Butter Analysis

It is composed of 80% to 90% butterfat, milk proteins, up to 16% water,

and can contain salt as well. Butter is typically light yellow and has a
variety of uses.

Analytes

 Fat
 Moisture
 Solid Fat Content (SFC)

Solid Fat Content (SFC) is an important parameter in dairy products and

especially in butter. It is a measure of the amount of solid fraction of
crystallized fat in terms of weight percentage and is a good indicator of
the functional characteristics of milk fat.


Preparation of Sample of Butter
Warm the sample in an airtight container with the lid screwed down
tightly or with the glass stopper in an oven or water bath maintained at
37 ± 2°[Link] vigorously to obtain a homogeneous fluid emulsion free
from un softened pieces. In case, the sample does not mix up properly
(water separation can be seen) reject the sample. For analysis of butter
fat heat a portion of emulsified butter in a beaker to a temperature of
50 – 60°C until the fat separates. Filter the fat layer through a dried filter
paper into a dry vessel. Melt the filtered fat if necessary and refilter to
obtain clear fat free from water.
Determination of Moisture in Butter
Apparatus
A. Hot air oven: Maintained at 100°C.
B. Flat bottom moisture dish: Dishes of height at least 25 mm and at
least 50 mm in diameter, and made of appropriate material (for example
stainless steel, nickel or aluminium) not affected by boiling water.
C. Glass rods with one end flattened and about 9 cm in length.
D. Desiccator with an efficient desiccant.

E. Boling water-bath with rings to take dishes of 50 mm diameter.

F. Clay pipe triangles.
Procedure
. Clean the dish and the glass rod and dry them in the hot air oven
maintained at 100°C for at least 1 h.
. Allow to cool to the room temperature in a desiccator and weigh the
dish.
Accurately weigh (to the nearest 0.1 mg) into the dish 3 to 4 g of the
prepared butter sample.
. Place the dish on a boiling water-bath supported on a clay pipe triangle
for at least 20 min, stirring at frequent intervals until no moisture can be
seen. Wipe the bottom of the dish and transfer it to the oven maintained
at 100 °C and keep it for 90 min.
Allow the dish to cool in the desiccator and weigh to the nearest 0.1 mg.
. Heat the dish again in an oven for 30 min. Repeat the process of
heating, cooling and weighing until the differences between two
consecutive weights does not exceed 0.1mg preserve the residue for the
determination of [Link] weight of butter sample taken for
moisture determination is 5 g and drying temperature is 102 ± 2°C for 1
h.
Calculation
Moisture, % by mass = M1 − M2=M3
M3 − Mx 100
Where, M1 = mass in g, of the dish with the material before heating to
constant weight;
M2 = mass in g, of the dish with the material after heating to constant
weight; and
M = mass in g, of the empty dry dish.
Determination of non-fat solids and fat contents
Determination of Fat and Curd (Milk solids not Fat) in Butter
Fat portion is removed with the help of petroleum ether and residue left
behind is dried for determination of curd content. In case of table butter,
it is curd and salt content and thus salt content has to be determined
separately for calculating curd content.

Apparatus
A. Gooch crucible or sintered funnel - with filter flask and adapter.
B. Glass funnel with folded 12.5 cm Whatman filter paper Grade 1.
C. Flat bottom flask: 250 ml capacity
D. Desiccator with efficient desiccant.
E. Asbestos.
F. Hot air oven: Maintained at 100 ± 1°C.
G. Conical flask: 250 ml capacity.
H. Glass beads
Reagent
n-Hexane or, alternatively, light petroleum hydrocarbon solvent
(petroleum spirit) with boiling range between 40 to 60°C. The reagent
shall not leave more than 1mg of residue after evaporation of 100m
Procedure
A. Prepare a mat in a Gooch crucible or sintered funnel. Dry it in a hot
air oven maintained at 100 °C, cool in the desiccator and weigh.
Alternatively, dry, cool and weigh ordinary glass funnel with folded 12.5

cm filter paper.
B. Melt the residue in the moisture dish and add 25 to 50 ml of
petroleum solvent and mix well.
C. Fit the crucible to the filter flask or place the funnel with filter paper
on a filter stand.
D. Wet the asbestos mat or the filter paper with petroleum solvent and
decant the fatty solution from the dish into the asbestos or the filter
paper, leaving the sediment in the dish.
E. Filter the solution and collect the filtrate in a clean, dried, tared 250
ml flat bottomflask containing 1 to 2 glass beads.
F. With the aid of a wash-bottle containing petroleum solvent, wash all
the fat and sediment from the dish into the crucible or the filter paper.
G. Finally, wash the crucible or the filter paper until free from fat,
collecting all the filtrate in the conical flask. Preserve the filtrate for the
determination of fat. Dry the crucible or filter paper in the oven
maintained at 100 °C for at least 30 min.
Note: If fat is to be determined only, transfer all the filtrate to a pre-dried
and weighed fat flaks containing 2-3 glass beads. Rinse the conical flask
with petroleum ether.
Evaporate the ether, first on the water-bath and then in the oven at
102±2°C for 1 houror till the time the constant weight is obtained.
Calculate the fat content form the residues obtained by using following
formula
% fat = (𝑊𝑒𝑖𝑔𝑡 𝑜𝑓 𝑓𝑎𝑡 𝑓𝑙𝑎𝑠𝑘+𝑓𝑎𝑡 𝑟𝑒𝑠𝑖𝑑𝑢𝑒𝑠)−𝑊𝑒𝑖𝑔𝑡 𝑜𝑓 𝑒𝑚𝑝𝑡𝑦 𝑓𝑙𝑎𝑠𝑘
𝑊𝑒𝑖𝑔𝑡 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 𝑡𝑎𝑘𝑒𝑛 𝑥 100
H. Cool in the desiccator and weigh. Repeat drying, cooling and
weighing until the loss of weight between the consecutive weighing does
not exceed 0.1 mg. Preserve the residue for the determination of salt.
Calculation
Curd and salt, % by mass (C) =(M1 − M2)M x 100
Where,M1 = mass in g, of the filter paper with residue; M2= mass in g,
of the filter paper alone; andM = mass in g, of the sample.
Percent Fat w/w = 100 - (M+C)
Where, M = Moisture percent
C = Curd & salt percent
Curd percent by weight is obtained by subtracting the value of salt
percent by weight from the value of C.
Determination of Salt Content in Butter
(Volhard's Method)
In this method, salt present in the butter sample is extracted with hot
water from the dried fat-free residue obtained in moisture
determination. The chlorides are precipitated by adding excess of silver
nitrate. The unused silver nitrate is titrated with potassium thiocyanate
using ferric ammonium sulphate indicator.
Reagents
A. Standard silver nitrate solution: 0.05 N, standardized against standard
sodium chloride. B. Nitric acid: sp. gr. 1.42 approx. 70 % (m/m).
C. Nitric acid: Approximately 5 N.
D. Ferric ammonium sulphate indicator solution: Dissolve 50 g of ferric
ammonium
sulphate [Fe2(SO4)3.(NH4)2SO4.24H2O] in 95 ml of water containing
5 ml of 5 N nitric acid.
E. Standard potassium thiocyanate (KCNS) solution (Approx. 0.05 N):
Standardized against standard silver nitrate. Weigh approx. 5.25 g
KCNS and dissolve in 1 L water.
Allow to stand overnight and filter, if necessary, to get a clear solution,
standardize by titration against 0.05 N AgNO3 and dilute with requisite
volume of water to get exactly 0.05 N KCNS solution.
Apparatus
A. Beakers: 100, 250 ml capacity.
B. Volumetric flask: 100 ml, 1 L capacity.
C. Conical flask: 250 ml capacity.
D. Water-bath: Maintained at 60 to 70°C.
Ag+ (excess) + Cl- AgCl (solid)
Ag++ SCN- AgSCN (solid)
Fe+3 + SCN- [FeSCN]+2(Reddish brown)
Apparatus
A. Beakers: 100, 250 ml capacity.
B. Volumetric flask: 100 ml, 1 L capacity.
C. Conical flask: 250 ml capacity.
D. Water-bath: Maintained at 60 to 70°C.
Procedure
A. Extract the salt from the residue of curd and salt by repeated washing
of the Gooch crucible or filter paper with hot water, or by placing the
crucible or filter paper in a beaker of hot water.
B. Collect the rinsing in a 100 ml volumetric flask passing the solution
through a filter paper. Allow to cool to room temperature and make up
to volume.
C. Take 25 ml water extract into a 250 ml conical flask, and add an
excess (normally 25 to 30 ml) of 0.05 N silver nitrate solution.
D. Acidify with nitric acid; add 2 ml of the indicator solution and 1 ml
nitrobenzene.
Mix and determine the excess of silver nitrate by titration with the
potassium thiocyanate solution until the appearance of an orange tint,
which persist for 15 s.
E. In the same manner determine the equivalent of 25 ml or the added
amount of silver nitrate as thiocyanate using the same volumes of
reagents and water.
Calculation
NaCl, % by mass = 23.38 x N x (A−B) M
whereN = normality of potassium thiocyanate solution (0.005 N);
A = volume in ml, of potassium thiocyanate in blank titration;
B = volume in ml, of potassium thiocyanate in the sample titration; and
M = mass in g, of the butter sample.