Kwame Nkrumah University of

Science & Technology, Kumasi, Ghana

Moisture and Total Solids

Analysis

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 Moisture Content
• Important to food scientists for various reasons:
• 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.

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• Food Quality - the texture, taste, appearance
and stability of foods depends on the amount of
water they contain.

• Food Processing Operations - a 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.

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 MOISTURE
Ease of removal depends on how it exists in the food
product.

• Free water-This water retains its physical properties and

thus acts as the dispersing agent for colloids and the
solvent for salts.
• Bound Water -
o Adsorbed water-Tightly held or is occluded in cell
walls or protoplasm and is held tightly to proteins.

o Water of hydration- bound chemically, for

example, lactose monohydrate; hydrated salts
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 Determination of Moisture

1. Drying Methods
2. Distillation method
3. Chemical Methods
4. Physical Methods

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 Drying Methods
• Methods rely on measuring the mass of water in a known
mass of sample.
• The moisture content is determined by measuring the mass
of a food before and after the water is removed by drying.

• Total solids = the dry matter that remains after moisture

removal

• Basic Principle
– Water has a lower boiling point than the other major
components within foods such as lipids, protein and
carbohydrate.
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 Drying Methods

• Total solid is a measure of the amount of material

remaining after all the water has been evaporated

• Advantages - cheap, easy to use, many samples can be

analyzed simultaneously
•
• Disadvantages - destructive, time consuming

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 Calculations
• Moisture and total solids contents of food can be
calculated as follows using oven drying procedures:

• % Moisture (wt/wt) = wt H2O in sample × 100

wt of wet sample
% Moisture (wt/wt) = wt of wet sample - wt of dry sample ×100
wt of wet sample

% Total solids (wt/wt) = wt of dry sample × 100

wt of wet sample

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 Types of Oven
1. Convection Oven
– Greatest temperature variations -
because hot air slowly circulated without
the aid of fan, air movement is
obstructed further by pans placed in the
oven

2. Forced Draft Oven

– The least temperature differential across
the interior (< 1oC). Air is circulated by a
fan that forces air movement throughout
the oven cavity
– Drying period 0.75 – 24 hr, depending on
food sample and its pretreatment
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3. Vacuum oven
– Drying under reduced pressure (25 – 100mm
Hg).
– Able to obtain a more complete removal of
water and volatiles without decomposition
within a 3 – 6 h
4. Microwave Oven
– Water evaporation is due to absorption of
microwave energy, which causes them to
become thermally excited.
– Weighed samples are placed in a microwave
oven for a specified time and power-level and
their dried mass is weighed.

Advantage - simple
Disadvantage:- care must be taken to standardize the drying procedure
and ensure that the microwave energy is applied evenly across the sample.
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5. Infrared Drying
• Water molecules in the food evaporate because they
absorb infrared energy, which causes them to
become thermally excited.
• The sample to be analyzed is placed under an
infrared lamp and its mass is recorded as a function of
time.
• Advantages: rapid (10-25 min) and inexpensive
• This is because the IR energy penetrates into the sample, rather
than having to be conducted and convected inwards from the
surface of the sample.
• To produce consistent results, one must control
 the distance between the sample and IR lamp
 the dimensions of the samples
• IR drying methods are not officially recognized for moisture content
determinations because it is difficult to standardize the procedure.
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6. Moisture Analyzer
– Using a digital balance, the
test sample is placed on an
aluminum pan and the
constant temperature is
applied to the test sample.

– Instrument automatically
weighs and calculates the %
of moisture or solids
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 Practical Considerations
• Sample Dimensions
– Surface area of material exposed to the environment is
important
• Clumping and surface crust formation
– Mix the sample with dried sand to prevent clumping
• Decomposition of other food components
– High temp or too long drying time can cause
decomposition of some heat-sensitive components in the
food
• Volatilization of other food components
– Food with high volatile components should be analyzed
using distillation or chemical method.
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 Practical Considerations
• High moisture samples
– Dried in two stages to prevent spattering
• Sample pans
– Should be dried in the oven and stored in a dessicator prior
analysis
– Avoid contact with bare hands. Use tongs or cotton gloves
• Type of water
– free vs. bound water
– Example: % water in milk vs. non-fat dried milk.
• Temperature and power level variations
– Significant variations in temperature and power levels
within an drying instruments.
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 Distillation Methods
• Direct measurement of the amount of water removed from a
food sample by evaporation
• Involve co-distilling the moisture in a food sample with a high
boiling point solvent that is immiscible in water, collecting the
mixture that distills off and then measuring the volume of
water
• Advantages:
– Suitable for low moisture foods and foods containing volatile oils such
as herbs and spices
– Cheap, easy to set up and operate
• Disadvantage:
– Destructive, time consuming, involve flammable solvent, not applicable
for some types of foods
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 Distillation Methods
• Two distillation procedures: Direct and Reflux
distillations, with a variety of solvents
• Direct distillation: sample is heated in mineral oil or liquid
with a flash point well above boiling point of water. Other
immiscible liquids with boiling point slightly above water
can be used (e.g. toluene, xylene, and benzene).

• Reflux distillation: uses either a solvent less dense than

water (e.g. toluene, bp of 110.6 oC; or xylene with bp
137-140oC or solvent more dense than water (e.g.
tetrachlroethylene with bp 121oC
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Distillation Methods

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 Practical Consideration
• 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.

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Watch Video

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 Chemical Methods
• Moisture is determined by the reactions between water and
certain chemical reagents

• A chemical reagent is added to the food that reacts specifically

with water to produce a measurable change in the properties of
the system, e.g., mass, volume, pressure, pH, color, conductivity.

• Type of chemical method commonly used:

– Karl Fischer Titration
– Gas production Methods

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 Chemical Methods
• Measurable changes in the system are correlated to the moisture
content using calibration curves.

• For accurate measurement, chemical reagent must reacts

with all of the water molecules present, but not with any of
the other components in the food matrix.

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 Advantages?

• Chemical reaction do not involve application

of heat.
• Suitable for:
– Foods that contain thermally labile substances
that would change the mass of the food matrix
on heating (e.g., food containing high sugar
concentrations) or
– Foods that contain volatile components that
might be lost by heating (e.g. spices and herbs).

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 Karl-Fischer Titration

• Determine the low moisture foods

– (e.g. dried fruits and vegetables, confectionary, coffee,
oils and fats) or low moisture food high in sugar or
protein.

• It is based on the following reaction:

2H2O + SO2 + I2 → H2SO4 + 2HI

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 Karl-Fischer Titration
• Procedure
– The food to be analyzed is placed in a beaker
containing solvent and is then titrated with Karl Fisher
reagent (a solution that contains iodine).

– Iodine will reacts with remaining water in the samples.

– The endpoint color is dark red-brown.

– The volume of iodine solution required to titrate the

water is measured and can be related to the moisture
content using a pre-prepared calibration curve.

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 Karl-Fischer Titration

Main Difficulties and Source of Error

1. Incomplete water extraction
– Fineness of grind is important

2. Atmospheric moisture
– External air must not be allowed to infiltrate the
reaction chamber

3. Moisture adhering to walls of unit

– All glassware and utensils must be carefully dried

4. Interferences from certain food constituents

– Oxidation of ascorbic acid to dehydroascorbic acid
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• Gas Production Methods
– Commercial instruments are also available that utilize
specific reactions between chemical reagents and water
that lead to the production of a gas
– Example; when a food sample is mixed with powdered
calcium carbide, the amount of acetylene gas produced is
related to the moisture content.
– The amount of gas produced can be measured by
1. The volume of the gas produced
2. The decrease in the mass of the sample after the gas is
released
3. The increase in pressure of a closed vessel containing
the reactants

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 Physical Methods
1. Electrical methods
• Dielectric Method
• Moisture is determined by measuring the change in
capacitance or resistance to an electric current passed
through the sample
• Limited to food that contain not more than 30-35%
moisture.
 Conductivity method
• The conductivity of an electric current increases with the
percentage of moisture sample
• Must keep the temperature constant

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2. Hydrometry
 Measuring specific gravity or density
 Best applied to the analysis of solutions consisting of only
one component in a medium of water
 Commonly used in beverages, salt brines and sugar
solutions
 Example: Pycnometer, hydrometer, Westphal Balance.

3. Refractometry
– Determine the soluble solids in fruits and fruit products
– Rapid and accurate methods
– Principle: when a beam of light is passed from one medium
to another and the density differs, then the beam is bent or
refracted.
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4. Spectroscopic Methods

• Principle: Employs the interaction of electromagnetic

radiation with materials to obtain information about
their composition
– X-rays, UV-visible, NMR, microwaves and IR

• Methods ensure water in food samples absorb

electromagnetic radiation at characteristic wavelength
different from the other constituents

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– Measure absorption of radiation by molecules in foods
– Different functional groups absorb different frequencies of
infrared radiation
– For water, near-infrared (NIR) bands (1400-1450, 1920-
1950 nm) are characteristic of the –OH stretch of water
molecule

Not same as IR lamp and microwave evaporation methods:

– Absorption: low energy waves
– Evaporation: high energy waves

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 Methods to determine Water in Different
Molecular Environments

• Vapour Pressure Methods

– Determination of water activity
– Bound water is less volatile than free water
• Thermogravimetric Methods
– Measure the mass of a sample as it is heated at a controlled
rate
– Free water normally evaporates at a lower temperature
than bound water

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• Calorimetric Methods:
– Using Differential Scanning Calorimetry (DSC) and
Differential Thermal Analysis (DTA)
– Measure changes in the heat absorbed or released by a
material as its temperature is varied at a controlled rate.
Determines amount of water present in different molecular
environments: free water higher melting point than bound
• Spectroscopic Methods
– Nuclear magnetic resonance (NMR) – distinguish molecules
within materials based on their molecular mobility
– Molecular mobility for free water is higher than that of
bound water

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Comparison of the Methods

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Underlining Principle
• Oven drying methods: involve the removal of moisture
from the sample and then a weight determination of
the solids remaining.
• Distillation methods: Involve a separation of the
moisture from the solids. The moisture content is
calculated directly by volume.
• Chemical Methods: reflected as the amount of titrant
used.
• Dielectric and conductivity methods: electrical
properties of water

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Underlining Principle
• Hydrometric methods: based on the relationship
between specific gravity and moisture content

• Refractive Index: how water in a sample affects the

refraction of light

• NIR & microwave Methods: absorption at w/length

characteristic of the molecular vibration in water.

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• Intended Purposes

• Rapid analysis but less accurate: oven drying

methods, microwave drying, infrared drying and
moisture analyzer

• Rapid but require correlation to less empirical

methods: electrical, hydrometric, refractive index
and infrared analysis methods

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• Nature of Sample
• Oven Drying: problem with volatile compounds and
chemical degradation

• Distillation: minimize volatilization and decomposition

• Karl Fischer: Food with very low moisture or high in

fats and sugars

• Pycnometer, hydrometer and refractometer requires

liquid samples with limited constituents
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 Summary
• Types of water present: free, adsorbed and hydration of
water.
• Major difficulty in many methods is attempting to remove or
otherwise quantitate all water present.
• Factors to be considered in selecting moisture analysis:
– expected moisture content,
– nature of the other food constituents (i.e. highly volatile),
– equipment availability,
– speed necessary,
– accuracy and precision required and
– intended purpose (e.g. regulatory or in-plant control)

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Methods generally grouped into two (Park, 1996):
Four major analytical principles:
• Drying; Distillation; Chemical and Physical methods

Procedure for determination (Direct or indirect

measurement) based on scientific theory
• Direct: Moisture removed by drying, distillation etc
• Indirect: properties of the wet solid which depend on the
amount of water/ hydrogen atoms is measured then
compared/ calibrated against standard values precisely
determined using one or more of direct methods.

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Four Major principles Procedure for Determination

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Methods of analysis for water
Procedure Applicability Limitations Capital Selected references
costs
Physical removal of water
Air oven at Most foods, except Caramelization of sugars, Low AOAC International, 2002;
105°C those rich in sugars degradation of unsaturated Anklam, Burke and
and fats fats, loss of other volatiles Isengard, 2001;
Nielsen, 1998
Vacuum oven Most foods Loss of volatiles Low As above
at 60 - 70°C
Freeze-drying Most foods Slow, residual water in Medium As above
samples
Microwave Medium or high Charring Low As above
oven moisture
Dean & Stark Foods high in Safety of solvents used Low As above
distillation volatiles

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Chemical reactivity
Karl Low moisture, Low As above
Fischer hygroscopic foods
Physical methods
NMR Most foods Need for calibration with specific food High Bradley, 1998; Hester
and Quine, 1976
NIR Established for cereals Need for extensive calibration with High Williams, 1975
and some other foods specific food. Particle size
dependence
Chromatography
GLC Meat and meat products High Reineccius and
Addis, 1973
GSC Some meat products High Khayat, 1974
Notes:
References selected provide detailed procedures, evaluations or reviews.

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Tutorial after Break

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