1.

DETERMINATION OF MOISTURE CONTENT BY OVEN DRYING

METHOD
INTRODUCTION
The moisture content which results from oven drying method depends on the type of food stuff used. The
determination of moisture in a food is done for many purposes such as assessment of quality, quality
control, quality assurance, detection and estimation of adulteration, conformity with food standards and
other statutory requirement, calculation of total food solids content, assessment of stability, shelf life and
storage life.
Water in a food item can be present in 2 ways:
•
Free water (which is physically linked to the food matrix and easily
lost by evaporation or drying as a separate constituent)
•
Bound water ( include water molecules chemically bonded to ionic and
polar groups or water of crystallization or hydrates which is difficult to remove)
These types may occur in varying quantities in food and are held by physical chemical forces of diverse
nature. Even though the accuracy and precision of moisture result is low; the reproducibility results can be
obtained under a set of standardized condition.
The water activity of any product depends on,
•
The chemical composition of food
•
The state of aggregation of its constituent
•
The water content
•
Temperature of thThe shelf life of the product depends on water activity. Moisture can be determined by

using following methods,

•
Thermal Drying method
Drying either hot air oven at 105 0C in 2-3 hours or in vacuum ovens which is widely used for sugar based
foods. The measurement of the weight loss which results due to the evaporation of H 2O at or near boiling
point is taken here. The loss in weight depend on the particle size, weight of the sample used, type of the
dish and temperature variation in the ovens etc.
•
Chemical assay
This is based on the non-stoicheometric reaction of water.
•
Physical method
Involves physical and physiochemical reaction in food.
Oven drying method is widely used. The weight loss due to the removal of water by heating under specific
conditions is considered here. The loss of weight due to drying is considered as a measure of the
moisture content of the sample.
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MATERIALS AND METHOD

MATERIALS
Moisture dish made of stainless steel
Oven maintained at 1050C
Weighing balance
Cinnamon sample
METHOD
About 5 g of the sample was weighed in to a moisture dish which was previously dried in an oven and
weighed. Then the uncovered dish was dried along side for 21/2 hrs. The dish was covered and was
transferred to desiccators and weighed quickly as possible as the dish was cooled. The heating and
weighing procedures was repeated until successive weight did not differ by more than one milligram .Loss
in weights were recorded.
RESULTS AND CALCULATIONS
RESULTS

CALCULATIONS
Moisture % m/m
=
Weight loss
x 100
Weight of the sample
=
m2-m3
x 100
m2-m1
m1
=
Weight of empty dish
m2
=
Weight of empty dish + sample before drying
m3
=
Weight of empty dish + sample after drying

DISCUSSION

Oven drying method is widely used in determination of moisture. Water is removed due to heating at 105
°C. Loss of weight due to vaporization of water is taken as weight of moisture. But spices like cinnamon
contain volatile oil in addition to moisture and these volatile oils also get loss during oven drying. Due to
this the weight loss due to the loss of volatile oils also gets counted for moisture determination. This is the
main disadvantage of oven drying method. This method is not suitable to determine the moisture content
of thermally unstable compounds and this method removes only free water. Since oven drying method is
simple, low cost and easy, it is widely used for routine analysis.
The accuracy of results of moisture determination is affected by, drying temperature, relative humidity,
particle size of sample, handling method of sample, amount of sample, type of evaporation dish, variation
in temperature inside the oven. To minimize these errors various precautions should be taken. i.e. sample
should be dried in stainless steel containers, which is not decompose during heating. Three consecutive
samples were carried out to eliminate the errors of the handlers, usually 5 g of ground sample was taken
to facilitate the drying, and this encourages the evaporation because particle size is small

2. DETERMINATION OF MOISTURE CONTENT BY DEAN STARK

DISTILLATION METHOD
INTRODUCTION
Distillation methods are particularly useful for foods with low moisture content and for products containing
volatile oils such as herbs and spices. Since the oils remain dissolved in the organic solvent the
disadvantages are that they have often been reported to give low values and their requirements for
flammable solvent pose small but significant hazards

The Dean and Stark method is widely used in determination of moisture. A known weight of food is placed
in a flask with an organic solvent such as xylene or toluene. The organic solvent must be insoluble with
water; have a higher boiling point than water; be less dense than water; and be safe to use. The flask
containing the sample and the organic solvent is attached to a condenser by a side arm and the mixture is
heated. The water in the sample evaporates and moves up into the condenser where it is cooled and
converted back into liquid water, which then trickles into the graduated tube. When no more water gets
collect in the graduated tube, distillation is stopped and the volume of water is read from the tube.
Distillation with a boiling liquid provides an effective means of heat transfer, the water is removed rapidly.
If the boiling liquid is lighter than the water, the collecting trap usually contains a tube with tap at the
bottom and calibrated upward. This form requires reading only one meniscus in measuring the amount of
collected water. The calibrated portion of the tube may be cooled by a water bath to standard
temperature.
Many difficulties may arise in the determination of moisture by distillation method. These include relatively
low precision of the receiving measuring device, difficulties in reading the meniscus, adherence of
moisture droplets to the glass, over boiling, suitability of water in the distillation liquid, incomplete
evaporation of water and underestimation of moisture contents, and distillation of water-soluble
components. Adherence of water to the walls of the condenser tube of sides of the receiving tubes can
generally be prevented by using thoroughly cleaned glassware. Use of small amount of wetting agent will
also

improve meniscus reading. Incomplete recovery of water due to the formation of an

emulsion can be avoided by adding small amount of amyl or isobutyl alcohol.
MATERIALS AND METHOD
MATERIALS
Dean Stark Distillation unit
Measuring cylinder
Beaker (250 ml)
Drying oven
Weighing balance
Toluene
METHOD
All the glass wares were cleaned and dried in an oven. 50 ml Toluene solution and some pumice stones
were added to a boiling flask. The calibrated arm was fixed on the flask and was boiled until the
graduated tube gets constant volume of water.2.00 ml of water was added to the flask and was boiled
until constant volume obtained. Then accurately weighed (about 2 g) was added and boiled until the
graduated tube indicates a constant volume for the extracted water layer. This is equal to the same value
of water in gram.

RESULTS AND CALCULATIONS

RESULTS
CALCULATIONS
% moisture m/m = Volume of water collected in the graduated tube X 100
Weight of the sample
Volume of water added to the flask
=
2.0 ml
Recovered volume of water after distillation
=
1.95 ml
Correction factor
=
2.0 / 1.95 = 1.026
Weight of sample
=
2.0172 g
Volume of water contained in the sample
=
0.2 ml
Volume of water (x correction factor)
=
0.2 x 1.026 = 0.2052
Moisture content %
=
0.2052/2.0172 x 100

Moisture content of cinnamon

=
10.17 %

DISCUSSION

In this practical we have used toluene as the solvent. There are few reasons to do so,

Advantages in using toluene,

1.) It is immiscible with water .Then we can get a measurement.
2.) Low density than water.
3.) It has a high boiling point. So we can heat the sample till we get the whole water
amount out.
4.) Toluene will dissolves all the volatiles in the sample. So we can get the pure
measurement.
Advantages in this technique,
1.) Less contamination can happened
2.) Fewer utensils needed.
3.) No need to pay much attention.
Disadvantages in this technique
1.) Water drops will remains on the walls of the distillate tube. So can get a wrong
measurement.
Dean & Stark method is suitable for determination of moisture in foods containing volatile matters. But this
method is not suitable for routing testing and is employed only when conventional oven drying method is
not suitable. It is also not suitable determine small amount of water. It needs little attention, no
contamination.
The solvent should be irreversible, higher boiling point and lower specific gravity than water. Since
toluene has high boiling point (110-111 °C), lower density (0.86 g/ml) and immiscible with water, it was
used as the solvent. Other than the toluene, heptane, xylene a mixture of N-amyl alcohol and xylene can
be used as solvent. For high precision, a distillation factor correction was done by standardizing the
apparatus with known amount of water and measuring the recovered amount water.
Method of moisture determination is varied according to the sample to be tested. i.e. viscose foods such
as oils, fats done by adding clean dry sand , which facilitate evaporation by increasing surface area and to
avoid formation of films and crusts. Due to the experimental errors we got higher value for moisture
content.

REFERENCES:
•
Pearson, David, 1976, The chemical analysis of foods, First-4th ed. By H.E.Cox

Mendham J, 2003, Vogel’s Quantitative Chemical Analysis, Sixth edition.,

Pearson Education(Singapore)Pte.
•
Potter Norman N, Hotchickjss Joseph H, Food Science, Fifth edition, Cbs
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