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ῐ῎῍ῑῒ῏
No. 30, p. -ῌ+* ῍,**.῎

E#ects of Structural Fe Oxidation State on Physical-chemical
Properties of Smectites : Evidence from Infrared Spectroscopy
Dongfang HUO*, Claire-Isabelle FIALIPS*, Laibin YAN* and Joseph W. STUCKI** University of Illinois, College of Agricultural, Consumer, and Environmental Sciences,
W--,+ Turner Hall, ++*, South Goodwin Avenue, Urbana, IL 0+2*+ USA
Abstract
Redox reactions involving structural Fe in smectite clay minerals contribute signiﬁcantly tothe chemistry of soils and sediments. Changes in oxidation state from Fe (III) to Fe (II) alters theclay structure, which in turn modiﬁes the chemical nature of the smectite basal surfaces. Thesechanges in structure are readily observed by infrared spectroscopy. Structural OH groups areprogressively lost as the level of Fe (II) increases, and large shifts occur in the Si-O stretching andbending modes of the tetrahedral sheet. The communication between octahedral and tetrahedral
sheets alters the conﬁguration of basal oxygens, as well as changing the charge, pH, and reduction
potential of the surface. Infrared spectra also provide evidence for the formation of trioctahedral
domains as a result of extensive Fe (III) reduction.
Key words : pH, redox, charge, iron, clay.

+.

Introduction

The physical-chemical properties of smectites have great importance in agriculture, industry, and the environment because of theirhigh speciﬁc surface area and reactivity withplant nutrients, water, pesticides, organic pollutants, and other minerals. The smectite clay
minerals are largely responsible for properties
governing soil structure, porosity, and permeability. Every smectite contains some iron (Fe)in the octahedral sheet of its crystal structure(usually in the -ῌ valence state), and somesmectites also contain Fe (III) in the tetrahedral
sheet. Octahedral Fe (III) is susceptible to reduction and reoxidation (redox) processes,
which are common in nature due to bacterial
activity and are often associated with wetting
and drying events. The redox state of the clay
can also be readily manipulated in the laboratory using chemical reductants such as sodium
dithionite.
Redox reactions are signiﬁcant becausechanges in the oxidation state of the Fe areaccompanied by changes in the chemical properties and physical behavior of the clay.
A#ected properties and behaviors include
layer charge, cation exchange capacity, cation
ﬁxation (Stucki et al., +32. b ; Stucki and Roth,+311 ; Lear and Stucki, +32/ ; Gates et al., +33- ;Kostka et al., +333), swelling (Kostka et al., +333 ;Gates et al., +33- ; Stucki et al., +32. a), surface
area (Lear and Stucki, +323 ; Kostka et al., +333),
hydraulic conductivity (Shen et al., +33,), magnetization (Lear and Stucki, +321), surface pH(Cervini-Silva et al., ,*** b), capacity to degrade
organic compounds (Tor et al., ,*** ; Xu et al.,,**+ ; Cervini-Silva et al., ,*** a ; Yan and Bailey, ,**+ ; Hofstetter et al., ,**-), and reactivity
with redox-sensitive ions in solution (Taylor etal., ,*** ; Gan et al., +330 ; Ernstsen et al., +332).
The mechanism(s) by which a change in thevalence state of Fe controls these properties is
not well deﬁned, but certain ancillary changes
in structure during redox events and redox
cycles reveal certain clues from which hypotheses can be formulated. Structural changes
have been characterized by X-ray powder῏

4

di#raction (XRD) (Manceau et al., ,***),
Mössbauer spectroscopy (Lear and Stucki,+321), infrared spectroscopy (FTIR) (Stucki andRoth, +310 ; Fialips et al., ,**, a, b), uv-visible
spectroscopy (UV-VIS) (Anderson and Stucki,+313 ; Komadel et al., +33*), high-resolution
electron microscopy (HRTEM) (Stucki andTessier, +33+ ; Gates et al., +332 ; Kim et al., ,**-),
polarized extended X-ray absorption ﬁne structure spectroscopy (P-EXAFS) (Manceau et al.,,***), and X-ray absorption near-edge spectroscopy (XANES) (Manceau et al., ,***). Presented
here is evidence obtained primarily from FTIR
spectroscopy regarding changes in clay structure due to redox transformations.
,.

Materials and Methods

The smectites studied included Garﬁeld nontronite (sample API ---a from Wards Natural
Science Establishment, Rochester, New York,
USA) and ferruginous smectite (sample SWa-+
from the Source Clays Repository of The Clay
Minerals Society, USA). Structural Fe was
reduced either chemically using the methods
described by Stucki et al. (+32. c) or bacteriallyusing the method described by Kostka et al.
(+330). Structural Fe (II) and total Fe were determined quantitatively by the +,+*-phenanthroline method (Komadel and Stucki, +322)
and semi-quantitatively by Mössbauer spectroscopy.
Infrared spectra were obtained from driedﬁlms or from powders mixed with KBr using a
Midac Model ,*** FTIR spectrometer, andMössbauer spectra were obtained with a constant acceleration spectrometer operating witha triangle wave form over /+, data channels
using a /1Co (+*ῌ in Rh matrix) as the (-ray)source. Mössbauer spectra were deconvoluted
using a least-squares ﬁtting procedure, usuallyconstraining the component peaks to be ofLorentzian line shape.
All sample preparations, manipulations, andanalyses were performed using inert-atmosphere techniques. These included a controlledatmosphere liquid exchanger for replacing

30

,**.

and/or removing entrained salt solutions in
reduced suspensions, septum-sealed screw caps
on reaction vessels, and a glove box in which
the clay was dried either as a ﬁlm on a ﬁlter
membrane or as a freeze-dried powder.
-.

Results

The FTIR spectrum of smectite from .** to.,*** cm+ encompasses four principal spectral
regions in which signiﬁcant changes occur
during redox reactions. These regions are :Region I. -,.** to -,0** cm+, associated with
the O-H stretching vibrations of structural hydroxyls and adsorbed water ; Region II. +,***
to +,+/* cm+, associated with the Si-O vibrations ; Region III. 1/* to 3/* cm+, associatedwith the M-O-H bending modes (MFe, Al, orMg) ; and, Region IV. .**ῌ1** cm+, associatedwith various other modes involving Fe and Si.
Structural changes due to the reduction of octahedral Fe are readily monitored by changes
in all four of these regions of the spectrum.
Region I
The O-H stretching band in oxidized Fe (III)-rich, dioctahedral smectite is found at -,/1*
cm+ (Fig. +), characteristic of an [Fe (III)], OH
environment, and systematically shifts tolower wavelength to about -,/-/ cm+ as Fe (III)ions all become completely reduced to Fe (II).
The O-H stretching band also diminishes inintensity and two other features increase ; one
being a very broad band centered at about-,.** cm+ and the other being a sharp, small
band at -,0,, cm+. The latter small band islikely due to a portion of the Fe migrating to
adjacent vacant sites within the octahedral
sheet to form some trioctahedral [Fe (II)]- OHarrangements (Manceau et al., ,***). The position of this band is similar to the O-H stretching band in biotite, a trioctahedral mica where
the Fe (II) is clearly coordinated to OH from all
three octahedral sites. The relative intensity ofthis band is expected to be low because thesymmetrical electric ﬁeld due to uniform distribution of Fe (II) causes the OH dipole moment
to be oriented normal to the plane of the clay῎῍ : E#ects of Structural Fe Oxidation State on Physical-chemical Properties of Smectites : Evidence from Infrared Spectroscopy

Fig. +

5

FTIR spectra of O-H stretching region (Region I, see text) of Garﬁeld nontronite reduced tovarious levels by citrate-bicarbonate bu#ered dithionite suspension.

layer. This leads to a small interaction with theelectric ﬁeld vector of the incident infrared
radiation impinging on the oriented clay ﬁlm(Barshad and Kishk, +302). If the dipole orientation is normal to the clay layer, the band intensity should be pleiochroic, i.e., it should dependon the orientation of the clay ﬁlm. Conﬁrmation that this is indeed the case is given in
Fig. ,.
The broad band centered at about -,.** cmῌ+is assigned to H, O in the smectite structure. At
least two scenarios can be considered to explain the formation of this H, O band, namely,that the hydration energy of reduced smectite
is greater than oxidized smectite or that structural OH groups are converted to structural H,
O groups during reduction. Attention is drawn
to the fact that all samples were submitted tothe same dehydration process involving desiccation in vacuum and over P, O/ (Huo, +331),
which was e#ective in removing all adsorbed
H, O from the oxidized sample, as evidenced by
the absence of any signiﬁcant absorbance inthe -,,**ῌ-,.** cmῌ+ region for that sample, but
not from the reduced sample (Fig. +). The H, O
molecules responsible for the large band at

Fig. ,FTIR spectra of a 3/ῌ reduced Garﬁeld
nontronite ﬁlm oriented at 0*ῌ and 3*ῌ
relative to the incident beam, showing
pleochroic behavior of this band.

-,.** cmῌ+ in the reduced samples could, therefore, be adsorbed to the basal surfaces of thesmectite, but held to the surface with greater
energy than in the oxidized samples. Other
evidence for this scenario is found in thestudies of Yan and Stucki (+333, ,***), who6

30,**.

Fig. .
Fig. -FTIR spectra of the Si-O vibrations(Region II) of oxidized and reduced
Garﬁeld nontronite.

observed an increase in the interaction between basal Si-O groups and adsorbed H, O as
the extent of Fe reduction increased, and of
Stucki et al. (,***) who concluded that the surface hydration energy of reduced smectite is
greater than oxidized smectite.
A second scenario to explain the -,.** cm+band is that the H, O molecules are actually
located inside the clay layer as protonated OH
groups. Drits and Manceau (,***) proposed a
reduction reaction mechanism by which electron transfer to structural Fe (III) from reducing agents in solution is accompanied by protonation of structural OH groups. While theyfurther suggested that these internal H, O molecules then di#use back into solution, perhaps,
in reality, at least some of them remain in theoctahedral sheet in order to stabilize it withrespect to increased charge due to structural
Fe (II).
Region II
Changes are also observed in the Si-O
stretching region (Fig. -), including a large (upto .- cm+) downward shift of the main Si-O
stretching band of the reduced samples (Stucki

FTIR spectra of the M-O-H bending
modes (Regions III and IV) of oxidized
and reduced Garﬁeld nontronite.

and Roth, +310 ; Fialips et al., ,**, a, b ; Yanand Stucki, +333, ,***). Such a large shift indicates that the change in Fe oxidation state in
the octahedral sheet strongly a#ects the structural properties of the tetrahedral sheet, whichis also reﬂected in the alternate clock-wise,
counter-clock-wise rotations of the Si tetrahedra as measured by an increase in the crystallographic b-dimension 3.+-  to 3.,+ (Manceau et al., ,***).
These changes in the tetrahedral sheet a#ect
physical and chemical properties at the miner
al surface, such as those that are conﬁgurationally dependent. A good example of thisis found in the results of Yan and Stucki (+333,,***) who linked these changes in Si-O vibrations to the coupling of H, O molecules with thebasal oxygen surfaces. Other examples arefound in the change in pH (Cervini-Silva et al.,,*** b) and reduction potential (Cervini-Silva etal., ,*** a).
Region III
In the M-O-H deformation region (Fig. .), theprimary band is due to Fe (III)-O-H at 2,+ cm+,which shifts downward by about / cm+ withincreasing Fe reduction, then disappears alto-῏῎ : E#ects of Structural Fe Oxidation State on Physical-chemical Properties of Smectites : Evidence from Infrared Spectroscopy

gether, along with all other features in thisRegion, with complete Fe reduction. A lesser
band at 2.- cm῍+, which appears as a shoulder
on the principal peak, is assigned to an Fe-OH
bending mode, where the OH is taken as asingle unit. This assignment was originallygiven by Stucki and Roth (+310), but has notbeen widely accepted. Nevertheless, no better
assignment has been found. These major modiﬁcations clearly indicate that changes occurred within the clay crystal far beyond
merely a change in Fe oxidation state. Partial
dehydroxylation and redistribution of Fe, andperhaps Al, cations occurred upon reduction,changing the structural properties of the tetrahedral and octahedral sheets.
The loss of structural O-H stretching andbending vibrations is direct evidence that the
OH groups are intimately involved in the reduction mechanism of the smectites. In nontronite, the ratio of Fe to OH in the clay structure is about + : +. If electron transfer is accompanied by protonation of the structural OH(Drits and Manceau, ,***), one would expect
complete reduction to eliminate all structuralO-H vibrational modes and replace them witheither H-O-H modes or nothing, depending on
the extent to which the newly formed H-O-H
di#uses out of the smectite structure. Thisappears in fact to be the case (Figs. + and .).
Region IV
The bands in Region IV (Fig. .) seem to havesome correlations with the bands in Region III,
but these relationships are only poorly established at this point. The attribution of the /23
cm῍+ band is uncertain but it may be due to a
combined Si-O-Fe (III) bending mode (Stubicanand Roy, +30+ a, b). Upon reduction, this band
completely disappears and a new band emerges at 0/- cm῍+. No apparent connection isobserved between this new band and any ofthe disappearing ones in Region III, but a band
located in the same region is generally observed for [Fe (II)]- OH deformation modes intalcs (Wilkins and Ito, +310). The band at 0/cm῍+ in the fully reduced sample could, there-7

fore, be due to [Fe (II)]- OH deformation, which
supports the hypothesis of trioctahedral domain formation upon reduction. The high intensity of this band, however, seems to be outof proportion to the possible number of trioctahedral groupings, so an additional contribution to this band may exist. A possible
candidate is the band located at 01, cm῍+ in theunaltered nontronite, which is attributed to
Fe-O out-of-plane vibrations (Farmer, +31.).
This band is expected to shift to lower wavenumber upon Fe (III) reduction, but no evidence of such a shift was observed (Fialips etal., ,**, b).
Perhaps it does not change
signiﬁcantly upon reduction and could still bepresent in the spectrum of the fully reduced
sample, in which case the 0/- cm῍+ band observed for this sample could be generated by
the overlap of one band at 01, cm῍+ and one
band due to [Fe (II)]- OH deformation at lower
wavenumber.
..

Conclusions

Infrared spectra reveal signiﬁcant di#erences in structural vibrational modes in Ferich smectites when structural Fe (III) is
reduced to Fe (II). These di#erences clearly
indicate that structural OH groups are being
eliminated as a part of the reduction process,either directly by dehydroxylation or by protonation. The latter appears to be the better
explanation. A portion of the protonated hydroxyl groups evidently remain in the smectite
structure after complete reduction. Those sites
from which structural OH groups are lost
evoke a migration of the structural Fe from theoriginal site to an adjacent vacant site, thereby
creating a trioctahedral domain and a defect inthe octahedral sheet. The relative number ofsuch domains has yet to be determined.
References
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C. Farmer (eds)., 1/ῌ2-.

8

Barshad, I. and Kishk, F.M. (+302) : Oxidation offerrous iron in biotite and vermiculite alters
ﬁxation and replaceability of potassium. Science, +0, : +.*+ῌ+.*,.
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 A renewable source of reduction capacity.
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ferruginous
smectite.
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W. (,**, b) : E#ect of iron oxidation state on
the IR spectra of Garﬁeld nontronite. American Mineralogist, 21 : 0-*ῌ0.+.
Gan, H., Bailey, G.W. and Yu, Y.S. (+330) : Morphology of Lead (II) and Chromium (III) reaction
products on phyllosilicate surfaces as determined by atomic force microscopy. Clays andClay Minerals, .. : 1-.ῌ1.-.
Gates, W.P., Jaunet, A.-M., Tessier, D., Cole, M.A.,
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reduced by bacteria. Clays and Clay Minerals,.0 : .21ῌ.31.
Gates, W.P., Wilkinson, H.T. and Stucki, J.W. (+33-) :Swelling properties of microbially reduced ferruginous smectite. Clays and Clay Minerals,.+ : -0*ῌ-0..
Hofstetter, T.B., Schwarzenbach, R.P. and Haderlein, S.B. (,**-) : Reactivity of Fe (II) species
associated with clay minerals. Environmental
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Huo, D. (+331) : Infrared Study of Oxidized andReduced Nontronite and Ca-K Competition in
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Kim, J., Furukawa, Y., Daulton, T.E., Lavoie, D. and

30

,**.

Newell, S.W. (,**-) : Characterization of micro
bially Fe (III) reduced nontronite : environmental cell-transmission electron microscopy
study. Clays and Clay Minerals, /+ : -2,ῌ-23.
Komadel, P., Lear, P.R. and Stucki, J.W. (+33*) :Reduction and reoxidation of nontronite :Extent of reduction and reaction rates. Claysand Clay Minerals, -2 : ,*-ῌ,*2.
Komadel, P. and Stucki, J.W. (+322) : Quantitative
assay of minerals for Fe, and Fe- using +,+*-phenanthroline : III. A rapid photochemical
method. Clays and Clay Minerals, -0 : -13ῌ-2+.
Kostka, J.E., Stucki, J.W., Nealson, K.H. and Wu, J.
(+330) : Reduction of structural Fe (III) in
smectite by a pure culture of the Fe-reducing
bacterium Shewanella putrefaciens strain MR+. Clays and Clay Minerals, .. : /,,ῌ/,3.
Kostka, J.E., Wu, J., Nealson, K.H. and Stucki, J.W.
(+333) : E#ects of microbial reduction on physical and chemical properties of clay minerals.
Geochimica Cosmochimica Acta, 0- : -1*/ῌ
-1+-.
Lear, P.R. and Stucki, J.W. (+32/) : The role of structural hydrogen in the reduction and reoxidation of iron in nontronite. Clays and Clay Minerals, -- : /-3ῌ/./.
Lear, P.R. and Stucki, J.W. (+321) : Intervalence
electron transfer and magnetic exchange in
reduced nontronite. Clays and Clay Minerals,-/ : -1-ῌ-12.
Lear, P.R. and Stucki, J.W. (+323) : E#ects of ironoxidation state on the speciﬁc surface area of
nontronite. Clays and Clay Minerals, -1 : /.1ῌ//,.
Manceau A, Lanson, B., Drits, V.A., Chateigner, D.,
Wu, J., Huo, D., Gates, W.P. and Stucki, J.W.
(,***) : Oxidation-reduction mechanism ofiron in dioctahedral smectites. ,. Structuralchemistry of reduced Garﬁeld nontronite.
American Mineralogist, 2/ : +/-ῌ+1,.
Shen, S., Stucki, J.W. and Boast, C.W. (+33,) :E#ects of structural iron reduction on the hydraulic conductivity of Na-smectite. Clays andClay Minerals, .* : -2+ῌ-20.
Stubican, V. and Roy, R. (+30+ a) : Infrared spectraof layer-structure silicates. Journal of theAmerican Ceramic Society, .. : 0,/ῌ0,1.
Stubican, V. and Roy, R. (+30+ b) : Isomorpous substitution and infrared spectra of the layer silicates. American Mineralogist, .0 : -,ῌ/+.
Stucki, J.W. and Roth, C.B. (+310) : Interpretation of
infrared spectra of oxidized and reduced nontronite. Clays and Clay Minerals, ,. : ,3-ῌ,30.
Stucki, J.W. and Roth, C.B. (+311) : Oxidation- : E#ects of Structural Fe Oxidation State on Physical-chemical Properties of Smectites : Evidence from Infrared Spectroscopy

reduction mechanism for structural iron in
nontronite. Soil Sci. Soc. Am. J., .+ : 2*2῎2+..
Stucki, J.W. and Tessier, D. (+33+) : E#ects of ironoxidation state on the texture and structuralorder of Na-nontronite gels. Clays and Clay
Minerals, -3 : +-1῎+.-.
Stucki, J.W., Low, P.F., Roth, C.B. and Golden, D.C.
(+32. a) : E#ects of oxidation state of octahedral iron on clay swelling. Clays and Clay Minerals, -, : -/1῎-0,.
Stucki, J.W., Golden, D.C. and Roth, C.B. (+32. b) :E#ects of reduction and reoxidation of structural Fe on the surface charge and dissolutionof dioctahedral smectites. Clays and Clay Minerals, -, : -/*῎-/0.
Stucki, J.W., Golden, D.C. and Roth, C.B. (+32. c) :Preparation and handling of dithionite-reduced
smectite suspensions. Clays and Clay Minerals,-, : +3+῎+31.
Stucki, J.W., Wu, J., Gan, H., Komadel, P. and Banin,A. (,***) : E#ects of Fe oxidation state andorganic cations on smectite hydration. Claysand Clay Minerals, .2 : ,3*῎,32.
Taylor, R.W., Shen, S., Bleam, W.F. and Tu, S.-I.
(,***) : Chromate removal by dithionite-reduced
clays : evidence from direct x-ray adsorption
near edge spectroscopy (XANES) of chromate

reduction at clay surfaces. Clays and Clay Minerals, .2 : 0.2῎0/..
Tor, J.M., Xu, C., Stucki, J.W., Wander, M.M. andSims, G.K. (,***) : Triﬂuralin degradation under
microbiologically induced nitrate and Fe (III)
reduced conditions. Environmental Scienceand Technology, -. : -+.2῎-+/,.
Wilkins, R.W.T. and Ito, J. (+310) : Infrared spectraof some synthetic talcs. American Mineralogist, /, : +0.3῎+00+.
Xu, J.C., Sims, G.K., Kostka, J.E., Wu, J. and Stucki,
J.W. (,**+) : Fate of atrazine and alachlor inredox treated ferruginous smectite. Environmental Toxicology and Chemistry, ,* : ,1+1῎,1,..
Yan, L. and Bailey, G.W. (,**+) : Soprtion and abiotic redox transformation of nitrobenzene at
the smectite-water interface. Journal of Colloid and Interface Science, ,.+ : +.,῎+/-.
Yan, L. and Stucki, J.W. (+333) : E#ects of structural Fe oxidation state and hydration on layer
Si-O stretching vibrations of montmorillonite.
Langmuir, +/ : .0.2῎.0/1.
Yan, L. and Stucki, J.W. (,***) : Structural perturbations in the solid-water interface of redox
transformed nontronite. Journal of Colloid andInterface Science, ,,/ : .,3῎.-3.

 Fe 

 :  ! "#$% *ῌ ῎ *ῌ
 *ῌW** ῌ !ῌ"#$%&'

&'()*+,- Fe ./0123456789:;<=*+>?.@ABCD1E FeF῍G HI Fe FῌG J+K>LM+N>6O7+,-PNQR STU6&'(+VW,-+>X?YPZYD1E ,-.9[1\]I+N>6R ^_`a.:bUcd.efD1\ghi@1E ,- OH j6 Fe FῌG k

9+lggm.nonogp0]R . Wqr(+ Si-O stguvwx.

@yr(Pz{1E 2 Wqr(g . Wqr(+|}6VWK~+HiyAR W+ R
pH 9:;K>23r PN>1E ^_`a( HIR Fe F῍G 23++R-῎Wq&]1\gh]1E()*)+ : pHR K>23R  R R O7
 : ,**.  +  /  : ,**.  +  +0 <=^º » 30 ¼ ,**.

10

STUCKI   :
 Fe  0/ῌ  Feῌ    !" #$ῌ% Fe ῌ &'( )*+,
Stucki :--#./012 Favri ,**, a, b 345
26%7, 83# 9::;<=>?@A6
2BC +/ῌ  Fe ῌ DEFG26%7, -*<=  Fe # 9:HIJ+1
KLMNOPQ2R%7, -STA
#UVWX3%7, Y
Z#-*<=+3E[ \<]^_`abc0d e-Ef6
g26%7 Xu et al. ,**+ ; Kostka et al. ,**, ;Cervini-Silva et al., ,**-,:Fe # FTIR hijPklmnopqr

References Cited
Cervini-Silva, J., J.E. Kostka, R.A. Larson, J.W.
Stucki and J. Wu. (,**-) : Dehydrochlorinationof +,+,+ tricholoroethane and pentachloroethane by microbially reduced ferruginous
smectite. Environmental Toxicology andChemistry. ,, : +*.0῍+*/*.
Favre, F., V. Ernstsen, D. Tessier and P. Boivin.
(,**, a) : Short scale changes in soil properties
due to structural iron reduction. Geochimica et
Cosmochimica Acta- Goldschmidt Conference
Abstracts. A,,0.
Favre, F., D. Tessier, M. Abdelmoula, J.M. Genin, W.
P. Gates and P. Boivin. (,**, b) : Iron reduction
and changes in cation exchange capacity inintermittently waterlogged soil. EuropeanA stpui Mössbauer  *%vwx y- , +03 z{# |}
~N2 Q?A ORP wxE*
7, ORP  Fe # U*0
e%7+,
Stucki :6V0vU*0%7, + #%gxQ26%, z{# m
 ORP  Qc Komadel and Stucki,+322 Ue6#tpuiU3+ Fe ῌ Dc0E7
456%7, % 660 ¡e¢£\<¢£c0¤¥E¦ U*7§JV
126%7, § Eh¨iA©+3ª«M ¬7­ |}E®¯-¯626v¯+ °±²
%7, -*³´# Fe ῌ Rµwxe¶ Rµ ORP wx62·  e
¸6%7,

Journal of Soil Science. /- : +1/῍+2-.
Komadel, P. and J.W. Stucki. (+322) : Quantitative
assay of minerals for Fe,¹ and Fe-¹ using +,+*
-phenanthroline : III. A rapid photochemical
method. Clays and Clay Minerals. -0 : -13῍-2+.
Kostka, J.E., D.D. Dalton, H. Skelton, S. Dollhophand J.W. Stucki. (,**,) : Growth of iron (III)reducing bacteria on clay minerals as the soleelectron acceptor and comparison of growthyields on a variety of oxidized iron forms.
Applied and Environmental Microbiology. 02 :0,/0῍0,0,.
Xu, J.C., G.K. Sims, J.E. Kostka, J. Wu and J.W.
Stucki. (,**+) : Fate of atrazine and alachlor inredox treated ferruginous smectite. Environmental Toxicology and Chemistry. ,* : ,1+1῍
,1,..





J. Jpn. Soc. Soil Phys.
3
No. 30, p. +++2 ,**.

ΐῐ῔ΐῌ῏ῒ῍῎ῑ   *Point of zero charge of soil clays
Katsutoshi SAKURAI** Faculty of Agriculture, Kochi University, B-,**, Monobe, Nankoku 12-῍2/*,, Japan+30, a, b ; Wada and Greenland, +31*0 CxS~   

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12

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al., +322
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13

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3  sD %&" Sposito, +32+

 pH +@ 456

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 Z./&45[PZNC  >?nb@' [ n kP`a 3 ./@J


^_Bezghi@J.T Sakurai
et al., +323 c R/A sB & C

 [ ./\]12^_ Cation Exchange Capacity, CEC  pH 1 `a + M b'

Y+ 0123

Ecd e2fghi () 0Dj kP@' `a
M

[

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Ej() ezghi@J+j) +5 kP`a(

123 [ ./ ( !CB"mc8  E.+ pH V012)/ T 45! j kP pH #l BI94:J-§¨©ª«+ /¬[$  ­8K®¯O p°±²5P³

j O$() j%&

CEC  kP



')/

(m

I ( +E kBF ¡+'¢Gῌ pH £ ¡  ¤¥ H¦V

9L¥´M

E£Nµ¶ ) Sakurai et al., +322 Rn CEC )o45o·6   ¸¹

Ipq+*r^_BstQ sumB"+º»OWXn !CB"  & C 30 ¼ ,**.

14
  

Oxisols  

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  (&*+,B

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

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 low activity clay  

 23 HI 0' *+,1(   CEC  +0 cmol ! g clay"+ #$ ῌ-./B ? JECEC  +, cmol ! g clay"+ #$%&'(Soil Survey Sta#, +33,) *+, -./0' &1.#$234567'8

#\*kl:K]2SLM+ 9: ; .2 *+,NO,.Vg  .2 LP+45 <= +32, a, b ; Sakurai et al., +322,

BFQ( 1  HL

+323 aa ;s F= F T Rῌmno, 9:> ? Sakurai et al., +323-

pqr : E

Al     

*+,.@ABCD

UVklW.27'kl8 F( . ^_* , : + R

Sakurai et al., +323 cL. ῌE !FG*+, Sakurai et al.,)*# Sakurai et al., +33+

Saha et al., ,**-

Hydroxyaluminosilicate-Mt !F+*,

PZC Y0'45Z%&

Sakurai and Huang, +33/, +330, +332 ; Taniguchi&

et al., +333, ,***, ,**+ ; Saha et al., ,**+, ,**,, ,**-

0'\45 +30* ]$.X/ , $I= +330 ; Y0ῌ$I+332 ; Y0= +332
et al., +330, +332 ; Ishizuka et al., ,*** ; Kadir et=[#$.f0']g F7E ,D
T=¡1Z%&'(' {]JK [145^¢%&']

5£45Zg

#$. ¤_¥¦

3 *+,1(23 - Sakurai

N, PZC    

0 JK%LM& *+, NEOP' (2 &Q R  @S*,T=UV-WNOg UVklW.

27'klX+33*/  H" *+,# $I +33*

1

S Iwasaki et al., +331 a,\= 0'TB

b

=&

`§. ¨©1aª

fB+  b)*,#c«¬+ Innersphere complex ­7.27'

al., ,**+

&=Z445.27' 5  ,

PZC x*,#B

T 0'*+,-[    /4L NO,\  PZC VgB 5#\* ]2S^_ῌ#\6*`7 a£. NEw®Ead90kl 3

*+,1(-b a-c8=& VNO,\  PZC gB 5£.¯

1 Z9 0'd ῌ ef0']g$I

1B+33* 2Z9h#

,  e7  ,f 0'°g ±²,

*+,if!FeῌAl : E !jCa"^_*"klmnopqr";s "<t=SiO,
ῌ e *+,VgB " f0'Uehara and Gillman, +32+



uuῌe

! gB

>6B.&' FeῌAl : E ?@ .Av0^_*wklmnopqrxByzB

07'  *+,dC.Vg pH 1 D{.E -³ /4e7.

#B

7'(

)*]2S PZC

$I +33*

- hb´ ij &kµRE .2 lm.27'  b &Q µ#B  hb´n0ijo¶nB

Rhoton et al., ,**-·,²p¸N¹]2S<tqrMQ-°µ ;sV s.2

Z5 j Ca w;s  (| F}~.] ##0 PZC wº»t#B (  ./PG( 

,***

)*

Schwarz et al.,º» :¼ kl. ῌ



15

S., Hirota, M., Priantna, S. J. and Juairiah (,**+) :Characteristics of Ultisols under di#erent wild- ῌῌ ﬁre history in South Sumatra, Indonesia : I.

 !"#$%&'()*+,-./0$1&

Physico-chemical properties. Tropics, +* : /0/῍'()*+,-.2345 6789:

/2*.

;<=>!=?

ῌ  +332 : Kn gBh;<=@ABC /D&.EFGH1.

klc! ¡¢£¤¥? Rashid et al., ,**,

/ IJKLMῌ§¨©ῌNOP QGRST/,UVA $1./W$1.XMYZC[PAB\Q]

 PZC Y

ZC Korah et al., ,**-^

¤¥

¦{

Kn 03 : .22῍.31.
 +332 :¡¢£ª >« { ¬­®¯%n ., :31῍+*0.
Korah, J., Spieker, W.A. and Regalbuto, J.R. (,**-) :_/`abP Q>cdCef.gBh

Why ion-doped, PZC-altered silica and alumina

GRSTij

fail to inﬂuence platinum adsorption. Catalysis!ef.]kl

mn oUGpURAB\Q PZC P pH 
qAMrQ sC Boisvert et al., ,***^Letters, 2/ : +,-῍+,1.

  ,**+ : ῌ῍. °±²
{  n °±

ῌ ῏ ῎ ῍P³´µ

Kn pp. +++῍+-*n ¶·K¸¹zn ¶{Boisvert, J-P., Persello, J., Foissy, A., Castaing, J-C.

Mattoson, S. (+3-,) : The laws of soil colloidal behav-

and Cabane, B. (,***) : E#ect of surface charge

ior, IX. Amphoteric reactions and isoelectricon the adsorption mode of sodium poly (acrylate)weathering. Soil Sci., -. : ,*3῍,.*.

on alumina-coated TiO, used as coating pigment.

Morisaki, H., Kasahara, Y. and Hattori, T. (+33-) : The

Colloids Surfaces. A : Physicochem. Eng. As-

cell surface charge of fast- and slow-growing

pects, +02 : ,21῍,30.

bacteria isolated from grassland soil. J. Gen.

tu ῌ vw

xyz

+320 :tuῌvw { p. 1,n |}n ~{ῌ pH *.  ῌ  +32, a : Appl. Microbiol., -3 : 0/῍1..
Rashid, Md. M., Kang, Y. and Sakurai, K. (,**,) :Kn /- : -*0῍-+,.

Selenium chemistry in amorphous iron (hydr)oxide-applied soil as inﬂuenced by redox poten-ῌ ῌ +32, b : Agtial (Eh) and pH. Soil Sci. Plant Nutr., .2 : ,0+῍,03.

Cῌ kl { Rhoton, F.E., Romkens, M. J.M., Bigham, J.M., Zobeck,Kn /- : -1/῍-13.
Ishizuka, S., Tanaka, S., Sakurai, K., Hirai, H.,
Hirotani, H., Ogino, K., Lee, H.S. and Kendawang,

T.M. and Upchurch, D.R. (,**-) : Ferrihydrite inﬂuence on inﬁltration, runo# and soil loss. Soil
Sci. Soc. Am. J., 01 : +,,*῍+,,0.

J. J. (+332) : Characterization and distribution of

Saha, U.K., Taniguchi, S. and Sakurai, K. (,**+) : Ad-soils at Lambir Hills National Park in Sarawak,

sorption behavior of cadmium, zinc and lead on

Malaysia, with special reference to soil hardness

Hydroxyaluminium - and Hydroxyaluminosili-

and soil texture. Tropics, 2 : -+῍...

cate - Montmorillonite omplexes. Soil Sci. Soc.

Ishizuka, S., Sakurai, K., Sabang, J., Kendawang, J. J.

Am. J., 0/ : 03.῍1*-.

and Lee, H.S. (,***) : Soil characteristics of an

Saha, U.K., Taniguchi, S. and Sakurai, K. (,**,) : Si-abandoned shifting cultivation land in Sarawak,

multaneous adsorption of cadmium, zinc andMalaysia. Tropics, +* : ,/+῍,0-.

lead from their mixed solutions on hydro-

Iwasaki, K., Tsuji, M. and Sakurai, K. (+331) : Frac-

xyaluminum- hydroxyaluminosilicate- montmo-

tionation of copper and manganese in agricultur-

rillonite complexes. Soil Sci. Soc. Am. J., 00 : ++1῍al soils near an abandoned copper mine. Soil Sci.
Plant Nutr., .-, +/1῍+03.
Kadir, S., Sakurai, K., Ishizuka, S., Tanaka, S., Kubota,+,2.
Saha, U.K., Iwasaki, K. and Sakurai K. (,**-) : Desorption behavior of cadmium, zinc and lead sorbed 789 : 30 ; ,**.

16

on hydroxyaluminum- and hydroxyaluminosilicate- montmorillonite. Clays and Clay Miner-

charge (ZPC). Soil Sci. Plant Nutr., ., : 3-ῌ+*-.

ῌῌ +330 : ZPC!"#$%&'()*+ ,-./0 12,

als, /+ (/) : .2+ῌ.3,.
Sakurai, K., Ohdate, Y. and Kyuma, K. (+322) : Com-3456 01 : -,ῌ-3.

parison of salt titration and potentiometric titra-

Sakurai, K. and Huang, P.M. (+330) : Inﬂuence of po-tion methods for the determination of zero pointtassium chloride on desorption of cadmiumof charge (ZPC). Soil Sci. Plant Nutr., -. : +1+ῌ+2,.

sorbed on hydroxyaluminosilicate- montmo-

Sakurai, K., Ohdate, Y. and Kyuma, K. (+323 a) :rillonite complex. Soil Sci. Plant Nutr., ., : .1/ῌPotentiometric automatic titration (PAT) method to evaluate zero point of charge (ZPC) of.2+.
Sakurai, K. and Huang, P.M. (+332) : Intercalation ofvariable charge soils. Soil Sci. Plant Nutr., -/ :hydroxy-aluminosilicate

23ῌ+**.

num in montmorillonite and resultant phy-

Sakurai, K., Ohdate, Y. and Kyuma, K. (+323 b) :Factors a#ecting zero point of charge (ZPC) of
variable charge soils. Soil Sci. Plant Nutr., -/ : ,+
ῌ-+.

and

hydroxy-alumi-

sicochemical properties. Soil Sci. Soc. Am. J., 0, :-0,ῌ-02.
Sakurai, K., Tanaka, T., Ishizuka, S. and Kanzaki, M.
(+332) : Di#erences in soil properties of dry ever-

Sakurai, K., Nakayama, A., Watanabe, T. and K.

green and dry deciduous forests in the Sakaerat

Kyuma (+323 c) : Inﬂuences of aluminum ions on

Environmental Research Station. Tropics, 2 : 0+ῌ

the determination of ZPC (zero point of charge)of variable charge soils. Soil Sci. Plant Nutr., -/ :2*.
Schwarz, S., Lunkwitz, K., Kessler, B., Spiegler, U.,
Killmann, E. and Jaeger, W. (,***) : Adsorption0,-ῌ0--.
Sakurai, K., Teshima, A. and Kyuma, K. (+33*) :Changes in zero point of charge (ZPC), speciﬁc
surface area (SSA), and cation exchange capacity

and stability of colloidal silica. Colloids and Surfaces A, +0- : +1ῌ,1.
Soil Survey Sta# (+33,) : Keys to Soil Taxonomy, /th(CEC) of kaolinite and montmorillonite andedition. SMSS technical monograph No. +3.

strongly weathered soils caused by Fe and Al

Blacksburg, Virginia : Pocahontas Press, Inc. p.

coatings. Soil Sci. Plant Nutr., -0 : 1-ῌ2,.

 +33* : 

 ZPC

 

 -. : ,ῌ+..
Sakurai, K., Nakamura, Y. and Kyuma, K. (+33+) ://0.
Sposito, G. (+32+) : The operational deﬁnition of thezero point of charge in soils. Soil Sci. Soc. Am. J.,./ : ,3,ῌ,31.

Changes in zero point of charge (ZPC), phosphate

Taniguchi, S., Hiradate, S. and Sakurai, K. (+333) :retention and speciﬁc surface area of some vari-Speciation of aluminum in hydroxyaluminum

able charge soils after several chemical treat-and hydroxyalumino- silicate ions ﬁxed by Mt,

ments. Soil Sci. Plant Nutr., -1 : .-/ῌ....

using ,1Al-NMR and ICP-AES. Clay Sci., +* : ..-ῌ

Sakurai, K. and Huang, P.M. (+33/) : Chapter .. Cad-.//.

mium adsorption on the hydroxyaluminum-

Taniguchi, S., Yamagata, N. and Sakurai, K. (,***) :montmorillonite complexes inﬂuenced by oxa-

Cadmium Adsorption on Hydroxyalumino-sili-late. In : P.M. Huang, J. Berthelin, J.M. Bollag, W.

cate - Montmorillonite Complex as Inﬂuenced by

B. McGill and A.L. Page (Eds.), Environmental

Oxalate and Citrate. Soil Sci. Plant Nutr., .0 : -+/ῌ

impacts of soil component interactions. Vol. +”Lewis Publishers, FL, USA, p. -1ῌ...
Sakurai, K., Kozasa, S., Puriyakorn, B., Preechapanya,-,..
Taniguchi, S., Hiradate, S. and Sakurai, K. (,**+) :Speciation of Hydroxyaluminosilicate and Hy-

P., Tanpibal, V., Muangnil, K. and Prachaiyo, B.

droxyaluminium ions as a#ected by the pres-(+330) : Mineralogical and physico-chemical pro-ence of Montmorillonite : extraction experiment

perties of four Thai soils with special referencewith potassium chloride and speiation by ,1

to speciﬁc surface area (SSA) and zero point of

Al-NMR. Soil Sci. Plant Nutr., .1 : ---ῌ-.- .

 :Uehara, G.. and Gillman, G.P. (+32+) : The mineralogy,



17

soil clays. Clay Miner., 2 : ,.+ῌ,./.

chemistry, and physics of tropical soils with var-Wada, K. and Okamura, Y. (+32-) : Net charge charac-

iable charge clays. Westview Tropical Agricul-

teristics of Dystrandept B and theoretical predic-

ture Series, No. .. Westview Press, Boulder, Colorado. p. +1*.
van Raij, B. and Peech, M. (+31,) : Electrochemical
properties of some Oxisols and Alﬁsols of thetropics. Soil Sci. Soc. Am. Proc., -0 : /21ῌ/3-.
Wada, K. and Greenland, D. J. (+31*) : Selective dissolution and di#erential infrared spectroscopy forcharacterization of “amorphous” constituents intion. Soil Sci. Soc. Am. J., .- : 3*,ῌ3*/.
Yoshinaga, N. and Aomine, S. (+30, a) : Allophane insome Ando soils. Soil Sci. Plant Nutr., 2 : 0ῌ+-.
Yoshinaga, N. and Aomine, S. (+30, b) : Imogolite insome Ando soils. Soil Sci. Plant Nutr., 2 : ++.ῌ+,+.
 : ,**-  +,  /  : ,**.  +  ,0 

9Y0Z [ 30 \ ],**.

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PZC

IEP, PZNC, PZSE

CD.6

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J. Jpn. Soc. Soil Phys.
¼= aNo. 30, p. +3,0 ,**.



   *Settling Pattern, Settling Rate and Zeta Potential of Marine Clay
Fumiyoshi KONDO** Faculty of Agriculture, University of Miyazaki, +ῌ+ Gakuen Kibanadai-nishi, Miyazaki 223ῌ,+3,, Japan+     

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23

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Time-settling curves of typical zone settlingfor Ariake-kantaku clay in sea water.

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Fig. /

Time-settling curves of typical consolidation settling for Ariake-kantaku clay
in sea water.

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24

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Relationship between settling rate andorganic matter content in sea water (w*῍.,***ῌ).

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yOz!bOd"
 }JE&|xO &~'b (
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Relationship between zeta potential andsalt concentration.

|x {#

0ῌ ῏ ῎ ῐ*.-+0gῌL &>5)(*OO5R &~'

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Michaels, A.S. and Bolger, J.C. (+30,) : Settling rates   

and sediment volumes of ﬂocculated kaolin sus-   
! "#25

pensions. I & EC Fundamentals, + : ,.῎--.

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CD@EF!"%&%GH#IJK$%&'LM#()*LM $D

Ohtsubo, M., Egashira, K. and Takayama, M. (+32/) :NO8PQ#I ROST  J.K. Torrance LMU

Properties of a low-swelling smectitic marine

V$+,4WX- clay of interest in soil engineering. Canadian
Geotechnical Journal, ,, : ,.+῎,./.

ῌ ῑ ῐ ῍nY./0ῌ#()* R+32. : 1Z2345A,
[\]1Q67^_8` // : -,+῎sions. AIChE Journal, ,/ (0) : 3+-῎3-*.
Imai, G. (+32*) : Settling behavior of clay suspension.
Soils and Foundations, ,* (,) : 0+῎11.

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 R+33. : rZQ5

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Jstῌ

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Fitch, B. (+313) : Sedimentation of ﬂocculent suspen-

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R{Sf_ JK0 +2/ : 1-῎2*.
Kondo, F., Kunitake, M., Takayama, M. and Ohtsubo,

Torrance, J.K. (+32-) : Towards a general model ofquick clay development. Sedimentology, -* :/.1῎///.

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M. (+333) : E#ects of salt concentration on set-

Wilson, W. J. (+321) : Soil smectites and related inter-tling pattern and sediment volume of low-

stratiﬁed minerals. Proc. of the 2th International

swelling smectitic marine clays. Proc. of the ++thInternational Clay Conference, Ottawa, +331 :12+῎120.
Kondo, F. and Torrance, J.K. (,**- a) : Physical, chem-

Clay Conference, Denver, +32/ : +01῎+1-.

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Yong, R.N. and Sethi, A. J. (+311) : Turbidity and zeta

patterns of thoroughly disturbed soft marine

potential measurements of clay dispersibility.

clay. Trans. JSIDRE, ,,- : 23῎31.

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IJKLM !N
OP OPQR
J. Jpn. Soc. Soil Phys.
p-O }
No. 30, p. /+F/0 G,**.H

 ./ 
    : ,**-  +/  ++  ,,   : 

TDR 
 

Assessing TDR Method for Simultaneous
Monitoring of Water and Solute in Dune Soil         A B/vwy

Hossein DEHGHANISANIJῌ CDῌ]

 !"# TDR $%&'(Time domain reﬂectometry (TDR) is rapidly be-) + *"+ (,-./0 1"#2&

coming a popular method for measuring water con-

'3 ()-456+ (7 89(tent and solute concentration in the laboratory as

: ; 8 (:well as in the ﬁeld.

<='3 9(7 *.*/

Success or failure of TDR to>*.+ cm- cm?- -()*@+ A B!C./

measure solute resident concentration depends on

DE- "&+

the accuracy of the calibration used.

($7F< -*>.* cm -$()G *.+ cm- cm?- 56 *.-/>*.. cm- cm?-

In this study,

the accuracy of TDR method for monitoring water

CHI 4&+ J;K + / B!C./&#"and solute simultaneously, in dune soil was tested.

LMN*O&'3 ,0-#$7(0PQR

Test results showed that the TDR method has highL+(G . %56 / ST 5U#+ V< 1*>3* cm&WDEX;G'(&'3accuracy for monitoring soil water content, but it hasless accurate for monitoring soil electrical conductiv-

 : TDR, ()+ (0+ ,0

ity across a water content range of about ῍*.*- cm-/cm-.

 : TDR, soil water content, soil solution,

 !"#$%&
'()* +,-.
YZ  )[*  \YZ *dune soil, calibration.

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52 :     

Burhanuddin RASYID

 

1j0j\ 8ῌ8
Wood bark as a side-product of agriculture can beused as organic amendment in nutrients recycle and ῌ

 soil improvement. The e#ect of wood bark incorporation to three-phase composition of soils, soil resist-ance, hydraulic conductivity, and water retention!"#ῌ$%&ῌ'(

was investigated on clay and sandy soil. This study*

indicated that in soils tested, both samples have+,-ῌ . /012.34

 )di#erent tendencies when wood bark is incorporated

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to the basic of physical properties.

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in many countries, mostly past researches based on !"#$ %&'( )*sandy soils. This study gives an account for various
soil water

repellency classes of volcanic ash

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tent.

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phenomena of main drying process and three wett-

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(¼῎9No. 30, p. /1 0- ,**.



   *Numerical inverse procedure to estimate soil hydraulic properties using Excel
Kosuke NOBORIO** Faculty of Agriculture, Iwate University, -ῌ+2ῌ2 Ueda, Morioka, Iwate *,*ῌ2//*, Japan
Abstract
There is a big demand to predict water movement and solute transport in soil not only inagricultural but also in environmental ﬁelds.

To predict water distribution in soil, soil hydraulicproperties, i.e. a water characteristic curve and hydraulic conductivity, should be known in priori.
Measurement of soil hydraulic properties, however, is usually time consuming and laborious
work.

Recent improvements of computing power on PC enabled us to inversely estimate

hydraulic properties using a numerical simulation model along with experimental data.
Spreadsheet-type software, which has a macro language and a solver, is also popular. In thisstudy Excel was used to numerically simulate soil water movement using the ﬁnite di#erence
method written in Visual BASIC as a macro function. The solver function of Excel successfully
worked with the numerical model to estimate best-ﬁtted values for soil hydraulic properties bycomparing simulated results with temporal changes in soil water content measured.

The tempo-

ral changes in water content were measured with time domain reﬂectometry (TDR) at ,* cm below
the soil surface during water inﬁltration into loamy sand.

A water characteristic curve withparameters inversely estimated reasonably agreed with that with parameters experimentally
determined.

Saturated hydraulic conductivity inversely estimated also agreed well with that

determined by an experiment.

Excel would be alternative software to estimate soil hydraulicproperties with an inverse procedure.
Key words : inﬁltration, hydraulic conductivity, water characteristic curve, ﬁnite di#erence
method (FDM), time domain reﬂectometry (TDR)oUp qrsGs(tEuv$ p$+    

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῏ῒῌ+Appendix +draulic properties. Soil Sci. Soc. Am. J., 0, : 23.ῌ3*/.
van Genuchten, M. Th (+32*) : A closed form equation
for predicting the hydraulic conductivity of unsaturated soils. Soil Sci. Soc. Am. J., .. : 23,ῌ232.
Wraith, J.M. and D. Or. (+332) : Nonlinear parameter
estimation using spreadsheet software. J. Nat.
Resour. Life Sci. Educ., ,1 : +-ῌ+3.
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63
J. Jpn. Soc. Soil Phys.
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No. 30, p. 0/1* ,**.

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T-C amount in soil aggregates under di#erent pressures
following substrate incorporation
Yoshiko MUTO*, Kunio WATANABE* and Akira SHINJO** Faculty of Bioresources, Mie University, +/+/ Kamihama, Tsu, Mie /+.ῌ2/*1, Japan
Abstract
With the growing concern over the sustainable use of soil organic matter, it is important toknow the relationship between microbial activity and the physics of soil. This study measuredchanges in the T-C in soil aggregate and crushed aggregate at sub-atmospheric and atmosphericpressures, following substrate incorporation, to examine the e#ect of decompression on microbialactivity in soil. The T-C decreased rapidly in the beginning and decreased more slowly at latertime stages.

The decrease in T-C varied with pressure.

The decrease in T-C was greatest at agauge pressure of approximately ,* kPa. The decrease also di#ered between the aggregate
and crushed aggregate samples.

These results suggest that the chemical potential of soil waterchanges with decompression, a#ecting the vital activity of microbes.

Furthermore, soil aggre-

gates play an important role in this activity.
Key words : Decompression, Total carbon amount, Microbe, Soil water, Soil aggregate

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Jacinthe, P.A., Lal, R. and Kimble, J.M. (,**,) : E#ects

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70

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J. Jpn. Soc. Soil Phys.
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No. 30, p. 1+ 2+ ,**.

    *Spatial Variability Analysis of Soil Properties in a Hilly Upland Field
Junichi KASHIWAGI*
Graduate School of Agriculture, Hokkaido University,
Kita 3 Nishi 3, Kita-ku, Sapporo, *0*ῌ2/23, Japan
Abstract
Spatial variability of soil properties was studied by using correlation analysis with landscapeand geostatistical concepts on a +.,-ha upland ﬁeld in a hilly area. Soil properties of Ap horizon
were examined on a square grid at +.-m intervals and on three transects at 1-m intervals. The CV
values suggested that the variabilities of most soil properties were higher than the results
reported at any topographical conditions. These large variables depend on the result of soil
erosion and sedimentation in response to the landscape. At the eroded area, the thickness of Ap
horizon had been kept constant with subsoil by tillage, as a result Ap horizon was composed of
di#erent soil materials from sedimentation and erosion e#ects.

The spatial variability of pH,

total carbon content, phosphate absorption coe$cient, bulk density, stone, sand, silt and clay
content could be explained with topographical features ; however, available water content was
di$cult to explain. Moreover, former properties were distinguished at landscape model units,these contribute to the rational soil sampling system to realize regional soil management. The
multiple regression models of total carbon and stone content, using only topographic attributes
calculated from a digital elevation model (DEM), matched reasonably well with the observed data.
Key words : soil properties of Ap horizon, spatial variability, terrain analysis, geostatistics, spatial
distribution

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Burgess, T.M. and Webster, R. (+32* a) : Optimal\89:$

Interpolation and Isarithmic Mapping of Soil*..,

Moore et al. *+33-+ qrs./0

Properties, I The Semi-Variogram and Punctual

W&4:$ *..2, pHῌQ*`Nῌῌ#7 " D./0W&

0 *..+*.0 J*..*

R73?" =GHp=F$ \,P73v7 " ,=/q-*

! S7% pAj GP=?D C  " p373
 TPURJJKD  p(

Kriging. J. Soil Science, -+ : -+/ῌ--+.
Burgess, T.M. and Webster, R. (+32* b) : Optimal
Interpolation and Isarithmic Mapping of Soil
Properties, II Block Kriging. J. Soil Science, -+ :---ῌ-.+.
Beckett, P.H.T. and Webster, R. (+31+) : Soil Variability, Soils and Fertilizers. -. : +ῌ+/.

JVJ qrs./0W(X"Dalrymple, J.B., Blong, R. J. and Conacher, A. J. (+302) :< DD ppY =*An Hypothetical Nine Unit Landsurface Model.

p=F$(JD  =*(<\J

Zeitchrift fur Geomorphologie N.F. Bd., +, : 0*ῌ

D (u"10.

`a : '(Imade, A.S.W., Shibusawa, S., Sasao, A. and Hirako, S.

81Land. Soil Sci. Soc. Am. J., 0. : +1--῏+1-3.

(,**+) : Soil Parameters Maps in Paddy Field

Webster, R. and Burgess, T.M. (+32*) : Optimal

Using the Real Time Soil Spectrophotometer.

Interpolation and Isarithmic Mapping of Soil

Journal of JSAM, 0- (-) : /+῏/2.

Properties, III Changing Drift and Universal

Journal AG. and Ch. J. Huijberegts (+312) : Mining
Geostatistics. Academic Press.
King, D., Bourennane, H., Isambert, M. and Macaire, J.

Kriging. J. Soil Science, -+ : /*/῏/,..
Woods, L.E. and Schuman, G.E. (+322) : Cultivationand Slope Position E#ects on Soil Organic

J. (+333) : Relationship of the Presence of a Non-

Matter. Soil Sci. Soc. Am. J., /, : +-1+῏+-10.

Calcareous Clay-Loam Horizon to DEM Attri-

Zevenbergen, L.W. and Thorne, C.R. (+321) : Quantita-butes in a Gently Sloping Area. Geoderma, 23 :tive Analysis of Land Surface Topography.

3/῏+++.

Earth Surface Processes and Landforms, +, : .1῏Miller, M.P., Singer, M. J. and Nielsen, D.R. (+322) :Spatial Variability of Wheat Yield and Soil
Properties on Complex Hills. Soil Sci. Soc. Am. J.,/, : ++--῏++.+.
Moore, I.D., Grayson, R.B. and Ladson, A.R. (+33+) :Digital Terrain Modelling : A Review of Hydrological, Geomorphological and Biological Applications. Hydrological Processes, / : -῏-*.

/0.

 +320 :   /- : /2῏0..
 ,**- : !

"#$%

&!$'()*  3/ : ,+῏-,.
+,-. +31- : /0'(12ῌ pp. ,2῏-* 345
6 78
9:;ῌ<=> +31+ : ?7@ABCDECF

Moore, I.D., Gessler, P.E., Nielsen, G.A. and Peterson,&GHIJKLM NOPQR!STUV

G.A. (+33-) : Soil Attribute Prediction Using Ter-

TW ?XYZ[\ ῍Q R]^_`arain Analysis. Soil Sci. Soc. Am. J., /1 : ..-῏./,.

b -0 : .+῏.0.

Park, S. J., McSweeney, K. and Lowery, B. (,**+) :Identiﬁcation of the Spatial Distribution of Soils
Using a Process-based Terrain Characterization.
Geoderma, +*- : ,.3῏,1,.
Pennock, D. J. and Corre, M.D. (,**+) : Development
and Application of Landform Segmentation Procedures. Soil and Tillage Res., /2 : +/+῏+0,.

9:;ῌcdef +31/ : ghR!



ij NOPQSTUVTWMYZ[\ ῌQ R]^_`ab // : +῏2.
klmn +31+ : opqrs!CDECF&GHI
JtuQR!STUVTW ?XY
Z[\ ῌQ R]^_`ab -0 : +῏1.
vDwῌxyz{ῌ|D}{ +31+ : 4~=Timlin, D. J., Ya. Pachepsky, Snyder, V.A. and Bryant, !Ci0&GHIJtuQR

R.B. (+332) : Spatial Temporal Variability of Corn

!STUVTW ?XYZ[\ ῎Q R

Grain Yield on a Hillslope. Soil Sci. Soc. Am. J.,
0, : 10.῏11-.
Van Oost, K., Govers, G., Van Muysen, W. and Quine,]^_`ab -0 : .1῏/-.
 +32- : !$ & 
 .1 : 2῏+..

T.A. (,***) : Modeling Translocation and Disper- : ,**-  2  ,, sion of Soil Constituents by Tillage on Sloping : ,**.  +  ,- 
J. Jpn. Soc. Soil Phys.
¼2uNo. 30, p. 2- 22 ,**.








THF



*ῌ*ῌ*Frost Heave of Tetrahydrofuran Clathrate Hydrate on Porous Glass Powder
Kunio WATANABE*, Kousuke YOKOGAWA* and Yoshiko MUTO** Faculty of Bioresources, Mie University, +/+/ Kamihama, Tsu /+.ῌ2/*1, Japan
Abstract
The formation process of clathrate-hydrate in porous glass powder saturated with THF-water
mixture was observed using directional cooling apparatus.

When the cooling rate became lower,

THF hydrate grew with excluding glass particles and formed lens -like layer of hydrate in thesame manner as in the phenomenon of ice lens formation in the freezing of soil. The growth rateof hydrate lens was proportional to the supercooling degree of the growth surface and about
one-twentieth the growth rate of hydrate layer in THF-water mixture without glass particles.
When NaCl was added into the system, the growth of hydrate lens was inhibited depending on the
NaCl concentration.
Key words : THF clathrate hydrate, frost heave, glass powder, directional growth, in situ
observational., ,*** ; ,**,1+          

zS$Wc mnojklO{N |}"& c
higjklmnojkl5? ~

( N; -wxMI1  !"#"$%#"& '( )*+I u -'JKakKI THF 1 , -./01

23,445' 6&

47"&89:;<= >%#(>"&' -ῌ +330?@;  ,**+1  wxMmnojkl [\]^$A BCDE -FGῌ?H +33+1 IJKLM -Zhe etIYZ +*+,+*+2 m- 5^$al., ,***1  : N4 89:

W<( -Sloan, +33* ; Matsumoto, ,**,1; >OPQ RST468

fg5"WWc 6& +TUVW3& - ,***1 54X YZ

fg## $&  mnojk

I[\]^_$`(#"&aJ l"+$%Wc -Uchida,I+331 ; Uchida et al., +3331 $ CFCs -Chlorofluoro-NbO"& 'c d6A

%#"&efghigjklmnojkl
45' -Dallimore and Collett, +3311 "!"ecarbons1  "¡¢£¤ THF &mnojkl '¥¦§()¨*5"W©+Wc

-Iida et_"$   dpqlirostiM -THF1

al., ,***1 47"&ª«I¬­,<=mnojk

mnojklu:I -Rue# and Sloan, +32/1 v

l®¯°6(55IwxMmnojklyu: -Chuvilin et± -Mak and McMullan, +30/ ; Gough and Davidson,* ²³´´- µ/+.ῌ2/*1 ¶·..¸ +/+/
 : THF higjklmnojkl ./0 fig/; ¹0º(»1 NbmnojklQ"»+,\

84+31+ ; Sloan, +33* 

] 30 ¼ ,**.

8YZ[(+s,

Ross

THF +et al., +32+ ; Leaist et al., +32, ; Handa et al., +32.

  -t(  ;

YZ[2m+uv-P

<=8 Rue# and Sloan, +32/ w#2m

  !"#$%&'() *+&', -+uv1g#!"<xyz(=8 Chuvilin et./0  Uchida et al. +333 12

al., ,*** ; ,**,

+345+/0-6789:;

,, 

<<= <

THF +{># ?@  THF 8E+|}1\ *~... 8A4(8=>% THF ?"$%@A

Hanley et al.,-&'() , +*+B/0CC+323 !HI% THF -B]E8ik + :

+1 %|} ?@... p <c+HI%  +333 ; Nagashima et al., ,*** ;Iida et al., ,**+ 8DC  THF E2+

 THF E2 NaCl -C THF E2-D

FGHI-J< THF +',E< +* 1P YZ[(8/0+F +E !G% YZ[(+HI( 'K+ THF +LM< *=%!NO% THF E2+H-E8=88( %"+1P#Q $+&',|} <YZ[( D2+ THF 

NaCl +-

%RST+UVWX-() THF E

 NaCl   ῍2  JA4(

2%&'YZ[(+ FGHI-J\ *=%Ea*+2 d+ +.+ K+EL8, 

2, a*+2+ NaCl  Cintd LL 82

d+ +.+ K+E LL+.+ <E w -t(,+  !HI% THF Aldrich, 33.3ῌ NaCl ]E Y

a*-Mn 1.// mm  +/* mm +NYZ[Z[( ^)4'_` P0** -a*< THFk) O-P) k-Zzzk

+"?#$<ῌb+-&'(%DE 67 ¡¢£k8YZ[(Gough and Davidson, +31+ c-)#k-  #kQI- /< 2d, -.,!CDR k$S-2T5¤U¥¦R-+'e&'-/0(  THF E
P-.,

J\ k-%fg=

1h%) +ij

kl8CC

FGVW%$S1gG§ + kRS+# +* $S+#¨. %fg kM+#©XG-)1g , ª«

Devarakonda et al.,,.,1* ¬\ !HI­®#

 -.- nm +4oQ-5(©X *.+.¯*.*+/ mm¨+ °\ a*+G, +7p =+YZ[( Hq+"67%R -5(

m-j±²k³j´µ¶Z-<YZ/0=8 r8< 9: ,***

THF +',

+333 !HI%<YZ[(+2m 2n
mm 3\g+  THF ῌ+

Table +

a*+s,

Physical properties of sample+ : +1 sol4 Hydrate Water

Ice

Thermal cond4 Wm¨+ K¨+*4/0,a*4/,/a*4/0+,4+.
Speciﬁc heatkJ kg¨+ K¨+.4,+b,4+,-c.4,+1,4++Densitykg m¨331d
331d
+***
3+1
Melting point
Latent heat
kJ kg¨+

Di#usion coef4 m, s¨+

.4.e
,0*c
¨

+7m-£·¸²-+4*+*¨3 fMean diametermm,4,
Mean pore sizenm
-4Speciﬁc pore volume m- kg¨+ *4-+*¨Speciﬁc surface area m, kg¨+ +,3+*Density
kg m¨- ,+,**--¨

Glass powder¨

Hydraulic cond4m s¨++43+*¨2ik + : +1 + THF E2 + : +1sol. ¹º6ik+ THF hydrate Hydrate  .4. + E Water ¹º; Ice  * +[a Ross and Anderson (+32,), b Iida et al. (,**+), c Leaist et al. (+32,), d Gough andDavidson (+31+), e Hanley et al. (+323), f Gillen et al. (+31,)

¢£ : $%&NOF THF ¤%&HH! ¥¦

ῌ,

85

! NaCl <,

Table ,

NaCl concentration in solution andthe ratio of solution to glass powder

Name

Cint (῍)

LL (῍)

LL+4+w (῍)

S*
S**S**-w
S*S-**4**4**4-

++/
+,/
+,/
+.+2/

+,04/
+-14/
+-14/
+/14,*-4/

+,04,
+-04,
+//4/
+//4/
,*-41

- -+ 




ῌ+
Fig. +!"

YZ!

Schematic illustration of directionalcooling experiment.



#$%&'()*+,-./!01234 5 ,  ,. 6789:!

;S*

NaCl < *῍= !/>?@AB!C(DE 5F

&GHI + mm DE JKLM1$%&NO P
QR! S14/TU VW X

YZ[\
YZ]^
 YZ1ab_/!4`W\.VK#c@1adEe ;YZe

= 1fg. h]!/14$%&NOijXk4.1Wl +** mm -T>? ;5 ,=!/!>?1m- n\ijTo!

/14ῌ>?
\_4ῌ>?123[#4/$%&NO!pqr.0stu

1v>[\ 4/!w[ :v>x!)ῌ,Fig. ,!/>?@AB!C(Crystallization in glass powder
saturated with + : +1 THF solution.

+wg.K
hxij ;h:= 4/ .2 67T -.+0
mm -T>? -..*.y zK!"!>?@!

!YZ{|: h:4/}I~zA S /U  ;5 -=  ! VW 4/
THF HTU 1V -_

NOF!4H n!vsVW 
H E-,

5 . hxij4H!>? ;

= !67 5 / n!6!

H!>?@!n\\DE 5 ./ ! hxij!H14

VW!8967TU \!

x 

H!>?e]^eg ofg

ῌFig. -4/¡C(

The crystal burns readily in air.

±²³´ µ 30 ¶ #,**.%86   

i{HNm)   = |i{}'  THF 

S* S**- S**-w S*- 7 *.*-- mm sf+Kf+ *.*,* mm!" #...$% &'$ () *+,

sf+Kf+ *.*,. mm sf+Kf+ *.*-, mm sf+Kf+-*+./012)

T NaCl U~4hi&L

 .2 * NaCl 34

 56S}

/56 #S*% 7 89:*+  Z 0  X   S* S**- S**-w S*- 7, ..+-$ 7;  !"

*.,1 +..1 *.3+ ,.1/

& *.,1$ (<  => ?@ABCDE&a89:*+, #...f!"F(GHI JKL>M

X  %  ..+-$ ,.3-$ -..3$ +.0/$  =>L<L 56
el>M

HN& .2 OP

P]^ +K ;hWXa*+

QR ST NaCl U *.*-ῌ 56 #S**-% 7 ,./+m #*./ mm sf+Kf+% uhav*+m #+,.- mm

mm *.-ῌ 56 #S*-% 7 ,.*- mm

sf+Kf+%  +ῌ,/    =>ST NaCl UF2/

VKWXY)  #Z .%  [v:/ # +% &M >M=\]^_`7 ST NaCl U -ῌ 56 #S-% a7 BCazA*+m *+,

bcdF*+H 

h #Hh% & uhav*eL><  .2 OP

+m +ῌ,*+ῌ-*  M #Watanabe, ,**,% w*+, S* 7 ..*.$ S**- 7 ,.1-$

xy7R>*+mlhW

S*- 7 +.02$ S- bcd*+,

Xa*+m +ῌ,* 7; v

 VKWXSTUF2/

jk *+,7h

f*.-/$() #Z /%

FN/M JKL>MS**-w  VKWXST NaCl UF S**-g.H) #*.*-ῌ% 4hiF2/567;M jkST
NaCl U7; Nl 4hiF2)M 

Q) *+,2)  #Z . /%
-- 



==7 Z . <L*+m3
Z / <L*+,P]^ #nTo...fT% 3pI Z WX ¡G¢nTms nTmsoi KC 7
R>M ==7 i !"}' K W£¤ ¡G
¢ C W¤U7;M  ?@ABC&
MWX ¡G¢3nTmpt>¥ ¦§¨H©

 THF *+, Tgs  Tgs o...fn

0a *+m P]^qr3st Z 0b  uTmsfnTmp 7ª7|M JKL>M / Z 0  X

ha7*+tMv wxy jk?@ABCa7*+tMzA #Watanabe, ,**,% + : +1THF hW

THF hWXa7!"­' i 3 , THF hWX¤

Xa7*+tM THF *+mlsH

 ¡G¢3h jk +.20 $ kg molf+ *+m*+,P]^**- S*- S- ®¯M*+, NaCl

ῌ. 8l2°H*+¢ῌ/

Fig. . Growth amount of the warmest hydrate lens.

3 Tgs S *  « ¬ < L n Tmp 3 *.,1$ NaCl 
tM  S8l2°H*+,
Fig. /

Temperature at growth surface of
the warmest hydrate.

 : QRSkl8%w¼

THF sRS ! !xbyz

87

et al., ,**+3  nij4JCa/    oh-pqrl8sRS ! !t"uvw\xbyz{|}~ 4 %:jKL4.

DE THF 79C

QRSkl8%XY !& * 
G THF 7 NaCl &,- 

 !XY"*  !&"#>

&J*

 THF !XY"#<XY"#u%C G NaCl
&,-   !XY"#W
,- "#<M,-

&

%-.

 ObDE oQRSkl8mSXY
"# 2xbyz3 ij4JCar40>  XYD"ῌ0Fig. 0"#<"#u
2a3  !QRSkl8
 !XY 2b3 º78» QRSk
l8mSXY 78 THF  !
Growth rate and degree of supercoolingat the growth surface.
(a) THF hydrate in glass powder. (b) ice
in water, ice lens in glass powder, and
THF hydrate in solution.

xbt}~-eoxb%> &o
h-pqrl8 !t"uv4> %9(   !XY"#+7~ ¡¢r^_£  K¤o
4KL4h¥&¦ )§h¨©4ª/ %¦¯-°±4)

«I¬#1­%®
%²Ca³´µ4¶>- w  ¨ ©  ¨ © ·  : ¸  ¹ ¬ ¨ © ·2+.10*+/03 %

 +.3ῌ -.3ῌ 1.*ῌ  NaCl  ,.- 

0- 



 !"#$% NaCl &
Chuvilin, E.M., Perlova, E.V., Makhonina N.A. and!"#'()*  "#+ NaCl &

Yakushev, V.S. (,***) : Research of hydrate and,-./0

ice formation in soils during cyclic ﬂuctuations#1

2+3333  -ῌ  NaCl 456 + : +1THF 7

89:;< 2/ mm s=+3 9"#>

THF 

!"#+ NaCl 4?@A9B;CDE

of temperature. Ground Freezing. pp. 3ῌ+.,Balkema, Rotterdam.
Chuvilin, E.M., Makhonina, N.A., Titenskaya, O.A.

 !"#+9 NaCl & ../ῌF/.0ῌ

and Boldina, O.M. (,**,) : Petrophysical investi-

G9HI>

4JC KL9 #1 KL

gations on frozen sediments artiﬁcially saturat-!"#<&M 2N 0 ;*.*/ mmed by hydrate. Proceedings of the Fourth Inter-=+OP3 "#+ NaCl HI,-.

national Conference on Gas Hydrates : 1-.ῌ1-3.

 G QRSTU&V S**-w 9 S**-

Dallimore, S.R. and Collett, T.S. (+331) : Gas hydratess"#W&,-. 


2N /3 

associated

with

deep

!XY"#+9QRST% NaZ [Mackenziedelta,

N.W.T.,\ Cl= ]X^_& `* a 0"#+9 NaCl bc &V
defg%f 

permafrost

in

the

Canada : Regional

overview. Proceedings of the Seventh International Conference on Permafrost : ,*+ῌ,*0.

hCij QRSkl8m

Devarakonda, S., Groysman, A. and Myerson, A.S.

SXY"#+ NaCl bc 2Watanabe(+333) : THF-water hydrate crystallization : an

mn opq v 30 w ,**.

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Growth, ,*. : /,/ῌ/-2.

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THF ,-./0123456789:;<=;> ?@ABCD EF 0+ : +.3ῌ+/..
Nagashima, K., Yamamoto, Y. Takahashi, M. and

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rptu : ,**. t + u ,0 ῐ
J. Jpn. Soc. Soil Phys.
ῑ῏῎ῒΐῐ
No. 30, p. 23ῌ30 ῍,**.῎Physical Properties of Soils as Inﬂuenced
by Incorporation of Wood Bark
Burhanuddin RASYID*, Katsumi FUJII**, and Hiroyuki FUJISAKI*** The United Graduate School of Agricultural Sciences, Iwate University,-ῌ+2ῌ2 Ueda, Morioka-shi, Iwate *,*ῌ2//*, Japan** Dept. of Environmental Sciences, Faculty of Agriculture, Iwate University,-ῌ+2ῌ2 Ueda, Morioka-shi, Iwate *,*ῌ2//*, Japan
Abstract
The e#ect of incorporation of wood bark on three-phase composition of soil, soil resistance,
hydraulic conductivity, and water retention was investigated on clayey soil and sandy soil.
Application of wood bark was arranged at *.*ῌ, +.*ῌ, ,.*ῌ, -.*ῌ, ..*ῌ, and /.*ῌ of wood bark tosoil (dry weight basis).

Soil resistance was determined with a hand-held cone penetrometer(Yamanaka-shiki Koudokei), the hydraulic conductivity by using the variable head test technique, and water retention by the hanging water column method and centrifuge method. The
remarkable result was found in sandy soil such that incorporation of /ῌ wood bark produced
reduction of -+ῌ solid phase. The soil resistance was higher in compaction stage than cutting o#stage at both soils. In clayey soil, it decreased from +... kgf/cm, (*ῌ wood bark) to +*./ kgf/cm,(/ῌ wood bark) in compaction stage, but it varied in cutting o# stage with maximum at 3.1 kgf/
cm, (+ῌ wood bark) and minimum at 1.. kgf/cm, (-ῌ wood bark). Hydraulic conductivity inclayey soil reached to the maximum (-./῍+*ῌ. cm/s) with incorporation of /ῌ wood bark,
however in case of sandy soil it changed inconsistently as addition of wood bark. The increase inwater content by -ῌ wood bark was kept almost constant as ..+-ῌ even in low suction at pF *.2(ῌ*.0* kPa) and as ..*+ῌ in high suction at pF /./ (ῌ-+ MPa) in clayey soil, while in sandy soil, it
diminished from +..*ῌ at pF *.2 (ῌ*.0* kPa) to *.*+ῌ at pF .., (ῌ+./ MPa).

This study

demonstrated that incorporation of wood bark inﬂuenced the physical properties of clayey andsandy soil.
Key words : Wood bark, Three-phase composition, Soil resistance, Hydraulic conductivity, Water
retention+.

Introduction

Application of agricultural side product has
been widely practiced in agriculture ﬁeld. It
has been considered as a desirable material torecycle nutrients and soil amendment. For
decades, compost of animal manure is the mostpopular material of this product. However,increasing of plant residue from agriculture
production has changed motivation to utilize it
as a resource in soil amendment. Among thekinds of plant residues, wood bark can be pro-

posed as a material for this purpose. This
material is made by lumber mill as by-productsof lumber and which is usually burned up or
thrown into the ground.
Numerous researches have revealed the utilization of crop residues and its e#ect on soil
physical properties, such as the inﬂuence onpore size distribution (Anderson et al., +33* ;Emerson, +33/), the stabilization of soil aggregates (Tisdall and Oades, +32,), the e#ect oncompaction and compression behavior (Gupta
et al., +311 ; Zhang and Hartge, +33/), water-῏  30

90

stability of soil aggregates (Mazurak et al.,+311). The inﬂuence of addition of wood bark
into soils on physical properties could be due tothe change in the three-phase composition ofsoil. The properties have interaction to thedecreasing of bulk density and increase inwater content. Tester (+33*) showed that compost signiﬁcantly reduced the bulk density(./ῌ for the ,.* Mg ha+ compost rate). Decrease in bulk density was associated with increase in the water content of compostamended soils and an increase in soil absorption capacity as a result of increased surface
area and organic matter (Gupta et al., +311).
This e#ect can be allowed to change the soil’s
water-retention characteristics. Da Silva (+331)
reported increasing in available water holding
capacity of *.*-3 and *.*,* (m-/m-) for soil with
1 and -/ῌ clay when organic matter content
was increased by *.*+ kg/kg.
Although the experiment on the utilizationof organic matter is well documented, but little
literature has been published especially on application of wood bark for soil amendment andits e#ect on physical properties of soil. For the
optimal application of wood bark in soil
amendment, it is important to know the inﬂuence of wood bark on physical properties
when it is incorporated into the soils. The
purpose of this study was to examine thee#ects of application of wood bark on threephase composition, soil resistance, hydraulicconductivity and water retention.
,.

Materials and Methods

Two kinds of soils taken from the sitearound Morioka-city were used in this experiment. The clayey soil had dry bulk density of*.1, Mg m-, particle density of ,.01 Mg m-,and water content by weight *./- kg kg+,whereas sandy soil with dry bulk density of+./. Mg m-, particle density of ,.20 Mg m-,and water content by weight *.,* kg kg+.
Wood bark of cedar was shredded into thinﬁber and then processed to compost material
used as a source of organic matter. The wood,**.

bark ﬁber had particle density of +.1* Mg mand a water content by weight +.*- kg kg+.
The experiment was arranged at rates *.*ῌ,+.*ῌ, ,.*ῌ, -.*ῌ, ..*ῌ and /.*ῌ of wood bark tosoil (dry weight basis).
For soil resistance test, soil compaction
device is used. The device consists of mold andrammer. The mold is cylindrical stainless steel
rings, +* cm in diameter and +,.1 cm in height.
Penetrometer resistance was determined usinga hand-held cone-penetrometer (Yamanakashiki koudokei). Two stage measurements
were conducted to obtain resistance proﬁle according to the height of sample. The ﬁrst stage
was compaction stage. Samples are added into
mold and compacted sequentially on threelayers of . cm, 2 cm, and +,.1 cm in height.
Measurements were conducted on each layer
after sample was compacted by dropping therammer ,/ times from a height of +* cm. The
second stage is cutting o# stage. After compaction, samples were jacked up and taken out
from compaction device by cutting o# an
upper column of samples. Measurements weremade on the shaved o# layers of +* cm, 0 cm,
and , cm in height. Five points penetrometer
resistance were taken in each sample layer forboth stage conditions.
The three-phase composition was calculated
from the volume of total sample in the cylinderof the compaction device. With +,*** cm- of thetotal sample used in the cylinder, the mass
weight of solid, water, and bark were calculated from the data of water contents of eachcomponent. Then this mass weight was converted to the volume proportion of solid, water,and bark by using each particle density. Gas
phase volume remained, when subtracting
volume of solid, water, and bark from +,*** cm-.
The composition of solid, water, gas and bark
was determined by converting the volume proportion into percentage of each phase.
The measurement of hydraulic conductivity
was made using falling head test technique.
Each sample of clayey and sandy soils was
prepared so as to keep the same component of῏῎ : Physical Properties of Soils as Inﬂuenced by Incorporation of Wood Bark

the sample performed in the soil resistance test.
The samples were placed into the column sampler with / cm in diameter and /.+ cm in height.
These samples were set onto stainless steel
tray where ﬁlled with water to saturate the soil
samples for .2 hrs. Then a saturated sample
was set up at the apparatus. The hydraulicconductivity was determined from the magniﬁcation of the rate of the water fall in the standpipe from a height h+ (ﬁxed in +1.+ cm) to h,(ﬁxed in +*.* cm) at time t. This procedure wasrepeated three times for each sample. Then thehydraulic conductivity is calculated using thefollowing expression :k῍

91Fig. +

Three-phase composition of clayey soil
as related to incorporation of woodbark.

Fig. ,

Three phase composition of sandy soil
as related to incorporation of wood
bark.

h+
,.-aL
log+*
At
h,

where a is cross-section area of the stand pipe,
L is height of the sample, A is cross-section of
the sample, t is the descent time of the water
falling in the stand pipe from a height of thewater level h+῍+1.+ cm to h,῍+*.* cm.
Water retention was determined using hanging water column method and centrifuge
method. In hanging water column method, thesample held in ring sample was placed on a
porous ceramic plate. A step change in suction
at the bottom of the plate was induced bylowering a hanging water column connected tothe plate. The water column was set up 0./ cm,/-.2 cm and 30.2 cm lower than the central pointof sample, which was equal with the suction
values of pF *.2 (ῌ*.0* kPa), pF +.1 (ῌ/.* kPa),
and pF ,.* (ῌ+* kPa), respectively. Measurements of higher suction were done by centrifuge method for the same sample at pF ,.1 (ῌ/*kPa), pF -.. (ῌ*.,/ MPa), and pF .., (ῌ+./ MPa),and suction of pF /./ (ῌ-+ MPa) and pF 1.*(ῌ+.* GPa) were measured in air dried and ovendried condition, respectively.
-.

Results and Discussion-. + Three-phase composition of soils
Three-phase compositions of clayey andsandy soils as a#ected by wood bark incorporation are presented in Fig. + and Fig. ,.
Result indicated that in both soils, three-phase composition changed at any rate ofwood bark incorporation. For clayey soil, addition of /ῌ wood bark means the relative ratio
to soil (dry weight basis), and yields +.3ῌ composition to total volume. This mixing process
reduces -.,ῌ of solid phase. Thus incorporation of ﬁne ﬁbrous materials causes more spacethan themselves.
In case of sandy soil, this tendency appeared
more signiﬁcantly. That is, /ῌ of wood bark
incorporation corresponded to -.1ῌ volume
ratio to total, then it causes +1.0ῌ reduction ofsolid phase. Thus incorporating one volume ofwood bark ﬁber, ..2 times volume of sandy soil
would be replaced.

92ΐῐ῎῔῕ῑ ῒ 30 ῏ ῌ,**.῍-. , Soils Resistance
Soil resistances in each level of wood barkaddition are shown in Fig. - for clayey soil andFig. . for sandy soil. In all treatments, soil
resistance tended to decrease with raising theelevation of sample layers for compaction andcutting o# stages.
For clayey soil, curve in the sample control
showed little di#erence of soil resistance atcompaction stage, but it was high at cutting o#stage as rise of the sample layers. For thetreated samples, soil resistance decreased as

Fig. -

Soil resistance curves of clayey soil as
related to di#rernt level of wood bark
incorporation.

raised of sample layers at any level of woodbark addition. For the average as can be discerned in Table +, soil resistance increasedslightly from +... kgf/cm, to +../ kgf/cm, as
addition of +ῌ wood bark in compaction stage.
And then, it decreased steadily to +*..3 kgf/cm,
at addition of /ῌ wood bark. This pattern was
not observed in cutting o# stage. There was arise in soil resistances from 2.3 kgf/cm, at *ῌ
wood bark to ++.2 kgf/cm, at ,ῌ wood bark.
However, it descended strongly 1.. kgf/cm, byaddition of /ῌ wood bark.

Fig. .

Soil resistance curves of sandy soil as
related to di#erent level of wood bark
incorporation.

ῑῐ : Physical Properties of Soils as Inﬂuenced by Incorporation of Wood BarkIn the case of sandy soil, soil resistancetended to decrease as rise of sample layers ineach level of treatment at both stages of measurement. For the average, soil resistance dropped from +..1 kgf/cm, at *ῌ wood bark to 1..
kgf/cm, at -ῌ wood bark, and it increased
when wood bark added more than -ῌ in compaction stage. In cutting o# stage, soil resistance declined from 0.0 kgf/cm, at *ῌ woodbark to ..2 kgf/cm, at -ῌ wood bark, but it
increased to 1.+ῌ kgf/cm, at .ῌ wood bark,then decreased to ..3 kgf/cm, at /ῌ wood barkaddition (Table +).
The di#erence of penetrometer resistance ofboth soils could be attributed to the process
worked at the two stages. In compaction stage,
the whole sample was compacted within threepieces from bottom to top. In the bottom piece,
sample would be packed tightly because itsheight is at most . cm, so rammer impact
should be transmitted within all the samples.
Then tight structure would arise and whichleaded to high soil resistance. In the top piece,
rammer impact would spread into the taller
sample as +,.1 cm, which correspond to low
e$ciency of compaction. Thus the higher
layer exhibited the lower resistance. For cutting o# stage, three test surfaces for resistancemeasurement were produced from top tobottom, after all the compaction procedure. As

Table +

93

described just above, the top piece of sample
su#ered only one compaction process, while
the bottom had been compacted three times.
Therefore lower layer more compacted andshowed higher resistance.
-. - Hydraulic Conductivity
Hydraulic conductivity of clayey and sandy
soil showed di#erent trends at any rate ofwood bark incorporation (Fig. /). In clayey
soil, hydraulic conductivity ascended from +.,῏+*῎. cm/s (*ῌ wood bark) to ,.*῏+*῎. cm/s(-ῌ wood bark), and then it exhibited the maximum at -./῏+*῎. cm/s (/ῌ wood bark). Thus
the hydraulic conductivity increased smoothly
as the addition of wood bark. However, in caseof sandy soil, treated sample showed complex
behavior of hydraulic conductivity at any levelof wood bark incorporation. In the sample
added by ,ῌ wood bark, the hydraulic conductivity was dropped to the minimum value of ..*῏+*῎. cm/s. On increasing level to /ῌ of woodbark, the hydraulic conductivity reached thevalue of +.+῏+*῎- cm/s almost the same withthe control sample (*ῌ wood bark).
The result in clayey soil was expected fromthe fact that incorporation of wood bark subtracted solid phase and ﬁlled with water phaseand gas phase. Increasing of total pore space
could a#ect the developing of the hydraulictransport in porous media (Gupta et al., +311).

Average of soil resistance of clayey andsandy soil
Soil resistance (kgf/cm,)

Wood
bark
(ῌ)

*
+
,
.
/

Clayey soil
Compt.
stage

Cuttingo# stage.

Sandy soil
Compt.
stage

Cuttingo# stage.

+.4. ῌ-4.῍ 243 ῌ+43῍ +.41 ῌ*43῍+.4/ ῌ.4-῍ 34* ῌ,4.῍ 341 ῌ*42῍+,4/ ῌ.41῍ ++42 ῌ,43῍ 24. ῌ*4/῍+,4. ῌ.4*῍ +*4/ ῌ,4*῍ 14. ῌ*4-῍++40 ῌ-4.῍ 140 ῌ+41῍ 142 ῌ*42῍+*4/ ῌ,42῍ 14. ῌ+40῍ 242 ῌ*40῍

040 ῌ*4,῍/4, ῌ*4.῍/4, ῌ*4/῍.42 ῌ*4.῍
14+ ῌ*4,῍.43 ῌ*4,῍( ) Standard deviation

Fig. /

Hydraulic conductivity of clayey andsandy soil as a function of wood bark
incorporation.

94

If we assume that pore system is fully saturated and is composed of straight round tubesof uniform radius r, the Hagen-Poiseuille model
can be applied to the water movement in it.
Then H-P model predicts that water ﬂux is
proportional to the cross-sectional area ratio ofpore to total, namely, porosity, and to thesquare of the radius. In the case of clayey soil,
porosity expanded from 1-.0/ῌ to 10.20ῌ by/ῌ incorporation of wood bark, but its increasing ratio +.*. is far smaller than that of hydraulic conductivity such as -.*-. Therefore we cannot explain these experimental results only byporosity increasing, but by pore radius expansion.
-. . Soil Water Retention
Di#erent characteristic of water retention of
clayey soil and sandy soil as a#ected by woodbark incorporation at any suction level is presented in Fig. 0. The result showed that in any
suction level, clayey soil had higher ability toretain water than sandy soil as e#ect of woodbark added.
For clayey soil, the e#ect of incorporation ofwood bark was more obvious than sandy soil.
For example, the increment of water content(from 0..-0ῌ to 02..3ῌ) caused by -ῌ woodbark was ..+-ῌ at low suction of pF *.2 (*.0*kPa), and which is almost kept as ..*.ῌ (from.2./*ῌ to /,./.ῌ) at pF ,.1 (/* kPa), then to..*+ῌ (from -0..2ῌ to .*..3ῌ) at pF /./ (-+MPa). Based on the Young-Laplace equation
which explains hydrostatic suction in a capillary tube, capillary rise (ym) can be obtained as
inversely proportional to the tube radius r, as
follows,ym,sῌrrw
where s is the surface tension and rw is thedensity of water.
Using this equation, we can derive the equivalent capillary tube radius re for each suction,such as re*.+, mm for pF *.2, +../ mm for pF,.1. However, at high suction such as pF /./, we
can not postulate the capillary rise model, because re drops down to ,.-/ nm, which is not an
actual capillary size but surface adsorption

30

,**.

scale. Thus the e#ect of wood bark incorporation to clayey soil typically appears in ﬁne poresystem of nm scale, and enlarges its porosity as,.3ῌ at least. From three-phase composition
results for clayey soil (Fig. +), -ῌ incorporation
caused only +.00ῌ increase in porosity. This
discrepancy of observed data between two
ﬁgures is interesting problem which should be
examined further.
In case of sandy soil, incorporation e#ect islimited relatively at low suction. As shown in
Fig. 0, improvement of water content took+..*ῌ (from .-./.ῌ to ...3.ῌ) at pF *.2, butwhich decreased to *.01ῌ (from -,.1.ῌ to--..+ῌ) at pF +.1, then almost diminished at pF,.*. From the Young-Laplace equation, equivalent capillary radius can be calculated as re*.+, mm (pF *.2), +../ mm (pF +.1), and 1.,1 mm (pF

Fig. 0

Water retention curves of clayey andsandy soils as following the incorporation of wood bark at di#erent
suction.

῍ῌ : Physical Properties of Soils as Inﬂuenced by Incorporation of Wood Bark,.*). This estimation proved that incorporationof wood bark is e#ective only to the development of coarse pore system whose capillaryradius is larger than *.*+ mm. From threephase transition (Fig. ,), -ῌ incorporation
yielded +-./ῌ increase in porosity. Comparison of these two results proves that wood bark
incorporation would enlarge the capillary poresize of sandy soil matrix, but does not increase
the number of capillary tubes.
..

Conclusion

The results of this study indicated changes
in soil-physical properties as the e#ect of woodbark incorporation to clayey soil and sandy
soil. The three-phase composition of sandy soil
responded clearly to the addition of wood bark.
A comparison of penetration resistance of compaction and cutting o# stages designated thathigher soil resistance of compaction stage
resulted from process worked at the stage
measurements. Reduction of soil resistancetowards incorporation of wood bark showed inclayey soil. Hydraulic conductivity of clayeysoil increased as wood bark addition, but itchanged inconsistently in sandy soil. H-P
model presumed can be applied to analysis
increasing of hydraulic conductivity in clayey
soil, especially pore radius expansion. Soilwater retention in clayey soil was higher thansandy soil. In clayey soil, the wide range ofwater content is almost the same in each ofsuction level. The ability of clayey soil toretained water was explained by the YoungLaplace (capillary rise) model.
This study indicated that clayey and sandy
soils had di#erent tendencies when wood bark
incorporated. The basic physical properties ofboth soils considered as an important factor.
There are some interesting phenomena still
remained in this study. Therefore further ex-95

periment is needed to obtain more information
on how wood bark make interaction with soilwater system and which works to change thephysical properties of both soils and will betheme to next research.
Acknowledgements
The author would like to thank the Ministryof Education, Science, Sports and Culture,
Japan for the provision of the scholarshipwhich lead to this study.
References
Anderson, S.H., Gantzer, C. J. and Brown, J.R.
(+33*) : Soil physical properties after +** yearsof continuous cultivation, J. Soil Water Cons.
./ : p. ++1ῌ+,+.
Da Silva, A.P. and Kay, B.D. (+331) : Estimating theleast limiting water range of soils from properties and management, Soil Sci.. Am. J. 0+ :p. 211ῌ22-.
Emerson, W.W., (+33/) : Water retention, organic C,
and soil texture, p. ,.+ῌ,./, In : Sumner et al.
(ed.). (+333) : Handbook of Soil Science, CRC
Press, p. A.,.,ῌA.,/*.
Gupta, S.C., Dowdy, R.H., and Larson, W.E. (+311) :Hydraulic and thermal properties of a sandy
soil as inﬂuenced by incorporation of sewage
sludge, Soil Sci. Soc. Am. J. .+ : p. 0*+ῌ0*/.
Mazurak, A.P., Chesnin, L., Thijeel, A.A. (+311) :E#ects of Beef Cattle Manure on Waterstability of Soil Aggregates, Soil Sci. Soc. Am.
J. .+ : p. 0+-ῌ0+/.
Tester, C.F., (+33*) : Organic Amendment E#ects on
Physical and Chemical Properties of a Sandy
Soil, Soil Sci. Soc. Am. J., /. : p. 2,1ῌ2-+.
Tisdall, J.M., and Oades, J.M. (+32,) : Organic
matter and water stable aggregates in soils, J.
Soil Sci., -- : p. +.+ῌ+0-.
Zhang, H.Q., and Hartge, K.H. (+33/) : Mechanicalproperties of soils as Inﬂuenced by the Incorporation of organic matter, In : Hartge, K.H.,
and Stewart, B.A. (ed.) : Advances in Soil Sci.,
Soil Structure Its Development and Function,
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Sweden. Global Change Biology, 1 : +1+ῌ+2*.
Beckwith, C. W. and Baird, A. J. (,**+) : E#ect of biogenic gas bubbles on water ﬂow through poorly
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Tokida, T., Miyazaki, T, Mizoguchi, M. and Seki, K.
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Journal of the Japanese Societyof
Soil Physics
March ῍ῌῌ῎

No. 30Contents

Foreword ῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌH. NAGANOMAῌ +./th Symposium, Japanese Society of Soil Physics“Interface Science and Measurement in Soil Physics”
Reviews
E#ects of Structural Fe Oxidation State on Physical-chemical Properties of Smectites :Evidence from Infrared SpectroscopyῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌD. HUO, C. FIALIPS, L. YAN and J.W. STUCKIῌ Point of zero charge of soil clays ῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌK. SAKURAIῌ ++My Research
Settling Pattern, Settling Rate and Zeta Potential of Marine Clay ῌῌῌῌῌF. KONDOῌ +3
Water retention, adsorption, and microstructure of allophane and imogoliteῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌJ. KARUBEῌ ,1
Lectures
Structure of Clay Paste and its Relationships to Mechanical PropertiesῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌK. FUJII and N. ISHIKAWAῌ -/Miscellaneous
Discussion in the ./th Symposium, JSSP ῌῌῌῌῌῌῌῌH. YOSHISAKO and H. INOUEῌ .Abstract of Poster session ῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌ /+Original Papers
Numerical inverse procedure to estimate soil hydraulic properties using ExcelῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌK. NOBORIOῌ /1
T-C amount in soil aggregates under di#erent pressures following substrate incorporation ῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌY. MUTO, K. WATANABE and A. SHINJOῌ 0/
Spatial Variability Analysis of Soil Properties in a Hilly Upland FieldῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌJ. KASHIWAGIῌ 1+
Frost Heave of Tetrahydrofuran Clathrate Hydrate on Porous Glass PowderῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌK. WATANABE, K. YOKOGAWA and Y. MUTOῌ 2Physical Properties of Soils as Inﬂuenced by Incorporation of Wood Bark
ῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌB. RASYID, K. FUJII and H. FUJISAKIῌ 23
Miscellaneous
Gas Sampling from Waterlogged Peat with a Newly Designed InstrumentῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌT. TOKIDA, M. MIZOGUCHI and T. MIYAZAKIῌ 31
Readers’ column ῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌK. UENOῌ+*+Book review ῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌT. HIRASAWAῌ+*Announcements ῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌ+*/Editor’s Postscript ῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌῌ+*3

Japanese Society of Soil Physics
Department of Environmental Management Engineering
Faculty of Environmental Science and Technology, Okayama University-ῌ+ῌ+ Tsushimaonaka, Okayama 1**ῌ2/-*, Japan