Food Analysis

Determination of
Moisture and Water
Content in Food

Moisture Analyzer
Karl Fischer Titration
Analytical Balances

The Ultimate Moisture & Water Guide

Proven Methods & Procedures
Moisture and water content are among the most important parameters measured in food.
The content of moisture is inversely related to the dry matter of a food item – hence there
are direct economic effects on consumers and processors. More importantly, the moisture
content in food also influences its stability and quality. Needless to say that moisture is a
topic of many regulations and legislation.

The following guide will:

• Give an introduction to the topic
• Present the different methods of moisture and water content determination
• Provide for selected applications and results
• Give tips and tricks for easier water content and moisture determination

Content

1. Determining Moisture and Water Content in the Food Industry 3
1.1 Water Binds in Different Ways 3
1.2 Technologies for Moisture Analysis 3
2. Thermogravimetric Methods for Moisture Analysis 4
2.1 The Measurement Principle 4
2.2 Thermogravimetric Methods with Drying Ovens 5
2.3 Moisture Analysis with a Moisture Analyzer 7
3. Determining Water Content Using the Karl Fischer Method 8
3.1 The Measurement Principle 8
3.2 Solutions for More Reliability and User Comfort 9
4. Conclusion 10
Overview of Advantages/Disadvantages of Presented Methods 11

METTLER TOLEDO Moisture Guide 2

1. Determining Moisture and Water Content in the Food Industry

Moisture analysis, or water content determination, play an important role in all areas of the food industry, from
incoming/outgoing goods inspections, production and storage, to the development of new versions of products.
The industry is under high pressure to keep prices low while at the same time producing enormous volumes,
and for this reason moisture analysis must be very fast, precise, and reliable. Furthermore, there are an increas-
ing number of regulations which must be observed. Results and measurement procedures must therefore be
reliably documented.

Technically there are several moisture analysis procedures available. Which option is right depends on very dif-
ferent factors. The main features, advantages, and risks of these procedures are presented in the following.

1.1 Water Binds in Different Ways

Almost every natural substance contains water. In the simplest case, water is adsorbed from the air humidity on
the surface of particles. It can also be stored deep in the pore systems of solid substances, or exist as chemi-
cally bound water. Almost all forms exist in foods and ingredients. In addition to well defined products such as
all-purpose sugar or alcoholic drinks, there are also complex cellular structures such as dried fruits or meats,
in which water is bound both by sorption on the surface and by capillarity between particles. Water also exists
deep in cells where it is very difficult to measure. For this reason, analysis and sample preparation methods
must be selected based on the properties of the product being examined.

1.2 Technologies for Moisture Analysis

There are four types of methods for analyzing moisture:
– thermogravimetric analysis
(oven drying, halogen/IR drying, microwave drying, etc.)
– chemical analysis
(Karl Fischer titration, calcium carbide testing)
– spectroscopic analysis
(IR spectroscopy, microwave spectroscopy, H-NMR spectroscopy)
– other types of analysis
(gas chromatography, density determination, refractometry, etc.)

A range of factors must be weighed up when selecting a method of analysis: the available sample volume, the
number of samples, the measurement speed, the feasibility of automation, the accuracy, or even the physical
chemical properties of the sample – all play a large role in the decision-making process.

HX204 Moisture Analyzer XPE205 Analytical Balance V30S Karl Fischer Titrator
Automatic moisture determination Moisture determination Water content determination
with Halogen Moisture Analyzer by loss on drying method with Karl Fischer titration

Fig. 1: Moisture analysis made easy with powerful and reliable measuring instruments.

METTLER TOLEDO Moisture Guide 3

Temperature-sensitive or liquid samples and substances, which include many foods, must be analyzed care-
fully with thermogravimetric methods. As with most vitamins, enzymes, or flavoring agents, thermogravimetric
­methods are not feasible.

Insoluble solids with chemically combined water or distinct pore systems, however, can be titrated with the Karl
Fischer method if the water is made accessible e.g. using a homogenizer or an oven to evaporate the sample’s
water.

METTLER TOLEDO provides a variety of solutions for moisture analysis. Two thermogravimetric methods and the
Karl Fischer titration method are described here in detail.

2. Thermogravimetric Methods for Moisture Analysis

All moisture analysis methods that follow the principle of differential weighing can be called thermogravimetric
methods. Thermogravimetric analysis is historically the classical method of analysis. It is used as a reference
method and is defined in many regulations governing the food industry. The principle is simple, but in practice
there are several potential sources of error to be noted.
The central element in all thermogravimetric methods is the balance.

2.1 The Measurement Principle: A sample is weighed and then heated so that the moisture content is released.
Once the sample is cooled in the desiccator, it is weighed again. The difference between the initial weighing and
the second weighing is used to calculate the moisture content. In this procedure, the heating temperature and
heating duration are important considerations. Reproducible and traceable results can only be obtained under
identical conditions.
For this reason, results obtained through alternative methods, such as using a moisture analyzer, must be refer-
enced against this drying over method.

Advantages: This method produces very precise results. It is simple and cost effective. The use of intelligent in-
struments reduces the risk of error significantly and can be automated to a great extent. This allows for a greater
sample throughput to be achieved.

Disadvantages: Many substances decompose to some extent when heated, leading to a loss in weight. Further-
more, heating causes calcination of all substances that evaporate or form volatile azeotropes below 100 °C. This
includes many alcohols, flavoring agents, or acetic acid. Another consideration is that parts of the sample may
evaporate along with the water. Handling is very laborious. There is a risk of mixing up the samples, and simple
errors in calculation or the transfer of the weighing results are virtually impossible to prevent with large sample
volumes and manual documentation.

Fig. 2: Typical sources of error during

manual processing: mixing up samples,
miscalculation, and mistakes when
transferring data.

METTLER TOLEDO Moisture Guide 4

2.2 Thermogravimetric Methods with Drying Ovens
The two important advantages of drying ovens in moisture analysis are the
sample throughput and the flexibility when it comes to sample volumes/
sizes. On the other hand, the time it takes to obtain a result must be taken
into consideration, because extended heating periods and cooling phases
must be observed.

Fig. 3: The XPE205 analytical balance from METTLER TOLEDO offers high
performance, ease of use, and minimal risk of error thanks to its clever design.

Clever Solutions Reduce the Risk of Error

Many of the mentioned risks can be eliminated with balances from METTLER TOLEDO's Excellence Line. In the
XPE models, the differential weighing method is integrated in the user software of the balances.

The method can be started from the touch screen and the software guides the user through the entire process
from taring and initial weighing to the final weighing procedure. All measurement data are automatically saved
and can be accessed for years after. A connected label printer can automatically print out heat-resistant labels
with barcodes for identifying each sample. After heat treatment in the drying oven (generally three hours at
105 °C) and then cooling in the desiccator, the sample is uniquely identified via the barcode, the second weigh-
ing result is assigned to this code, and all calculations are carried out automatically by the software. The bal-
ance displays the result. Complete documentation with all measurement results can be printed by a connected
printer. These technical solutions provided by the Excellence balances from METTLER TOLEDO significantly re-
duce the risk of error, particular with large sample volumes and high throughputs. In additional to being easy to
use, the balances also offer several clever solutions that provide more user comfort and measuring reliability in
and around the weighing chamber.

1 2 3 4 5

One Click® Weight Dry Result Calculation Docunebtatuib

Fig. 4: The display shows the entire process step by step: OneClick start, unique sample identification via barcodes, initial weighing,
­drying, second weighing, automatic calculation and logging of measurement results, and complete documentation

Ideas for Better User Comfort

The large weighing chambers of the XPE analytical balances allow for easy weighing and provide plenty of
space even for large weighing containers. A particular advantage in terms of comfort and handling are the
hands-free doors on the Excellence XPE analytical balances, which open automatically. The doors are controlled
by the SmartSense infrared sensors on both sides of the terminal, which react as soon as an object or the hand
of the operator approaches them.

METTLER TOLEDO Moisture Guide 5

The SmartGrid® grid weighing pan is another special feature of these balances. It prevents incorrect results due
to the weighed goods falling next to the tare container and also reduces the influence of drafts in the weighing
chamber. The stabilization time, during which the measurement data fluctuates before reaching a stable value, is
therefore much faster than with conventional balances. Measurement results can be obtained more quickly as a
result. SmartGrid makes the weighing chamber extremely easy to clean.

In addition to the SmartGrid grid weighing pan, METTLER TOLEDO also offers
a number of holders, ErgoClips, which are especially made to fit any tare
container imaginable, in order to ensure its secure hold and work-friendly
position.

Fig. 5: No measurement errors caused by spills, fast measurement stabilization, and easy to
clean: SmartGrid® from METTLER TOLEDO.

Ideas for Ensuring Accurate Results with GWP Recommendation and Verification
The free GWP Recommendation service helps you to select the right weighing device by matching its metrologi-
cal performance to your exact measurement needs. Each GWP Recommendation report includes minimum
weight and safety factor calculations to confirm that you have selected the right device for your process.
www.mt.com/gwp-recommendation

The GWP Verification service calibrates your weighing equipment, assesses risks, recommends measures to
improve accuracy and ensures compliance with process and regulatory requirements. GWP Verification can be
issued for any weighing device independent of model or manufacturer. It provides all necessary information to
maintain lifelong accuracy of your balances and scales; an audit-proof documentation included.
www.mt.com/gwp-verification

Compliance, Networking, and Central Control with LabX

LabX is another step that contributes to more reliability, traceability, compliance with regulations, and increased
user comfort. This software module links all balances into one network. A PC does not need to be connected to
the balance itself. Access to the database via an Ethernet interface, for example, would suffice.

Fig. 6: LabX links the METTLER TOLEDO

instruments in your lab and allows central
control and monitoring.

METTLER TOLEDO Moisture Guide 6

Quality supervisors or lab managers can freely define their own methods, user authorizations, read/write rights,
and a number of other security parameters and then apply to either certain balances or all connected devices.

The "Loss on Drying" method is integrated in LabX as standard and can be started on the balance by One Click®.
The user is guided through the process step by step. All entries are shown on the balance display and the
measurement results are automatically and digitally calculated. The laborious and error-prone entry of weighing
results and the subsequent manual calculation of the moisture content are now a thing of the past.

This multifaceted combination of solutions, additional functions, and auxiliary measures significantly reduces
the risk of error in the "Loss on Drying" method. The risk of incorrect weighing results is virtually eliminated with
these tools. User comfort is increased at the same time. Without these numerous safety functions, the "Loss on
Drying" method is not sustainable in the long term without errors occurring. In particular, without these clever
solutions, the often large number of samples increases the risk of mixing up samples or writing down the wrong
measurement results.

2.3 Moisture Analysis with a Moisture Analyzer

A moisture analyzer produces moisture content results much more quickly. The measurement principle is the
same as the thermogravimetric method.with the only difference being the type of heat source. The sample is
heated by absorption of infrared radiation. METTLER TOLEDO moisture analyzers use fast and durable halogen
lamps to heat the samples.

Advantages: The most important advantage is the significantly reduced measurement time, thanks to the
­efficient heat source. Results can be obtained within 2–10 minutes. The samples are heated quickly and evenly,
and measurements provide very good reproducibility with very easy handling. Large sample volumes can be
measured, which is an important factor with inhomogeneous samples. Because of the automated procedure the
risk of error is overall reduced.

Disadvantages: All gravimetric methods, even the moisture analyzer, carry the risk of substances decomposing
to some extent or other volatile components besides water evaporating. Samples can only be measured one at a
time.

Halogen Technology
Halogen technology is the key to moisture analyzers. Halogen technology makes it possible to heat the samples
more quickly and precisely. All moisture analyzers from METTLER TOLEDO are f­itted with this innovative heating
technology.

Fig. 7: It doesn't get better than this: fast moisture

analysis with the HX204 from METTLER TOLEDO
with 0.001% readability.

METTLER TOLEDO Moisture Guide 7

Transfer and calculation errors are virtually eliminated thanks to minimal user intervention and automatic logging
within the devices. Customized methods are started with One Click® and the user is guided through the process
by the display. Similarly to the balances, METTLER TOLEDO moisture analyzers also allow users to set individual
user rights to ensure that quality criteria are met. The calculated results can be printed out or transferred to PC
via USB.

Large Library of Validated Measurement Methods

The drying oven method is typically the reference method. It is recommended to compare the results of the
moisture analyzer to this reference due to the strong dependence of the results on the temperature and heating
duration. METTLER TOLEDO has an intensive library of validated moisture methods for more than 100 samples
giving users a great start for their specific samples (www.mt.com/moisture-methods). If a user is examining
substances which are not included in this library, comparable components can be selected and then the method
just needs to be adapted. This approach ensures compliant results and saves valuable time of method develop-
ment.

Use for Process Control

The instruments are easy to clean, and the easy handling reduces the risk of error. Thanks to their automatic
documentation of results, the moisture analyzers are perfect for use in at-line process control, for high sample
throughputs, or in regulated areas.

In contrast to the "Loss in Drying" method, however, measurements can

only be performed one at a time rather a large number simultaneously.
Results can be obtained within 2 – 10 minutes instead of several hours.

The large sample pans also allow for larger samples to be measured. This
is an advantage when the sample material is inhomogeneous, as is com-
mon with foods.

Fig. 8: Large sample pans and easy cleaning make the halogen moisture analyzers perfect
for quick measurement tasks

3. Determining Water Content Using the Karl Fischer Method

In contrast to thermogravimetric analysis, Karl Fischer titration is a specific method that only determines water
content. Bound and adsorbed water and water deep inside a solid substance can be analyzed. The water con-
tent can be determined within a range of just a few ppm to 100%. The measurement results are extremely pre-
cise and very reproducible.

3.1 The Measurement Principle

The chemical principle of the method is based on the oxidation of sulfur dioxide by iodine in an alcoholic solu-
tion in the presence of a base (derived from the Bunsen reaction) according to the general formula:

2 H2O + SO2 + I2 + CH3OH + 3 Base → BaseHSO4CH3 + 2 BaseHI

Karl Fischer used pyridine as his base, which posed high health and ecological risks and produced a slower
­reaction than the reagents used today. Methanol was used as a solvent and also presented a health risk.

METTLER TOLEDO Moisture Guide 8

Modern Karl Fischer reactions use imidazole as a base, for example, and ethanol as a solvent. These chemicals
significantly reduce the poisonous properties of the reagents. Imidazole or other amines increase the speed of
the reaction.

Various studies have shown that the reaction occurs as follows:

H2O + SO2 + I2 + ROH + 3 Base → BaseHSO4R + 2 BaseHI

Karl Fischer titration can be volumetric or coulometric. Both methods are different only in the way the iodine
is introduced to the reaction. While volumetric titration is performed with a burette, coulometric titration is per-
formed with a generator electrode. As soon as the iodine stays a solution, the end point is reached. Coulometric
titration is mainly suitable to determine very low water content. In the food industry, however, the majority of
substances have a high water content; therefore usually volumetric titration is performed. Auxiliary solvents can
easily be used to dissolve fat, oils, or sugar, for example.

Advantages: The Karl Fischer method is very accurate, selective for water, and a recognized reference method.
It is suitable for trace analysis as well as very high water content. The method can be extensively automated
through suitable sample changers and thus allows for very high sample throughputs. Furthermore, Karl Fischer
titration can virtually be used for any water content determination task.

Disadvantages: As a chemical process, Karl Fischer titration requires a certain amount of chemical knowledge
in order to handle the chemicals properly, organize the space for the safe storage of the reagents, and properly
dispose of used reagents.

The titer of the Karl Fischer solution must be regularly checked. This task is greatly simplified by modern titrators.
The methods usually have to be adapted to the sample matrix in order for the water to be accessible for titration.

Due to the sensitivity particularly of coulometric titration, the risk of error caused by external water sources such
as from the air, solution, container, or carrier gas increases.

3.2 Solutions for More Reliability and User Comfort

METTLER TOLEDO offers suitable instruments for both Karl Fischer methods, which provide efficiency, user com-
fort, and measurement reliability. The optimal solution can be found in a range of titrators. Accessory systems
and sample changers make it possible to accelerate the water content determination process significantly and
automate extensively.

Large, easy-to-read color touch screens guide the user safely through all steps of the analysis. Customized
home screens with set shortcuts are available in order to simplify use and ensure that only reliable methods can
be used. Additional functions, such as titer or blank determination, can be triggered via One Click®.

The titrators automatically detect which titrant is being used as soon as the
burette is inserted. An RFID chip enables communication and stores the
­concentration and shelf-life information. This technology protects against
­using expired or incorrect titrants.

Fig. 9: Burettes with RFID technology. The burettes and titrants are automatically detected. In
other words, accidentally using expired or incorrect titrants is now a thing of the past

METTLER TOLEDO Moisture Guide 9

 Homogenizer: A high-speed agitator breaks up solid samples that are insol-
uble in Karl Fischer reagents. The water contained in the sample is released
for measurement. The homogenizer is controlled via TTL IO interface by the
titrator.

Fig. 10: The volumetric Karl Fischer titrator with homogenizer is the perfect combination for
solid and pasty samples.

Oven sample changers: The Stromboli oven sample changer makes it possible for up to 14 solid or pasty sam-
ples to be titrated, for example, without supervision. A gas flow transports the water extracted from the sample
by the increased oven temperature directly to the titrator. As with drying methods, however, this method also
risks the sample material to be decomposed and thus producing additional water.

Solvent Manager: The Solvent Manager is a practical and helpful accessory controlled by the titrator. Used re-
agents are removed from the titration cell and fresh reagents are supplied, all fully automatically. The process
starts via One Click®. This prevents contact between lab personnel and the chemicals.

LabX PC Software: LabX can be used to operate and monitor all connected titrators from a central point. All
measurement values are automatically saved and can be accessed in the long term via sample identification.
This meets the requirements of important regulations such as 21 CFR Part 11. This chapter of the Code of Federal
Regulations in the USA covers topics such as electronic records, their archiving, electronic signatures, and trace-
ability.

4. Conclusion
Water/moisture content is a universal factor. It indicates the quality, storage shelf life, and processability of a
raw material, intermediate, or end product. For example, substances which are too dry in production may cause
problems with static discharge or affect the consistency of the end product. If substances are too moist, they
may agglomerate or get stuck inside the pipes. They may have a reduced shelf life.

Moisture/water content is also an important quality criterion influencing taste and consistency.

International and national standards define the permitted thresholds for moisture/water content for products sold
commercially. Regulators such as the BRC (British Retail Consortium), IFS (International Featured Standards), or
GFSI (Global Food Safety Initiative) are having an increasing impact on the production, processing, and sale of
foods. This increases the work involved in quality assurance and demands more and more modern and efficient
solutions. Analysis methods must be clearly described and tested. The method, its parameters, and the permit-
ted measurement tolerance are defined.

Many food producers themselves have strict criteria for measurement accuracy, reliability, and traceability in or-
der to ensure the quality of their products. These SOPs (Standard Operating Procedures) describe the entire mea-
surement process, including sample volume, number of required measurements, maximum tolerable deviation,
and procedures when errors are discovered.

METTLER TOLEDO's solutions support customers in the food production and processing industry, in food retail,
and in the control and testing of food products.

METTLER TOLEDO Moisture Guide 10

Clever ideas and solutions ensure high efficiency, user comfort, and measurement reliability. Each of the pre-
sented methods has its own advantages and disadvantages. Moisture analyzers and Karl Fischer titrators are
unbeaten when it comes to measurement duration. The drying oven method is better with large sample quanti-
ties and volumes. Karl Fischer titrators offer selectivity for water from low to high water content levels, and make
it possible to automate the water content determination process.

All users can find the right solution for their individual requirements in METTLER TOLEDO's range of sophisticated
instruments.

Overview of Advantages/Disadvantages of Presented Methods

Drying Ovens
Advantages • large number of samples
at same time, thus higher
throughput possible
• large sample volumes
possible
• high accuracy
Disadvantages • measurements only avail-
able after several hours
• sample material may
­decompose
• other liquid components
such as alcohol, flavors,
or acetic acid evaporate
• laborious procedure with
several working steps
• very high risk of error
­(particularly during man-
ual data entry and calcu-
lation)
• high risk of error when
­using hygroscopic sample
material
Moisture Analyzers Karl Fischer
• fast measurement • fast measurement
(approx. 2– 10 min.) (approx. 2 – 5 min.)
• large sample volumes • very accurate
­possible (also suitable for trace
• easy handling analysis)
• reduced risk of error • selective for water
• high throughput possible
with automation
• universal
• sample material may • methods depend on
­decompose or evaporate ­sample matrix
• no automation possible • risk of error caused by
• only one measurement can incorrectly entered water
be performed at a time (ambient air, solvent)
• other volatile components • use and storage of
such as alcohol, flavors, chemical reagents
or acetic acid evaporate

METTLER TOLEDO Moisture Guide 11

Good Measuring Practices
Five Steps to Improved Measuring Results

Good Measuring Practices by METTLER TOLEDO is a global program sup-

porting you in laboratory and production environments with quality assur-
ance measures for balances, scales, pipettes and analytical instruments.
The five steps of all Good Measuring Practices guidelines start with an
evaluation of the measuring needs of your processes and their ­associated
risks. We also take into account regulatory requirements and norms
­relevant to your industry.
With this information, Good Measuring Practices provide straight forward
recommendations for selecting, installing, calibrating and operating of
weighing and measuring instruments.­

www.mt.com/gwp for weighing

www.mt.com/gtp for titration
www.mt.com/gpp for pipetting
www.mt.com/gdrp for density and refractometry

5
Routine 1
Operation Evaluation

Good
Measuring
4
Calibration / Practices 2
Qualification Selection

3
Installation /
Training

www.mt.com
For more information

Mettler-Toledo Group
Laboratory Division
www.mt.com/contacts

Subject to technical changes

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