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DETERMINATION OF MOISTURE CONTENT

Name:T.L.V. PEIRIS
Index no : GS/MSc/Food/3630/08

Date Performed: 21/11/2009


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 the product

The 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 1050C 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 H2O 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.

MATERIALS AND METHOD

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MATERIALS

Moisture dish made of stainless steel


Oven maintained at 105 0C
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

1st Sample/g 2nd Sample/g 3rd Sample/g


Weight of dish 44.4284 54.2295 46.9371
Weight of sample(g) 5.0418 5.0785 5.0197
Initial weight(g) 49.4702 59.3080 51.9468
1st time 49.3185 58.8285 51.5003
Weight of dish + lid
2nd time 48.9075 55.8084 51.4825
+ sample(after
3rd time 48.7088 54.4858 51.1642
drying)(g)
4th time 48.7088 54.4858 51.1642

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

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1st Sample 2nd Sample 3rd Sample
Weight of dish (g)( m1 ) 44.4284 54.2295 46.9371
Weight of sample before drying(g) 5.0418 5.0785 5.0197
Weight of dish (g)+ Weight of 49.4702 59.3080 51.9468
sample before drying(g) ( m2 )
Weight of dish+sample(after drying) 48.7088 54.4858 51.1642
(g)( m3 )
m2-m3 x 100 15.10 16.19 15.19
m2-m1

Moisture Content of Cinnamon = 15.10+16.19+15.19 = 15.69 %


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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

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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.

Dean & Stark Distillation Unit

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

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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

Volume of the samples Volume indicated in graduated tube


from the sample volume
2 ml of water 1.95 ml
Sample X ml 1.03ml

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
= 10.17 %
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.


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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.

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