Powder Technology, 7 (1973) 45-50 45

0 ElsevierSequoiaS.A., Lausanne - Printedin the Netherlands

Effect of conditioners on the flow properties of powdered sucrose

M. PELEG and C. H. MANNHEIM

Deparrment of Food Engineering and Biotechnology, Technion-Zsmel lmtirure OJ Technology, Haif (Zsrmzi)

(Received January 3,1972; in revised form June 14.1972)

Summary b) as lubricants of the reducing the

friction between the particles,
The effect of two anticaking agents, calcium (c)
stearate and aluminium silicate, on the physical
characteristics of powdered sugar was studied. Tile
compressibility of the powder was found to be a
useful criterion for evaluating :he cohesiveness of aL4-‘,
these powders. It was shown that anticaking agents pharmaceuticals by Craik and Miller6 and by
which reduced cohesiveness also reduced compressi- Pilpel’, and fertilizers were surveyed by Zimon8
bility while increasing the initial bulk density. Mois- and Pietsch’.
ture, which increased cohesiveness, had the opposite Nash et aLv studied the effect of Cab-0-Sil
effect on compressibility and bulk density. (a silicate conditioner) on the physical properties
Cohesion and angle of internal friction were of Carbowax and found that the addition of Cab-
measured using the Jenike FZow Factor Tester. 0-Sil reduced the tensile aud shear strength and
Results indicated that cohesion decreased with the changed the bulk density and the electrostatic
addition of anticaking agents while increasing with charge.
moislure. The angle of internalfriction was found to In this work we tried to evaluate the effect of two
.decrease with the addition of calcium stearate while conditioners on the flowability and some physical
ahuninium silicate sIightIy increased it. Ccking properties of powdered sucrose. The conditioners
observations showed that tJzese flow conditioners selected were aluminium silicate as a representative
acted like anticaking agents and vice versa. of the silicates group and calcium stearate as a
representative of the stearates group.

INTRODUCTION
Flow difftculties in the food industry as well as
other industries are often overcome by the use of
anticaking agents, also called flow conditioners.
Flow conditioners are usually very fine powders
with subsieve particle size. The most common iu
use are various types of silicates, stearates, phos-
phates, diatomacecus earth, starch, magnesium
oxide, talcum and fatty amines’**.
They are generally used in concentrations up to
3%_ As food additives their use is often limited to
the 1% level and in addition they must conform to
food legislation. The mode of action of the condi-
tioners in caking inhibition and in improvement
of flowability can be explained in three ways
as a barrier powder particles,
attractive forces,
EXPERIMENTAL
Commercial beet sugar (Sugaf Israel) was ground
in a laboratory mill (Junior Lab. Mil!, 5 in., Christy
& Norris Ltd., England) and sieved to obtain
fractions of: - 40+ 60 mesh, - 60-c 80 mesh and
-SO+ 100 mesh. The fractions were dried over-
night in a vacuum oven at 7@C, sieved again and
sealed in tin cans.
Part of the sugar was allowed to equilibrate at
250 C and 52% R.H. in a desiccator using saturated
magnesium nitrate solutions to obtain the desired
humidity. Portions of each sugar fraction were
admixed with 1,2 and 3% calcium stearate (techni-
cal grade, British Drug Houses, England) or with
precipitated aluminium silicate (British Drug Hous-
es, England).
46 M. PELEG, C. H. MANNHEIM

All materials were subjected to shear analysis
using a Jenike Flow Factor Tester model HS-TS”.
Bulk density and compressibility were measured in
a lucite cell with cross-sectional area of 11.95 cm’
and 4.5 cm height. Powder was poured into the cell
using a top ring to obtain an excess quantity of
powder in the cell. Before weighing the cell the top
ring was removed and the excess powder was
scraped off.
Compressibility was measured in terms of bulk
density after applying compaction pressures in the
range 0.04-0.6 kg/cm’. When determining com-
pressibility, columns of 5 cm height were formcl
and in this position the cell was compacted for 2
minutes before starting the bulk density determi-
nation. The relationship between bulk density and
the applied pressure was plotted and was used for
the @culation of compressibility_
RESULTS AND DISCUSSION
Bulk density and conzpressibiiity. Results of bulk
density measurements and the relationship between
bulk density and compaction pressure for various
fractions of powdered sucrose are given in Tables
1-3. Regression analysis of the results showed
that highly significant correlations were obtained

TABLE 1

Bulk density and compressibility of powdered sucrose +40-60 mesh

No. R.H. Conditioner Inirial Eqztarion consumrs NO. Correlation

(%) kfareriol % bulk b LI of coeficient
density compres- measure- r
(s/cm’) sibilirr menrs

1 DV NOX _ 0.804 0.078 1.025 8 0.862**

2 Dry AI-Sil i 0.939 0.053 1.030 19 o.s3s**
3 Dry Ca-Ste 1 1.080 0.032 0.891 7 0.615*
4 52 None _ 0.768 0.075 1.013 15 - 0.970***
5 52 AI-S11 1 0.93 1 0.054 0.946 8 0.944***
6 52 AI-Sil 2 0.981 0.053 0.972 6 0.968***
7 52 AI-S11 3 0.956 0.065 0.974 7 0.968***
8 -7 Ca-ste 1 1.045 0.033 1.099 7 0.880**
9 :I Ca-ste 2 0.926 0.040 1.022 7 0.937***
10 52 Ca-Ste 3 0.958 0.043 1.019 7 0.914-**

AI-Sil. aluminium silicate: Ca-Ste, calcium-stearate.

* Significant at 90% level.
** Significant at 95% level.
*** Sirmilicant at 99% level.

TABLE 2
Coropressibility of powdered sucrose + 60- 80 mesh

No. R.H. Conditioner Iniriol Equation constants No. of Correlarion

% A4oteriol % bulk b o meosure- coeficient
densit~~ compres- ments r
(.4jfm? sibility

1 Dry None _ 0.622 0.152 0.960 10 0.988***

2 DV Al-Sil 1 0.755 0.092 0.935 14 0.855***
3 Dry Ca-Ste 1 0.953 0.056 1.036 15 .0.983***
4 52 None - 0.498 0.185 0.961 17 0_938***
52 AI-Sil 1 0.815 0.068 0.892 17 0.979=**
2 52 Al-Sil 2 0.854 0.046 1.073 9 0.985+**
7 52 AI-Sil 3 0.799 0.093 1.159 7 0.993***
8 52 Ca-Ste 1 0.998 0.038 1.052 15 0_942***
9 52 Ca-Ste 2 0.988 0.039 0.937 7 0_9u***
10 52 Ca-Ste 3 0.959 0.043 0.942 7 0.910***

l ** Significant at 99 % level.
 FLOW PROPERTIES OF POWDERED SUCROSE 47

TABLE 3
Compressibility of powdered sucrose + 80- 100 mesh

NO. R.H. Conditioner Initial Equation con:tants No. of Correlation

(%I Material % bulk b a measure- coqficient
density c0,?,pZS- ments i-
k7/cm3) sibiliry
~~_
1 Dry None - 0.632 0.106 0.916 10 0.906***
2 DV AI-Sil 1 0.735 0.064 0.890 18 0.719*
3 DV Ca-ste 1 0.828 0.104 0.981 15 0.992***
4 52 None - 0.610 0.112 0.936 17 o-973***
5 52 AI-Sil 1 0.73 1 0.085 0.803 13 0.983***
6 5, Al-SiI 2 0.756 0.046 0.856 23 o-943***
7 52 AI-Sil 3 0.772 0.064 0.876 23 0.986***
8 52 Ca-ste 1 0.867 0.102 0.940 22 0.987***
9 52 Ca-Ste 2 0.903 0.057 0.962 17 0.978***
10 52 Ca-ste 3 0.934 0.064 1.003 21 0.978’**

** Signiliant at 90% level.

*** Significant at 99 o/0level.

between the apparent bulk density and the loga-
rithm of pressure in the range of pressures used.
The correlation therefore fitted the following
equation :
B.D.=a+b IogP
where
B-D. is bulk density,
a is a constant representing the extrapolated bulk
density at 1.0 kg/cm’ pressure,
b is the slope of the straight line,
P is the pressure applied (kg/cm’)_
The constant b, which represents the change of bulk
density due to pressure, was called the compressi-
bility-
The results given in Tables l-3 show that mois-
ture, in the absence of flow conditioners, caused a
slight increase in compressibility.
Both flow conditioners, under the conditions
tested, caused a considerable increase in bulk
density and a considerable decrease in compressi-
bility.
These results can be explained by the role of the
inter-particle forces in the internal arrangement of a
powder bed. The more cohesive the powder, due to
moisture for example, the more open a structure it
can maintain due to support from the inter-particle
attractive forces. This obviously results in a rela-
tively low bulk density. Under pressure, the open
structure collapses and therefore a considerable
compressibility is obtained. When anticaking agents
are added, interparticle forces are considerably
reduced. In this case &hepowder tends to occupy a
smaller volume than befare, showing greater bulk
density. Pressure in the latter case causes mainiy
the filling of random voids and as such has little
effect on density, resulting in small compressibility_
No trend was found on the influence of the various
conditioner concentrations used. This might be
due to the unknown size distribution within the
sugar fractions examined which could have lead
to a different coverage of the solid surface of the
sugar by the conditioners.
CALCULATION OF COHESION
Results obtained in Jenikc’s Flow Factor Tester
were subjected to linear regression. It was found
that the yield data, each containing six measure-
ments_ were on straight lines (Tables 4-6). Cohesion
was calculated by extrapolating the yield curve to
zero normal load. The fact that the yield curves were
straight lines enabled numerical calculation of the
Mohr circles, using a routine computer procedure’ I.
As shown in Tables 4,5 and 6, cohesion increased
with the increase in adsorbed water and decreased
with the admixture of both anticaking agents
employed_
As in the case of compressibility th_ere was no
significant influence of either particle size of the
sugar or the concentration of the conditioner added.
This might be due to experimental errors as well
as to the non-uniform size distribution of the sugar
particles as already mentioned.
The angle of internal friction was found to
decrease with the powder humidity, increase slight-
48 M. PELEG, C. H. MANNHEIM

TABLE 4
Effect of ~WIJflow conditioners on the flow properties of powdered sucrose - 40+ 60 mesh

NO. R.H. Conditioner’ Regression of yield Correlation Cohesion’ Angle of

(%I Material % curwz coefficient (s/cm’) internal
fiicrior?
(deg)

1 Dry None - S=O.637+0.851 V 0.994*** 9.0 42.7

2 Dry AI-Sil 1 s=o_490+0.913 v 0.998*-* 6.9 43.6
3 Dry Ca-ste 1 S=O.398+0.790 V 0.997-c* 5.6 412
4 52 None - S=1.083+0.700 V 0.986*** 15.3 39.6

z 52 AI-B1
AI-SiI 2
1 ss=o.551+0.919
= 0.750 + 0.927 v 0.994***
0_999*** 10.6
7.8 45.4
45.3
7 52 AI-SiI 3 S = 0.485 + 0.956 V 0.988*** 6.8 44.3
8 52 Ca-ste 1 s=o.350+0.746 v 0999*** 4.9 38.4
9 52 Ca-Ste 2 S=O.318+0.737 V 0.998-‘- 4.5 38.3
10 52 Ca-Ste 3 S= 0.280 -+-0.734 V 0.999*** 3.9 37.7

’ Al-Sil. aluminium silicate; Ca-Ste. calcium stearate.

’ Curve obtained at initial consolidation load of 6.5 kg.
3 An average value of four calculations under four different initial consolidation pressures.

TABLE 5

Effect of two flow conditioners on the flow properties of powdered sucrose -60+80 mesh

NO. R.H. Conditioner Regression of yield Correlation Cohesion Angle of

(%) Material % curze coeficient (g/cm’) intern51
ftiction
(deg)

1 NOllC? - S=O.516+0.729 V 0.991*** 7.3 38.8

2 Al-Sil 1 s = 0.545 + 0.730 v 0992*-• 7.7 39.3
3 =Y Ca-Ste 1 S=O335+0.650 V 0.996+** 4.7 34.6
4 52 NC.Ile - S = 0.807 •t 0.669 V 0.997”’ 4.4 36.8
5 52 Al-Sil : S = 0.299 + 0.936 V 0.996”* 4.2 424
6 52 Al-U S = 0910+ 0.787 V 0.995**- 128 422
7 52 AI-Sil 3 S=O.704+0.811 V 0.996*‘= 9.9 42s
8 52 Ca-Ste 1 S=O.320+0.693 V 0.999*** 4.5 36.6
9 52 Ca-Ste 2 S=O.378+0.675 V 0.9992’• 5.3 35.3
10 52 Ca-Ste 3 S=O.514+0.671 V 0.989*** 7.2 35.6

TABLE 6

Effect of two flow conditioners cm the flow properties of powdered sucrose -8O+ 100 mesh

No. R.H. Conditioner Regression of yield Correlation Cohesion Angie of

(%I Material % clime coeficient (g/cm’) intern51
ffiction
(de4

1 Dry NolIe S= 0.654 + 0.747 V 0.997**+ 9.2 40.9

2 . Dry Al-Sil S=0514+0.746 v 0.994*** 7.2 41.4
3 Dry Ca-Ste S=O_459+0.596 V 0.999*** 6.5 33.4
4 52 None s=0.917+0_700 v 0.997*-• 129 38.4
5 52 Al-Sil s=o.604+0.793 v 0.998=** 8.5 41.7
6 52 Al-Sil S=O.298+0.871 V o-999*-* 42 42.0
7 52 Al-Sil S=O.726+0.814 V 0.999-g• 102 423
8 52 Ca-ste S=O587+0.627 V 0.995*-* 8.2 35-4
9 52 Ca-Ste S=O576+0.614 V 0.988’*+ 8.1 35.3
10 52 Ca-ste s=o.540+0.590 v 0.995-g* 72 34.2
FLOW PROPERTIESOF POWDERED SUCROSE 49

F (al Y-h RH
zl
5 (b) Dry
(cl Y%W+LI-SiI
s Cd) Y%mi*G3-ste
57-
x? 6-
.g5-
-04-
.z 3
5 2-
s 1-
‘0- 5 10 15 20 25
P&jot- mnsiidotion force (kg)

Fig. I. FIowfunctionsof powderedSUCTOS~

withtwo antirakiigagents.

calcium stearate was the observation of oscillations

during shear measurements, called the slip stick
effect. The addition of aIuminium silicate had no
influence on the type of curve obtained in the Flow
Factor Tester.
The flow function values of the various fractions
are plotted in Fig. 1. It seemed that both condi-
tioners improved the flowability of the powdered
sugar, with calcium stearate giving a slightly better
effect.

COHESION AND CAKING

Samples of sugar fractions were sealed in glass

.-Eo*Mw
.-W+lCGW
I
OO lo
cohes-,” Cgr/dJ
Fig.2. The relationship between cohesion and caking of powder-
ed s”ci-ose.
ly with the addition of aluminium silicate, and
decrease considerably with the addition of calcium
stearate.
These results can be explained by the formation
of a solution film on the sugar solid interface due to
moisture uptake. This film contributes to the in-
crease in cohesion due to the formation of liquid’
bridges between the particles. However, when an
external shear force is applied and deformation
occnrs this film acts as a lubricant and as such de-
creases the friction.
Calcium stearate, being fatty by structure, ap-
parently acted as a more effective lubricant than
the solution film. Therefore a considerable decrease
(of 3-5 degrees) was observed in all cases where
calcium stearate was added. Another effect of
jars and stored at 2S’C. Daily inspection was nade
and the time for visual appearance of caking was
recorded. The results are given in Fig 2. It was ob-
15 served that the more cohesive the powder the greater
was its tendency to cake. All samples containing
flow conditioners (cohesion values exceeding 7
g/cm”) did not cake during 60 days, indicating that
the conditioners acted as successful anticaking
agents. Although many factors such as temperature
changes, purity, etc. are involved in the mechanism
of caking, and although the hardness of the cakes
formed was not evaluated, it seems that cohesion
measurements might be used as objective criteria
for the prediction of caking.
The authors wish to express their sincere thanks
to Mr. A. Birks and Mr. J. C. Williams, Postgradu-
ate School of Studies in Powder Technology,
University of Bradford, for their useful guidance,
Mr. I. Saguy for his help in programming and
Mrs. Sharf and M. Rauchwerger for their technical
aid.
This work was supported by the US. Dept- of
Agriculture, Grant No. FG IS 288 under pubIic
law 480.
50
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