Professional Documents
Culture Documents
7 Water Content
w ALTER H. GARDNER
Washington State University
Pullman, Washington
1.18
1.16 kAOLINITE'
..
~ 1.14
z
::;)
..
~ 1.12
.. 1.08
....r
<!1
;;:; 1.06
~
QUA~rz O~ FELDSPAR
I • 00 t..=::::L=::C==J:::::::::l::::=~~6~~:t:-:-~ 0
o 100 200 300 400 SOO 00 700 eo
TEMPERATURE, DC.
Fig. 7-1. Weight loss of clay minerals as a function of temperature. The weight of
the sample at a temperature of 800°C. or greater is taken to be unity. Water
content percentages on a mass basis may be obtained by subtracting 1 from the
ordinate figure and multiplying by 100. (The numbers to the right of the decimal
thus may he regarded as percentages.) (Nutting, 1943.)
water and adsorbed water, and it is often difficult to tell them apart. 1 Some
representative thermal dehydration curves (after Nutting, 1943) are pre-
sented in Fig. 7-1. 2 These curves show the weight loss of samples that were
initially at room temperature and in equilibrium with room humidity of ap-
proximately 60%, as the samples were heated to constant weight at various
temperatures. The weight at a temperature of 800°e. or slightly higher is
taken to be unity. It is not clear from the curves what part of the water is
adsorbed water and what part is structural water. But it should be obvious
from these curves that for colloidal minerals it is important to specify the
1 The term "structural water" refers to water derived from components of the
mineral lattice itself, whereas the term "adsorbed water" refers to water attached
to the mineral lattice but which is not a structural component of the lattice. Some
adsorbed water may be located with respect to the laUice in such a way that the diffi-
culty of removal is comparable to that for structural water. (Difficulty here refers
generally to the temperature required for removal and possibly to the fineness of the
particles). The exact situation depends upon the nature of the particular mineral.
2 It should be recognized that the character of the thermal dehydration curve de-
pends upon the purity of the sample, so that it is unlikely that curves for the same
type of minerals constructed by various workers would be identical.
86 WATER CONTENT
Since the variances due to the random error of all three weighings are likely
to be nearly the same, equation [8] is approximated by
V _
: _:
= 2V",lI,t
(y - t)2
[1 + (y --
(x - t)2] .
t)2
[9]
Combining equation [3] with equation [9] and replacing (y - t) by the dry
mass of the soil z gives:
[10]
For water contents and sample sizes ordinarily encountered in soils work,
()2 is negligible so that equation [10] further reduces to
Vo = 4V",y,t «()
Z2
+ 1) [II]
Us = 2U",II,1 VO + 1• [12]
Z
[13]
and equation [8] is not needed since the tare weight is not obtained inde-
pendently. However, if the tare compensation involves a constant bias, this
does affect the accuracy of the resulting water content figure. The effect on
water content values of a constant bias e due to a tare error or other causes,
90 WATER CONTENT
Ue = U X • lI vi + (0 + 1)2 [17J
Y
which, when 82 is regarded as negligible, reduces to
[19J
1.0
~ .8 \ \\ ~ "':L"
\~ ~\. s¥
~
i
.ct:
a::
lJJ
,7
,6
,5 ~
(]'=
• 01 \ ~l'
"'- ~~"-
'" '"
5%
f-
z
~ .4
f1 =
• Ol. II
\\ '\ "" "- ~
5%" ~ 5~
~ ~. r........,
(.) ,3
cr
lJJ
~ ,2
~~
~ ~ 50%
~
• I
\ .::::::-
5~-":
~~
10 20 30 40 50 60 70 80 90 100
DRY MASS, %, GMS.
Fig. 7-2. Error in water content measurements as a function of the dry mass of the
sample at various weighing precisions and for 5% and 50% water contents on a
dry-mass basis (equation [19]). The value of E is 300o, and the weighing precision
is the standard deviation 00 for the balance in grams. When tare compensation is
used E should be multiplied by (2)'/2/2, and where n replicate determinations are
made, by a factor of 1/(n)'/2. If z is taken as the wet mass of the sample the error
E from the graph should be multiplied by (0 + I), as can be seen from equation
[20]. The dashed curves, for 50% water content, result when the o' term in equa-
tions [10] and [17] is not ignored.
7-2.2.1 INTRODUCTION
7-2.2.2 METHOD
the soil make for low precision. Because of this low precision, it is possible
to discard large stones prior to oven-drying without affecting the precision.
Rocks and stones to be discarded are carefully and quickly brushed to
avoid soil loss and to reduce evaporation loss, and then are weighed.
Conventional cylindrical tube samplers may be used in some gravelly and
stony soils. However, as the number or size of stones increases, the utility
of such sampling devices diminishes. In these kinds of soils it is important
to determine the volume sampled each time a water content determination
is to be made. Where core-type samplers can be used this is not difficult.
However, where large rocks and stones interfere seriously, other methods
must be used. One useful method involves sampling with a spade or shovel
and determining the volume of the hole which is dug. The volume may be
measured by placing a rubber or plastic membrane in the hole and filling
it with water from a container filled to a known volume. The quantity of
water used in filling the hole is easily determined. Grain millet or dry
sand which flQw easily and pack easily to constant bulk density may also
be used to fill the hole; and, if the material is to be discarded, the rubber
or plastic membrane is not needed. A detailed description of the method is
given in section 30-3. No simple, inexpensive methods have as yet been
developed for sampling beyond shallow depths without digging an access
hole.
Certain general requirements must be met in the development of a pro-
cedure for obtaining accurate and reproducible water content measure-
ments. Foremost of these is the requirement that the sample be dried at a
specified temperature to constant weight with nothing being lost but water.
This is rarely possible with a colloidal material like soil, particularly if it
contains any appreciable organic matter. Weight losses during drying at
100 0 to 110°e. for periods as long as 15 days have been observed in soils
ranging from fine sands to silty clay loams. Because of this it is important
to specify the details of the drying procedure used in rcporting watcr con-
tents whcre precisc values arc nceded.
Since accuracy in water content determinations hinges upon existcnce of
a dcfinable dry condition which, with soil, can only be based upon subjcc-
tive judgment, it is more appropriate to refer to reproducibility than to
accuracy. Reproducibility in water content measurements can be achieved
in two ways: (1) treating every sample of a set to be compared exactly
thc same way in terms of such things as sample size and depth in the con-
tainer, drying temperature, and drying time; or (2) following techniques
which lead to equilibria which are as nearly independent of such variables
as is possible. From the latter point of view, the nature of the thermal de-
hydration curves (Fig. 7-1) suggests the desirability of choosing a drying
temperature in a region where the weight change of the colloidal constitu-
ents with temperature is at a minimum. Where the nature of the mineral
coIloids in a sample is unknown, the best temperature, as inferred from the
96 WATER CONTENT
curves of Fig. 7-1, is probably between 165° and 175°C. However, at such
temperatures, organic matter oxidation and decomposition is likely to be
excessive. Temperatures below about 50°C. appear to be required if oxida-
tion of the organic fraction is to be avoided. Hence, for a soil sample con-
taining organic matter, it is necessary to compromise unless elaborate
methods of determination are used.
Vacuum drying at relatively low temperature, with the temperature being
carefully controlled and specified when reporting, probably provides the
most reproducible drying data. To assure perfectly dry conditions, the usual
practice is to include a desiccant such as magnesium perchlorate in the
oven. This is necessary since ordinary vacuum drying ovens are not con-
structed to be leak-proof, and some air is pulled continuously into the dry-
ing chamber. Drying times are considerably shortened by use of vacuum
techniques. When a vacuum oven and careful techniques are substituted for
the ordinary oven, considerable improvement in reproducibility is possible.
7-2.3.1 INTRODUCTION
be used for larger samples and increased precision). Prepare a tripod which
fits inside the lid to support a 140-mesh screen (a screen with approxi-
mately O.l-mm. openings, preferably made of stainless steel). Make the
tripod just high enough to leave a l-cm. opening above the lip of the lid to
admit air to the burning alcohol under the screen. Make the diameter of
the base of the tripod several millimeters smaller than the diameter of the
can, thus permitting the can to function as a lid to cover the screen, tripod,
and sample during cooling and weighing. For weighing, use a balance,
preferably of direct-reading type, with a capacity of approximately 100 g.
or more and a precision of ±0.03 g. (standard deviation 0.01 g.) or less.
7-2.3.2.2 Reagent. Ethyl, methyl or propyl alcohol, technical grade.
7-2.3.2.3 Procedure. Place the screen and supporting tripod in the
open lid of the can, and weigh this and the bottom of the can (which now
forms a lid) together to obtain a tare weight. Spread about 10 g. of the
wet sample uniformly over the screen, quickly replace the cover, and weigh
the apparatu~ and sample together. Then drip alcohol onto the sample
with a medicine dropper until the sample is saturated and alcohol begins to
drip into the bottom cup. (Approximately 1/2 to 1 ml. of alcohol is re-
quired per gram of sample.) After saturation of the sample, ignite the alco-
hol and allow it to burn itself out. After a short cooling period (unless
high precision is desired the apparatus need not be completely cooled),
weigh the apparatus and soil again. Then apply additional alcohol as at
first, with precaution to avoid vapor "explosions" which may occur if the
sample is too hot. These may blow soil out of the container. Repeat the
burning and weighing process until constant weight is achieved. In many
tests of the method, only two burnings have been required to achieve the
desired precision of measurement. Compute the water content by standard
gravimetric methods described in section 7-2.2.
7-2.3.2.4 Comments. The major difference between this method and
ordinary methods using oven-drying lies in the temperature used to remove
the water. Bouyoucos (1937) reported finding temperatures of about
130°e. in the center of the sample and of about 160°C. near the edge.
Oganesyan (1958) reported temperatures of about 120° to l30°C. in the
surface of the soil and 90° to 100°e. at the center, increasing to from 110°
to 120°e. for the last few seconds of the burning. From the dehydration
curves of Fig. 7-], it is obvious that the soil will not have dried uniformly.
Likewise at such high temperatures, some organic matter is certain to have
been oxidized. However, such temperatures frequently are encountered in
drying ovens. Hence, the method can be expected to be no worse than
oven-drying methods under conditions where precise oven temperatures are
not maintained. A great many data reported in the literature show that the
Illethod produces results close to those of oven drying.
Although Bouyollcos (1938) regarded 11 % organic matter as the upper
limit for lise of the method, other investigators have successfully used this
98 WATER CONTENT
7-3.1 Introduction
7-3.2.1 PRINCIPLES
Electrical and thermal conductivity and electrical capacitance of porous
materials vary with water content. Such properties of materials can or-
100 WATER CONTENT
7-3.2.2 METHOD
7-3.2.2.1 Special Apparatus.
1. Wheatstone Bridge for measuring resistance: Bridges in common use
are of the alternating current type (usually 1,000 cycle) to avoid
polarization at the electrodes in the porous block. Both null-point and
deflection-type instruments are used. Because of ease of reading, deflec-
tion-type bridges, involving measurement of bridge unbalance, are prob-
ably the most common. Resistances to be measured range from a few
hundred ohms to 200,000 or more ohms, a single calibration curve often
covering as much as 100,000 ohms.
2. Porous blocks: Blocks now availablen arc made of a variety of porous
materials ranging from nylon cloth (Bouyoucos, 1949) and fiberglas
(Colman and Hendrix, 1949) to casting plasters (Bouyoucos and
Mick, 1940; Perrier and Marsh, 1958; and numerous others), the most
common being some form of gypsum. Various grades and kinds of cast-
ing plaster are mixed with different amounts of water and in a variety
of ways, including in some instances pouring the mix into the mold in
a partial vacuum. In some instances resin is added to the mix, which
changes the electrical characteristics and decomposition rate in the soil
(Bouyoucos, 1953). The method of preparation as well as the mix
governs the porosity of the block and the resulting response curve.
Some types of gypsum last longer in soil than others, Hydrocal B 11
(manufactured by U. S. Gypsum Co.) being the most resistant of cur-
rent plasters used.
• Several types of commercial blocks are available from such companies as the
W. R. Ames Co., Milpitas, Calif.; Delmhorst Instruments Co., Boonton, New Jersey;
Soilmoisture Equipment Co., Santa Barbara, Calif.; and Industrial Instruments Inc.,
Cedar Grove, New Jersey. Beckman Instruments, Berkeley Instruments Division,
Richmond, Calif., supplies fiberglas units which also contain a thermistor for tem-
perature measurement. These companies also handle resistance bridges for use with the
blocks.
102 WATER CONTENT
Then measure the resistance. Plot the resistance as a function of water con-
tent (3-cycle semilogarithmic paper is convenient).
To install a block in the field, form a hole vertically from the surface
or horizontally in the side of a trench. Wet the block thoroughly, place it
in the hole, and then pack soil around it to assure good contact with
the surrounding soil. Bring the leads to the surface, running them hori-
zontally for a short distance beneath the surface to assure that no con-
tinuous channel exists along the leads for passage of free water. After
equilibrium is reached, usually overnight, make resistance measurements
as desired, and convert them to water content values with a calibration
curve.
7-3.2.2.3 Comments. In calibration as well as under field conditions,
true water content equilibria are rarely reached, particularly in the dry
range. However, the uncertainty of the water content inference, at best,
does not justify an elaborate and time-consuming calibration. Under prac-
tical conditions when the resistance reading approaches a constant value,
equilibrium may be assumed to be close. In the wet range, for most porous
blocks, the resistance change with changing water content is small and the
precision is low. Precision is also affected by changes in the calibration
curve over successive wetting and drying cycles (Cannell, 1958). Blocks
have not proved satisfactory in sandy soils or in soils which shrink or
swell considerably.
It is common practice to place blocks into uniform groups according to
their resistance at saturation and to calibrate only selected blocks from
each group (Tanner, et aI., 1949). This practice does not completely en-
sure obtaining groups of blocks with like calibration curves. But, consid-
ering the low precision of the method when it is used for water content
determination, it is probably an adequate procedure.
The calibration procedure described is for desorption. The procedure
cannot be reversed easily to provide a sorption curve because of difficul-
ties associated with partially wetting a soil mass. However, a tedious pro-
cedure, involving condensation of water in a soil sample in a humidity
chamber, can be used for obtaining a sorption curve.
Calibration is often carried out in the field by obtaining water content
values gravimetrically and plotting them against resistance readings. Or,
blocks are placed in pots containing growing plants and the water content
determined by weighing the pot, with an estimate of plant weight being
subtracted (Cannell, 1958).
Electrical conductivity of a porous block depends upon the electrolyte
concentration of the conducting fluid as well as upon the cross section of
this fluid or water content. In a porous block made from an inert material,
the electrolyte which carries the current comes from the soil solution. Even
a small change in electrolyte concentration of the soil will influence the
resistance under such circumstances. In blocks made from gypsum the
104 WATER CONTENT
7-3.3.1 PRINCIPLES
Hydrogen nuclei have a marked property for scattering and slowing
neutrons. This property is exploited in the neutron method for measuring
water content. High-energy neutrons (O.Lto 10 Mev.) emitted from a
radioactive substance such as a radium-beryllium or americium-beryllium
neutron source are slowed and changed in direction by elastic collisions
with atomic nuclei. This process is called "thermalization," the neutrons
being reduced in energy to about the thermal energy of atoms in a sub-
stance at room temperature.
The two major factors involved in scattering and slowing of neutrons
are the transfer of energy at each collision and the statistical probability
of collision.
The average energy transfer at collision of a neutron with other nuclei
7-3 INDIRECT METHODS 1 05
depends largely upon the mass number of the nuclei encountered. The
average number of collisions required to slow a neutron from 2 Mev. to
thermal energies is 18 for hydrogen, 67 for lithium, 86 for beryllium, 114
for carbon, 150 for oxygen and 9A + 6 for nuclei with large mass numbers
A (Weinberg and Wigner, 1958, Table 10.1).
The statistical probability of collision is dealt with using the concept of
"scattering cross section" 10 which is a statistically derived, cross sectional
area measured in barns which is proportional to the probability of collision,
in this case, between neutrons and other nuclei. This scattering cross
section depends upon the nature of the nuclei encountered and the energy
of the neutron. The scattering cross section for hydrogen varies from about
1 barn at 10 Mev. to about 13 barns at 0.1 Mev. The cross section varies
considerably as the neutron continues to lose energy but is somewhat
higher in the thermal energy range. Other elements found in soil with
appreciable scattering cross sections (2 to 5 barns) are beryllium, carbon,
nitrogen, oxygen, and fluorine.
Considering both energy transfer and scattering cross section, it is evident
that hydrogen, having a nucleus of about the same size and mass as the
neutron, has a much greater thermalizing effect on fast neutrons than any
other element. In addition, when both hydrogen and oxygen are considered,
water has a marked effect on slowing or thermalizing neutrons. This is
particularly true in the thermal range.
The quantity of hydrogen in the soil ranges from near zero for dry coarse
sand to as much as 8 % of the mass of a fine-textured soil with 50%
water content when structural water (see footnote 1) is included in the
computation. Most of the hydrogen in soil is associated with water, and
lesser amounts with organic matter.
As fast neutrons lose energy and become thermalized, another nuclear-
matter interaction becomes increasingly important-neutron capture with
the release of other nuclear particles or energy. Of the elements usually
present in soil in quantities of 1 % or greater, the capture cross section for
thermal neutrons is greatest for iron (2.53 barns) and potassium (2.07
barns). The other most common elements in the soil, silicon, aluminum,
hydrogen, carbon and oxygen, have capture cross sections of 0.16, 0.23,
0.33, 0.003, 0.0002 barns. Several elements present in soil in small, or
even minute, quantities such as cadmium with an absorption cross section
of 2,450 barns, boron with 755 barns, lithium with 71 barns, or chlorine
with 34 barns, can have an appreciable effect on neutron capture.
10 Neutrons interact with matter in two general ways: namely, by elastic and inelastic
7-3.3.2 METHOD
7-3.3.2.1 Special Apparatus.
1. Small fast-neutron source such as radium- or americium-beryllium:
Such sources are good indefinitely because of their long half-lives.
2. ShIeld for storage of the neutron source between readings and when
the unit is not in use: The shield may also serve as a standard absorber
for checking the equipment or for providing the standard count when
data are computed on a count to count-in-standard ratio basis. The
shield must protect the user against both neutrons and gamma rays-
particularly with use of a Ra-Be source, which has a relatively high
gamma emission. Shielding commonly used consists of lead and paraffin
or polyethylene in a cylindrical shaped unit with a cylindrical hole
through the axis to accommodate the probe. A lead sphere (with
cylindrical hole) approximately 13 cm. in diameter immediately sur-
rounds the probe at the location of the neutron source, and the balance
of the cylinder is filled with paraffin or polyethylene. The outer diameter
is approximately 30 cm. The unit is made so that it can be set over the
7-3 INDIRECT METHODS 109
soil access hole and the probe lowered through the bottom of the shield
into the hole. The soil between the source and the operator provides
adequate protection when the probe is in use.
3. Detector of slow neutrons: There are several types, but the one used
most commonly for water-content measurement is a BFa-enriched
proportional counter mounted in a cylindrical arrangement with a
transistorized preamplifier mounted in the cable end. The neutron
source is mounted in a lead shield at the bottom of the gas-filled detec-
tor tube in some probes, and in others in a lead shield on the side of the
case at the center of the sensitive volume of the gas-filled detector. l l In
the second type the diameter of the probe is sufficiently greater than
the diameter of the gas-filled detector to accommodate the source and
lead shielding. This detector, when operated properly, is insensitive to
fast neutrons and to gamma radiation given off by the source. The de-
tector is filled with BFa gas, ordinarily at a pressure of about 20 cm. of
Hg, and a high positive voltage is imposed on a wire running axially
through the tube center. When a thermalized neutron encounters a BlU
nucleus and is absorbed, an alpha particle (the helium nucleus) is
emitted. The alpha particle moves to the charged wire, creating an
electrical pulse. This minute pulse is amplified by a preamplifier con-
tained in the probe and picked up by a conventional scaler, and the
number of events over a measured time interval is counted. Alternatively
the pulse can be picked up on a count-rate meter. A BIO atom is lost
each time a neutron is absorbed, but the number of BIO atoms in the
detector tube is sufficiently large that the detector will last for many
years.
4. Portable scaler or rate meter: A number of suitable scalers or scaler-
rate meter combinations are available from commercial suppliers such
as Troxler Laboratories or Nuclear-Chicago. A scaler should have at
least 5 decades for about lOG counts and an accurate timer. Counting
times of Yz, 1, and 2 minutes are desirable. These units are operated by
11 Troxler Laboratories (P.O. Box 5997, Raleigh, North Carolina 27607) supplies
probes of the first type in two different probe diameters, 1.865 and 1.5 inches, and
using either a 3-mc. radium-beryllium or a lOO-mc. americium-beryllium fast-neutron
source located on the radial axis at the bottom of the detector tube. These probes are
designed and calibrated for use in a 1.9 or 1.555 inch i.d. aluminum irrigation tubing.
They may be calibrated for other types of tubing. Nuclear-Chicago (333 East
Howard Avenue, Des Plaines, III. 60018) supplies probes of the second type with either
an americium-beryllium or radium-beryllium neutron source at the approximate
center, lengthwise, of a 1-inch detector tube contained in a 1.5-inch cylindrical hous-
ing. This probe is designed for use in 1.555 inch i.d. aluminum or steel tubing. Use
of americium permits high neutron flux with low gamma flux, thus simplifying the
shielding problem.
Surface probes are commercially available from both Troxler and Nuclear-Chicago.
By use of a special kit, the Troxler depth probe may be converted to a surface probe.
Both companies supply several different models, some of which are combination mois-
ture and density units.
1 10 WATER CONTENT
is of different size or material from that in which the probe was calibrated.
For maximum reproducibility of water content measurements, the probe
should fit the access tubing as closely as practical.
The field calibration check may be used for detecting large differences
in calibration due to unusual soil cQnditions. However, field calibration
should not be relied upon for precision work because of the inaccuracies
associated with the determination of the volume-basis water content values
required. These inaccuracies arise from errors in measurement of both the
mass-basis water content (see section 7-2.2) and the bulk density. Field
variation in both water content and bulk density, which can occur over a
relatively short distance, particularly in a heterogeneous soil, introduces an
additional confounding factor. For these reasons, unless the calibration
curve is considerably in error, water content inferences from the neutron
measurements may well be better than those obtained by direct sampling.
Accurate calibration curves require the usc of large homogeneous bodies
of soil with carefully regulated water content. Some useful checking can
be done with substitute neutron absorbers (such as CdCl 2 -water solutions)
in smaller containers. However, techniques are sufficiently complicated
that persons attempting calibration should consult original literature sources
such as Van Bavel et al. (1961), Holmes (1956), and Holmes and Jenkin-
son (1959).
Although the resolution of neutron water content measurements is low,
the precision of measurement for large samples is good. There arc three
sources of error associated with such measurements: (1) random variation
in count rate due to random variation in fast-ncutron cmission from the
source, (2) errors associated with the counting equipment, including the
timer, and (3) errors as~ociated with the calibration curve. If the calibra-
tion curve has been prepared with care using long counting times, then the
third error primarily involves differences between field conditions and cali-
bration conditions, and the accuracy of the water content determination
used in the calibration (sec section 7-2.2). Differences in soil composition,
soil bulk density, and geometry of the calibration arrangement can all influ-
ence the reliability of the calibration curve.
With equipment available commercially at the present time, instrumenta-
tion errors usually may be reduced to a small value, particularly when data
are handled on a count-ratio basis. The size of the error depends upon
characteristics of particular equipment. However, it is common practice to
multiply the standard deviation due to random emission by a factor of 1.5
to 2 to account for instrument error. For 10,000 counts per minute the
standard deviation for scattering and absorption would be 100 counts per
minute. For common equipment, deviation of the order of 200 counts per
minute should be expected. Calibration-curve errors must be considered
subjectively since they can be large or small, depending upon care taken in
the calibration process and the degree to which field conditions are com-
7-3 INDIRECT METHODS 1 13
[31]
If the limit of precision due to random emission errors only is taken as 30"0e
as was done for equation [19] earlier, then the water content error due to
random counting errors only is
£e=1
, - &, --.
SN./,{!
[32]
increasing the count rate through increasing the source strength. A useful
statistical guide for choosing an appropriate counting time has been pub-
lished by Merriam (1962).
The size of random counting error to be tolerated should depend upon
the size of the error anticipated due to field variability. This can vary
widely. Stone et al. (1960) obtained coefficients of variation of 1.5% to
2.5 %, with an average difference in water content between gravimetric
and neutron values of <0.1 inch of water per 6-inch depth of soil, or in
volume percent, 1.67. These differences were believed to be due more to
limitations of bulk density determination than to the neutron water-content
determination. At 40% water content, standard deviations corresponding
to 1.5% and 2.5% coefficients of variation would be 0.6% and 1.0%
water content, or in terms of Eo (99.7% certainty), 1.8% and 3.0%. Van
Bavel (1962b) suggested that experience indicates a standard deviation
of 0.01 volume fraction (8 as used here) in the calibration relation found
experimentally compared to the true relation between count rate and
water content. This would correspond to an Eo value of 0.03 or 3 % water
content. On this basis he concluded that a Ra-Be neutron source strength
between 1 and 2 me. is more nearly compatible with the precision of the
normal calibration than is the usual 2 to 5 me. source, and that lower cost
and the reduced health hazard would be advantageous for general applica-
tions of the neutron method.
One additional factor relating to use of the neutron method for field
water-content measurement should be considered. The presence of a metal
tube in the soil can have an effect upon soil temperature because of the
greater heat conductivity of metal compared to soil. Average temperature
differences between soil adjacent to an aluminum access tube and the sur-
rounding soil within the surface 2 feet did not exceed 3 of. during August
and May, and the largest average temperature gradient was 0.7°F. per inch
in work reported by Hanks and Bowers (1960). This work was done in a
silty clay loam, and no measurable influence on water content in soil sur-
rounding the access tube was observed. Unless temperature conditions of
extraordinary nature are encountered, the influence of the access tube on
water content due to temperature gradients probably is minor.
7-3.4. J PRINCIPLES
ington State University where fast and thermal neutron fluxes available at heam
ports are 4 X 10 1" and 1.2 X 10 1" neutrons per em." per second (Stewart, G. L., 1962.
Water content measurement by neutron attenuation and applications to unsaturated
flow of water in soil. Unpublished Ph.D. Thesis, Washington State University).
7-3 INDIRECT METHODS 117
at constant bulk density in the laboratory which is unequaled except for the
neutron method. The gamma ray method has been successfully used to
follow rapid water content change in soil columns undergoing wetting
(Gurr and MarshaIJ, 1960; Ferguson and Gardner, 1962; Gurr, 1962;
Rawlins and Gardner, 1963) and to monitor water content change in the
root zone of growing plants (Ashton, 1956; Hsieh14).
7-3.4.2 METHOD
7-3.4.2.1 Special Apparatus.
1. Source of gamma radiation: Cs 137, which emits gamma rays at 0.661
Mev. and has a half-life of 30 years, is well suited for water-content
measurements. The size of the source required depends upon the use
to be made of the equipment. Sources of 20 or 25 mc. have been satis-
factorily used. However, where rapidly changing water content is to be
followed, so that counting times of only a few seconds are required,
or where resolution of the order of a millimeter or less is required,
much larger sources are desirable. Sources from 100 to 500 mc. have
proved satisfactory under these more stringent conditions. Lead shield-
ing required for safe operation, of course, increases with increasing
source size.
2. Lead shield and collimator: The source is housed in a lead shield with
a suitable collimating hole or slit. With a protective plug for the collimat-
ing slit, the shield serves also as a storage container. Ideally the collimat-
ing hole should be drilled appropriately to serve for gross measurements
and to accept lead plugs with smaller collimating holes or slits for
measurements where greater resolution is desired. A hole about 3 cm.
in diameter will accommodate a collimating plug containing a 1- by
20-mm. slit or any number of other slits or holes that might be desired.
The collimating plug should have the form of a bolt with a large head
to cover the space between the bolt and lead block and should be 5 to
10 cm.long.
The dimensions of the block depend upon the source strength; but,
for greatest convenience where weight is not an important factor, the
block should be thick enough to reduce radiation in its vicinity to values
only slightly above natural background so that special precautions re-
quired in the vicinity of such radiation hazards may be minimized.
Normal background varies from 0.01 to 0.03 mR. (millirontgen) per
hour. One millirontgen in air is about 5% less than 1 mrad. (the rad. is
the unit of physical radiation dose) in tissu~ so that for practical con-
siderations they may be regarded as equivalent.
In the design of shielding and collimators, it is necessary to determine
14 Hsieh, J. J. C. 1962. A technique for controlling soil water content in the vicinity
of root hairs and its application to soil-water-plant studies. Unpublished Ph.D. Thesis,
Washington State University, Pullman.
118 WATER CONTENT
the dose rate in terms of source strength, shielding thickness, and dis-
tance from the source. This may be determined by the following formula.
The dose rate in mrad. per hour at a distance R in cm. from a point-
source of gamma radiation at strength A in mc. and energy Eo in Mev.
and with shielding of thickness t in cm. of a material with a linear atten-
uation coefficient po in cm.- I is (as inferred from equations [2], [3] and
[4] of Blizard (1958)
where B(p.,t) is the build-up factor, P-a/P in cm. 2 per g. is the energy-
absorption mass-attenuation coefficient for the source energy and the
material in which the dose is to be calculated (p is the density) and
where the numerical constant has units of (g. X rad./Mev. X mc.
X hr.).15 For 0.661 Mev. gamma radiation from a CSI37 source, POa/p,
measured in tissue, is about 0.0323 cm. 2 per g. (Evans, 1968). For
0.661 Mev. gamma radiation po is 0.717 cm.- I , and the build-up factor
B(p.,t) for lead thicknesses from 2 to 15 cm. is approximated by 1.4 +
0.21t (a dimensionless factor) so that equation [42] (inferred from
data in Tables 1 and 4, Blizard, 1958, and Evans, 1968) is:
A
D(R,t) = (5.1 + 0.76t)l()3 R2 exp (-0.717t) mrad./hr. [43J
For a 100-mc. CS I37 source with 11.6 cm. of lead shielding, the radia-
tion at the surface of the lead is about 2.5 mrad. per hour, and at 1 m.
from the surface it is about 0.03 mrad. per hour or the equivalent of
background radiation.
On the average, the A.E.C. dosage limitations are 100 mrem. per
week or 5 rem. per year (the rem. is the "radiation equivalent, man")
for persons 18 years of age or older. For gamma radiation, 1 rem. is
the equivalent of 1 rad., so that 0.03 to 2.5 mrad. per hr. is well within
A.E.C. regulations. 16
3. Gamma-sensitive probe: Scintillation-type gamma-sensitive probes are
the most satisfactory. A 2-inch phototube probe containing a preampli-
fier and equipped with a I-inch thallium..activated sodium iodide crystal
is adequate for many measurements. However, the crystal size may
be increased for greater sensitivity. A second lead collimator about
5 cm. long and containing a thin slit or hole is aligned with the source
collimator and with an intervening space large enough to accommodate
the soil container. The scintillation crystal, with a surrounding lead
lJI For gamma sources with more than one peak in an energy range which would
contribute significantly to the dose rate, equation [42] must be applied to each peak
and the dose rates summed.
,. For a more complete description of A.E.C. regulations see Part 20-Standards
for Protection Against Radiation (Chapter I, Title 10, Code of Federal regulations).
7-3 INDIRECT METHODS 119
17 Preset count also may be convenient where constancy of the standard deviation
due to random emission is more important than constancy of the observation time.
Print-out capability also has considerable utility.
18 The mass absorption coefficients for water at 0.5, 0.6 and 0.8 Mev. are given as
where p is the old density corresponding to the old N d, and No is the count
for the empty soil container. The error in water content inferences is signifi-
cantly reduced if errors in Nd and No are negligible. Since Nd and No are
counted infrequently compared to N rn , it is usually possible to count for a
much longer time, reducing the count to the equivalent counting time as
used to obtain N m. If the counting times for N a and No are 5 to 10 times
that for N m , the error in water content will be affected < 10%.
Dead-times of the counting equipment of the order of 1 to 10 p'sec per
count are common with typical equipment. For 106 , 5 X 105 , 3 X 105 ,
2 X 105 and 1 X 105 counts per minute using CS137 in 15 cm. of dry soil
and for a water content of 0.30 g. per cm. 3 , the error being largest in wet
soil, water content measurements will be too low by approximately 4.1 X
IOSd t , 2.1 X 103 d t , 1.2 X 10 3d t , 0.82 X 10 3d t , and 0.42 X 103d t g./cm. 3 ,
where d t is the dead-time in seconds. 19
The precision of the method varies with the thickness and density of
the soil column, the adsorption characteristics of the soil, and the size of
counts N m and N a. To involve the counting time explicitly, the gamma ray
intensity I as counts per unit time is introduced, so that Imt = N", and
lat = N d , where t is the counting interval. Equation [37] becomes
() = In (Imt/M) [50]
-P.w S
and the variance, with reasonable assumptions, becomes
[51]
'" During a short time interval as a pulse builds up, referred to as "dead-time," a
counter is insensitive to additional pulses. Correcting for dead-time involves multiply-
ing the dead-time per count by the number of counts to obtain total dead-time and
subtracting this from the measured counting interval.. 0r, a corrected count can be
obtained by multiplying the observed count by the.r'atio of the total counting time
to the total minus dead-time. Applied to the count ratio used in equation [37] where
the additional subscript "0" is used to denote "observed," I, to denote the counting
interval and d, the dead-time per count, the corrected ratio becomes
Nm = Nmo I, - Ndod,.
[49J
Nd Ndo t, - Nmod,
122 WATER CONTENT
To reduce the error, the counting time for Idt, which is measured infre-
quently and usually under conditions where time is not pressing, is in-
creased by a factor of 3 or 4 over that for Imt. However, the computation
requires that t be the same for both Imt and Idt, and so the longer count Idt'
is reduced to comparable size through division by n where n = t' /t. Thus
I dt' /n is the time-equivalent count to I dt and may replace it in equations
[51] and [52].
The standard deviation ofln(/mt/ldt'/n) is
Idt' /n Idt' /n 1 I 2 Umt)2 2
Uln (Im/IId/'ln) = Im t U(ImtI1.t'ln) = Im t Idt'/n '\jU1m/ + Ud t'/n)2 U(ldt'ln) • [53J
U6= 1
JJ.wSV Imt '\j
'1+lmt=
Idt'
1
JJ.wSV Im t '\j
'I+ nldt
lmt • [54J
Where n is 3 or 4, the second term under the radical may be neglected with
only small effect on U8 (ca. 10% ) so that equation [54] becomes
1 1
[55J
U6 = JJ. wS V l mt = JJ.wSVNm
or, substituting N m from equation [38],
U6 = exp [S/2C!J..p. JJ.w8) + + S'JJ.cPcJ . [56J
JJ.wSVNo
The optimum value of soil column thickness S may be obtained by equating
duu/dS, obtained by differentiation of equation [56], to zero; thus
dU6 = exp [S/2(JJ.8P. + JJ. w8)J exp (S'JJ.cPc) [1/2'-. + 8) _ (I/S)J = 0 [57J
ds v
JJ.wS No \J.'SP' JJ.w
and
S = 2/C!J..p. + JJ. w8) . [58]
= =
For 1'-8 0.07785 and P-w 0.08559 as determined by Gurr (1962), us-
ing a 25-mc. CS137 source emitting 0.661 Mev. gamma rays, and with the
discriminator set at 0.55 Mev. and for a bulk density of 1.3 g. per cm. 3 ,
the optimum sample thickness ranged from 19 cm. at low water content to
14 cm. at high water content.
The basic gamma count rate 10 with only air between the source and
scintillation crystal, and hence the precision and resolution possible in
water content measurement, depends upon the strength of the gamma
source, the range of gamma energies counted, the geometry of the equip-
ment, and the efficiency with which gamma radiation is measured. The
7-3 INDIRECT METHODS 123
source emits gamma rays in all directions, with the intensity of the gamma
field decreasing with the square of the distance from the source (neglecting
the absorption of air in the path and assuming a point source). 20 Under
these conditions, the fraction of the radiation reaching the face of the scintil-
lation crystal depends upon the degree of collimation and the distance from
the source. With an absorber in the beam, some scattered and secondary
radiation reaches the crystal so that the inverse square law no longer holds.
However, if a discriminator is used, so that only gamma rays of the maxi-
mum energy which are emitted from the source are counted, the effect of
scattered and secondary radiation is eliminated.
In practice if a discriminator is not used, primary, secondary, and
scattered radiation is counted, and the equations describing the attenuation
do not hold if used with absorption coefficients which have been determined
for particular energy values. However, equation [50], with /Lw determined
empirically, does hold reasonably well over the range of water contents of
interest, plotting as a straight line in 8 and In (lmt/ I at), or log (Irut/1at) .
The chief value to counting only particular gamma energies through use
of a discriminator circuit in the counter lies in the improvement of resolu-
tion. Scattered and secondary radiation can come from regions outside the
narrow collimated beam path, hence decreasing the resolution. For this
reason some discrimination is desirable. However, it must be recognized
that excessive discrimination can reduce the count rate to a point where
precision, as affected by random source emission, is severely reduced.
Gurr (1962), with a 25-mc. CS137 source, successfully used a discriminator
set to count energies from 0.50 to 0.66 Mev. It is obvious that with larger
sources discrimination is practical.
With discrimination such that an approximately monoenergetic gamma
beam may be assumed, the resolution possible for given precision, source
strength and experimental arrangement can be computed. If the area of the
collimator at the face of the crystal is a (assuming this to be the minimum
collimator restriction), and the distance from the crystal face is r, then the
fraction of the total radiation reaching the crystal, neglecting the absorption
of air in the path, is a/ (411"r2). The count rate lois proportional to the
product of this fraction and the strength of the source Z; thus,
[59]
where the proportionality factor k absorbs all other factors relating to the
intensity of the gamma beam as it reaches the crystal face and is absorbed
and counted, and to characteristics of the electronic circuits involved in
counting. If the source strength is too higij, so that simultaneous pulses
occur (coincidence losses), this effect too is absorbed in the k. The range
of gamma energies counted is an important component of this constant.
Several other factors are involved, the most important being the efficiency
of the scintillation crystal, which is related to its size, particularly its depth
in this case, since the collimated beam can be made small enough to fit
on the face of most crystals which are used. The size of a scintillation crystal
is generally given as the diameter of the face. However, the thickness is
usually about equal to the diameter. If the source strength Z is in mc.,
the distance from the source to scintillation crystal face r in cm., the
collimator area at the face of the crystal a in cm. 2 and lois in counts per
minute, the units of k will be counts per min. per mc. A value of k, de-
termined experimentally for a 1.75-cm. diameter, 2.5-cm.-thick thallium-
activated sodium iodide crystal with the discriminator set to accept pu)<:es
only above 0.55 Mev., is 3.62 X 108 (inferred from data of Gurr, 1962).
In this laboratory a value of 7.98 x 108 for k was determined for a Har-
shaw21 2-inch diameter, 2-inch thick thallium-activated sodium iodide
crystal operating with the discriminator set to accept only pulses above
0.53 Mev. and with R.I.D.L. equipment. 22
Replacing the count No in equation [56] by its equivalent lot, substituting
this into equation [59] and solving explicitly for the source strength, leads
to
Z = 41l"r2 exp [S(1L8PS + ILwO) + 2S' ILcPcJ • [60J
ka IL;S20"~ t
At high water content, say 40% (8 = 0.4) where the error is largest, for
soil at 1.3 g. per cm. 3 bulk density, held in a plastic container with 0.62-cm.-
thick walls, 1.19 g. per cm.s density, and an absorption coefficient of
0.08747 cm. 2 per g. and with absorption coefficients for soil and water of
0.07785 and 0.08559 cm. 2 per g. as used by Gurr (1962), equation [60]
can be reduced to
Z = 1.95 X 103 r 2 exp(O.l356S) . [61]
kaS2O"~t
For a typical situation where r is 36 cm., Sis 16 cm., a is 0.4 cm. 2, and k
is taken to be 7.98 X 108 , and where counting is done for 1 min. with a
desired precision of ±0.5% water content (30"0 = 0.005) due only to
errors associated with random emission, the required source strength Z is
94 mc. Counting for 5 minutes would reduce the required source strength
to 19 mc., or leaving the source strength at 94 mc. and counting for 5
minutes would bring the precision to approximately ±0.2 % water content
(30"0improved = 30"0/(t)l/2 = 0.0022).
'" Model 10-17 scintillation preamplifier, Model 40-B high-voltage power supply,
Model 30-19 linear amplifier and discriminator and a Model 35-7 linear/log count
rate meter, Radiation Instrument Development Lab., Div. of Nuclear-Chicago, 4501
West North Ave., Melrose Park, Ill.
7-4 LITERATURE 1 25
often is more useful than equations [55] or [56] for approximating the size
of the standard deviation in water content due to the random emission of
a CS137 source used under typical conditions. For the geometry and source
strength used by Gurr (1962) and a k-value inferred from his data,
the standard deviation computed is 0.0011 g. per cm. 3 (0.0011/1.444 =
0.00076 g. per g.), which is comparable to the value, 0.0007 g. per g.,
which he gives as the expected error due to the counting process.
If long counting times are practicable in an experiment, high precision
is possible with relatively small sources and at high resolution. However,
if rapid measurement is important, then either the resolution must be low
or the source strength high. In such cases, since k increases with increasing
crystal size, large scintillation crystals are desirable. If resolution and count-
ing time are not important factors, as in an experiment involving measure-
ment of gross water content in a container of soil with growing plants,
source strengths of the order of 20 mc. are usually adequate. Also, small
crystals are considerably less expensive than large ones, and crystals of the
order of 1 inch or less may often be adequate under such conditions.