Chemistry

Department

CHM4383
Assignment topic
‘Analysis of Ice Cream’
Instructor: Prof. Ayman Qayyum

Submitted by
Usman Ghani Section: CF3-17
ID: R2F17BSCH0062 Submission Date: 7th May
Semester: 8th Due Date: 7th May
Analysis of Ice Cream
Introduction:

Ice cream is a frozen blend of a sweetened cream mixture and air with added flavourings. It is usually made from
dairy products such as milk and cream combined with fruits or other ingredients and flavours. It is sweetened with
sugar or sugar substitutes. The mixture is stirred to incorporate air spaces. The result is smooth, semi-solid foam that
is solid at very low temperature (<2°C or 35°F)

Compositions
Milkfat >10% - 16%
Milk solids-not-fat (snf): 9% - 12%
Sucrose 10% - 14%
Corn syrup solids 4% - 5%
Stabilizers 0% - 0.4%
Emulsifiers 0% - 0.25%
Water 55% - 64%

Analysis:
• Sampling
• Estimation of Fat
• Estimation of Water
• Estimation of Sugars
• Estimation of Protein
• Estimation of MSNF Content

Preparation of Sample of Ice Cream

For samples taken in small packages, remove the packaging and place the sample in a clean, dry container
fitted with an airtight closure. For samples taken from bulk or from large packages, keep them in their sampling
containers.

Plain Product

Allow the sample to soften at room temperature. It is not advisable to soften the ice-cream sample by heating
on water bath or over flame because melted fat tends to separate and rises to the surface. After softening of ice-
cream, mix it thoroughly by stirring with spoon or eggbeater or by pouring back and forth between beakers.

Fruit nut and Chocolate Ice-Cream containing Insoluble Particles

Use a mixer capable of comminuting product to fine, uniform pulp. Use 100 - 200 g of ice-cream sample to
fill the cup of mixer full to about one-third. Melt the product at room temperature or in an incubator at 37°C in a
closed container. Transfer entire contents to the mixer cup and mix until insoluble particles are finely divided (about
3-5 min for fruit ice-cream and up to 7 min for nut ice-cream). Alternatively, the product may be grounded in
porcelain or glass pestle and mortar.

Transfer the mixed ice-cream sample to a suitable container for convenience in weighing. After weighing
operation, return the remainder of the ice-cream sample to the refrigerator, preferably at a temperature not exceeding
-15°C.

In case of ice cream, where the chocolate or similar covering portions forms a separate layer, it shall be
removed and only the ice cream portion shall be taken for analysis.

Note: For determination of over-run in ice-cream, the entire ice-cream carton/cup should be taken as such.

Determination of Total Solids in the Ice Cream

Apparatus

A. Flat bottomed dishes of Aluminium, Nickel or Stainless steel not affected by boiling water, 7-8 cm in diameter
and not more than 2.5 cm deep provided with short stirring rods having a widened flat end.

B. Sand which passes through 500 micron I.S sieve and is retained on 180 micron sieve. It shall be prepared by
digesting with conc. HCl followed by thorough washing with water. It shall be dried and ignited to red heat.

C. Oven: Well ventilated and maintained at 100 ± 2°C.

Protocol

Heat the moisture dish containing 20 g of prepared sand and glass stirring rod in the oven for 1 hour. Cool and
weigh. Add about 5 g of sample into the dish. Add a few drops of water to assist in spreading the sample with glass
rod. Place dish on a boiling water bath for 29 - 30 minutes. Wipe bottom of dish and transfer to the air oven. Dry for
about 4 hours, remove dish to an efficient desiccator, allow to cool and weigh. Replace dish in oven for a further
period of 1 hour, transfer to desiccator, allow it to cool and weigh. Repeat the process of heating and cooling till
consecutive weighing agree within
0.5 mg. Calculate total solids from loss in weight observed.

Determination of Weight per Unit Volume or Over-run in Ice Cream

Over-run is usually defined as the volume of ice-cream obtained in excess of the volume of the mix. It is
usually expressed as a percentage. This increased volume is composed mainly of the air incorporated during the
freezing process. The amount of air which is incorporated depends upon the composition of mix and the way it is
processed. In this test, the volume of water and alcohol used corresponds with the volume of air originally contained
in the ice-cream and the difference between the sum of these two and capacity of the flask is equivalent to the volume
occupied by the sample.

Apparatus

A. Beaker: 400 ml.

B. Volumetric flask: 250 ml.

C. Glass funnel.

Reagent: n-Amyl alcohol (sp. gr. 0.817).

Protocol

A. Weigh a unit of ice-cream and from it calculate the weight of ice-cream per litre. For example, 200 ml of a full
carton of ice-cream can be obtained, the ice-cream carefully removed and the empty dry carton weighed. The
difference in weights between the carton when filled and when empty is, therefore, the weight of 200 ml of frozen
ice- cream. Five times this weight would then equal the weight of a litre. To determine the weight of the mix,
proceed as below (B):

B. Weigh and record the exact weight of a clean, dry 400 ml beaker. Into the beaker, weigh exactly 130 g of the
frozen ice-cream.

C. Place the beaker in water bath warmed to 49°C and melt.

D. Weigh and record the exact weight of a 250-ml volumetric flask.

E. Using a glass funnel, transfer 130 g of melted ice-cream into the 250 ml volumetric flask.

F. Add exactly 10 g of n-amyl alcohol to the flask and mix to break the surface tension of the melted ice-cream and
release the incorporated air. 10 g of n-amyl alcohol occupies a volume of 12.24 ml.

G. Cool the flask with contents to 15.5°C using a cold water or ice water bath.

H. Rinse the beaker containing melted mix with several small rinsing of water, adding each rinse to the 250 ml flask.

I. Again cool the flask with contents to 15.5°C and using the final rinse water, bring the volume to 250 ml mark.
The bottom of the meniscus should correspond with the mark when temperature is exactly 15.5°C. Dry the
outside of the flask and reweigh.

J. Calculate the weight in g of the contents. Calculate the weight in g of the water added
to the flask. Calculate the volume in ml occupied by the sample of ice-cream. Determine the sp. gr. of the mix by
dividing its weight (130 g) by the volume in ml, which it occupied. Determine the weight in g per litre of mix by
multiplying by the specific gravity.

Determination of Fat in Ice-Cream (Rose-Gottlieb method)

Accurately weigh 4-5 g of the thoroughly mixed sample directly into fat extraction flask or Mojonnier tube,
using free flowing pipette, dilute with water to approximately 10 ml, working sample into lower chamber and mix by
shaking. Add 2 ml ammonia; mix thoroughly, heat in water bath for 20 min at 60°C with occasional shaking, cool
and proceed as in Section 1.3.4.2.2 (beginning "Add 10 ml alcohol and mix well"). Identify the clear extracted fat to
confirm whether it is dairy fat or not by checking refractive index at 40°C and GLC composition as per clause 1.2.11.

Determination of Protein (Kjeldahl method) in Ice Cream

The protein content is determined from the organic Nitrogen content by Kjeldahl method. The various
nitrogenous compounds are converted into ammonium sulphate by boiling with concentrated sulphuric acid. The
ammonium sulphate formed is decomposed with an alkali (NaOH) and the ammonia liberated is absorbed in excess
of standard solution of acid and then back titrated with standard alkali.

Apparatus

A. Kjeldahl digestion flask - 500 or 800 ml

B. Kjeldahl distillation apparatus, -same digestion flask fitted with rubber stopper through which passes lower end of
efficient rubber bulb or trap to prevent mechanical carry-over of NaOH during distillation.

C. Conical flask, 250 ml

D. Burette 50 ml.

Reagents

A. Concentrated Sulphuric acid – sp.gr. 1.84

B. Sodium Hydroxide solution (45%): Dissolve 450 g of Sodium Hydroxide in 1000 ml water

C. Standard Sulphuric acid solution (0.1 N)

D. Standard Sodium Hydroxide solution (0.1 N)

E. Methyl Red Indicator solution: Dissolve 0.5 g methyl red in 100 ml of alcohol

Protocol

Weigh quickly about 5-8 g of the prepared ice-cream sample and transfer to a 500 or 800 ml Kjeldahl flask
taking care to see that no portion of the sample clings to the neck of the flask. Add 0.5g of copper sulphate, 15 g of
potassium sulphate and 40 ml of concentrated sulphuric acid. Add two to three glass beads. Place the flask in an
inclined position on the stand in the digestion chamber and digest. Heat the flask gently at low flame until the initial
frothing ceases and the mixture boils steadily at a moderate rate. During heating rotate the flask several times.
Continue heating for about an hour or more until the colour of the digest is pale blue. Cool the digest and add slowly
200 ml of water. Cool, add a piece of granulated zinc or anti bump granules and carefully pour down the side of the
flask sufficient sodium hydroxide solution (450g/ litre) to make the contents strongly alkaline(about 110 ml) before
mixing the acid and alkaline layer. Connect the flask to a distillation apparatus incorporating an efficient flash head
and condenser. To the condenser fit a delivery tube which dips just below the surface of the pipetted volume of
standard acid contained in a conical flask receiver. Mix the contents of the digestion flask and boil until 150 ml have
distilled into the receiver. Add 5 drops of methyl red indicator and titrate with 0.1 N sodium hydroxide solution.
Carry out a blank titration.

1 ml of 0.1 N H2SO4 = 0.0014g N.

In case of dairy ice cream / kulfi calculate milk protein as N x 6.38 In case of Frozen Dessert calculate total protein
as N x 6.25

Determination of Added Starch in Ice Cream

The sample is made free from fat and the starch is precipitated with alcohol and made free from sugar. The
precipitated starch is subjected to acid hydrolysis. The hydrolysate is freed from proteins using lead acetate and
deleaded with ammonium oxalate. The reducing sugar is determined by Lane and Eynon method and multiplied with
0.9 to calculate the starch content.

Protocol

Weigh 20 - 50 g of ice cream sample into a 500 ml beaker depending on the approximate starch content of the
sample. Defat the sample with 5-6 washings with 15- 20 ml portions of petroleum ether (40-60°C). Add enough
water to make 100 ml, heat to 50-60°C (avoiding any gelatinisation of starch) and let stand for 1 hour stirring
frequently to ensure complete solution of sugars. Cool and add equal volume of alcohol, mix, let stand for 1 hour or
more.

Centrifuge for 20 minutes at approximately 4000 rpm so that the precipitate is closely packed at the bottom of
the centrifuge tubes. Filter the solution using Whatman filter paper No 1. Transfer the precipitate using 5% alcohol
on the filter paper. Wash the precipitate on the filter paper with successive 50 ml portions of 50% alcohol and filter
until the washings are sugar free.

Transfer the residue to a 500 ml conical flask with about 200 ml water and add 20 ml of conc. HCl of sp. gr.
1.125. Hydrolyse starch by refluxing in a boiling water bath for 2- 2 ½ hours. Cool, transfer the hydrolysate to a 250
ml volumetric flask, neutralise with Sod hydroxide and make it alkaline using litmus paper. Make up to volume.
Shake thoroughly. Allow to settle for 20 minutes and filter. Determine reducing sugars by Lane and Eynon method
and calculate starch content by multiplying total reducing sugars with 0.9.

Citation:
1) (A.O.A.C 17th edn,2000 Modified Official method- 925.50 for starch in confectionary)
2) (Pearson’s Composition and Analysis of Foods,9th edn,1991 page 17).
3) (Pearson’s Composition and analysis of foods 9th edn,1991 page 604).
4) (IS:2802: 1964 (Reaffirmed 1995) Specification for ice-cream. Bureau of Indian Standards, New Delhi).
5) (IS 2802 – 1964 – Specification for Ice cream. Bureau of Indian Standards, New Delhi.; Pearson’s
Composition and analysis of foods,9th edn,1991 page 604).
6) (IS 2802 – 1964 Specification for Ice cream. Bureau of Indian Standards, New Delhi /A.O.A.C 17edn,2000,
Official method 969.20. Ice cream and Frozen Desserts).