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04 Moisture Analysis

The document discusses different methods for analyzing moisture content in food samples, including gravimetric methods using oven or vacuumed oven drying and azeotropic distillation. It outlines the principles, procedures, advantages, and limitations of each method. The gravimetric oven method involves weighing samples before and after drying to constant weight in an oven at 105°C. The vacuumed oven method dries samples under low pressure to allow water to evaporate at lower temperatures. Azeotropic distillation involves distilling water from samples using an immiscible solvent mixture. The document provides details on performing moisture analysis using the oven method on various food samples and calculating moisture content.

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169 views

04 Moisture Analysis

The document discusses different methods for analyzing moisture content in food samples, including gravimetric methods using oven or vacuumed oven drying and azeotropic distillation. It outlines the principles, procedures, advantages, and limitations of each method. The gravimetric oven method involves weighing samples before and after drying to constant weight in an oven at 105°C. The vacuumed oven method dries samples under low pressure to allow water to evaporate at lower temperatures. Azeotropic distillation involves distilling water from samples using an immiscible solvent mixture. The document provides details on performing moisture analysis using the oven method on various food samples and calculating moisture content.

Uploaded by

Melati Aprilani
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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Unit 3

Moisture Analysis

3.1. Course Objectives


After completing this laboratory work, students are able to demonstrate
moisture analyses of food samples using gravimetric method (oven and vacuumed-
oven method) and azeotropic distillation method.

3.2. Course Learning Outcomes


After completing this laboratory work, students are expected to be able to:
1. explain the principles of moisture analysis.
2. Select the appropriate method of moisture content analysis considering the
characteristics of food matrix.
3. demonstrate skills to moisture content analysis using oven, vacuumed-oven, and
the azeotropic distillation methods.
4. calculate moisture content of food sample in wet basis and dry basis.

3.3. Principles of Analysis


3.3.1.1. Gravimetric method
Moisture content analysis by a gravimetric method is done by evaporating
water from the food matrix using a drying oven. Drying process may use air drying
oven or vacuumed-drying oven.
Moisture analysis using an air drying oven is based on the weight lost. There-
fore, samples should have high heat stability and do not contain other volatile
components. Factors that may affect the moisture analysis by oven method of which
is at the step of samples weighing, drying, and treatment after drying. The oven
conditions, such as temperature fluctuation, flow speed and air humidity in oven are
also important factors influencing the result of analysis.
In the vacuumed drying oven method, samples are dried in conditions of low
pressure (vacuum) so that water can evaporate under normal boiling point of water,
i.e. 60-70oC (Figure 3.1). The pressure used in this method generally ranges from 25
to 100 mmHg. AOAC (1999) recommends a vacuumed oven method for sample

25
26 Moisture Analysis

analysis containing sugars (e.g fructose), because sugars tend to decompose at a


higher temperature.

Figure 3.1. Vacuumed-oven for moisture analysis

3.3.1.2. Azeotropic distillation method


There are two types of distillation methods that can be applied, namely a direct
distillation and azeotropic distillation. In the direct distillation, water is evaporated
directly from immiscible solvents. During heating, evaporated water is condensed,
and then collected in a measuring cup and a specified volume. Measured volume of
water is used to determine the moisture content.
In azeotropic distillation method, water is evaporated together with solvents
that are immiscible at a fixed ratio. For example, in normal conditions the boiling
point of water and toluene is 100oC and 110.8oC respectively, but in a mixture
solvent, water and toluene (ratio 20:80) will jointly evaporate at a temperature of
85oC. Vaporized water and solvent are condensed. Because water and toluene are
immiscible, they will separate after condensing, and water volume can be measured.
To obtain a high accuracy in moisture analysis using azeotropic method, distilla-
tion factors need to be specified. Factors distillation is a factor to determine the
amount of water that is absolutely pure water is evaporated, so that it can be a
correction factor in the calculation of moisture content.
There are three types of solvents commonly used for azeotropic distillation, ie
toluene, xylene (dimethyl benzene) and tetrachlororethylene. Toluene and xylene
have lower specific gravities than that of water. The density and boiling point of
toluene is 0.866 and 110.8oC respectively, while density of o-dimethyl benzene, m-
dimethyl benzene, p-dimethyl benzene are 0.861, 0.867 and 0.861 respectively. They
have respective boiling point of 144, 138.8 and 138.5oC. Tetrachloroethylene has a
higher specific gravity and boiling point than that of water, i.e 1.600 and 143.3oC
respectively.
By using a solvent which has a lower specific gravity than water, water will be
present at the bottom of the glass container so that the volume measurement will be
easily done. The use of solvents with a higher specific gravity measurements is diffi-
cult, because water will be set at the top of the glass container and to read the
volume must use two meniscus, thereby it will reduce the data accuracy.
Food Analysis Laboratory Manual 27

The advantages azeotropic distillation methods are: (a) the moisture content is
set directly and the end result is the real value of moisture content, not because of
the weight loss of sample; (b) the results are much more rigorous than a drying oven
for the number of examples used; (c) a shorter time for analysis (0.5-1 hours); (d) the
equipment is simple and easy to obtain; (e) the effect of environmental humidity can
be avoided; (f) prevent oxidation during heating; and (g) analysis is simple and easy
to handle. While the weakness azeotropic distillation methods are: (a) the surface of
the glass used tool must always be maintained clean and dry; (b) alcohols or glycerol
may be distilled along with water so that the data obtained are higher than the
actual value; (C) use flammable solvent; (D) partially toxic solvent (such as benzene);
and (e) the accuracy of reading the volume of limited condensed water.
3.3.1.3. Karl Fischer Method
Karl Fischer method is used to measure the moisture content of sample based on
the principle of volumetric titration method. Titrant used is Karl Fischer solvent, a
mixture of iodine, sulfur dioxide and pyridine in methanol solution. During the
titration process, reduction reaction of iodine by the sulfur dioxide in the presence of
water occur (Figure 3.2). The reduction reaction of iodine will occur until water
completely removed as indicated by the appearance of a brown color due to the
excess iodine.

+ + + H2O 2 +

N N N N N
I2 SO2 HI SO3

+ CH3OH

N N
SO3 H SO4CH3
Brown Mahagony Color

Figure 3.2. Reaction during moisture analysis using Karl Fischer method

Karl Fischer reagent is very sensitive to water, so that this method can be
applied to moisture analysis in food that has a very low moisture content in
products such as oil/fats, sugar, honey and dry ingredients. Karl Fischer method can
be used to measure the moisture content to a concentration of 1 ppm.

3.4. Procedures
3.4.1. Experiment 1: Moisture Analysis using Oven Method (SNI 01-2891-1992)
Samples
 Baby food
 Mungbean flour
 Milk powder
 Instant noodles
 Rice flour
 Soybean flour
28 Moisture Analysis

Equipment
 Cup aluminum (lid)
 Desiccator contains desiccant material (such as dried phosphorus pentoxide,
calcium chrloride or granular silica gel)
 Oven (105ºC)
 Analytical balance
 Thermometer
 Clamp cup (tweezers)

Analytical Procedures
Checking oven temperature
1. Before the oven is used for the analysis of water content, check the oven tempe-
rature by inserting a calibrated thermometer in the oven.
2. Wait until the thermometer reaches the desired temperature (about 5 minutes).
3. Check oven temperature for 5 times. Record the read temperature.
4. Calculate the average value, standard deviation, and Horwitz RSD
Analytical step
1. Dry empty cups that have been coded using a pencil and lid in the oven for 15
minutes.
2. Cool the dish in the desiccator. Take the cup dry with a clamp.
3. Weigh the dry cup.
4. Weigh 1-2 g sample in the cup.
5. Dry in oven temperature of 105ºC for 3 hours.
6. Cool in a desiccator.
7. Weigh. Repeat weighing to obtain constant weight (≤ 0.0005 g).
Calculation
1. Calculate the water content in the wet and dry bases as follows:
a. Moisture content in wet basis:
Moisture (g/100 g wet basis)  W  (W1  W2) x 100
W
b. Moisture content in dry basis:
Moisture (g/100 g dry basis)  W  (W1  W2) x 100
W1  W2
where : W = sample weight before drying (g)
W1 = sample weight + dried empty cup (g)
W2 = dried empty cup (g)
2. Calculate the average value, standard deviation, and Horwitz RSD.

3.5. References
AOAC International. 1999. Official Method of Analysis 925.45 Chapter 44.1.03 p. 2.
Apriyantono, A., D. Fardiaz, N.L. Puspitasari, S. Yasni and S. Budiyanto. 1989. Petunjuk
Praktikum Analisis Pangan. IPB Press, Bogor.
Badan Standardisasi Nasional. 1992. SNI 01-2891-1992: Cara Uji Makanan dan Minuman.
Food Analysis Laboratory Manual 29

Belitz, H.D, W and W Grosch. Food Chemistry. 1999. Springer, Berlin Heidenberg, New
York, Barcelona, Hongkong, London, Milan, Paris, Singapore, Tokyo.
Fardiaz, D., N.L. Puspitasari, and C.H. Wijaya. 1991. Analisis Pangan (Monograf). Labo-
ratorium Kimia dan Biokimia Pangan, PAU Pangan dan Gizi, IPB.
Fennema, O.R (ed). Principles of Food Science (Part I Food Chemistry). 1985. Marcel Dekker,
INC, New York and Basel.
30 Moisture Analysis

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