Gravimetric Determination of Water by UNIT A1.

1
Drying and Weighing
Water (moisture) in a sample is measured gravimetrically by determining the weight loss
in a sample after it has been placed in an appropriate oven (convection, vacuum, or
microwave) for a given time. In addition, there are automatic moisture analyzers available
that utilize infrared lamps as a heat source. These types of moisture analyzers are fast but
many times are matrix dependent, which requires some trial-and-error testing to deter-
mine the correct settings (power and time). Water and moisture are used interchangeably
in the description of these protocols. In addition, it is assumed in the gravimetric method
that only water is removed in the drying process, when in fact there may be volatile loss
in some samples.
Although the measurement of weight loss due to evaporation of water is frequently used
to calculate moisture content, it should be pointed out that the value obtained may not be
a true measure of water content. In some samples, only a proportion of the water present
is lost at the drying temperature. The balance (bound water) is difficult to remove
completely. In addition, the water lost may actually increase as the temperature is raised.
Some samples with high fat content may exhibit volatile oil loss at drying temperatures
of 100°C. Weight loss may also be dependent on such factors as particle size, weight of
samples used, type of dish used, and temperature variations in the oven from shelf to shelf.
Thus, it is important to compare results obtained using the same drying conditions.
This unit provides three protocols for which there are established procedures for various
matrices. The Basic Protocol describes water removal and quantitation after a sample is
placed in a convection oven. It is probably the method of choice when one does not know
which method to choose when dealing with an unknown matrix, or when one looks at
samples that foam excessively in the vacuum oven method or “react,” such as popcorn
under vacuum. Alternate Protocol 1 describes water removal and quantitation after a
sample is placed in a vacuum oven. Because it is at reduced pressure, drying times are
slightly reduced compared to the convection method. In addition, drying temperatures
<100°C are possible, which is important for samples that may decompose at higher drying
temperatures. Alternate Protocol 2 describes water removal using a microwave source
where such analyzers measure and calculate loss automatically.

MEASURING MOISTURE USING A CONVECTION OVEN BASIC

Water is measured in a sample by determining the loss in weight for the sample after it PROTOCOL
has been dried in a convection oven. The method requires only a small amount of
homogeneous sample and can measure an effective range of 0.01% to 99.99% water.
Materials
Homogeneous sample
Convection oven capable of maintaining a temperature of 103° ± 2°C
Aluminum weighing dishes (with or without covers)
Desiccator with desiccant
Balance capable of measuring ±0.1 mg
1. Set the temperature of a convection oven to 105°C.
2. Dry an aluminum weighing dish (and cover, if used) ≥1 hr at 105°C. Cool and store
dried dish in a desiccator. Cool ≥30 min before using.
Covered weighing dishes are useful when analyzing samples that splatter. Weighing dishes Gravimetric
without covers may otherwise be preferred, as they are disposable. Measurements of
Water
Contributed by Rennie P. Ruiz A1.1.1
Current Protocols in Food Analytical Chemistry (2001) A1.1.1-A1.1.6
Copyright © 2001 by John Wiley & Sons, Inc.
 3. Weigh empty, dried dish (with cover, if used) to nearest 0.1 mg.
4. Add 3 to 10 g homogeneous sample to dish and weigh (with cover, if used) to nearest
0.1 mg.
5. Place dish with sample into oven and dry 4 hr.
6. Remove dish with dried sample and cool 30 min in a desiccator.
7. Weigh cooled dish with dried sample.
8. Return dish with sample to oven, dry for another hour, cool, and reweigh.
9. If weight has not changed, test is done. If weight is lower, continue drying for 1-hr
periods and reweighing until constant weight is achieved.
Depending on the sample, drying times can be ≥16 hr.
10. Calculate moisture as the percent loss in weight after drying.

ALTERNATE MEASURING MOISTURE USING A VACUUM OVEN

PROTOCOL 1
Water is measured in a sample by determining the loss in weight for the sample after it
has been dried in a vacuum oven. The method requires only a small amount of homoge-
neous sample and can measure an effective range of 0.01% to 99.99% water. As indicated
earlier, the vacuum oven method allows one to dry samples at temperatures <100°C. Some
matrices may require drying at 70°C (Table A1.1.1), but the following procedure addresses
a drying temperature between 95° and 100°C.
Additional Materials (also see Basic Protocol)
Sulfuric acid
Vacuum oven capable of withstanding vacuum ≤100 mmHg and maintaining
temperature of 95° to 100°C
Vacuum pump capable of maintaining a vacuum ≤100 mmHg
500-ml gas washing bottle
CAUTION: Sulfuric acid is hazardous, causing severe burns, and must be handled and
disposed of accordingly. See Safety Appendix (APPENDIX 2B).
1. Set up a vacuum oven by connecting the oven air outlet to a vacuum pump. Connect
the oven air inlet to a 500-ml gas washing bottle that contains sulfuric acid. Set oven
temperature to 95° to 100°C.
The sulfuric acid is used to dry the air that is admitted during drying.
2. Dry an aluminum weighing dish (and cover, if used) ≥1 hr at 100°C. Cool and store
dried dish in a desiccator. Cool ≥30 min before using.
Covered weighing dishes are useful when analyzing samples that splatter. Weighing dishes
without covers may otherwise be preferred, as they are disposable.
3. Weigh empty, dried dish (with cover, if used) to nearest 0.1 mg.
4. Add 3 to 10 g homogeneous sample to dish and weigh (with cover, if used) to nearest
0.1 mg.
5. Place dish with samples into vacuum oven and close oven door.

Gravimetric
6. Close both air inlet and outlet valves to oven. Start vacuum pump and slowly evacuate
Determination of air from inside the oven by opening the oven outlet valve. Once pressure is ≤100
Water by Drying mmHg, open oven air inlet slightly so that air is drawn into the gas washing bottle,
and Weighing

A1.1.2
Current Protocols in Food Analytical Chemistry
Table A1.1.1 Recommended Moisture Protocols

Matrix Recommended oven type Conditions

Animal feeds Vacuum 2 hr at 95°-100°C
Ice cream/frozen desserts Convection 3.5 hr at 100°C
Cheese Vacuum 4 hr at 100°C
Dried milk Vacuum 5 hr at 100°C
Seafood Convection 4 hr at 100°C
Meat Convection 16-18 hr at 100°C
Meat and poultry products Microwave Mode 2
Dried eggs Convection 5 hr at 98°-100°C
Frozen french-fried potatoes Convection 16 hr at 103°C
Tomato/tomato products Microwave Mode 1, 4 min
Canned vegetables Vacuum Constant weight at 70°C
Dried fruits Vacuum 6 hr at 70°C
Fruit/fruit products Vacuum Constant weight at 70°C
Nuts/nut products Vacuum 5 hr at 95°-100°C
Flour Vacuum 5 hr at 98°-100°C
Sugars Convection 3 hr at 70°C
Sugars Vacuum 3 hr at 100°C

through the sulfuric acid, and into the oven at a rate of ∼2 bubbles/sec. Dry sample
4 hr.
7. Isolate vacuum pump by closing oven outlet valve and carefully admitting dried air
into oven (by slowly opening air inlet valve fully), increasing the pressure inside oven
until the door can be easily opened. Remove drying dish with sample and cool 30
min in a desiccator.
8. Weigh cooled dish with sample.
9. Repeat steps 5 to 8, except dry for 1 hr.
10. If weight has not changed, test is done. If weight is lower, continue drying for 1-hr
periods and reweighing until constant weight is achieved.
Most samples take ∼4 hr to dry.
11. Calculate moisture as the percent loss in weight after drying.

MEASURING MOISTURE USING A MICROWAVE MOISTURE ANALYZER ALTERNATE

PROTOCOL 2
Water is measured in a sample using a microwave moisture analyzer that uses microwave
energy to remove water. The instrument weighs the sample both before and after drying
and calculates the percent moisture automatically. The analyzer can measure an effective
range of 0.1% to 99.9% water, but may have problems at the lower range due to burning
or scorching, especially if there is a high sugar content.
The microwave moisture analyzer allows one to dry a sample by two modes. Mode 1 dries
a sample at a specific power setting for a given time period. Mode 2 dries a sample at a
specific power setting using a time period that is determined by the analyzer itself, ending
the run when no weight change is achieved within a preset time interval criterion. This
protocol looks only at Mode 1 operation.
Gravimetric
Measurements of
Water

A1.1.3
Current Protocols in Food Analytical Chemistry
 Materials
Homogeneous sample
Microwave moisture analyzer (e.g., AVC-80, CEM Corp.)
Fiberglass sample pads
1. Turn on a microwave analyzer and let warm up 30 min.
2. Set analyzer for Mode 1 operation, setting power to 100%, display to % moisture,
and drying time interval to 4 min.
3. Dry two fiberglass sample pads by placing them on the balance ring, dropping cover
over pads, and closing analyzer door.
4. Press “tare,” wait for reading to stabilize, then press “run” to start drying program.
5. When drying is done, press “tare,” wait for reading to stabilize, and then remove
fiberglass pads.
6. Deposit ∼1 to 2 g sample onto the rough side of one fiberglass pad. If sample is a
liquid, use a pipet to cover as much of the pad as possible. If a semisolid, use a spatula
to spread as evenly as possible. Avoid lumps. Apply sample as quickly as possible to
avoid loss of moisture during application.
7. Place second pad, rough side down, on top of sample and place pads and sample on
balance ring in analyzer.
8. Drop cover over sample, close analyzer door, wait for displayed weight to stabilize,
and then start the drying process by pressing “run.”
Program ends after 4 min and calculates percent moisture automatically.
9. Remove pads and inspect dried sample for areas of scorching, burning, or wetness.
If these conditions exist, repeat test, being careful to spread the sample as evenly as
possible onto pad.
Scorching and burning may indicate that the power setting is too high, and wetness may
indicate improper spreading of the sample.
When running many samples, several sets of pads can be placed inside the analyzer so that
they may dry while samples are actually being run. This way, separate sets of pads do not
have to be dried individually, and it is possible to begin at step 5 to tare the dried pads
before use.

COMMENTARY
Background Information
Moisture analyses are important because
samples contain water either as chemically
combined hydrates or as occluded surface-ad-
sorbed moisture. Water is an inherent part of
most biological substances and constitutes
>90% of the fresh weight of some plant mate-
rials. To afford reproducible analytical results,
samples are usually dried before analysis and
the percentage composition of the sample is
then calculated on a dry basis.
Gravimetric analyses for moisture are prob-
Gravimetric ably the easiest procedures to use, as there are
Determination of no chemicals to prepare. Manpower is at a
Water by Drying
and Weighing minimum, requiring only a weighing step be-
fore and after heating in an appropriate oven.
As an example, ∼29 of the 35 moisture methods
recognized by the Association of Official Ana-
lytical Chemists (AOAC) for nutritional label-
ing are gravimetric methods using some sort of
a drying oven (Sullivan and Carpenter, 1993).
The only concern with gravimetric methods,
using either a vacuum or convection oven, is
the amount of time required for drying. Most
samples take ∼4 hr in a vacuum oven. Use of a
convection oven, at 1 atm and slightly higher
temperature, could add as much as 16 hr de-
pending on the sample (e.g., unpopped corn
kernels). Because of the long drying times,

A1.1.4
Current Protocols in Food Analytical Chemistry
analyzing as many samples as possible at one
time can maximize sample throughout.
Microwave moisture analyzers are the next
step in gravimetric analyses by focusing on
much shorter drying times. Currently there are
only a few matrices recognized by the AOAC
for use in the microwave drying method (Sul-
livan and Carpenter, 1993). Although there
hasn’t been a collaborative study for AOAC
approval to support other matrices, the micro-
wave moisture analyzer has been used success-
fully in such matrices as grains (Okabe et al.,
1973) and flours (Davis and Lai, 1984).
The choice of which protocol to use will
depend on what type of matrix is being tested.
As a first suggestion, Table A1.1.1 is provided
based on the matrices and methodologies cur-
rently recognized by the AOAC (Sullivan and
Carpenter, 1993). As one can see, many matri-
ces can be run by more than one gravimetric
technique. The method used will depend on the
matrix or on the end use of the dried sample.
For a general review of all methods, Karmas
(1980) has written an evaluation with emphasis
on food matrices.
Critical Parameters and
Troubleshooting
All gravimetric methods require only a very
small amount of sample (between 1 and 10 g
depending on the moisture level). Therefore,
sample homogeneity is very critical and special
care must be given to sample blending before
subsampling for analysis. The method used for
homogenization will depend on the type of
sample being analyzed. Blenders, homogeniz-
ers, mincers, food processors, and graters are
currently available for dry, moist, and very wet
samples. Because these devices produce heat,
it is very important not to overhomogenize,
which causes moisture to be lost. Once a sample
has been properly homogenized, it is important
to either run the sample for moisture as soon as
possible or transfer it to either a dry glass or
plastic container with a well-fitting closure or
seal.
In the gravimetric method, low-moisture
samples will only produce a very small loss of
weight upon drying. It is important not to con-
taminate the samples when drying them or
transferring them to the oven or desiccator. Do
not handle dishes with bare hands; use tongs or
Kimwipes. Assuming that good weighing tech-
niques are used, the other source of problems
stems from the drying portion of the test. Sam-
Current Protocols in Food Analytical Chemistry
ples that foam excessively or splatter when
heated require the use of covered weighing
dishes. Covers also prevent cross-contamina-
tion to neighboring samples in the oven should
splattering occur. Very high-moisture samples
can also be dried, after initial weighing, in a
convection oven to reduce the volume before
drying in a vacuum oven. This may help with
samples that foam and spill over the sides of
the weighing dish. For the microwave oven
method, how the sample is placed on the fiber-
glass pad is critical. Samples must be spread
out as smoothly as possible with the spatula.
Lumps and thick areas of sample on the pad
may not be completely dried at the end of the
test. Improper spreading of the sample, or two
high of a power setting, may also lead to areas
of scorching or burning on the pad.
Anticipated Results
The concentration range for gravimetric
analyses of moisture is between 0.01% and
99.99%. Relative standard deviations of ±1%
are achievable.
Literature Cited
Davis, A.B. and Lai, C.S 1984. Microwave utiliza-
tion in the rapid determination of flour moisture.
Cereal Chem. 61:1-4.
Karmas, E. 1980. Techniques for measurement of
moisture content of foods. Food Techno. 34:52-
59.
Okabe, T., Huang, M.T., and Okamura, S. 1973. A
new method for the measurement of grain mois-
ture content by the use of microwaves. J. Agric.
Eng. Res. 18:59-64.
Sullivan, D.M. and Carpenter, D.E. (eds.) 1993.
Methods of Analysis for Nutritional Labeling.
Association of Official Analytical Chemists
(AOAC) International, Arlington, Va.
Key References
American Association of Cereal Chemists, Inc.
1995. Approved Methods of the AACC, 9th ed.
American Association of Cereal Chemists
(AACC), Inc., St. Paul, Minn.
Current methodologies for use on grains and grain
products recognized by the AACC, including mois-
ture analyses based on convection, vacuum, and
microwave ovens.
Cunniff, P. (ed.) 1998. Official Methods of Analysis
of the Association of Official Analytical Chem-
ists, 16th ed., 4th revision. AOAC International,
Gaithersburg, Md.
Current methodologies for use on foods and non-
food products recognized by the AOAC, including
moisture analyses based on convection, vacuum,
and microwave ovens. Gravimetric
Measurements of
Water
A1.1.5
 Kirk, R.S. and Sawyer, R. 1991. Person’s Composi-
tion and Analysis of Foods, 9th ed. Logman
Scientific & Technical, Essex, England.
A useful introduction to general food analysis.
Pomeranz, Y. and Meloan, C.E. 1994 Food Analysis,
3rd ed. Chapman & Hall, New York.
A useful introduction to general food analysis.

Contributed by Rennie P. Ruiz

Hunt-Wesson, Inc.
Fullerton, California

Gravimetric
Determination of
Water by Drying
and Weighing

A1.1.6
Current Protocols in Food Analytical Chemistry