2.

6 On-Line Measurement
of Moisture Content
Satoru Watano
Osaka Prefecture University, Sakai, Osaka, Japan

2.6.1  Introduction
Powder-handling processes are mainly categorized into wet and dry processes.1,2 In wet processes,
the degree of wetness (moisture content) seriously affects physical properties (size, shape, density,
etc.) of the final products. In order to produce the desired product efficiently and continuously with-
out difficulty, monitoring and control of moisture content are required. Even in dry processes, mois-
ture content sometimes causes problems. Generally, powder materials contain moisture, to some
extent as water of hydration, bound water, and so forth, which exists on the powder surface or forms
liquid bridges between powders. Moisture on the powder surface greatly changes the powder’s
properties such as flowability and internal friction, causing handling problems. The liquid bridges
generate agglomeration of powders and adhesion to the vessel wall. In all cases, control of moisture
content is necessary in order to avoid problems.

2.6.2  Electrical Methods

Table 6.1 lists moisture sensors and their measuring principles. In powder-handling processes, there
are no sensors which can measure moisture content directly. Therefore moisture content is deter-
mined by using the correlation between indirect parameters (absorbance of spectrum, dielectric
constant, etc.) and moisture content that have been previously measured by a direct method (such
as the drying method).
So far, chemical, electrical, and optical methods, as well as methods applying radioactive rays and
nuclear magnetic resonance spectrometry, have been available for powder-handling processes. Among
them, electrical and optical methods have been widely used in industrial practical application.
In the following, electrical and optical methods for measuring moisture content of powder mate-
rials are briefly explained.
Figure 6.1 illustrates a schematic diagram of an electrical resistance-type moisture sensor. In this
sensor, moisture content is determined by measuring the electrical resistance change due to moisture
increase/decrease. As seen in the figure, powder samples are packed between two electrodes, and
apparent specific resistance R is determined by measuring the applied voltage V and the electric
current I as

VS (6.1)
R
Id
where S and d indicate areas of electrode and distance between the two electrode, respectively. The
apparent specific resistance R varies with moisture content W as

log R a log W  b (6.2)

317

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Table 6.1  List of Moisture Sensors

318
Methods Principle of measurement Continuous Detach/contact to Wide Range
measurement powder bed application
Normal drying 0.1~100%
Drying method Infrared heating Measuring weight loss due to drying of × Contact j
High frequency induction heating wet samples.
0.01~20%
Distillation method Perform distillation and measure water × Contact j
Chemical method volume.
Water is titrated with KF reagent 0.001~100%
Karl Fischer (KF) titration method containing iodine, sulfur dioxide and × Contact j
pyridine in methanol. Infinitesimal
moisture content can be determined.
Electric resistance method (DC) Measure electric resistance change 3~50%
(direct current) due to moisture j Contact j
increase/decrease.
Measure electric current (high 0.1~60%
Electric method Method applying high frequency frequency) change due to moisture j Contact j
increase/decrease. Smaller quantity of
water can be detected than the DC
method.
Method applying dielectric Measure dielectric constant change due to j Contact j 2~25%
constant (electrostatic capacity) moisture increase/decrease.
Method applying infrared ray Measure absorbance of infrared –ray at j Detach j 1~90%
Optical method absorption band (1.43, 1.94µm) of
water near infrared.
Method applying microwave Measure attenuation of microwave due to j Detach j 1~90%

Powder Technology
water.
Nuclear Magnetic Contact 0.1~90%
Resonance (NMR) Sample is dissolved in a solvent and its NMR × ×
Spectrometer is measured.

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Method measuring moderation/ Measure moderation/ scattering of neutron/γ- 2~80%

On-Line Measurement of Moisture Content

Method applying scattering ray due to water.
radioactive rays Method measuring attenuation strength Measure attenuation strength of β or γ- rays j Detach ×
due to water.
Other method Balanced relative humidity Calculate moisture content by relative j Detach j 1~80%
humidity, which is balanced with
circumstances.

 : Possible ×: Impossible A: Very good B: good C: Poor

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 320 Powder Technology

Figure 6.1 Schematic diagram of electrical resistance-type moisture sensor.

where a and b are constants depending on the shape of electrode, properties of powder materials, and
circumstance conditions (humidity and temperature). By using Equation 6.2, moisture content can be
determined. For the electric current, direct current (DC) or high-frequency alternating current is used.
The electrical resistance-type moisture sensor is widely used since its electrical circuit is simple,
the measurement principle is easy, and the measurement time is short. However, it has some draw-
backs: (1) temperature correlation is required since the electrical resistance generates heat, (2) it cannot
be used for a powder bed that moves during the measurement since powder packing conditions affect
the resistance, and (3) measurement error may occur if the powder sample contains electrolyte.
Figure 6.2 shows a schematic diagram of a dielectric constant-type moisture sensor. Assuming
that the electrical capacity when powder materials exist inside between two electrodes or inside a
cylindrical electrode is C1, and the one without any powder materials is C0, the apparent dielectric
constant a is obtained as

C1 (6.3)
a  0
C0

By using the apparent dielectric constant, moisture content can be determined, since the apparent
dielectric constant a shows an approximately linear relationship to moisture content as

 a  j  kw (6.4)

where j and k are constants. These constants require previous calibration, since they vary with dif-
ferent powder materials. The dielectric constant-type moisture sensor has merits in that it is less
affected by temperature and packing conditions than the electrical resistance-type moisture sensor.
However, its circuit is complicated, and it cannot measure moisture content of powder materials
containing electrical conductors, such as metal and coal powders.

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 On-Line Measurement of Moisture Content 321

Figure 6.2 Schematic diagram of a dielectric constant-type moisture sensor.

A microwave-type moisture sensor is able to measure moisture content continuously without

touching the objective material. Figure 6.3 investigates absorbance characteristics of microwaves
in the case of flour and cornstarch powders. When the microwaves are transmitted to the powder
material containing water, water absorbs the microwaves and the microwaves attenuate. Since the
degree of attenuation has a correlation to moisture content, as shown in Figure 6.3, moisture content
of powder materials can be determined. However, the system is complicated to avoid the microwave
leakage. In addition, the measured value may vary to some extent, depending on the leakage/refrac-
tion, powder surface condition, and temperature.

2.6.3  Infrared Moisture Sensor

In general, an optical sensor utilizes the principle that physical values (concentration, distance, etc.)
are indirectly detected by using the absorbed/reflected energy of spectra when the spectra are radi-
ated to the object. The so-called spectra are categorized into ultraviolet, optical, and infrared rays,
depending on the wavelength, and each sensor uses a specific wavelength, which fits characteristics
of the measured object.
Figure 6.4 shows infrared (IR) absorption characteristics.3,4 Water absorbs infrared spectra
markedly at wavelengths of 1.43, 1.94, and 3.0 μm, due to the resonance with atomic vibration
between oxygen and hydrogen in water molecules. Since energy of IR spectrum is absorbed remark-
ably at these wavelengths in proportion to moisture content, moisture content can be detected by
measuring the difference between the irradiated energy and the reflected one. Since the absorption
spectrum measurement is easily disturbed by granule surface conditions and fluctuation in beam

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Figure 6.3 Relationship between degree of microwave attenuation and moisture

content.

length, a reference method which calculates the reflected energy ratio of the absorbed spectrum
(1.94 μm) and of the bilateral unabsorbed spectrum (reference spectrum of 1.78 and 2.14 μm) has
been adopted. This cancels out any disturbance, since the disturbance affects the absorbed and
unabsorbed spectra equally.
Details of the IR moisture sensor are illustrated in Figure 6.5. The continuous light from the source
is condensed by a condenser, then changed to a chopper beam by passing through a rotating sector of
four optical filters composed of the different selective spectra of 1.94 μm for absorption, the bilateral
1.78 and 2.14 μm for unabsorbed references, and a visible spectrum for targeting. When these portions
of the spectra are irradiated to the object, the absorption spectrum is absorbed in proportion to the
moisture content of the object, while the reference spectra are fully reflected.4 These spectra are trans-
formed into electrical signals, and the degree of absorptivity, defined as the ratio of energy absorbed to
the supplied energy of the spectrum, is calculated. Based on the degree of absorptivity, the absorbance
X, the output from the moisture sensor, is calculated using the following equation:

 ( k  V2  V3 )  2 
X  k0  In  2 
 k1  V1  (6.5)

where, V1, V2, and V3 show absorption at 1.94, 1.78, and 2.14 μm in the IR spectra after temperature
compensation, respectively, and k0 , k1, and k2 indicate the calibration coefficients, respectively.

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 On-Line Measurement of Moisture Content 323

Figure 6.4 IR absorption characteristics of powder material (lactose and cornstarch

mixed 7:3 by weight) under various moisture contents.

Although the infrared moisture sensor is able to measure moisture content continuously without
touching to the object and is not influenced by powder density and packing conditions very much,
it measures moisture content on the surface or just below the surface of the object due to the long
wavelength. Normally, moisture is distributed inside the powder material, and there are variations in
moisture content between the surface and the core. Therefore, in order to measure moisture content
by using the infrared sensor, a calibration curve between sensor output (surface moisture content
detected by IR sensor) and total moisture content measured by a drying method is used.
Figure 6.6 indicates the calibration curves when the lactose and cornstarch mixing ratio was
varied.3 The calibration curves are different depending on the powder materials.3 It is because the
powder’s physical properties such as water-absorbing potential, surface conditions, IR refraction
characteristics, and moisture distribution are different.

2.6.4  Application of Moisture Control to Powder-

Handling Processes
Wet granulation is one of the most sensitive operations to moisture content. Wet granulation is
defined as a size enlargement that adheres or sticks powders together by using liquid binders to
produce granules having the desired size, shape, and density. The properties of the final product are
significantly influenced by the moisture content.5,6,7 Therefore, monitoring and control of moisture
content are required to produce the desired product continuously and with high accuracy.

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 324 Powder Technology

Figure 6.5 Details of IR moisture sensor.

Figure 6.6 Calibration curves under various lactose and cornstarch mixing ratios.

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 On-Line Measurement of Moisture Content 325

Figure 6.7 Relationship between granule mass median diameter and moisture
content.

Figure 6.8 Moisture control system in fluidized-bed granulation.

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 326 Powder Technology

Figure 6.7 illustrates a system which measures and controls moisture content by using an IR
moisture sensor in a fluidized-bed granulation.4,8,9 The IR detector and fluidized-bed vessel are con-
nected by optical fibers, and heated purge air is blown at the extremity of the sensor (the place where
the optical fibers are connected at the vessel wall) to prevent powder sticking.
Figure 6.8 indicates the relationship between granule mass median diameter and moisture con-
tent when powder samples composed of lactose, cornstarch, and hydroxypropylcellulose (HPC) are
granulated by a purified water (binder).3 Figure 6.8 shows the granule mass median diameter has a
linear relationship to the moisture content, implying that granule growth can be controlled by mea-
suring and controlling the moisture content.
In the Japanese pharmaceutical industry, automatic manufacturing of drugs (granules) is com-
monly conducted by fluidized-bed granulation with moisture control, and uniform properties can be
maintained easily.10

References
1. Gotoh, K., Masuda, H., and Higashitani, K., Eds., Powder Technology Handbook, 2nd Ed., Marcel
Dekker, New York, 1997.
2. Society of Powder Technology Japan, Ed., Huntaikogaku binran, 2nd Ed., Nikkan Kogyo Shinbun,
Tokyo, 1998.
3. Watano, S., Hideo, H., Sato, Y., Miyanami, K., and Yasutomo, T., Adv. Powder Technol., 7, 279–289,
1996.
4. Watano, S., Sato, Y., and Miyanami, K., J. Chem. Eng. Jpn., 28, 282–287, 1995.
5. Watano, S., Morikawa, T., and Miyanami, K., J. Chem. Eng. Jpn., 28, 171–178, 1995.
6. Watano, S., Morikawa, T., and Miyanami, K., Chem. Pharm. Bull., 44, 409–415, 1996.
7. Schaefer, T. and Worts, O., Arch. Pharm. Chem. Sci., 5, 178–193, 1977.
8. Watano, S., Yamamoto, A., and Miyanami, K., Chem. Pharm. Bull., 42, 133–137, 1994.
9. Watano, S., Takashima, H., and Miyanami, K., J. Chem. Eng. Jpn., 30, 223–229, 1997.
10. Watano, S., Takashima, H., Miyanami, K., Murakami, T., and Sato, T., Chem. Pharm. Bull., 42,
1302–1307, 1994.

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