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444 SSSAJ: Volume 75: Number 2 • March–April 2011 Soil Sci. Soc. Am. J. 75:444–455 Posted online 16 Feb. 2011 doi:10.2136/sssaj2010.0088 Received 23 Feb. 2010. *Corresponding author (guy.richard@orleans.inra.fr). © Soil Science Society of America, 5585 Guilford Rd., Madison WI 53711 USA All rights reserved. No part of this periodical may be reproduced or transmitted in any form or by any means, electronic or mechanical, including photocopying, recording, or any information storage and retrieval system, without permission in writing from the publisher. Permission for printing and for reprinting the material contained herein has been obtained by the publisher. Clay Dispersion from Soil as a Function of Antecedent Water Potential Soil Physics The amount of clay that disperses from soil into water is of great agricultural and environmental signifi cance. Dispersion implies “zero strength”, and the soil structure can collapse with major reductions in water infi ltration rates and soil aeration status. Th erefore, clay dispersion is a cause of poor soil stability in water and this can contribute to soil erodibility and mud fl ows (Boardman, 2010). Th e presence of dispersed clay in soil can also cause the soil to become hard and non- friable when it dries as a result of cementation (Kay and Dexter, 1992). In this pa- per, we investigate the amount of RDC in soils. Readily dispersible clay is the part of the clay fraction of soils that is easily or potentially dispersible in water when small amounts of mechanical energy are applied to soil. We consider only the phenomenon of clay dispersion and not the phenomenon of slaking. However, we mention slaking briefl y here because some of the discussion on eff ects of antecedent water potentials and pretreatments is also relevant to work on clay dispersion. Slaking is the breakdown of soil into micro- aggregates (i.e., <250 μm) when it is immersed rapidly in water (Emerson, 1954; Panabokke and Quirk, 1957). Most research on soil (or aggregate) stability has involved measurements of the amount of slaking by the method of wet sieving of air-dried aggregates (e.g., Tisdall and Oades, 1980). Th is method involves the rapid wetting of the aggregates and then sieving the resulting fragments under water by Anthony R. Dexter INRA, UR0272 Science du sol Centre de Recherche d’Orléans CS40001 Ardon 45075 Orléans cedex 2, France and Institute of Soil Science and Plant Cultivation (IUNG-PIB) ul. Czartoryskich 8, 24–100 Pulawy Poland Guy Richard* INRA, UR0272 Science du sol Centre de Recherche d’Orléans CS40001 Ardon 45075 Orléans cedex 2, France Ewa A. Czyz INRAUR0272 Science du sol Centre de Recherche d’Orléans CS40001 Ardon 45075 Orléans cedex 2, France and Institute of Soil Science and Plant Cultivation (IUNG-PIB) ul. Czartoryskich 8 24–100 Pulawy, Poland and Rzeszów University Faculty of Biology and Agriculture Aleja Rejtana 16c 35–959 Rzeszów, Poland Joëlle Davy Michel Hardy Odile Duval INRA, UR0272 Science du sol Centre de Recherche d’Orléans CS40001 Ardon 45075 Orléans cedex 2, France Two standard tests for soil stability in water involve assessment of the readily dispersible clay (RDC) content of predried soil samples. It is shown that this predrying limits the applicability of the tests to very dry soils. Ways to avoid this limitation are developed. Undisturbed soil samples were collected from the 10- to 15-cm depth of arable topsoils at Villamblain and Faux Perche and from the 0- to 5-cm depth from plowed and direct-drilled plots at Boigneville. Th ese soils in north-central France were collected from the fi eld when moist (near fi eld capacity). A range of water contents and corresponding pore water potentials (or suctions h) was produced by slow drying in air. For moist soils at fi eld capacity (h = 100 hPa) the amount of RDC was large. Readily dispersible clay decreased progressively with increasing antecedent suction, h. For soil samples dried to beyond h > 10 MPa, the RDC was reduced to small values. With such intensely dried soils, rewetting for up to 2 wk did not reverse the eff ect on RDC. At h = 4500 hPa, re-equilibration to h = 100 hPa reversed the eff ect of this moderate drying on RDC. Two standard conditions (moist and dry) are proposed for measurement of clay dispersion from soil into water. Th e moist condition is relevant to soil at the end of a long, wet period (e.g., at the end of the winter in temperate climates), whereas the dry condition is relevant to dry surface crusts and dry topsoils. We conjecture that the soil “resets” during long, wet periods to values of stability and RDC at equilibrium with fi eld capacity. Experimental procedures used to determine the content of RDC in moist and dry soils are described. Abbreviations: C, total clay; CC, complexed clay; CEC, cation-exchange capacity; COC, complexed organic carbon; CT, conventional tillage; DD, direct drilling; EC, electrical conductivity; GG, Groenevelt and Grant; NCC, non-complexed clay; NCOC, non-complexed organic carbon; OC, organic carbon; RDC, readily dispersible clay; T, turbidity. Published March, 2011 SSSAJ: Volume 75: Number 2 • March–April 2011 445 the method originally described by Yoder (1936). In contrast, Chan and Mullins (1994) prepared aggregates at a range of antecedent water potentials by wetting them in a series of slow- wetting stages to prevent disturbance of the structure before they subjected them to the slaking tests. Th e RDC has been found to be sensitive to the hydraulic history (the history of dryings and rewettings) to which the soil has been subjected. Early in the 20th century, it was already observed that the amount of dispersed material was smaller when soil was initially drier (Keen and Hall, 1926). More recently Gaţe (2006) found that the content of RDC was reduced by a factor of about 20 by preliminary air-drying. Drying can occur when soil samples are stored in the laboratory and can also occur naturally in the fi eld by evaporation under the action of radiation and wind. Clay particles in moist soil when aligned in face-to-face arrangement are not normally in direct contact, but have water (actually, electrolyte solution) between them. Such arrangements of particles are able to support mechanical stresses (Smith et al., 2009). Whether solid-to-solid contact occurs when there are wedge-shaped pores and corner-to-face interactions was left an open question by Mitchell (1962) although his Fig. 5 shows an intervening water fi lm with the absence of contact. Th e thickness of these interparticle layers of water is governed by the balance between the repulsive force due to the interactions between the electrical double layers and the attractive van der Waals force (Israelachvili and Adams, 1978). Th e repulsive force depends strongly on the nature of the particle surface, adsorbed cations, and the electrolyte solution, whereas the attractive force is essentially independent of these factors (Israelachvili and Adams, 1978). As the soil dries, the electrical double layer becomes progressively thinner. When the inter- particle layer of water reduces to about a 5-nm thickness, then the surfaces fall into direct contact under the infl uence of the van der Waals forces. Th is eff ect is essentially irreversible due to the dominance of the attractive forces. Th e conditions under which soil particles come into direct mineral-mineral contact have also been discussed by Kemper et al. (1989). Th ese strong eff ects of drying have implications for the applicability of the results from standard tests of soil stability and clay dispersion that require intense drying as a pretreatment. Such tests include the Emerson test (Emerson, 1967; AS, 1997) which specifi es preliminary air-drying, and the Le Bissonnais test (Le Bissonnais, 1996; AFNOR, 2005) which specifi es preliminary drying in an oven at 40°C. Th ese predrying treatments have theadvantage of being reproducible, but questions remain about whether they are relevant to soils in the fi eld and about the consequences for subsequent parts of the test procedures. Any predrying necessarily produces a requirement for rewetting because clay dispersion and aggregate stability tests are done in water. Th e literature on this subject is huge because of lack of standardization of the methodologies. We feel that it is not appropriate to try to review the whole subject here, but rather to give some key examples to illustrate the issues. Le Bissonnais (1996) used two rates of rewetting of his dried samples: (a) “slow” wetting at a water suction, h, of 3 hPa before analysis of clay dispersion and (b) rapid wetting by immersion in water for analysis of slaking. A study of the eff ects of the suction of the source of water used for rewetting showed that for remolded and dried samples of a silty clay loam and a silt loam, the water had to be at suctions, h, larger than 24 and 30 hPa, respectively, for the formation of micro-cracks to be avoided (Dexter et al., 1984). We therefore question whether wetting at 3 hPa as used by Le Bissonnais (1996) is slow enough to prevent structural changes within samples of all soils. In contrast, Panabokke and Quirk (1957) and Angers et al. (2008), used slow wetting at a 100-hPa suction. Chan and Mullins (1994) and Kay and Dexter (1990), who required fi nal suctions of 3 and 10 hPa, respectively, fi rst wetted their dried samples at 100 hPa for 1 wk before reducing the suction to the fi nal, required value over a further week. Th is procedure prevented structural disruption in the samples. However, Th orburn et al. (1989) found that rewetting of air- dried aggregates of an intensely swelling-shrinking clay soil at 100 hPa still induced small structural changes, and therefore that wetting at an even greater suction was required for this type of soil. Nevertheless, the results of Dexter et al. (1984) presented above together with the other observations, suggest that a suction of 100 hPa is appropriate for slow wetting of most soils because it avoids structural disruption in previously dried samples. Rewetting of dried samples has also been done using mist (Kemper and Koch, 1966) to provide slow wetting and using wetting under vacuum to prevent aggregate “bursting” by entrapped air (although this does not prevent fragmentation by diff erential swelling). Th e whole subject of clay dispersion and soil stability is confounded by the absence of universally accepted standard methods for collection, storage and pretreatments of soil samples. Many laboratories have their own methods, and this usually makes comparison of results impossible. Soils that contain RDC can form surface crusts or can “hard-set” on drying (Kay and Dexter, 1992). Th ese eff ects can prevent crop emergence and can increase the energy requirement for tillage. It has been shown that the tensile strength of soil when dry is approximately proportional to the amount of RDC that was present before drying (Chan, 1989; Shanmuganathan and Oades, 1982; Watts et al., 1996). Similarly, the soil friability is smaller when more RDC is present (Shanmuganathan and Oades, 1982; Dexter and Watts, 2000). Th e content of RDC in soil has been found to be negatively correlated with a measure of soil physical quality, S (Gaţe, 2006). Soil physical quality is given by the slope of the water-retention curve at its infl ection point (when plotted as gravimetric water content against the logarithm of pore water suction). Soils with high S have been found to be more friable (Dexter, 2004), easier to till (Keller et al., 2007) and are not hard-setting (Dexter, 2004). Th ese eff ects of S on soil physical behavior are consistent with the eff ects of RDC on friability described above. Soils with high S also have lower penetration resistance (Dexter et al., 2007) and 446 SSSAJ: Volume 75: Number 2 • March–April 2011 higher saturated hydraulic conductivity (Han et al., 2008) which are further attributes of soils with good physical quality. Most previous work has been based on soil samples that are initially either dry or at (or close to) fi eld capacity. In this paper, the sensitivity of RDC to initial soil water potential over the whole range of potential from pF2 to pF6.47 is reported for the fi rst time. Here, pF is defi ned conventionally as pF = log10(h), where h is the pore water suction measured as a water column height (cm). Th is enables the behavior of soil in the laboratory and the fi eld to be better understood. It also enables problems associated with predrying (e.g., during storage or as a standard pretreatment) on the results of soil stability tests to be either avoided or taken into consideration. We propose procedures to avoid or to minimize these problems and thereby to improve the accuracy of comparisons of RDC content between soils. MATERIALS AND METHODS Soil Sampling Samples of arable soils from northern France were collected with minimum disturbance in the spring of 2007 from soils that had not been tilled in that year. Th e soils were selected to have a range of clay and OC contents. Th e Villamblain and Faux Perche soils were on private farms and were managed conventionally including plowing to a 25-cm depth. Th e Boigneville A and B soils were located at the Institut Technique des Céréales and Fourrages at Boigneville. Th e Boigneville A soil was conventionally tilled by plowing (CT) whereas the Boigneville B soil was direct-drilled (DD). Th e plots with these treatments were established in 1970. Th e Villamblain and Faux Perche soils were sampled at the 10- to 15-cm depth. Th e Boigneville soils were sampled at the 0- to 5-cm depth to obtain the higher organic carbon content near the surface in the DD treatment. All the soils were cropped annually with cereals. Th e soils were at or close to fi eld capacity at the time of sampling. Here, the term “fi eld capacity” is used in the sense of the water content to which a soil in the fi eld will drain over a period of 2 or 3 d starting from saturation. Measurements show that the pore water suction at fi eld capacity is around h = 100 hPa (corresponding to pF2). Aft er collection, the samples were kept moist in air-tight containers and were stored until required in a refrigerated room at 4°C to minimize any eff ects due to biological activity. Characterization of the Soil Solids Subsamples of the soils were analyzed by the Laboratoire d’Analyses des Sols d’Arras for particle-size distribution (by sieving and sedimentation) according to French standard NF X 31–107 and content of OC (by combustion at 1000°C) according to French standard NF ISO 10694. Correction for carbonate carbon was not necessary for these soils. Exchangeable cations were analyzed by the same laboratory using the cobaltihexamine chloride method according to French standard NF X 31–130. Full details of these experimental procedures are described at http://www.lille.inra.fr/las/methodes_d_analyse/sols/ (verifi ed 24 Jan. 2011). Th e clay fractions (<2 μm) were separated and prepared according to Robert and Tessier (1974). Th ree pretreatments were prepared: Mg–saturated with Mg; EG–saturated with Mg + ethylene glycol; and K– heated at 520°C. Th e mineralogy of the clay fractions was studied using an x-ray diff ractometer (Bruker AXS model D8 Advance, Bruker AXS Inc., Madison, WI) with a Cobalt anode giving a wavelength of 0.179 nm. Th e pretreatments enable diff erent clay minerals to be identifi ed and separated. For example, the peaks from kaolin at 0.714 and 0.357 nm disappear aft er heating to 520°C; the peak for chlorite at 1.40 nm persists aft er heating; and smectite gives a wide peak at 1.72 nm aft er the EG treatment. Th e diff ractograms were analyzed to give qualitative estimates of the diff erent clay minerals present. Water Retention Characteristics The water retention characteristics of the experimental soils were required to enable us to calculate the water potentials corresponding to diff erent soil gravimetric water contents and also as part of the soil physical characterization. We used the pF scale for water potential as defi ned above. Because of the small errors involved, we assumed that potentials based on h measured in cm H2O and in hPa are equivalent (more accurately, 1 cm H2O = 0.906 hPa at latitude 50°N, which gives an error in pF values of 0.043 for all values of h, which may be neglected in the context of this paper). Soil water retention was measured using two methods. In the range h = 10 to 15000 hPa (i.e., pF1.0–pF4.2) of pore water suction the water retention was measured on membrane and ceramic pressure plate extractors in conventional ways (e.g., Klute, 1986; Reynolds and Topp, 2008). Th e samples were collected and stored moist, were then saturated for 1 d and then drained to 12 water potentials equally spaced over the above range of pF. Separate duplicate samples were measured for each soil and each suction. Th e mean values of the resulting gravimetric water contents were used in the curve-fi tting and calculations. To extend the range of measurements to drier conditions, we equilibrated samples over saturated solutions of the salts KCl, NaCl, NaBr, MgCl2, and LiCl to produce values of relative humidity of 85.1, 75.7, 59.1, 33.1, and 11.3%, respectively at 20°C (ASTM, 2002). Th e Kelvin equation shows that these values correspond to pF values of 5.34, 5.58, 5.85, 6.18 and 6.47, respectively (Dexter and Richard, 2009). Solution saturation was maintained by keeping each solution in contact with excess, un-dissolved salt. Th e samples together with their saturated salt solutions were kept in sealed plastic boxes which were kept in larger thermally insulated boxes which were kept in a constant temperature room. Every week, the boxes were opened and the solutions stirred to destroy any fi lms that might have formed at the liquid surface. At these times, samples were taken for measurement of the gravimetric water content. When no further weight loss was occurring, it was assumed that thermodynamic equilibrium had been reached in which case the samples were ready for use. Equilibration required about 1 mo over LiCl and 3 mo over KCl. Th e choice of water retention equation was critical. We used the Groenevelt and Grant (2004) equation because it is based on thermodynamic principles (Groenevelt and Bolt, 1972) and is appropriate for systems in thermodynamic equilibrium. Th is is in contrast to other water retention equations, for example, the van Genuchten (1980) equation, which oft en predict fi nite residual water contents as pF →∞. Finite residual water contents are a characteristic of soils that have been dried by immiscible displacement (e.g., in which air displaces water) and SSSAJ: Volume 75: Number 2 • March–April 2011 447 which are not in thermodynamic equilibrium. With drying by diff usion (e.g., slow evaporation, as done here), there is no residual water content and the system is at (or close to) thermodynamic equilibrium. Water retention data over the whole range of applied potentials (1.0 < pF < 6.47) were fi tted to the Groenevelt and Grant (2004) equation: w k k k n n= − ( ) ⎛ ⎝ ⎜⎜ ⎞ ⎠ ⎟⎟− − ( ) ⎛ ⎝ ⎜⎜ ⎞ ⎠ ⎟⎟ ⎡ ⎣ ⎢ ⎢ ⎤ ⎦ ⎥ ⎥ 1 0 0 0exp exp pF pF [1] where k1, k0, and n are adjustable parameters. Th is equation states that the water content will be zero at pF0. Before we used Eq. [1], we determined the value of pF0. Th is was done using the water contents obtained by equilibrating samples of the soils over saturated salt solutions as described above. For each soil, the value of pF at which the water content is predicted to be zero was obtained by extrapolation. Th e mean of these values for the four soils was then used as pF0 in the calculations for all the soils. Equation [1] has an infl ection point (a point where the curvature = zero) at: pFi n nk n = +( ) ⎡ ⎣ ⎢ ⎤ ⎦ ⎥0 1 1 [2] w k k pF n ni n= − ( ) ⎛ ⎝ ⎜ ⎜ ⎞ ⎠ ⎟ ⎟ − − +( )⎛ ⎝ ⎜ ⎞ ⎠ ⎟ ⎡ ⎣ ⎢ ⎢ ⎤ ⎦ ⎥ ⎥ 1 0 0 1 exp exp [3] Th e curve of w plotted against pF has a slope at the infl ection point given by: d d pF w k n n nk n nk n n ( ) =− − +( )⎡ ⎣ ⎢ ⎤ ⎦ ⎥ +⎡ ⎣ ⎢ ⎤ ⎦ ⎥ +( ) 1 0 0 1 1 1 exp * [ / ] [4] Th e slope at the infl ection point when w is plotted against ln(h) has been used as an index of soil physical quality, S. In previous work, S was calculated from fi tted parameters of the van Genuchten (1980) water retention equation. Here, the slope is calculated from the fi tted parameters of the Groenevelt and Grant (2004) equation, as in Eq. [4], above. Th is procedure gives values for the slope at the infl ection point which we designate S*: S dw d pF * ln *= − ( ) ( ) 1 10 [5] In Eq. [5], the minus sign is added simply to make values of the index positive. Values of S and S* are very close and are considered to be equivalent for the purposes of this paper. Values of S > 0.035 are associated with good soil physical properties whereas values of S < 0.035 are associated with poor soil physical properties. However, the changes in behavior are progressive and there is no sudden change at S = 0.035. A fuller description of S and of the soil physical behavior associated with diff erent values of S is given in Dexter and Czyz (2007). Th e Groenevelt and Grant (GG) equation, Eq. [1], was inverted to enable the values of pore water suction, expressed as pF, corresponding to diff erent gravimetric water contents, w, to be calculated using pF n k k pF w kn = ⎛ ⎝ ⎜ ⎞ ⎠ ⎟ − − ( ) ⎛ ⎝ ⎜⎜ ⎞ ⎠ ⎟⎟− ⎡ ⎣ ⎢ ⎢ ⎤ ⎦ ⎥ ⎥ ⎧ ⎨ ⎪ ⎪⎪exp ln ln exp 1 0 0 0 1⎩⎩ ⎪ ⎪ ⎪ ⎫ ⎬ ⎪ ⎪⎪ ⎭ ⎪ ⎪ ⎪ ⎡ ⎣ ⎢ ⎢ ⎢ ⎢ ⎢ ⎢ ⎤ ⎦ ⎥ ⎥ ⎥ ⎥ ⎥ ⎥ [6] Th e GG equation is appropriate for all soil-water systems that are in thermodynamic equilibrium irrespective of whether equilibrium has been attained through convective or diff usive movement of water (e.g., evaporative drying). We therefore used the GG equation for all calculations in this paper. Estimation of the Specifi c Surface Areas Th e specifi c surface areas of the soils were estimated by two methods. Th e fi rst was the method of described in Kutilek and Nielsen (1994). In this method, the equilibrium gravimetric water content, wm, at a relative humidity of 20% is related to the specifi c surface area, Am, by Am = 3160wm, m2 g−1 [7] Th e second was based on the correlation between Am and the cation exchange capacity (CEC) that was obtained by Bruand and Tessier (2000) using data measured on 31 horizons of French soils. Th ey measured Am of the clay fraction by N adsorption. Th e regression equation given in their Fig. 1 can be inverted and rescaled to give: Am = 2.13 CEC + 3.19, m2 g−1, r2 = 0.85 [8] where the CEC values are in cmol kg−1 as in our Table 2. Although Bruand and Tessier (2000) measured only the clay fraction, we applied Eq. [10] to the whole soil on the assumption that most of the surface area and the CEC of the whole soil are associated with the clay fraction. Slow Drying Experiments We needed to dry soil samples from fi eld capacity (pF2) to the whole range of water potentials from pF2 to air-dry which is around pF6. Th e middle part of this range, from about pF4.2 to pF5.2 is diffi cult to produce using normal experimental techniques. Porous ceramic plates are reaching the limits of their eff ectiveness at around pF4.2 (Gee et al., 2002; Cresswell et al., 2008). Equilibration over osmotic solutions is diffi cult for values of pF < 5.3 because it requires very accurate temperature control to avoid problems with condensation and takes an excessively long time. For these reasons, we decided to produce the whole range of water potentials by slow-drying of initially moist soil samples in air. Subsamples ofthe soils of about 20 g were crumbled by hand without shearing into 1- to 3-mm aggregates and were placed in plastic bags that had numerous small pin-holes in them. Th ese bags with soil were placed on horizontal drying racks in the laboratory at 22°C. Th e subsamples dried very slowly by loss of water vapor through the pin-holes. It was assumed that water would redistribute relatively rapidly in the vapor phase within the bags to give a relatively uniform water potential or pF. If the redistribution within the bags is more rapid than water loss from the bags, then the soil within the bags will be in quasi-equilibrium. Th e bags were weighed every day, and from knowledge of the initial mass of moist soil in each bag and its initial water content, it was possible to calculate 448 SSSAJ: Volume 75: Number 2 • March–April 2011 the water content of the soil at that time. From the water content and the water retention curve, it was possible to calculate the pF of the water remaining in the soil. Th is slow drying of soil from fi eld capacity (about pF2) to air-dry (about pF6) took about 4 wk. We required a range of pF values for each soil. Th erefore, we calculated the mass that each soil + bag should have to give the required values of pF. When a soil had dried so that the approximate required mass of soil + bag had been attained, then the soil samples were taken from the bags. About one-half was used for measurement of the gravimetric water content in two replicates and the other half was used for measurement of RDC and electrical conductivity (EC). Measurement of Readily dispersible Clay Th e content of RDC was measured at the diff erent water contents produced by slow drying of initially moist soil as described above. Readily dispersible clay was measured by the amount of white light scattered by the colloidal particles (mostly clay) in aqueous suspension using a turbidimeter which measures the turbidity, T (NTU/[g L−1]) of a suspension; T is proportional to the concentration of the particles in suspension. Th e principles and limitations of turbidity measurement are discussed by Sadar (1998). Th e method used in this work for measurement of the RDC content of soils is based on that described previously (Czyz et al., 2002; Czyz and Dexter, 2008). It was further developed and improved for this work and is described in full in the Appendix. Th e EC of the solutions obtained aft er immersion of dried soil in 125 mL of deionized water was measured with a Hanna model HI99300 conductivity meter (Hanna Instruments, Woonsocket, RI) that was calibrated periodically with standard solutions. Th e reversibility of the eff ects of drying on RDC was investigated in two ways as follows. Method 1: low intensity drying with slow rewetting. Samples of the moist soil were dried on ceramic pressure plate extractors to h = 4500 hPa (or pF3.65) for 4 d. Th ey were then taken from the pressure plate and wetted to h = 10 hPa for 2 d and then dried to “fi eld capacity” at h = 100 hPa (or pF2) for 4 d. Th e purpose of the wetting to 10 hPa before drying to 100 hPa was to ensure that the samples were on the “drying limb” of the water characteristic curve. Method 2: high intensity drying followed by rapid rewetting In the case of the samples that had been dried to h > 10 MPa (pF > 5), the test of reversibility of the eff ect of drying was to rapidly rewet the samples by immersion and to leave the samples in water for up to 2 wk. Soil Drying in the Field To relate our laboratory studies above to reality, we sought to answer the question “how dry do soils become in the fi eld”? Although we did not have data for the French soils described above, we had data for the top 2 cm of an arable sandy loam at the Waite Institute in Adelaide, South Australia. Th e climate in South Australia is Mediterranean with cool, wet winters, and hot, dry summers. Th ese measurements were made in 1981 by the fi rst author and have not been published previously. Forty samples were collected each working day (20 at 09.00 h and 20 at 15.00 h) and the gravimetric water contents were measured. Th is was continued for a period of about 9 mo fi nishing on December 18. It should be noted that Australia is in the southern hemisphere, and therefore that mid-summer occurs on December 21. Th e mean gravimetric water content at each sampling time was calculated. Th e water retention characteristic was measured using sintered- glass funnels with hanging water columns and with ceramic pressure plate extractors. Th e pF values corresponding to the measured fi eld water contents were calculated with Eq. [6] using the value pF0 measured as described and were ranked within each of the months September-December. RESULTS AND DISCUSSION Soil Characteristics Th e compositions of the experimental soils are given in Table 1. Information about the clay mineralogy and exchangeable cations is given in Table 2 which shows that calcium-saturated illite and chlorite were the principal clay fractions. Th e amounts of complexed and non-complexed clay and OCwere estimated as described in Dexter et al. (2008) and are presented in Table 3. Th e water retention characteristics obtained by drying over saturated salt solutions are shown in Fig. 1. It can be seen that there is very little eff ect of organic matter on water retention Fig. 1. Water retention for values of pF > 5.34 as obtained by equilibration of samples over saturated salt solutions. Table 1. Compositions of the experimental soils together with the USDA texture classes, contents of organic carbon (OC) and the measured values of pH. Soil Villamblain Boigneville A (CT) Boigenville B (DD) Faux Perche (9P55) clay, g kg−1 331 260 236 118 fi ne silt 326 285 299 342 coarse silt 326 375 387 487 fi ne sand 13 63 61 30 coarse sand 4 17 17 23 USDA texture class† si cl l si l si l si OC, g kg−1 13.0 13.3 28.9 12.1 pH 7.90 6.33 4.86 7.91 † si = silt, cl = clay, l = loam. SSSAJ: Volume 75: Number 2 • March–April 2011 449 for pF > 5.3 as shown by the comparison of the results for the Boigneville A and B soils. Th e results shown in Fig. 1 were fi tted to Eq. [9] and the resulting parameters are given in Table 4. w B C pF= + ( ) , kg kg−1 [9] Equation [9] is not applicable at saturation (h = 0), where the pF = −∞, but gives a good fi t over the experimental range 5.34 < pF < 6.47. As can be seen in Fig. 1 and can be calculated from Eq. [9] with the appropriate coeffi cients, extrapolation of these results gives the prediction that the water content, w, would be zero at pF = 6.65 ± 0.02 for these soils. Th is is the value that we used for pF0 in Eq. [1], [3], and [6]. Th e fi tted parameters of the Groenevelt and Grant (2004) water retention equation for the four soils are given in Table 5. As an example, the 17-point water-retention data for the Boigneville A soil are shown in Fig. 2 together with the smooth curves corresponding to the fi tted Groenevelt and Grant (GG) water retention equation described above. Th e results and fi ts for the other three soils were equally good. Th e specifi c surface areas calculated by the two methods are given in Table 6. It can be seen that the results are similar except for the Boigneville B soil that has a large content of organic matter. Th ese values put our soils into Class II of Dogan et al. (2007). Amounts of Readily Dispersible Clay Th e amounts of RDC obtained by the slow drying treatment and the application of Eq. [6] are shown in Fig. 3. It can be seen that RDC decreases progressively with increasing antecedent pF reaching approximately constant or asymptotic values for pF > 5, approximately. Th e RDC data for the slowly air-dried samples were fi tted to RDC = k + Eexp[-F(pF-2)], NTU/(g L−1) [10] where k, E, and F are adjustable coeffi cients. Th e term X = (pF– 2) was chosen so that X would have the value 0 at fi eld capacity (heretaken to be h = 100 hPa). At fi eld capacity, Eq. [10] shows that RDCfc = k + E whereas the asymptotic value of RDC for high values of pF is given by k. It should be noted that for saturated soil, for which h = 0, the pF value is −∞. Th e fi tted parameters for Eq.[10] are given in Table 7 which shows that the value of the exponent F is similar for all the soils with an approximate average value of F = 1. In other words, an increase in the initial pF of the soil water by 1 reduces the amount of RDC by a factor of 1/e = 0.37, approximately. Th is is in spite of the diff erences in the compositions of the four experimental soils. For our experimental soils, Eq. [10] can be approximated by RDC pF RDC RDC RDC edry fc dry pF( ) ( )− − ⎡ ⎣ ⎢ ⎢ ⎤ ⎦ ⎥ ⎥ = − −2 [11] Table 2. Mineralogy of the clay fraction and exchangeable cations in the experimental soils. Soil Villamblain Boigneville A (CT) Boigneville B (DD) Faux Perche (9P55) Mineralogy illite low dominant dominant some kaolinite medium high high high vermiculite medium some some some smectite medium low low none chlorite high very low very low medium quarts very low very low very low very low Exchangeable cations Ca, cmol kg−1 18.6 13.2 6.84 9.50 Mg, cmol kg−1 0.86 0.73 0.60 0.44 K, cmol kg−1 0.59 0.71 1.09 0.43 Na, cmol kg−1 0.060 0.038 0.042 0.024 CEC, cmol kg−1 20.1 14.7 9.9 9.3 Table 3. Measured amounts of clay (C) and organic carbon (OC) with estimated amounts of complexed clay (CC), non-complexed clay (NCC), complexed organic carbon (COC) and non-complexed organic carbon (NCOC) in the experimental soils. Soil Villamblain Boigneville A (CT) Boigneville B (DD) Faux Perche (9P55) C, g kg−1 331 260 236 118 OC, g kg−1 13.0 13.3 28.9 12.1 CC, g kg−1 130 133 236 118 NCC, g kg−1 201 127 0 0 COC, g kg−1 13.0 13.3 23.6 11.8 NCOC, g kg−1 0.0 0.0 5.3 0.3 Table 4. Parameters of the water retention equation (Eq. [9]) for soils dried over saturated salt solutions to values of pF in the range 5.34 < pF < 6.47. Also given are the values of the intercept, pF0, at which the water content, w, is predicted to be zero. Soil Villamblain Boigneville A (CT) Boigneville B (DD) Faux Perche (9P55) B, kg kg−1 0.3567 0.2650 0.2475 0.1190 C, kg kg−1 -0.05395 −0.03987 −0.03713 −0.01780 r2 0.997 0.986 0.998 0.990 pF0 6.61 6.65 6.66 6.68 Table 5. Fitted values of the parameters of the Groenevelt and Grant (GG) water retention equations and of the index of soil physical quality, S*. Soil Villamblain Boigneville A (CT) Boigneville B (DD) Faux Perche (9P55) k1, kg kg−1 2.4224 0.6508 0.4338 0.2765 k0 7.2667 6.8770 12.0482 80.1106 n 0.6459 1.0453 2.0658 3.9006 S* 0.0267 0.0245 0.0475 0.0576 450 SSSAJ: Volume 75: Number 2 • March–April 2011 for values of pF > 2. We suggest that Eq. [11], together with values of RDCfc and RDCdry measured as described in the Appendix, provides estimates of the content of RDC(pF) at any value of pF for any soil that has not been drier than pF since the last long wet period. However, Eq. [11] needs to be tested on a wider range of soils than were used in this study. We suggest that diff erent soils should be compared at pF2. However, soils are oft en collected in the fi eld when drier than this. In this case, we suggest that the soil samples be wetted slowly at h = 100 hPa for 1 wk before measurement of RDCfc. From the values given in Table 7, it is possible to calculate the ratio (k+E)/k which is the ratio of RDC from soil at fi eld capacity to that from intensively dried soil. Th is ratio has values of 28, 27, 10, and 22 for the Villamblain, Boigneville A, Boigneville B, and Faux-Perche soils, respectively. Th ese values are similar to those found for Polish soils by Gaţe (2006). Th e Polish soils had smaller contents of clay, on average, than the French soils used here. Th e smaller value of this ratio for the Boigneville B soil is mainly because of the eff ect of organic matter in reducing the dispersion of clay from the soil when moist (i.e., at fi eld capacity). Values of RDCfc calculated as above may be compared with the measured values of total clay (C) and estimates of non-complexed clay, NCC, given in Table 3. Th is comparison shows that when all of the clay is complexed with organic matter, then the amount of RDCfc is close to zero. Also given in Table 3 are the values of non- complexed organic carbon, NCOC, calculated as described by Dexter et al. (2008). Th e van der Waals force decreases as the sixth power of distance from a surface whereas the pore water suction between parallel plates (such as clay plates) decreases as the fi rst power of the plate separation (Kutilek and Nielson, 1994). Th erefore, we can use estimates of pore water suction down to 5 nm spacing. Th e capillarity equation for parallel plates (Kutilek and Nielson, 1994) shows that the pore water suction at this spacing is 28 MPa which corresponds to pF5.4. However, the clay plates are not parallel (Bruand and Zimmer, 1992), so we shall make an informed guess that the clay particle surfaces begin to fall into solid-solid contact at pF5.0. For soil wetter than this, we hypothesize that the eff ect of drying on RDC is reversible whereas for soil drier than this, we hypothesize that the eff ect of drying is irreversible. Th is estimated value of pF5.0 is bracketted nicely by the values of pF3.65 at which we found reversibility and pF6.0 at which we found irreversibility. Th e exact value of pF at which the eff ect on RDC becomes irreversible remains unknown. Figure 4 shows the values of RDC for soil samples that had been equilibrated over saturated salt solutions. Th ese results Fig. 2. Fit of the Groenevelt and Grant (GG) water retention equation for the Boigneville A soil. Experimental points are as follows: circles are from membrane and ceramic pressure plate extractors, and squares are from equilibration over saturated salt solutions. Table 6. Estimates of the specifi c surface area (m2 g−1) for the whole soil as estimated by water adsorption at pF6.34 and cation exchange capacity (CEC). Soil Villamblain Boigneville A (CT) Boigneville B (DD) Faux Perche (9P55) (a) water adsorption 51.9 44.0 43.5 22.0 (b) CEC method 46.0 34.5 24.3 23.0 Fig. 3. Amount of readily dispersible clay, RDC [NTU/(g L−1)], as a function of antecedent water potential (expressed as X = pF-2 where the origin, X = 0, has been shifted to correspond to fi eld capacity, pF2). Note that all values of pF were obtained using Eq. [6]. SSSAJ: Volume 75: Number 2 • March–April 2011 451 show a slight increase in RDC with increasing pF in the range 5.34 < pF < 6.47. Th is eff ect is diff erent from that expected from Eq. [10]. We conjecture that this may be due to greater eff ects when drier soil is rewetted (c.f. heat of wetting). Comparison of the results in Fig. 3 and 4 shows that there must be some value of pF at which the amount of RDC is minimum. Th e results from the experiments reported here do not allow us to determine this value with any accuracy. Th e values of RDC at high pF obtained by the air-drying method (RDCAD) were always larger than the values obtained by drying over saturated salt solutions (RDCSS). Th e average diff erence, ΔRDC was 0.04 NTU/(g L−1). We conjecture that this diff erence may be due to non-uniform drying of the soil in the perforated plastic bags. Th is will need to be tested in future experimental work. However, this small value of ΔRDC does not aff ect the conclusions from this work. When soil was dried from pF2 to pF3.65, and then slowly rewetted to pF2 on a sand table (Method 1, described above), then the original value of RDC was obtained (100% regain) which is consistent with the discussion above. Electrical Conductivity Th e values of EC of the solutions produced during the RDC tests are shown in Fig. 5. It can be seen that for the Villamblain and Faux Perche soils the resulting EC is greaterwhen the soil is initially drier (with correlations of r = 0.56, p < 0.0001 and r = 0.95, p < 0.0001 for these soils, respectively). Th is is consistent with the idea that when soil is initially drier, there will be greater disruption of the system on rewetting, for example by increased heat of wetting (Prunty and Bell, 2005). For the Boigneville A soils, there is no signifi cant correlation (r = 0.074, p = 0.77). In contrast, the Boigneville B soil shows a negative correlation (r = −0.60, p = 0.0089). Th is latter soil has a high content of organic matter and a content of NCOC of 5.3 g kg−1 as shown in Table 3. We can hypothesize that organic matter protects the system against the eff ects of rapid rewetting. Th is may be because the organic matter is more hydrophobic when the soil is drier (Bayer and Schaumann, 2007) and that greater hydrophobicity leads to slower rewetting (Doerr et al., 2000; Hallett et al., 2004). Th ese observations, although preliminary, enable us to propose an hypothesis for future testing: that is, that d(EC)/d(pF) is negative when NCOC is present. To learn more about this EC phenomenon, we analyzed the supernatant in the 30-mL turbidimeter cells aft er measurement of turbidity for the cations Al, Ca, Fe, K, Mg, and Na. We found that the EC was strongly correlated with the concentrations of Ca and K in solution aft er the rapid wetting as shown in Eq. [12]. Table 7. Values of the parameters of Eq. [10] giving RDC [NTU/(g L−1)] as a function of antecedent water potential in the range 2 < pF < 6. Soil Villamblain Boigneville A (CT) Boigneville B (DD) Faux Perche (9P55) K, NTU/(g L−1) 0.143 0.134 0.089 0.157 E, NTU/(g L−1) 3.906 3.499 0.838 3.339 F 1.128 0.719 1.017 1.031 r2 0.984 0.978 0.941 - Fig. 4. Amount of readily dispersible clay, RDC [NTU/(g L−1)], as a function of antecedent water potential (expressed as pF) for values of pF > 5.34. Samples were equilibrated over saturated salt solutions. Fig. 5. Electrical conductivity (EC) of the suspension after adding soil that had been dried to different values of antecedent water potential (expressed as X = pF-2 where the origin, X = 0, has been shifted to correspond to fi eld capacity, pF2). Note that all values of pF were obtained using Eq. [6]. 452 SSSAJ: Volume 75: Number 2 • March–April 2011 EC = 0.3 + 4.40[Ca] + 5.02[K], r2 = 0.975 [12] (±3.2) (±0.43) (±0.48) where EC is in μS cm−1 and the concentrations [Ca] and [K], are in mg L−1. Th ere was no statistically signifi cant correlation with the other cations analyzed. Further work with a wider range of soils is needed to elucidate the mechanisms and processes that occur during rewetting of soil samples. However, the measurement of EC does seem to be one method of gaining useful information. In additional experiments, not described here, we showed that the changes in the electrolyte composition and concentration following immersion of dried versus moist soil had no signifi cant eff ect on the amounts of dispersed clay in suspension. Th e water contents measured in the fi eld in South Australia were converted into pF values using Eq. [7] using the same value of pF0 = 6.65. Th e results are shown in Fig. 6 where it can be seen that soil can become dry enough under natural conditions to undergo the eff ects described above. It is likely that the soil will become even drier during January and February, although this was not measured. Th e results presented above can be considered in relation to annual cycles of tillage and climate. For arable (i.e., plowed) soils the tilled layer becomes mixed every year. It can then be argued that over a period of many years, all of the soil in the arable layer will have been at the surface and will have been subjected to intense drying and rewetting many times. A logical conclusion from this is that all of the clay in the arable layer will have become stabilized and will have a low content of RDC as described above. If the depth of plowing is P cm and the depth to which an intensity of drying suffi cient for the “irreversible” changes discussed above to occur is D cm, then we can model this very simply. We have done this with values of D/P = 0.05, 0.1 and 0.2 and obtained the results that 90% of the change will have occurred aft er 45, 21, and 9 yr, respectively. Our experimental results for moist arable soils show that there is a lot of RDC present at the end of a long, wet period such as the winter in temperate climates. Th erefore, the changes induced by drying and rewetting that we have reported above cannot be irreversible. Similar results were obtained with the tensile strength of arable soils in South Australia which has a Mediterranean climate (Kay and Dexter, 1992). At the end of the long, wet winter, the tensile strength of the air-dried soil samples was found to be high. Th is was attributed to the cementation produced by the particles of dispersed clay as the soil dried. However, this value reduced linearly with increasing number of natural wetting/drying events during the summer. Th ese wetting/drying events were easily countable during the predominantly hot, dry summers in that area. Each year, the tensile strength started from a high value again showing that during the long, wet winter of approximately 6 mo duration, the clay had dispersed and could again contribute to cementation when the soil dried. We have not yet discovered either the mechanism or the dynamics of this “re-setting”. It seems that the soil “resets” its internal clock during long, wet periods (e.g., winter in temperate climates) as described by Kay and Dexter (1992). Th e evidence suggests that this resetting occurs in spite of the surfaces “falling into direct contact, which is essentially irreversibly”, as described in the introduction. Th is “resetting” clearly needs to be the subject of future research. CONCLUSIONS Th e experiments reported above involved the eff ects of drying of initially moist soil by vapor diff usion (evaporation). Th is is conceptually and physically diff erent from the immiscible displacement method of soil drying (or dewatering) that is normally done in the laboratory on pressure plate extractors for determination of the water retention characteristics. We have shown that water contents resulting from equilibration through vapor diff usion are well-described over the whole range of pF by the Groenevelt and Grant (2004) equation. We found the value of the term pF0 in this equation to be pF6.65 ± 0.02. Readily dispersible clay was found to decrease from RDCfc at fi eld capacity (pF2) to a minimum of RDCdry under air-dry conditions (typically pF6). Th is decrease was exponential (to within experimental error) with an increase in the initial pF of the soil water by 1 reducing the amount of RDC by a factor of 1/e = 0.37, approximately. Equation [11] enables the eff ect of predrying to diff erent values of pF on the content of RDC of the four experimental soils to be estimated. Diff erences between soils aff ect mainly the term RDCfc and this illustrates the importance of measuring the properties of moist soil that has not been dried. Th e tests of soil stability (including clay dispersion) proposed by Emerson (1967) and Le Bissonnais (1996) form the bases for Australian (Australian Standard, 1997) and French (Association Française de Normalisation, 2005) standard methods. Both of these tests involve a soil pretreatment that includes intensive drying of the soil. Th e Emerson test requires air-drying whereas, the Le Bissonnais test requires drying in an oven at 40°C. Under Fig. 6. Dryness of the top 2 cm of soil in the fi eld in South Australia. The curves show, for the months September–December 1981, the proportions of the time for which the soil was drier than the corresponding values of pF. SSSAJ: Volume 75: Number 2 • March–April 2011 453 typical laboratory conditions,with an air temperature of 22°C and a relative humidity of 50%, these procedures produce intensities of drying of pF5.98 and pF6.40, respectively (Dexter and Richard, 2009). We have shown that this fi rst value can be reached in the fi eld whereas this latter value is drier than was found for the top 2 cm of soil in December (mid-summer) in South Australia (Fig. 6). Such high intensities of predrying are not appropriate for studies of clay dispersion from soils that are moist because the drying pretreatment changes the dispersibility of the clay fraction irreversibly (or at least for periods of >2 wk). Th e Emerson (1967) and Le Bissonnais (1996) tests give only measures of the clay dispersion from soil that has been intensely dried before rewetting (equivalent to k in Eq. [10] and Table 7). We have shown that the dispersion of clay from initially moist soils is much greater and can be measured accurately by the methods described in this paper. We believe that an adequate understanding of clay dispersion from soil requires the analysis of initially moist as well as dried samples. Th is conclusion is consistent with the recommendation given by Pojasok and Kay (1990) and Kjaergaard et al. (2004) that soil samples should be collected when they are at fi eld capacity and should be kept moist during storage. We suggest that the RDC content of diff erent soils should be compared at pF2. However, when soils are collected drier than this, we suggest that the soil samples be wetted slowly at h = 100 hPa for 1 wk before measurement of RDCfc. Alternatively, Eq. [11] may be used to estimate the amount of RDC that may be expected. A simple mixing theory suggests that all of the arable layer of the soil should have been intensively dried and rapidly rewetted many times in the past. Th erefore, we might expect that there would be a negligible content of RDC in the arable layer. Th e fact that this is not so, suggests that the eff ect of intensive drying and rewetting is not irreversible but perhaps only slowly reversible. However, in arable soils there is also an annual input of mechanical energy from tillage operations that may contribute toward reversal of the eff ect of drying (Watts et al., 1996). Th e work described above on the eff ects of drying on soil physical properties leads to the proposal for having two pretreatments for determination of RDC and soil stability in general: one for soils that are dry in the fi eld and one for soils that are moist and that have not dried since the previous long, wet period. Th ese give indications of the instability of soils at diff erent times of year. Th e experimental procedures used for measurement of RDC are described in the Appendix. We support strongly the fi nal statement of Angers et al. (2008) which we simplify slightly as follows: “Because variations in sampling, storage, and pretreatment aff ect the results, all steps in the analysis should be described in great detail when research results are published”. APPENDIX Experimental Procedure used to Determine the Content of Readily Dispersible Clay in Moist and Dry Soil A. Types of Test We describe two types of test:Test 1. For moist soil to determine the content of RDC at fi eld capacity, RDCfc, where fi eld capacity is de- fi ned as a pore water suction of h = 100 cm H2O = pF2 ≈ 98.6 hPa. Th is is relevant to erosion of soil or transport of colloids in the spring and during snow melt, etc. To determine RDCfc the soil must be ini- tially wetter than a suction of 0.45 MPa, and must not have been drier than this on any occasion since the last long wet period (e.g., winter in temperate climates). Test 2. For dry soil to determine RDCdry, which is relevant to the response of soil to rapid wetting in dry periods that may occur aft er seed- ing or in summer thunderstorms, etc. Th is test involves conditions simi- lar to those used in the Australian (AS, 1997) and French (Association Française de Normalisation, 2005) tests of soil stability. To determine RDCdry the soil can be collected at any degree of wetness. B. Sample Collection and Storage Soil samples must be taken from the fi eld with the minimum dis- turbance possible. Th e sampling strategy (depths and spatial distribu- tion of samples) will depend on the hypotheses to be tested. We nor- mally take 5 or 10 replicates depending on the heterogeneity of the soil and on the desired accuracy of the mean values. Th e samples should be placed in air-tight containers for transport to the laboratory. Th e sam- ples should be placed in the shade and kept as cool as possible. At the laboratory, put the samples in hermetically sealed containers and store in a constant temperature room at 4°C until required. C. Standardization of Initial Conditions For Test 1, samples for RDCfc should be placed on a sand table adjusted to a suction of h = 100 cm H2O. Th ey should be left for 4 d for the water and the soil to equilibrate. For Test 2, samples for RDCdry should be dried in a convection oven at 40°C for 2 d. With average labo- ratory conditions of air temperature of 20°C and relative humidity of 50%, this produces an equilibrium water potential of pF6.35 (Dexter and Richard, 2009). Aft er equilibration, the samples should be moved rapidly to a vac- uum desiccator (without desiccant) to prevent exchanges of water with the atmosphere (and to cool to room temperature in the case of Test 2). Samples for the RDCfc and RDCdry tests must not be placed together in the same desiccator. D. Equipment A turbidimeter is required to measure the amount of colloids (mostly clay) in suspension. It must measure the turbidity of suspen- sions from the amount of white light scattered. It should not be sensitive to solution color (we used a Hach model 2100AN turbidimeter, Hach Company, Loveland, CO). Also required are: a laboratory balance that weighs to 3-digit accuracy (that is to 1 mg), laboratory convection oven to work at 105°C, and a pi- pette with the capacity of the glass turbidimeter cells (30 mL in our case). 454 SSSAJ: Volume 75: Number 2 • March–April 2011 Clean plastic bottles with large-opening screw tops, and Vb = 150 mL capacity. We use about 100 of these. Each bottle must be numbered and calibrated by adding 125 mL of water (most easily determined by weighing on a balance) and drawing a horizontal line at the surface of added water. Th ese lines then enable water to be added to make 125 mL of suspension in the tests. Th e importance of having accurate volumes is because the energy input to the suspension depends strongly on the volume of the air bubble in the bottles. In this example, the volume of air is Va = 150 – 125 = 25 mL). A large, clean plastic container to hold a supply (e.g., 20 L) of dis- tilled or deionized water. Th is water must be allowed to stand in the laboratory for several hours before use for two reasons. First, it must be equilibrated at the laboratory temperature (20–22°C); and second, be- cause dissolved gases may come out of solution producing microbubbles that can aff ect the turbidity readings. Th ese microbubbles may be invis- ible to the naked eye. E. Measurement Procedure First, determine the gravimetric water content, w, kg kg−1 or g g−1, of a subsample of the soil by oven-drying at 105°C. While this is drying, weigh 4 to 5 g of moist soil (mass = Mm) and place it in one of the cali- brated plastic bottles. Th en, add distilled or deionized water to make the volume of the soil + water in the bottle up to 125 mL. Screw the plastic top on the bottle. Record the time, T1. Aft er 1 h (time = T2 = T1 + 1 h), agitate the soil + water in a stan- dard way by holding the bottle in one hand and inverting it four times. Each inversion should take about 0.5 s. Th en loosen the plastic bottle top so that it can be removed later without disturbing the suspension or the sediment in the bottle. Leave the bottle to stand for 18 h (time = T3 = T2 + 18h), without any disturbance for sedimentation to proceed at room temperature (20–22°C). Th is time of 18 h is convenient because it enables samples to be prepared in the aft ernoon and measured the next morning. Aft er the 18 h wait, take 30 mL of suspension from the center of the bottle with the pipette without disturbing the suspension or the sed- iment in the bottle. Put the collected suspension in the glass turbidim- eter cell by running it down the inside of the cell to avoid the formation of bubbles that can aff ect the turbidity reading. Measure the turbidity in units of NTU (Nephelometric Turbidity Units). Th is value of turbidity is a measure of the colloidal content (mostly clay) because the larger min- eral particles will have sedimented from the initial suspension. F. Calculations Calculate the mass of dry soil particles, Md, in the sample from the moist mass, Mm, and the gravimetric water content, w, using Md = Mm/(1+w) where Md and Mm are in g. Normalize the measured turbidity to take account of the eff ects of diff erent initial water contents and diff erent initial masses of moist soil: Normalized turbidity = NTU/(g L−1) where g L−1 is the mass concentration of soil particles in the suspension. For the example given above, we have: Normalized turbidity = NTU/(1000*Md/125) G. Relating NTU to Absolute Clay Contents If the suspension used in the turbidimeter cell is dried and weighed (this will require a 4 or 5 digit balance), then the mass concentration of clay giving a certain turbidimeter reading can be calculated directly. Alternatively, if the agitation by four inversions in Section E, above, is replaced by complete dispersion as is done in standard methods of par- ticle-size analysis (e.g., involving chemical dispersion with sodium meta- phosphate, and intense mechanical dispersion using ultrasound and/or intense stirring), then the NTU value corresponding to the known total clay content of the soil may be determined. Knowledge of this enables the clay contents corresponding to other NTU values to be calculated. A fac- tor K may be defi ned which, when multiplied by the turbidity in NTU/ (gL−1) gives the amount of dispersed clay in g (100 g soil)−1. Calibration factors, obtained as described above, that relate tur- bidimeter readings to absolute amounts of clay in suspension diff er slightly between soils. Th is is because the diff erent clay minerals present may have diff erent particle shapes, size distributions and diff erent light- scattering properties. H. Reporting of Results Th e content of RDC can be reported either in terms of normalized turbidity units: RDCfc = NTU/(g L−1) or RDCdry = NTU/(g L−1), as appropriate or in terms of absolute clay contents RDCfc = g (100 g soil)−1 or RDCdry = g (100 g soil)−1, as appropriate. ACKNOWLEDGMENTS A. R. Dexter thanks the leSTUDIUM Institute of Advanced Studies in Orléans, France for the fi nancial support that made his work in INRA, Orléans possible. Th e authors also thank the INRA Environment and Agriculture Division for the award of a “Projet innovant” and the French Agency for the Environment and Energy Management (ADEME) for the award of a grant. Dr. N.R.A. Bird of Rothamsted Research is thanked for mathematical assistance. Olivier Josière is thanked for his help with the mineralogical tests. REFERENCES Association Française de Normalisation. 2005. Qualité du sol. Mesure de la stabilité d’agrégats de sols pour l’évaluation de la sensibilité à la battance et à l’érosion hydrique. 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