ROLL OF PH AND DOUBLE SULPHITATION TECHNIQUE USED IN

SUGAR INDUSTRY

INTRODUCTION

Sugar Cane
Sugar industry is second largest agro industry in India. Basic raw materials
required is sugar cane. The sugar cane crop products direct source of food sucrose
and a range of by product, which are vast potential reserves for human and animal
consumption.
In a typical sugar industry 100 tonnes of cane produces the following
10- tones of sugar
04- tones of molasses
03- tones of filter mud
0.3- tones of furnace oil
120- tones of fuel gases (at 180 degree cels)
1500- kwh surplus electricity
30- tones of bagasse (26 tonnes is used as captive fuel and 4 tonnes remain
surplus)
Apart from this 30 tonnes of cane tops and leaves are left in field.
Sugarcane generally grown in palaeotropical origin and eastern Asia.
Scientifically Sugar cane is named SACCHARUM OFFICINARUM. It is aC4
plant i.e cane leaves has more efficient assimilation of CO 2 which causes
photosynthesis.
Sugar is produced in the leaves of all known land plants by the process
called photosynthesis, by the combination of CO 2 and water in cells which contain
chlorophyll, in presence of sunlight. Oxygen is given off in the process. The same

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sugar is present in fruits like orange, apples and pine apples, etc. However, since
sugarcane and the sugar beet stores sugar more abundantly than other plants, they
have become the major sources of sugar.

Sugar cane juice contains typically water (83%), Sucrose (15%), reducing
sugar (0.6-0.9%) inorganic non-sugar (0.5%) and mineral water (0.5%).

Non sugars in raw cane juice are carbohydrates other than sugar viz
hemicelluloses (0.5%), Pectin (0.5%) organic non sugars like albumins (7%),
proteins (2%) amino acids (10%) and amides (15%) apart from these, juice also
contains organic acids (13%) coloring matter lipids (17%) inorganic salts (7%) and
silicone matter (2%)

Ash is the matter, which is left after carbonization of the material, and is
mostly mineral water. In clear juice, the ash content particularly in northern region
ranges from 0.7 to 1% of clear juice. While in other parts (ie) Maharastra, North of
U.P. region Karnataka it ranges from 0.4 to 0.5%. But normally the composition
of ash is approximately the same throughout; the quantity of potash is much more
as compared to other especially, Fe, Al and Mg. The general composition of ash is
follows;

1. K2O - 2.5% High 3.5%

2. Na2O - 4% Low 1.5%
3. Fe2O3 & Al2O3 - 9% Low 5.5%
4. CaO - 10% Low 8.0%
5. SO4 (SO3) - 2.5%
6. Mgo - 7.5% Low 6.5%
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7. Sio2 (complex) - 3%
8. P2O5 - 3.5-4%
9. Cl - 3%
10. N - 0.5%

The colors in cane juice can be divided into their groups, which develop
during the different stages of processing. The Colour bodies which are originally
colored, the Colour bodies which are originally non colored but develop colours
during process and the colored compounds while are themselves non colored
substances and formation of new products during processing and become colored
compounds.

The originally colored bodies are classified into water soluble and insoluble
anthocyanins, hydro methyl, furfural, hydroxy methyl juice and nitro generous
glycoside are water soluble chlorophyll, xanthophylls and carotene are water
insoluble.

Organic non sugars are somethings later part in to the formation of different
complexes which may exhibit some amount of colour but normally they do not
take part in the formation of colour and so can be classed as completely non
colouring impurities. These including starch organic acid, aromatic acid, oxalic
arid, succinic acid and formic arid, protein, since carbohydrates, which are non-
sugar waxes and fats.

The compounds which are not originally colored acquire colour during extraction
by reaction with contains, other impurities present in juice and with substance

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added from outside. This behavior changes at different temperatures and PH
while reacting with other elements present in juice. They form altogether new
complex compounds while exhibit colouring. They can be subdivided into
polyphenols (tannins, sauharin, sugar, thyamins and melonoidings) and
nitrocompounds (amins arids like leonine tyrocine and glycines amides, albumines,
gluose and fructose).

The polyphenols react with Fe and oxygen is an alkaline medium give dark
coloured compound. The amino acids and acids etc react with reducing sugars and
added lime to form colored compounds. The reaction is known as maillarde
reaction.

The compounds of non-sugars that develop colour due to decomposition are

classified in to melonoidins and caramels. The sugar under goes maillarde reaction
or Browning’s action with amino acids and form dark colored complex compounds
called melonoidins.
The sugar burns with mineral acids (sulphuric acid) that is degradation
product of sugar, with inorganic acids and ferric substances the red brown
substances become osculated into sugar crystal at low PH when the sugar crystal
burns, itself produce changed substance while gets embedded into the sugar
molecule and produce dark coloured substances called caramels.

There are five forms of constituent present is the juice is the broad lime.
They are sucrose reducing sugar, inorganic acids, organic non-sugars, mineral salts
of organic and inorganic complex compounds. Gums, proteins, many of coloured

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compounds of Fe, Al and si are the examples of colloidal state. Chlorophyll, wax
and oil are the example of crystalloid dispersion. Crush and dust are examples of
suspensions. Fungi and there microorganisms are example of microorganic
substances.

MANUFACTURE OF SUGAR - A STUDY:

Manufacture of sugar involves several unit operations. The raw juice

extracted by the mills having natural PH 5.0 to 5.4 is pumped to the clarification
section and weighed. It is then heated to 60°C to 70°C to coagulate proteins and
amino acids at their iso-electric point using exhaust steam of turbines and treated
with milk of lime and sulphur dioxide gas in a continuous liming and Sulphitation
vessel to 7.0 PH. After absorption to sulphur-di-oxide gas by the incoming juice in
the absorption tower. Excess air and vapour all vent out through pipe. The treated
juice is again heated to 100°C in a set of secondary juice heaters and sent to the sub
sides known as clarifiers. The precipitates that settle in clarifiers is separately with
vacuum filters to separate the juice and the solid portion is known as filter cake
(or) press mud. This clarified juice (ie) separated juice liquid coming out from
clarified is passed through evaporator, to evaporate the water contained in the juice
up to the syrup which contain about 60 % of solid.

This syrup is further heated with SO2 gas up to PH of 4.8-5.0 and stored in
supply tanks before being taken into pan for crystallization.
After absorption of the SO2 gas by the incoming syrup in the absorption
tower, excess air and vapour vent out through pipe. Crystallization in vacuum pans
is done by slurry seeding technique and further developed to the required size as
per the necessity. The boiling steam is adjusted according to the purities of juice
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and quality of final product required. The molasses is separated in the centrifugal
machine.

The crystal separated from centrifugal machine by steam and water is

discharged to sugar conveyers known as grass hoppers. Sugar is dried with hot air
and subsequently cooled. It is then bagged according to size and colour.

During milling the juice and fiber are separated and the separated fibre either
to produce current or sold for paper plant. The water present in cane juice will be
evaporated in the process and the condensed vapors all taken for boiler feed water.
There is a power generation plant in the Salem Co-operative Sugar Mills Ltd.,
Where steam turbines to produce power for the production of steam. Water is
taken from sugarcane itself. Fuel is also takes. Sugarcane after production of
power the exhaust steam is used for heating the cane juice.

There is a distillery plant where the final molasses are used.

COMPOSITION OF CANE & CANE JUICE:

1. Water : 69/75%
2. Sucrose : 8.15%

3. Reducing sugar (Dextrose such as glucose, laevulose : 0.8-2%

such as fructose)

4. Organic matter other than sugars (Proteins, organic : 0.5-1%

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 acids, pentosan, pectin, wax coloring matters etc.,)

5. Inorganic compounds (such as phosphates, chlorides, : 0.2-0.6%

sulphates, Nitrates, Silicates of Na1k, ca, mg, A1 &
Fe)
6. Nitrogenous bodies (Albunilnoids, ancides, : 0.5-1%
aminoacids, ammonia, Xanthine bases etc.,

7. Ash : 0.3-0.8%

8. Fibre (lignin, cellulose, Hemi cellulose etc.,) : 12-16%

COMPOSITION OF CANE JUICE:

1. Sugar dissolved solids : 75-92%

2. Sucrose : 70-88%

3. Glucose : 2-4%

4. Fructose : 2-4%

5. Salts : 3-4.5%

6. Inorganic acids : 1.5-4.5%

7. Organic acids : 1.0-3.0%

8. Gums and pectin : 0.5-0.6%

9. PH of juice : 4.5-5.2%

CANE:
The hole of the material as delivered to the cane carrier.

FIBER:
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 The dry water insoluble in the cane.

IMBIBITIONS:
The process in which water or juice is sprayed on bagasse to min and dilute
the juice presents is the bagasse.

ABSOLUTE JUICE:
All the dissolved solids in the cane plus the total water in the cane and cane
minus filter.

UNDILUTED JUICE:
The juice expressed by the mills or retained in the bagasse for purposes of
calculation.

FIRST EXPRESSED JUICE:

The juice expressed by the first mill rollers and the milling tandem.

PRIMARY JUICE:
All the juice expressed before dilution begin.

SECONDARY JUICE:
The diluted juice which together with the primary juice form mixed juice.

LAST MILL JUICE:

The juice expressed by the last mill of the milling tandem.

MIXED JUICE:
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 The composite juice coming from first and second mill, which is sent to the
boiling house.

SYRUP:
The concentrated juice which from the last body of the evaporator.

CLEAR JUICE:
The supernatant liquid from the settling tank after the removal of impurities.

SUGAR:
The crystal including any adherent molasses recovered from the Massecuite
by mechanical mean.

REDUCING SUGAR:
The glucose and fructose present in the can juice is called reducing sugar.
To led reducing sugar matter determined according to the method described and
expressed in term of invert sugar.

SUCROSE:
This disaccharide of that name also known as sucrose. Indicated by the
formula C12 H22 O11.

CLEARGET DIVISION:
Clear get, a French man in 1849 invented a methods where by the sucrose in
sugar solution could be measured on the Polaris cope regardless of the amount of
invert sugar present. The method used in practice is Jackson and Gills
modification method.
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BAGASSE:
The residual obtained from crushed cane in one or more mills.

FILTER CAKE:
The residual removed from muddy or settling by it.

MOLASSES:
It is the mother liquor is the Massecuite, which is separated from the crystal
by mechanical means.

ASH:
The residual after incineration of all organic matter e.g. sulphate ash when
incinerated with sulphuric acid.

BRIX:
Strictly speaking brix is the percentage by weight of the solids in a pure
sucrose solution. By general acceptance the brix represents the apparent solid in a
sugar as deter mined by the prix hydrometer.

POL:
The value determined by direct or single polarization of the normal sugar
solution in a saccharimeter is used in the calculation.

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INTER CARRIER
The prepared cane which enters the crusher or the first mills as well as the
material, which leaves the latter and travels from mill to mill to the end of the
tandem.
The intermediate carriers are the conveyors which moves the bagasse from
one mill to the feed of the next.

IMBIBITION
Even when bagasse is subjected to high and repeated pressures. It never
gives up all the juice it contains. It approaches minimum moisture of 45% in
general. 40% in the most favourable cases, that is it retains a high proportion of
juice amounting roughly to half its weight.
In order to extract as much as possible of the sugar which it retains. It is
therefore necessary to resort to an orifice since this moisture content cannot be
reduced the effort will be made to replace by water. The juice comprising it, it is
this orifice, which constitutes IMBIBITION.
DIFFERENT SYSTEM OF IMBIBITION
SIMPLE IMBIBITION
The simplest procedure which comes to mind is to add the water to the
bagasse after each mill. This procedure is called simple imbibitions.
COMPOUND IMBIBITION:
In this system water is added before the last mill and the last mill juice to
penultimate will and so on. Finally the primary juice and the mixed juice are taken
to weigh scale. This system however consumes much water which has to be
evaporated later is effective one.

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COMPOSITION OF CANE JUICE
1. sugar dissolved Solids : 75-92%
2. Sucrose : 70-88%
3. Glucose : 2-4%
4. Fructose : 2-4%
5. Salts : 3-4.5%
6. Inorganic acids : 1.5-4.5%
7. Organic acids : 1.0-3.0%
8. Gums and pectins : 0.5-0.6%
9. pH of juice : 4.5-5.2%

PURPOSE OF ADDITION OF PHOSPHORIC ACID IN RAW JUICE

The phosphate content of the juice is the most important factor inefficient
clarification. In sugar cane the phosphates are inorganic as well as organic. The
inorganic phosphates exist as free phosphate ions. Where as the organic exists in
the form of phospholipids. Phospho proteins, Nucleotides, phosphates and hexose
phosphates.
It is under stand able that only the free phosphate ions take put in juice
clarification therefore, juices with adequate quantity of inorganic phosphates are
most desirable. Generally phosphate content of 300 PPM phosphorous pent oxide
is sufficient for better clarification since the phosphate content in juice is normally
less then the desired level, Orthophosphoric. Acid is added in raw juice in diluted
form at 3.5 degree brix. The addition is about 0.0005% on cane.

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TREATMENT OF JUICE AND JUICE HEATING
The cane juice that arrives from the mills contain many soluble and
insoluble impurities. It is turbid and viscous in nature not suitable to manufacture
white sugar. Hence it is necessary to remove the unwanted impurities the stage
known as clarification. It starts from juice heating advantages of it are
1. Deactivates microorganisms responsible for inversion.
2. Increases mixing of M.O.L and sulphur dioxide gas in the juice Sulphitor.
3. Accelerates formation of heavy colloid in the clarifier and thus increases
setting rate.
JUICE HEATING AND CONSTRUCTION OF JUICE HEATERS
Multi tubular vertical juice heaters are used as heat exchangers. Plate and
frame type heaters are also used.
Juice circulation is inside the tubes and the vapour / Steam out side the
tubes. Suitable headers force the juice to pass a certain number of times from
bottom to top and from top to bottom of the heater by restricting the juice each
time to few of the tubes.
The cylindrical shell, made up of M.S plate containing the tube plates is
extended position being divided into compartments by battles. Except for the first
compartment by which the juice enters and the last or outlet. Both of which are
located in the top upper recess for vertical heaters each compartment provides for
two passes, upward and downward. If there are tubes per pass for example there
will be 18 tubes for each compartment 9 upward and 9 downward flow. A view
from above of the top compartment and of the bottom compartment and of the
cover. Showing the made of circulation is given in the figure. Hence while
constructing a juice heater the three important design features are
1. Rapid flow of juice and steam through the heating tubes.
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 2. Efficient removal of condensate water and incondensable gases.
3. Less subject to scaling.

METHOD OF HEATING
The raw juice after weighment is heated uniformly in a juice heater to 70
degree Celsius with Exhaust/Vapour from second body of the both quadruple
evaporator in a single stage heating by two heaters of vertical type. This is then
treated with milk of lime and Sulphitation gas in the juice Sulphitor vessel. To
Coagulate the albuminous or colloidal impurities of the insoluble impurities in the
classifier; the juice is heated to a temperature of 102 degree Celsius successively
by single stage heating by two heaters with exhaust/vapour from vapour
cell/vapour from 1 body
LIME PREPARATION UNIT
MILK OF LIME PREPARATION
The Factory is not having any lime kiln of its own and hence the factory is
purchasing the bunt shell lime from the market to meet its requirement with
scheduled programme of supply throughout the season. The available CaO content
of this supplied burnt shell lime varies from 55 to 75 and the price is being fixed
accordingly. The lime is being intended from the store for one day consumption
and brought to the lime station. The burnt shell lime is being slacked in big lime
slacker with hot water about 55 degree cellcius and the milk of lime that is coming
after the slacker being stored in 3 nos. of storage tanks. The grit’s from the slacker
removed outside means of a screen conveyor the storage vessels are provided with
stirrers in order to avoid any settling of the fine particles in the milk of lime
solution. The milk of lime solution is maintained at 15 to 20 brix and the daily
consumption come up to 4000 kgs. They are very particular in the lime preparation
frequently for about 3 to 4 times in a shift in order to prepare a fresh solution of
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milk of lime for getting a better results in a clarification of process since freshly
prepared CacoH)2 solution is having a better clarification effect.
Lime consumption in this factory is about 0.15% on cane.
SULPHUR DIOXIDE GAS PLANT
In the juice Sulphitation process sulphur dioxide gas acts as a bleaching
agent and it is very important clarification after lime.
Both slaked lime and sulphur dioxide gas are added to the hot raw juice at
70 degree Celsius in the juice Sulphitation vessel continuously.
The sulphur dioxide is generated by burning sulphur in excess of air in
sulphur burners. The reaction taking place at a temperature of 363 degree cellius is
as under.
S+O2 SO2
The gas generally contains 12-16% sulphur dioxide. The formation of small
amount of sulphur trioxide cannot be avoided. This is owing to the reaction.
2SO2+O2 2SO3
If the oven gas is humid the sulphur trioxide formed is transformed in to
sulphuric acid.
SO3+H2O H2SO4
Sulphurie acid reacts with lime to form soluble calciumsulphate, which
increases the lime salt content of clarified juice. Also if increases the corrosion of
metallic surface. At temperatures below 200 deg Celsius the rate of reaction is so
slow that practically no sulphur trioxide is formed. Hence sudden cooling of
sulphur dioxide in the sublimation is helpful in keeping sulphur trioxide percentage
low.

CONSTRUCTION AND WORKING

Batch type sulphur burner consists of
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 1. Melting chamber made of cast iron surrounded by steam jacket.
2. Steam passed is 100 Psig, batch of 50 kg of sulphur loaded in the melting
chamber per charge.
3. A small storage tank with operating valves stays as a convey to the furnace.
4. Dry compressed air is passed in to the furnace by controlling primary air
valve.
5. Furnace cooled with cooled water jacket to control the temperature to about
200 deg Celsius. Then the gas is successively cooled by cooling columns to
70-75 degree Celsius.

SCRUBBER
Cooling the cleaning of sulphur dioxide is done in a vessel called scrubber.
This is a thick shell of cast iron, which is water-jacketed to cool the gas. Since it is
factory own make no bricks is filled to remove the sublimed sulphur.

The sulphur dioxide of the generated gas is found as 10-11% The only draw
backs in the factory regarding the sulphur dioxide generation is that there is no Air
dryer arrangement for the burners

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 CANE JUICE SULPHITATION
VESSEL

MILLS

JUICE SULPHITATION VESSEL

RAW JUICE FROM MILLS
(4.5-5.2ph)

JUICE HEATERS (SECONDARY)

RAW JUICE PRIMARY HEATING 103-105C
HEATING

MOLASSES FLASH TANK

SUGAR
CLARIFIER
(DORR-444-TYPE)
SETITING AID

CLEAR JUICE 6.9-7.1

PH & 96-98c MUDDY JUICE

EVAPARATER VACUUM FILTER

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 PAN BOILING

FILTER CAKE
FILTRATE
CRYSTALLISATION

USED AS MANURE IN
THE FIELD
CARBONATION:

Carbonation implies formation of carbonate of lime for purification of juice

and was introduced in cane sugar manufacture for the first time in java in 1876.
The technology of carbonation was similar to that being practiced in beet sugar
industry and involved addition of excess lime to hot juice follow by Co 2 in two
stages. The first saturated juice was filtered and the filtrate saturated to the point of
obtaining minimum CaO content in the juice in the early stage 4 – 5 % lime stone
was used on cane, which increased the cost of the production of white sugar.
Studies on the various reactions taking place in carbonation and their influence on
the sugar recovery aspects, conducted in the subsequent decades threw more light
on the chemistry of the carbonation process and lead to establishing optimum
condition with regard to temperature, PH, time of reaction and lime doses.

Since then number of modification were introduced in the process such as

(i) middle juice carbonation,

(ii) use of phosphates, besides control systems and continuous operations.
Carbonation is employed only for white sugar manufacture from cane in
some developing countries and is gradually being replaced in India in
favour of sulphitation.

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PRINCIPLES:

Calcium hydroxide combines with carbon dioxide to form calcium

carbonate.

Ca (OH) 2 + CO2 CaCo3 + H2O.

In a saturated Ca(CO3) solution the solubility product will be-

C= (Ca++) (CO3--) / CaCO3

Thus for lower concentration of Ca++ in solution the concentration of CO3

—has to be high.
When carbonate reaction is brought about as above in juice, complex
compounds of lime, CaCO3 with juice components are produced. According to
Van Ginneken and Aten1 when lime and CO2 are made to react in sucrose solution,
the precipitate formed is a complex compound of sucrocarbonate of lime
represented by the formula-

[Ca(OH)2]m[CaCO3]n[C12H22O11]z

These unstable compounds are formed at high pH>11 which are

decomposed at lower pH.

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 The temperature of first carbonation should be 55°C and not higher in view
of the rapid decomposition of reducing sugars at higher temperature and high pH.
The saturation and filtration of carbonated juice takes place in two stages for
completion of precipitation of lime and removal of non-sugars. The second
carbonation is preceded by heating of filtered juice from first carbonation to 70°C
to check growth of microorganism particularly the lactic acid bacteria. In the
second carbonation the lowest CaO is aimed at and to facilitate precipitate
formation and good filtration for removal of nonsugars a certain minimum amount
of CaO i.e. 300-800 mgm. Per litre has to be maintained in filtered juice of first
carbonation. In the first carbonation optimum pH is 10-10.5 while the second
carbonation juice pH comes down to 8-8.5.The residual alkalinity is brought down
to neutral state i.e. 7-7.2 pH by applying sulphitation.

PROCESS

(a) First carbonation: The raw juice is heated to 55°C and to the hot juice
milk of lime of 15°Be’ is added to 10.5 pH. The limed juice is retained in
this condition at least for four minutes to ensure floc formation,
dehydration of gums and pectins and formation of calcium pectinate.
This step is followed by carbonation in which the dose of lime and
saturation are so adjusted as the maintain level of alkalinity at 500 to
1000 mgm of CaO on phenolphthalein using Dupont paper for control.
On completion of lime dose the final juice will have alkalinity of 400-
800 mgms. Cao. Total lime consumption is 1-1.5% on cane, or in terms
of limestone 2.5-3% on cane. This treated juice along with the precipitate
is filtered either in filter presses or continuous filters and filtrates sent for
second carbonation.
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 (b) Second carbonation stage involves saturation of the filtrates which have
pH of 10-10.5, to precipitate free CaO and bring down level of titratable
CaO as completely as possible. In second carbonation 200-400 mgm.
CaO per litre of juice are precipitated and the final pH is about 8-8.5.
The second carbonation is preceded by heating the filtrates from first
filtration to 70°C. This preheating avoids development of lactic acid
forming bacteria and helps formation of CaCO 3 precipitate. After
reaching the desired state of saturation and precipitate formation, the
juice is filtered again and the filtrates sent for neutralization in
sulphitation tank where the pH of juice is brought down to 7-7.2.

The advantages of this process are-

(i) reduction in lime consumption by 30-40%,
(ii) elimination of sulphates with consequent reduction in scale formation in
the evaporator,
(iii) higher non-sugar removal as compared to raw-juice carbonation².

PRECAUTIONS

Carbonation is a robust process of clarification which yields positive

nonsugar reduction and thereby higher recoverable sugar from juice than
sulphitation or defecation methods provided all the conditions of the process are
observed with respect to—
(i) pH and CaO content
(ii) temperature
(iii) time of reaction.
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A part from the proper dosing of lime it is essential to observe following
precautions—
(i) Sanitary conditions at the filter station assume special significance and
filtration after second carbonation has to be at 70°C to prevent microbial
growth particularly the lactic acid forming bacteria which thrive at the
expense of sugar.
(ii) Longer contact of alkali, than required for the reactions results in greater
destruction of reducing sugars.
Washing of filter cake at the end of filtration cycle needs to be thorough to reduce
loss of sugar in filtercake.

SCOPE AND OBJECTIVE OF THE WORK:

Our main aim is to produce good quality white sugar. In the manufacture of
sugar in sugar industry. Various process are followed, ie carbonation and
sulphitation process. In salem Co-op. sugar mills double sulplitation technique is
used to produce good quality white sugar.

Double sulphitation means, “Juice sulphitation and syrup sulphitation. In

juice sulphitation milk of lime and So2 gas is passed to mixed juice, to remove all
non sugars from mixed juice and the juice is converted into clear juice. The clear
juice is evaporated by using steam to converted in to concentrated syrup.

In syrup sulphitation process the So 2 gas is passed through concentrated

syrup to bleaching the syrup and reduces the viscosity and syrup assists the
crystallization process.

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 In the manufacture of sugar PH is the main rote to controlling the process.
Maintaining PH is an important one because the acidity and basicity of the sugar
juices are removed and they are converted in to neutral PH range of 7.0.

In the sugar industry the mixed juice having the PH range of 4.5 to 5.3. In
order to convert the neutral PH of 7.0.

The mixed juice is acidic in nature. In acidic condition the inversion of

sucrose is possibility is more. So we raise the PH from 5.2 to 7.0 by adding milk of
lime and So2 gas to remove the impurities from mixed juice to clear juice and
finally we get the 7.0 PH of clear juice for the single sulphitation process.

The clear juice is concentrated to syrup by using evaporator. That is called

syrup.

The syrup emerged out from the last body of the evaporator will be dark in
colour and viscous.

The So2 gas is passed through syrup. The PH is maintained at about 4.9 to
5.1 which is analyzed once in hour.

There fore the rote of PH and double sulphitation techniques are very very
important to each other in good quality white sugar manufacturing process.

Though a great many experiments on lab and semi technical scale and a 14
day trial on full factory scale, in the year 1936 – 1940 developed the double

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sulphitation process. The name for this process was chosen in confinity with the
double carbonation method. Briefly, the double sulphitation is as follows.

The process starts with a treatment of the mixed juice by a single

sulphtation. Then the sulphited juice is gradually alkalized with lime to about PH
10.5, this being performed in 10 minutes. Separation of the formed sediment from
the clear juice is now carried out by filtration of the whole alkalize juice, at about
65°C sulphitation of alkalize filtrate to neutral reaction and a second filtration
follows, the second filtrate being the thin juice.

Compared with single sulphitation, the double method removes more non
sugars, colouring substances, SiO2 and MgO2 are affected; these are almost
insoluble in the highly alkaline medium during the first filtration, but mostly
dissolve in the single alkaline sulphitation process by the subsequent
neutralization.

The aforementioned full scale factory trial with double sulphitation resulted
white sugars with 30 – 40 % better, extinction coefficients and improved reflection
values of white sugars. Hence the quality of these sugar came near to that of
carbonation sugars. Lime and Sulphur quantities consumed were about 80 %
higher than usual.

Hence we discuss the, “role of PH and double sulphitation technique used in

sugar industry” briefly in the following titles.

RESULTS AND DISCUSSION:

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 Sugar industry is an agro-based industry. In sugar industry while sugar can
be produced by various process like defecation, double sulphitation, double
carbonization, phosphors-sulphitation and iron exchange process.

PH
The term PH denotes the hydrogen ion concentration. In other words it is
the logarithm of concentration of hydrogen ion reciprocal.
Ie.
PH=log 10 1/H+ (or)-Log 10(H+)
In every aqueous solution the product of the concentration of hydrogen ions
(H+) and hydroxyl ion (OH-) is a constant at constant temperature. This product is
equal to CO-14 at 22C. In pure water as well as in neutral solution the
concentration of (H+) and (COH) being equal to CO7. The value of such solution
will thus be
PH= -log CO-7=7.0
The solutions of PH values below 7.0 are acidic and solutions with PH
values above 7.0 are alkaline. The entire PH range is thus from 0 to 14, the limit of
acidity being represented by PH=0 and the limit of alkalinity being represented by
PH=14

1.The mixed juice and clear juice are analyzed by Bromothymal blue paper and PH
meter.
In Bromothymal blue paper the mixed juice PH = 5.0
In Bromothymal blue paper the clear juice PH = 7.0

And

25
 In PH meter the mixed juice PH = 5.12
In PH meter the clear juice PH = 6.95.

The PH analyzing methods the Bromothymal blue paper methods is used by

unskilled persons. The are not knowing anything. So the paper colour change in the
juice, they are maintained PH.

The PH meter method is used in the laboratory. In laboratory, juices condensate

waters, and spraypond waters and Boiler feed water and syrup PH are analyzed.
This method of analyzing we get accurate result so we are analyzed by PH meter.

The mixed juice having the PH = 5.0 this is acidic PH. In the acidic medium
there is inversion takes place. So to avoid this to raise the PH, we are adding cheap
alkaline medium of milk of lime. From the mixed juice PH how much quality of
milk of lime is added is observed.

The clear juice PH is 7.0. The clear juice PH is cheeked once in hour by PH
meter. Because we are maintaining the clear juice PH of neutral, ie 7.0. The PH is
below or above the neutral PH of 7.0, there is inversion takes place.

If inversion takes place, sugar loss will be more in processing.

Table : 1

PH 5.5.06 5.5.06 6.5.06 6.5.06 8.5.06 8.5.06

Primary Juice 5.27 5.32 5.29 5.31 5.35 5.28
Mixed Juice 4.98 4.80 4.83 4.92 4.87 4.97
Sulphured juice 7.36 7.25 7.18 7.31 7.35 7.26

26
Clear Juice 7.08 6.93 6.85 7.02 6.97 7.01
Unsulphured syrup 6.5 6.62 6.68 6.53 6.55 6.70
Sulphured juice 4.86 4.73 4.62 4.65 4.75 4.87
Sugar PH 6.4 6.31 6.40 6.32 6.39 6.43
ICUMSA Values 75 70 82 78 79 85
Spray Pond PH
Inlet 7.0 7.03 7.12 7.11 7.09 7.05
Outlet 7.2 7.12 7.24 7.29 7.11 7.26

SK1 8.74 8.53 8.32 8.42 8.56 8.76

SK2 8.25 8.32 8.22 8.35 8.26 8.24

Condensate water PH
Evaparator 8.3 8.28 8.25 8.29 8.20 8.26

Pan-1 8.79 8.42 8.15 8.23 8.5 8.25

Pan-2 8.78 8.40 8.04 8.20 8.33 8.23

Pan-3 8.76 8.01 8.09 8.15 8.31 8.22

Pan-4 8.74 8.32 8.12 8.12 8.27 8.19

Pan-5 8.73 8.36 8.20 8.09 8.25 8.16

Pan-6 8.54 8.35 8.22 8.05 8.20 8.14

Pan-7 7.95 8.27 8.25 8.01 8.13 8.10

ETP
Inlet 5.5 5.60 5.63 5.69 5.70 5.49

Outlet 7.5 7.62 7.53 7.69 7.73 7.52

Table : 2
PH 9.5.06 10.5.06 11.5.06 12.5.06 13.5.06 15.5.06
Primary Juice 5.34 5.20 5.22 5.40 5.12 5.43
Mixed Juice 4.85 4.90 5.02 4.95 4.84 5.06
Sulphured juice 7.20 7.33 7.35 7.29 7.29 7.42
Clear Juice 7.05 7.12 7.15 7.08 6.93 6.82
Unsulphured syrup 6.64 6.79 6.59 6.65 6.71 6.73
Sulphured juice 4.65 4.89 4.91 4.75 7.83 4.69
Sugar PH 6.49 6.39 6.50 6.35 6.44 6.5
ICUMSA Values 87 74 90 76 83 92

27
Spray Pond PH
Inlet 7.1 7.04 7.01 7.05 7.13 7.26

Outlet 7.2 7.29 7.31 7.28 7.23 7.31

SK1 8.8 8.66 8.82 8.69 8.76 8.59

SK2 8.3 8.43 8.36 8.35 8.23 8.5

Condensate water PH
Evaparator 8.25 8.12 8.23 8.26 8.31 8.36

Pan-1 8.03 8.11 8.22 8.25 8.30 8.29

Pan-2 8.02 8.09 8.19 8.22 8.38 8.28

Pan-3 8.06 8.07 8.13 8.19 8.26 8.27

Pan-4 8.01 8.04 8.11 8.17 8.23 8.25

Pan-5 7.98 8.01 8.09 8.15 8.19 8.23

Pan-6 7.96 7.98 8.07 8.11 8.17 8.20

Pan-7 7.95 7.96 8.05 8.09 8.15 8.19

ETP
Inlet 5.46 5.62 5.53 5.52 5.5 5.6

Outlet 7.85 7.75 7.68 7.53 7.76 7.8

Table : 3
PH 16.5.06 17.5.06 18.5.06 19.5.06 20.5.06
Primary Juice 5.23 5.31 5.25 5.36 5.25
Mixed Juice 4.82 4.91 4.93 4.82 4.79
Sulphured juice 7.39 7.26 7.30 7.31 7.35
Clear Juice 7.09 6.93 7.14 7.18 7.08
Unsulphured syrup 6.78 6.80 6.65 6.5 6.62
Sulphured juice 4.93 4.82 4.72 4.87 4.75
Sugar PH 6.45 6.50 6.42 6.47 6.32
ICUMSA Values 93 95 92 96 89
Spray Pond PH
Inlet 7.15 7.06 7.18 7.11 7.07
Outlet 7.25 7.18 7.26 7.3 7.15

28
SK1 8.8 8.75 8.61 8.75 8.82
SK2 8.42 8.33 8.25 8.32 8.21
Condensate water PH
Evaparator 8.29 8.31 8.27 8.30 8.28
Pan-1 8.23 8.00 8.12 8.28 8.78

Pan-2 8.21 7.98 8.11 8.25 8.76

Pan-3 8.19 7.97 8.08 8.20 8.74

Pan-4 8.18 7.95 8.05 8.18 8.72

Pan-5 8.17 7.94 8.03 8.17 8.69

Pan-6 8.13 7.92 8.00 8.15 8.65

Pan-7 8.10 7.89 7.98 8.11 8.60

ETP
Inlet 5.7 5.52 5.49 5.55 5.63

Outlet 7.79 7.91 7.62 7.68 7.79

Out of this various intermediate products and condensate waters are

analyzed by PH meter.

1. Primary juice: PH : 5.27 to 5.35.

This indicates the cane quality entering the mills.

2. Mixed juice: PH : 4.87 to 4.98.

This result indicates the juice quality entering in the clarification process.

3. Sulphured Juice: PH : 7.25 to 7.36.

29
 It indicates the quantity of adding Milk of lime in the juice.

4. Clear juice: PH : 6.85 to 6.70.

This result indicates juice clarity we are maintaining the PH : 7.0.

5. Unsulphured syrup : PH : 6.50 to 6.70.

This result indicates how much quantity to So 2 gas adding in unsulphured

syrup.

6. Sulphured syrup : PH : 4.62 to 4.87.

This result indicates the syrup sulphitation. PH is maintained 4.5 to 5.0 very
good.

7. Sugar PH: and ICUMSA

ICUMSA value indicates the quality of sugar. The ICUMSA value is below
100 is very good and the actual sugar solution PH is 6.3 to 6.5.

8. Spray PH:

The spray inlet, outlet PH is checked every two hours. It will maintained
neutral PH of 7.0. It is going to low PH corrosion takes place in spray pond pipe
limes. The water going higher PH is above 7.0 erosion takes place. So we are
maintained 7.0 PH.
30
Condensate waters

Semikestner Ist body of evaporator, and pan condensates are checked the PH
once in hour. Because these water is used for boiler feed. It should not come below
7.0 PH. It will maintained always above 7.0. This water going low PH if the sugar
take will be come. This water is not used for Boiler feed.

EXPERIMENT RESULT
Purity of M.J 80.18
Moisture % of filter cake 71 %
PH range 6.9
Phosphate content 325 PPM
Calcium oxide in M.J 900PPM
Cao in C.J 1280PPM
Lime 79.64

CaO

Our Result

CaO content in mixed juice = 900 ppm

CaO content in clear juice = 1280 ppm.

31
 The above result is better complimented by CaO content of lime. The
difference is maintained at 400 ppm between the Raw Juice (900 – 950 ppm) and
clear juice (1300 – 1350 ppm).

Lime is the most commonly used material in clarifying cane juice and is
effective in removing insoluble colouring compounds. It is only slightly soluble in
water but sucrose greatly increases its solubility.

Usually only sufficient lime is added to neutralize the organic acids

originally contained in the cane juice. In addition to other non sugar materials such
as waxes and gums, the insoluble coloured compounds, some in combination with
the calcium, are precipitated and subsequently removed. The method of
clarification has a considerable effect on the amount of soluble lime salts
remaining in the clarified juice.

Excessive lime addition must be avoided to minimize color formation and

prevent poor quality dark colored sugars.

Whatever process of juice clarification is followed, lime is the main

clarification agent.

The quality of purchased sample of lime must be very good precipitation and
coagulation reaction in juice are caused due to the reaction between clarifying
agents of So2 and milk of lime.

It has been mentioned that cane juice has many substances, both organic and
inorganic, we tend to increase the solubility of calcium compounds. It is not
32
surprising, therefore, that the calcium in juice becomes greater in lime clarification.
The amount of calcium in raw juice is highly variable, but the increase is
independent of the initial content. The average change of CaO with PH of clarified
juice . It indicates an increasing in CaO content with higher PH.

The fact that the original calcium in the juice is not precipitated during
clarification, by pointing out that the calcium ion conceutration is less important in
the phosphate precipitation than is the PH effect due to ionization of phosphoric
acid. When lime is added the calcium content of the juice increases by essentially
the same amount as if the initial calcium concentration had been zero. The
important factor remains, however, that the Ca ion activity in cane juice is low, due
to the presence of several calcium regulators. Hence, an increased amount is
necessary to produce the same equilibrium concentration in an ionic reaction, such
as the precipitation of calcium phosphate.

4. Phosphate content in mixed juice & clear juice

By uranium acetate method

The phosphate content of mixed juice

Before addition of phosphoric acid = 275 ppm

After addition of phosphoric acid = 325 ppm

The Phosphate content in clear juice.

33
 Before addition of phosphoric acid = 75 ppm

After addition of phosphoric acid = 100 ppm

The amount of P2O5 present in mixed juice to be subjected to the purification

process is other greatest practical significance for the clarification of cane juice.
The P2O5 reacts with the added lime to form insoluble calcium phosphate, which
appear to be the main purifying agents in connection with the removal of other non
sugars. The composition of the precipitate formed can not be represented by a
simple formula. It consists of a mixture of di-calcium phosphate and tri-calcium
phosphate respectively.

The application of phosphoric acid as a clarifying agent in the sugar industry

is one of the oldest techniques for the improvement of clarification by lime.

The unsatisfactory results in clarification of cane juices have been explained

by an insufficient amount of P2O5 per litre of juice. Experimental studies in Java,
Hawaii, British, West Indies and Cuba demonstrated that juices with a P2O5
content higher than 300 to 350 mg per litre did not as a rule cause particular
difficulties in obtaining well clarified juice and satisfactory settling.

With lower P2O5 content in juices it has been found that the extra addition of
P2O5 as a soluble phosphate to the juice to a level of 300 mg P 2O5 per litre is able
to solve clarification problems.

Phosphate containg compounds have a great significance in cane sugar

manufacture. The results of the clarification of juices with lime depends to a great
34
extent on the amount of P2O5 present in raw juice. The largest part of the P 2O5
present in mixed juice is precipitated in liming of the juice and is removed as
insoluble calcium phosphate.

In the determination of the phosphate content of clarified juice it has been

found that usually the amount of organic phosphate present is of the same
magnitude as the amounts to be determined by a direct calorimetric method in the
juices. The phosphates have the tendency to precipitate during the concentration of
the juices. This causes a relative increase in phosphates, found in the manufactured
sugars, compared to the amount of phosphate in clarified juice or phosphate
present in the molasses.

Syrup sulphitation

This is a product resulting from the concentration of purified juice via

evaporation of the excess of water in multiple evaporator effects. The syrup can be
sulphured syrup, when a small amount of So2 gas is added to evaporator syrup.

The sulphured syrup PH is being maintained at about 4.8 to 5.0. The So 2 gas
has a bleaching action on syrup and sulphitation of syrup assists the crystallization
process.

35
MATERIALS AND METHODS

1.EXPERIMENTAL PROCEDURES FOR PH ANALYSIS

Experiment No: 1

OBJECT:
To determine the PH of the given sample by;
1. Test Paper 2. PH meter
PROCEDURE:
1.TEST PAPER:
Dip the test paper in the liquid whose PH is to be tested when the paper
change colour according to the PH the shade of this colour is matched with graded
tints on a standard shade card and the corresponding PH found.
Ex: PH found of mix juice by PH paper : 5.0
PH of clear juice by PH paper : 7.0
2.PH METER:
First standardize the PH meter as following note the temperature of the
standard buffer solution and set the temperature control to the corresponding
setting. Dip the electrode is the standard buffer solution and set the function
switch etc proper PH ranges check that the PH of the buffer solution is indicated
correctly on the display. If the reading is not correct then adjust the zero control
switch. When the instrument is standardized remove the electrodes in distilled
water and dry it. Dip the dried electrodes into the liquid whose PH is to be
determined. Set the function switch. To proper PH range. Allow time for the
reaching to stablise. Read the PH directly from the display. (Note-Buffer
standardization and all subsequent PH measurements are to be made with solutions
at the same temperature)

36
 STANDARDISATION PROCEDURE FOR CONTROL CLYNAMIC PH
METER:
1. Press power ON/OFF switch at the rear to ON position.
2. Connect glass and reference electrode to appropriate terminal at the rear.
3. Set the temp compensation knob to the temperature of solution ‘or’
connect the pt. 100 to the rear terminal and press the MAN ‘T’/AUTO
‘T’ switch to auto T position.
4. Place electrodes in buffer ‘T’.
5. Press “Stand by/Read switch to Read” to stand by.
6. Adjust ASM control knob to read ‘7’ PH in the display.
7. Bring the S and by/Read switch back to stand by.
8. Remove the electrode from buffer ‘7’ wash the electrodes and place them
in buffer 4 or buffer 9.2 and repeat the above procedure. Adjust SLP
control knob to read 4 PH or 9.2PH in the display.
9. Check back buffer ‘7’ 4.0 and 9.2 adjust if necessary.
10. Now your instrument ready for measurement.

Ex: PH of Mixed Juice tested by PH meter - 5.12

PH of Clear Juice tested by PH meter - 6.95
Experiment No: 2
Object :
To determine the PH of the given sample
By

1. Test paper
2. pH meter

37
Procedure:
1.The test paper was dipped in the liquid whose PH is to be tested. The paper
colour changed according to the PH. The shade of this colour was matched with
graded tints on a standard shade card and the corresponding PH was found.
The PH meter was first standardized at the temperature of the standard
buffer solution and the temperature control was set to the corresponding setting.
The electrodes was dipped in the standard buffer solution and the function switch
was set to proper pH as on the display After the instrument was standardized. The
electrode was removed and rinsed in distilled water and dried. The dried electrode
was dipped in the solution of unknown PH. The PH was read directly from the
display.
Result :
The pH of the given sample
1.Bromo thymal blue paper method PH = 6.9
2. PH meter PH = 6.89

38
Experiment No:3
Analysis of PH in mixed juice and clear juice.
Object:
To determine the PH of mixed juice and clear juice.
a. Reagents Required:
Distilled water
b. Apparatus Required:
PH meter
Beaker
Procedure:
50 ml of mixed juice and 50 ml of clear juice taken in individual beaker.
Now we check the PH by a PH meter.

Result:
1. PH of mixed juice : 5.01
2. PH of clear juice : 6.98

39
2.Experimental Procedure for Juice sulphitation process
EXPERIMENT NO.1
Object
To determine Cao content in the Mixed Juice by EDTA method.

a.Reagents Required:
M/56 EDTA solution (6.6473 g bi sodium salt of ethylene
diamineterracetic acid was weighed accurately, dissolved in distilled water
and made up the solution to 1000ml.
Ammonia of C.P.quality
Lead sub acetate : Horne’s dry lead
Potassium Ferro cyanide (Merck quality) powder
Erichrome Black T (weight 0.1g of Erichrome Black T in 100ml of rectified spirit
or absolute alcotol)

b. Apparatus Required:
Calibrated Brix spindle
Brix cylinder
Conical flasks of 250 ml
Funnels
Calibrated 10 ml. Pipette
Procedure
Take the juice syrup or molasses samples as obtained from the factory. In
case of juices no dilution is required. In case of molasses dilute to 5° Bx
Transfer about 150ml of the juice or diluted solution into a conical flask.
Clarify the solution by lead sub acetate, as in Horne’s method (Add if necessary
some amount of active carbon)
40
 Transfer about 60ml of the clarified solution into a dry conical flask or flask
previously rinsed with the clarified solution, Add powdered potassium Ferro
cyanide little by little till not further precipitate forms. Shake thoroughly and
filter Test the filtrate for absence of lead with potassium iodide Collect the lead
free filtrate in a conical flask. Pipette out 10ml of this filtrate in to a clean
conical flask previously rinsed with distilled water and dried. Add 5 drops of
ammonia – (indicator) solution when a pink red colour appears. Titrate against
EDTA
Solution shaking the contents of the flask after every additional of EDTA
solution The end point is indicated by the sharp change of colour from red to
blue. Note the volume of the titrant.

Mixed Juice
Titration reading =Vml = 9.0ml
Cao in Mixed Juice = 9.0X100=900 PPM

41
Experiment No:2

Object
To determine the phosphate content in the Mixed Juice by
Uranium Acetate method
a. Uranium Acetate Method:
About 35g of chemically pure uranium acetate was dissolved in distilled
water 50ml glacial acetic acid was added to it and the solution made up to one liter
b. Standardization of uranium solution
9.583g of chemically pure mono basic potassium phosphate (KH 2PO4) was
dissolved in one liter of water 25 ml of this solution was added from a burette to
the cold phosphate solution till a few drops with drawn with a pipette give a brown
precipitation with a drop reaction plate dusted with potassium Ferro cyanide. It is
heated between 90 deg C and 100 deg C and again added the uranium solution
until a brown precipitate of uranium Ferro cyanide appears.
When a 100g sample is titrated (100ml juice is usually taken as 100g) each
milliliter of the uranium solution is equivalent to 0.005 percent of P2O5.
c. Procedure for Analysis:
100ml of juice is taken and added one milliliter of 10% ammonium
hydroxide solution and acidified with 50 ml glacial acetic acid per litter of
distilled water. It is titrated against standard uranium solution and potassium
Ferro cyanide as an indicator and added a small portion of clear liquid from the
drop pipette for the determination of end point. Nearly the whole of the uranium
solution should be added in the cold and the titration finished at 90°-100°C
When the solution contains the slightest excess of uranium the addition of a.
drop of solution to the Ferro cyanide the drop reaction plate produces a brown
precipitate of uranium Ferro cyanide.
42
Calculation
Before addition

Titration Reading = 5.5 ml

1ml of uranium acetate solution = 0.005g of P2O5
5.5 ml of uranium acetate solution =0.005X5.5
100 ml of juice =10X0.005X5.5X1000gms. of P2O5

= 275
Calculation
After addition

Titration Reading = 6.5 ml

1ml of uranium acetate solution = 0.005g of P2O5
6.5 ml of uranium acetate solution =0.005X6.5
100 ml of juice =10X0.005X6.5X1000gms. of P2O5
=325

43
Experiment No:3

Object
To determine Cao content in the Clear Juice by EDTA method.

a. Reagents Required:
M/56 EDTA solution (6.6473 g bi sodium salt of ethylene
diamineterracetic acid was weighed accurately, dissolved in distilled water
and made up the solution to 1000ml.
Ammonia of C.P.quality
Lead sub acetate : Horne’s dry lead
Potassium Ferro cyanide (Merck quality) powder
Erichrome Black T (weight 0.1g of Erichrome Black T in 100ml of rectified spirit
or absolute alcotol)

b. Apparatus Required:
Calibrated Brix spindle
Brix cylinder
Conical flasks of 250 ml
Funnels
Calibrated 10 ml. Pipette
Procedure
Take the juice syrup or molasses samples as obtained from the factory. In
case of juices no dilution is required. In case of molasses dilute to 5° Bx
Transfer about 150ml of the juice or diluted solution into a conical flask.
Clarify the solution by lead sub acetate, as in Horne’s method (Add if necessary
some amount of active carbon)
44
 Transfer about 60ml of the clarified solution into a dry conical flask or flask
previously rinsed with the clarified solution, Add powdered potassium Ferro
cyanide little by little till not further precipitate forms. Shake thoroughly and
filter Test the filtrate for absence of lead with potassium iodide Collect the lead
free filtrate in a conical flask. Pipette out 10ml of this filtrate in to a clean
conical flask previously rinsed with distilled water and dried. Add 5 drops of
ammonia – (indicator) solution when a pink red colour appears. Titrate against
EDTA.

Solution shaking the contents of the flask after every additional of EDTA
solution The end point is indicated by the sharp change of colour from red to
blue. Note the volume of the titrant.

Clear Juice
Titration reading = 12.8ml
Cao in Clear Juice =1280 (12.8X100)

45
Experiment No:4

Object
To determine the phosphate content in the clear juice by
Uranium Acetate method
a. Uranium Acetate Method:
About 35g of chemically pure uranium acetate was dissolved in distilled
water 50ml glacial acetic acid was added to it and the solution made up to one liter
b. Standardization of uranium solution
9.583g of chemically pure mono basic potassium phosphate (KH 2PO4) was
dissolved in one liter of water 25 ml of this solution was added from a burette to
the cold phosphate solution till a few drops with drawn with a pipette give a brown
precipitation with a drop reaction plate dusted with potassium Ferro cyanide. It is
heated between 90 deg C and 100 deg C and again added the uranium solution
until a brown precipitate of uranium Ferro cyanide appears.
When a 100g sample is titrated (100ml juice is usually taken as 100g) each
milliliter of the uranium solution is equivalent to 0.005 percent of P2O5.
c. Procedure for Analysis:
100ml of juice is taken and added one milliliter of 10% ammonium
hydroxide solution and acidified with 50 ml glacial acetic acid per litter of
distilled water. It is titrated against standard uranium solution and potassium
Ferro cyanide as an indicator and added a small portion of clear liquid from the
drop pipette for the determination of end point. Nearly the whole of the uranium
solution should be added in the cold and the titration finished at 90°-100°C
When the solution contains the slightest excess of uranium the addition of a.
drop of solution to the Ferro cyanide the drop reaction plate produces a brown
precipitate of uranium Ferro cyanide.
46
Calculation
Before addition
Titration Reading = 1.5 ml
1ml of uranium acetate solution = 0.005g of P2O5
1.5 ml of uranium acetate solution =0.005X1.5
100 ml of juice =10X0.005X1.5X1000gms. of P2O5

=75 PPM
After addition
Titration Reading = 2.0 ml
1ml of uranium acetate solution = 0.005g of P2O5
2.0 ml of uranium acetate solution =0.005X2.0
100 ml of juice =10X0.005X2.0X1000gms. of P2O5

=100 PPM

47
3. Experimental procedure for syrup sulphitation process
Experiment No:1
a. Unsulphured syrup analysis:
Object
To determine the PH, Brix and purity of unsulphured syrup.

Reagents Required:
Leadsubecetate
Distilled water
Apparatus Required:
PH meter
Polarimeter
Brix hydrometer
Procedure:
The unsulphered syrup is taken from sampling devices. From this 50 ml
syrup is taken in a beaker and analysis of PH by PH meter.
About 300 ml of unsulphered syrup is weighing and 600ml of water is added and
dissolved and pol in a Brik cylinder. Then 150 ml of this solution clarified by
leadsubacetate powder. This solution is used for polarization by using polarimeter.
Brix hydrometer is used to determine the Brix of the solution.

48
Result:
PH of the unsulphered syrup = 6.5
Observed Brix Reading = 18.0
Temperature = 30°
Brix = 18.18
Pol Reading = 59.9
Pol % = 14.57
Purity = 80.14
Corrected Brix = 54.54
Corrected Pol % = 43.71
Corrected Purity = 80.14

49
Experiment No:2

b Sulphured syrup analysis:

Object
To determine the PH, Brix and purity of Sulphured syrup.

Reagents Required:
Leadsubecetate
Distilled water
Apparatus Required:
PH meter
Polarimeter
Brix hydrometer
Procedure:
The Sulphered syrup is taken from sampling devices. From this 50 ml syrup
is taken in a beaker and analysis of PH by PH meter.
About 300 ml of Sulphered syrup is weighing and 600ml of water is added and
dissolved and pol in a Brik cylinder. Then 150 ml of this solution clarified by
leadsubacetate powder. This solution is used for polarization by using polarimeter.
Brix hydrometer is used to determine the Brix of the solution.

50
Result:
PH of the Sulphered syrup = 4.8
Observed Brix Reading = 17.9
Temperature = 30°
Brix = 18.08
Pol Reading = 59.4
Pol % = 14.45
Purity = 79.92
Corrected Brix = 54.24
Corrected Pol % = 43.35
Corrected Purity = 79.92

51
Conclusion:
We are discussed about the cane juice clarification process and control of
PH in the treatment of cane juice.

To produce brilliant white good quality sugar we concentrated the following

in the cane juice clarification and PH control in Juice.

1. Purchase of good quality lime, Sulphur and phosphoric acid.

2. Maintain sulphured juice PH 7.2 to 7.4.
3. Maintain clear juice PH 6.9 to 7.0.
4. Raw Juice temp is 65ºC and treated juice temp is 105ºC.
5. Retention time in the juice sulphitor is 8 minutes.
6. The difference between mixed juice and clear juice is 400 for CaO.
7. The phosphate content in juices are maintained as allowed limit as discussed
above.
8. The sulphured syrup PH is 4.8 to 5.0.

In clarification section the above mentioned parameters are maintation in

process we are produce good quality low ICUMSA brilliant white sugar.

52
BIBHIOGRAPHY

1. K Onna & Tamays’Proc. Hawaiin Sugar Technogists

Association’1979…..P.141143
2. SJ. Marches ‘Principles of Sugar Technology’ by P.Honig vol.p.584.
1. J. Marches ‘Principles of Sugar Technology’ by P.Honig P.607.
2. C.F.Marches ‘Principles of Sugar Technology’ by P.Honig P.608.
3. C.F.K. Douwes dekker ‘Principles of Sugar Technology’
Vol.I.P.397.
4. J.G.Davies ‘Principles of Sugar Technology’ Vol.I.P.541.
5. J.Marches ‘Principles of Sugar Technology’ Vol.I.P.618-620.
J.Marches ‘Proc.ISSCT’ 1956…p.582.
6. B.H.Hoshing & N.G.Patel ‘Proc. Deccan Sugar Technologists
Association’ 1967….p.191.
7. K.Douwes Kekker ‘Principles of Sugar Technology’ by Honig……
p.363.
8. A.C.Raha, RB Nigam A.K.Agarwal & P.Sanyal, ‘Proc, Sugar Tech.
Association of India’ 1975…p.23-28.
Also private communication, work at Phaltan Sugar Wks.
Sakharwadi Maharashtra.
9. J.Marches ‘Principles of Sugar Technology’ Vol.I…p.592.
10. G.K.Limaye ‘Proc. Deccan Sugar Tech. Association India’ 1967
M23-M32.
11. J.Marches ‘Principles of Sugar Technology’ by P.Honig Vol.I…
p.625.
12. B.B.Bandi ‘Proc. Deccan Sugar Tech. Association’ 1959….p.63-64.
13. S.N.Gundu Rao, P.V.S.Sastry & M.R.Bhalerao ‘Proc. ISSCT’ 1956
India, p.209.
14. D.P.Kulkarni, J.R.Unde ‘Proc. Sugar Tech. Association of India’
1973…P.M.115.
15. D.P.KULKARNI, M.K.Patil & K.C.Vora, ‘I.S.J.’ 1967 p.297-301.
16. N.P.Randhwa ‘Proc. Sugar Tech. Association of India’ 1980 p.m.
109-112.
17. G.N.Acharya 1981 ‘Proc D.S.T.A. Central Electronics Engg.
Research Institute, Pilani. PE.51.
also A.P.Chinnaswamy, K.Thurthmalai, S.Vishwanathan, ‘Proc
ISSCT’ XX Congress Brazil 1988.
also G.N. Acharya Bhartiya Sugar August 1988 p.9-39.
Also Laxmi Narayan KSN Rao, K.Srinivasan & G.N. Acharya ‘Proc
Seminar’ on ‘Juice Clarification practices followed in India with

53
 reference to design and control system’ organized by DSI & CEERI
at Pune on 11-12-1987.
18. O.P.Tripathi ‘Proc. Sugar Tech. Association of India’ 1981 .p E33.
19. S.K.D.Agarwal ‘Proc. Sugar Tech. Association of India’
1962….p.100.
20. S.C.Sharma ‘Proc. Sugar Technologists Association of India’
1980.P.M.73.
21. S.C.Sharma, ‘Proc. ISSCT’ 1980.P.2137,2143.
22. N.A.Ramaiah, S.K.D.Agarwal, P.C.Johery & L.P.Tiwari, ‘Proc.
Sugar Tech Association of India’ 1975. p.M1-M6.
23. D.P.Kulkarni, M.K.Patil ‘Proc. DSTA’ India 1965 p.119.
24. S.C.Gupta, N.A.Ramaiah ‘Proc. DSTA’ India 1965.p.119.
25. D.P.Kulkarni, J.R.Unde, ‘Proc STA’ India 1974 p.m.70.
26. J.M.Saba & N.S.Jain ‘Proc. STA’ India 1956.
27. D.P.Kulkarni ‘Proc. DSTA’ India 1967 p.147-160.
28. cf Chen & Meade ‘Cane Sugar Handbook’ 10th edition p.183.
29. Dubey R.S., Mavi S.S., c.f.’Proc. ISSCT’ 1956 p.408.
Experimental work at ‘Phaltan Sugar Works Ltd.’ Sakharwadi Dist.
Satara. India.
30. S.C.Gupta, N.A.Ramaiah, S.K.D.Agarwal, R.P.Shukla, K.K.Mathur
‘Proc. Sugar Technologists’ Association of India’ Kanpur 1972
p.M99-M129.
31. S.C.Sharma & Mahesh Narain ‘Proc. Sugar Technologists’
Association of India’ Kanpur 1972 p.M19-M23.
32. N.O.Schmidt ‘Proc. ISSCT’ India 1956 p.612.
33. Other references—
(i) ‘Seminar’ on Preparation of Lime solution-Sulphur dioxide
and Phosphate in cane juice clarification held in Pune on
26-4-81by ‘Deccan Sugar Technologists Association’ (I)
Pune.
(ii) ‘Inorganic Chemistry’ by Partington.
(iii) Outlines of ‘Chemical Technology’ by Dryden.
(iv) ‘General Chemistry’ by W.E.Miller & J.A.Barker.
(v) ‘Machinery & equipment for Cane Sugar Factory’ by
L.A.Tromp 1946 Edition.
(vi) ‘Handbook of Cane Sugar Engineering’ by E Hugot &
Jenkina 1971 Ed.
(vii) ‘Cane Sugar’ by Noel Deerr 1921 Ed.
34. Van Ginneken and Aten c.f.Principles of Sugar Technology Ed.
P.Honig Part I 1953.p.672.
54
35. T.Y.Chou Ibid p.711-724.
36. S.L.Sang, Z.H.Hsu & H.T.Cheng Proc.I.S.S.C.T. XIV Congress
1971 p.1560-1563.
37. P.Honig Principles of Sugar Technology Part I 1853p.655-710.
38. c.f.E.Hugot Handbook of Cane Sugar Engineering 2nd
Ed.1972.p.417.
39. S.L.Sang. C.H.Chen & J.F.Tong Proc. Sugar Tech. Assn. India
1975.p.M17-M21.
40. U.P.Singh & R.K.Gupta Proc. Sugar Tech. Assn. India 1971 p.M49-
M57.
41. N.K.Sawney Ibid p.M58-M65.
42. J.D.Taneja, R.N.Dass & R.P.Agarwal Proc. Sugar Tech. Assn. India
1965 p.61-67.
Also S.C.Sharma Proc. Sugar Tech. Assn. India 1971 p.M73-M98.
43. S.P.Mishra Proc. Sugar Tech. Assn. India 1979 p.M1-M9.
44. L.A.Tromp Machinery and Equipment of the Cane Sugar Factory
1946 p.342.
45. E.Hugot Handbook of Cane Sugar Engineering IIIEd. P.422.
46. P.Honig C.F.Ibid p.426.
47. Shaslikarth R miss sushakar P.Jiphe 1 (1995) 6.
48. R.B.C.Mathur Hand Book of sugar Technology.
49. Plater Honic – Principles of sugar Technology.

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