The Ultimate Moisture & Water Guide: Proven Methods & Procedures
The Ultimate Moisture & Water Guide: Proven Methods & Procedures
Determination of
Moisture and Water
Content in Food
Moisture Analyzer
Karl Fischer Titration
Analytical Balances
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
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.
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.
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.
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. 3: The XPE205 analytical balance from METTLER TOLEDO offers high
performance, ease of use, and minimal risk of error thanks to its clever design.
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
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
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
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.
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.
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
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.
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.
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
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.
All users can find the right solution for their individual requirements in METTLER TOLEDO's range of sophisticated
instruments.
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