Agglomeration of Milk Powder and Its Influence on

Reconstitution Properties
E. NEFF ~ and H. A. L. MORRIS
Department of: Food Technology, Massey University
Palmerston North, New Zealand

Abstract enlargement or agglomeration operations used

Powder granulation involving rewetting, in many industries. One operation is that of
granulation, drying', and screening has been wet granulation used in the pharmaceutieaI
used to simulate commercial instantizing of and fertilizer industries.
nonfat dried milk (NteDM). Effects of Undoubtedly. much work has been done oll
rewetting moisture on dispersibility, sink- the agglomeration of food powders and, in
ability, solubility, bulk density, and poros- particular NFDd,[, by instantizing processes.
ity of the redried granulated product bare Unfortunately little has been published, as most
been studied, with effects of particle size instantizing processes are patented. Neverthe-
on reeonstitution. Rewetting moisture is less, the paucity of information indicates the
most critical in actual granule formation, difficulty in conducting controlled experiments
a sharp break point occurring at 11-12% in commercially available instantizing equip-
moisture, and optinmm conditions for re- ment.
constitution coinciding with this point. The rewetting moisture content during ag-
Granulation increased dispersibility of glomeration is acknowledged as commercially
powder from 41 to 62% at optinmm re- important, but the range of rewetting moistures
wetting conditions, whereas beyond the specified in patents shows great variation, and
break point there occurred a sharp de- appears to be the basis of differences between
crease in dispersibility and solubility. patents. ]d~or example, Peebles (22) specified
Optimum particle or granule size for the an optimum rewetting moisture of 15% ; Louder
reconstitution has been determined by and Hodson (15) an optinmm of 5.5%; and
sieve fractionation of the granulated prod- Scott (24) specified 10-14% rewetting n,oisture.
uct. Particle size of 200 > represented Processes for instantizing milk powders are
optinmm dispersibility associated with in- described by Bullock (5).
finite sinkability. Two major variables Peck (21) and Little and Mitchell (14) de-
influencing reeonstitution of instantized scribe wet granulation practices in the phar-
NFD.K are rewetting moisture and particle umceutical industw, giving no quantitative
size of the redried product. moisture requirements.
More £undamental research has been done
It is well known that nonfat dried nfilk on the mechanism of granule formation frmn
(NF1)M) a~d other powders, sucl~ as chocolate moist powdered material, such as moist sand,
mix, sugars, starches, etc., may be instantized in a troubling-type drum mixer by Newitt and
by a rewetting'-redrying process. Mort and Conway-Jones (20) and Capes and Danek-
Hedriek (18) emphasized the importance of wefts (6). Newitt and Conway-Jones (20) de-
instantizing in the United States and stated scribe three states of water in an assembly of
that practically all NFD;~{ for home use was spherical particles, viz., pendular, funicular,
instantized. Hall and Hedrick (9) described and capillary state. The capillaw state is a
the manufacture of instant milk powders, while saturation of the voids between particles with
other agglomerated and instantized food pow- liquid. These workers postulate that in granu-
ders are discussed by Moore et al. (17), Claus latiou a kneading action occurs, resulting in
and Brooks (7), Miller and Powell (16), and decreasing internal pore space; hence, if suf-
Lachmann (13). ficient water is present the pores may become
What is not well recognized, bowever, is saturated to form stable granules. Capes and
that instantizing processes are similar to size Danckwerts (6) extended this work and showed
Received for loubliea.tion June 20, 1967. that in granulation of sand significant growth
Present address: Department of Agriculture, of granules occurred only when liquid contents
Melbourne, Australia. This work was done at were equal to between 90 and 110% of the
Massey University during tenure of an Australian amount required to l]tl tim voids in a highly
Dairy Produce Boa.rd Studentship. compacted sample. S~ituration or' voids in the
330
 MILK POWDER, AGGLOMERATION
aggregated particles with liquid is necessary
to obtain a stable system.
Another important factor affecting reconsti-
tution characteristics of powder is particle size.
However, conclusive evidence is lacking con-
cerning the optimum particle size for milk
powder as revealed by King (12).
Bockian et al. (4) noted that instant pow-
ders consisted of very large aggregates of
180-840 ~, and suggested that this may be one
of the main factors affectin~ disoersibility of
instant N:FDM. Similarly, Peebles (22) con-
sidered it important that ap~)roximately g0%
of instant NFDM have particle sizes greater
{hun 74 t~ to obfain a powder of desired charac-
teristics.
Swanson (25) fractionated tmwders into dif-
:ferent sizes and concluded that NFDM particles
of 30-50 ~ in diameter seemed to wet and dis-
perse most readily, whereas, sizes on either side
showed decreased dispersibility. Baker and
Bertok (2) sieve-fractionated powders and con-
cluded that decreased particle size was associ-
ated with decreased wettability and dispersibil-
it-,.
Hall and Hedrick (9) stated that manufac-
turers of instant N]~DM are fully aware of the
importance of particle size. They describe a
desirable particle distribution as being in the
range 100-500 tL; no more than 10-15% of
weight of particles should be less than 150
in diameter. Similarly, Claus and Brooks (7)
dealt with the properties of instantized wheat
flours, emphasizing increased particle size.
Researchers have shown the importance of
particle size on dispersion of a food powder,
although there appears to be little evidence for
specifying an optimum size, even for NFDM.
Pyne and Coulter (23) emphasized that there
must exist an optimum size corresponding to
maximum dispersibility. They found that dis-
persion of milk powders is inversely propor-
tional to the surface-to-mass ratio while the
rate of solution is directly proportional to this
ratio. I t is reasonable to deduce, therefore, that
an optimum surface-to-mass ratio, or particle
size, exists, and is related to optimum re-
constitution characteristics.
It was the aim of our study to simulate
an agglomeration process, applying the prin-
ciples of wet granulation. Once a simulated
instantizing process has been developed, it can
then readily be employed to study some of the
hasie factors controlling the process; such as,
effects of rewetting moisture and of particle
size on the reconstitution properties of NFDM.
331
Experimental Procedure
Dispersibility. The dispersibility of the
NFDM powders and granules was deternfined
by a modification of the American D17 Milk
Institute (ADMI) method, described by Neff
and Morris (19). Dispersibility is expressed as
the percentage of powder reconstituted under
conditions of test.
SinkabiIity index. The sinkability index of a
powder was determined by the method of Neff
and Morris (19), being expressed as mg of
powder sinking per minute per em-~ of area.
Solubility index. This was deternfined by
the ADMI method (1), being expressed as ml
of' sediment.
Bulk density, particle density, and porosity.
These properties of a powder were determined
by a hexane displacement method, described by
Beckett et al. (3). The method measures the
bulk density and porosity of a loosely compac-
ted sample. Bulk density and particle density
are expressed as g/ee, while porosity is ex-
pressed as ec of voids per cc of bulk powder.
Moisture. Moisture was determined by dry-
ing weighed samples in a fan-assisted air oven
at 102-103 C for three hours. Moisture was
expressed on a wet weight basis.
State of lactose in NFDM. The railk powder
was examined for crystalline lactose by polar-
ized light microscopy, as described by King
(11).
Sieve separatim~. Sieving of samples was
done using British Standards test sieves, to-
gether with a mechanical sieve vibrator. All
powder handling and sieving was done in a
room held at a relative humidity of 40%, to
nfinimize moisture pickup and facilitate han-
dling.
Procedure for granulation. A granu]ation
procedure, similar to that used in the phar-
maceutical industry as described by Peck (21),
was adopted. A mixer (Kenwood Chef model)
was used for the first two steps. This mixer
employs planetary motion, ensuring thorough
nfixing. The beater was used for the rewetting
operation, while the colander and sieve at-
tachment was used to force moistened particles
through a screen, having a rotating paddle
fitted with scraper blades which travel over the
surface of a screen inside the colander bowl.
I n this study the finer of the two screens was
employed, having holes of 1,600 ~ in diameter.
The speed of the mixer was regulated with a
variable voltage control, as the control for the
Kenwood could not be regulated to low speeds.
The four steps used in this procedure were
as follows :
.J. DAIRY SOlE~OE YOL. 51, NO. 3
332
1). Two hundred grams of powder were
placed in the mixer bowl and the heater set
in motion. The quantity of water needed was
allowed to drip slowly and in stages. Regular
manual stirring with a rubber plate scraper was
also used to eliminate quiescent spots in the
mixer. Mixing required 10-15 minutes. Through-
out this work, powder samples and water were
used at 18 C.
2). Af t er allowing the moistened mix to
stand for 5-10 minutes, granulation was done
in the colander and sieve attachment. F o r most
of this work the moistened N F D M was granu-
lated through a screen having holes 1,600 tL in
diameter. However, granule size was also varied
Fia. 1. Four steps in the granulation procedure. A. Mixing and rewetting of base powder. B. Granu-
lation in colander and sieve attachment. C. Tray drying at 60 C. D. Dry screening through 2,000-~
sieve.
J , ~)AII~Y S C I E N C E ~ O L , 5 1 , NO, 3
N E F I ~~ A N D MORRIS
hy wtwing screen size. For this purpose special
screens were e(mstrncted by soldering standard
wire mesh on to a perforated supporting base
plate to fit into the colander attachment of
the Kenwood Chef mixer.
3). The moist granules were spread on to
a tray and air-dried at 60 C in a fan-assisted
dryer for 50-60 minutes, drying time being ad-
justed to give a final product of 3.0-4.0%
moisture. The granules on the drying tray
were stirred periodically during d r y i n g
4). The dried granules were passed through
a 2,000-/* (B.S. 8-mesh) sieve to eliminate large
clumps formed during drying.
 MILK POWDER AGGLOMERATION 333

The four stages in this procedure are de- by sampling the product after treatment in the
picted in Fig. 1. colander and sieve attachment. Some drying
occurred during granulation, as moist powder
Results and Discussion 2
was forced through the screen, but it was not
Temperature of d~'ying of granules. In dry- significant. I t was found more satisfactory to
ing moist granules it was desired to effect a sample after granulation.
minimum of heat damage. Some experimenta- Therefore, both powders were granulated
tion was done to determine a satisfactory drying corresponding to a range of rewetting mois-
temperature-time combination which would give tures. They were analyzed for dispersibility,
minimum damage. The solubility index of the sinkability index, solubility index, bulk density,
dried granules was the index of heat damage. and porosity. Results are presented in Figs.
Results are presented in Table 1. 2 and 3.
The effect of rewetting moisture upon actual
TABLE 1
granule formation is shown in Fig. 4 for Niro
Effect of various drying conditions on solubility
index of granules NFDM.
The critical nature of rewetting moisture on
Drying the properties of the final product is self-
condi-
tions Initial Final Solu- evident in every respect. Firstly, the rewetting
on moist mois- tools- bility moisture content controlled the actual granulat-
granules tm'e ture index
i ,
(%) - - (ml)
8Oj
70 iIi'"' ' ' = ' NIRO NFDM
Control Niro BREAK PT, AT
NFDM 3.5 0.] 0 11-5% MOIST.
43 C/165 mia 11.5 4.~0 0.10
49 C/100 rain 11.5 3.7 0.10 0
54 C/100 rain 11.5 3.3 0.15 J 50
60 C/ 55 rain 11.5 3.2 0.] 0
71 C/ 35 min 11.5 3.2 0.40 i
40- J'lROGERS NFDM j
-w 30- 01 BREAK PT. AT --'~J'
As can be seen for granules, initially at ~1 12'2°/oMOIST. ~ "
11.5% moisture no heat damage was reflected
in the solubility index until the drying tempera- i

ture was raised above 60 C. I t was, therefore, 10- 1

I
decided to tray-dry all granules at 60 C for
0
50-60 minutes, i.e., to reduce moistures to 3.0- ,4
i
; ; 1'o 1~2 14 16 1'8
4.0% 8-0- I ~ / INFINITE
Effect of rewetting moisture. As discussed SINKABIL[TY Ar
11-5% REWETTING
earlier, there is considerable evidence to sug- MOISTURE AND
gest the importance of rewetting moisture in U 6,0- Ji NIRO ABOVE
determining stable granule or agglomerate for- Oi N F D M 7
mation. But, there is no evidence of the effect zaL9
Gzx
of rewetting moisture on the properties of 4o zo,,
instant powders such as instant NFD3/[. Em- 1
ploying the technique of wet granulation, it I
I
is possible to study such relationships.
I
Two samples of commercial NFDM, viz., 2.0 ~,
,4 ; ~; lb ;2 & ;s 1;
Niro N F D M and Rogers NFDIV[, were granu- I
10, t
lated over a range of rewetting moistures. All ,
these samples were granulated through the 8. I
1,600-t~ screen and then dried and sieved as I

described. Rewetting moistures were determined ~" ~w J[

Ol BREAK / NFDM
~X,,n.
jl,~ ~1 POIN('~ ? ROGERS
Samples of NFDM employed have been desig- O_z
t ~x
j Oi \ ~ / 1 NFDM
nated Niro NFDM mtd Rogers NFDM, referring
to the spray dryers used in manufacture. Such
reference has been included for the sake of com- C, ,A ,,~~ - -- - O - --
}j
I i - i - T I I I
pleteness only, and is not intended to discriminate 2 4 6 8 10 12 14 16 18 20'
between these or any other types of spray dryers, REWETTING MOISTURE % WEIGHT
nor are the samples necessarily typical of the FIG. 2. Properties of granulated nonf&t dr 3-
spray dryers. milks (redried).
3. DAIRYSOZ~:XCEVOL. 5[, NO. 3.
334 N~F~ ~ D ~oaazs

0"60 ;, i I i i , , itt and Conway-Jones (20) and Capes and

!

0-55- % ROGERS Danekwerts (6). Taking the break point for

NFDM at 12% moisture, the comparison is
~m 0,50. made in Table 2. A break point moisture of
~'o
zo
', 12% is comparable to 16.4% on a v / v basis,
wj :
and to 16% void saturation as compared with
~ 0.40- 96% void saturation for the granulation of sand.
~. ~'I NFDM ~ ~ I / This shows clearly that void saturation is not
necessary in the granulation of a noninert
powder such as NFDM, adhesion o£ particles
0-30- I ~/g
I
BREAK POINT
in this case no doubt being assisted by dissolved
0-25 i solids to form a binder solution.
,,; ~ ; 6 1'2 ~'~ & ?s
I The effect of rewetting moisture upon the re-
0.8- ~ BREAK POINT constitution characteristics of the redried granu-
lated powders is shown in Fig. 2. The dispersi-
u3 I NIRO
0
I NFDM f - ' l l ~-~
bility of both Niro NFDM and Rogers NFDM
could be increased markedly, optimum condi-
tions coinciding with break point rewetting.
ou g', x"~"- ROGERS ~0. At this optimum, dispersibility values are equal
~- U 0,' ~,, ~- NFDM
0"6. to those of instant powders, as revealed by
analysis of commercial samples by Neff and
Morris (19). The sinkability index of the Niro
NFDM increases with increases in rewetting
nmisture. At break point rewetting and above
REWETTING MOISTURE % WEIGHT
the sinkability index has been termed infinite,
Fro, 3, Properties of grmmlatecl non,fat dry as the granules lose all tendency to float on the
milks (redried). surface of the water. Siukability index values
were not determined for the Rogers NFDM,
ing process. With increasing moisture content a but showed an identical trend when examined
point was reached where the granulated product qualitatively. The solubility index of samples
changed from a fluffy powder with a poor flow shows a sharp increase beyond break point re-
to well-formed granules of excellent flow prop- wetting, whereas below break point, solubility
erties. The point at which this change oc- indices are satisfactory and would pass ADMI
curred has been called the break point~ and may standards of 1.0 ml.
be detected in Fig. 4. The increase in dispersibility and sinkability
It is interesting to compare the break point index up to the break point suggests that this
moistures obtained in the granulation of NFDM is due to the process of size enlargement. De-
with those for the granulation of sand by New- creased dispersibility beyond break point is
more difficult to explain and nmst be attributed
to increase in solubility index; that is, the
decrease in solubility proper of granules pro-
duced at these higher rewetting moistures. Two
further observations giving evidence of the

TABLE 2

Comparison of brea.k point moistures in the granu-

lation of sand and nonfat dry milk
Sand NFDM
Density :g/co 2.61 1.20
Void volume:ec void 0.270 0.83
g solid
(=0.50 ce/ec)
Granulation break point at:
Moisture v/v 68% 16.4%
Fro. 4. Samples of redried granulated Niro Moisture cc/g 0.260 0.136
nonfat dry milk showing effect of rewetting mois- Void saturation 96% 16%
ture upon granule formation.
5. DAIR.Y SCIENCE ~OL. 51, NO. 3
 MILK POWDER, AGGLOI~ER,ATION
critical nature of the rewetting nmisture were
made :
1) Granules produced at above break point
rewetting appeared to be more yellow than
samples below break point. This could be p a r t l y
attributed to an optical effect, due to increased
particle size (demonstrated by grinding up
granules to a finer particle size), but it was
concluded that some of this color change was
due to a chemical effect.
2) During rewetting of NFDM, then at
approximately 14% rewetting moisture, the
mix passed through a definite doughy stage.
This is as if a gel state had been formed during
mixing.
These observations suggest that at above
break point moistures, additional water is avail-
able for reaction above the minimum required
to act as a binding liquid for granulation. The
possibility exists that some of this water may
combine with protein to form a gel; removal
of such water would be more difficult upon
subsequent drying" and could account for the
increased solubility index and decreased dis-
persibility. F u r t h e r support for the critical
nature of this rewetting moisture comes from
a study of the browning reaction, with as-
sociated insolubilization, in a N F D M system.
Such changes are comprehensively discussed by
Coulter et at. (8). I t is noted that moisture is
an important factor in determining rate of
browning', the optimmn moisture for browning
in a N F D M system being approximately 12-
~4%.
Samples of the redried granulated Niro
N F D M were also examined for state of lac-
tose. I t was found that as rewetting moisture
increased, there was a gradual increase of
crystalline lactose, with a shal~p change to pre-
dominantly crystalline lactose coinciding" again
with break point rewetting conditions.
The bulk density and porosity measurements
shown in Fig. 3 are quite interesting, especially
when compared with the corresponding dis-
persibility curves in Fig. 2. Again it is seen
that minimum bulk density values, or maximum
porosities, coincide with break point conditions.
The strong correlation observed between dis-
persibilities of samples and their porosities (or
inversely, bulk densities) is interesting, in
view of the findings of H a r p e r et al. (10).
They consider that the concentration of milk
solids in the vicinity of powder particles is an
important factor in their instant solubility;
hence, the lower the bulk density the higher
the instant solubility of a powder. Although
the effect of increasing porosity as the break
point is approached would certainly assist the
335
dispersibility Of the powder, it will be shown
that the effect of particle size also is most im-
portant.
Peebles (22) in his instantizing patent of
N F D M notes that optinmm rewetting, e.laimed
to be 15% moisture, corresponds with a mini-
mmn bulk density of the product. He states
that if too much water is introduced, it becomes
readily apparent by a decrease in the apparent
bulk of the material. Peebles stated this as
a qualitative observation, whereas our study has
shown conclusively the critical nature of re-
wetting moisture upon both dispersibility char-
acteristics and bulk density of the product.
Another interesting point emerges from Figs.
2 and 3 when comparing Niro ~ F D M and
R ~ ' e r s N F D M ; uamely, the very narrow range
of rewetting moistures over which the Rogers
N F D M may be instantized. This result illus-
trates the notion held in the dried milk industry
in the United States float some types of N F D 3 I
are comparatively difficult to instantize. The
reason for this is not clear, although it was
noted in our work that the sample of Rogers
N F D M had an extremely low mean particle
s~_ze, being less than 10 tL.
Effect of particle size. A p a r t from having
elucidated optimum rewetting conditions, it
would be desirable to determine optimmn par-
ticle size of N F D M with respect to dispersibil-
ity. This was approached in three ways: I )
Granulation through different size screens at
above break point moistures; 2) sieving of large
sample produced at break point rewetting to
give different size fractions; 3) grinding of
large sample of granules produced at above
break point rewetting, followed by sieving to
obtain different size fractions.
Granula.tion thro.ugh diff'ere~t .~ize screens.
Batches of Niro N F D M were moistened as
described, using the same quantity of rewetting
water in each case, so as to yield granules of
approximately 14% moisture before redrying.
Instead of grauulation being achieved through
the 1,600-~ screen, as in all the other work, in
this case granulation was done through the
specially manufactured screens of differing
mesh size. Screens down to 80 mesh were manu-
factured, but the finest mesh through which
moistened N F D M could be granulated was 40
mesh. Increasing difficulty was encountered
in forcing the moistened mix through the
screens, as the mesh aperture size was de-
creased. This was evident in drying which oc-
curred during actual granulation--increasing
difficulty in granulation leading to greater
moisture loss. This can be seen in Table 3,
showing the moisture contents of the granulated
J. DAIRY SCIE~-CE V(>L. 51, NO. 3
336 NEFF AND ~[0RRIS

TABLE 3
Moist.ur~ content of nonfat dry milk granulated 70" NIRO NFDM
through different size screens GRANULATED AT 11,6%
,MOISTURE (REDR)ED)
60-
Screen
size Aperture Moisture ~_ 50-
_3
40-
(~) (%) aWL~
:z
]0 Mesh 2,000 14.0 fL ~ 30-
Kenwood screen 1,600 13.6 2O-
]6 Mesh 1,000 13.7 GRANULATED AT 14°/oMOtSTURE
30 Mesh 500 13.3 ~0- (REDRIED AND GROUND )
40 Mesh 390 12.7
o 26o 460 680 860 ~obo
IO-O,

JJ
samples. All batches were rewet with equal INFINITE SINKAGILITy
9.O- ~ /~ NIRO NFDM
quantities of water, and moistures were de- --GRANULATED AT 14°/o MO[STURE
~ermined on the granulated NFD~I. 5.O" (REDRIED AND GROUND)

Since the same amount of moisture was added 7.0-

x
to all five batches initially, these samples may _z 8O-
be assmned to represent equivalent rewetting
~5 . . . . . . . . . . . .
umistures (viz,, 14.0%), the only variable being /~GRANULATED AT 11'E°1~ MOISTURE
m--~ 4-0" (REDRIED)
the granulation size. Good granules were <Z
formed in all cases.
Samples were analyzed for dispersibility .(

porosity, and solubility index. The results are 2.0 200 4~0 5(~0 5~0 10'00 ~200
SIEVE FRACTION -- PARTJCLE SIZE -- MICRONS
presented in Fig. 5.
Sieving of sample prod~ced at break point. FIG. 6 . E f f e c t o f p a r t i c l e size On r c c o n s t i t u t i o n
o f n o n 2 a t d r y milk.
Four batches of Niro N F D M were granu-
]ated using the ],600-t~ screen. The same quan- sieving to yield sufficient fractions in each size
tity of moisture was added to each batch to range for analysis. Eight sieve fractions were
correspond to approximately break point re- obtained and analyzed for dispersibility and
wetting. The moisture content of the moist sinkability index, the results being presented
granules was 11.6%.
in Fig. 6. In addition, a particle size distribu-
Under break point conditions a wide size tion curve was obtained and is presented in
distribution is produced in the dried product. Fig. 7.
Production of four batches, therefore, allowed
Sieving of ground granules. Four batches of
~O ~ , , , i
Niro NFDM were granulated, using the 1,600-~
screen. Again equal quantities of water were

t NIRO NFDM
GRANULATED AT
(REDRIED)
14% MOISTURE
added to each batch but this time corresponding
moisture in the moist granules. The
to 1 4 . 0 %
dried granules were then ground to give a wide
size distribution for subsequent sieving. It
was found that an attrition mill, or coffee
grinder, gave a wide size distribution suitable
for this purpose.
E~4
°1 460 8oo 12'oo
NIRO NFDM
16100 2000
The ground granules were sieve-separated to
w
GRANULATED AT 14°1oMOISTURE
~e (REDRIED) give eight fractions, which were analyzed for
~J
mu G,T
dispersibility and sinkability indices. The re-
2o sults are presented in Fig. 6.
OZ"
From Fig. 5 it can be seen that dispersibility
SE
~8o 88o ~2'oo ~5'o0 2obo of a redried granulated product increases as
e- NiRO NFDM the granulation size is decreased from 2,000
GRANULATED AT 14%MOISTURE
(REDR~ED) to 390 t~- It must be remembered that these
granules were produced by rewetting to 14.0%
J o 4-
moisture, which is well beyond the optimum for
~ •
reeonstitution. Yet, even so, the dispersibility
is increased from 25.0 to 54.3% merely by
0 o ~6o ~& dOG ~560 ~o'o0 2~oo
GRANULATION SCREEN S I Z E MICRONS decreasing granulation size. However, as wet
FIG. 5. Effect of granulation screen size on granulation could not be achieved through finer
properties of nonfat dry milk. screens, an optimum size for granulation has
~T. DAI}~¥ SCIENCE VO]J. 51, NO. 3
 MILK
25 I I I i
NIRO NFDM
GRANULATED AT 11-6/,,MOISTURE
( RED lED
I.--
z20-
bJ
n,-
U.I
a.
z15-
O
I-.-
(9
<
U-IO_
u3
L,O
<
5-
0 !
10 20 35 4S '0
Fro. 7. Particle size distribution of break point granulation of nonfat dry milk.
not been determined. All that can be deduced
from Fig. 5 is that an optimum granulation
size will be less than 390 tL.
Porosity and solubility index determinations
in Fig. 5 show only very slight change with
granulation size. This is as would be expected
as, theoretically, porosity will be independent
of particle size, providing a population con-
sists of spherical particles all of the same
diameter.
Figure 6 shows the effect of particle size
upon reeonstitution characteristics for a nmre
complete particle size range. I n this instance,
an optimum particle size has been determined.
I n both granulated powders, that is, rewetting
to 11.6 and 14.0% moisture, the optinmm par-
ticle size has been determined at approximately
200-t~ diameter. This optimum represents op-
timum dispersibility togther with infinite sink-
ability. I t may be emphasized that the maxi-
mum dispersibility of 75% obtained for the
optinmm size, optimum rewetting fraction is
higher than any commercial instant powders
tested by Neff and Morris (19).
I t should be noted that beyond 130 and 180
particle size for the 14.0 and 11.6% rewet
granules, respectively, there was an infinite
sinkability index, when the powder no longer
floated on surface of the reconstituted liquid.
POWDER AGGLOMERATION 337
I I I I I
o /'~
] \
I
1 O0 250 350 400
' 500
' '
1000 2000
PARTICLE SIZE MICRONS
(LOG SCALE)
This phenonlenon of a particle sinking beyond
a critical size would require a knowledge of
solid-liquid surface tensions and contact angles
at the water surface for any quantitative treat-
ment. However, qualitatively this change to
infinite sinkability may be explained as fol-
lows: The force tending to submerge a par-
ticle on the surface is its weight less the buoy-
ancy effect. As the radius, R, of a particle
increases, this force will increase as a function
of R ~. On the other hand, the force supporting
the particle on the surface is due to a surface
tension effect, being a function of perimeter in
contact with the water. This supporting force
will vary with R only. Therefore, on increase
in particle size the surface perimeter-to-mass
ratio of the particle will decrease. I t is rea-
sonable to predict, therefore, that a critical size
exists where the force tending to submerge the
particle becomes greater than the force tending
to support the particle at the surface. This
critical size appears to be approximately 130-
180 ~ for N F D M granules.
F r o m the particle size distribution curve in
Fig. 7 it is seen that at break point rewetting
the final product consists of a population
with two definite peaks at 130 and 680 F. This
is interesting, because optimum size is ap-
proximately 200 t~, indicating that dispersibility
J . ])AIRY SCIENCE V0~. 51, NO. 3
338
of this p r o d u c t could be increased f u r t h e r by
r e d u c i n g the oversize fraction.
Since the w e i g h t f r a c t i o n a n d d i s p e r s i b i l i t y
of each size f r a c t i o n is k n o w n ( F i g . 6 a n d 7)
in the case of the 11.6% rewet g r a n u l a t i o n , it
is possible to calculate a weighted average dis-
p e r s i b i l i t y f o r the mixed g r a n u l a t i o n . The
weighted a v e r a g e dispersibility is 52.7%. I n
comparison, the m e a s u r e d d i s p e r s i b i l i t y of a
smnple of the n o n f r a c t i o n a t e d g r a n u l a t i o n is
52.4%. This close a g r e e m e n t emphasizes the
i m p o r t a n c e of p a r t i c l e size in influencing dis-
persibility.
F i g u r e 6 serves well to i l l u s t r a t e the i m p o r -
tance of both p a r t i c l e size a n d r e w e t t i n g mois-
ture on the dispersibility of the final r e d r i e d
g r a n u l a t e d p r o d u c t . The 14.0% r c w e t g r a n u l a -
tion exhibits a lower dispersibility t h a n the
11.6% r e w e t p r o d u c t at a n y p a r t i c u l a r p a r t i c l e
size. F o r example, a t 400 ~ size the f o r m e r
p r o d u c t has a d i s p e r s i b i l i t y of 25.3%, while
the 11.6% rower p r o d u c t has a dispersibility
of 67%.
Acknowledg ments
The authors gratefully acknowledge the advice
of and discussion with G. ]3. Latimer of the Food
Technology Department, Massey University, and
the co-operatlon of various staff members of the
New Zealand Dairy Reseaxch Institute.
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