Module 7. Final
Module 7. Final
Massecuite-Crystallization
And
Molasses Exhaustibility
Module 7: Massecuite-Crystallization and Molasses Exhaustibility
Table of Content
Unit One: General ........................................................................................................................ 4
1.1 Introduction ..................................................................................................................... 4
1.2 The Use of Crystallizers.................................................................................................. 6
1.3 The Operation of Crystallizers ........................................................................................ 6
1.3.1 Lubrication and Reheating of Massecuites ............................................................. 7
1.3.2 Power Requirement to Derive Crystallizers ........................................................... 7
1.4 Pumping of Massecuites ................................................................................................. 8
1.4.1 Calculation of the Output of a Rota Pump .................................................................. 9
Unit Two: Types of Crystallizers .............................................................................................. 12
2.1 Air-Cooled Crystallizers ............................................................................................... 12
2.2 Water – Cooled Crystallizers ........................................................................................ 12
2.3 Vacuum Crystallizers .................................................................................................... 14
2.4 Batch and Continuous Crystallizers .............................................................................. 15
2.5 Massecuite Reheating ................................................................................................... 19
2.6 Crystal Percent Brix in Massecuite ............................................................................... 20
Unit Three: Molasses Exhaustibility ......................................................................................... 35
3.1 What is Molasses?......................................................................................................... 35
3.1.1 What is the Composition of Molasses?.................................................................. 36
3.1.2 Physical Properties ................................................................................................. 36
3.2 Factors Influencing Exhaustibility of Final Molasses .................................................. 39
3.3 The “Nutsch Bomb” Experment ................................................................................... 42
3.4 The Importance of Factory Set-Up ............................................................................... 44
3.5 Losses in Final Molasses ................................................................................................. 44
3.6 Calculation of the Quantity of “C” Massecuite ............................................................... 47
3.7 Decomposition of Molasses ............................................................................................. 50
3.8 Sugar Produced From Molasses.................................................................................... 51
3.8.1 Introduction ........................................................................................................... 51
3.8.2 The Principle behind the Process .......................................................................... 51
3.9 Development of a Better Formula................................................................................. 55
3.10 Analysis of New Formula for Molasses Exhaustion...................................................... 62
Module Introduction
Dear trainees! I welcome you to module seven of the course “Cane Sugar Manufacturing” In this
seventh module we will discuss Massecuite-crystallization and Molasses Exhaustibility.
The module is divided into three units. The first unit deals with massecuite crystallizers. It
discuss about why crystallization is followed after vacuum pan and describes properly the uses
and different types of crystallizers. At around the end of the unit it explains about lubrication and
reheating. It also discuss about massecuite pumping and efficiency calculation of pumps.
The second unit of the module focuses on the issues of the advantages and disadvantages of
different crystallizers. It compares and contrasts the batch and continuous crystallizers. In
addition to these it explains by giving illustrative example how to calculate the crystal percent
Brix in “A”, “B” and “C” massecuite.
The third unit, the last unit of the module, is mainly devoted on the exhaustibility of final
molasses. It deals at the beginning of the unit about molasses and its composition and
calculations to gain in sugar if the purity of final molasses is reduced. It also deals about factors
influencing exhaustibility of final molasses and how to determine the performance of
crystallizers using “Nutsch Bomb”. Finally it describes the influence of the factory set-up and
types of equipments on recovery of sucrose.
Unit One
General
Unit Objectives
At the end of this unit training, the trainees will be able to:
1.1 Introduction
After completion of a strike, the massecuite is still saturated or slightly supersaturated at the
temperature in the pan (70 to 75 0C). On cooling, it becomes supersaturated and further growth
of the crystals is possible. This is the reason why vacuum pans are followed by crystallizers.
Assume the massecuite is cooled from point at point “B”, which corresponds to a temperature
drop of “∆t”. At point “B”, the supersaturation has increased and is proportional to the distance
“Bx”, while at point “A”, it was only “Ay”. If the massecuite is cooled further, there would be a
danger that point “B” would move into the labile zone and false grain could be formed.
The massecuite from the pans (“A”, “B”, or “C”) is dropped into a strike receiver under the
pans, from which it is pumped to the cooling crystallizers. In modern factories, massecuites are
gravitated to crystallizers. The massecuite, after some cooling in the receiver, is supersaturated.
If allowed to stand undisturbed, the crystals will continue to grow until the mother liquor in the
crystal vicinity is exhausted. Migration of sucrose molecules will be inhibited by the viscosity of
the mother liquor and crystal growth will stop.
a) Renew the layer of mother liquor around the crystals and ensure uniform supersatuation
There are practical limits to the temperature to which a massecuite can be cooled in crystallizers.
Viscosity is inversely proportional to temperature (it doubles for every 5 – 10 0C drop in
temperature), and a point reached at which the power required for agitation and the strength of
the equipment limits operation at lower temperatures. In addition, crystals growth rate is also
reduced at higher viscosities.
Crystallizer capacity and the use of crystallizers on various massecuites vary from country to
country. In all, crystallizers are always used on “C” massecuites because they are essential for a
good exhaustion of final molasses.
Another approach to crystallization is to recover the maximum amount of sugar at each strike
(starting with the “A” strike) by cooling, to reduce sugar recirculation in the factory. This
practice is followed in Mauritius and in all sugar producing countries.
“A” massecuites are cooled from a strike temperature of about 70 0C to about 40 0C, and are
centrifuged at this temperature without any reheating.
“B” massecuties are normally cooled to about 40 – 50 0C, and again there is no reheating before
centrifugation.
“C” massecuites are cooled to between 30 and 40 0C in Mauritius and centrifuged with or
without reheating, in some cases. In some countries, the massecuites cannot be cooled to below
40 0C because of high viscosities and have to be reheated to 60 0C before centrifugation.
The retention time in crystallizers varies for the various types of massecuites and also with the
viscosity. It is obvious that retention time is shorter in water cooled than in air-cooled units
(Ratio of 1:3). Optimum retention times are listed below.
The optimum retention time should be determined for each massecuite at every factory by
running NUTSCH purities at various retention times.
With very viscous massecuites, it may be preferable to cool the massecuites to the temperature at
which it can be centrifuged, and to hold it at this temperature than to cool further and then have
to lubricate the massecuties on to reheat in crystallizers.
Massecuites should not be boiled at Brixes that causes problems with pumping and in
crystallizers. On the other hand, inadequate equipment should not be the reason for lower Brixes
in massecuite. Addition of water of lubrication should be discarded.
When reheating before centrifugation is required because of high viscosity, a properly designed
massecuites re heater should be used.
The power will vary with the design and shape of the agitators, the speed of rotation and
massecuites viscosity.
Speed of rotation is usually kept at 1/3 to ½ to reduce power. Faster rotation does not appear to
improve exhaustion. At this low speed, heavy reducers are required with an electric drive and
several attempts have been made to use hydraulic motors or hydraulic rams. They have met with
limited success.
Power required to drive cooling agitators in U-shaped crystallizers varies from 0.12 to 0.3 hp/m3.
Because of their high viscosity and crystals content, masseccuites can only be pumped by
special positive displacement pumps.
The most commonly used type of pump is the ROTA. It is a very simple and sturdy pump. Rotary
gear pumps are more commonly used on molasses. (See Figure 1.2 and 1.3)
Massecuites pumps should be sized for handling peak flows of not less than 35 to 50 % above
normal.
At the high viscosities involved, the pressure drop across bends, valves, etc. can be very high,
and pipe lines should be kept as straight as possible with are radius bends. These pumps are
positive displacement pumps and there should be no valves in the delivery line.
The pump suction should always be submerged and the pumps and pipelines should be steamed
out (low-pressure steam) and drained after use.
Because of the influence of viscosity on power and flow, massecuites should be pumped hot, i.e.
from the strike receiver immediately after striking, and then allowed to gravitate through the
crystallizers to the centrifugals. The high cost of staging for crystallizers may influence this
layout and in some modern factories. “C” massecuites flows from the last crystallizers into a re
heater from which it is pumped to the centrifugals. It would be better to let massecuites gravitate
to the centrifugals through the re heater.
π D2
W = 60 ( − S ) L . n . Pv
4
Where/ W = Litres/hour
D = Diameter of Pump (dm)
S = Cross Section of Impeller (dm2)
L = Width of Pump Parallel to Shaft (dm)
n = R.P.M
Pv = Volumetric efficiency of Pump = 0.6 - 0.75 depending on the Viscosity
Example:
Calculate the efficiency of a Rota Pump for “C” massecuite with the following Characteristics:
W = 40,000 Litres/hour
D = 381 mm
S = 3.0 dm2
n = 31 R.P.M
L = 346 mm
W
Pv =
π D 2
60 ( − S) L. n
4
40,000 40,000
Pv = =
3.14 × 3.81 2
60 × 8.402 × 3.46 × 31
60 ( − 3.0) 3.46 × 31
4
40,000
= = 0.74
54,074
1. With the help of a supersaturation diagram, explain the principle behind the use of
crystallizers.
3. If it not possible to cool all massecuite (“A”, “B”, and “C”) which one would be
more important to cool and why?
4. Describe the two types of pumps generally used to pump massecuites and give the
advantages and disadvantages of each type.
7. Explain with the help of diagram what can happen if a massecuite is cooled too rapidly
after the dropping from the vacuum pan.
8. With the help of diagram describe briefly the two kinds of pumps which are used for
pumping massecuite.
Unit Two
Types of Crystallizers
Unit Objectives
At the end of this unit training, the trainees will be able to:
a) Horizontal
Horizontal crystallizers are U-shaped with a horizontal hollow shaft through which water flows
to tubes which are welded at right angles to the shaft. The best known of this type is the
BLANCHARD, with S-shaped tubes arranged in a spiral on the central hollow shift. Water
circulates from tube to tube due to the rotary movement.
A simplified copy of the Balnchard with straight tubes is common in Mauritius and in many
countries.
b) Vertical
Vertical crystallizers are a relatively new development. They are cylindrical towers with a
vertical shaft to which are fitted scraper arms which may or not contain cooling elements. In
some models, finned tubes have been used as cooling elements. In others, hollow plates are used,
but the most common is the Toury type which is described below:
It consists of a tower about 4.5 to 5 m in diameter with fixed banks of tubes set about 900 mm
apart. The tubes can vary in diameter from 75 mm to 50 mm. the tubs’ banks are scraped by
rotating arms attached to a central shaft. Water flows from bottom to top and massecuites from
top bottom. The temperature drop across a “C” massecuites vertical crystallizer is about 15 0C
and the heat transfer about 215 watt/m2. These crystallizers can be set in series, but because of
head loss, the number of units in series is usually limited to two. Liquidation pumps are required.
A typical installation is shown in Fig.2.1.
Massecuite from strike receiver or straight from discharge of a continuous pan is fed in to
cylindrical crystallizers, which is kept at a higher vacuum (lower temperature) than that in the
pan. The massecuites flashes and the crystallizers is fed from the bottom with green “A”
molasses which has previously been re heated (plate heat exchanger) to a higher temperature
than that in the crystallizer. It, therefore, also flashes and contributes to agitation in the
crystallizers.
Vacuum crystallizers have a short retention time (± 20 minutes), and produced a good increase in
crystals size, with a large drop in purity. They require a temperature difference of at least 12 0C
between the temperature of the massecuite in the pan and in the crystallizer. Because of viscosity
limitations, they cannot be used on low grade products.
Labour Saving
The only serious disadvantage is the difficulty of taking one unit off line for repairs.
A typical layout of continuous crystallizers and cooling water is shown in Figs.2.2 and 2.3.
1. Short circuiting should be avoided by the use of baffles (both overflow and underflow)
2. there must be sufficient head for flow of massecuites (crystallizers at different levels)
3. the connections between units should be large and deep with weir plates for flow
adjustment
Additional massecuites gutters and crystallizer drainage valves can be used to convert batch
operation of one unit has to be discharged.
Continuous crystallizer should be operated full at all times, and the tendency of operators to
centrifuge massecuites faster than it is fed to the crystallizers to get spare capacity at the back
should be resisted. Automatic level controllers are advisable.
The use of the last crystallizers as a massecuites re heater as shown in Figs. 2.2, 2.3 and 2.4 is
not recommended, but it is advisable to be able to circulate warm water in all the crystallizers to
prevent the massecuties from becoming too viscous in case of long stops.
a) Water –cooled crystallizers through which hot water is circulated (not recommended for
reasons already discussed).
c) Specially designed heaters with hot water flowing in tubes and the massecuite outside.
Finned tubes are used. The temperature of the water should not be more than 2 to 3 0C
above that of the massecuite and large surface areas are therefore required. Channeling
of massecuite can easily occur. The head loss through massecuite re heaters can be
important, hence proper design is required.
“A” – Massecuite:
Crystal Percent Brix in Massecuite after Dropping
Figure 2.7: View of the Upper Bank of Cooling Elements of a Vertical Crystallizer
Figure 2.14: Cooling System with Stationary Discs. (Ned. Ind. Industrie)
1. With the help of diagram give a description of the Toory type vertical crystallizer.
2. Draw a setup for three vertical crystallizers installed in series and show the cooling water
and massecuite path.
3. Give the advantage of using vertical crystallizers against the horizontal ones.
7. What are the advantages and disadvantages of vertical crystallizers compared to batch
crystallizers?
10. Explain why cooling by refrigerator water has not been successful.
11. Explain with the help of a diagram the set-up for the two vertical cooling crystallizers
installed in a series. Show the path of the cooling water and the massecuite.
13. Explain the main difference in the design principle behind a crystallizers and an
efficient massecuite reheater.
16. Give a brief description of the principle of operation efficient massecuite reheater.
18. Give a brief description of a working principle behind a continuous vacuum crystallizer.
Unit Three
Molasses Exhaustibility
Unit Objectives
At the end of this unit training, the trainees will be able to:
What is Molasses?
Molasses is one of the by-products of the sugar industry. Hence, as all by-products, it will
contain a certain amount of sugar will be lost when molasses is evacuated from the factory.
Losses in molasses can be very high-in practice it amounts to more than 50 % of all losses i.e.
losses in bagasses, losses in filter –cake and in undetermined losses.
Water 20 %
Sucrose 35 %
Glucose 7%
Fructose 9%
Ashes 12 %
Nitrogenous and Non-nitrogenous Compounds,
Wax, Colourants, Carbohydrates 17 %
100 %
VISCOSITY is one of the most important factors that will affect the exhaustibility of molasses.
From Fig.1 below, we can see that at a high Brix (80) the viscosity at 40 0C is more than double
of the viscosity at 50 0C.
The problem does not start in the factory itself but much earlier, for example:
All the factors mentioned above will directly and indirectly affect the exhaustibility of final
molasses due to viscosity.
Calculation to Show the Gain in Sugar for a Crop of 300,000 Tons of Cane with One Degree Fall
in Molasses Purity
Data
Weight of Crushed Cane 300,000 tonnes
Purity of Mixed Juice 88.20
Purity of Final Molasses 37.70
Purity of Sugar 99.00
Mixed Juice % Cane 105.00
Sucrose in Mixed Juice % Cane 13.02
Sucrose Extracted % Juice 12.00
Sucrose % Mixed Juice 12.40
Polarization of Sugar 98.50
Calculation:
12.00
Pr actical Boiling House Re cov ery = × 100 = 92.17
13.02
92.17
Hence, Boiling House Efficiency = × 100 = 99.68
92.47
Now, if the purity of final molasses was 36.7 instead of 37.7, then theoretical B.H.R. would be:
92.79 × 99.68
= 92.49
100
100
And weight of sugar @ 98.5 O Polarization = 125 × = 127 tonnes
98.5
a) The purity of the “C” massecuite. It should be neither too high nor too low. If too high,
sufficient drop in purity will not be obtained in practice. If too low, viscosity of
massecuite will necessarily be very high and crystals will be small, thus aggravating the
difficulty of molasses separation in the centrifugal. A purity of 59 - 60 is recommended
for Mauritius. However, depending on prevailing conditions the required purity of “C”
massecuite may be different (See Fig. 3.2 below: Graph –Purity of “C” Massecuite).
b) The Purity of the “C” sugar should be at least 84 - 85 otherwise too much molasses and
impurities are re circulated and crystallization is rendered very difficult because of
increasing viscosity of the mother liquor.
From experience and by calculation, it may be proved that the volume of “C” massecuite is
highly influenced by the purity of “C” sugar.
N.B. Very often people think that when the purity of the “C” sugar is low this means that they
are losing less sugar in their final molasses. For the reason given above this observation is NOT
TRUE at all, because recycling a lot of impurities is like getting involved in a vicious circle, and
sometimes it is better to accept losing a bit of sugar in the final molasses by “washing” the “C”
sugar crystals in the centrifugal for a few days so as to remove more impurities to get things back
to normal.
A normal situation exists when a good “C” sugar is produced, having a purity of 85 without
using too much water in the “C” centrifugal and so avoiding re dissolving sucrose in that
important stage of the process.
c) The temperature of massecuite at the time of curing should not be higher than 55 0C,
which is considered the near optimum temperature when curing heavy density
massecuites.
d) The size of the crystals should be around 0.25 - 0.30 mm. However, if the viscosity of
massecuite is snot too high, smaller grain will give better exhaustion of molasses due to a
greater area of crystals.
e) The massecuite should contain crystals of the same size and from any false grain. False
grains will block the passage of molasses and more water will have to be used in the
centrifugals in order to produce a “C” sugar of the required purity. When false grin
passes through the screen, they contribute to the increase of the purity of final molasses.
f) The “C” centrifugal screen should be examined regularly and damaged screens should be
replaced at once.
g) The reducing sugar/ash ratio should be greater than 1.5. It has long known that the
solubility of sucrose is decreased in the presence of reducing sugars and that most
inorganic salts tend to increases its solubility. Hence the importance of aiming at the right
pH during clarification thus avoiding the use of excess lime.
P = 36 - 0.08 r + 0.26 C
Note: Non Sucrose = Dry Substance – Sucrose; and “P” is usually less than “P1” ( which
is the purity of molasses produced). “P” is compared with the true purity “P1” of the
molasses obtained in practice; the difference (P - P1) indicates the gain in purity. Which
remains to be realized in order to attain theoretical exhaustibility.
Example: If “P1” = 38 and “P” = 35.5, the potential gain impurity (38 - 35.5) is 2.5
points. This means that every effort should be made to decrease “P1” so as to come
closer to or even less than “P”.
In Mauritius, since 1996, a formula was developed by M.S.I.R.I., which reads as follows:
4 × R
Re ference Purity ( R.P) = 44.6 −
A
Where/ R = R.S % non sucrose
However, this formula has been revised recently and a new equation has been developed and it is
equal to:
R 3.72 R
Re ference Purity ( R.P) = 36.82 + 157 −
Nse log A
Where/ R/Nse = Ratio of R.S. to non sucrose
In order to asses the performance of the water-cooled crystallizers and that of the centrifugal, a
molasses separator is used and it is called a “NUTSCH BOMB” or a massecuite filter (See
Fig.3.3).
When the massecuite in the water –cooled crystallizer is ready for centrifuging another sample is
taken. The mother liquor is separated by the same means and is analyzed for purity. The
difference between the two purities represents the exhaustion attained in the crystallizer.
Example:
Difference in Purities = 5
The use of the Nutsch Bomb is also very interesting to explain the drop in purity between a “C”
massecuite and its final molasses. The total drop in purity is made up of the sum of:
Pans used in boiling c massecuites must have very good circulation and have sufficient capacity
for the hours of operation required to obtain good results. massecucites must be cooled after
striking for a minimum of 30 hours in water cooed crystallizer . The equipment must be strong
enough to handle high brix massecuites increasing in viscosity during cooling. After cooling “C”
massecuites should be reheated to a temperature of 55 0C or more if required under controlled
conditions. Massecuites should be made to gravitate through the crystallizers, massecuites hater
and the centrifugals. No dilution should be done. Obviously, good pan work resulting in
massecuites with the required crystals content high Brix as well as form crystals without false
grain should always e the aim.
It is well known that molasses % cane depends mainly on the quality of the coming in the
factory; however, this is not only reason. There are certainly other factors that will influence the
weight of the molasses in the factory.
a) Clarification Efficiency
a) Clarification Efficiency
The clarification process is well known to eliminate impurities (mostly inorganic matter) from
juice (i.e. the ashes). If the ashes are not removed with the scum, they will find their way through
the whole sugar process and will be found in the final molasses where over and above their
weights, they are going to maintain more sugar in solution. It is well known that in all target
purity developed, the ashes content has a tendency to increase the purit5y of the final molasses.
If during the processing, reducing sugars are destroyed or sucrose is inverted and sometimes the
two happen at the same time, we can say that, as a result of such, impurities are developed during
the processing. This is why wee must pay careful attention to the following
The latter may not highly influence the level of ashes, but they can be more easily controlled.
River water, which may sometimes contain a high concentration of impurities, should e replaced
by condensate whenever this is possible, i.e. for the imbibition on the mills, for the preparation of
flocculant, for the injection water in the centrifugals. Water that has been used for the wet
scrubber in the decompression chamber to remove ashes from flue gasses of the chimney should
never be re-used in the factory for the process. Similarly, the utilization of ashes in the filtration
process is NOT recommended.
The molasses scale must e as accurate as possible. Even if the price of that product is much
lower than the price of sugar, its exact weight must be known in order to have a good chemical
control ion the factory.
Careful attention must also be paid to the sampling method of final molasses. The pipe used to
collect the sample of molasses must be big enough to allow the samples to flow quite easily.
Otherwise, the sample will contain a greeter proportion of molasses at a lower Brix. A small
volumetric pump is the best alternative to have a representative sample of final molasses.
For a factory crushing 400,000 tonnes of cane per crop, if the loss of molasses % cane can be
reduced by 0.5, this will represent a gain of six million rupees on its profit.
Calculation:
0.5 × 400,000
Difference in the Weight of Molasses = = 2,000 tonnes
100
If that molasses contain a minimum of 30 % saccharose, hence the weight of saccharose in that
weight of molasses will be:
30 × 2,000
= = 600 tonnes
100
0 .5 × 100
Equivalent of Sugar @ 98.50 Pol = = 609 tonnes
98.50
If the price of sugar is Birr 10,000 per tonne, gain in money is:
Data
Purity of Molasses 36
Calculation:
B
Kg Brix in 105 Kg of Mixed Juice = 105 ×
100
105 B
Now using Cobenze’s diagram, the weight of Brix in molasses to be obtained from Kg
100
Brix in mixed juice of purity “P” can be calculated thus:
99 − P
Hence Solids or Brix in Molasses % Brix in Mixed Juice = × 100
63
105 B
Then for Brix in Mixed Juice there are;
100
Now, if from “C” massecuite we obtain “C” sugar and molasses, using Cobenze’s diagram we
can calculate the weight of “C” massecuite that would yield.
99 − P 105 B
× Kg in Molasses
63 100
27
Hence Kg Brix in Molasses % Brix in " C" Mas sec uite = × 100
49
49
and Kg Brix in " C" Mas sec uite per 100 Kg in Molasses = × 100
27
(99 − P) 105 B
and for × Kg Brix in Molasses there will be :
63 100
49 100 99 − P 105 B
× × ×
27 100 63 100
3.025 100
× B × (99 − P) ×
100 95.3
3.174
× B × (99 − P) Kg of " C" Mas sec uite
100
Now, the volume of “C” massecuite is obtained by dividing by the specific gravity at 95.3 Brix
which is 1.519. This will give the weight of c massecuite per 100 Kg cane.
3.174 1
( × B × (99 − P) × × 10 ) Litres / Tonnes of Cane
100 1.519
N.B. this calculation is purely theoretical. However, it is based on factual factory performance
figures. It is important in the since that it will help to have an estimate of the volume of “C”
massecuite and this will help to fix crushing rate to cope with the amount of “C” massecuite to
be expected.
However, it is better to rely on the volumes of massecuites given by the laboratory in its weekly
report. These volumes are based on those of massecuites, which have been boiled and cured
during factory operations.
Sometimes, molasses decomposes very rapidly and as the reaction is exothermic, there is
obviously destruction of the molasses, i.e. the molasses becomes a carbonized mass.
In 1955, a whole reservoir of molasses (2,990 m3) was destroyed at Porto Rico.
In the afternoon of 5 June, preliminary signs of the problem became apparent. In fact there was
like a heavy explosion coming from the reservoir where the molasses was stocked since 4 April.
After the explosion, the molasses overflowed from the reservoir of the capacity of 7,570 m3.
They tried, without success, to empty the reservoir in a nearby river. An intense heat came from
the reservoir and this rising temperature evaporated a large quantity of water and acid vapour.
After all the water from the molasses was evaporated, the latter was transformed in a solid
carbonized mass.
There was an investigation following this accident and the report presented showed the following
points:
ii) It is recommended to re circulate the molasses with the aim to reduce the possibility of
heat liberation in stagnant molasses which otherwise would raise the temperature.
iii) The cause of the accident was due to the rising temperature of the molasses during
storage.
3.8.1 Introduction
The industrial chromatography is developed due to the use of the simulated mobile bed technic
which has allowed a fundamental optimization of this new technology.
Among the most recent application, the recuperation of saccharose presents in the molasses is
certainly the most attractive, both industrially and economically. However, the molasses has to
undergo a pre-treatment for the removal of calcium and certain colloidal matter.
The principle behind the separation of two or more components is very well known. It is based
on the difference in affinity of an absorbent, such as an iron-exchanged resin, for components in
a mixture. These different affinities are related to the speed of migration equally different at a
resin bed.
Example:
Molasses are composed of sugar and non-sugar. The affinity of the resin is more important for
the saccharose. Its speed of migration will thus be slower than the speed of the “non -sugars”.
Hence, in a column of resin, if we introduce molasses which is continuously washed with water.
The fact that the speeds of migration are different, we observe the flowing curve.
At the beginning, the effluent will be richer in non sugars; then after some time, the remaining
sugars will eventually come out. However, this technic does not allow an optimum use of the
resin bed and needs a significant difference in affinity amount the component in order to obtain a
more important separation. And in order to do so, the overall resin bed is divided into multiple
columns having different points of injection as well as extraction as shown below:
The resin used in chromatography should be in the K+ form to obtain the ideal separation and
this implies that the molasses does not contain any Ca++ ions.
This is why sugar factories must be equipped with a deliming unit (which is the best
solution) or the molasses should be delimed before its passage through the chromatographic
separator.
During the process, the molasses has to be diluted a lot (to each tonne of molasses, seven tonnes
of water are added). This of course contributes to make the process very expensive because of
the steam needed to evaporate water for saccharose recovery. The water used is usually
condensate. The quantity of sugar recovered is 90 %, with a purity of 920.
The study was done at the Mauritius sugar Research institute by Mrs L.Wong Sak Koi and Mr S.
Sakurdeep.
Summary: Samples of molasses were taken from the 19 sugar factories of Mauritius during
sugar campaign 1990 – 1991 and were analyzed for their Brix sucrose, reducing
sugar and ashes of sulphate.
An analytical study of the data obtained, taking into account the fraction of non
sucrose and non sugar, was done to look for any simple or multiple linear relations.
The following equation was obtained for calculating the reference purity of the
molasses:
157 R 3.72 R
3.82 + −
NSE Log A
This new equation gives a better indication of the exhaustion of the molasses than that calculated
in 1968, which is:
4R
Re ference Purity = 44.6 −
A
Introduction
It is nowadays known all thought the would that the principle source of sugar loss during the
processing of sugar lies in the molasses. However, the quantity of sucrose that can be extracted
depends to certain on some factors which are:
(a) Viscosity
(d) The nature and Quantity of Non Sugar Present in the Molasses ,mainly:
After the publication of the famous formula of Dowes –Dekker (1949) concerning the theoretical
maximum exhaustion of molasses which equal to 35.886 – 8.088 R/NSe + 26.047 A/NSe,
many countries have developed their own equation in such a way to be able to predict the aiming
purity of the molasses after determination of the nature and amount of non sucrose present ion
the molasses.
The formulae for calculating the exhaustion of molasses were determined from analytical study
of data obtained concerning the real purity of molasses and the quantity of non sucrose present.
Some of these formulate were derived form results obtained in laboratories using adequate
specialized equipment for exhausting, as far as possible, the molasses samples (like this is done
in South Africa and Hawaii). The purity of the molasses which we can predict from these
formulae are well known by the name of target purity , even through it would have been more
appropriate to call if the reference purity. It must also be said that in practice, these reference
purities are sometimes higher than the true purity obtained.
The formula used in Mauritius recently was calculated in 1968 by J.D. de Rivaltz de St. Antoine
and his team, and was equal to:
4R
Re ference Purity ( R.P) = 44.6 − .......... ......................(1)
A
With a correlation coefficient of 0.45.the difference between the true purity and the reference
purity gives a good indication of molasses exhaustion.
but with the improvement brought gradually in the factory at the boiling and centrifuging
department , the possibilities of molasses exhaustion had changed the data and it was time to
review the formulate developed in 1968.
The composite samples of final molasses coming from 19 factories (collected throughout a
period of 15 days) were analyzed for their refractometric Brix, sucrose, reducing sugars and
sulphate ashes (See graph below).
True Purity Vs. Reference Purity For Harvest 1990 and 1991 Equation 1 = 44.6 – 4R/A
The tables (1990 and 1991) give the average, maximum and minimum of the differences in
reference purity * obtained from each of the 19 factories.
*The reference purity has been calculated with the formula of equation I.
Table 1 1990 Crop average of parameters analyzed and RPD for each factory
Table 2 1991 Crop average of parameters analyzed and RPD for each factory
If we now look at the individual mean of the 19 sugar factories for the two consecutive years, we
see that the reference purity dos not vary much and is equal to 41 ± 1 and can therefore make
us draw erroneous conclusions (the general mean of the reference purity for the whole island was
41).
This observation proves that there is an urgent need to review the whole question.
If we make a list of all the formulae used throughout the world to calculate the reference purity.
We observe the following.
Table 3
Different Equations to Calculate the Reference Purity (RP)
Used throughout the World
After having done a statistical analysis by computer, it was decided to use the following
equation:
When applying the new formula to the values obtained in 1990 and 1991, we obtain, for the
molasses from the sugar factories in Mauritius, a reference purity which is more realistic as
shown by the graph below.
Regression between True Purity and Reference Purity (II) for 1990 and 1991 Data
Equation II: 36.82 + 157 R/Nse – 3.72 R/Log A
With the utilization of Equation II, the higher the reducing sugar content, the lower is the amount
of sucrose as well as the reference purity. This corresponds well to the fact that the reducing
sugars reduce the solubility of sucrose in the molasses and, therefore, contribute to the decreases
in molasses content.
The higher the ash content, the higher is the reference purity. This is due to the fact that the
principal components of the mineral slats (potassium and sodium) which are well known for
increasing sucrose solubility increase the amount of molasses.
From the point of view of Dr. N.Deer (1921), in a well exhausted molasses: for one part of non
sugar, there is 0.455 part of water in order to keep it in solution, and for each unit of water, there
is 1.8 parts of dissolved sucrose Therefore, there is 0.82 part of sucrose for each part of non
sucrose
But if we calculate the ratio S/NSe for all the sugar factories of Mauritius, we observe that the
ratio is around 0.70.
1 N.S. = 0.455 H2O or for 0.455 part of H2O, there is 1 part of N.S.
1.8
And for 1.0 = × 1.0 = 0.82 Part of Sucrose
2.2
Table 4
Ratio for All these Factories
FACTORY Crop Average of S/NSe Ratio
1990 1991
1. 0.70 0.73
2. 0.63 0.66
3. 0.62 0.64
4 0.72 0.70
5 0.84 0.87
6 0.67 0.70
7 0.72 0.77
8 0.68 0.74
9 0.78 0.77
10 0.72 0.77
11 0.74 0.76
12 0.58 0.58
13 0.75 0.74
14 0.70 0.69
15 0.78 0.78
16 0.66 0.66
17 0.65 0.64
18 0.64 0.66
19 0.69 0.77
Average 0.70 0.72
It is also interesting to note that factory No.12 has a very low ratio which is 0.58 and which
proves that there is always room for improvement ion the exhaustion of molasses.
Conclusion
The new equation is certainly more precise for indicating the theoretical exhaustion of the
molasses, but it must not be forgotten that these formulate were derived from statistical data. The
possibility of obtaining, in practice, a lower purity for the molasses is large since the molasses
used for the analysis is not and will it self never be completely exhausted.
1. What are the different factors that will directly influence exhaustibility of final molasses?
2. With what apparatus and how can we explain the drop in purity between a “C”
massecuite and its final molasses?
3. What are the factors that will influence the weight of molasses in the factory?
5. With are the different factors that will influence exhaustibility of final molasses when
boiling low grade massecuite?
6. What is Maillard Reaction? How can it be prevented during storage of final molasses?
7. Why is the purity of “C” sugar important and what is its influence on the volume of “C”
massecuite produced?
8. Explain the importance of “C” massecuite purity in the exhaustion of final molasses.
9. What will be the loss in the sugar, for a crop of 500,000 tonnes of cane with two degrees
if molasses purity of:
13. (a) Explain the importance of reducing sugar and ashes content in the exhaustibility of
final molasses?
(b) Why is it important to determine the target purity of molasses?
14. Calculate the gain in sugar at a Pol of 98.50 after having reduced the purity of final
molasses by one degree for a factory with the following data:
15. What is the influence of “C” – Magma or “C”- Sugar purity on the volume of “C”
massecuite produced?