(GS/M.Sc.

/FOOD/3608/08)

Determination of
moisture
B.K.K.K. Jinadasa

2010

09TH JANUARY 2010

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1.1. Introduction

Moisture determination is one of the most important and most widely used measurements in the
food industry. Since the amount of dry matter in a food is inversely related to the amount of
moisture it contains, moisture content is of direct importance to the processor and the consumer.
Moisture determination is important in following areas.

· Legal and Labeling Requirements. There are legal limits to the maximum or minimum
amount of water that must be present in certain types of food.
· Economic. The cost of many foods depends on the amount of water they contain - water
is an inexpensive ingredient, and manufacturers often try to incorporate as much as
possible in a food, without exceeding some maximum legal requirement.
· Microbial Stability. The propensity of microorganisms to grow in foods depends on their
water content. For this reason many foods are dried below some critical moisture content.
· Food Quality. The texture, taste, appearance and stability of foods depend on the amount
of water they contain.
· Food Processing Operations. Knowledge of the moisture content is often necessary to
predict the behavior of foods during processing, e.g. mixing, drying, flow through a pipe
or packaging.

Foods are heterogeneous materials that contain different proportions of chemically bound,
physically bound, capillary, trapped or bulk water. In addition, foods may contain water that is
present in different physical states: gas, liquid or solid. The fact that water molecules can exist in
a number of different molecular environments, with different physicochemical properties, can be
problematic when determining the moisture content of foods.
Measured value of the moisture content of a particular food may depend on the experimental
technique used to carry out the measurement. Methods for the determination of moisture can be
divided into drying methods, distillation procedures, chemical assays, and physical procedures.

Moisture determination methods:

Ø Oven drying method
Ø Sand Pan Technique: Mix sample with sand to increase surface area and prevent crusting
on surface.
Ø Microwave Drying: More rapid than oven techniques and more expensive, but speed
makes it economical for the food industry. Problems of uneven heating.
Ø Infrared Drying: Penetrating heat goes into the sample for drying. Problems with uneven
heating and poor accuracy.
Ø Reflux Distillation: Moisture distilled from an immiscible solvent. May be used for very
low moisture samples. Problems of emulsions and water droplets sticking to glassware.
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1.2. Determination of moisture by oven drying method

1.2.1. Material

Moisture dish made of stainless steel

Oven maintained at 105ºC
Weighing balance

Sample – Cinnamon balk

1.2.2. Procedure

5 g of crushed cinnamon was weighed into three moisture dishes (previously dried in the oven
and weighed) separately and kept in the oven for drying with the lids alongside for three hours.
Drying was carried out till the samples obtained constant weights.

1.2.3. Calculation

1.2.4. Results

Wt of empty Wt of sample Wt after drying (sample Wt of sample Moisture content

container (g) (g) + container) (g) after drying (g) (%)
68.8049 5.0031 73.2592 0.5488 10.9692
70.0481 5.0133 74.5002 0.5612 11.1942
71.0111 5.0238 75.4450 0.5899 11.7421

Moisture content – 11.30 %

1.2.5. Discussion

The rate and extent of moisture removal depends on the size and shape of the sample, and how
finely it is ground. The greater the surface area of material exposed to the environment, the faster
the rate of moisture removal.

Some samples tend to clump together or form a semi-permeable surface crust during the drying
procedure. This can lead to erroneous and irreproducible results because the loss of moisture is
restricted by the clumps or crust. For this reason samples are often mixed with dried sand to
prevent clumping and surface crust formation.
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Under normal laboratory conditions pure water boils at 100 o C. Nevertheless, if solutes are
present in a sample the boiling point of water is elevated. Consequently, the rate of moisture loss
from the sample becomes slower than expected.

Free water is most easily removed from foods by evaporation, whereas more severe conditions
are needed to remove chemically or physically bound water. If the temperature of drying is too
high, or the drying is carried out for too long, there may be decomposition of some of the heat-
sensitive components in the food. This will cause a change in the mass of the food matrix and
lead to errors in the moisture content determination. Foods that are particularly susceptible to
thermal decomposition should be analyzed using alternative methods, e.g. chemical or physical.

It is often assumed that the weight loss of a food upon heating is entirely due to evaporation of
the water. In practice, foods often contain other volatile constituents that can also be lost during
heating, e.g., flavors or odors. For foods that do contain significant amounts of volatile
components (e.g. spices and herbs) it is necessary to use alternative methods to determine their
moisture content, e.g., distillation, chemical or physical methods.

It is important to use appropriate containers to contain samples, and to handle them correctly,
when carrying out a moisture content analysis. Typically stainless steel pans are used because
they have a high thermal conductivity. These pans usually have lids to prevent spattering of the
sample, which would lead to weight loss and therefore erroneous results. Pans should be handled
with tongs because fingerprints can contribute to the mass of a sample. Pans should be dried in
an oven and stored in desiccators prior to use to ensure that no residual moisture is attached to
them.

Advantages: Precise; relatively cheap; Easy to use; Many samples can be analyzed
simultaneously

Disadvantages: Destructive; Unsuitable for some types of food; Time consuming

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1.3. Determination of moisture by Dean and Stark distillation method

1.3.1. Materials

Dean and Stark distillation unit

Measuring cylinder
Beaker
Drying oven
Weighing balance

Amyl alcohol and Toluene

1.3.2. Method

All the glass ware were thoroughly cleaned and dried in the oven before starting the practical. 75
mL of amyl alcohol and 50 mL were mixed then 50 mL solution and few pumice stones were
added to the distillation flask and the calibrated arm was fixed to the flask. Flask was heated with
the contents for about 30 minutes till the graduated tube obtained a constant volume of water.
Then 2 mL of water was added to the flask and boiled until a constant volume obtained. (This
was done to calibrate the apparatus).
After the calibration step 2 g of crushed cinnamon sample was placed in the flask containing
toluene and allowed to distill until a constant water level was obtained.

1.3.3. Results and calculations

Weight of sample = 2.0186 g

Amount of water obtained from 2 ml of water = 2.0 mL
Water level after sample distillation = 2.15 mL
Water gained from the sample = 0.15 mL

Amount of water collected from the sample = 2 ×0.15 = 0.15

2
Moisture content of the sample = 0.15 × 100
2.0186

= 7.43 %

1.3.4. Discussion

This method is used to measure the moisture content of samples which contain low moisture
level and high volatile content. 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 results obtained in oven drying method and distillation method are 11.30 % and 7.43 %
respectively. As the results show the value obtained from the distillation method should be lower
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than the value obtained from the oven drying method since in the oven drying method volatile
compounds may also remove while drying and that will counted as moisture loss.
There are a number of practical factors that can lead to erroneous results:
Emulsions can sometimes form between the water and the solvent which are difficult to separate;
water droplets can adhere to the inside of the glassware, decomposition of thermally labile
samples can occur at the elevated temperatures used.

Advantages:
Suitable for application to foods with low moisture contents; Suitable for application to foods
containing volatile oils, such as herbs or spices, since the oils remain dissolved in the organic
solvent, and therefore do not interfere with the measurement of the water; Equipment is
relatively cheap, easy to setup and operate; Distillation methods have been officially sanctioned
for a number of food applications.

Disadvantages:
Relatively time-consuming; Involves the use of flammable solvents, difficulties in reading the
meniscus, adherence of moisture droplets to the glass, over boiling, incomplete evaporation of
water and under estimation of moisture contents and distillation of water soluble compounds.

Adherence of water to the walls of the condenser tube or sides of the receiving tubes can
generally be prevented by using thoroughly cleaned glass ware.
Incomplete recovery of water due to the formation of an emulsion can sometimes be avoided by
adding small amounts of amyl or isobutyl alcohol.
Foods in powder form tend to bump during the distillation through overheating on the bottom of
the flask. This can be overcome by introducing pumice stones.
Dispersing the tested material on diatomaceous earth is useful with many viscous foods rich in
sugar or protein.