Instituto Tecnológico

de Tuxtepec
ANÁLISIS DE ALIMENTOS

UNIDAD 2
Moisture and Total Solids
Analysis
MAESTRIA EN CIENCIAS EN
ALIMENTOS

DRA. CECILIA EUGENIA MARTÍNEZ SÁNCHEZ

 Water

is an essential constituent of many foods. It

may occur as an intracellular or extracellular
component in vegetable and animal products,
as a dispersing medium or solvent in a variety
of products, as the dispersed phase in some
emulsified products such as butter and
margarine, and as a minor constituent in other
foods
The presence of water influences the chemical
and microbiological deterioration of foods. Also,
removal (drying) or freezing of water is essential
to some methods of food preservation.
Fundamental changes in the product may take
place in both instances.
 Moisture assays: Can be one of the most important
analyses performed on a food product and yet one of the
most difficult from which to obtain accurate and precise
data. this chapter describes various methods for moisture
analysis – their principles, procedures, applications,
cautions, advantages, and disadvantages.

 Water activity measurement: also is described, since it

parallels the measurement of total moisture as an important
stability and quality factor. with an understanding of
techniques described, one can apply appropriate moisture
analyses to a wide variety of food products.
 Importance of Moisture Assay

One of the most fundamental and important analytical

procedures that can be performed on a food product is an assay
for the amount of moisture. The dry matter that remains after
moisture removal is commonly referred to as total solids. This
analytical value is of great economic importance to a food
manufacturer because water is an inexpensive filler. The
following listing gives some examples in which moisture content
is important to the food processor.
Moisture is a quality factor in the preservation of
some products and affects stability in:

(a) Dehydrated vegetables and fruits

(b) Dried milks

(c) Powdered eggs

(d) Dehydrated potatoes

(e) Spices and herbs

 Moisture is used as a quality factor for

(a) Jams and jellies to prevent sugar

crystallization

(b) Sugar syrups

(c) Prepared cereals

 Reduced moisture is used for convenience in
packaging or shipping of

(a) Concentrated milks

(b) Liquid cane sugar (67% solids) and liquid

corn sweetener (80% solids)

(c) Dehydrated products (these are difficult to

package if too high in moisture)

(d) Concentrated fruit juices

in compositional standards (i.e., Standards
of
Identity)
(a) Cheddar cheese must be ≤39% moisture.

(b) Enriched flour must be ≤15% moisture.

(c) Pineapple juice must have soluble solids of ≥10.5°Brix (conditions
specified).

(d) Glucose syrup must have ≥70% total solids.

(e) The percentage of addedwater in processed meats is commonly
specified.

Computations of the nutritional value of foods require that you know the moisture
content.
Moisture data are used to express results of other analytical determinations on a
uniform basis [i.e., dry weight basis (dwb)].
 Water content of food
10

Accurate determination of water is difficult;

 not all water is free (freezes or evaporates)
 may be bound by ionic and polar species in food
Therefore the keeping qualities of food should be
measured by aw (range 0.1-1) rather than
moisture content
 aw activity ranges
11

High moisture foods aw 0.97 to 1;

 highly susceptible to deterioration by micro-
organisms
 milk, fruit, vegetables, meat etc

Intermediate moisture foods aw 0.6 to 0.9

 shelf stable without refrigeration or heat
processing
 susceptible to enzymic browning & Maillard
reaction
 cheese, jams, jellies etc
 aw activity ranges
12

Low moisture foods aw < 0.6

 stable to deterioration
 except lipid oxidation
 dried milk, cereals
 Forms of Water in Foods

Free water
 Water retains its physical properties

Capillary water
Water is held tightly within spaces within a food that are
surrounded by a physical barrier
 E.g. An emulsion droplet

Bound water
 Water is bound physically (e.g. in protein) or chemically
(e.g. Na2SO4. 10H2O)
Depending on the form of the water present in a
food, the method used for determining moisture may
measure more or less of the moisture present. This
is the reason for official methods with stated procedures.
However, several official methods may
exist for a particular product. For example, the AOAC
International methods for cheese include: Method
926.08, vacuum oven; 948.12, forced draft oven; 977.11,
microwave oven; 969.19, distillation (5). Usually, the
first method listed by AOAC International is preferred
over others in any section.
Determination of Moisture: Methods

1. Drying Methods
 Oven drying methods
2. Distillation method
 Dean and Stark Method
3. Chemical Methods
 Karl Fisher
 Gas production
4. Physical Methods
 Drying Methods

 These 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.
 Basic Principle
 Water has a lower boiling point than the other major components
within foods such as lipids, protein and carbohydrate.
Sometimes, moisture content also reported as
“total solid”
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
Methods of water measurement -Oven
18
drying
Loss of weight on heating used to calculate
moisture content of sample
 convection oven, 101-105oC, several hours - overnight,
heat stable samples
 forced draft oven
 better air circulation
 vacuum oven, approx. 70oC (25-100 mmHg), several
hours - overnight, heat unstable samples (sugars)
 Types of Oven

1. Convection Oven
 Greatest temperature
variations - because
hot air slowly circulated
with out 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
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 hr
4. Microwave Oven
 Weighed samples are
placed in a microwave
oven for a specified
time and power-level
and their dried mass is
weighed.
 23

Pure water evaporates at 100oC at sea level.

 boiling point increases with increased concentration

Sample preparation for oven drying;

 liquids may be pre-dried over a steam bath before drying
in oven
 high moisture solids such as yoghurt and humus mixed
with known weight of pre-heated and cooled sand and a
small glass rod that remains in sample pan
 24

Sample preparation
 mill to consistent particle size of 1mm
 eliminate exposure to atmosphere
 store in airtight small container with minimal headspace
Sample pans
 aluminum with cover
 pre-heated at 100OC for 3 hrs
 cool and store in desiccators
 Oven drying Advantages/Disadvantages
Advantages;
 simple, little expense and reasonably accurate
Disadvantages;
 unsuitable for products
 C6H12O6  6C + 6H2O (produce moisture)
 sucrose hydrolysis (utilise moisture)
 containing volatile constituents
 acetic & butyric acids; alcohols, esters & aldehydes
 variation
between samples due to variation in
sample particle size
25
5. Infrared lamp drying
 Principle of drying:
Similar to microwave
oven
 Advantages: rapid and
inexpensive
 This is because the IR
energy penetrates into
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.
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
 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.
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.
 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
Dean and Stark Method
A known weight of sample is placed in a flask with
immiscible organic solvent such as xylene or toluene.
The flask containing the sample and 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 to the
condenser
Liquid water will be collected in graduated tube
When no more water collected, distillation is stopped.
Distillation Methods
 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.
 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
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.
Chemical reaction do not involve application of
heat.
Therefore, they are 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).
 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

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.
Major 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
 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
 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
 Electrical methods
- Dielectric46 constant Meter
Instruments need
calibration against known
samples
Sample density and
temperature affect the
reliability
Useful for continues
measurements
Limited to food systems
that contain no more than
http://www.brookhaven.co.uk/
30-35% moisture images/products/bi-870.jpg
 Conductivity method
 The conductivity of an electric current increases with the
percentage of moisture sample
 Must keep the temperature constant
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.
Hydrometers
49
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.
 51

 refractive index of a solution increases with concentration

of solute
 refractometer calibrates in Brix used for carbohydrate-
based solutions
 Brix = g sucrose/100g sample
Refractometer
52
4. Infrared Analysis
 Principle:
 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
 Freezing point - Cryoscope
54
Freezing point
 AOAC approved (method 961.07)
 used to test for added water in milk
 AOAC standard freezing point taken as - 0.527C
 the FDA rejects milk if freezing point > than - 0.503C
Expression of compositional data on
‘as is’ or ‘dry basis’
55

‘as is’, ‘as received’, ‘fresh sample’

 refers to composition (eg fat content) of sample as a
percentage of food as received from original source
‘dry matter basis’, ‘dry basis’
 refer to composition (eg fat content) as a percentage of the
total solids in the sample
Moisture and total solids contents of food can be
calculated using one of the equations below:

 % Moisture (wt/wt) = wt H2O in sample X 100

wt of wet sample

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

wt of wet sample

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

wt of wet sample
 Calculating composition
57
on ‘dry basis’
from ‘as is’ analysis
The Bligh & Dyer method requires fat to be
extracted from a fresh, ‘as is’ sample (not pre-
dried)
 % fat ‘as is’ is calculated as follows:
% fat (as is) = wt fat extracted (g) x 100
fresh sample wt (g)
 to convert fat content on ‘as is’ basis to ‘dry basis’ the
following equation is used
% fat (dry basis) = % fat (as is) / dry matter coefficient
 58

 TheSoxhlet method requires fat to be

extracted from a pre-dried sample of
food
 % fat ‘dry basis’ is calculated as follows:
% fat (dry basis) = wt fat extracted (g) x 100
wt of pre-dried sample (g)
 to convert fat content on ‘dry basis’ to ‘as is’
basis (eg the % fat in the original sample
before drying) the following equation is
used:
% fat (as is) = % fat (dry basis) x dry matter coefficient
Measurement of water activity (aw)
59

A better indicator of food perishailiby than

moisture content
Refers to water not tightly bound to other
food molecules
a = P / Po = ERH / 100
w
 aw = water activity
 P = partial pressure of water above sample
 Po = vapour pressure of pure water at same

temp.
 ERH = equilibrium relative humidity

surrounding product
 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
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.
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
 Comparison of the Methods

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
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 Methods: absorption at w/length characteristic
of the molecular vibration in water.
 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
 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
 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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