Processing

THE RHEOLOGICAL BEHAVIOUR AND PREFUGALLING OF

LOW GRADE MASSECUITES

Timbul Ananta and Edi Purnomo

Indonesian Sugar Research Institute

ABSTRACT
Work and experiments to minimize the negative influences of mas-
secuite temperature, rheological behaviour of final molasses, crystal size,
crystal uniformity and crystal content are reviewed. Viscosity measure-
ments show that Indonesian (Java) low grade massecuites have low
viscosity figures in comparison with viscosities of Australian and South
African molasses. The relationship between calculated crystal content and
viscosity ratio is statistically significant. The prefugalling operation up to
a certain crystal content and viscosity ratio of the final massecuites which
was done at sugar factories, shows a decrease in the viscosity ratio and
to a certain extent a decrease of the practical difference.

INTRODUCTION
The rheological behaviour of sugar factory products, especially the final
massecuite has a big influence on the efficiency of the boiling house in a sugar
factory. The rheological behaviour of a mixture of sucrose crystals and impure
sucrose solutions depends on the following factors: temperature, rheological
behaviour of the mother liquor, crystal content, crystal size and crystal form. Efforts
are made in the sugar industry to minimize the negative influences of these factors.
The influence of the crystal content on the efficiency of the boiling house became
especially important after the adoption of continuous centrifugals, continuous
crystallizers and vertical crystallizers.

LITERATURE SURVEY
The influence of temperature
Michely and De Gyulay21 found a relation between viscosity and temperature
for final cane molasses of constant purity at different dry matter contents. For
saturated molasses at a given purity, usually there exists a temperature of minimum
viscosity; in the tests reported that temperature was found to be between 50 OC and
60 "C. It has become common practice to prepare for the separation of crystals
from final molasses by reheating the cooled final massecuites to 50 "C to 60 OC.
Temperature has a strong influence on the rheological behaviour of massecuites
but the relationship is complex and the experiments of Done9, Kaga17 and Awang
and White2 did not produce a significant correlation between temperature and
TIMBUL ANANTA AND ED1 PURNOMO 689
viscosity ratio at a constant crystal content. Garcia12 gave nomograms for cal-
culating the effect of temperature on the flow index of non-Newtonian massecuites
and molasses.
The influence of the rheological behaviour of final molasses
Jennings and others 25> 5, 22 found great influences of gums and polysac-
159

charides on the rheological behaviour of impure sucrose solutions. Sugar beets enter
the sugar factory cleaner than cane stalks. Sugar beet juices are purified more in-
tensively by liming and carbonatation and at a higher temperature in comparison
with cane juice. These are the reasons why cane juice contains more polysaccharides
and gums in comparison with beet juices. Cane molasses have a relatively higher
viscosity value and are mostly non-Newtonian bodies, while beet molasses are usually
Newtonian bodies. The viscosity value of beet molasses decrease with the desugarisa-
tion of the m o l a ~ s e 28,
s ~3.~ ~
The contrary happens with cane molasses: the viscosity values increase with
the desugarisation of the molasses20* 23. TO avoid high viscosity molasses
l81

extraneous matter shall be separated as much as possible from the cane. The cane
should be harvested when the cane stalks are mature. The time between harvesting
and milling should be as short as possible. Burnt cane should be harvested and milled
as quickly as possible. The trash should not exceed 5%. Juice purification should
be done according to the standards. The amount of chemicals used, the temperature
and pH should be controlled.
The influence of size and uniformity of crystals
The influence of crystal size is less than that of crystal content. Done9 found
that crystal size has practically no influence on the rheological behaviour of
massecuites. Kelly19> l3 found that larger crystals increase the viscosity of
2l

massecuites at constant crystal content and temperature. Awang and White2 stated
further that the influence of crystal size diminished with reduction in crystal size
distribution. Kaga17, Thiele and LuhrZ7found that smaller crystals should increase
the viscosity of the massecuites with the same crystal content. When the crystal size
decreases collisions occur more frequently and the viscosity increases. Delavier7
stated that the ratio of the viscosity ( q),, of the suspension and viscosity ( q),,
of the corresponding mother liquor, when the suspended particles are spherical,
is independent of the size of the particles, and depends only on the volume of the
particle content of the suspension. If the particles are not spheres, the viscosity of
the suspension increases considerably for the same relative volume of suspended
particles and the rheological behaviour becomes very complex.
Based on the results of Carebet4 the use of fondant for full seeding is now
common in the Indonesian sugar industry and has done much to increase the
uniformity of crystal size in the final massecuites.
The influence of crystal content
Crystal content is an imp,ortant factor in the rheological behaviour of mas-
secuites. When plotting crystal content against log viscosity, Done9 found that the
slope of the curve increases with increasing crystal content, especially when the crystal
content is higher than 30%. Kaga17 did not find the same tendency up to 40%
 PROCESSING I
crystal content. T e r e n t e ~ Gromkovskii14,
~~, Artyukov and ~ a r ~ a z huseda ' model
rnassecuites with a crystal content up to 52%. From all experiments it can be con-
cluded that the viscosity of massecuites increases with increasing crystal content.
This paper deals with efforts to reduce the crystal content of processed
massecuites by prefugalling, so that the boiling house efficiency will increase because
of the low viscosity of the massecuites. This pre-fugalling has been applied success-
fully in the beet sugar industry ( ~ e i n e f e l d ~It~ )developed
. after the introduction
of continuous centrifugals, continuous crystallizers and vertical crystallizers.
MATERIALS AND METHODS
Viscosity trials
Samples of massecuites were taken before the continuous centrifugals and the
corresponding molasses were sampled without dilution. These samples were analysed
for sucrose by double polarization, brix by refractometer and viscosity using a Searle
type rotation viscometer (Brookfield viscometer with spindles No. 6 and 7). The
crystal content was calculated from the analytical results according to first
principles -

Crystal % massecuite = [(P,, - P,,)/(100 - P,,)] x Bx,, where

P,, = gravity purity of massecuite
P,, = gravity purity of molasses
Bx,, = brix of massecuite

Prefugalling trials
Trangkil has 6 batch and 4 continuous crystallizers. The massecuites flow first
into the batch crystallizers. Hot molasses is returned and mixed in proportion 10%
to 20% with the original massecuite; the mixture is pumped to the continuous crystal-
lizer~.The cooled massecuite has a temperature of 47 "C and before entering the
centrifugal is reheated to 54 "C. The D prefugalled sugar is mixed with the rest
of the D sugar.
Similar operations are carried out at Sragi and Krebet Baru 11. Sragi has one
strike receiver and 9 continuous crystallizers while Krebet Baru I1 has one strike
receiver and 3 continuous crystallizers. The hot prefugalled molasses at Trangkil
and Krebet Baru I1 is pumped back and mixed in the strike receiver, while at Sragi
the hot prefugalled molasses flows straight to the continuous crystallizers.
The flow of the massecuites at each factory is shown in Fig. 1.
Samples taken were:
- D massecuite as dropped from the vacuum pan
- Massecuite and mother liquor at entrance into the centrifugals
- Final molasses and D sugar.
The samples were analysed for pol, brix by piknometer (Java method), sucrose
by double polarization, conductivity ash, reducing sugars (Lane and Eynon) and
viscosity using a Searle type Brookfield viscosimeter with Spindles No. 6 and 7.
Practical difference (P.D.) means the difference between the obtained purity and
the target purity according to Douwes Dekkerlo.
TIMBUL ANANTA AND ED1 PURNOMO

uua reheater

4
final mo-
lasses
w "D"
D.l.sugar
centrifugal

receiver

u+ d~stributionmixer
and reheater

+
D.1.sugar
final molasses

receiver

Krebet Baru I1 sf.

continuous crystalli-
distributi- zer m i s t r i b u t i o n mixer

"D"centrifuga1
final molasses

receiver

FIGURE 1. Prefugalling in Sragi, Trangkil and Krebet Baru II S.F.

RESULTS AND DISCUSSION

Viscosity trials
From Table I it can be seen that the viscosity figures of Indonesian massecuites
are lower than those in Australia (277 to 1790 P a s at 50 OC, Henderson and
692 PROCESSING

Kirby15) and South Africa (540.to 840 Pa s at 60 O C , De Robillard8) at practically

the same purity figures. (Note: 1 Pa s = 10 poises).

TABLE I. RESULTS OF VISCOSITY TRIALS

Sugar rlma
factory Pas
Ngadirejo 215
130
320
Gending 95
90
97
125
Jatiroto 190
190
190
222
Prajekan 65
175
140
Tasikmadu 100
135
82
145
Assembag us 175
170
105
Krian 125
390
140
Gempolkrep 135
135
140,
125
130

The much lower viscosity of Indonesian products may be explained by the

different composition of the nonsugars substances, which might be influenced by
the specific conditions of the Java cane, among others the processing of only plant
cane, the manual harvesting of the cane green and with rather careful detrashing.
In those factories in Indonesia in which ratoon cane is processed, preharvest burning
is done, especially outside Java, and during unfavourable weather conditions the
viscosity figures of the products usually increase.
The relations between the main quantities for characterizing the massecuites
and the respective molasses were statistically evaluated. Correlation between the
brix of the massecuites and the absolute viscosity of the massecuites was not
significant. Between the calculated crystal content and the absolute viscosity a
TIMBUL ANANTA AND EDI PURNOMO 693
positive correlation has been found to be r = 0.48** (crystal content against log
viscosity ratio r = 0.52**). Between the calculated crystal content and the viscosity
ratio, VR, a positive correlation has been found to be r = 0.58** (crystal content
against log viscosity ratio r = 0.64**).
Taking the equation of Gromkovski and Fursov13 as a basis for an evaluation
of the function between the crystal content and the log viscosity ratio - the crystal
size of Indonesian low grade massecuites is about 0.3 mm - a diagram was prepared,
see Figure 2. Crystal sizes 0.2 and 0.4 mm were used to calculate the respective curves.
The numerical values for Indonesian massecuite samples tended to follow the 0.4
mm curve. It has to be mentioned that during the factory tests the massecuites and
molasses could not be deaerated, so the figures represent the'values as they are found
under practical conditions of the sugar factory. It is well known that viscosity is
increased and rheologic behaviour is changed when bubbles are dispersed in crystal
suspensions and sugar solutions. It is of importance in those processes in which
low grade massecuites are refugalled and the run-off recycled to the massecuite,
(Smolnik and ~ e l a v i e rReir~efeld~~).
~~, A regression curve of better approximation
than a linear one was calculated for crystal content and viscosity ratio; it was VR
= 21.005 - 1.115 x + 0.018 x2. For any selected crystal content the viscosity of
the final massecuite can be predicted from the viscosity of the molasses, assumed

Gromkovskii & Fursov

-------- Viscosity trials

FIGURE 2. Comparison of Gromkovskii and Fursov equation and results of viscosi-

ty trials and its equation.
694 PROCESSING

TABLE II. RESULTS OF TRIALS WITH PREFUGALLING

Trangkil SF Sragi SF Krebet Baru SF

Prefuge % Prefuge OO
/ Prefuge O/O

VR 8,3 7,8 6,9 3,5 9,2 5,9 3,8 3,5

11,4 5,5 9,4 4,2 7,O 5,8 3,9 3,4
9,2 4,5 9,6 4,8 8,8 5,4 3,8 3,7
7,8 5,8 7,5 4,1
Crystal con- 40,5 39,5 39,O 37,6 46,5 41,O 393 36,l
tent OO/ 40,8 34,7 40,4 48,5 44,6 41,2 38,6 37,4
40,O 39,8 41,2 36,8 44,l 42,2 38,8 36,4
41,6 40,O 40,6 34,8
Practical 6,4 4,3 7,7 2,9 7,O 5,9 5,9 7,8
difference 4,5 6,6 7,3 1,2 8,5 6,l 3,3 7,4
6,4 2,9 5,1 1,7 7,O 6,5 2,7 8,O
5,3 5,9 6,9 5,5
Apparentpu- 59,2 59,3 61,6 61,5 64,O 59,7 61,3 60,8
rity of the 58,5 57,6 60,9 62,O 62,O 60,l 60,7 62,5
original D 58,9 58,9 60,6 61,2 61,3 60,l 60,4 62,O
massecuite 59,1 593 61,2 61,5
Apparentpu- 59,2 56,9 61,6 57,O 64,O 58,1 573 57,l
rity of D 58,5 55,3 60,9 56,8 62,O 57,6 56,2 58,1
massecuite 58,9 56,9 60,6 56,6 61,3 59,8 57,1 57,6
after prefuge 59,1 57,4 61,2 57,2
Prefugalling trials
The results of the prefugalling trials are shown in Table 11. The relationships
of the percentage of massecuite pre-fugalled, the respective VR, C, and PD were
statistically evaluated. Table I11 shows the results of the statistical evaluation.
Regression lines have been drawn for the correlation of % prefugalled massecuite
(P,) v C,,; P, v VR; P, v PD as shown in Figure 3.
The VR decreases with an increase in P, acording to the regression line VR
= 8.292 - 0.26 P, which means that, in the interests of massecuite viscosity,
prefugalling up to 20% can be recommended. However the PD, which decreases
significantly up to 15% is improved very little by a rise to 20% prefugalling.
The prefugalling of massecuites reduces crystal content, but if this is reduced
too much, the rate of crystallization will be lowered so the purity of final molasses
 VR
and
P.D.

0 5 10 15 20
OO
/ prefugalling

FIGURE 3. A = % prefuge V. crystal content (C,,)

B = OO/ prefuge V. practic. diff. (P.D.)
C = prefuge V. viscosity ratio (VR)
 PROCESSING

will rise. This happened in the second test a t Trangkil a n d the fourth test at Sragi
I
where the crystal contents were respectively 34.7% a n d 34.8%.
There does also exist a positive correlation between crystal content and viscosity
ratio. T h e correlation was f o u n d t o b e r = 0.59XXf o r r = 28. T h e regression
equation was VR = - 11 928 + 0.453 C,,. According t o Table I1 a n d this
regression line prefugalling u p to 37%, which corresponds to a VR = 5.0 does not
bring any problems a n d can b e recommended.

CONCLUSION
Indonesian low grade massecuites have relatively low levels of viscosity i n
comparison with Australian a n d South African products. T h e relationship between
calculated crystal content a n d viscosity ratio is statistically significant. T h e viscosity
ratio of final massecuites can b e predicted f r o m t h e regression equation if the
viscosity of t h e molasses is known.
F r o m the viewpoint of viscosity ratio a n d practical difference prefugalling to
a crystal content of 37% is recommended. This corresponds to a viscosity ratio of 5.
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