Exercise no 1.

Date:

Sampling of milk
Introduction
Sampling of milk and milk products shall be done by an experienced person who is familiar with
the techniques and is well acquainted with the knowledge of the subject. It is not possible to lay
down a single sampling procedure which will be applicable in all the cases. The sampling
procedure, therefore, differs according to the nature of the material and the purpose for which it is
needed.
Sampling is defined as the small portion of milk representing a particular batch or quantity of milk.
Sampling of milk is essential to determine the Physico – chemical and bacteriological quality of
milk. Milk sample should be true representative of whole volume of milk therefore thorough
mixing of milk before the sampling
All precautions shall be taken to prevent contamination and adulteration. For chemical
examination, the sampling equipment shall be clean and dry. For bacteriological examination, all
equipment’s including plunger, sample bottles and rubber stoppers shall be sterile and the samples
shall be collected under aseptic conditions. If subsequent analysis or interpretation is to be of some
value, it is very important that sample should be a true representative of the bulk. Since milk fat is
of lower density than the other constituents of milk, it tends to rise to the surface. Therefore,
thorough mixing of milk with a proper instrument which will reach the entire depth of the liquid
is essential to ensure a representative sample of the entire batch. In small batches, it should be
possible to accomplish mixing by pouring the entire quantity of milk from one container to another,
three or four times. Larger batches of milk shall be thoroughly agitated by a hand stirrer or by
mechanical means. Milk churns easily at 26.5 to 29.5°C and agitation near this temperature shall
be avoided.
Milk sampling is 3 types
1. Fresh or Spot Sampling: Sample is tested as early as possible after collection because no
preservative is added in this type of sampling.
2. Composite Sampling: Samples prepared from different combination of milk taken from different
container in a relative proportions.
3. Time Compose Sample: Sample is prepared by combining the different- different milk samples
from daily supplies of milk received from the same source or milk supplier over a period of 10-
15days. Such sampling required addition of preservative of milk.
Objective of Sampling:
1. To determine the Physico-chemical properties.

2. To determine the Bacteriological quality of milk sample.

Requirement:
1. Plunger: It is the stainless steel/ Galvanized iron/ aluminum. It consist of metallic rod, fitted
with a perforated metallic disc at one end and handle at another end. For 40L milk can, the length
of rod should be 1m with a diameter of disc 150mm, perforated 6 holes each of 12.5mm
diameter, on a pitch circle of 100mm in diameter. For milk storage tanks/tankers, length of rod is
1.8m with disc having 300mm and pitch circle of 100mm diameter.

Milk can Plunger

2. Mechanical Stirrer: It work on electric motor with a shaft fitted with propeller blades. These
stirrer are permanently fixed in storage tanks/ tankers.

Mechanical stirrer

,cz kdvjvdbj .mcm

sdslkljlbbfdd
3. Milk sampling dipper: It is made up of stainless steel/galvanized iron/aluminum. It consist of
metallic rod fitted with the bowl at one end and handle at another end. For fresh or spot sample its
capacity is 80-150ml and 15-20ml for composed sample.

Dipper

4. Milk sampling bottles: These are made up of glass or high density sterilized plastic having a
capacity of 100-250ml. These bottles have wide mouth with air tight with plastic lid.

Glass bottles Plastic bottles

5. Sampling Tubes or Milk Thief: These are straight metallic tube 60cm in length with 6mm
inner diameter and open at both ends. It is used for obtaining samples from uniformly sized
containers. The samples is drawn by closing the top of the tubes with fingers.

Milk Thief
Labels: Each sample container (bottles or jars or other container) shall be sealed air-tight after
filling and a label marked with the following particulars should be put on the container:
Purpose of sampling:
Sampling of milk and milk products is generally done for Chemical analysis, Bacteriological
analysis, Sensory analysis etc. The sample should bear the following information to ensure the
tractability of the sample.

 Name of the supplier/manufacturer

 Date and time of sampling and place of sampling

 Nature of the product like: Milk sample, Butter sample, Ghee sample, Milk powder etc.

 Identification number, name, designation and signature of the person responsible for
taking the sample

 Mass or volume of the sample

 Particular of the stock/ unit from which the sample is taken i.e.

Stock number
Batch number
Code number

 Preservative added or not to keep the sample suitable/ fit for analysis.

 If yes, then
- The nature of preservative added
- Quantity of preservative added

 If no preservative is added, then storage, temperature during transit or transportation

till analysis is done, should be mentioned.

Examples-

Store at refrigerated temperature

Store at room temperature etc.

 Additional Information: if sample is taken from a food which has some certification
mark like ISI, Agmark etc, then in that case, give additional information such as
 Mark (ISI/Agmark)

Grade (Special, General etc)

Agmark label no./Batch no.

Name packing station where the food was packed etc.

Procedure:
The method of sampling is determine by the purpose and condition under which sample
is to be taken.
1. Mix the milk thoroughly in the container with the help of plunger several time to ensure
uniformity of milk sample.
2. Move the plunger up and downwards and don’t allow the milk to stand for more than 5
minutes.
3. Take a sterile dipper and insert it in the milk container and collect samples below the surface
of milk.
4. Transfer the milk sample from dipper to sampling bottle which may contain milk preservative
if the time for analysis has to be delayed.
5. Mark the sample no. or animal no. on the sampling bottles and send t for the bacteriological
examination as soon as possible.

Precautions:
1. All equipment’s and apparatus should be dry and clean.
2. Whenever preservative is added indicate it on the label.
3. Freshly drawn milk may contain about the 10% gases hence sampling should be done at least
1h after draining.
4. Mixing of milk should be thoroughly.
5. During transport sampling bottle should not be exposed to sunlight.
6. if, Sampling has to be done for bacteriological examination, then plunger, dipper and sampling
bottle utilized for collection of milk should be sterilized.

Observation:
Results/ interpretation:

Question 1. Enlist the preservative of milk.

Question 2. Why milk transportation is recommended in dark brown glass bottles.

Question 3. What is normal bacterial count of the raw milk.

Exercise No. 2 Date:

Determination of fat percentage by Gerber’s method

Introduction: Milk fat is most variable component of milk and it is also used for determining the
purchase and selling pricing of milk therefore estimation of fat in milk is an important for
determining the adulteration of milk with water and defatting the milk (skim milk).

Dr. N Gerber nationality of Zurich Switzerland invented a method in year 1892-1895 for
determining the FAT content and other constituents of milk by Gerber’s centrifuge methods. Fairly
similar test was famous in the United State of America was Babcock test although Gerber’s
centrifuge method also got significance attention as well. Gerber’s method commonly used in
Europe and India.

Principles:
H2SO4 is used to increase specific gravity of milk serum which makes greater difference
between milk serum and fat globules. It also destroys stickiness of milk by dissolving all the SNF.
The free fat globules rise to the surface by subsequent application of centrifugal force to this
mixture and heat produced due to mixing of acid and milk, causing melting of fat. It facilitates the
fat particles to come to the surface freely. The specific gravity of fat is 0.9 and that of acid milk
mixtures is 1.43. This situation promotes complete separation of fat when proper centrifugal force
is applied. Due to application of centrifugal force lighter substances (Butter fat) are thrown towards
center and rest of serum portion that is heavier is thrown towards the periphery Addition of amyl
alcohol helps for separation of fat from the milk acid mixture and also prevents the charging of fat
and sugar by the H2SO4.

Material Required:

1. Milk sample
2. 10.75ml capacity pipette

3. 10ml H2SO4 capacity tilt measuring flask (sp.gr..1.82)

4. 1ml Amyl alcohol capacity tilt measuring flask (sp.gr.0.82-0.83)
5. Gerber’s butyrometer
6. Butyrometer key
7. Butyrometer rubber stopper
8. Gerber’s centrifuge machine (1100 rpm)
9. Butyrometer stand
10. Water bath

Procedure:

1. Take a dry and clean butyrometer and keep it in butyrometer stand with open end upwards.
2. Add 10 ml of H2SO4 into the butyrometer with the help of tilt measure. Care should be
taken not to moisten the inside of neck.
3. After properly mixing transfer 10.75 ml of milk sample in the butyrometer drop by drop so
that it forms a separate layer above the acid.
4. Then transfer 1 ml of amyl alcohol with tilt measure.
5. Fix the lock stopper with the help of guiding pin/regulating pin by holding the butyrometer
in the palm of left hand.
6. Shake the butyrometer without inverting until all the solid particles are dissolved and
mahogany red colour is obtained.
7. Place the butyrometer in the water bath for 5 mins. Then place the butyrometer in the
centrifuge. Stem should remain towards the center. Balance the machine by putting filled
butyrometer in opposite direction.
8. Rotate the centrifuge at 1100-1200 rpm for 4-5 minutes.
9. Take out the butyrometer from the centrifuge machine. If fat column is not clear, then put
the butyrometer in water bath maintained at 68oC with stem upward for 2 minutes.
10. Note the fat column in the graduated stand by adjusting lower end of fat column against 0
or a unit graduation by pushing or pulling the stopper slightly.

Precaution:
1. Carryout through mixing of milk before testing.
2. Amyl alcohol must be pure.
3. Sulphuric acid is to be added gently by the sides of the butyrometer without wetting the neck
of the butyrometer. Avoid direct pouring of milk on acid.
4. The three fluids viz. Sulphuric acid, milk and amyl alcohol should be added gently, so that
they form three distinct layers.
5. Rubber stopper should be dry, clean and without crack.
6. Before centrifuging the butyrometer, see that there is no curdy white material left undissolved.
7. The centrifuge must be properly balanced.
8. Always carry out the test in duplicate.
9. Butyrometer should be free from Na2CO3 (soda ash) if cleaned by Na2CO3 otherwise it lowers
the specific gravity and strength of Sulphuric acid.
10. Use butyrometer stand for shaking of butyrometer contents to dissolve the SNF content of
milk.

Amyl Alcohol Sulphuric Acid

Key and Rubber stopper Butyrometers

Observation:

Results/ Interpretation:

Question 1. Write the Fat percentage value of different spices

Question 2. Write the Factors that affect the Fat content of milk
Question 3. Write the Fat soluble vitamins and pigment found in the milk
Question 4. Explain why ghee obtain from cow milk fat is yellowish in color while not that of
buffalo milk.
Exercise No.-3 Date:

Determination of specific gravity of milk

Introduction: Milk is often subjected to various processes before being allowed for marketing.
During processing of milk there will be change in the density or the specific gravity of milk. A
number of factors influence density or specific gravity of milk such as addition or removal of
water, cream or other components etc. and temperature and pressure used during the processing
of milk.

Define: Specific gravity is the ratio of density of any substance to the density of standard
substance (water) at 4ºC.
Specific gravity of normal milk is 1.028 to 1.032.
Specific gravity of milk can be determined by any of the following methods –

1. By Quevenne Lactometer (calibrated at 15.6oC) or, ISI Lactometer (calibrated at 27oC).

2. By specific gravity bottle

3. By westphal balance.

NOTE: When hydrometer is immersed in a liquid (i.e., milk) an upward thrust is felt on
hydrometer which is equal to the weight of liquid (i.e., milk) displaced by hydrometer.

Material methods:

1. Lactometer

2. Lactometer glass cylinder

3. Milk sample

4. Thermometer

Procedure:

1. Mix the milk sample thoroughly.

2. Bring the temperature of the milk to calibrated lactometer temperature.
 3. Pour the milk sample into glass cylinder up to its 2/3rd capacity.
4. Keep the lactometer in glass cylinder containing milk.
5. Pour the milk up to the brim of cylinder.
6. Lower the lactometer up to zero mark and leave it to find it its own level.

Observation:
1.Note the lactometer reading by observing the point on the stem to which milk reaches.
2.Record the temperature of milk.

Calculations: Specific gravity of milk can be calculated by following formula-

Sp. gravity = Correct lactometer reading (C.L.R) + 1
1000
Determination of correct lactometer reading: It has been seen that milk at the point of contact
on stem of lactometer, is slightly elevated than the actual level, therefore it is necessary to
determine the meniscus for each instrument. Generally in all small lactometer having a diameter
of stem of 5 mm, 0.5 is added in O.L.R. as meniscus error observed.

In case if it is not possible to bring the temperature of milk to calibrated lactometer

temperature, a correction factor is applied for temperature variation. For every 1 oF rise in
temperature of milk than calibrated temperature of lactometer, 0.1 should be added and for every
1oF fall in temperature of milk than calibrated lactometer temperature, 0.1 should be subtracted
from observed lactometer reading.

Hence,
C.L.R = Observed lactometer reading (O.L.R.) + Meniscus error + Temperature difference
x 0.1

Precautions:

1. Sp. gravity of milk should be recorded at least one hour after milking because in recently
drawn milk air present lowers the sp. gravity of milk.
2. Sample should be thoroughly mixed otherwise a fat layer will be formed at the top.
 3. Cylinder should be slightly wider and deeper than the lactometer.
4. The lactometer should not touch the cylinder.
5. The lactometer must be kept clean otherwise it will not give accurate result if a film of milk
is allowed to dry on it.
6. Milk should be filled in the cylinder up to the brim.

Zeal Lactometer Lactometer glass cylinder

Observation:

Results/ Interpretation:

Question 1. How the specific gravity of milk is change with addition of water and rise in
temperature of milk sample?
Question 2. Write the specific gravity of the following

Specific gravity of different substance Value

Water
Skim milk
Cow milk
Buffalo milk
SNF (solid not fat)
Lactose

Question 3. Justify the statement specific gravity of milk is quick test for adulteration of milk
with H2O and solids.
Exercise no. 4 Date:

Determination of total solids and solids-not-fat content of milk sample

Introduction: Milk mainly have two content moisture (i.e., H20) and Total Solids. Water
percentage in milk is always above 80 percentage (Cow 85-87% and Buffalo milk 84-86%). All
the milk constituents are either suspended or dissolved in milk e.g., Lactose, some mineral, gaseous
and pigment like carotene, Xanthophyll are found in dissolved state while protein (Casein) found
in colloidal states and milk fat are suspended in milk and form a creamy layer on top of surface if,
milk sample kept undisturbed for some length of time.

Total solids of milk are of two types

1. Milk Fat

2. Solid Not Fat (i.e., SNF)

Milk Fat are small globular micelles particle having average diameter of 2-5µm (Cow 3-8µm and
Buffalo 4-10µm) there fat globule form fat in water type of emulsion. Fat provide color, flavor,
energy (Cow milk 75cal/100g and Buffalo milk 100cal/100g) and Nutritive value to milk.

SNF= TS- Fat

Material Required:

1. Milk sample
2. Lactometer
3. Thermometer
4. Lactometer cylinder
5. Gerber centrifuge machine (1100 rpm)
6. Amyl alcohol (sp. gr. 0.815 – 0.825)
7. Conc. H2SO4 (sp. gr. 1.820 – 0.825)
8. 10.75 ml capacity milk pipette
9. Butyrometer.
10. Richmond scale
Objective: To determination of Total solids (TS) and Solid not Fat (SNF) content by formula:
This method is based on the principle that specific gravity of milk is based on the proportion of
water, fat and SNF in the milk. Thereby determining the fat and specific gravity of milk we can
determine the T.S and SNF content of milk.

Calculation:

1. By Richmond’s formula at 84 oC
% T.S = __G + 1.2 F + 0.14 i, e: TS=0.25(CLR) + 1.2 F + 0.14
4
% SNF = _ G _+ 0.2 F + 0.14 i, e: MSNF=0.25(CLR) + 0.2 F + 0.14
4
Where,
G is the correct lactometer reading, F is fat content of milk

2. By Revised formula at 20 oC

% T.S = G + 1.2 F i,e. : TS=0.25(CLR) + 1.21 F + 0.66

4
% SNF = G + 0.2 F i,e. : MSNF=0.25(CLR) + 0.21 F + 0.66
4
3. Fleischmann’s formula
% T.S = G + 1.2 F + 0.25
4
% SNF = G + 0.2 F + 0.25
4
4. SNF (%) = TS (%) – Fat (%)
S.N.F content of milk can also be determined as %SNF = % TS __ % Fat calculations
Richmond’s devised a slide rule which is known as ‘Milk Scale’ for correcting the
observed specific gravity to standard temperature of 60oF and for finding total solids.
Procedure:

1. Determine the fat percentage and lactometer reading in the given sample of milk as done
in the previous exercises.
2. To correct the lactometer readings bring the observed lactometer reading in the sliding
scale to 60o in the temperature scale. The correct lactometer reading will be found against
the observed temperature of milk.
To find the total solids in the milk adjust the arrow mark in the sliding scale to the percent
of fat found. The percentage of total solids will be found against the corrected lactometer
reading in the lower right hand portion of the sliding scale.

Observation:

Result / Interpretation:

Question 1. Write the Fat and SNF percentage of the following

Composition

Product FAT% SNF%

Raw milk
Homogenized milk
Skim milk
Fortified skim milk
Light cream
Heavy cream
Single toned milk
Double toned milk
Question 2. Supposed you have to prepare a cream containing 5% of fat and 9% SNF from a
cream sample having 15% of fat and 30% SNF. How you would prepared it?

Question 3. Write the average fat percentage value of the following milk

MILK FAT%
Cow milk
Buffalo milk
Goat milk
Sheep milk
Camel milk
Mare
Whale

Question 4. Write the factors that affect the fat percentage of the milk