate good flowability, 30o-45o some cohesiveness,
the imprecise word, flowability. It is often claimed that 45o-55o true cohesiveness, and >55o sluggish or very high
devices available for measuring shear strength can also cohesiveness and very limited flowability. Geldart et al.
measure flowability, even though they were primarily de- (1990) and Antequera et al. (1994) were more inclined to
veloped to provide information needed to design storage use the 40o criteria, based on the data of Brown and Rich-
hoppers. For example, the method invented by Jenike ards (1970), in classifying free-flowing and cohesive pow-
(1964), which takes time and skill to use, measures the ders. Although the measurement of angle of repose has
ability of the powder to start flowing or not. Fortunately sometimes met industrial and academic needs for a simple
other simpler and quicker methods are available for moni- and quick test that can disclose changes in the flow prop-
toring powder flow and providing relative measures of erties of powders as they pass through processing and
flowability. It is not appropriate to review here all the handling equipment, Geldart et al. (1990) pointed out that
methods available since a recent book edited by there was no general agreement as to the best design or
McGlinchey (2005) performs this function admirably. In this size of equipment, for the way that a test should be done,
paper, we concentrate rather on a well known powder or the optimum amount of powder that should be used. The
property, angle of repose (AOR) that we have re-examined four most common methods in use until recently are shown
and for which we have developed, over several years, a in Fig. 1.
Geldart, Abdullah, Hassanpour, Nwoke & Wouters: Characterisation of Powder Flowability 105

cially if it exhibits some cohesiveness. The semi-cone


formed should have a well-defined, sharp apex, but some-
times, if the pouring has been done too quickly, a distinct
semi-cone may not be formed, because the apex may be
ragged making an accurate reading of the height of the
semi-cone impossible, in which case that test should be
repeated with the pouring done more slowly.

Fig. 1 Measurement of static and dynamic angle of repose.

In method I powder is poured into the funnel which is


held at a fixed height above the flat base whereas in
method II the funnel is filled with the test powder which is
then raised gradually to allow the sample to flow out. Both
these methods require that the powder should be able to
flow through the small funnel, and cohesive powders may
not do so. Moreover, the powders do not become aerated
as they often do in production processes, unlike methods vibrator

III and IV in which some ambient gas is entrained during vibrating chute

the test. In none of these methods is it easy to measure the funnel


angle accurately. Methods III and IV require equipment that
must be mounted on a shaft passing through a low friction
bearing so that it can be tilted gradually until slipping oc-
curs and the angle measured. The shaft and bearing often
needs to be dismantled for thorough cleaning between
tests, an inconvenience that slows down the testing pro-
chute
cedure.
By working closely with a large UK chemical company, baseboard

Professor Geldart and his research students at the univer-


sity of Bradford developed a piece of equipment in which
backplate
the powder is made to flow so that it forms a semi-cone
Fig. 2 Mark 4 Powder Research Ltd. AOR tester.
whose height and average radius are easy to measure and
from which the dynamic AOR can be readily calculated or
read from a table. The equipment has passed through Another commonly used simple method for characteris-
ing powders that are cohesive or semi-cohesive should be
several stages of development and comparison of ex-
mentioned, the Hausner Ratio (Grey & Beddow, 1969) in
perimental values of AOR with practical experience on
which the tapped and aerated bulk densities are measured
operating a large soda ash plant has confirmed it as a
and the former is divided by the latter. It turns out that there
reliable device that is robust and easy to use even for co-
is a good correlation between AOR and HR as shown later.
hesive powders using quite small samples of powder. A
picture of the Mark 4 (most recent version) of the tester is
shown in Fig. 2. A representative sample of the powder to
3. Materials Used
be tested (100 grams is the preferred mass) is weighed out Two types of powders have been used in some of our
+/- 1 g and put into a metal beaker. If the powder appears recent work: spherical and porous Fluid Cracking Catalyst
to be free-flowing, the 100 g sample is poured slowly and (FCC) (Fig. 3), and angular and non-porous aluminum
gently on to the upper converging chute, taking about oxide trihydrate (Fig. 4) used as a Fire Retardant Filler
20 sec for the entire sample. If the powder shows signs of (FRF). Graded powder mixtures were tested for both
cohesiveness or reluctance to flow, the vibratory motor is powders. In order to form a series of powder samples
switched on so that the powder flows down the upper chute, having different mean particle sizes, small amounts of
into the metal hopper and onto the lower sloping chute that cohesive fine 7-micron particles were added in increments
directs the powder against the vertical wall. The powder to a coarser 79-micron FCC and 63-micron FRF which
should not be allowed to accumulate in the hopper, espe- were used as base materials to form mixtures having mass
106 CHINA PARTICUOLOGY Vol. 4, Nos. 3-4, 2006

percentages of fines of 1, 2, 5, 10, 20, 40, 50, 60, 70, 80 60


=88.3dsv-0.26
and 90%. 50 R 2 = 0.97

40

Angle of Repose,
30

20
=79.7dsv-0.25 FRF mixtures
10 R 2 = 0.97 FCC mixtures

0
0 10 20 30 40 50 60 70 80
Sauter diameter, dsv / m

Fig. 6 Angle of repose versus Sauter diameter.


Fig. 3 The spherical shape of FCC particles.
60

55 FRF mixtures
FCC mixtures = 36.2HR - 13.4

50 R 2 = 0.97
Linear (FRF mixtures)
Linear (FCC mixtures)
45

Angle of Repose
40

35
= 29.8HR - 5.4
R 2 = 0.97
30

25
1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.9
Hausner Ratio-

Fig. 7 Angle of repose versus Hausner ratio.


Fig. 4 The angular shape of FRF particles.
It should be noted that in Geldarts classification of
powders (1973) according to their behaviour in fluidized
4. Results and Discussion beds, powders having values of HR<1.25 fall into groups A,
The Hausner ratios of samples of the two materials having B, or D, while powders having values of HR>1.25-1.4
the smallest mean sizes are very similar as shown in Fig. 5. show semi-cohesive properties, and powders with HR>1.4
As with almost all powders the Hausner ratio decreases as are cohesive and difficult to fluidize. As seen in Fig. 6, such
particle size increases. This confirms that an increase of powders also have AOR values ~40o.
particle size of a powder mixture is always accompanied by a Similar trends were observed in our earlier studies on
decrease in cohesiveness (Abdullah & Geldart, 1999). The soda ash, sodium bicarbonate, and lactose. Note that the
same trend is observed in Fig. 6, where the angles of repose linear relationship between HR and AOR is slightly less
for both materials gradually decrease as the mean size in- apparent in Fig. 8 than in Fig. 7 because of the greater
creases, indicating that both powders change from cohesive number of experimental points shown in the former. It was
to more free flowing with increasing mean size. The found that by calculating the bulk density ba of the
near-perfect linear relationships observed between Hausner semi-cone and plotting AOR/ba versus Sauter mean size
ratio and angle of repose (Fig. 7) confirm that both parame- the data from all these materials could be shown on one
ters are good indicators of powder flowability. graph, Fig. 9.

2.0
50
HR = 2.65d sv-0.19
1.9 FRF mixtures
45
1.8 R 2 = 1.00
FCC mixtures

1.7
AOR / degrees

40
Hausner Ratio, / -

1.6

1.5 35
HR = 1.4
1.4 sodium bicarbonate
1.3 HR = 1.25 30 FCC
1.2
HR = 2.77d sv-0.21
soda ash
25
1.1 lactose
R 2 = 0.99
1.0
20
0 10 20 30 40 50 60 70 80 1 1.2 1.4 1.6 1.8 2 2.2
Sauter diameter, d sv / m
Hausner Ratio / -

Fig. 5 Hausner Ratio versus Sauter mean diameter dsv. Fig. 8 AOR versus HR.
Geldart, Abdullah, Hassanpour, Nwoke & Wouters: Characterisation of Powder Flowability 107

the smallest standard deviation, it is suggested that this is


the optimum sample size to use when measuring angle of
repose using the Powder Research Ltd. AOR Tester. Our
experience is that if 100 g are not available, the most
consistent results are obtained if the same sample size is
always used for the powders to be tested.

Table 1 Average values and standard deviations on 5 tests each on


various sample masses of avicel & starch
Avicel Starch
Sample Average Std. Dev. / Average Std. Dev. /
Mass / g AOR / Deg. Deg. AOR / Deg. Deg.
Fig. 9 Weighted AOR/ba versus surface/volume mean size (Sauter 50 38.4 0.33 36.91 1.98
mean size). 100 38.3 0.32 36.91 0.47
150 37.0 1.02 NA NA
200 NA NA 34.75 0.74
The mass of powder used in the experimental results
shown above was kept constant at 200 g, but during the
formulation of new products in some industries, particularly 5. Conclusions
pharmaceuticals, it is not always possible to make 200 g When measured using a robust, simple, well-engineered
available, so our most recent work has been aimed at de- device, Angle of Repose can be used to characterise a
termining whether the mass of the sample has an influence wide range of powders in order to monitor their flow be-
on either AOR or weighted AOR. For this phase of our haviour in existing items of production units on a day to day
studies we used starch and avicel, both somewhat basis. There is a close correlation between the Hausner
semi-cohesive and commonly used as additives in the food ratio and the AOR, but we prefer the latter because it is
and pharmaceutical industries. The results of these ex- easier to measure and involves rather more powder
periments, as shown in Figs. 10 and 11, indicate that re- movement such as often occurs in powder processing.
ducing the sample size from 200 or 150 g to 100 g causes
an increase in AOR though a further reduction to 50 g does
not have an effect. In all our experiments each sample was References
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Because for both powders sample masses of 100 g gave Manuscript received December 14, 2005 and accepted April 2, 2006.

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