119

Chapter 8

CLARIFICATION OF CANE JUICE

Every sugar technologist knows that, without good clarification of sugar

cane juice, the production of good quality raw sugar is impossible. The pur-
pose of clarification is the precipitation and removal of all possible non-
sugars, organic and inorganic, and the preservation of the maximum sucrose
and reducing sugars possible in the clarified juice. Poor clarification of cane
juices complicates the entire process of sugar manufacture. In many cases
where juices remain dirty after prolonged settling, it is necessary to stop
grinding and allow additional time for settling the mud. This quite often
occurs in raw sugar factories which receive mechanically-harvested or
mechanically-loaded sugar cane, a subject discussed in Chapter 3. Generally,
when difficulties in clarification and settling of mud arise, it is recommended
to increase the capacity of the clarification station by installation of addi-
tional continuous clarifiers. However, excessive capacity in clarifiers may
result in loss of sugar. Therefore, increase in settling capacity must be care-
fully planned and the different factors taken into consideration. The greatest
part of sugar cane juice is water and organic compounds, mostly sucrose,
dextrose and lévulose, the last two supposedly in equal amounts. There are
other less important reducing substances present, and approximately 0.5%
of the cane juice consists of soluble inorganic compounds or ashes. A certain
amount of fiber, mainly cellulose, also remains in sugar cane juice after
crushing, which passes through the cush-cush screen in the form of so-
called 'bagacillo'. The raw cane juice is generally limed to ca. pH 8.0 in order
to obtain clarified juice of about pH 6.8—7.2.

Clarification Process

Importance ofP2Os in Clarification

In the clarification of sugar cane juices the presence of an adequate

amount of phosphoric acid is very important. Insufficient available P 2O s in
the cane juice is one of the causes of poor clarification. The amount of P 2O s
present in cane juice must be no less than 300 ppm. If the juice is deficient
in P 2O s, it must be made up to this minimum before liming. The P 2O s added
to the cane juice can be in the form of phosphoric acid (H 3P0 4) 85% syrupy,
mono-calcium phosphate (CaH 4(P0 4) 2 · H 20 ) or tri-calcium phosphate
(Ca 3(P0 4) 2), which is of the fertilizer type. The latter two should be
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prepared in aqueous solution in a small tank or wooden barrel. It takes some-

what longer to leach P 2O s from tri-calcium phosphate. All of these phos-
phates contain ca. 48% of available P 2O s. The juices treated with phos-
phates should be limed to pH 8.0—8.5. Formerly, this was presumed to
form tri-calcium phosphate directly, but according to Carpenter (1965), the
reaction produces a mixture which seems to be octa-calcium phosphate
pentahydrate and hydroxyapatite, with sometimes a little anhydrous
dicalcium phosphate present.
There are other clarifying agents on the market, which in some cases may
improve the quality of clarified juice, but on the whole it has not yet been
proven that any product is more beneficial to clarification than phosphoric
acid and lime. It must always be remembered that phosphoric acid should be
added before liming.

Temperature for Clarification

Another important factor in the clarification process is the temperature.

The limed raw juice entering the clarifier should be heated in heaters to
104°C (220°F), slightly above the boiling point of cane juices of 13—16°
Brix. At this temperature the viscosity of cane juices is reduced, and when
juice passes through the flash tank, the occluded gases are eliminated. At a
lower temperature, clarification becomes more difficult because of slower
settling of suspended matters in juice. Elevated temperature is important
because it aids the necessary coagulation of albumin and nitrogen substances
and flocculation of lime and phosphates in juice. On the other hand, high
temperatures lead to destruction of invert sugar. With increasing pH and
rising temperature the rate of invert sugar destruction increases. The stability
of invert sugar is maximum at pH 3.0.

Destruction of Invert Sugar

Sucrose is quite stable and at above pH 7.0 can withstand quite high
temperatures. There is, however, a danger of destruction of invert sugar,
which in the presence of an excessive amount of lime forms acids which
lower the pH and cause inversion of sucrose. Inverted sucrose will form more
organic acids, which in turn produce further inversion. This will increase
losses of sucrose in final molasses, because sucrose will have a tendency to
replace the lost invert sugar, and therefore the yield in crystallized sugar will
decrease (see Chapter 13).

Variations in pH in the Clarifier

It has often been observed that the pH of juices in clarifiers varies in dif-
ferent compartments. If liming has not been correctly executed, the varia-
tion will be sufficiently great as to produce overliming of juices in some
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clarifier compartments and underliming in others. Hence, the destruction of

invert sugars, the formation of acids and the inversion of sucrose will occur
in some compartments, while in others sucrose inversion will be induced
because of low pH.

Effect of Retention Time on Juices

The retention time of juices in clarifiers at high temperature has a great

effect upon the juice and its components. If the juices are refractory, or con-
tain a large amount of suspended matter of low density, it may seem logical
to retain the juice as long as possible in the clarifiers. For this reason, many
sugar factories install clarifiers of excessive capacity, especially in cane sugar
factories which grind mechanically-harvested or loaded cane. Because of the
larger capacity of the clarifiers, and the consequent excessive retention time,
the vicious circle of destruction and inversion begins. Hence, excessive
capacity should be avoided in order to preserve the sucrose, dextrose and
lévulose of the raw juice. Other means can be found to eliminate the exces-
sive mud which was brought with sugar cane from the fields.

Purity of Clarified Juice

Increase of Apparent Purity of Clarified Juice

In many sugar factories, a rise of apparent purity can be observed in the

juice after clarification. This is due to destruction of lévulose (levorotatory
sugar) which polarizes to the left, leaving dextrose, which is a more stable
sugar and is dextrorotatory, and therefore polarizes to the right. Its polariza-
tion adds to the polarization of sucrose and results in a higher apparent
purity. Also because of a destruction of lévulose and formation of acids the
Brix of juice decreases and this also increases apparent purity. Actually,
apparent purity should remain without much change. If true purity is deter-
mined by the Clerget method, there is no appreciable difference in purities
of raw cane juice and clarified.

Glucose Ratio

In many raw sugar factories, inversion is measured in terms of the Glucose

Ratio
Percentage reducing sugars X 100
Glucose Ratio =
Percentage sucrose (Pol.)
This formula has little value for determination of inversion. If lévulose is
destroyed during the process of clarification, the Pol. will increase and there-
122

fore the Glucose Ratio will decrease. However, inversion of some sucrose
may occur meanwhile, forming dextrose and lévulose. Therefore, it is pos-
sible that by destruction of both sucrose and invert sugars the relation be-
tween the two sugars may remain the same, though there has been inversion.
Most sugar factories show a decrease in Glucose Ratio from mixed juice to
clarified juice, and an increase of apparent purity.

Ash Ratio

The Ash Ratio, which is sometimes used to indicate whether direct polari-
zation has decreased, is inaccurate for the same reason as is the Glucose
Ratio.
6
Sugars per 100 Brix

A better indication of inversion than those described above is to compare

total sugars in mixed and clarified juices. Since the amount of invert sugar in
mixed juice is rather small, it will not affect direct polarization appreciably
and therefore (D.Pol+invert) can be considered as the total sugars, and
should be calculated for solids, or 100°Brix. The losses of sucrose, reducing
sugars or Brix in clarified juice or syrup can be determined using the
Chloride Ratio method (Davis et al.).

Preservation of Juices During Shut-down

When sugar factories stop operating over the weekend for cleaning evap-
orators and heaters, the drop of apparent purity of clarified juice is usually
very great. Normally, before grinding ceases, the lime dose in the liming sta-
tion is increased, and the juice which remains in clarifiers is overlimed. When
grinding is resumed, there is a considerable increase in color of clarified juice
and decrease in purity, indicating a large loss of sucrose. The pH also drops,
which shows the formation of acids.
To prevent loss of sugar, the following procedure should be used: the
mixed juice should be limed as usual, and 3—4 h before shut-down, the pH
of limed juice should be raised, not by excess of lime, but by adding soda
ash (Na 2C0 3). When grinding is resumed, a slight increase in color of
clarified juice and a small drop in pH will be observed. However, purity will
remain practically unchanged. In one factory, during eight shut-downs the
average apparent purity of clarified juice before shut-down was 82.8% and
apparent purity at the beginning of grinding after shut-down averaged
75.07%. In the same factory, after shut-down 25 lb of sodium carbonate per
1000 gal of clarified juice (3 kg per 1000 1) were gradually added to the
draw-off box, and clear juice from all compartments was circulated for three
or more hours. Because the experiments were conducted at the end of the
crop, the apparent purities were higher, and the following results were
 123

obtained: apparent purity of clarified juice before shut-down was 87.63

and the pH 6.4; after soda ash was added and at resumption of grinding the
apparent purity was 87.76 with the pH 7.20. The same practice was
adopted in other raw sugar factories with similarly good results.

Cleaning

Liquidation

It is very important that continuous clarifiers be liquidated during the crop

from time to time for thorough cleaning, the more often, the better. The
period of operation of clarifier without liquidation should not exceed six
weeks.
During continuous clarification, most of the mud which settles on trays
in the clarifier is removed by 'squeegees' and finds its way into the mud
thickening compartment, from which it is removed by diaphragm pumps.
Nevertheless, a certain amount of mud always remains on the trays. Mud is
the perfect medium for development of microorganisms. Thermophilic
bacteria can withstand 125°C (257°F), a temperature higher than is ever
attained in the clarification process. The microorganisms, growing and multi-
plying in the mud which is not removed by the squeegees, after a certain
period of time produce gases which eventually find their way toward the
surface, and in moving upward produce a disturbance in the clarifier and
prevent settling of the lighter type of mud.

Cleaning the Trays

To improve scraping of mud from trays in the clarifier, a chain can be

attached to the scraper arm near the central shaft and at the end of the arm.
This chain should lie at an angle of ca. 30° with the tray top for maximum
drag effect. The type of chain recommended is 0.25 in (6.35 mm)-thick
logging chain, having eight links per foot. One dragging chain for each
settling tray is sufficient.

Screening

Screening of Juices

Thorough screening of raw juices is not advisable. A certain amount of

bagacillo should be eliminated in cush-cush, but complete removal of
bagacillo before clarification acts adversely upon settling. However, screening
of clarified juice is beneficial for crystallization of sugar and further refining
of raw sugars.
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Screening of Clarified Juice

After clarified juice leaves the continuous clarifier it should be screened

to remove bagacillo and fine suspended particles, especially when the raw
sugar factory refines its own raw sugar. Screened juice will produce better
quality raw sugar which is easier to refine. Bagacillo embedded in the crystal
will affect good clarification in the refinery, slow the filtration process and
increase color upon heating.

Screens

Among the different types of screen for clarified juice are rotary and
rectangular vibrating screens. One of the most effective screening machines
for juice is the Sweco Vibro-energy Separator (Figs. 8.1 and 8.2), which has a
vibrating and gyratory motion. The screened juices acquire a slightly
increased color because of oxidation, but this is offset by improved clarity
and brilliancy of juice, which is important to produce high quality raw sugar.

Types of Continuous Clarifier

Stationary batch clarifiers for juice have been replaced almost everywhere
by continuous clarifiers. The better known of these on the market are
RapiDorr 444, the Graver clarifier and "Prima Sep" (both manufactured by
Graver), Bach clarifier, an improved version of which is the Poly-Cell
clarifier, and BMA clarifier.

.oversizedischarge

upper weight

lower frame

flat table

springs

lower weight

•angle lead
graduated
adjustment

Fig. 8 . 1 . Cutaway of Sweco Vibro-energy Separator (courtesy of Southwestern

Engineering Co., Los Angeles, CA, U.S.A.).
 125

Fig. 8.2. Installation of S w e c o separators in the Pennick and Ford plant at Harvey,
Louisiana (courtesy of Southwestern Engineering Co., Los Angeles, CA, U.S.A.).

RapiDorr 444

RapiDorr 444, manufactured by the Dorr-Oliver Company, is a four-

compartment machine with a small-diameter feed chamber at the top (Fig.
8.3). It also has a foam removal apparatus. The feed is distributed to the
various compartments through a hollow rotating central tube, which is
divided vertically. The raw juice is introduced evenly into all four compart-
ments. At each point of introduction, there is a large-diameter feedwell for
uniform feeding and flocculation. The RapiDorr 444 is actually four single-
compartment clarifiers superimposed one above the other. There are one or
two separate pumps for mud withdrawal. Clarified juice is withdrawn from
all four compartments. The limed juice is introduced at the center and flows
outward at a decreasing velocity. Settled muds are moved inward for better
concentration by blades attached to the arms, which are flexibly connected
to the central feed tube.
Normal range of capacities will be in the range 0.70—0.80 ft 2 (0.065—
0.0743 m 2) of thickening area per ton of cane per day, or 24—28 gal (80.8—
106 1) capacity by volume per ton of cane ground. The variation in volume
depends on cleanness of sugar cane. The minimum retention time recom-
mended is 2 h, and the maximum is 3 h. To avoid losses of sugar in the clarif-
126

Fig. 8.3. The RapiDorr 4 4 4 clarifier (courtesy of Dorr—Oliver Co., Stamford, CT, U.S.A.).

ication process, the minimum retention time is desirable. To start operation

of the RapiDorr 444 clarifier, the connecting valves between all compart-
ments must be open. Consequently, at the start it is operated like a conven-
tional machine. After the overflow rate is established, the valves are closed
and the RapiDorr 444 is operated as four separate clarifiers, with the con-
comitant benefits of mud concentration and ease of removal.

Graver Clarifier

The Graver clarifier has trays slanting toward the periphery. The theory
is that settling mud acts as a filtering medium on its way downward. Instead
of being concentrated on each tray, the mud is dispersed, and thickening
occurs at the bottom compartment.
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Prima-Sep Clarifier

The Prima-Sep clarifier has retained the principles of the Graver clarifier,
but with modifications. The upper tray slants downwards toward the center
where primary mud thickens and is removed through a separate mud sump
into the main sump which is located at the bottom. The other trays are
slanted toward the periphery, and are progressively smaller in diameter from
top to bottom (Anon., 1960).

BMA Clarifier

The BMA continuous clarifier for sugar cane juice comprises a cylindrical
container of sheet steel with a conical bottom inclined at a 10° angle (Fig.
8.4). The cover supports both drive and center shaft. The clarifier is divided
into several compartments with conically inclined trays. For a larger grinding
rate, the clarifier is bigger. It has one inlet compartment and five
clarifying compartments, with the bottom one higher for mud concentra-
tion. Each tray is employed for settling of mud. The mud is discharged from
the trays into the mud cone by arms at each compartment. The arms are

Fig. 8.4. The BMA continuous cane-juice clarifier (courtesy of BMA, Braunschweig
G.F.R.).
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driven by a central shaft, the driving assembly of which is mounted on the

top of the clarifier.
Unclarified limed sugar cane juice heated to a minimum temperature of
103°C (218°F) is fed through a distributor device to two or more clarifiers
through an inlet installed tangentially to the inlet compartment. The froth is
diverted into the froth channel by two skimmers and conducted to the mud-
thickening compartment. The clarifying process begins in the inlet compart-
ment, so that preclarified juice is introduced into the five clarifier compart-
ments through the hollow shaft. When entering each compartment, the
kinetic energy of the slow-flowing juice is converted to a perfectly laminar
flow. An immediate settling of the coarser solid particles into the scum cone
is accomplished, so that the settling area is required only for the settling of
the fine particles. The clarified juice is withdrawn at the outer periphery of
each compartment, at eight points at the highest level, by a piping system to
one draining pipe to an overflow box located on the service platform. The
overflow from each draining pipe is adjustable in height, so the quantity and
clarity of the juice withdrawn from each compartment may be controlled
very accurately. For each draft of the clarified juice sample valves are
provided.

Poly-Cell Clarifier

A completely new design of continuous clarifier for cane juice is in-

corporated into the Bach Poly-Cell clarifier (Fig. 8.5). It is a cylindrical tank
 129

with a steep conical bottom which is the mud compartment and thickener.
Inside the clarifier there are many vertical pipes on which are mounted a
very large number of settling chambers. These are small, steeply inclined
cones with open bottoms, and there may be as many as several thousands of
them spaced closely (ca. 3 in). The mill juice, conventionally treated by
liming and heating, enters the clarifier, and mud settles on the surface of the
cones. Under the cone at the top there is a small perforation in the
supporting pipe, permitting clarified juice to run into the pipe, while the
settled mud slides readily from the steep cone surface and flows down into
the mud compartment. If only one inch of juice in the upper end of a cone is
clarified, the juice runs clear from all the small settling chambers, and for
that reason the retention time in the clarifier is claimed to be only one half
or a third of that in a conventional tray type clarifier. Because of the short
retention time, losses of sucrose by inversion are greatly reduced, there is a
smaller drop of pH and therefore less lime is required, which consequently
reduces scaling of evaporators.

Clarification

Volume of Clarified Juice

It should be remembered that the total volume of clarified juice is some-

what larger than the volume of raw mixed juice per ton of cane, because a
certain amount of juice withdrawn from the clarifier with mud is returned to
the liming station with the addition of some wash-water from the mud
filters.

Coagulants

Among coagulants used to improve clarification of refractory juices is

Separan AP-30. Also, Hodag flocculants (Floes 411, 422 and 433) of high
molecular weight polyacrylamide polymers are effective in coagulation and
flocculation. Because of their high activity, only a few ppm are required.
Those products increase the rate of floe formation and rapid settling of mud,
which is easily filtered and washed. High molecular weight polymers are
slow-dissolving, and therefore correct installation must be provided for the
preparation of stock solutions.
Another anionic polymer, Sucrofloc 275, used for clarification of sugar
cane juices is manufactured by Drew Chemical Corporation.

Fig. 8.5 (facing page). Bach Poly-Cell clarifier shown during conversion at Glades Sugar
House, Florida. A great number of small cones are already installed (courtesy of Glades
Sugar House, Belle Glade, FL, U.S.A.).
130

Addition of Electrolytes to the Mud

Electrolytes in amounts of a few ppm can be added to the settled mud

(Rapi-Floc and Eimco process). The filtrate returned to the liming tank,
however, carries a sufficient amount of electrolytes.

Clarification Optimization

Each type of continuous clarifier for sugar cane juice can produce good
quality clarified juice with the required brilliancy and clarity, provided it is
properly operated and raw cane juice is correctly treated. To accomplish
this, the following recommendations are made:
(1) In case the sugar cane is mechanically harvested and loaded, and there-
fore contains a large proportion of field dirt (which may be sand, clay, muck
etc.), it is advisable to wash the cane prior to processing, or clean mixed
juices to prevent excessive retention of hot juice in clarifiers, or the sugar
cane can be dry cleaned by fans blowing air. Today, such fans are installed
in the harvester
(2) If cane juice is difficult to clarify it should be treated with phosphoric
acid before continuous liming. In some cases poly-electrolytes can be used to
increase rate of coagulation. However, exaggerated doses may affect boiling
of low-grade massecuite.
(3) There must be correct liming and proper contact time to accomplish
complete reaction and flocculation.
(4) Prior to clarification the cane juice must be rapidly heated to 104°C
(220°F), and pumping of juice must be uniform. The hot juice must flow
through the flash tank and gases must be separated from the juice.
(5) The pH of cane juice must be the same in all compartments of the
clarifier.
(6) The retention time in the clarifier should be as brief as possible (2—3 h
or less).
(7) Clarified juice should be screened and adjusted if necessary to ca.
pH 6.8—7.2 with a small amount of soda ash (Na 2C0 3) before it is reheated
and pumped to evaporators.

References

A n o n y m o u s , 1 9 6 0 . Sugar Azucar, 5 5 : 42—42.

Carpenter, F.G., 1 9 6 5 . Current activities of the cane-sugar refining research project.
Annu. Proc. Sugar Technol. Ind., 2 4 : 1—135.
Davis, J.G., et al. Undetected losses during evaporation and pan boiling. Dept. Sugar
Technol., Imperial College o f Tropical Agriculture, Circular No. 29.