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Dairy Chemistry 2 PDF
Dairy Chemistry 2 PDF
Introduction
Cream is the fatty portion of milk which rises to the top of milk on quiescent storage and is rich in fat. It is
produced by separation of un-homogenized whole milk. The concentration of non-fat components (SNF) in
cream is in the proportion to the amount of non-fat components transferred from the original milk from
which cream is obtained. The indigenous product similar to cream is malai.
Legal Definition
According to Food Safety and Standards Regulations (FSSR) 2011, Cream including sterilized cream means
the product of cow or buffalo milk or a combination thereof. It shall be free from starch and other
1. Low fat cream-containing milk fat not less than 25.0 percent by weight.
2. Medium fat cream-containing milk fat not less than 40.0 percent by weight.
3. High fat cream-containing milk fat not less than 60.0 percent by weight.
Note:- Cream sold without any indication about milk fat content shall be treated as high fat cream.
Classification
The fat in cream varies from 18-85%. As the fat percentage in cream increase the components of milk in
cream gradually decreases. The SNF content constitutes lower proportions than present in milk. Broadly,
cream may be classified into two groups:
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Table cream
20-25% milk fat
Light cream
Coffee cream
30-45% milk fat
Whipping cream
Heavy cream
65-85% milk fat
Plastic cream
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or without coagulation
In general, the following types of cream are relevant to market and industrial purposes:
Table Cream: This type of cream contained 18 to 22% fat and used for eating directly. Various food
preparations are made from this cream as fruit cream etc.
Light Cream or Thin Cream: Fat percentage in this type of cream is about 20 to 25 and used for table
purpose and for manufacturing of cream cottage cheese etc.
Coffee Cream: This is light or thin type fresh cream containing 18 to 25 percent fat. It is used mostly in
coffee making. If this cream has any lactic acid, it becomes coagulated after adding to coffee. These
cream coagulates are known as “Cream feathers”. This feathering may be prevented by addition of
sodium citrate to this slight acidic cream. If the water which used in coffee making has more calcium,
accelerate the cream feathering. The addition of 0.05% sodium citrate also reduces the hardness and
thickness of cream plug in cream bottles.
Heavy Cream: This type of cream contains 30 to 40% fat and used in production of butter and ice
cream. Sometimes it can be used in paneer production.
Plastic Cream: The cream of 30-40% fat re-separated to obtain the cream of 80 per cent and this rich
cream is known as plastic cream. Mostly this type of cream is used for ghee production. This cream can
be produced directly from milk which is separated in an especially designed plastic cream separator.
Whipped Cream: When the normal cream (30-40% fat) is incorporated with air, the air bubbles are
stabilized by protein adsorption. The fat globules are assemble around these air bubbles. As whipping
continues, these air cells subdivided into smaller one each with adsorbed layer and in numerable fat
globules. At the maximum stiffness, these smaller air cells (nuclei) are surrounded by films of adsorbed
protein which is so thin that drainage is at a minimum and the structure of dry foam is set up. The
favorable temperature for whipping is 10Type equation here. C. Over whipping may produces a buttery
product. The cream pasteurization and sugar addition declines the whipping rate in cream. Some of the
dairy plants used Nitrous oxide gas for cream whipping. Whipped cream is used in cakes and ice cream
etc. for decorative purpose.
Sour Cream: This type of cream are produced by inoculating sweet, pasteurized and homogenized
cream with a starter culture containing lactic acid producing and aroma producing microorganism and
incubated to proceed fermentation. This cream has 0.6% lactic acid, clean flavour and smooth texture.
Sometimes rennet can be added @ 0.03 ml/gal cream to get more firm product. Sour cream should be
stored at 40 oF or less temperature to check the further increase in acidity.
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Clotted cream: To obtain the clotted cream, milk is scalded for fifteen minutes at about 85-90 oC in
shallow pan and allowed to form a cream layer. Considerable evaporation occurs from the cream layer
and on cooling over a period of twenty four hours, the clotted cream may be removed. The main
difference between ordinary cream and clotted cream are the decreased ratio of SNF/water and relatively
higher proportion of protein in the clotted cream.
Frozen Cream: Cream is frozen to improve its keeping quality. Pasteurize the ordinary cream (40-50%
fat) at 77 oC for 15 minutes and packing in paper, plastic or tin containers after cooling at 4 oC or below.
Freeze quickly this packaged cream and store at 12 oC or below. This stored cream is used during
shortage in preparation of ice-cream etc. During storage the fat globule membrane may ruptured by ice
crystals. Therefore, this cream tends to Oil-off on thawing. This Oiling-off impairs the whipping
characteristics of the ice cream.
Sterilized or Canned Cream: Homogenize the 20% cream at 80 oC using pressure 175 kg/cm2 in the
first stage and 35 kg/cm2 in the second stage and cooled to 16 oC immediately. Tri-sodium phosphate is
added @ 0.2% as a stabilizer to the cream. This cream is packaged in tin cans or bottles and sterilized in
following manner:
Reconstituted Cream: By vigorous emulsification of unsalted plain butter in milk or separated milk
or reconstituted milk or condensed milk, the fat globules are dispersed and coated with a layer of
adsorbed protein, the resulted product is closely resembles with cream and known are reconstituted
cream.
Synthetic Cream: In the artificial cream, butter fat is substituted with margarine fat and resulted
product is known as synthetic cream. Margarine is an imitation and substitute of butter. In production
of synthetic cream, the refined oils are carefully blended to have some physical cream, the refined
oils are carefully blended to have some physical properties resemble to butter fat. Synthetic cream
may have some emulsifying agents such as egg yolk, vegetable lecithin and glycerol- Mono or di-
stearated etc.
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Whey Cream: Separation is sometimes used to remove fat from cheese whey and resulted cream is
known as whey cream. It is slightly differs in composition from regular fresh cream obtained from
milk.
Composition of Cream
Cream generally contains all the constituents of milk but non-fat constituents are inversely proportional
to the fat content.
Composition of cream
SNF of cream can be calculated by taking the ratio of water to SNF of milk
If ratio of water to SNF of milk is 10:1, then the approximate SNF in cream = (100 - F/11) where F is fat
content of cream. SNF in cream can be estimated as:
Physico-Chemical Properties
Some of the important physico chemical properties relevant to cream processing and consumption are
discussed below:
Viscosity
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It is the resistance offered by the liquid to flow. Consumer judges the richness of cream by its viscosity. The
factors affecting the viscosity of cream are given below:
Clumping: It refers to the tendency of fat globules to adhere loosely to one another and form
clumps. Clumping depends on fat globule size, temperature (maximum at 7 oC), agitation and
method of separation. The greater is the clumping, greater will be the viscosity.
Whipping quality
Whipping means emulsion of gas or foam production by beating of cream. Whipped cream has remarkable
stability. This is used in cakes, ice creams and for decorative purposes. The most satisfactory fat content for
production of whipping cream is 30-35%. The optimum aging period is 24 hours at 4 oC . Homogenization,
acidity and stabilizers in cream reduces the whip-ability of cream.
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Specific gravity
Specific gravity of cream is inversely proportional to the fat percentage as shown below:
4.0 1.032
6.0 1.030
10.0 1.025
20.0 1.013
30.0 1.003
40.0 0.995
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CHEMISTRY OF CREAMING AND FACTORS AFFECTING THE SAME-I
Introduction
When milk is allowed to stand un-disturbed for some time, an upward motion of the fat globules
takes place, leading to the formation of a surface layer on milk in which the percentage of fat is
considerably increased. This upward motion of fat based on the fact that milk fat is lighter than
the skim milk portion. At 16°C, the average density of milk fat is 0.93 and of skim milk is
1.0404. Therefore when milk (a mixture of fat and skim milk) is subjected to either gravity or
centrifugal force, the two components, cream (fat-rich portion of milk) and skim milk (reduced-
fat portion of milk), by virtue of their differing densities, separate from each other.
The cream separation process has significant economic importance, as it controls the efficiency
of the fat separation. The key objective is to manufacture skim milk with the lowest possible fat
content, which corresponds to good separation efficiency. Knowledge of the basics of the fat
separation is important for an optimal de-creaming process. Cream separation is based on the
facts that fat exists in poly-disperse system in an emulsified state and that the specific density
difference between milk fat (p = 0.93 g/cm3) and skim milk (p = 1.035 g/cm3) is fairly large.
Basically two processes for fat separation are possible, natural de-creaming and separation with
machines. Natural creaming has no industrial significance.
Separation Processes
There are two methods of cream separation viz.,
· Gravity Method
· Centrifugal Method
Where,
However, in practice the factors affecting the rate of rise of fat in gravity method of separation
are:
Size of fat globules: As the size of fat globules increases, the rate at which fat rises also
increases. Larger fat globules rise faster than smaller ones. Thus, in buffalo milk gravity
creaming occurs faster due to the larger fat globules than those in cow milk.
Clumping: A clump or cluster acts like a single globule in so far as movement through
skim milk is concerned. Thereby the effective ‘r’ is increased, which in turn increases
velocity, as shown below
41.0 242
There are five various methods for separating the cream using gravity method:
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i. Shallow Pan Method: Milk is allowed to stand in a pan of 10 cm depth and 45-60 cm
diameter at 7°C for 24 h. During this time, cream rises to the surface.
ii. Deep Pan Method: Milk is allowed to stand in pan of 20” depth and 8 to 12” diameter at
10°C for 24 h. These tall cans have glass on one side of can and a faucet placed near the bottom.
Skim milk is drawn through the faucet.
iii. Water Dilution Method: Milk is diluted with water and allows standing for 12 h at 37.7°C
temperature. Water would make the milk less viscous, thus facilitating the rising of the fat
globules.
iv. Scalding Method: Heating and cooling of milk slowly causes the formation of cream layer
at surface of milk
v. Jersey Creamery Method: Milk is heated to 40°C using hot water in the jacketed vat and
then cool to 10°C using chilled water in place of hot water in the jacket of Vat. The cream will
be separated rapidly on cooling, immediately after heating the milk, by increasing the difference
in densities of milk fat and serum.
Gravity method being very slow, it is no longer used commercially for cream separation.
V = r2 *((as - df) / n) * N2 * R * K
Where,
df = density of fat
K = Constant
It will be seen from the above that the speed (rate) of cream separation is increased by:
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CHEMISTRY OF CREAMING AND FACTORS AFFECTING THE SAME-II
Introduction
Normally the objective of separation is to attempt to recover all the fat in the whole milk within the cream
fraction, with the minimum amount of fat being retained in the skim milk. Skimming efficiency is assessed
as the fat content of the skim milk. If the skim milk is to be converted into skim powder or casein then it is
important that the fat content be low, to meet various specifications and functional requirements of these
products.
The cream screw/outlet consists of a small, threaded, hollow screw pierced by a circular orifice through
which the cream emerges. This screw can be driven IN or OUT, thus bringing it nearer to, or away from, the
centre of rotation. Similarly, the skim milk screw/outlet is for the removal of skim milk. Once the cream
screw or skim milk screw has been adjusted, the cream separator delivers, under normal conditions, a
definite ratio of skim milk and cream, which is usually 90:10 (or 85:15) by volume. Basically, any change in
the separation procedures which alters the relative quantities of skim milk and cream will influence the fat
test of the cream. By altering the position of the cream screw (or skim milk screw), the ratio of skim milk to
cream changes. Thus, when the cream screw is moved IN towards the axis of rotation, a higher fat
percentage in cream is obtained, and vice versa; this is because the force tending to discharge cream through
the orifice is decreased ('R' in the formula F = KWRN2 is decreased),. A smaller proportion of cream is
therefore discharged, which, contains the same quantity of fat, resulting in a higher fat percentage. Screwing
OUT the cream screw produces thinner cream. Similarly, the skim milk screw OUT results in richer cream,
and vice versa.
The higher the fat percentage in milk, the higher the per cent fat in cream, and vice versa. Since practically
all the fat in milk is contained in the cream, the cream from the separation of high-fat milk has a higher fat
content than that from low-fat milk; a greater fat content in cream, the amount of which remains unaltered in
the two cases, will obviously show a higher fat percentage in it, and vice versa.
The higher the rate of milk inflow, the lower the fat percentage in cream, and vice versa. When the rate of
inflow increases, the discharge from the cream outlet increases. As the skim milk discharge remains constant
(with constant centrifugal force); more cream containing the same amount of fat results in a lower fat test,
and vice versa.
5.Temperature of milk
An increase in temperature of milk leads to both an increase in density difference between milk fat and
skim milk. So increase in temperature will lead to lower separation efficiency. Higher temperature will lead
to disruption of fat globule which will result in heavy fat losses in skim milk. The fat losses are higher at 70
O
C than at 54.5 OC. The optimum separation temperature is 40 OC. Higher temperature leads to protein
Cold milk separators that will operate at temperatures less than 10 OC are available. These allow separation
of milk as it is received at the factory, and although fat losses to skim milk are somewhat higher they do
sometimes allow substantial savings in energy and capital costs. In some cheese making operations heat
treatment of the milk is undesirable and cold milk separators offer some advantages. In addition cold milk
separators produce cream with greater phospholipids content which gives better whipping properties. The
major modification in a cold milk separator is wider disc spacing than in a conventional model to allow
adequate flow of the more viscous cold cream.
The greater the quantity of water or skim milk added to flush the bowl, the lower the fat percentage in
cream, and vice versa. The addition of more water or skim milk will cause an increase in the amount of
cream produced, which, with the same fat content, will show a lower fat test.
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Factors affecting fat losses in skim milk
The important factors influencing the fat losses in skim milk obtained through centrifugal separation are
discussed below:
1. Temperature of milk
The lower the temperature of milk, the higher the fat losses in skim milk and vice versa. For efficient
separation, the temperature of milk should be above the melting point of fat, so that the milk fat in the fat
globules is entirely in liquid form. A satisfactory temperature for separation is around 40 OC. The higher the
temperature, the more efficient is the separation. There is no marked increase in efficiency after 43-49 OC.
On the other hand, separation at low temperatures (in warm-milk separators) may lead to partial clogging of
the bowl due to high viscosity of cream at these temperatures, resulting in a greater fat loss in skim milk.
The lower the speed of the bowl, the higher the fat loss in skim milk, and vice-versa. At below-rated speed
there will be more fat loss in skim milk because insufficient centrifugal force is generated for efficient cream
separation. However, at above rated speeds, the skimming efficiency will not increase greatly.
The higher the rate of inflow of milk, the higher will be the fat losses in skim milk, and vice versa. If the
rate of inflow is increased above the designed capacity of the separator, the milk passes through the bowl too
rapidly and do not to allow for complete separation, thereby resulting in a higher fat loss in skim milk. On
the other hand, underfeeding the separator does not greatly increase the efficiency of the separation.
A good separator is designed to give efficient skimming within a fairly wide range of positions of the cream
screw, so that the fat test of the cream can be varied without influencing the efficiency of skimming. With
most separators, the position of the cream screw has little effect on the fat test of skim milk until the cream
test is above 45 to 50 per cent. From this point up to a 60 per cent fat test in cream, the fat content of the
skim milk increases. Separation of very thick cream at low temperatures may lead to higher losses due to
clogging of the bowl with viscous cream.
Vibration of separator: This reduces the efficiency of separation by disturbing the currents of cream
and skim milk. Vibration is caused by installation on an insufficiently firm foundation, the bowl being
out of balance, bearings being worn out, the axis of rotation not exactly vertical, etc.
Condition of the discs: Discs in an unsatisfactory condition suffer a loss of skimming efficiency due to
the uneven flow of the counter-current streams of cream and skim milk between them. An unsatisfactory
disc is one which is out of shape, dirty, scratched or rough.
If too much slime accumulates, the fat loss in skim milk increases; this is caused not only by a disturbance in
the even flow of the counter-currents of cream and skim milk, but by reduction in the centrifugal force
(because of decrease in the 'effective' diameter of the bowl).
Separator slime (which is usually considered identical with clarifier slime) consists of the slimy mass which
accumulates inside the bowl shell of the cream separator. It is made up of foreign matter, milk proteins,
leucocytes, fragments of the secreting cells from the udder, fat calcium-phosphate and other minerals,
bacteria and, occasionally, red blood corpuscles.
The greater the number of fat globules of less than 2 µm size, the higher the fat loss in skim milk and vice
versa. Fat globules of less than 2 µm size usually enter the skim milk, as they are not subject to sufficient
The higher the degree and temperature of agitation, the greater will be the loss of fat in skim milk and vice
versa. Agitation of hot milk causes the disintegration of normal fat globules in to smaller ones which escape
the effect of centrifugal force there by leading to more fat loss in skim milk.
The greater the amount of air in milk the higher the fat losses in skim milk. If the milk delivered to the
separator contains entrapped air bubbles, centrifugal force will disturb the counter-current streams of cream
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and skim milk between the discs, and lower the efficiency of separation. The effect of air in the milk is
greater with hermetic than with non-hermetic cream separators.
The higher the acidity of milk, the lower the efficiency of separation, the lower the stability of casein
particles which in turn get precipitated and clog the bowl there by lowering the efficiency of separation.
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COMPOSITION OF BUTTER
Butter is principally composed of milk fat, moisture, salt and curd. It also contains small amount
of fat, lactose, acids, phospholipids, air, microorganisms, enzymes and vitamins. The proportion
of principal constituents in butter is largely controlled by the method of manufacture and this is
turn is chiefly regulated to conform to the standards of butter prescribed by regulatory
authorities such as codex and FSSAI.
Composition of butter
Introduction
Butter, a fat rich dairy product obtained by churning cream and working the granules thus obtained into a
compact mass, has been a staple item of diet in many countries of the world. Up to the middle of the
nineteenth century, manufacture of this product was mainly confined to the farm on cottage scales. It was
only after the development of centrifugal cream separator in 1879, fat testing methods by Babcock (1890)
and Gerber (1892) together with introduction of artificial refrigeration and pasteurization around 1980, the
industrial production of butter developed rapidly. Prior to 1970 most of the world’s butter was manufactured
by batch-process. However, since World War-II, continuous processes have been introduced to achieve
increased manufacturing efficiencies. Regardless of manufacturing method employed, the essential feature
of churning evolves destabilization of cream emulsion by means of mechanical agitation.
Butter and other fat spreads can be characterized by the type of emulsion. In milk or cream, fat is dispersed
in the continuous phase of serum while in butter, there is a reversal of phase i.e. fat becomes the continuous
phase with serum dispersed in it. This phase reversal is carried out by churning cream in butter churns.
Steps involved in the conventional process of butter making which comprises preparation of cream and
churning and working are given in Figs. 18.1 and 18.2 and described below.
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Preparation of Cream
Commercial butter can be produced from both sweets as well as cultured cream. Very little cultured butter is
produced in India and U.S.A., although in Europe and Canada, cultured butter is an important product.
However, most creamery prefer to produce butter from sweet cream as it result in sweet butter milk which
has better economic value than sour butter-milk that results when sour/cultured cream is churned.
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Flow Diagram of Butter Manufacturing
1. Neutralization of cream
Sour cream must be neutralized to make butter of good keeping quality. It is under stood that by
neutralization of cream acidity of cream is reduced. Churning of High acid cream may cause high fat loss
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which can be prevented by neutralization. In pasteurization of sour cream, the casein curdles, by entrapping
fat globules, as the bulk of curd goes in butter milk, causing high fat loss.
Objectives of neutralization
1. The objectives of neutralization are to reduce the acidity in cream to a point (0.14 -0.16%) which
permits pasteurization without risk of curdling, to produce butter which keeps well in cold storage
2. To avoid excess loss of fat which result from the churning cream i.e excessively sour.
3. To guard against undesirable flavors which may result when a cream of high acid which is subjected
for pasteurization at higher temperatures.
4. To improve the keeping quality of butter from high acid cream. Salted-acid-butter develops a fish
flavor during commercial storage at -23 to -29 OC.
Soda neutralizer
84 90
NF=84/90=0.933
106 90
NF= 106/180=0.58
40 90
NF=40/90=0.444
Lime neutralizers
74 90×2=180
NF= 74/180=0.411
58 180
NF= 58/180=0.322
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NF = Neutralization factor
The quantitative relationship between amount of lactic acid present in solution and amount of pure
neutralizer required to give exact neutralization is fixed and definite amount of CO2 is driven off by air.
Ex: 90g of lactic acid requires 84g NaHCO3 (or) 106g Na2CO3 (or) 40g of NaOH for neutralization.
Acidity in cream is present chiefly in the serum portion and not in fat. The acidity in cream as a whole
known as cream acidity (C.A.) while the acidity per cent found in serum is known as cream serum acidity
(C.S.A). Cream serum acidity is more reliable than cream acidity.
CA % = Serum % in cream
CSA% 100
Accurate neutralization of sour cream is important to get a desired quality product. Neutralization is
influenced by several factors such as:
i. Accuracy in sampling.
There are five essential steps to follow for cream neutralization. These are:
The safe maximum limit of churning acidity varies with the richness of the cream. Since the acidity of cream
is chiefly contained in the cream serum, cream serum acidity adjustment would give better results.
= 0.357%
Usually serum acidity is kept at 0.35% to achieve best keeping quality of butter.
Ex.1 cream test 20% fat, serum acidity 0.35% is desired what should be the acid test of the cream?
= 0.80 × 0.35
= 0.28%
Representative sample should be taken. Weight of cream should be accurately measured as the final amount
of neutralizer will be dependent on the weight of cream.
Effect of CO2 on acidity should be taken care especially in high acid cream (acidly > 0.65%)
N. F. for
Neutralizer should be dissolved or emulsified in clean water, diluted to approx. 20 times its weight with
water; the solution must be distributed quickly & uniformly throughout the entire batch of cream and mixed
thoroughly with cream. For efficient mixing, neutralizer is usually sprayed onto the surface of well agitated
cream. While the neutralizer is added, the cream should be agitated vigorously and continuously. Agitation
of cream is preferable for 5-10 min after neutralization. Temperature at the time of neutralization should be
30oC. (High enough for smooth consistency & low enough to prevent abnormal heat curdling of the sour
cream)
The above precautions are essential, if efficiency of neutralization, protection of butter against neutralizer
flavour, oily metallic flavour and mealy body, avoidance of pasteurizing difficulties and prevention of
excessive fat losses in the buttermilk are to be assured.
Acidity should not be checked immediately after neutralization because of the following reasons:
In case of lime and Magnesia neutralizers, the neutralizing action is slow. It completes after
pasteurization & cooling.
In case of soda neutralizers, CO2 is liberated and this reacts acid toward the phenolphthalein
indicator. After pasteurization, expulsion of CO2 is largely accomplished. Therefore, testing acidity
after pasteurization would give correct results.
Fresh cream always contains some dissolved carbon dioxide (as carbonic acid) which reacts with sodium
hydroxide during titration and shows a higher acidity test. But the carbon dioxide does not react with sodium
bicarbonate neutralizer and consequently over neutralization results.
1. To avoid the intense effect on flavor of a large amount of any one neutralizer with high-acid cream.
2. To avoid production of excessive carbon dioxide by the use of sodium bicarbonate with high-acid cream
For this purpose the cream is first neutralized with lime neutralizer and brings the cream acidity down to
0.3-0.4 percent. Next use soda neutralizer to bring the cream acidity down to the desired level.
8 .Neutralizing Precautions
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In order to secure the desired results, i.e., accurate acid reduction, absence of objectionable neutralizer flavor
and of excessive fat losses, make sure of the correctness of weight of cream and acid test. Do not heat the
sour cream above 85 to 90OF, before neutralization, use the correct amount of neutralizer in properly diluted
form, distribute it evenly over the cream, and continue agitation of the neutralized cream for 5 to 10 minutes
before starting to pasteurize.
9. Type of Neutralizers
Neutralizers in order to accomplish the purpose, for which they are used in the creamery, must have alkaline
properties. They must be alkalis, alkaline earths or their substances. An alkali is a substance that has the
property of neutralizing acids, forming salts with them. The neutralizers used for reducing acidity in cream
belong to either one or the other of two groups namely.
Lime Neutralizers
Soda Neutralizers
Lime neutralizers
The principal constituent of the majority of lime neutralizers is calcium. Many of the lime neutralizer’s
available for cream neutralization also contain some magnesium. The various commercial lime neutralizers
differ from one another chiefly with respect to the proportion of calcium and magnesium they contain. They
are conveniently placed in three groups, as follows:
a. Low magnesium limes: Containing 5% or less of magnesium. A well Known brand of creamery lime
belonging to this group is peerless lime.
b. Medium magnesium limes: Containing about 30-35% magnesium. To this group belong such brands ad
Kelly Island lime, Neutra-Lac and Neutra-Lime.
c. High magnesium limes: Containing about 45 to 55% magnesium. All wood lime is an outstanding
representative of this group. All magnesium limes in the form of magnesium oxide and magnesium
carbonate are also available. They are artificially prepared limes and demand a higher price than the natural
limes. Their effect on the flavor of cream and butter however is outstandingly favorable.
Calcium carbonate - low solubility, low alkalinity unsuitable for cream neutralization and action is very
slow.
In general the medium and high magnesium limes react somewhat more satisfactorily in the cream than the
low magnesium limes. The higher the magnesium oxide content of lime the greater is its alkalinity and its
neutralizing strength.
Soda neutralizers
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Soda neutralizers commonly used in the creamery are:
3. Mixtures off baking soda and soda ash, such as Sodium sesquicarbonate, Neutralene and Wyandotte.
1. Purity: Soda Neutralizers will have less than 0.1 impurities whereas lime neutralizers will have
sand and clay.
2. Solubility: Sodium Neutralizers are completely soluble whereas lime neutralizers are slightly
soluble in waste.
4. Action on casein: Soda neutralizers will have solvent and softening action and assist in
minimizing clogging during processing. Lime neutralizers tend to granulate (or) precipitate
casein which results in bitter lime flavor on pasteurization.
5. Acid reaction: Soda Neutralizers act on serum acidity first. In lime neutralizers the calcium has
natural affinity towards casein, lime particles attach themselves mechanically to casein and it is
not completely available for neutralizing the lactic acid. The neutralizing capacity of lime
neutralizer is 80-85%.
6. Foaming effect: Soda neutralizers will produce violent foam when there is high acidity
NaHCO3 has more effect than Na2CO3. Lime neutralizers do not create foam.
7. Neutralizing strength: Soda neutralizers are weaker alkalis than lime neutralizers about twice
as many kilograms of soda neutralizers are required to neutralize given amount of acid as
compared to lime neutralizers.
9. Effect on texture of butter: In case of high acid cream especially neutralizes to a low point
there is a tendency to butter from lime neutralizer cream will give less smooth texture than soda
neutralizers.
10. Effect on flavor of butter: Soda neutralizers produce soapy type of flavor. Lime neutralizers
produces course lime flavor. In over all the butter will give neutralizer flavors.
Standardization of cream
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It refers to adjustment of fat to desired level. It is done by adding calculated quantity of skim milk or butter
milk. Desired level of fat in cream for butter making is 33 to 40 per cent. Standardization to both higher and
lower level leads to higher fat loss in butter milk. Reduction of fat by adding water should be avoided as it
interferes ripening of cream and also results in butter with “flat” or “washed off” flavour.
Pasteurization of cream
It refers to adjustment every particle of cream to a temperature not less that 71OC and holding it at that
temperature for at least 20 min or any suitable temperature-time combination using properly operated
equipments. The main objectives of pasteurization are: (i) it destroys pathogenic microorganisms in cream
so as to make it, and the resultant butter, safe for human consumption. (ii) It also destroys bacteria, yeast,
mould, enzymes and other biochemical agents that may lower keeping quality. (iii) It also eliminates some
of the gaseous and training substances. A number of equipment viz. LTLT (law temperature long time, 74 OC
for 30 min); HTST (high temperature short time, 85 oC for 15s.) and Vacreator, a direct steam injection
method, can be employed for this purpose. More severe heat treatment of cream should be avoided as
higher, the temperature the greater the migration of copper from the milk serum into milk fat globules. This
increases the level of copper associated with the milk fat making it more prone to the development of
oxidative rancidity and reduce the shelf-life of butter.
Pasteurization of cream for making ripened cream butter is commonly carried out at higher temperature than
for sweet cream butter e.g. 90-95oC for 15 or 105-110oC with no holding. Severe heat treatment denatures
whey proteins, particularly lactoglobulins, exposing-SH groups which act as antioxidants and can enhance
starter growth.
Ripening of cream
Ripening refers to the process of fermentation of cream with the help of suitable starter culture. This step
can be eliminated if sweet-cream butter is desired. The main object of cream ripening is to produce butter
with higher diacetyl content. Ripening improves the keeping quality of salted butter but it reduces the
keeping quality of a salted butter. Starter culture consisting of a mixture of both acid producing
(Streptococcus lactis, S.cremories) and flavour producing (S.diacetylactis, Leuconostoc citrovorum and/or
Leuc. dextranicum) organisms is added. Amount of starter added depends on several factors and usually
ranges between 0.5-2.0 percent of the weight of the cream. After being thoroughly mixed, the cream is
incubated at about 21oC till desired an acidity is reached. Cream is subsequently cooled to 5-10� C to arrest
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Biosynthesis of diacetyl is not sufficient above pH 5.2. Stopping fermentation of cream by cooling at pH
5.1-5.3, results in a milder flavour; whereas continuing fermentation upto pH 4.5-4.7 results in higher levels
of both diacetyl and lactic acid, giving more pronounced flavour.
1. Purpose
The fundamental objects of cream ripening are to produce butter with a pleasing, pronounced flavor and
aroma, and to produce this flavor and aroma uniformly from day to day. Ripening also influences somewhat
the exhaustiveness of churning and it affects the keeping quality of the butter variously, according to quality
of original cream, churning acidity, and whether made into salted or unsalted butter.
2. Starter culture
Mixture of both acid producing organisms (Lactococcus lactis, L. cremoris) and flavour producing
organisms (S. lactis subsp. diacetylactis, Leuconostoc citrovorum and/or Leuconostoc dextranicum). Starter
culture is added at the rate of 0.5 to 2.0% of the weight of cream and incubated at about 21 oC till desired
acidity is reached. Usually it takes 15-16 hrs.
The mildly acid and pronounced “nutty” flavor that is characteristic of the pleasing flavor of good butter is
usually accompanied by a high, attractive aroma. The typical butter flavor is due to the presence of diacetyl
in combination with lactic acid, carbon dioxide, acetoin and intermediary products such as acetaldehyde, and
probably other aromatic products as yet not definitely determined. These substances are the products of
fermentation, brought about by the associative action of lactic acid-producing bacteria and citric acid-
fermenting bacteria.
These bacteria are propagated and their flavor and aroma substances produced in the starter. During cream
ripening the starter that is added to the cream, therefore, functions in two ways. It seeds the cream with
species of bacteria that are capable of producing the desired aroma and flavor substances in the cream, and it
adds to the cream the aroma and flavor substances produced and already contained in the starter.
Cream ripened with a normal starter shows a varying ratio of diacetyl to acetoin. In the case of 20% cream, a
ripening temperature of 17˚C. (62.6˚F) yields the largest amount of diacetyl. With increasing fat content the
amount of diacetyl + acetoin increases. Cream testing 40% fat yields higher diacetyl content in the butter
than 20% cream, or whole milk. The diacetyl content of butter to affect its flavor as follows:
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Amount of Diacetyl Flavor
Butter contains a relatively small proportion of the diacetyl and acetoin content of the cream from which it is
made. Fresh buttermilk contains larger amounts of diacetyl and acetoin than the corresponding butter and
than the original cream, at churning time. The serum of butter contains larger amounts of diacetyl + acetoin
than the fat of the same butter. The wash water contains appreciable amounts of diacetyl + acetoin. Churning
2 liters of cream yields the following amounts of diacetyl in the buttermilk, wash water and butter:
The following amounts of diacetyl + acetoin are present in washed and unwashed butter:
These findings indicate that in commercial manufacture of butter, particularly in the case of unsalted butter,
excessive washing gives the finished butter, even when made from properly ripened cream, a disappointing
“washed-out” flavor.
The development of flavor and aroma in butter by cream ripening, or by any other process of manufacture,
can be of value only, provided that it does not impair or destroy the keeping quality of the resulting butter.
The ripening of cream affects the keeping quality of butter in two fundamental ways, namely, by its control
of age deterioration due to bacterial causes, and by its influence on age deterioration due to chemical causes.
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Bacteriological effect
The ripening of cream improves the keeping quality of butter as far as keeping quality is dependent on
freedom from age deterioration due to biological causes. Cream ripening assists in controlling bacterial
deterioration in butter. In butter made from ripened cream there is a great prevalence of lactic acid bacteria
and a relatively high acidity and probably an abundance of lactate salts. These agencies are antagonistic to
the great majority of flavor-damaging organisms that may be present in the butter, thus retarding their
action, preserving the fresh or desired flavor, and prolonging the keeping quality of the butter.
Chemical Effect
Cream ripening does not improve the chemical stability of butter. On the contrary, under average
commercial conditions of manufacture, the ripening of cream to a full aroma and flavor shortens the life of
salted butter. The usual flavor defects that develop with age in butter made from fully ripened cream are
oily-metallic, fishy and sometimes tallowy flavor. There is a tendency also to intensify the well-known cold
storage flavor. This is especially true of salted butter made from cream that arrives at the factory in sour
fermented condition, is neutralized, pasteurized and re-ripened to a high acidity. It applies also, through to a
somewhat lesser extent, to salted butter made from ripened sweet cream. It does not apply to unsalted butter.
Salted butter made from sweet, unripened cream, or from sour cream, neutralized and pasteurized, keeps
better from the standpoint of absence of flavor deterioration due to chemical causes, than salted butter made
from the same cream ripened to a full flavor and aroma.
For fresh consumption salted butter, cream of moderate richness (30% fat) may safely be ripened to about
0.25 to 0.30% acid. For salted butter of commercial cold storage, it has been found preferable not to ripen
the cream and to churn it at an acidity of about 0.21% acid or lower. In case of unsalted butter, the cream
may be ripened to any acidity without jeopardizing keeping quality.
Cooling and ageing are processes which prepare the cream for subsequent operation of churning. When
cream leaves the pasteurizer, the fat in the globule is in liquid form. When cream is cooled, fat
crystallization starts, cream will not churn unless the butter fat is at least partially crystallized. If
solidification of fat is not sufficient, the fat losses in butter are high. Rate of cooling has an important
influence on the body and texture of butter. The temperature to which cream is cooled is chosen is such a
way that the butter produced is of optimum consistency and cream churns to butter in a responsible time of
about 35-45 minutes. Churning at too high temperature may give butter with “greasy” body which may work
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up too quickly and become sticky. Generally cooling temperature in summer should be 7-9OC and that if in
winter (10 OC-13 OC).
Before churning, cream is subjected to a program of cooling designed to control the crystallization of the fat
so that the resultant butter has the right consistency.
Butter fat contains varying amounts of soft and hard fats. The relative amounts of fatty acids with high
melting point determine whether the fat will be hard or soft. Soft fat has a high content of low-melting fatty
acids and at room temperature this fat has a large continuous fat phase with a low solid phase, i.e.
crystallized, high-melting fat. On the other hand, in a hard fat, the solid phase of high-melting fat is much
larger than the continuous fat phase of low-melting fatty acids.
In butter making, if the cream is always subjected to the same treatment it will be the chemical composition
of the milk fat that determines the butter's consistency. A soft milk fat will make a soft and greasy butter,
whereas butter from hard milk fat will be hard and stiff.
Pasteurization causes the fat in the fat globules to liquefy. And when the cream is subsequently cooled a
proportion of the fat will crystallize. If cooling is rapid, the crystals will be many and small; if gradual the
yield will be fewer but larger crystals. The more violent the cooling process, the more will be the fat that
will crystallize to form the solid phase, and the less the liquid fat that can be squeezed out of the fat globules
during churning and working.
The crystals bind the liquid fat to their surface by adsorption. Since the total surface area is much greater if
the crystals are many and small, more liquid fat will be adsorbed than if the crystals were larger and fewer.
In the former case, churning and working will press only a small proportion of the liquid fat from the fat
globules. The continuous fat phase will consequently be small and the butter firm. In the latter case, the
opposite applies. A larger amount of liquid fat will be pressed out; the continuous phase will be large and the
butter soft.
So by modifying the cooling program for the cream, it is possible to regulate the size of the crystals in the fat
globules and in this way influence both the magnitude and the nature of the important continuous fat phase.
For optimum consistency where the iodine value is low, i.e. the butterfat is hard, as much as possible of the
hardest fat must be converted to as few crystals as possible, so that little of the liquid fat is bound to the
crystals. The liquid fat phase in the fat globules will thereby be maximized and much of it can be pressed out
during churning and working, resulting in butter with a relatively large continuous phase of liquid fat and
with the hard fat concentrated to the solid phase.
The program of treatment necessary to achieve this result comprises the following stages:
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rapid cooling to about 8oC and storage for about 2 hours at this temperature; heating gently to 20 -
21oC and storage at this temperature for at least 2 hours (water at 27 - 29oC is used for heating)
Cooling to about 8oC causes the formation of a large number of small crystals that bind fat from the
liquid continuous phase to their surface.
With an increase in the iodine value, the heating temperature is accordingly reduced from 20-21oC.
Consequently a larger number of fat crystals will form and more liquid fat will be adsorbed than is the case
with the hard fat program. For iodine values up to 39, the heating temperature can be as low as 15oC.
Where the iodine value is greater than 39-40 the "summer method" of treatment is used. After pasteurization
the cream is cooled to 20oC. If the iodine value is around 39 - 40 the cream is cooled to about 8oC, and if 41
or greater to 6oC. It is generally held that aging temperatures below the 20 o level will give a soft butter.
Churning of Cream
It is during the churning process that cream is converted into butter. Here the fat gloubles are disrupted
under controlled conditions to destabilize o/w emulsion and bring about agglomeration of milk fat. What
happens during churning has been explained by various theories of churning as discussed in lesson 8.3. The
sequence of events that occur during churning is as follows:
i) Churning is initiated by agitation of cream causing incorporation of numerous air bubbles into the
cream.
ii) With incorporation of air there is increase in the volume of cream and air plasma interface.
iii) Surface active (such as frictional, impact, concussion etc.) causes partial disruption of fat globule
membrane
iv) The fat film, thus formed, serve as a foam depressant causing the air bubble to burst.
v) The liquid fat also serves as cementing material causing fat globules to clump together and
eventually butter grains are formed which floats in plasma i.e. butter milk.
Initial working
Working of butter is essentially a kneading process in which butter granules are formed into a compact
mass. During this operation, any excess moisture or buttermilk is removed. However, the emulsion (w/o) at
this stage is not fully stable.
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Salting of butter
In conventional process, butter may be salted by adding salt to butter churn after initial working of butter.
Salt to be added must be high quality e.g. IS 1845:1961, with low level of lead, iron and copper. The grain
should be fine, all passing through IS: sieve-85 (aperture 8424). It should be 99.5 to 99.8% sodium chloride
and microbial count should be less than 10/g. Salt sets up osmotic gradient which draws water from the
butter grains. This can lead butter to be leaky. Salted butter should therefore, must be thoroughly worked.
Salt may be added either in dry form or as saturated brine solution.
Adjustment of moisture
After the addition of salt, the moisture content in butter is adjusted by adding calculated amount of
additional water. In most countries, maximum limits of 16% is placed on the level of moisture. Amount of
water is to be added in a batch of butter is calculated as follows:
Starter distillates, if required, may also be added at this stage to enhance the flavour of resultant butter, if
cream has not been cultured.
develop “mottles” on standing. Moisture droplet size normally ranges from 1 to 15 micron and there are
approximately 10 billion droplets per gram of butter. Working affects the colour of butter (making is slightly
light). Working also increase air content (this favors growth of microorganisms, oxidative effects and
therefore poor keeping quality). Vacuum working of butter may be carried out with advantage to reduce the
air content of butter. Vacuum range from 15-40 cm of Hg may be used. Air content of conventional butter
range from 3-7% by volume with an average of 4 ml/100 while that of vacuum worked butter it is about 1
ml/100g.
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CHURNING OF CREAM
Introduction
Churning is the process of converting cream into butter through appropriate mechanical
manipulations leading to the conversion of oil-in-water (O/W) emulsion of cream into
water-in-oil (W/O) emulsion desired in butter. The emulsion change accompanied by
removal of buttermilk and working of butter yields the desired structure and texture in
the product.
Theories of Churning
The conversion of oil-in-water (O/W) emulsion of cream into water-in-oil (W/O)
emulsion to form butter has been explained by various theories of churning. These
are discussed below:
This theory was proposed by Fischer and Hooker in 1927, the theory is therefore also referred as
Fischer and Hooker’s theory. According to this theory churning is a process of phase reversal
i.e. changing of oil in water emulsion (O/W) to water in oil emulsion (W/O). The stability of
emulsion is related to the relative volumes of the two constituents present. When oil and water
are mixed together, the resulting suspension may be a suspension of (o/w) or suspension of w/o.
The type of emulsion obtained depends on the proportion of the two main constituents present,
the order in which they are added and the type of emulsifier used.
In churning cream, initially the ratio of surface area to volume (S/V) of the fat globules is large.
When the churning proceeds, surface area decreases and with progressive churning, surface area
keeps on decreasing. The reduced surface area can no longer hold all the butter milk so it breaks
i.e. separates out.
Agitation of cream during the churning process causes coalescence and clumping of fat globules
until eventually the ratio of surface area to volume of the fat units becomes so small that the
reduced surface area can no longer contain the butter milk in stable form. The O/W emulsion
then suddenly breaks; giving butter grains consisting of an emulsion of W/O and free butter
milk.
The supportive evidence of this theory is established by the fact that in normal butter, water is
not in continuous phase. It has been demonstrated that plastic cream, containing 80-82% fat,
conducts electricity and it responds to the pH determination showing water is in continuous
phase but butter is a very poor conductor of electricity and pH determination cannot be done on
butter but only on serum separated from it.
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Microscopic structural studies conducted by Rahn (1928) revealed that butter is not a true W/O
emulsion. A proportion of globular fat are still intact in worked butter. He explained that since
butter fat is cooled and largely crystallized before the start of churning, true W/O type emulsion
is rarely possible.
This theory was put forward by Rahn (1928). According to Rahn, cream (and also milk)
contains a foam producing substance which gets solidified gradually when cream (or milk) is
agitated.
During churning first foam is produced. The fat globules then, due to surface tension, tend to
concentrate on the foam bubble and thus are bought into such close contact that clumping of fat
globules take place. Subsequently the foam producing substance assumes a solid character and
the foam collapse. The fat globules then coalesce and butter is formed.
According to Rahn’s theory, fat in cream at churning time is completely crystallized and the
pass in to butter with their membrane intact and thus butter is a compact mass of fat globules in
which butter milk, water and air are distributed as small globules.
Rahn’s theory was based on his findings that air was necessary for normal churning of butter.
Application of normal amount of mechanical agitation, in the absence of air did not result in
churning of cream. The effect of overloading of churn resulting in increased churning time
supported this theory (in case of overloading the churn, there was no sufficient space in the
churn for the formation of required amount of foam hence more time).
This theory was, however, subsequently criticized because of the fact that foam formation i.e.
presence of air, is not required in some of the continuous butter making processes developed
subsequently.
King’s theory was proposed in 1930 and 1953 and it is regarded as the modern theory.
According to this theory, what happens during churning is mid-way between the ‘Phase
Reversal theory’ and Foam theory. The modern concept has been summarized by Mc Dowall as
follows:
i) The fat in the cooled cream, at churning temperature, is present as clusters of fat globules.
And within each globule it is present partly in solid and partly in liquid form.
ii) Agitation (churning) breaks up the clusters and causes foam formation. The globules become
concentrated to some extent in the film around the air babble in the foam and thus are brought
into close contact of each other.
iii) The movement of the globules over one another in the foam film and the direct concussion
between them causes a gradual wearing away of the emulsion protecting surface layer (of
phospholipid protein complex). The globules then adhere together to form larger and larger
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particles. Eventually these particles become visible as butter grains. The grains enclose some of
the air from the foam. The fat still mainly remains in globular form.
iv) The working of the butter grains causes the globules to move over one another. Some of
them, under the effect of friction and pressure cause some yields out a portion of the liquid fat,
others are broken during working. Finally there is enough free liquid fat present to enclose the
water droplets, air bubbles and intact fat globules.
Factors Influencing Churn ability of Cream
The factors which influence the churnability of cream can be classified into two groups as
Factors related to the initial character of the cream includes chemical composition of the butter
fat, size of fat globules, richness of cream and viscosity of cream while factors related to
processing conditions are churning temperature, fullness of churn, speed of churn, design of
churn etc. All these factors are discusses in the following sections.
Churnability of cream is greatly influenced by the proportion of soft fats (low melting point fat)
and hard fats (high melting points). This proportion determines the degree of fat solidification in
the cooled cream. If the proportion of soft fats is more than the churning period will be
shortened, butter made will have less firmness and there will be more fat losses in butter milk. If
the proportion of soft fats is low, it will prolong the churning period.
If rich cream is churned at a high temperature the butter will form in a remarkable short time,
providing all other conditions are favourable. Thin cream churns much more slowly, and can be
churned at high temperature than thick cream, without injuring the quality of butter when rich
cream is churned at a high temperature and the butter forms in a short time (about 10 min), the
butter will usually be greasy in body and will not contain a much of butter milk, which will be
more or less difficult to remove on washing. When thick cream is churned, the butter does not
break in the form of small round granules, as it does when thin cream is churned.
When thick cream is (36 to 38% fat) is churned at as high a temperature as is consistent with
getting a good texture, the best result are obtained. This type of cream produces less butter milk
and consequently less part loss in the butter milk and this will give increase over run and the
breaking of the butter at the end of the churning will be such as to cause the granules to appear
large and flaky, rather than small round granules. The more flaky granules of butter will retain
more moisture than the small, harder granules under the same treatment.
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When thick cream is churned and the temperature is moderately high, it is almost impossible to
churn the butter into granules. This condition causes butter from thick cream to contain more
moisture than butter from thin cream.
The more viscous the cream, more time is required to complete the churning process. More
viscosity diminishes the freedom of movement of the fat globules, lessens their opportunity of
being brought together and retard coalescence, thereby increases churning time.
Cream containing large fat-globules (avg. diameter 4.6µ) churn more quickly than cream
containing small globules. Cream containing small fat globules (avg. diameter 3.4 µ) churn with
difficulty and require twice as much time to break as the large globule cream. The butter made
from such cream has short grains and crumbly character.
The temperature is one of the most influential factors in determining the churnability of cream.
The higher the temperature of cream, the sooner the churning process will be completed. Too
high a churning temperature is however not desirable. It causes the butter to contain soft lumps
instead of in a flaky granular form. This is deleterious to the quality of the butter. It causes first a
greasy texture of butter, and secondly, it causes the incorporation of too much butter milk in the
butter. This butter milk contains lactose, curd, and water, which when present together in butter,
are likely to sour and in other ways deteriorate the butter. Curd and lactose should be excluded
from butter as much as possible, in order to eliminate food for bacteria which may be present.
Too low temperature is also undesirable although it is better to have the temperature a little low
rather than too high. Cream at low temperature becomes more viscous. On agitation in the churn
such cream if it is very thick will adhere to the sides of the churn and rotate with it without
agitating; consequently no churning will take place. Too low a temperature brings the butter in
such a firm condition that it takes up salt with difficulty, and when this hard butter is being
worked, a large portion of the water in the butter is expressed, and the overrun will be lessened
to a great extent without increasing the commercial value of the butter.
The degree of hardness of the fat in cream is the governing factor in deciding the temperature
during churning. The hardness of the fat depends upon:
During spring, the cows yield milk containing a longer proportion of soft fats; consequently the
churning temperature is always lower in the spring than in the winter. During the winter, when
the cows are fed on dry food chiefly the harder fat increases in quantity, therefore, a higher
churning temperature is necessary during that time.
The nature of food fed affects the melting point of butter to a considerable extent. Cotton seed
will cause butter to become hard. When larger amount of cotton seed is fed, the butter assumes a
crumby, hard condition.
It can be concluded that the churning temperature may vary between wide limits, but the average
desirable churning temperature according to the season is
For maximum agitation to take place during churning, the cream must dash from side to side or
from top to bottom. Optimum load for maximum agitation should be one third to one half full.
Overloading of the churn diminishes free space in the churn, diminishes concussions and leads
to increase in churning time. The overloaded cream may be churned at higher temperature so
that churning time is not prolonged but this is not recommended as higher temperature increases
fat loss in butter milk and produces soft and leaky butter.
Under loading the churn is not economical for the manufacturer and at the same time the cream
will adhere to the inner side of the churn and delay churning.
Proper agitation is necessary for churning cream into butter. The speed of the churn provides
agitation to cream. So, the maximum speed of the churn is the speed that yields the maximum
amount of agitation. It is dependent on the ratio of centrifugal force and gravity force.
Centrifugal force should be less than gravitational force.
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(8)Churning Difficulties
The causes of churning difficulties are usually associated with the peculiar character of the
cream and particularly where the source of cream is confined to a single herd. Usual causes of
prolonged churning time and difficulty in formation of butter are excessive hardness of fat,
small fat globules, use of thin cream for butter making and high protein content in cream.
i) Excessive hardness of fat: Winter cream usually contains more hard fats. Use of such cream
for butter making prolongs churning time because it diminishes the ability of fat globules to
coalesce during churning.
ii) Small fat globules: cream that contains small fat globules takes more time for churning as the
ratio of membrane material to fat increases and thus provides increased protection to fat
globules.
iii) High protein content: such cream delays butter formation because of increased
viscosity that minimizes the force of concussion between the globules.
iv) Use of thin cream: Such cream also have increased protection due to higher membrane
protein to fat ratio and also due to intervening serum that keeps globules apart during churning.
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BUTTER: COLOUR
Introduction
Butter colours are required to manufacture uniform quality butter all the year round as the
natural components (like carotene) responsible for colour in butter, varies according to many
factors like season, breed, stage of lactation, feed among others. Therefore, a calculated amount
of colour is added in butter so that it does not have influence of varying natural colouring
components present in milk or cream.
– It should have such permanency of emulsion as to prevent settling out upon standing
The butter color should be preferably added to the cream while loading the churn. Alternatively,
it may be added to and mixed with salt just before final working of the butter. It is then worked
into the butter and distributed uniformly.
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CHEMISTRY OF GHEE
Introduction
Competition in the organized ghee production sector leads to create brand value to the
product. This brand value comes with quality and special features associated with the
product. Today, consumers are much aware of the brand quality through media.
Manufacturers or producers are looking forward continuously for innovations that helps to
create market for their product, may be through mode of packing, through product aesthetic
quality.
Fatty acid composition of buffalo milk ghee also varies from cow milk ghee. The amount of
butyric acid is significantly higher in buffalo than in cow ghee. The levels of short chain
fatty acids caproic to myristic are significantly higher in cow than buffalo ghee where as
levels of palmitic and steoric are higher in buffalo than in cow ghee. Major fatty acid in
buffalo and cow milk fat is given in table 36.3.
Ghee made from buffalo milk is white (lack of carotenoids) with greenish tinge and that
made from cow milk is golden yellow. The characteristic colour of buffalo fat has been
attributed to “tetrapyrozole” pigments- “biliverdin and bilivubin” this pigment is conjugated
to a protein in milk, but is released during the manufacturing process of ghee making. Thus,
imparting yellowish-green colour to buffalo ghee.
During manufacturing, water gets evaporated and fat present in the cream or butter getting
concentrated (curd particles (MSNF present in cream or butter) starts settling at the bottom
during clarification process. Flavour formation in ghee happens during fermentation of
cream and during clarification process. Colour development and granulation also happens
during clarification for the subsequent packaging of ghee.
Free fatty acids, carbonyls and lactones are the major groups of compounds contributing to
ghee flavour. The flavour profile is affected by method of preparation temperature of
clarification and storage period.
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1. Carbonyls
2.Lactones
The lactone level in buffalo ghee has found to be higher than that in cow ghee. It was the
highest in direct cream (DC) ghee, followed by creamery butter (CB) and lowest in desi
ghee. The lactose level in butter (12 ppm) increased 1.9, 2.4, 2.8 and 3.0 fold on clarifying at
110 OC, 120 OC, 140 OC and 180 OC respectively. Clarification butter at 100-120 OC doubles
the lactones level from butter. The lactone level in ghee showed a significant rise on storage.
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(ii) Oxidation - Saturated and unsaturated aldehyde, ketones, alcohols and
hydrocarbons.
1. Texture of ghee
When ghee is stored at room temperature, it crystallizes into three distinct fractions or layers,
(i) Oily (ii) granular semi-solid at the bottom and (iii) hard flakes portion floating on the
surface and sticking to the sides of the container.
According to Singhal et al. Layer formation in ghee could be prevented by storing it at 20 OC
or below immediately after preparation. Ghee thus solidified could subsequently be stored at
higher temperature without formation of layer. The liquid portion of ghee varies with storage
temperature, shape and size of container, repeated heating and agitation, ripening of
cream/butter, storage and handling, external seeding etc.
2. Market quality of ghee
Consumer judge the quality of ghee base on its inherence flavour, colour and appearance.
Ghee should have characteristic pleasant, nulty, slightly cooked rich aroma. Ghee flavour is
best described as lack of blandness, sweetly rather than acid. Golden yellow to light yellow
colour of ghee is appreciated largely. Granular appearance of the product rather more score
as it is important quality as well as purity preventer of ghee.
Apart from above sensory characteristics, its chemical and other physical preventers are
evaluated to judge the quality of ghee and also to prevent adulteration of ghee.
(i) Refractive Index: It is the ratio of the velocity of light in vacuum to the velocity of
light in the sample medium. More generally, it is expressed as the ratio between the sine
of the angle of incidence to the sine of the angle of refraction when a ray of light of a
definite wave length wave length (usually 589.3 µm the mean of the D-lines of sodium)
passes from air into the fat. In case of milk fat reading is normally made at 40 OC using
Abbe refractometer and its values range from 1.4157 to 1.4566. This value is low in
comparison to the other fats and oils. The RI if ghee is influenced by both the molecular
weight and the degree of saturation of the component fatty acids. RI could be used as
indicator of adultration.
(ii) Iodine Number: It is defined as number of grams of iodine absorbed by 100 g of fat
under specified conditions. Thus constant is a measure of the unsaturated linkages
present in a fat. The iodine number for milk fat falls within the range of 26 to 35 which is
low in comparison to other fat and oils. This is estimated using Wig’s method. One
molecule of halogen compound is absorbed by each unsaturated linkage and the
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absorption is expressed as the equivalent number of grams of iodine absorbed by 100 g
of fat.
(vi) Melting Point: Melting point for milk fat ranges from 30 OC to 41 OC as reported in
literature.
(i) Raw-materials (Milk, Dahi, Cream, Butter) used for ghee making
Milk used should be clean, fresh and strained. Use of ripened cream, butter improves the
flavour score of ghee.
(ii) Method of preparation and temperature of clarification
Flavour compounds of ghee vary according to its method of preparation. For example
desi methods have more volatile Carbonyl compounds than cream method. Temperature
of clarification also has influence on the quantity of Carbonyl compounds and lactones
formation during ghee production.
(iii) Type of feed
It is the main factor affecting variation in fatty acid composition of milk fat. Roughages
in the feed mainly consist of cellulose contribute to the formation of fatty acid of 4 to 16
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carbon chain length and lipid content of the feed contributes to the formation if long
chain fatty acid if C16 and above. Animals fed with cotton seed meal will have high
amount of C1010 and C1210 fatty acids.
(iv) Season
In winter and monsoon, the granulation is more due to changes in the fatty acid profile.
Winter ghee showed higher acidity, melting point and grain size where as in summer the
saponification value was found to be higher.
Grading of Ghee
The quality of ghee can be judged by physical and chemical analysis. Customer can only perceive
appearance, taste and aroma of ghee. Therefore grading i.e. classification according to its quality
and purity is necessary to assure the customer. The Agricultural Produce (Grading & Marking)
Act, 1936 empowers the Central Government to fix quality standards, known as “AGMARK”
standards and to prescribe terms and conditions for using the seal of “AGMARK”. The word
'AGMARK' is a derivative of "Agricultural Marketing".
Objectives of AGMARK
i). To assure the consumer a producer of pre-tested quality and purity
ii). To enable manufacturers of high grade product to obtain better returns
iii). To develop an orderly marketing of the commodities by eliminating malpractices
when transferring from producer to consumer.
AGMARK is a certification mark of Government of India to ensure the purity and quality of
Agricultural and allied products in India. The Act empowers the Directorate of Marketing and
Inspection to
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AGMARK grades of ghee
Grade Letter and Circular
border colour
Special Red
General Green
Standard Chocolate
The labels shall be printed on the watermark paper of the Government of India and shall
have a micro tint back ground bearing the words “Government of India” in olive green color
Each label shall have printed thereon a serial number along with a letter or letters denoting
the series, e.g. A054987.
Each label shall have printed thereon the approximate weight content of the package on
which it is affixed.
Design of label
The word “Regional” shall be printed on each label used on a package of the ghee not conforming
to the normal physical and chemical constants specified as follows.
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AGMARK standards of ghee
Parameters Special Grade General Grade Standard Grade
Baudouin Test Negative Negative Negative
Butyro-refractomer 40.0- 43.0 40.0- 43.0 40.0-43.0
reading at 40 OC
Reichert Meissl Not less than 28.0 Not less than Not less than 28.0
value 28.0
Polenske value 1.0 - 2.0 1.0 - 2.0 1.0 - 2.0
Moisture content Not more than Not more than Not more than
0.3% 0.3% 0.3%
Percentage of Free Not more than 1.4 Not more than Not more than
Fatty Acid (as 2.5 3.0
oleic acid)
For cotton tracts areas such as part of Saurshtra and Madya Pradesh following standards are
applicable.
AGMARK standards for ghee produced in cotton tract areas
Parameters Special Grade
Winter Summer
Baudouin Test Negative Negative
Butyro-refractomer reading at 40 OC 41.5 - 43.0 42.5 - 45.0
Reichert Meissl value Not less than 23.0 Not less than 21.0#
Polenske value 0.5- 1.2 0.5 - 1.0
Moisture content Not more than Not more than
0.3% 0.3%
Percentage of Free Fatty Acid (as oleic Not more than 1.4 Not more than 2.5
acid)
General and Standard grade have Percentage of Free Fatty Acids (as Oleic acid) shall not
exceed 2.5 and 3.0 respectively.
According to the law it is not compulsory for every trader and manufacturer, to get his
produce certified under AGMARK symbol. Presently it is only a voluntary scheme of the
Government.
Requirements of High Grade Ghee
Consumer judges the quality and accepts it on the basis of three main attributes, taste and
aroma(flavour), granularity and colour.
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1. Flavour: High grade ghee should have natural sweet and pleasant odour, an agreeable
taste and it should be free from rancidity and any other objectionable falvour. A
pleasant, nutty, slightly cooked aroma is appreciable in the product.
2. Texture: Large uniform grains with very little liquid fat is desirable, greasy texture is
objectionable. Upon melting ghee should be clear, transparent, free from sediment and
foreign colouring matter.
3. Colour: The colour should be uniform throughout, it should be bright yellow for cow
milk ghee and white with or without a yellow or greenish tint for buffalo milk ghee.
Adulterants in Ghee
Adulteration of ghee in India is more prevalent especially in unorganized sector. Being the
most expensive fat people started to adulterate the product to make profits. Major adulterants
of ghee are as follows:
Government has made it compulsory that all Vanaspati must contain a maximum of 5% of
Sesame oil which can be identified in ghee by a simple colour test (known as Baudouin test).
By means of this Adultration of ghee with Vanaspati an extent of 3% can be detected.
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PHYSICO-CHEMICAL CHANGES TAKES PLACE DURING KHOA MAKING AND
STORAGE OF KHOA
(1)Quality of milk
In India both cow and buffalo milks are used for manufacture of traditional dairy products
depending on the availability and suitability of milk for a particular product. However, the
quality of the products greatly depends on the type of milk used for their preparation. Yield
of Danedar is and Dhap type of Khoa from buffalo milk is 24% and 25%.
a) Species of Animal: Buffalo milk is preferred over cow milk for khoa making because it
yields a product with soft, loose body and smooth granular texture which is highly suitable
for the preparation of sweets. The buffalo milk gives a greater out burn than that from cow
milk. The average yield from buffalo milk is 21.6-23% and from cow milk it is 18.3-18.5%
due to the higher T.S. Content in buffalo milk moisture content in khoa. Khoa from cow
milk is of inferior quality due to its dry surface, sticky and sandy texture and salty taste
(due to higher chloride and citrate content (Citrate buffalo milk 0.18%, cow milk 0.18%
and chloride: buffalo milk 0.07% and cow milk 0.10%)) which is not considered suitable
for manufacturing of best quality khoa based sweets.
b) Fat content in milk: A minimum fat level of 4% in cow milk and 5.5% in buffalo milk
is essential for production of khoa with desirable body and texture and to meet the FFA
requirements also. A lower fat content results in undesirable hard body and coarse texture
in the finished product which is not suitable for good quality sweets preparation. The fat
level higher than the minimum improves the quality of the final product. (The higher
emulsifying capacity of buffalo milk fat due to the presence of higher proportion of butyric
acid containing triglycerides (50%) than only 35% in cow milk fat and higher fat content in
buffalo milk is responsible for smooth and mellowy texture of buffalo milk khoa)
c) Acidity of milk: Fresh sweet milk yields the best quality khoa, while developed acidity
in milk produces an undesirable, coarse texture sour smell and bitter taste in to the khoa
which is unsuitable for sweet preparation.
d) Presence of additives and adulterants: Neutralization of high acidic milk improves the
texture, but does not improve the flavour of khoa. Further it gives saltish taste in the final
product.
Presence of colostrum in milk has a marked effect on the colour of khoa, which is deep
yellow with cow colostrums. It also gives pasty texture in the final product making it not
suitable for sweet making.
Adulteration of milk with water produces a brown khoa and a proportionate reduction in
the yield. Texture and flavour of khoa are not affected much when adulterated with starch
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the physical quality of khoa is considerably affected. It develops a harder body and a pasty
sticky texture not suitable for the preparation of confections.
Speed of Stirring: The speed of stirring should be optimum. It depends on the type of
machine/ method. In case of traditional method the optimum speed is about 100 rpm
where as in continuous systems it depends upon the type of machine used (it is slightly
more). The optimum speed of stirring prevents burning of milk solids and helps in
developing desirable body and texture in khoa. Low speed results in to the burning of
khoa. Higher speed makes the product pasty and sticky.
The changes in physico-chemical characteristics of milk during khoa making take place
due to three actions. 1) concentration 2) heating and 3) Stirring and scraping
1) Change of state
The removal of moisture from milk results into concentration of milk solids. This
eventually changes the state of milk from liquid to solid/ semisolid. All the constituents
including lactic acidity increase in proportion to the degree of concentration. pH
decreases.
3) Coagulation of casein
Due to the combined action of heat and concentration coagulation of casein tends to
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increase logarithmically with milk solids concentration and forms a complex with
denatured whey protein.
Free fat formation: (Free fat in khoa is 60% of the total fat in khoa, Cow khoa = 50%
of the total fat). By vigorous stirring and scraping, the fat globule membrane ruptures,
thereby releasing considerable amount of free fat in khoa.
Change in colour intensity: The colour of khoa becomes intense with brownish tinge
due to formation of melanoiodins pigment. The browning reaction is maillard type
reaction due to interaction between aldose group of lactose and free amino group of
casein.
Increase in iron content: From 2 to 4 ppm iron content in milk, the iron content of
khoa increases more than 100 ppm due to the incorporation of additional quantities of
iron from the karahi and the khunti by vigorous scraping.
Moisture: Loss of moisture takes place resulting into dry and hard surface of khoa. The
extent of evaporation however depends on the temperature of storage and packaging
material. The higher the storage temperature the higher is the rate of evaporation. More
the water vapour transmission rate (WVTR) of package faster the loss of water from
khoa. Minimum loss of moisture takes place in case of tins and maximum loss in
parchment paper.
Acidity: Lactic acidity increases with the storage period. Higher percentage increase take
place at higher temperature and vice-versa. The pH normally decreases during storage
corresponding to the increase in acidity.
Deterioration in fat: The peroxide value increases due to oxidative spoilage during
storage of khoa, particularly at ambient temperature. The hydrolytic rancidity in khoa take
place thereby increasing the free fatty acids measured as % oleic acid.
Breakdown in milk protein: There is break down of milk protein in khoa as recorded by
the increase in tyrosine value.
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Changes in organoleptic quality: The changes in organoleptic quality of khoa during
storage include development of off flavour (stale, sour, oxidized, etc) hardening of body
and texture and increase in intensity of colour.
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PANEER
Chemistry of Milk Coagulation During Paneer Production
Paneer prepared from buffalo milk possess desirable frying properties, body and texture as
compared to cow milk. The cow milk paneer is soft, weak and fragile and during cooking it
tends to disintegrate. However, cow milk and buffalo milk mixed in equal quantity yields
better product than cow milk. Paneer made from skim milk has chewy and rubbery texture
and hard body.
(2) Quality of milk
Milk must be fresh and free from off falvour. Growth of psycrotrophic organisms should be
minimized to restrict the off-flavour development. Acidic milk having a titratable acidity of
more than 0.20% lactic acid yields a product of inferior quality. Milk with COB positive and
low acidity (sweet curdling) is not suitable for paneer making. Paneer made from such milk
has weak body and texture, more moisture, acidic smell and not safe for human
consumption.
(3) Type, strength and temperature of coagulant
Product yield and moisture retention are directly influenced by the type and concentration of
the acid and the mode of delivery and blending into the hot milk. Citric acid is generally used
as a coagulant. Lemon or lime juice or vinegar imparts a typical flavour to the product. 1%
solution of citric acid yields good quality of paneer. Sufficient acid is added gently but
quickly blended with the milk (within one min) to reach optimum pH of coagulation.
Normally 1.8 to 2.0 kg citric acid is required for coagulating 1000lit of milk. High acid
concentration imparts acidic flavour, hardness and causes greater solids loss. Whey cultured
with Lactobacillus acidophilus at a level of 2% and incubated overnight at 37 OC can be used
as a substitute for citric acid. However acidic whey must be heat treated to destroy these
lactic organisms before use to prevent loss of shelf life of paneer. Coagulation temperature
influences the moisture content of paneer. It is reported that an increase in temperature from
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60 OC to 86 OC decreases the moisture content from 59 to 49%. However, optimum
coagulation temperature for best organoleptic and frying quality product is 76 OC.
(4) Heat treatment of milk
This is one of the technological requirements of the process which affects the sensory and
microbiological quality of paneer. The objective of heating milk is to prepare it for rapid iso-
electric precipitation, control the moisture content, develop typical body and texture, create
conditions conducive to the destruction of pathogenic and other microflora present in milk
and ensure safety as well as keeping quality of the final product. The milk is heated to 90 OC
without holding or 82 OC for 5min in order to maximize the total solids recovery. Whey
proteins especially β-lactoglobulin and α-lactalbumin form a complex with Қ-casein and
retained with the curd thus increasing the yield of the product. The high heat treatment
imparts desirable cooked flavour by controlled liberation of sulphydryl compounds.
(5) Coagulation temperature
It influences the moisture content of paneer. An increase in temperature from 60 OC to 86 OC
decreases the moisture in paneer from 59 to 49%. At 70 OC, paneer made from buffalo milk
has the best organoleptic and frying quality in terms of shape retention, softness and
integrity.
(6) pH of coagulation
The optimum pH of coagulation of milk at 70 OC is 5.30-5.35 for better product quality and
maximum recovery of solids when made from buffalo milk. The moisture retention in paneer
decreases with the reduction in pH and consequently the yield also decreases. At pH more
than 5.35 the paneer is very soft with fragile and crumbly body. Optimum pH for paneer
preparation from cow milk is 5.2.
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CHHANA
Factors influencing quality of chhana
(1)Type of milk
Cow milk produces chhana with moist surface, light yellow colour, soft body, smooth
texture and mildly acidic flavour which is more suitable for sweet preparation than buffalo
milk chhana. Buffalo milk produces chhana with hard body and coarse texture, with white
colour and greasy surface. Sweets prepared from buffalo milk chhana are hard, coarse and
less spongy. Colostrum milk produces pasty Chhana with deeper yellow colour and
unsuitable for rasogolla production.
(2)Quality of milk
1.Fat level
Minimum 3.5 to 4% fat in cow milk and 5% fat in buffalo milk gives a satisfactory body and
texture in chhana. Lower than 3.5% fat leads to hard body and coarse texture while higher
fat level results in greasy surface.
2. Acidity
Acidic milk produces chhana with sour smell and bitter taste hence unfit for sweet making.
Addition of neutralizer to slightly acidic milk helps in getting chhana suitable for sandesh
and not for rasogolla. Milk with 0.25-0.28% LA can be used by adding 0.2% Sodium Citrate
followed by thorough washing of the coagulum.
Organic acids, like citric acid, lactic acid or sour whey are normally used. Lactic acid
produces granular chhana suitable for rasogolla making. Citric acid gives pasty texture
suitable for sandesh making. However, dilute solution of citric acid can also be used for
making chhana suitable for rasogolla. Sour whey with (0.9% LA) can also be used for
producing good quality chhana. Calcium lactate produces chhana with bright white colour,
soft body and smooth texture and pleasant flavour and most suitable for sandesh making.
2. Strength
Low acid strength (0.5%) results in very soft body and smooth texture suitable for rasogolla
but unsuitable for sandesh making. The optimum strength of coagulant should be between
0.5 to 0.8% citric or lactic acid to produce good quality chhana suitable for making both
rasogolla and sandesh. However, calcium lactate of 4% solution produces most satisfactory
quality chhana.
3.Quantity
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The quantity of coagulant required is dependent on the type of milk. Generally, 2 to 2.5 g of
citric acid per kg of fresh milk and 2.5 to 3.9 gm of lactic acid and 6 to 12 gm of calcium
lactate per kg are required individually for complete coagulation.
4.Temperature and pH of coagulation
As the coagulation temperature decreases, the moisture content of chhana increases resulting
in softer body and smooth texture. Higher coagulation temperature imparts graininess and
hardness to chhana. Optimum coagulation temperature of cow milk is 80 to 85 OC and pH is
5.4 and that of buffalo milk is 70 to 75 OC and pH is 5.7.
Higher speed of stirring during coagulation reduces the moisture content of chhana and
increases its hardness, optimum speed is 40-50 rpm.
6. Method of Straining
Delayed straining produces a soft and smooth texture chhana than immediate straining.
Delayed straining gives a higher proportion of moisture, yield, recovery of milk solids and
lower hardness. Delayed straining is recommended for buffalo milk.
The recovery of milk solids and yield of chhana is influenced by the heat treatment given to
milk prior to acidification. The heat treatment prior to acidification involves temperature to
which milk is heated, the rate of heating, temperature to which milk is cooled and the rate of
cooling. Several heat induced changes occur during heating; denaturation of whey proteins
and their subsequent association with casein micelles, precipitation of calcium phosphate
onto the casein micelles and dissociation of κ-casein from the micelle. The degree of
denaturation of whey proteins depends on time temperature combination during heating and
is mainly determined by maximum temperature to which milk is heated. Whey protein
denaturation at above 70 OC is two step process, first an infolding of whey proteins takes
pace followed aggregation. α-lactalbumin shown the higher resistance to denudation and it
reported that 95 OC temperature denaturates all the whey proteins.
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CHEMISTRY OF CHEESE
Milk-clotting Enzymes from Plants
Enzymes from many plant sources may be used as clotting enzymes in cheesemaking but
most of the plant proteases are strongly proteolytic and cause extensive digestion of the curd,
resulting in reduced yields, bitter flavors and pasty-bodied cheese.
1.Papain
The latex of the plant Carica papaya yields papain and several other proteases. It has
powerful milk clotting activity but it is also highly proteolytic. It requires a free sulfhydryl
group for its catalytic activity.
2.Ficin
Ficin is present in the latex of several species of the genus Ficus (fig) such as Ficus
glomarata, Ficus religiosa and Ficus carica but the best source is Ficus carica. Cheese made
with ficin develops bitter flavor which decreases in intensity during curing.
3.Others
Bromelain from pineapple has also been considered as a possible substitute for calf rennet.
An enzyme extracted from Withania coagulans was also used in the manufacture of Surati
and Cheddar cheese. Extracts from the flower petals of Cynara cardunculus were used for
the manufacture of Serra cheese from sheep’s milk by Portuguese farmers.
4.Microbial Rennet
A large number of microorganisms are known to produce milk clotting enzymes. The
possibility of a few of the microorganisms proving successful as rennet substitutes may
appear from the fact that they play an important part during the manufacture of cheese.
Microbial enzymes are known to exhibit considerable variations in the range of activity,
substrate specificity and mode of action. Even more important is the fact that they can be
produced economically on any desired scale.
Many hundreds of bacterial and fungal cultures have been investigated for milk clotting
enzymes and their proteolytic abilities. Milk clotting enzymes from bacteria like
Streptococcus liquefaciens, Micrococcus caseolyticus, Bacillus cereus, B. polymyxa, B.
mesentericus, B. coagulans and B. subtilis have been used as coagulating enzymes. Milk
clotting enzymes from fungi are also used during cheese making. Some of the fungi
producing such enzymes are Aspergillus nidulans, A. galucus, Syncephalastrum racemosum,
and Cladosporium herbarum.
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Various strains of these organisms behave differently; therefore, the cheese maker should use
only well tried and tested rennet for the types of cheese contemplated. The activity of various
microbial rennets varies according to pH and enzyme system.
The protease of the Mucor miehei coagulants degrade casein fairly rapidly in the pH range
5.5-7.0; but inspite of this, the incidence of bitter cheese using this enzyme is low. The
enzyme is very sensitive to temperatures in the region 37-45°C and is destroyed at 70°C.
This enzyme is used successfully for many types of cheese.
Mucor pusillus extract is also used as microbial rennet. It is highly proteolytic than calf
rennet or the Mucor miehei extract. An increase in calcium ion concentration in milk
decreases the clotting time but activity of this enzyme is not so pH-dependent as for other
coagulants. It tends to give hard curds because of its high proteolytic activity and the curd
tends to lose fat into the whey, thereby giving lower yield as compared to others. Thus, this
enzyme is usually used in combination with other enzymes.
The enzyme extracted from Endothia parasitica is more caseolytic than those from Mucor
sp. or calf rennet and tends to produce more bitter flavors in high moisture cheese.
Continuous research is being carried out in exploring the milk coagulating activity of
enzymes from different cultures. Recently, commercial starter ‘natto’ (Bacillus subtilis) has
been studied for its milk clotting activity and it was found to be a potential rennet substitute.
5.Recombinant Chymosin
many rennet substitutes are used for cheesemaking but many of these proteolytic enzymes
from microbial or plant origin cause flavor, texture and yield changes in certain types of
cheese that are different than those produced by calf rennet. Further, they are not suitable for
long ripening cheeses as they have a different range of non-specific activities than chymosin
and do not produce the correct flavors on prolonged ripening.
In addition to the benefit that such chymosin can be produced in large-scale fermentors at
low cost, recombinant and highly pure chymosin also has some other advantages such as
specific, low proteolytic activity, predictable coagulation behavior and vegetarian approval.
With the advent of various sources of rennet substitutes, a number of firms are
manufacturing these substitutes at commercial level. Among these microbial rennet is most
widely used.
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Enzymatic Coagulation of Milk
The enzymatic coagulation of milk is essentially a two stage process (Fig. 16.3). As
discussed earlier, the casein micelle is stabilized by κ-casein layer on the surface of the
micelle. The enzymes present in rennet (proteinases) hydrolyse κ-casein layer to form
paracasein micelles which aggregate in presence of calcium and thus milk is coagulated. The
hydrolysis of the κ-casein layer is called as the primary phase of rennet coagulation while the
aggregation of paracasein micelles in presence of calcium is called the secondary phase of
rennet coagulation of milk.
RENNET
CASEIN PARA-K- CASEIN + GLYCOMACROPEPTIDES
The amino acid chain forming the κ-casein molecule consists of 169 amino acids. Rennet
enzymes act specifically at 105 (phenyl alanine)-106 (methionine) bond of this amino acid,
thereby splitting it into two parts. One part consists of amino acids from 1-105, called as
para-κ-casein. This part is insoluble and remains in the curd together with αs and β-casein.
The other part of amino acids from 106-169 is soluble part. These amino acids are dominated
by polar amino acids and the carbohydrate, which gives this part its hydrophilic properties.
This part of the κ-casein molecule is called the glycomacro-peptide and is released into the
whey in cheesemaking.
The formation of the curd is due to the sudden removal of the hydrophilic macropeptides and
the imbalance in intermolecular forces caused thereby. Bonds between hydrophobic sites
start to develop and are enforced by calcium bonds which develop as the water molecules in
the micelles start to leave the structure. This process is usually referred to as the phase of
coagulation and syneresis. Hydrolysis of κ-casein during the primary phase of rennet action
releases the highly charged, hydrophilic C-terminal segment of κ-casein (macropeptide), as a
result of which the zeta potential of the casein micelles is reduced from -10/-20 to -5/-7 mV
and the protruding peptides are removed from their surfaces, thus destroying the principal
micelle-stabilizing factors (electrostatic and steric) and their colloidal stability. When
roughly 85% of the total κ-casein has been hydrolyzed, the stability of the micelles is
reduced to such an extent that when they collide, they remain in contact and eventually build
into a three-dimensional network, referred to as a coagulum or gel.
The primary and secondary phase of rennet coagulation are affected by some of the
compositional and environmental factors like milk composition, temperature, pH, calcium
content, pre-heating of milk, rennet concentration etc. The effects of all these factors are
summarized here.
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1.Composition of milk
Variation in the composition of milk mainly affects the rate of coagulation and the curd
firmness. Fast coagulation results in firmer curd. The rate of clotting is largely dependent on
the nature of the casein micelles and the equilibrium with the calcium phosphate and calcium
ions. The firmness of the curd are affected by pH value, calcium concentration, temperature,
fat content and the ratio of rennin to casein. The rennet coagulation time (RCT) is markedly
affected by the protein content in milk. RCT decreases with protein content in the range of 2-
3%. Further increase in milk protein level i.e. more than 3% result in a slight increase in
gelation time. This is due to decrease in rennet:casein ratio, which necessitates an increase in
the time required to generate sufficient hydrolysis of κ-casein to induce aggregation of
paracasein micelles. A minimum protein content of 2.5-3.0 is necessary to obtain gel in
about 30-40 minutes during cheesemaking. Increase in fat content also results in decreased
RCT but the effect is lower than that of the protein content.
Heating milk to pasteurization temperature has beneficial effect on rennet coagulation due to
heat induced precipitation of calcium phosphate and a concomitant decrease in pH. But
heating further to higher temperatures causes other effects which in combination dominate
the positive effects of heating to pasteurization. Some such effects are:
• Whey protein denaturation and the interaction of denatured β-lactoglobulin with micellar κ-
casein
3.Set temperature
The principal effect of set temperature is on the secondary phase of enzymatic coagulation,
which does not occur at temperatures below around 18°C. Above this temperature, the
coagulation time decreases to a broad minimum at 40-45°C and then increases again, as the
enzyme becomes denatured. In cheesemaking, rennet coagulation normally occurs at around
31°C. This is necessary to optimize the growth of starter bacteria which will not survive the
temperature more than 40°C. In addition, the structure of the coagulum is improved at the
lower temperature, which is therefore used even for cheeses made using thermophilic
cultures.
4.Rennet concentration
The rate of enzymatic coagulation is directly related to the concentration of enzyme. Increase
in concentration of rennet decrease RCT. During cheesemaking, rennet is added in such a
concentration so as to coagulate the milk 30-40 minutes. More rennet concentrations can be
used to shorten the coagulation time but it leads to retention of more rennet in the curd which
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has pronounced effect in ripening of the cheese, particularly proteolysis. Some studies also
suggest that using increased concentration of rennet may jeopardize the curd firming rate and
curd firmness.
The concentration of calcium ions mainly affect the secondary phase of enzymatic
coagulation. Increased calcium concentration is beneficial for coagulation of milk. For this
reason, sometimes CaCl2 is added to milk prior to cheese making. This promotes cheese
making via three beneficial changes, viz. an increase in calcium ion concentration, an
increase in the concentration of colloidal calcium phosphate and a concomitant decrease in
pH (the addition of CaCl2 to 0.02%, i.e. 1.8 mM Ca, reduces the pH by ~ 0.05-0.1 units,
depending on protein level).
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CHEMICAL, PHYSICAL, MICROBIOLOGICAL AND SENSORY
CHANGES
Cheese Ripening
Unique characteristics of each cheese variety are determined by the curd manufacturing
operations but these characteristics are largely developed during ripening process. For
example, the type of microflora established in the curd is determined by the
manufacturing process but its effect on cheese characteristics develop largely during the
ripening process.
Ripening involves microbial and chemical changes which are responsible for
development of typical characteristics of varieties of cheeses. Microbial changes involve
death and lysis of the starter cells, development of non-starter microflora and growth of
secondary microflora. Ripening usually causes softening of the cheese texture due to
hydrolysis of the casein matrix, change in pH and change in water binding ability of the
curd. Flavor production is largely described by a series of biochemical events taking
place during ripening.
The primary events occuring during cheese ripening are metabolism of residual lactose,
lactate metabolism, proteolysis and lipolysis. These reactions are mainly responsible for
textural changes and development of flavor in cheese. However, many secondary
changes occur simultaneously and modify cheese texture and flavor. Since the
biochemistry of cheese ripening is complex, the objective of this chapter is to present an
overview of the principal biochemical pathways contributing towards cheese ripening.
Lactic acid bacteria (LAB) is added in the form of starter culture to cheese metabolize
lactose to lactate. The rate and extent of acidification influence texture of the curd by
controlling the rate of demineralization. The pH of the cheese curd is largely determined
by the extent of acidification during manufacturing process. This influences the
solubility of the casein, which in turn affects the texture of curd. pH also affects the
activity of enzymes involved in ripening, thereby having an
indirect effect on cheese texture and flavor development.
Most of the lactose is lost in whey during cheese manufacturing. However, low levels of
lactose remains in the curd. This residual lactose is converted to L-lactate during early
stages of ripening by the action of starter bacteria. The rate of conversion is dependent
on temperature and salt-in-moisture levels of the curd. Starter activity is stopped very
quickly at the end of manufacturing operations due to low pH, salt addition and lesser
amount of fermentable lactose. Lactose that remains unfermented by the starter is
probably metabolized by non-starter lactic acid bacteria (NSLAB) flora present in curd
and they convert the residual lactose to D-lactate. D-lactate can also be formed by the
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racemisation of L-lactate.
Lactate Metabolism
Lactose can be metabolized to acetate, ethanol, formate and CO2 depending on the
population of NSLAB and availability of O2. In cheese wrapped with film, oxidation of
lactate occurs to a lesser extent due to low level of O2 available.
The above mentioned metabolisms contribute negatively towards cheese ripening. There
are some positive contributions also of lactate metabolism. This is essential for cheese
varieties characterized by the development of large eyes during ripening such as
Emmental cheese. Propionibacterium freudenrichii metabolise lactate to propionate,
acetate, CO2 and H2O. Propionate and acetate contribute to the flavor of cheese while
CO2 is mainly responsible for eye formation.
Lipolysis
Milk fat is essential for the development of the correct flavor in cheese during ripening.
Cheddar and other cheeses normally made from whole milk do not develop correct
flavor when made from skim milk or milks in which milk fat has been replaced with
other lipids. Lipids may undergo oxidative or hydrolytic degradation in foods but the
redox potential of cheese is very low, so mainly hydrolytic degradation of lipids takes
place in cheese. The triglycerides present in cheese are hydrolyzed by lipases which
result in the formation of fatty acids.
• Rennet
• Starter culture
• Starter adjuncts
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• Non starter bacteria (may come through ingredients or contamination)
Low level of lipolysis is required for the development of flavor of cheese but excessive
lipolysis causes rancidity. Lipolysis of milk fat results in production of free fatty acids
which contribute to the flavor of cheese and also act as precursors for development of
other flavor compounds in cheese like esters, lactones, ketones and aldehydes. These
secondary fat-derived compounds can be very potent flavor compounds.
Fatty acid esters are produced by reaction of fatty acids with an alcohol; ethyl esters are
most common in cheese. Thioesters are formed by reaction of a fatty acid with a thiol
compound formed via the catabolism of sulphur-containing amino acids. Fatty acid
lactones are formed by the intramolecular esterification of hydroxyacids; γ- and δ-
lactones contribute to the flavor of a number of cheese varieties. n-methyl ketones are
formed by the partial β-oxidation of fatty acids.
Liberation of short and medium chain fatty acids from milk fat by lipolysis contribute
directly to cheese flavor. This degree of flavor development depends on the variety of
cheese. For example, it is very extensive in some hard Italian varieties, smear cheeses
and blue mold cheeses. Excessive lipolysis causes rancidity in cheese varieties like
Cheddar and Gouda.
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Production of flavor compounds from fatty acids during cheese
ripening:
Proteolysis
Proteolysis is the most important and complex of all the events during ripening of cheese.
The extent
and pattern of proteolysis is also used as an index of cheese ripening and quality of cheese.
Proteolysis contributes significantly towards development of texture and flavor in cheese.
Textural changes (softening of cheese curd) occur due to breakdown of protein network
and release of carboxyl and amino groups resulting in the binding of more water and thus
decrease water activity (aw). Proteolysis leads to the formation of peptides and free amino
acids which contribute to cheese flavor. These amino acids also act as precursors for many
reactions like transamination, deamination, decarboxylation, desulphuration, catabolism of
aromatic compounds such as tyrosine, phenylalanine, tryptophan, etc. and generate many
important flavor compounds. Proteolysis in cheese is catalysed by proteinases and
peptidases and they originate from the following sources:
• Coagulant
• Milk
• Starter LAB
The final products of proteolysis are amino acids, the concentration of which depends
on the cheese variety. The concentration of amino acids in cheese at a given stage of
ripening is the net result of the liberation of amino acids from the caseins by proteolysis
and their catabolism or transformation into other amino acids by the cheese microflora.
Medium and small peptides contribute to a brothy background flavor in many cheese
varieties; short, hydrophobic peptides are bitter. Amino acids contribute directly to
cheese flavor as some amino acids taste sweet (e.g. Gly, Ser, Thr, Ala, Pro), sour (e.g.
His, Glu, Asp) or bitter (e.g. Arg, Met, Val, Leu, Phe, Tyr, Ile, Trp).
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Proteolysis in cheese during ripening
Microorganisms including bacteria, yeasts and molds are present in cheese and
contribute to the ripening process through their metabolic activity. The enzymes released
by these microorganisms also add to the various metabolic activities like proteolysis,
glycolysis and lipolysis.
Microorganisms in cheese may gain entry through their intended addition in the form
of starter culture and they may be associated with the ingredients used in cheese
making. The microflora associated with cheese ripening may be divided into two groups
- the starter bacteria and non-starter bacteria. Starter bacteria are primarily responsible
for acid production during manufacture to reduce the pH of milk to the desired level.
The secondary microflora do not play any active role during cheese manufacture but
contribute to the ripening process.
The factors controlling the growth of microorganisms in cheese include water activity,
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concentration of salt, oxidation-reduction potential, pH, ripening temperature, and the
presence or absence of bacteriocins (produced by some starters).
Water activity
Water activity (aw) is defined as the ratio of the vapor pressure of water in a material (p)
to the vapor
pressure of pure water (po) at the same temperature. Its value ranges from 0 to 1.0. It
expresses the water availability rather than total water present in the system. Water
activity of cheese reduces during ripening process. This may be due to several reasons
like:
• Hydrolysis of proteins to peptides and amino acids and of lipids to glycerol and fatty
acids
• The salt and organic acids (lactate, acetate, and propionate) dissolved in the
moisture of the cheese reduce the vapor pressure
The salt normally used in cheese making is about 2% of the weight of the curd. Salt is
added to cheese mainly to suppress growth of unwanted microorganism and to assist the
physico-chemical changes in the curd. The growth of unwanted microorganisms is
essentially curbed by reduction in aw as salt act as a humectant.
Oxidation-Reduction potential
pH
Most bacteria require a neutral pH value for optimum growth and grow poorly at pH
values below
5.0. The pH of cheese curd after manufacture generally lies within the range 4.5-5.3, so
pH is also a significant factor in controlling bacterial growth in cheese. LAB, especially
lactobacilli, generally has pH optima below 7, and Lactobacillus spp. can grow at pH
4.0. Most yeasts and molds can grow at pH values below 3.0, although their optimal
range is from 5 to 7. B. linens, an important organism in smear-ripened cheese, cannot
grow below pH 6.0. Micrococcus spp., which are commonly found on the surface of
soft cheeses, cannot grow at pH 5 and only slowly at pH 5.5.
Temperature
development of typical flavor, body and texture of cheese. Ripening temperature for
Cheddar cheese is 6-8°C while Camembert and other mold-ripened cheeses are ripened
at 10-15°C. Emmental cheese is ripened initially for 2-3 weeks at a low temperature (~
12°C), after which the temperature is increased to 20-24°C for 2-4 weeks to promote the
growth of propionic acid bacteria and the fermentation of lactate to propionate, acetate,
and CO2. The temperature is then reduced again to around 4°C. Use of higher ripening
temperature is one of the techniques used for accelerated ripening of cheese but it also
stimulates the growth of other microorganisms present in cheese.
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PHYSICO-CHEMICAL CHANGES TAKES PLACE DURING MANUFACTURING
OF CONCENTRATED MILKS
Introduction
In course of manufacture of concentrated and dried milks, raw milk is subjected to various
pretreatments, which in turn determine to a great extent, the physical, chemical, microbiological
and organoleptic characteristics as well as the shelf life of the finished product. The
technological aspects of various pretreatments and their significance in the manufacture of dried
milks are discussed here.
The following pretreatments are given to milk during the processing schedule:
2. Standardization
3. Forewarming /Preheating
5. Homogenization
Filtration
The basis for high quality and fine flavor of the product is "clean milk" in preference to "cleaned
milk". However, for sanitary, ethical as well as for technological reasons the milk that is
received at the dairy is filtered and/or centrifuged.
Weigh can strainers, strainers and filters in the milk line or a duplicate filter unit with by-pass
connection are general filtration techniques. Bactocatch method developed by Alfa-Laval Co.,
Sweden, involves filtration of the milk through ceramic filters prior to pasteurization. This
microfiltration technique removes 99.6% of the bacteria in the milk so that the following normal
low pasteurization results in 50% life extension when milk is kept at 8°C. The advantages of this
process are:
Economical
Excellent quality low heat powder for cheesemaking, least adverse effect on rennetability,
curd characteristics etc.
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Centrifugation
There are three types of centrifugal processes to which milk may be subjected during
manufacture of dried milks. These are
Clarification
Bactofugation
2. Improved shelf life of powder due to reduced tendency of oxidation and lipolysis due to
removal of slime, foreign materials (which may act as chemical reaction catalyst),
leucocytes, lipolytic bacteria and enzymes etc.
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6. Improved bacteriological quality of finished product.
Standardization
Milk intended for dry milk manufacture is standardized to obtain a product of expected
quality, to meet the legal standards and to optimize yield and profit.
In manufacture of dried milks, the milk fat and SNF are so standardized that the finished
product will meet the standards of not less than 26% fat (BIS, IDF and ADPI standards
for whole milk powder).
The fat to SNF ratio adjustment is done by addition of calculated amount of cream or
skim milk to the milk. This purpose is accomplished in the present day industry by use of
tri-purpose separator which has the standardizing device too. Other computerized systems
are also used commercially.
Preheating of milk to at least the boiling temperature of the first effect evaporation is essential,
so that evaporation can start immediately the milk enters the heating tubes. The most common
boiling temperatures of the first effect in the food industry are between 40-100°C. Heating of
milk to a temperature exceeding the boiling temperature of the first effect are required for the
purpose of:
(b) Pasteurization effect - improved microbiological quality of resultant product due to microbial
inactivation. Heat treatment employed in manufacture of low and high heat powders had
profound effect on bacterial profile. Both pasteurization and high heat treatment (90°C, 10 min)
almost completely eliminate psychrotrophic bacteria. Pasteurization had little effect on either
thermoduric or spore counts whereas high heat treatment brought about significant reduction in
bacterial numbers.
(c) To lengthen the running time of evaporators (as most of the whey proteins are denatured
when milk is preheated before evaporation).
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(d) To generate specific properties in the resultant milk powders, e.g. heat stability, viscosity,
etc. by altering the characteristics of some of the components of milk such as casein, whey
protein, mineral balance etc.
(e) To improve oxidative stability of whole milk powder during storage. This is due to
production of -SH groups and other reducing substances in milk on account of heating.
The actual treatment required depends on many factors, including the composition of milk as
influenced by the breed, season, climate etc. and the equipment including type and construction
of heater. The influence of spray drying on WPNI is negligible.
The viscosity of the concentrate has bearing on drying efficiency as well as certain properties of
the dried milks. In general, high concentrate viscosity can be the source of many practical
problems by increasing the likelihood of blockage of feed lines and in the calandria of
evaporators.
(a) Saving of energy as it is more efficient to heat the concentrate by means of steam or hot
water than to use heat from the air supplied to the dryer. The evaporation capacity of the dryer is
increased by ~ 5% when the concentrate is supplied to the atomizer at 70°C instead of 50°C.
(b) The average size of the droplets into which the concentrate is atomized is reduced due to the
lower viscosity. This facilitates the drying making it possible to reduce the air outlet temperature
and still maintain the specified moisture content of the powder. The lower outlet temperature
results in increased capacity and gentler drying which results in improved powder quality -
especially solubility.
(c) As the temperature conditions in the last stages of the evaporator and in the feed tank for the
dryer can be favorable for growth of micro organisms, heat treatment of the concentrate
immediately before drying will contribute to safeguard the bacteriological quality of the powder.
Heating of the concentrate must be done in such a way that no holding takes place, i.e. the
concentrate heater must be placed immediately before the atomizer. This is necessary in order to
avoid the so called "age-thickening" which occurs very rapidly at temperatures above 60°C. The
time dependent thickening of hot concentrate is irreversible and results in very high viscosity.
Table 4.3 shows changes in viscosity of concentrated skim milk (39%TS) held for varying
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period at 75°C. Table 4.4 shows the effect of storing concentrated skim milk (39%TS) at 50°C
and 60°C on powder solubility. Since concentrate is a complex system its heating has to be done
carefully to minimize adverse effects of heating on chemical and physical characteristics of the
concentrate. Otherwise, such change will reflect on the quality of resultant milk powders. Tables
4.5 and 4.6 show influence of concentrate heating on the various characteristics of whole milk
powder.
Homogenization
The purpose of homogenizing milk/concentrate prior to spray drying is to reduce the size
of the fat globules and consequently to change the physical structure in such a way that
the dried product obtained has a low free fat content.
The type of homogenizer, the stage at which product is homogenized, the temperatures
and pressures of homogenization employed have profound effect on the various
properties of the concentrate and this in turn have influence on the quality of resultant
milk powders.
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PHYSICO-CHEMICAL CHANGES TAKES PLACE DURING
MANUFACTURING OF CONDENSED MILK
Introduction
Concentrated milks are liquid milk preserves with considerably reduced water content. Water is
removed by evaporation. Preservation is achieved either by sterilization, leading to a product
called evaporated milk , or by creating conditions that do not allow growth of microorganisms.
The latter is generally realized by addition of a large quantity of sucrose and exclusion of
oxygen. The resulting product is called sweetened condensed milk .
These products were initially meant for use in regions where milk was hardly or not available.
The milks were packaged in small cans. The contents were often diluted with water before
consumption to resemble plain milk. Currently, alternative products are used more often, such as
whole milk powder or recombined milk. For the concentrated milks, some alternative forms of
use are developed, and processing and packaging have been modified. The consumption of
sweetened condensed milk has greatly declined.
Product Properties
● Maillard reactions are of paramount importance for the flavor and color of evaporated milk.
The temperature and duration of the heat treatment during manufacture determine the initial
concentration of the reaction products, but ongoing Maillard reactions occur during storage,
especially at a high temperature. The milk eventually develops a stale flavor also due to Maillard
reactions. The flavor after a long storage time differs considerably from that directly after
intense heating. This is because the complicated set of reactions involved leads to different
reaction products at different temperatures. A sterilized milk flavor may be appreciated by some
people when the milk is used in coffee. Off-flavors due to autoxidation need not occur.
● When the milk is used in coffee, the brown color is often desirable to prevent the coffee from
acquiring a grayish hue. The brown color depends greatly on the Maillard reactions, although
the color of the fat plays a part.
2.Viscosity
The viscosity of evaporated milk is often considered an important quality mark. Many
consumers prefer the milk to be viscous. However, it should pour as like thin cream. This can be
achieved by sterilization in such a way that visible heat coagulation is barely prevented. UHT
evaporated milk is always less viscous and, therefore, κ -carrageenan is often added.
3.Age thinning
If the original milk contains bacterial lipases and proteinases due to growth of psychrotrophs,
these enzymes may remain active in the evaporated milk and lead to strong deterioration, i.e.,
soapy-rancid and bitter flavors, and to age thinning. Evaporated skim milk may even become
more or less transparent due to proteinase activity.
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4.Nutritive value
The nutritional value of evaporated milk can be significantly decreased as compared to that of
plain milk. In-container sterilization can destroy up to 10% of the available lysine, about half of
the vitamins B1, B12, and C, and smaller proportions of vitamin B6 and folic acid. All of these
changes are far smaller when UHT heating is applied.
The nutritive value of the sweetened and unsweetened condensed milk is very high. Both of
them are rich in fat and fat soluble vitamins viz. A, D, E & K and body building proteins, bone
forming minerals and energy giving lactose. While sweetened condensed milk is especially high
in energy giving sucrose because of the added sugar, evaporated milk is suitable for infant
feeding since it makes a soft curd and is easily digested.
5.Heat Stability
Concentrated milk is very less stable during sterilization than non-evaporated milk, and the
fairly intensive homogenization applied decreases the heat stability further. Moreover,
evaporated milk should increase in viscosity during sterilization. Essentially, the viscosity
increases by incipient coagulation. A subtle process optimalization is needed to meet these
requirements.
Therefore, the milk must be preheated before evaporation in such a way that most serum
proteins are denatured. Otherwise, the evaporated milk forms a gel during sterilization due to its
high concentration of serum proteins. Preheating is, for example, for 3 min at 120°C.
6.Effect of stabilization
The pH should always be adjusted. Preheating and evaporation have lowered the pH to about 6.2
or 6.1, and that is far below the optimum pH. In practice, Na 2HPO4 . 12H2O is usually added,
but NaOH can also be used.
7.Effect of homogenization
UHT heating of evaporated milk after homogenization is not possible. Even traditional
sterilization is difficult if the milk is highly concentrated or if the evaporated milk is intensely
homogenized. There are some other factors affecting heat stability. It can be improved by
lowering the calcium content of the milk before evaporation by means of ion exchange.
Addition of 0.05% H2O2 or about 15 µ mol Cu2+ (from 0.5 to 1 mg . kg − 1 ) after preheating but
before evaporation tends to increase the heat stability.
8.Creaming
Creaming of evaporated milk eventually leads to formation of a solid cream plug that cannot be
redispersed. This may be due to bridging of adjacent fat globules because of ‘fusion’ of the
fragments of casein micelles in their surface layers. Accordingly, intensive homogenization is
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necessary. A higher viscosity of the evaporated milk often involves a slower creaming, but the
relations are not straightforward. Generally, a high viscosity is due to approaching heat
coagulation. The homogenized fat globules tend to participate in this coagulation and hence to
form clusters, which will cream rapidly. κ -carrageenan is often added to decrease creaming rate.
The homogenization has an adverse effect on the heat stability and, consequently, the
homogenization pressure should not be high. The largest fat globules exhibit creaming, and
therefore the aim should be to have the relative diameter of the globule size distribution as small
as possible. The width is greatly affected by the type of homogenizer used.
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AGE THICKENING AND GELATION OF CONDENSED MILK
Introduction
When evaporated milk is kept, its viscosity may initially decrease slightly. This may be
explained in terms of the casein micelle aggregates formed during sterilization which changes
from an irregular to a spherical shape, and as a result the effective volume fraction decreases.
Subsequently, the viscosity increases, and it becomes strongly dependent on the shear rate, the
milk displays a yield stress, and a gel is formed that firms rapidly.
Mechanism
The mechanism involved in the age thickening or gelation is not quite clear. However, in most
cases, gelation is not caused by proteolytic enzymes or Maillard reactions, although the latter
parallel the gelation. Also, gelation is not related to heat coagulation. It does not depend
significantly on the pH, and its rate increases rather than decreases after lowering of the calcium
content.
Electron microscopy reveals that thread-like protrusions appear on the casein micelles, which
eventually form a network. It is likely that a slow change in the micellar calcium phosphate is at
least partly responsible for the changes observed, but a definitive explanation is still lacking.
Age thickening and gelation occur faster in UHT-evaporated milk. It may then be due to
proteolysis caused by enzymes released by psychrotrophs, but also if such enzymes are absent,
fast age gelation occurs. A more intense sterilization after evaporation delays gelation whereas it
is faster in more concentrated milk and at a higher storage temperature.
Conventional evaporated milk only gels if kept for a long time at a high temperature. Extensive
Maillard reactions also occur. Rapid gelation can occur if the evaporated milk before its
sterilization is kept refrigerated at 4°C for a few days.
The sweetened condensed milk is highly concentrated. Its mass concentration ratio is very high
and because of this and the high sugar content, the product is highly viscous, i.e., η a is
approximately 2 Pa . s, about 1000 times the viscosity of milk. The product is somewhat glassy
in appearance because the fat globules show little light scattering as the refractive index of the
continuous phase is almost equal to that of fat. The turbidity of the product is largely due to
lactose crystals. Most of the lactose crystallizes because of its supersaturation.
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1.Viscosity
Viscosity, the most important property of recombined SCM, should be ~ 35 poise in fresh
product which can increase up to 3 times, yet giving good acceptance. Too low viscosity poses
air incorporation at filling and fat separation problems. Too high initial viscosity accelerates rate
of age thickening.
1. Manufacture,
3. Homogenization,
4. Pasteurization and
5. Storage temperature.
2.Colour
The color of recombined EM varies with use of anhydrous milk fat, powder and level of heat
treatment. Colour and flavour of recombined SCM are affected by raw materials used and severe
pasteurization conditions employed. Homogenization is found to lighten the colour.
3.Flavour
Flavour of the product can be improved by use of buttermilk powder due to higher
phospholipids content. Holding the product for some period, at least for 7 days after production
and before release, allows post manufacturing hydration of dry ingredients and normalization of
flavour characteristics.
The most preferred flavour in recombined WMP results when fresh whole milk, commercial
additives and fresh buttermilk powder contributing number of flavour compounds lost during
the preparation of anhydrous milk fat are included in the mix. Incorporation of distilled
monoglycerides or buttermilk powder provides best flavour stability on extended storage of
recombined WMP. Powders with moisture level below 3% provide best flavour initially and
during storage. Moisture content >5% leads to crystallization of lactose resulting in lumpy
powder, increased free fat and increase in colour development within 2-3 months.
4.Fat separation
The efficient homogenization, absorption of casein on fat globule, product viscosity and
minimum fat globule clustering controls the fat separation in recombined EM. High ambient
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temperature increases the defect. Addition of carrageenan gives best control of fat separation but
have greater tendency towards gelation. Formation of a stable fat globule from anhydrous milk
fat and SNF is very important for recombined evaporated milk.
Homogenization reduces fat globule size as well as increases viscosity thereby reduce fat
separation tendency. Commonly employed pressures are up to 10 MPa, about 3.5 MPa being
most common. Homogenization of reconstituted skim milk with milk fat (at 50 kg/cm 2 or 150
kg/cm2) increases viscosity, while recombined SCM made using recombined cream (0.7-0.9 %
protein, 20.2-20.9 % fat) age thickens slowly. Age thickening is also accelerated by higher
storage period and temperature as well as by higher proteins and lower whey protein nitrogen
with changed casein fraction. The pasteurization conditions can be used to control viscosity but
is less convenient to use.
5.Lactose crystallization
The second important quality determining factor for recombined SCM is lactose crystallization
which can be controlled by storage temperature and using dry seeding procedure.
High temperatures preheat treatment of milk, as part of manufacture of full-cream milk powder;
can reduce the susceptibility of product to oxidation during storage as a result of development of
sulfhydryl compounds. However, such heat treatment is not always compatible with the
development of required specific functional properties.
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PHYSICO-CHEMICAL CHANGES DURING MANUFACTURE OF CONDENSED
MILK-I
Introduction
There are numerous changes occurring in the condensed milks during their manufacture. They
are because of the inherent properties of the milks, any additives like sugars, stabilizers etc.
added and the processing variables. Some of the product specific changes of commercial
importance are discussed here.
Apart from the increase of most of the solute concentrations, removal of water from milk causes
numerous changes in properties, which often are approximately proportional to concentration
factor. The changes also depend on other conditions, such as heat treatment and
homogenization. Some important changes in properties are:
The Calcium ions activity increases only slightly because calcium phosphate, which is
saturated in milk, turns into an undissolved state. As the water content decreases,
association of ionic species increases and also ionic groups of proteins are neutralized.
The conformation of proteins changes because ionic strength, pH, and other salt equilibria
change. When milk is highly concentrated, the solvent quality decreases. Thus, the
tendency of the protein molecules to associate and to attain a compact conformation is
increased. Coalescence of casein micelles causes them to increase in size. This increase is
smaller if the milk has been intensely preheated, presumably because β-lactoglobulin and
other serum proteins have become associated with casein.
The viscosity increases and the liquid become non-Newtonian and finally solid-like.
Evaporated Milk
1.Viscosity
Viscosity is defined as resistance to the motion of the molecules of a fluid body among
themselves caused by internal frictions as opposed to mobility. This is measured by viscometer.
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Viscosity of fresh milk changes by the preheating of milk. The condensing operation causes a
slight but definite increase in viscosity. This is due to increase in concentration of milk solids.
The increase in viscosity that gives the finished product its full body, however occur during
process of sterilization. In general HTST yields a thin body and low viscosity, while LTLT
process yield a full body and little more viscosity.
In sterilization process, the rate of thickening is greatest, shortly before the occurrence of a
visible coagulation. It is observed that the thickening does not proceed rapidly until above 10
min before coagulation. This is because the thickening or increase in viscosity during
sterilization appears to be a part of the function of coagulation. Thickening in sterilization is in
fact the beginning of coagulation. It is very slow and gradual and in normal commercial process
of sterilization, covering a period of approximately 20 minutes at the full sterilizing temperature.
The proportion of milk proteins coagulated while sufficient to increase viscosity, is too limited
for curd to become visible. The increase in viscosity which milk undergoes toward the end of
sterilizing process has to do with progressive coagulation of the milk proteins. Table-13.1.
below shows the viscosity changes during successive steps in manufacture of evaporated milk:
It is observed further that for a heavy creamy body, the heat stability of milk should not exceed
30–40 minutes. Milks with heat stability in excess of 50 min will be exceedingly thin at the end
of sterilization at 115°C for 30 min unless an increase in solids content is depended upon to
build up body. The viscosity produced during sterilization is controlled mainly by the heat
stability of milk. Therefore, factors which affect the heat stability of milk will certainly affect
the viscosity of milk. Following factors gives low heat stability, high viscosity and very thick
body and vice-versa:
Consumer desires a product with a good body that suggests richness. The heat stability sufficient
to avoid visible coagulation or curdling during sterilization process is required but maximum
heat stability is not desirable because such high stability results into objectionably thin milk.
Evaporated milk becomes thinner with age. This loss of viscosity increases with the temperature
of storage. The decrease in viscosity begins immediately. The rate at which viscosity is lost is
accelerated at high storage temperature Thus it is observed that at or above 30°C, evaporated
milk looses as much as 40% of viscosity (original) during first 10 days of storage. While at
15.6°C or below, the age thinning is very slight. It is reduced after which the rate of thinning is
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much more gradual. Age thinning of evaporated milk may therefore be definitely retarded and
the attainment of final viscosity delayed by use of relatively low storage temperature. A study
shows viscosity loss upon storage for 110 days of 58.75% at 26°C, 40% at 15.6°C & 11.25% at
7.2°C. But this depends upon quality of raw material (milk) used. Better grade milk lost less
viscosity than the low grade initial milk with the same temperature and time of storage.
In case of some evaporated milks, the viscosity increases later in the storage period even to the
gel formation. This tendency is greatest with milks that had received relatively light heat
treatment and those of high solids concentration. These results of gel formation in prolonged
storage are supported by commercial experiences especially with samples with high TS
evaporated milks incubated at tropical temperatures.
Further it is observed that evaporated milks that have been sterilized by the HTST process
(135°C for 0.5 min) thicken quickly during storage. When the gel is broken before it becomes
firm, the product wheyed off. When sterilized in the conventional manner (115.6°C for 20 min),
gel formation is slow and holds the water better than from the HTST process. Since long fluidity
in storage is a marketable property of primary magnitude, it appears that the more severe heat
treatment of commercial process (115.6°C for 20 min) that retards thickening in storage is
commercially preferable to the less drastic treatment of momentary exposure to high sterilizing
heat.
Neither the mechanism underlying age thinning nor that responsible for age thickening appears
to be well understood. It may be due to insufficient time for the attainment of new solubility
equilibrium of the Calcium and Magnesium salts when using HTST method of sterilization.
When solutions of these salts are heated, it takes considerable time to attain that. Their
peculiarity of being less soluble at higher temperature may be contributing to the reaction of
these salts.
In the HTST method of sterilization, conditions are thus less favorable than those of the LTLT
procedure (115.6°C for 20 min). This suggests the possibility that, less of Ca and Mg content is
rendered insoluble. This condition might encourage the protein particles to swell and to form a
gel or it may be as low continuation of the coagulation process accompanied by an operation of
caseinate molecule which finally produces an irreversible gel structure.
The proteins of some evaporated milks have a tendency to settle during storage. This is found
more common in evaporated skim milk than evaporated whole milk. Homogenization retards
protein separation in evaporated whole milk. It is observed that, fat in evaporated milk is a factor
to maintain a normal dispersion of milk constituents during long period of storage. It is observed
in this respect that fat acts to counter balance the protein settling to bottom.
Our aim is to get Evaporated Milk of good body and to avoid fat separation. During age thinning
and before age thickening sets in, there is definite tendency to objectionable fat separation. This
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tendency emphasizes importance of efficient homogenization that ensure reduction of at least
90% of fat globules to 2 µ or smaller. Such efficiency can be obtained by taking following care:
Keeping the clearance surface of valve and valve seat smooth and intact by regrinding or
resurfacing
It is observed that HTST sterilization provides little opportunity to control body hence through a
heavier body, control of the extent of fat separation can be achieved. Again here the LTLT
procedure (115.6°C for 20 min) proves helpful. Fat separation in this more viscous body is
slower and less intense. In case of LTLT, fat layer get re-emulsified easily than in case of HTST
sterilization process.
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PHYSICO-CHEMICAL CHANGES TAKING PLACE DURING MANUFACTURE OF
CONDENSED MILK-II
Introduction
During the processing of evaporated and sweetened condensed milks the physico-chemical
changes that take place are further elaborated here.
Colour
Browning of milk is attributed to reaction of sugar in milk. But when solution of sucrose,
lactose, dextrose are heated separately, it do not show any sign of browning or caramel flavour.
The colour changes in evaporated milk are not in direct relation of time, but it is the reaction of
catalytic nature. Similarly, solution of sugar and proteins when heated, a marked brown colour
develops and colour could not be removed by washing and also whey is clear showing no sign
of any colour.
It appears that in the lactose - protein reaction, responsible for the darkening of milk proteins,
certain amino acids are involved. The sugar combines with NH 2 group which is alkaline,
neutralizing the alkalinity and leaving the acid group free, thereby causing a reduction of pH
accompanied by the formation of highly coloured product. It is well known that sugar heated
with an alkali turns brown; hence the amino acid - sugar complex which is alkaline would tend
to assume a brown colour. This would be the case especially with a reducing sugar such as
lactose, because of the availability of the aldehyde groups, which are naturally present in
reducing sugar. This is further proved as if we add formaldehyde, (being having a great affinity
for amino acid) to evaporated milk at the time of sterilization, milk remains quite white.
It is found that time and temperature of heating is an important factor contributing towards
colour of the milk. In addition it is noted that
1. Within the time of forewarming applied generally, the product suffers no decisive
change in colour. If it is for long period (30’), effect is intense.
2. Homogenization tends to diminish the colour of the product because of a finer sub
division of the fat globules which prevent such penetration of the rays of light as it would
reveal the butter fat more nearly in its natural colour which is yellow.
3. Storage causes progressive darkening with increase in time and temperature. At (5°C)
there is no change in colour.
It is observed that for each 10°C decrease in forewarming temperature, the holding period is
increased ~ 2.5 fold without causing an increase in colour.
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Cooked Flavor
Though cooked flavour is of little significance in our country, but still its mechanism is to be
studied. Heat treatment in processing tends to produce a cooked flavour in evaporated milk. This
is true also of fresh milk and milk products in general. It is generally observed that cooked
flavour accompanies the darkening of colour. HTST process produces less cooked flavour than
LTLT process. HTST sterilization treatment (135°C for 0.5 min) also reduces the extent of
sterilization, decreases the viscosity and also fat separation etc. occur. So because of these
limitation factors, LTLT process is important.
The reactions involved in production of cooked flavour are not sufficiently clear. It is observed
that when heating skim milk, cream, milk, EM, etc., -SH compounds are produced (provided
heated to high temperature or at low temperature for longer time) from one or more proteins
present. However, it is found that -SH compounds are wholly responsible for cooked flavour.
Five hours heating at 70°C produces full cooked flavour. It is shown that in the reaction causing
cooked flavour of milk by heat, O2 is taken up and CO2 is produced. Oxidation condition
inhibits the formation of -SH group.
There is a tendency in some evaporated milk upon ageing for granular deposit to form in the
can. This deposit has a whitish colour, it is gritty and insoluble and seemingly of non-crystalline
character. On analysis these granular structure are found to contain Tri Calcium Citrate -
Ca3(H5O7)2 and Tri Calcium Phoshate - Ca3 (PO4)2. These salts have peculiarity of being less
soluble in hot rather than in cold solution.
The tendency for increased concentration of milk solids to cause an increase in the amount of
sediment produced is well known to evaporated milk manufacturers. An increase in
concentration necessarily increases Ca, Mg, citric acid and PO 4 content in the milk and thus
provides possibility of precipitation. This can be controlled by addition of casein stabilizer.
The precipitation of mineral salts in the form of white sand like deposits is an age defect of
Evaporated Milk. The temperature of storage appears to be a controlling factor in this respect.
By this process, natural property of milk is retained better than that with the process of low
temperature long duration. The major advantages are to avoid cooked flavour and colour
changes. By HTST sterilization, heat stability will be better in concentrated product than with
conventional method of sterilization, but the problems that are encountered in this process are
insufficient viscosity and thin body which ultimately increase the tendency of fat separation on
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storage. Self stability of product is relatively small and gelation may occur during storage
period. Some of the different types of processes developed are:
(2) Continuous Flow Sterilization: Here temperature is 145°C or higher with only few seconds
holding and with subsequent aseptic canning. For avoiding the problems due to this sterilization
process, increase the viscosity and reduce the age thickening.
Several methods are supplementing temperature treatment which may be given before or after
sterilization. They may be given to the product during coming up period or cooking period and
get the advantage of avoiding cooked flavour.
When heat treatment is given to milk in manufacture of concentrated milk, the acidity measured
in terms of H+ concentration and titratable acidity is increased. The rate of formation of acid in
concentrated product is in proportion of time and temperature treatment.
It is also related to concentration of lactose. If the milk is heated in open pan, then the acidity
will slightly drop in the beginning followed by an increase in acidity which will continue till the
coagulation of casein. Initial decrease in acidity is due to loss of CO 2 dissolved in milk which
usually contributes to 0.01-0.02% of the total acidity expressed as lactic acid. The increase in
acidity on further treatment is due to breaking down of casein causing cleavage of phosphorus
containing acid, probably nucleic acid and to a lesser extent to oxidation of lactose. The actual
increase in acidity due to conventional temperature time ratio of forewarning in SCM is very
slight. This slight increase in acidity is compensated by the initial loss of acidity due to
expulsion of CO2. Whereas in case of evaporated milk, the reaction of sterilization heat
treatment in conventional type procedure is more and in addition, the milk is also heated at
higher temperature of forewarming. Due to this treatment, usually there is increase in acidity
approximately 0.05 - 0.1% during the sterilization process than the normal acidity due to
concentration.
The increase in acidity is in direct relation with time and temperature of storage. The acid
producing reaction due to heat treatment is continued even when the concentrated product is
held in storage room. The rate of acid formation will be very slow depending upon the
temperature of storage. SCM of 64.5% sugar ratio having initial acidity of 0.43% and the
original bacterial count 4381/g when stored at different temperatures resulted in to increase in
acidity.
This increase in acidity is mainly due to chemical changes as there was no increase in
microorganisms during storage.
1.Age thickening
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The main change in sweetened condensed milk during storage is presumably age thickening and,
finally, gelation. Sweetened condensed milk is far more concentrated than evaporated milk.
However, it does not thicken markedly faster with age. It is usually assumed that added sucrose
inhibits age thickening. Sucrose increases the Ca2+ activity. A difference with evaporated milk is
that an initial decrease in viscosity before age thickening is not observed. The viscosity in
sweetened condensed milk increases almost linearly with time. The following main factors
affect age thickening in sweetened condensed milk:
The variation in the type of milk and season occurs among batches of milk.
Higher preheating treatment yields higher initial viscosity, and gel can form earlier.
Hence, UHT heating is now generally applied.
The addition of sugar at later stage in the evaporating process results in lesser age
thickening.
The influence of added salts varies widely and depends on the stage at which it is added.
Salts are added up to 0.2%. Adding a small amount of sodium tetrapolyphosphate (e.g.
0.03%) mostly delays age thickening considerably, whereas adding more may have the
opposite effect.
2.Maillard browning
Ongoing Maillard reactions are inevitable. Brown discoloration is stronger as the storage
temperature is higher, the milk is evaporated to a higher concentration, and more intense heating
is applied. Additional Maillard reactions occur if the added sucrose contains invert sugar.
3.Oxidative changes
4.Lactose crystallization
Sweetened condensed milk contains around 38 to 45 g lactose per 100 g water. The solubility of
lactose at room temperature is about 20 g per 100 g water, but in sweetened condensed milk the
solubility is about half as much due to the presence of sucrose. It implies that 75% of the lactose
tends to crystallize, meaning about 8 g per 100 g sweetened condensed milk. Due to the high
viscosity, nucleation will be slow and only a few nuclei would be formed per unit volume of
milk, leading to large crystals.
Without special measures, the product will obtain a relatively high quantity of large crystals.
These crystals settle and are responsible for a sandy mouth feel. Although the crystals may not
be so large as to be felt singly in the mouth, they can be large enough to cause a non-smooth
impression. To avoid this, they should be smaller than about 8 µm in length.
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Preventing crystallization is not possible and, accordingly, a large number of crystals should be
obtained. Satisfactory results can be reached by using seed lactose. Adding 0.03% seed lactose
represents 0.004 times the amount of lactose to be crystallized. The final size of the crystals in
the product should not exceed 8 µ m. Consequently, the seed lactose would contain enough seed
crystals (one per crystal to be formed) if its crystal size does not exceed about (0.004 x 83)⅓, i.e.,
1.25 µm. Such tiny crystals can be made by intensive grinding of α -lactose hydrate.
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PHYSICO-CHEMICAL CHANGES TAKES PLACE DURING MANUFACTURING OF
DRIED MILKS
WPN INDEX AND HEAT DENATURATION
Introduction
Heat treatment of the original product or the concentrate can cause denaturation of serum
proteins; the conditions during spray drying are rarely such as to cause extensive heat
denaturation. The extent of denaturation is an important quality mark in relation to the use of
milk powder. For instance, if the powder is to be used in cheese making, practically no serum
protein should have been denatured in view of the rennetability; in infant formulas, on the other
hand, the rennetability should be poor.
WPNI
The extent of the denaturation of serum protein can be used as a measure of the heating intensity
applied. This is true also where denaturation by itself may be of no importance, but other
changes associated with intense heat treatment are. An example is the flavour of a powder to be
used in beverage milk, which requires a mild heat treatment. An intensive heat treatment is
needed for some other uses, for instance, to acquire good stability against heat coagulation in the
manufacture of recombined evaporated milk, or a high viscosity of the final product when
making yogurt from reconstituted milk. It is also desired if milk powder is used in milk
chocolate; presumably, Maillard products contribute to its flavor.
The whey protein nitrogen index (WPN index) is generally used to classify milk powders
according to the intensity of the heat treatment(s) applied during manufacture. To that end, the
amount of denaturable serum protein left in the reconstituted product is estimated, usually by
making acid whey and determining the quantity of protein that precipitates on heating the whey.
This can be done by Kjeldahl analysis of protein nitrogen or by means of a much easier turbidity
test that is calibrated on the Kjeldahl method. The result is expressed as the quantity of
undenatured serum protein per gram of skim milk powder.
High drying temperatures can result in undesirable changes in the dried product. Generally, it is
only after the powder has been dissolved again that the changes involved are noticed. Three
quite different categories of undesirable changes can be distinguished:
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1.Heat denaturation and killing of microbes
a. T he reaction rate is highly dependent on temperature, but the reaction is much slower and
less dependent on temperature at low water content.
b. Some results for the inactivation of phosphatase are showing that, a higher average drying
temperature and the higher dry-matter content of the liquid gives more inactivation because this
goes along with a higher viscosity and hence, on average, larger drops. Therefore, a longer
heating time is needed at a dry-matter content in which the inactivation rate still is appreciable.
However, the largest drops contain the greatest amount of material.
c. Killing of bacteria is higher as the average drying temperature is higher. The initial increase of
survival of bacteria with increasing dry-matter content is presumably due to a substantial
decrease in heat sensitivity of the organism.
d. Heat denaturation of globular proteins and consequently, inactivation of enzymes and killing
of microorganisms greatly depend on water content. It may also occur that removal of water
increases the concentration of a reactant or catalyst for heat inactivation; this is presumably the
case for chymosin in whey, because at, say, 40% dry matter, a w and diffusivity are not greatly
lowered.
2.Insolubility
a. Part of the protein may be rendered insoluble during the drying process due to heat
coagulation.
b. The powder contains particles that do not dissolve in water, but the amount is a tiny fraction
of the powder.
shows that insolubility increases with increasing outlet temperature and increasing dry-matter
content of the milk. It also greatly depends on drier design. Presumably, heat coagulation mainly
occurs in some (large) drops or powder particles that recirculate in the drier and become wetted
again. A cumulation of high temperatures and high dry matter content for a relatively long time
then causes the problem. Modern driers tend to give very small insolubility figures.
a. These can form at high drying temperatures because the outer rind of a drying droplet
soon reaches a glassy state; the pressure gradients developing in the particle then cause
these very thin cracks to form.
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b. In case of whole milk powder, part of the fat can now be extracted from the powder by
solvents like chloroform or light petroleum. The extractable fat is often called free fat, but
that is a misleading term.
Autoxidation of lipids
Autoxidation of lipids follows quite a different pattern. The reaction rate is high for low a w .
Possible causes are that water lowers the lifetime of free radicals, slows down the decomposition
of hydroperoxides, and lowers the catalytic activity of metal ions, such as Cu 2+. The rate of
many reactions greatly depends on the water content; shows Rate of Maillard reactions (—) and
of protein becoming insoluble (---) in concentrated skim milk at high temperature (~80°C) as a
function of water content.
Because of an increase in the concentration of reactants, the rate of bimolecular reactions at first
increases due to removal of water. On further increase of Q* , the reaction rate often decreases
again; this decrease would be caused by reduced diffusivity. A good example is the Maillard
reaction. The irreversible loss of solubility of milk protein in milk powders, and the rate of
gelation of concentrated milks show a trend similar to curve 5. On removal of water from milk,
it thus is advisable to pass the level of approximately 10% water in the product as quickly as
possible.
Relative reaction rate ( Kr) of various reactions plotted against the water activity (aw) of
(concentrated) skim milk (powder). The upper abscissa scale gives the water content (% w/w).
Thus, the influence of some process variables on product properties is inevitably complex as the
relationship between two parameters may depend on other variables and also it is mostly not
possible to vary only one process variable. However, it is observed that a two-stage drying
provides increased possibilities to make powder with various desirable characteristics.
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THE MILK POWDER SYSTEM
Introduction
The milk powder manufactured undergo several changes while conversion from liquid milk to
dry product. They are:
The dried milk exhibits a well pronounced dual physical structure – the primary structure,
which is the internal build-up of the powder particles from the milk solids and small
amounts of mois¬ture and air and – the secondary structure which represents a typical
powder, a system of closely packed solid particles in a gas.
The structural elements of dried milk particles are – lactose, either amorphous or partly
crystalline, casein micelles and whey protein particles, fat in globular or non-globular
(free fat) forms and air as spherical cells. The fat, protein and air are presumably
dispersed in continuous phase of amorphous lactose.
The whole milk and infant milk powders are rich in fat (20-37%) and hence need
protection against oxygen and moisture, therefore, generally tinplate cans are used and the
packaging is done under nitrogen cover to replace air with nitrogen in the tins. Skim milk
powders have very low fat (1.5%) and as such a good moisture barrier material like multi
wall paper sacks with one polythene liner is used. Recently, some skim milk powder has
also been sold on polythene bags and even high density polythene bottles are being tried
for retail packs.
The milk powders are concentrated mass of milk components in the form of particles with
small amount of moisture and air. If sufficient care is not taken to protect them from high
humidity, high temperature of storage and the entry of air, the deterioration processes are
accelerated.
These changes while manufacture occurs in a sequence. They are discussed here:
Atomizing pure water in a drying chamber in the usual way causes the water droplets to
reach the wet-bulb temperature and to vaporize within 0.1s at this temperature.
The presence of dry matter in the droplets, however, makes an enormous difference. T he
diffusion coefficient of water decrease substantially with increasing dry-matter content.
Accordingly, the vaporization is significantly slowed down.
In the drying droplet, temperature equalization occurs in less than about 10 ms. i.e. the
temperature is virtually constant throughout a droplet during drying.
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Drying Stages
• Initially, the droplet has a very high velocity relative to the drying air.
• Therefore, there is a first stage during which circulation of liquid in the droplet occurs;
this circulation greatly enhances transfer of heat and mass.
• For a droplet of 50 µ m diameter, this stage lasts for ~2 ms. In this time, the droplet
covers a distance of about 10 cm and loses a small percentage of its water.
• Its velocity compared to the air decreases to the extent that the formed surface tension
gradient of the drop surface arrests internal circulation of liquid.
• But in the second drying stage, the difference in velocity between drop and air is still
great enough to accelerate water transport.
• The transport in the droplet occurs by diffusion but in the air by convection.
• After about 25 ms the relative velocity of the droplet has decreased so far that the water
transport has become essentially equal to that from a stationary droplet.
• Relative to the air, the droplet then has covered a distance of a few decimeters and has
lost about 30% of its original water.
• In the third stage, lasting at least a few seconds, the droplet loses the rest of the water by
diffusion.
Drying Process
During drying the air temperature decreases and the humidity of the drying air increases.
Moreover, the droplets vary in size and the smallest ones will dry fastest.
In practice, the mixing is always between the two extremes. For driers with a spinning
disk, the situation tends to be fairly close to perfect mixing. In most driers with nozzles, it
tends to be closer to concurrent flows. In all situations, the drying time may very by a
factor of, say, 100 between the smallest and the largest drops. This is of great importance
for fouling of the drying chamber; the largest drops have the greatest chance of hitting the
wall and of being insufficiently dry to prevent sticking to the wall.
Another factor that affects drying rate is the presence of vacuoles in the drying drops. It
leads to significantly faster drying.
1.Concentration gradients
A rapid decrease in drying rate of the droplets occurs after the water content is reduced to, say,
15%. A strong concentration gradient forms rapidly during drying. The higher the drying
temperature, the stronger the effect. Therefore, stronger gradients occur for cocurrent drying. A
dry outer layer, i.e., a kind of rind, is formed and because of this, the water transport is slowed
down considerably. The temperature can rise significantly in the dry outer layer because a dried
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material assumes the air temperature, not the wet-bulb temperature. In other words, the decrease
in temperature near the surface of the droplet caused by consumption of the heat of vaporization
becomes far smaller because the vaporization of water is slower. Because temperature
equalization happens very quickly, the whole drying droplet increases in temperature.
The concentration gradients are not of a lasting nature. The relatively dry outer layer of the
droplet soon becomes firm and eventually glassy. This causes the droplet to resist further
shrinkage. The droplet can react by forming vacuoles or by becoming dimpled. Especially at a
low water content of the particles, so-called hair cracks may be formed.
2.Aroma retention
Besides water, the drying droplets lose other volatile components, including flavor compounds
(aroma). In many cases, however, the loss of flavor compounds is far less than expected, in spite
of their volatility because of the following conditions
• The effective diffusion coefficient of most flavor components in the relatively dry outer layer
of the droplet decreases far stronger with decreasing water content than the diffusion coefficient
of water does due to the greater molar mass.
• Thus, the aroma retention - retaining flavor compounds during drying - increases with
* Droplet size because in larger droplets, the outer layer from which the flavor components get
lost has a relatively smaller volume and
* Drying temperature because, at a higher temperature a solid rind forms more rapidly.
• Formation of vacuoles diminishes aroma retention, especially if hair cracks develop in the
particles and the vacuoles come into contact with the surrounding air.
• Dissolved milk powder often has a cooked flavor, which results from the flavor compounds
formed during preheating and possibly during evaporation.
• During drying, conditions are mostly not such that off-flavors are induced. On the contrary, a
considerable part of the volatile sulfhydryl compounds is removed. A cooked flavor mainly
results from methyl ketones and lactones formed by heating of the fat and from Maillard
products which are almost absent in skim milk powder.
3.Water Activity
If the water content of a product decreases, its water activity ( a w ) also decreases. Water
activity is expressed as a fraction. In pure water a w = 1; in a system without water, a w = 0.
Due to the very low water activity in milk powders, it exhibits following changes
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Diffusion coefficients decrease: At low water content the effect is very strong. The diffusion
coefficient of water decreases from approximately 10 -9m2 s-1 in milk to 10-16m2s-1 in skim milk
powder with a small percentage of water.
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The Physico-Chemical Changes During Storage of Milk Powders
It has been observed that the life of roller dried whole milk powder from cow's milk is about 10
months; the spray dried product however cannot be stored more than 6 months at 17°C and half
of this time at 27°C.
Although the milk powders are not sterile products, the low water activity does not permit
microbial growth and microbial activity. The same is true of enzymic activity. The changes
occurring in milk powders on storage are of physical, chemical and physicochemical in nature.
Both the lipids and the non-lipid constituents of milk undergo such changes and normally the
rates of such reactions are accelerated with the elevation of storage temperature and levels of
moisture and oxygen in the product.
The quality of milk and the processing parameters adopted while manufacture of milk powders
are also the major factors determining their storage stability.
The most important variable determining the rate of undesirable changes in milk powder is the
water content . When comparing different types of powder, it is probably easiest to consider
water activity ( a w ). The relationship depends on the composition of the product.
The higher aw of whole milk powder as compared to skim milk powder of the same water
content is caused by the fat not affecting aw .
Whey powder has aw slightly different from that of skim milk powder because in a dry
product the soluble constituents (especially sugar and salts) decrease a w somewhat less
than casein. This is only true, however, as long as all lactose is amorphous, which often
does not apply to whey powder.
Crystalline lactose binds water very strongly, and that is also why the usual oven-drying
methods to estimate the water content do not include the bulk of the water of
crystallization. If the water content excluding the water of crystallization is taken as a
basis, then a w is even higher for the powder with crystallized lactose.
It is thus advisable to make milk powder sufficiently dry and to keep it in that condition.
If it is not hermetically sealed from the outside air, it will attract water in most climates.
The higher the temperature, the higher the water activity. Because several reactions are
faster at a higher aw , this implies that a temperature increase may well cause an extra
acceleration of deterioration.
The deterioration effect may be especially strong if the powder loses its glassy state. A
lactose–water mixture will be at most ambient temperatures in the glassy state if its water
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activity is below 0.3. Because lactose is the dominant component of the amorphous
material in a powder particle, about the same relation is supposed to hold for the powder.
This means that most dairy powders are in the glassy state (i.e., the nonfat part of the
material), except if the water content is high and the temperature is also high. A change in
conditions leading to a glass–liquid transition will strongly accelerate most reactions and
physical changes occurring in a powder.
The user of dried milk is concerned mainly with the flavour defects which arise during storage.
Following aspects are important which affect the colour and flavour of dry milks:
The use of poor quality milk is not desirable for manufacture of good quality dry milk.
Some feed taints may be removed during the course of vacuum evaporation or drying, but
not always.
Acidity already developed in the milk will be retained in the powder, which acquires an
unpleasant flavour.
Neutralization of acid milk has been practiced, but the flavour of the resulting powder
remains unsatisfactory and the colour may darken. Very acid milk cannot be dried by the
roller process. First quality powder should not exceed an acidity of 0.15 (as lactic acid),
and no powder should exceed 0.17%.
Assuming that good quality milk has been used, the most likely defect of freshly made
powder is some degree of burnt flavour. A distinct burnt flavour is only likely to occur in
spray powder following considerable overheating in the drying chamber, but may arise
much more readily in roller powder owing to overheating on the rollers or faulty
adjustment of the scraper knives. In any case, roller powders always possess a distinct
cooked flavour. The flavour of spray powder is influenced considerably by the milk
preheating temperature used. Thus "low-heat" powder or powder from "ultra-high
temperature" processed milk gives reconstituted milk having a flavour close to that of
pasteurized milk. "High-heat" powder when reconstituted possesses a more cooked
flavour, which however, is not unpleasant and indeed is preferred by some consumers. In
practice, storage changes produce various flavour defects which mask other factors and
after 2-3 months the "low-heat" powder is commonly inferior if special precautions have
not been taken.
The colour and flavor changes will progress during prolonged storage if conditions like
elevated temperature in combination with increased moisture content prevail. Although
much research remains to be done, two major types of deterioration are well recognized,
affecting fat in one case and protein plus lactose in the other. Ultimately these affect the
flavour, solubility, colour and nutritional value of the powder. Two major categories of
reactions are:
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(b) The non enzymatic browning commonly known as the Millard reaction.
The former is associated with the tallowiness whereas presumably both these reactions
contribute to stale and allied flavours. With the advancement of storage, the discolouration will
also progress and fluorescence substances are also produced.
3. Fat decomposition
Oxidation of the fat leading to the production of flat, and finally marked tallowy off-flavours is a
major storage defect of full cream powder and some times occurs to a lesser extent in the
residual fat content of separated milk powder. Some of the observations made by different
workers are
The chemical changes result from the addition of oxygen to the double bonds of
unsaturated glycerides, giving peroxides which can be estimated by chemical means.
In the oxidation of linoleic acid, the C-11 methylene group is preferential point of attack.
Many other volatile aliphatic compounds such as alcohols, lactones, esters, acids and
hydrocarbons arise from oxidation of unsaturated fatty acids.
At first, the peroxides accumulate but later they decompose to various aldehydes, ketones
and acids which impart the unpleasant flavours.
Aldehydes are detectable with colour reagents but the sense of taste is much more
sensitive than chemical tests.
The reaction commences with a slow linear induction phase, followed by a period of
rapid exponential change and combination with oxygen, large quantity of O2 can be
absorbed. The break point at which the oxidation changes from first to second phase is
generally found to be at 37 weeks in whole milk powder.
Peroxides are formed when the container contains an excess of free O2, but later
decomposition of peroxides exceeds the rate of their formation.
The keeping quality of individual "low heat" powders varies considerably - from 4-12
months in temperate climates and perhaps half this time in hot climates.
Though the development of poor flavour is parallel to O2 absorption, the ratio is not
constant and the most stable powders require the most O2 in order to deteriorate to a
given flavour value.
The odour and flavour profiles of dried milk with addition of antioxidants (BHA/BHT &
Maillard reaction mixtures from histidine and glucose) and stored under air and nitrogen
are as follows
The Maillard reaction products are as effective as BHA/BHT in retarding the development
of oxidative off flavours and off odours.
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Samples to which antioxidants are added or samples stored under nitrogen retain a higher
acceptance for storage times as long as 84 weeks.
The 2, 3 butadione has a sweet and buttery odour and flavour at low concentrations and
the branched chain aldehydes, the Strecker aldehydes are generally described as having
fruity odours and flavours at low concentrations.
The sulphur compounds are known to impart cooked odours and flavours.
Some compounds, 1-octen-3-one and 1-octene-3-ol that are known to give rise to metallic
and mushroom odour and flavour respectively in oxidatively deteriorated milk products.
Factors affecting oxidative stability of lipids in dried milks include oxygen, moisture,
temperature, light and metals like copper and iron. These influence the system depending
upon their fat content, presence or absence of antioxidant and packaging under the
nitrogen atmosphere.
The use of antioxidants instead of nitrogen gas packaging, derived from various materials
showing promise as practical antioxidants are: wheat germ oil, gum guaiac, rice bran
concentrate mixed tocopherols, oat flour and special preparations made from ethyl
gallate, ascorbic acid, nordihydroguaiaretic acid (NDGA), thiourea, hydroquinone
monobenzyl ether, flavones, querectin, ascorbyl, palmitate, histide, tryptophan,
phosphoric acid either alone or in combination of a few.
For addition of any antioxidant legal acceptance is must and for the present in India, no
antioxidant other than lecithin, ascorbic acid and tocopherol is permitted accepting BHA
not more than 0.01% by weight in milk powder. In infant milk no antioxidant is
permitted.
Inspite of some fairly promising indications that antioxidants retard tallowiness in dry
milks, packaging in inert gas is the most efficient method at present available for
preventing fat deterioration.
4.Fat hydrolysis
True rancidity results from the hydrolysis of fat to free fatty acids such as butyric acid. The
lipolytic enzymes involved can be derived from the milk itself or they may be of
microbiological origin. This defect has become unusual since strict attention is now given to
both milk production and plant hygiene and higher preheating temperatures which inactivate
lipases.
The other flavours are described as "stale" or most characteristically as like "Coconut". A
‘toffee” flavour may also be a form of the same defect. They are produced only from milk fat
and do not occur in dried separated milk. The defect is accelerated by high-temperature storage
and by high moisture content, but is independent of O2 and occurs in gas packed powder. This
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form of deterioration seems to occur at a fairly early stage during storage, it develops before the
fat oxidation defect from which it also differs in flavour. There is strong evidence that the
change is caused by a rearrangement of monoethenoid fatty acids in milk fat to form lactones
and that δ-decalactone in minute quantities is the substance responsible for the coconut flavour.
The origin of this lactone is thought to be 9-deconoic acid. These rearrangements involve no O2
and the empirical formulae remain the same. No definite method of prevention has been
suggested except low-temperature storage.
In the absence of special precautions, oxidation occurs rather more rapidly in spray than in roller
powders, but in recent years much progress has been made in extending the life of spray
powders. With full-cream powder the main cause of deterioration is overcome if fat oxidation is
prevented, other possible defects being within the control of manufacturer. Hence, to keep the
autoxidation within reasonable limits for a long time, following measures should be taken:
1. High Temperature Preheating: The milk should be intensely heated to form antioxidants.
The problem is, of course, that the heat treatment also causes a distinct cooked flavor. Compared
with pre-heating the milk at 73.8°C, preheating at 82.2°C improves the keeping quality of the
powder, whilst at 87.8°C, the increase is 3-5 times. The mechanism is not fully understood, but
in general it is associated with the formation of trace of protein decomposition products
containing a sulfhydryl group which function as antioxidants and prolong the induction period.
Natural milk proteins contain no free -SH groups, but in the denatured protein formed in heated
milk, such groups become unmasked and reactive. The first action may be the formation of
cysteine followed by further reaction at the exposed sulfur ends of the chains to split off H 2S or
methyl mercaptan. Traces of H2S are detectable in the heated milk. The action of -SH group is
uncertain, but may be due in part to prevention of the catalytic action of heavy metals by
removing them as sulfides.
2. High temperature preheating may also prevent changes produced by enzymes derived from
the raw milk or from bacteria, thus improves the bacteriological quality of the powder and
preserves the vitamin content during storage.
3. The rate of autoxidation strongly increases with decreasing a w ; however, to prevent other
types of deterioration (especially Maillard reactions) a w should be as low as possible. The
effective Q 10 of the autoxidation reaction in milk powder is relatively low (about 1.5) because
a higher temperature also causes higher a w . The most suitable water content is generally 2.5 to
3%.
4. Packing in Inert Gas: This depends upon prevention of the chemical reaction by removing
the O2 from the container and replacing it with N2 or CO2 usually the former. It is the only
method which completely prevents oxidation for practical purposes and can extend storage life
up to 7-10 years even at high temperature. Oxygen should be removed as effectively as possible
by gas flushing. A problem is that the vacuoles in the powder particles contain some air, hence,
O2. Either the powder should contain hardly any vacuoles or the gas flushing should be repeated
after a few days. Equilibrating the gas inside and outside the vacuoles by diffusion takes several
days in whole milk powder (several weeks in skim milk powder). Equilibration is faster if the
powder particles have a greater number of cracks.
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5. Addition of Antioxidants: Of the more successful substances “Ascorbic acid” added
@0.03% in the liquid milk prolongs powder keeping quality by several months but disappears
during storage. The most effective antioxidants appear to be esters of gallic acid particularly
Ethyl or Propyl gallate. The incorporation of as little as 0.07% of ethyl gallate in the powder
prolongs the keeping quality to about two years when only low temperature preheating has been
used. Ethyl gallate is non-toxic and has no effect on flavour; it does not disappear during storage
and appears to remain unchanged. Keeping quality may be extended still further by combining
high-temperature preheating with the addition of ethyl gallate. In this way, it is possible to
produce powders having a keeping quality of from 3-4 years in temperate climates.
Nordihydroguaiaretic acid has also been found effective when added @ 0.04% of the weight of
the fat.
6. The rate of deterioration increases rapidly with rise of storage temperature. The keeping
quality of an unstable powder may fall as low as 6 weeks in a tropical climate.
8. The powder should be packaged in such a way that air and light are kept out. Generally, this
implies packaging in cans.
9. Rigorous measures should be employed against contamination of the milk with heavy metals
such as copper and iron which act as catalysts and shorten the induction phase. Stainless steel
equipment should be used.
10. Other less certain factors are the possible presence of oxidizing enzymes of microbiological
origin in the milk and seasonal variations in the glycerides-composition of the fat.
Millard reactions between protein and lactose produce a series of storage defects which often
occur together in a progressive sequence of stale flavours, increasing loss of solubility,
unpleasant "glue" flavour and darkening or brown discoloration. These changes may occur in all
types of powder but are associated predominantly with separated dried milk and tend to be most
pronounced in roller dried powders. They are greatly accelerated by high-storage temperatures
and in addition, the moisture content of the powder is a major factor. Critical moisture levels
appear to be about 5% for spray powder and 4% for roller powder. Above these figures, the
defects are accentuated.
This reaction in addition to accounting for the major part of browning, the protein-carbohydrate
complex or its decomposition products also result in production of reducing substances,
fluorescent compounds and disagreeable flavour materials. About 80 different compounds have
been isolated and identified which include furanics, lactones, pyrazines, pyridines, acetyl
pyrrole, amides, pyrolidinone, succinate, glutarimides, carboxylic acids, acetone, 2-heptanone,
maltol etc.
One of the first reaction products detected in Maillard reaction is hydroxymethyl furfural
(HMF), the concentration of which increases with storage time, temperature and moisture
content. Many of the products of Maillard reaction are aroma substances (aldehydes,
reductones, other furfurals etc.) which have an appetizing odour, but high levels of these
compounds may cause considerable odours and off flavours. The ε-amino groups of
lysine are mainly involved and because the compounds formed during the reaction such
as fructoselysine, furosine etc. are resistant to enzymes, the content of available lysine is
reduced, but usually only to a small extent. Another result of the reaction is the
production of substances which lead to colour changes, but only in a more advanced stage
of the reaction.
Browning reactions of the Maillard type occur if the storage of powdered dairy products
at ambient temperature and having the moisture content ≥ 5%. The HMF content is
further increased in milk powder with added iron or added Vitamin A.
With the progress of Maillard reaction, the decrease of amino-N is closely related to
increase in combined sugar, increase in oxygen absorption and carbon dioxide
production, increase in colour and reducing power and decrease in solubility .
A number of compounds have been shown to inhibit the browning reaction. In milk
products, active -SH groups serve as natural inhibitors in retarding the heat induced
browning, but the mechanism is not understood. Sodium bisulphite, sulphur dioxide and
fo rmaldehyde also inhibit browning in milk system as well as in simpler amino acid-
sugar solutions.
First the lactose absorbs moisture and changes to crystalline L -lactose monohydrate
containing 5% water of crystallization.
In powders of low moisture content, the lactose is present in the amorphous α and β-
forms (1: 1.5) with only 0.5 to 5.0% of lactose hydrate. If the moisture content and the
temperature remain low, the lactose preserves its amorphous form and no deterioration
occurs. If the moisture content is high, as much as 40-60% of the lactose may be hydrated
in a fresh powder and at levels of 6.5 to 7.0% for full-cream powder and 7.5 to 8.0% for
separated milk powder crystallization becomes rapid and complete (dried milk can also
absorb moisture very readily from the air). Such powders may show an apparent decrease
in their moisture content. There is often a loss of free-flowing properties and possibly
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some definite "Caking" of the powder. The impervious lactose envelope around spray
powder particles probably changes to a crystalline lattice.
The free lactose content of the powder then falls and an insoluble protein-lactose
compound is formed which contains lactose equivalent to the quantity of the free soluble
lactose which has disappeared. The reaction is presumed to occur between the aldehyde
group of the lactose and a protein-amino group. The amino group mainly involved is that
of lysine, and about 40% of the original lysine disappears, which considerably reduces the
nutritional value of the powder. As the protein - lactose reaction proceeds, the remaining
protein also becomes progressively insoluble and eventually the loss of solubility may be
pronounced, particularly of roller -dried milk.
The final stage involves a decomposition of the protein - lactose compound to form
products which include substances having an unpleasant glue-like flavour and a brown
colour. The reaction involves absorption of O2, and the evolution of CO2, but the exact
nature of the breakdown and the identification of the decomposition products are
uncertain. In general, the O2 reacts preferentially with the fat in full-cream powders, and
tallowy flavours predominates, whilst the stale and gluey flavours are more characteristic
of separated milk powder, but both forms of deterioration can proceed simultaneously.
If the powder is gas packed, the protein lactose reaction and loss of solubility may still
occur, but the final changes are much less serious. There may be some development of
brown colour and a slight caramalize flavour, but unpleasant flavours are unusual. It
would appear that development of the gluey flavour requires a supply of O 2. Gas packing
is therefore partially effective but is not a real solution.
The manufacturer can avoid these defects of browning more simply and with greater certainty
by producing powders by limiting heat treatments and time and of low moisture content and
using moisture-proof packaging combined with low storage temperatures.
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PHYSICO-CHEMICAL CHANGES TAKES PLACE DURING MANUFACTURING OF
ICE-CREAM
PREPARATION OF ICE CREAM
1.Homogenizing Mix
Homogenization of ice cream mix is a most essential step to make a permanent and uniform
suspension of the fat by reducing the size of the fat droplets to a very small diameter, preferably
not more than 2 µm.
Advantages of homogenization
Proper homogenization of the mix will never allow the fat to form the cream layer
Smoother texture
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Homogenization of mix is usually done at temperature ranging from 63 to77°C. A pressure of
2000 to 2500 psi (135 to 170 kg/cm2) with one valve or 2500 to 3000 psi (170 to 200 kg/cm2) on
the first and 500 psi(35 kg/cm2) on the second stage will usually give good results for an average
mix.
2.Pasteurization of Mix
Pasteurization is done to destroy all the pathogenic bacteria in the mix so as to render the final
product safe for human consumption
It improves flavour.
Rapid heating and holding of the mix at definite temperature and rapid cooling below 5°C
ensures proper pasteurization.
The temperature time combination for pasteurization of the mix as per BIS is as follows
UHT pasteurization – 98.8 to 128.3°C for not less than 0-40 seconds
High temperature pasteurization is preferred as there is a greater bacterial kill resulting in low
bacterial count in ice cream
Better flavour
Saving of stabilizer
Increased capacity
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3. Cooling of Mix
After pasteurization, the mix should be rapidly cooled to a temperature below 4°C using a plate
heat exchanger. Unless the mix is cooled to a temperature of 4°C or lower, it will become very
viscous and the ice cream will not melt down smoothly. Also, temperatures below 5°C retard the
growth of bacteria.
4. Ageing of Mix
Crystallization of fats
4. Freezing of Mix
The function of the freezing process is to freeze a portion of the water in the mix and to
incorporate air into the mix. This involves:-
a) Lowering the temperature of the mix from ageing temperature to the freezing point
d) Cooling ice cream from the temperature at which it is drawn from the freezer to
hardening room temperature.
The first phase of freezing process accounts for the freezing of 33 to 67 per cent of the water and
the second phase (hardening process) accounts for freezing another 23-57 per cent depending on
the drawing temperature.
The temperature of the mix which is put into the freezer drops very rapidly while the sensible
heat is being removed and before any ice crystals are formed. This process takes less than a
minute or two. Meanwhile, the rapid agitation reduces the viscosity by partially destroying the
gel structure and by breaking up the fat-globule clusters and also hastens incorporation of air
into the mix.
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When the freezing point is reached, the liquid water changes to ice crystals which appear in the
mix. These ice crystals are practically pure water in a solid form, and thus the sugar as well as
the other solutes becomes more concentrated in the remaining liquid water. Increasing the
concentration of the solutes slightly depresses the freezing point and when the freezing point is
continuously lowered, more ice crystals are formed increasing the concentration of sugar and
other solutes in the remaining liquid water until the concentration is so great that further freezing
will not occur. Thus all the water does not freeze even after long periods in the hardening room.
In hardening process, the aim is to reduce the temperature of the product to at least 0 oF in the
center of the package as quickly as possible. After the ice cream reaches this point, it is only
necessary to store it at a uniformly low temperature to prevent ice melting and recrystallization.
To freeze more water in the ice cream that has been drawn from the freezer and filled in
the container to obtain better consistency.
Hardening time: The time necessary for the temperature at the center of the package to drop
to -18°C is known as ‘hardening time’. A hardening time of 6-8 h for 19 liters (5 gal). package is
considered as ‘excellent’ operation when performed in hardening rooms. When hardening
tunnels are used, the rate of hardening is several times faster.
Hardening process
After ice cream is drawn from the freezer, it is put into containers to be placed in hardening
room. Here the freezing process is continued without agitation until the temperature of ice cream
reaches -18°C or lower, preferably -26.1°C (-15°F ).
Quick hardening is desirable, since slow hardening favours formation of large ice crystals and a
corresponding coarseness of texture.
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Whether several containers are bundled together
Very small containers harden quickly, but they warm up quickly when removed from the
freezing temperatures. Hence, they are more prone to body and texture damage as a result of
heat shock. This also applies to novelties (stick bars, small cups,etc.). Large containers (i.e.
11.34 liters) harden much slower in the interior(cooling is largely by conduction) and must be
given ample time to reach -18°Cin the interior.
If containers are stacked before they are adequately hardened, deformation may occur and some
overrun may be squeezed out causing surface discoloration.
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STABILIZERS AND EMULSIFIERS – SELECTION, MECHANISM OF ACTION,
INFLUENCE ON MIX AND ICE CREAM, PROPRIETARY STABILIZER BLENDS
Introduction
The stabilizers are a group of compounds, usually polysaccharides that are responsible for
adding viscosity to the unfrozen portion of water and thus holding this water so that it cannot
migrate within the product. This results ice cream that is firmer to the chew. Without stabilizers,
the ice cream would become coarse and icy very quickly due to the migration of the free water
and growth of existing ice crystals. Although excellent ice cream products can be made with
only the natural stabilizing and emulsifying materials present in milk such as milk proteins and
phosphates, additional stabilizers and emulsifiers have potential benefits.
Emulsifiers aid in the production of drier ice cream upon extrusion with smoother body and
texture and good stand up or melt resistance. The emulsifying agents commonly used in ice
cream are mono and diglycerides and polysorbate-80, polyoxyethylene sorbitan monooleate.
Milk also contains some naturally emulsifying compounds that aid in the manufacture of ice
cream. These include milk proteins, phosphates and citrates. Egg yolks may also be used as an
emulsifier as they are high in lecithin.
Stabilizers
Major functions performed by stabilizer in ice cream include contributing to body or ‘substance’
and creaminess, imparting a smooth texture and providing melting resistance to ice cream.
Excessive use of stabilizers, however, may result in gumminess, poor meltdown and interfere
with flavour release. The most important functions of stabilizers is to ‘stabilize’ the product
texture i.e. to prevent or minimize detrimental effect of heat shock during storage and
distribution.
Selection
The following factors are important in choosing a stabilizer:
Mechanism of action
Capable of imbibing large quantities of water while still remaining dispersed in water and
forming colloidal solutions, stabilizers are functionally also termed as hydrocolloids. These
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viscogenic compounds are primarily polysaccharides although, gelatin a well known stabilizer is
a protein in nature. The most apparent effect of stabilizers is the increased viscosity of the
continuous liquid phase. The effect of stabilizers on viscosity exhibits considerable interaction
with milk constituents. For instance, the basic viscosity of stabilizer solution is generally not
affected by heat treatment in the absence of milk solids, but in their presence, within creasing
total solids, the effect of stabilizer on heat induced increase in viscosity of the system becomes
more pronounced.
Upon hardening, the water content of ice cream falls considerably with a concomitant increase
in the concentration of stabilizer in the liquid phase. The increased stabilizer concentration
together with decreased temperature greatly increases the viscosity, there by substantially
reducing diffusion and mobility of the liquid in the frozen product. Also, gel formation induced
by stabilizer in the mix is believed to effect, considerably, immobilization of the liquid. The
movement of water is hindered partly by the ability of hydrocolloids to form hydrogen bonds,
too. Thus, refreezing of water that originated from melting of ice due to temperature fluctuations
would not permit the formation of large ice crystals. It should, however, be noted that merely by
increasing the viscosity the desired stabilization of ice structure may not be achieved. Increasing
the viscosity of a 36% TS mix by addition of 5% polyethylene glycol had no effect on ice
crystal size in the frozen dessert.
Certain stabilizers such as guar gum are effective thickening agents with no gelling ability.
Further, the way stabilizers influence the body and texture perception in frozen ice cream could
be related to their molecular structure and orientation besides their gel forming or viscosity
building ability. However, extrapolation of results from model systems to ice cream is difficult
as the later is a complex system with high concentrations of salt, sugar and stabilizers, which
interact with other molecules, e.g. protein.
The most profound involvement of stabilizers in promoting smoothness through control of ice
crystal size begins after initial freezing and hardening. Once the ice crystals are formed, the
influence of stabilizers is to do exactly what it implies… stabilize the size of the ice crystals
against growth as a result of temperature fluctuation (heats hock). There is an increase in mean
ice crystal size each time the temperature fluctuates. Stabilizers help create a situation where a
higher proportion of water which changes state during temperature rise recrystallizes as small
crystals. This is thought to occur through the formation of a system (with high viscosity and /or
a gel structure) which immobilizes the melted water, thereby reducing the degree to which it can
migrate to existing ice crystals and deposit on them when it refreezes. The net effect is to slow
the rate of ice crystal growth whenever heat shock occurs.
This is a major function at the time the product is drawn, during hardening and at the time of
consumption. It involves the participation of the stabilizer ingredients in determining the
cohesiveness of the product, particularly those aspects described by such adjectives as chewy,
sticky, weak, gummy, etc.
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3. Effect on whipping and overrun retention
The structure which is established as water freezes and stabilizer and its complexes are
concentrated also play a role in providing strength to the air cell wall. Stabilizer are therefore
involved in the amount of air which is incorporated and the degree to which the air cells are
stable.
The structure which results from the interaction of gums with water and other ingredients has a
direct bearing on the rate of melting and appearance of the melted product. The meltdown
appearance function is outcome to the role of stabilizer with respect to protecting against serum
separation and fat destabilization in that by reducing the degree of destabilization of fat and
protein, stabilizers canavoid the development of curdy appearance in melted product.
5. Effect on sandiness
Sandiness is caused by lactose,the defect was more prevalent 50-60 years ago and is rarely seen
today. This is because of the type of stabilizers used these days (CMC, natural
gums,carrageenan, etc.), which functions in a manner similar to control of ice crystal size
through decreasing the mobility of unfrozen water during heat shock. The supersaturated stages
in which sugars responsible for sandiness are prone to crystallize in frozen desserts are reached
at temperature associated with a high stabilizer concentration. This encourages the distribution
of the crystallizing lactose over a large number of small crystals rather than a lesser number of
larger crystals which ultimately grow to a size where they can be perceived. Microcrystalline
cellulose is particularly effective in this function, probably by providing an additional seeding
function which encourages the development of small crystals.
Ageing of ice cream mix is an important processing step with regard to stabilizer action.
Hydration of stabilizer is the most obvious effect of ageing, although not all stabilizers require
ageing for complete hydration. The effects of ageing are more pronounced with gelatin
stabilizers, and improvements in ice cream and freezing performance becomes more evident as
the ageing time increases from 4 to 12 h or more . Even mixes containing stabilizers which
require no ageing for complete activation benefit from a certain minimum ageing due to milk
protein hydration and fat crystallization.
Emulsifires
Emulsifier are surface active agents known to improve the sensory quality of ice cream by
aiding the whipping process, improving air cell distribution and enhancing the products heat
shock resistance. They also impart a dry appearance and stiffness or ‘stand up’ property to the
product being extruded from the freezer. These effects are brought about by the inter facial
properties of emulsifiers. Their ability to reduce surface tension seems to promote development
of smaller but numerous air cells.
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The primary effect of emulsifiers in ice cream is related to their ability to de-emulsify the fat
globule membrane formed during homogenization. This de-emulsifications arising from the
disruption of the fat globule membranes during freezing, facilitates the agglomeration and
coalescence of fat globules,leading to partial churning out of the fat phase. The agglomerated fat
globules stabilize air cells. Thus, emulsifiers are used to improve the whipping qualities of ice
cream by producing smallerice crystals and smaller air cells, resulting in a smoother ice cream
texture and drier, stiffer ice cream. Generally, a mixture of high and low hydrophile-lipophile
balance (HLB) emulsifiers, such as mono- and diglycerides and polysorbate 80 are used. HLB
concept was put forth by Griffin in the year 1949. HLB number ranges from 0 to 20. The HLB
number is derived by calculating the proportion of the molecular weight of the emulsifier
molecule represented by the hydrophilic portion and dividing that value by 5. The HLB system
can be useful in describing an emulsifiers general characteristics; however, it is not precise
enough to be applied as a tool in identifying an exact HLB number which will exactly match a
specific emulsion need.
Selection
The following criteria are used in choosing an emulsifier
Mechanism of action
The two phase emulsion is stabilized by casein micelles adsorbed at the fat globule serum
interface in the homogenized ice cream mix. But when an emulsifier such as a monoglycerideis
used, the fat globules are covered with an emulsifier layer and the milk proteins form an outer
layer. Monoglycerides effectively compete with protein if they form crystals at the interface.
Hence, the outer protein layer tends to be repelled from the fat globules. As a result, the
emulsion is prone to destabilization by mechanical action during freezing. This destabilizing
effect, in conjunction with other processing factors, is considered to be primarily responsible for
development of the desired product structure.
The dry appearance of ice cream coming out of the freezer is believed to be caused by several
phenomena, one of which is an emulsifier induced clustering of fat globules at the liquid air
interface. Also, more air cells of smaller size foaming on account of presence of emulsifiers
appear to provide more surface with the available liquid, which implies that the liquid is spread
over a larger area.
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The de-emulsification effect of emulsifiers is related not only to the quantity of emulsifiers used
but also to the fat content of the product. With increasing emulsifier concentration, fat de-
emulsification is enhanced and beyond a certain limit, greasy texture and short body result due
to butter formation in the freezer. Higher fat levels magnify this de-emulsification phenomenon.
Thus, an emulsifier level just enough to provide the correct amount of ‘partial churning’ is
necessary, and less emulsifier is required in a high-fat ice cream than in a low fat one. Excessive
emulsifier may promote slow melting and curdy meltdown.
Different emulsifiers differ structurally, and so their action in ice cream differs, too. Obviously,
therefore, the quantity of emulsifier required varies with the type of emulsifier used. Mono- and
diglycerides are often used in combination, although the former is more effective. When
unsaturated fatty acids such as oleic acid are present in the molecule, these emulsifiers promote
better dryness at drawing from the freezer.The fat destabilization responsible for stiffness of the
frozen mix is in the decreasing order for mono laurate,monooleate, and mono stearate in that
sequence used at 0.1-0.2%, mono- and diglycerides are less likely to cause churning. However,
their drying and whipping ability is somewhat limited as compared to polysorbates which are
water soluble components of sorbitol. Tween 80 or polysorbate 80 (polyoxyethylene sorbitan
monooleate) has a high drying power and aids in heat shock resistance, but the unsaturated fatty
acid may undergo auto oxidation to develop an off flavour,particularly when a certain level is
exceeded. Used usually at 0.02 to 0.06%,Tween 80 in excess may cause churning especially in
soft serve and high fat ice creams. Another polysorbate, Tween 65 (polyoxyethylene sorbitan
tristearate) has a little lower drying power as compared to Tween 80 but has excellent whipping
properties. Because of its flavour stability, Tween 65 can be used at higher levels (e.g. 0.1%)
without any adverse effect on the products flavour. The fat destabilizing ability of different
polysorbates is in the order Tween 80> Tween 40 (polyoxyethylene sorbitan monopalmitate) >
Tween 60 (polyoxyethylene monostearate)> Tween.
It is necessary that for an emulsifier to be effective in ice cream mix, the latter has to be
homogenized. While milk protein, casein in particular helps achieve size reduction of fat
globules by homogenization,presence of emulsifiers promote greater size uniformity as, for
example, mix containing a monoglyceride displays upon homogenization, a very narrow band of
size distribution (about 1µ) as compared to mix without monoglyceride (1-5 µ).While
homogenization of ice cream mix helps to stabilize the oil-in-water emulsion, it is this
stabilizing effect in conjunction with the destabilizing effect of the emulsifier that results in the
desirable texture quality. The greatly decreased fat globule size coupled with controlled de-
emulsification caused by emulsifiers, in essence, brings about the development of the right kind
of structure and corresponding texture in ice cream.
During ageing of ice cram mix, milk fat crystallizes, much of crystallization taking place during
the first hour. Presence of emulsifiers leads to more extensive fat crystallization. The emulsifier
caused protein desorption from fat globules is time dependent and takes place during ageing.
Further, the initial desorption from the surface of the fat globules, in the presence of emulsifiers,
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occurs as the removal of a coherent protein layer rather than individual casein particles. The
process of deemulsificaiton continues into the freezer to yield the desired body and texture.
Emulsifiers and stabilizers contribute to a great extent, to the desired body and texture
characteristics of ice cream and frozen desserts. The mechanisms of their actions have been
studied extensively in recent times and their role in conjunction with various processing steps
have been delineated by various workers. It is well recognized that individual compounds vary
considerably in their emulsifying/ stabilizing effects and often a single compound is not entirely
satisfactory. Thus, a mixture of two or more emulsifiers/ stabilizers is generally preferred to
overcome the drawbacks of individual compounds.
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