Report

on
Quality assurance of RAW MATERIALS

Submitted by Submitted to
SANTOSH YADAV (11715319/H1705) Dr. Yogesh Gath

feburary Month Analysis Report

At SAHARA BAKERS PVT LTD, AYODHYA U.P
 TESTING OF THE RAW MATERIALS THEIR SOP, TESTING
PROCEDURE.

1. SMP

ANALYSIS OF SKIMMED MILK POWDER

Inspection of vehicle: Quality Assurance personnel should check the vehicle for filth,
moisture, foreign matter and off odour. If the condition of vehicle is found satisfactory then
the consignment should be unloaded. If the condition of vehicle is not satisfactory then the
consignment should be rejected.
Sampling for Sensory and chemical evaluation: Six bags should be picked randomly per every 100
bags received. Random collection of sample is necessary to make a representative sample.

Note: kindly note that 6 bags / every 100 bags and not per whole consignment. For e.g. If you
receive 500 bags at your end you have to randomly collect 30 bags from them for sampling.

The whole lot should be unloaded and while unloading randomly bags should be collected and
marked separately for sampling.

Take out the sample from each bags separately. ( all the 6 bags separately and mark them from 1 to
6)
Make composite sample by mixing the smp from each bags in equal proportion. (for e.g. say 25 gm
from each bag. ) this composite sample should be made in laboratory.

The composite sample should be divided into two portions, one for analysis at unit end and one
should be sent to Mumbai.

Analyse the sample for all the parameters as per our Parle specification.

In case of failure in any parameter, re sampling from another bags and retesting should be done to
confirm the rejection.

a) Appearance: The material should be smooth in feel. If found gritty then material should be
rejected. The material shall be white or white with greenish tinge or light cream in colour. It
shall be free from lumps except those that break up readily under slight pressure. It shall be
free from extraneous matter
b) Odour: The odour of the Skimmed Milk Powder shall be pleasant and clean. It C should have
typical milky note.
In case of any deviation in appearance and odour the consignment should be rejected.
c) Taste: Prepare 10 % milk solution by dissolving 10 Powder in 90 ml of g of luke warm water
(40-50 °C). It should have a milky note, There should not be any objectionable or off taste.
(soda, chemical, muddy extreme sweet, salty). It is recommended that this test should be
done by a group of trained people. This test is the most important and in case of any slight
deviation the material should be rejected.

Chemical analysis is to be done once the consignment is found ok for the appearance, odour
and taste.
Protein and Ash estimation takes longer time; it should be initiated simultaneously.
The whole consignment of SMP should be kept aside and in case of failure the material
should be sent back. QA approval has to be sought before consuming the material in
production. In case of any deviation the consignment should be rejected.

ANALYSIS OF SKIMMED MILK POWDER

 MOISTURE

PROCEDURE:
Weigh about 5-10 g of sample in Aluminium dish & keep it in an air oven for hour at a
temperature of 100+/- 2° C. Then remove the dish from the oven cove it with lid & cool it in
a desiccator. After cooling, weigh the disc again && note t reading. Continue the heating for
half an hour, till the difference between two successive weight readings is 5 mg.

CALCULATION:

Moisture % = (W1- W2) x 100/W

W1= Weight of dish + sample before drying

w2 Weight of dish + sample after drying
W = Weight of sample
Total Milk Solids= (100 - moisture %)
  TITRATABLE ACIDITY
Principle: The method is based on the titration of the sample with sodium
hydroxide to phenophthelein end point and by comparing the colour colour
obtained by mixing the rosaniline acetate or cobalt sulphate in a known volume
of milk sample.
REAGENTS:
Standard Sodium Hydroxide (0.1 N): Dissolve 4 g of sodium hydroxide in 100
ml of distii water and transfer to a 1 litre volumetric flask and make up to thee
mark. Standardize using potassium hydrogen phthalate as follows: Transfer 0.5 g
of potassium bipthalate, previously dried at 105 oC for 2 hours and accurately
weighed to a flask and dissolve it in 75 ml of carbon dioxide free water. Add 2
drops of phenolphthalein indicator and titrate against NaOH solution to a
permanent pink colour. Each 204.2 mg of potassium bipthalate is equivalent to 1
ml of 1N NaOH.

Normality of NaOH = Wt. of Potassium biphthalate/0.2042 X Burette reading

Phenolphthalein TS: Phenolphthalein solution To 1 g of phenolphthalein solved

in 100ml of 95% ethyl alcohol, add 0.IN sodium hydroxide till a faint pin
olphthalein dis. le till a faint pine color is obtained and dilute to 200 ml with
distilled water. Rosaniline acetate solution (0.12 g rosaniline acetate dissolved in
95% ethyl a cohol containing 0.5 ml of glacial acetic acid and diluted to 100 ml.
(Store in dark). To prepare working standard, dilute 1 ml to 500 ml with 95%
ethyl alcoho and water in the ratio of 1:1. Cobalt sulphate solution Dissolve 1.5
gm of Cobalt sulphate in water and dilute to 100ml.
 Reconstitution of milk powder: Weigh 10 g of skim milk powder, make upto
100 ml with warm distilled water at 24°C. Stir exactly for 90 seconds. Allow the sample
to stand until the foam settles. The period of standing after mixing should not exceed
15 minutes
PROCEDURE: Pipette 10 ml of reconstituted milk into each conical flask. To one flask
add. 1 m of working solution of rosaniline acetate or cobalt sulphate solution. This
solution will be external end point reference. To the other flask add 2 ml of
phenolpthalein solution and titrate with 0.1 N sodium hydroxide, stirring to mix the
sample. Continue titration until the colour is Comparable to the reference solution.

CALCULATION:

% Acidity (as lactic acid)= 9xN NaOH X B.R./ Weight of Sample in 10 ml solution taken for test

Note: During reconstitution we are dissoiving 10 gms of sample to make 100 m volume, so for
%Acidity calculate the sample wt. In 10 ml solution takén for titration. Otherwise determine solid not
fat in the sample by deducting moisture and milk fat and calculate acidity in terms of ml of 0.1N
NaOH/ 10 gm Milk solids not Fat as per requirement of A 11.02.11 as shown below.
 Acidity in terms of ml. =vol of 0.1 NaOH required for titration x N of NaOH x100 x100 x10/[100
( M+F) ]xwt of sample

F= Fat % of sample

M= Moisture % of sample

 PROTEIN
Protein is determined by kjehldahl's method. The weight of the sample to be taken is 0.5 g.

PRINCIPLE:

Kjeldahl's method for determining total nitrogen involves first heating the sample with conc. Sulfuric
acid. The reaction rate is accelerated by adding sodium sulphate to raise the boiling point. The
catalyst used is copper sulphate. The oxidation causes the nitrogen to be converted to ammonium
sulphate. After making alkaline with conc. NaOH, the liberated ammonia is distilled into HCI. The
protein content is obtained by multiplying total nitrogen by an empirical factor.

REAGENTS: Conc. Sulphuric acid Copper Sulphate ( LR ) Sodium Suiphate ( LR ) Granulated Zinc

1.1 N HCI: 8.5 ml conc. HCI per 1000 ml of distilled water and then standardize as follows:
Accurately weigh about 0.15 g of primary standard anhydrous sodium carbonate, that has been
heated in the oven at a temp of 270 °C for 1 hr. Dissolve it in 100 Or Water and add 2 drops of
methyl red TS. Titrate with HCI to faint pink colour. Heat the solution to boiling and continue
the titration until the pink colos. doesn't disappear. Each 52.99 mg of sodium carbonate is
equivalent to 1 mi 0.1 N HCI.

Normality of HCI =Wt. of Sodium bicarbonate/ml of HCI X 0.05299

0.1 N NaOH: 4 g of Analar Sodium Hydroxide per 1000 ml of distilled wateran. then standardize as
follows: Transfer 0.5 g of potassium bipthalate, previously dried at 105 °C for 2 hrs ane
accurately weighed to a flask and dissolve it in 75 ml of carbon dioxide free water Add 2 drops
of phenolphthalein indicator and titrate against NaOH solution to permanent pink colour. Each
204.2 mg of potassium bipthalate is equivalent to 1 ml of 0.1 N NaOH

Normality of NaOH =Wt. of Potassium bipthalate/ 0.2042 X ml of NaOH used for titration

45 % NaOH: 45 g NaOH in 100 ml of distil water

Methyl red indicator: 0.1 g of powder in 100 ml of alcohol.

PROCEDURE:

Weigh accurately about 0.5 g. of sample and transfer to a Kjeldahl's digestinn flask. Add 0.3 g. of
CuSO4 and 10 g of Na2SO4 to the flask. Add 25 ml of conc. H2SO4 and heat the flask gently in an
inclined position till the clear soln. is obtained. Then heat the flask on a high flame for 3 hrs (total
digestion time 3.5 to 4 hrs). Then cooi the digestion mixture to the room temp. Wash the digest into
the distillation assembly. To the the distilling flask with distilled water. Arrange the distillation
assembly. To thes receiving flask add 50 ml. of 0.1 N HCI using a volumetric (bulb) pipette with 2-4
drops of methy! red indicator. Connect the distillation apparatus with the delivery tube dipping in
the HCI solution. To the distillation flask add Zn metal pieces Then carefuliy add digestion mixture to
the flask. Rinse it with water. Add 90 ml of 45% NaOH soln. to it. Add sufficient water to the
assembly flask. Check whether thet is airtight. Start the water flow through the condenser. Start
heating the solution. Distil the liberated NH3 into HCI soln. Continue the heating till thrice the initial
vol. of HCI in the receiving flask is obtained. Open the tap & wash down the condenser & the
delivery tube into the receiver. Now put off the burner. the distillate with 0.1 N NaOH till pale
vellow colour is obtained. Perform the blank i.e. take 50 ml. of 0.1N HCI in a beaker using a
volumetric (bulb) pipette and titrate against the 0.1 N NaOH used for the test. Titrate For the
calculation on MSNF basis find out the Fat % by soxhlet method and take the value for calculation.

CALCULATIONS:
% Nitrogen = (B S) X 1.4 X normality of NaOH/ Wt. of the sample

% Protein On MSNF Basis = % nitrogen x empirical factor x 100/ 100 (Moisture% + Fat %)

 DETECTION OF UREA AS ADULTERANT

Method 1

REAGENTS

1. Ethanol

2. Concentrated HCI

3. 4-Dimethyl amino benzaldehyde

4. Indicator: Dissolve 1.6 g of 4 Dimethyl amino benzaldehyde in 10 .:m alcohol containing 10 % HCI

PROCEDURE

Prepare 10% solution of Skimmed Milk Powder. Take 5 ml of this solution in tube followed by 5 ml
of indicator. Distinct yellow colour indicates presence of urea.

Method 2

Reagents

1.Prepare 10% solution of Skimmed milk Powder. Take 5ml. In a test tube. gms of soyabean
powder. Mix the contents thoroughly by shaking the e tube. After 5 minutes, dip a red litmus paper
in it. Remove the paper after 1. minute. A change in colour from red to blue indicates the presence
of urea in the sample.

2. If required maintain a positive/ standard tube treating the 5 ml milk sout with 0.1 gm urea
simultaneously in the same manner as given in above st no. 1. to compare the colour change.

 DETECTION OF SUCROSE AS AN ADULTERANT

Milk powder adulterated with sucrose can be detected qualitatively by performing following test

SUCROSE TEST: Take 10 ml of 20% milk solution. Add 0.1 g of resorcinol and 2- 3 drops of conc. HCl
and boil in water bath for 2 min. A rose red colour indicates the presence of sucrose.
DETECTION OF STARCH AS AN ADULTERANTS: Milk powder adulterated with starch can be detected
qualitatively by performing following test

STARCH TEST:

REAGENT: lodine solution: Add sufficient iodine to 100 ml of 1 % potassium iodide soiution to
colour it deep yellow

PROCEDURE Boil 5 ml of milk sample for 1 min and cool. Add 2-3 drops of iodine solution. A
characteristic blue-purple colour indicates the presence of starch. Result should always be negative.

 DETECTION OF SOYA-FLOUR AS AN ADULTERANT

REAGENTS: 5% Urea solution OTHERS: Water bath at 40 °C, Litmus paper

PROCEDURE:

1. Take 0.5 gm of the sample under examination & mix it with 5 ml of a 5%% Solution of Urea.

2. Stopper the tube and heat at 40°C in a water bath for 3 hours placing a strip of red litmus paper
at the side

3. The litmus paper should be placed in such a way that it should not touch the sides of a test tube.
Paper should hang at the top of the test tube and also paper should not be dipped in the test
solution. lue owing to th

4. If Soya flour is present the litmus paper should be coloured blue liberation of ammonia. .

5. if required maintain a positive/ standard tube treating Soya bean f Simultane0usly in the same
manner as for SMP sampe. bean flour there is

6. For Blank directly heat 5ml of 5% urea solution to confirm that there is change in the colour of
litmus.

 DETECTION OF AMMONIUM COMPOUNDS AS ADULTERANT

REAGENTS:

NESSLER'S REAGENT:

Dissolve 8 g of mercuric chloride in 150ml. of distilled water, 60 g. of sodium hydroxide in 150ml. of

distilled water and 16 g potassium iodide in 150 ml, distilled water to make three solutions. Add
mercuric chloride solution and sodium hydroxide solution and mix well. Then add potassium iodide
solution and mal the volume up to 500 ml. Allow the solution to stand till it becomes clear a decant
to a well stoppered bottle.

SAMPLE PREPARATION: Make 10 % solution of Skimmed Milk Powder dissolving 10 g of SMP in 90

ml. of warm distilled water

PROCEDURE: Take 1 ml. SMP solution in the test tube and add 2 ml. of Nessler's Shake reagent. the
contents. Appearance of orange colour with brownish tinge or darker intensity indicates presence of
ammonium compound.

 DETECTION OF AMMONIUM SULPHATE AS ADULTERANT

REAGENTS: Citric acid &5% Barium chloride solution
 SAMPLE PREPARATION: Make 10 % solution of Skimmed Milk Powder byi dissoiving 10 g. of SMP in
90 ml. of warm distilled water.

PROCEDURE: 5 ml of hot milk solution is taken in a test tube and add 0.5 h ml 5% barium chloride.
Appearance of precipitate indicates the presence