11
Research Paper Comparison between grain-size analyses using laser diffraction and sedimentation methods C. Di Stefano, V. Ferro*, S. Mirabile Dipartimento di Ingegneria e tecnologie Agro-Forestali, Universita ` di Palermo, Viale delle Scienze, 9018 Palerrmo, Italy article info Article history: Received 3 December 2009 Received in revised form 15 March 2010 Accepted 18 March 2010 A comparison between laser diffraction method (LDM) and the sieve-hydrometer method (SHM) was carried out for 228 soil samples representing a different texture classification sampled in a Sicilian basin. The analysis demonstrated that the sand content measured by SHM can be assumed equal to that determined by LDM technique, while the clay fraction measured by LDM was lower than that measured by the SHM. A set of equations to transform LDM results to SHM results was proposed. The influence of the LDM measure- ments of clay on the estimated percentage of silt þ very fine sand particles (particle diameter ranging from 0.002 mm to 0.1 mm), which is useful for estimating soil erodibility, was also studied. ª 2010 IAgrE. Published by Elsevier Ltd. All rights reserved. 1. Introduction Particle-size distributions (PSDs) are fundamental physical properties of soil and are typically presented as the percentage of the total dry weight of soil occupied by a given size fraction. This property is commonly used for soil classification and for the estimation of some hydraulic properties (Campbell & Shiozawa, 1992). Over recent decades, various new methods for grain-size analysis have been developed. These new methods, (electro- resistance particle counting, time of transition, laser diffrac- tion (LD), optical determination of the PSD using image analysis) (Goossens, 2008; McCave & Syvitski, 1991) generally have the advantage of covering a wide range of grain sizes, and rapidly analysing small samples. Particles of sand size (0.05e2.00 mm) are usually deter- mined using sieving. The sieve defines a particle diameter as the length of the side of a square hole through which the particle can just pass (Allen, 1990). Finer particles are usually determined by classical sedimentation methods such as hydrometer or pipette (Gee & Bauder, 1986). Sieving combined with hydrometer method (SHM) has been adopted as an international standard to determine quantitatively the PSD of soils (Allen, 1990; Cooper, Haverland, Hendricks, & Knisel, 1984). With similar pretreatment techniques, the pipette method (PM) and hydrometer method (HM) - give comparable results (Liu, Odell, Etter, & Thornburn, 1966; Walter, Hallberg, & Fenton, 1978); however the PM requires that clay and silt fractions (<0.05 mm) are separated from the sand fraction using wet sieving. Sedimentation methods are time consuming, especially for the determination of the particles having a size less than 2 mm, since they require relatively large samples (10e20 g for the pipette and 50 g for the hydrometer). They also give unreliable results for particles 1 mm because of the effect of Brownian motion on the rate of sedimentation. A particle diameter obtained by the laser diffraction method (LDM) is equivalent to that of a sphere giving the same diffraction as the particles. A laser diffraction particle size analyser “sees” the particle as a two-dimensional object and it gives its grain size as a function of the cross-sectional area of the particle. * Corresponding author. E-mail address: [email protected] (V. Ferro). Available at www.sciencedirect.com journal homepage: www.elsevier.com/locate/issn/15375110 biosystems engineering 106 (2010) 205 e215 1537-5110/$ e see front matter ª 2010 IAgrE. Published by Elsevier Ltd. All rights reserved. doi:10.1016/j.biosystemseng.2010.03.013

Comparison between grain-size analyses using laser ... · A comparison between laser diffraction method (LDM) and the sieve-hydrometer method ... mined using sieving. The sieve defines

Embed Size (px)

Citation preview

Page 1: Comparison between grain-size analyses using laser ... · A comparison between laser diffraction method (LDM) and the sieve-hydrometer method ... mined using sieving. The sieve defines

b i o s y s t em s e ng i n e e r i n g 1 0 6 ( 2 0 1 0 ) 2 0 5e2 1 5

Avai lab le a t www.sc iencedi rec t .com

journa l homepage : www.e lsev ie r . com/ loca te / i ssn /15375110

Research Paper

Comparison between grain-size analyses using laserdiffraction and sedimentation methods

C. Di Stefano, V. Ferro*, S. Mirabile

Dipartimento di Ingegneria e tecnologie Agro-Forestali, Universita di Palermo, Viale delle Scienze, 9018 Palerrmo, Italy

a r t i c l e i n f o

Article history:

Received 3 December 2009

Received in revised form

15 March 2010

Accepted 18 March 2010

* Corresponding author.E-mail address: [email protected] (V. Ferro

1537-5110/$ e see front matter ª 2010 IAgrEdoi:10.1016/j.biosystemseng.2010.03.013

A comparison between laser diffraction method (LDM) and the sieve-hydrometer method

(SHM) was carried out for 228 soil samples representing a different texture classification

sampled in a Sicilian basin. The analysis demonstrated that the sand content measured by

SHM can be assumed equal to that determined by LDM technique, while the clay fraction

measured by LDM was lower than that measured by the SHM. A set of equations to

transform LDM results to SHM results was proposed. The influence of the LDM measure-

ments of clay on the estimated percentage of silt þ very fine sand particles (particle

diameter ranging from 0.002 mm to 0.1 mm), which is useful for estimating soil erodibility,

was also studied.

ª 2010 IAgrE. Published by Elsevier Ltd. All rights reserved.

1. Introduction with hydrometer method (SHM) has been adopted as an

Particle-size distributions (PSDs) are fundamental physical

properties of soil and are typically presented as the percentage

of the total dry weight of soil occupied by a given size fraction.

This property is commonly used for soil classification and for

the estimation of some hydraulic properties (Campbell &

Shiozawa, 1992).

Over recent decades, various new methods for grain-size

analysis have been developed. These new methods, (electro-

resistance particle counting, time of transition, laser diffrac-

tion (LD), optical determination of the PSD using image

analysis) (Goossens, 2008; McCave & Syvitski, 1991) generally

have the advantage of covering a wide range of grain sizes,

and rapidly analysing small samples.

Particles of sand size (0.05e2.00 mm) are usually deter-

mined using sieving. The sieve defines a particle diameter

as the length of the side of a square hole through which the

particle can just pass (Allen, 1990). Finer particles are usually

determined by classical sedimentation methods such as

hydrometer or pipette (Gee & Bauder, 1986). Sieving combined

).. Published by Elsevier Lt

international standard to determine quantitatively the PSD of

soils (Allen, 1990; Cooper, Haverland, Hendricks, & Knisel,

1984). With similar pretreatment techniques, the pipette

method (PM) and hydrometer method (HM) - give comparable

results (Liu, Odell, Etter, & Thornburn, 1966; Walter, Hallberg,

& Fenton, 1978); however the PM requires that clay and silt

fractions (<0.05 mm) are separated from the sand fraction

using wet sieving.

Sedimentationmethods are time consuming, especially for

the determination of the particles having a size less than 2 mm,

since they require relatively large samples (10e20 g for the

pipette and 50 g for the hydrometer). They also give unreliable

results for particles 1 mm because of the effect of Brownian

motion on the rate of sedimentation.

A particle diameter obtained by the laser diffraction

method (LDM) is equivalent to that of a sphere giving the same

diffraction as the particles. A laser diffraction particle size

analyser “sees” the particle as a two-dimensional object and it

gives its grain size as a function of the cross-sectional area of

the particle.

d. All rights reserved.

Page 2: Comparison between grain-size analyses using laser ... · A comparison between laser diffraction method (LDM) and the sieve-hydrometer method ... mined using sieving. The sieve defines

Nomenclature

Symbol or abbreviation

SHM sieve-hydrometer method

LDM laser diffraction met

PSD particle-size distribution

PM pipette method

HM hydrometer method

RI refractive index

PM-clay clay determined by pipette method

HM-clay clay determined by hydrometer method

nr real part of RI

ni imaginary term of RI

l wavelength of light

SASHM sand content determined with SHM

SALDM sand content determined with LDM

CLSHM clay content determined with SHM

CLLDM clay content determined with LDM

SIE estimate of silt percentage

RMSE root mean square error

K soil erodibility factor

f percentage of silt þ very fine sand particles

g percentage of sand coarser than very fine sand

d soil particle diameter

fE estimate of f

a coefficient Eq. (5)

b i o s y s t em s e n g i n e e r i n g 1 0 6 ( 2 0 1 0 ) 2 0 5e2 1 5206

Using a laser particle analyser the following assumptions

are made (Konert & Vandenberghe, 1997): (i) the analytical

transformation of diffraction patterns to grain sizes is based

on matrices, which are calculated for spheres. Thus, the

diffraction along the cross-sectional area of the particles is

assigned to diffraction of spheres; (ii) particle orientation is

assumed to be randomly distributed, even if the laser

measurements are carried out in a continuous suspension in

which the particles may be oriented with respect to its shape.

Determination of PSD by an LDM has interested soil scien-

tists for some time (Beuselinck, Govers, Poesen, Degraer, &

Froyen, 1998; de Boer, de Weerd, Thoenes, & Goossens, 1987;

Buurman, Pape, & Muggler, 1997, 2001; Eshel, Levy, Mingelgrin,

& Singer, 2004; McCave, Bryant, Cool, & Coughanowr, 1986;

Pieri, Bittelli, & Rossi Pisa, 2006) but its application has not

generally replaced the labour-intensive classical methods (i.e.

PM or HM). According to Buurman et al. (1997), this reluctance

mainly depends on three factors: (i) insufficient confidence in

the results of LDMs: studies on correlations of laser-clay deter-

minationswith clay determined by pipettemethod (PM-clay) or

clay determined by hydrometer method (HM-clay) are still

rare, and their correlations usually deviate from1:1; (ii) inmany

countries PMs or HMs are accepted as standard for particle size

analysis of soils; (iii) many available relationships/interpreta-

tions have been established with HM/PM textures and (iv) the

high cost of the laser-diffraction equipment.

Theuse of LDMs raises thequestionof howsimilar the laser

grain-size measurements are to those obtained by classical

techniques such as SHM. Thework of Buurman et al. (1997) and

Muggler, Pape, and Buurman (1997), which was carried out

usingsoil profiles, suggested that the relationshipbetweenPM-

clay and LDM-clay may depend on the properties of the clay

fraction itself. Loizeau, Arbouille, Santiago, and Vernet (1994),

using samples of fluvial and lacustrine sediments, found that

the laser grain-size distribution underestimated the clay

content with respect to the classic sedimentationmethod and

that this underestimation increased with increasing clay

content. They were not able to establish if the clay underesti-

mation derived from its mineralogical composition which is

related to the particle shape and no conclusion was made

about the effects on the other size classes.

Buurman et al. (2001) also noted that sand-size particles are

measured more or less equally by LDMs and PSMs while

measurement of the clay-size fraction by the LDM usually

results in smaller percentages than those obtained by PSM.

This means that the lower percentages of the clay fraction

measured by the LDM must be compensated for higher

percentages in the silt-size fraction.

According to Bah, Kravchuk, and Kirchhof (2009) the

differences between the two methods are attributable to the

heterogeneity of soil particle density and the deviation of

particle shapes from sphericity. Sedimentation methods

assume a single particle density, which is a major source of

error, whereas LDM measurements are independent of

particle density.

Deviations from sphericity affect both methods. In the case

of the LDM, an irregular shaped soil particle reflects a cross-

sectional area greater than that of a sphere having the same

volume. Thus, particles are assigned to larger size fractions of

the PSD underestimating the clay fraction. Nonspherical parti-

cles in SHMs have longer settling times than their equivalent

spheres,which results in anoverestimation of the clay fraction.

Taking into account that SHM is an accepted and certified

method, and that LDMprovidesmore information and ismore

efficient than SHM, a relevant question is to establish whether

a correlation exists between the fine sizes fractions obtained

by both methods.

Laser-diffraction instruments have different ranges of

measurement and use a different number of detectors to

cover this range (size classes). Since the accuracy of the

particle size distribution obtained by an LDM depends on the

number of detectors used for a specific size-range, then it is to

be expected that themeasurements in the fine fraction will be

specific for a given LD analyser (Buurman et al., 2001).

Recently Goossens (2008) carried out a comparative study of

ten instruments for measuring the grain-size distribution of

loamy sediments (clay percentage ranging from 2 to 15%) sus-

pended in water. The grain-size analyses were carried out on

four sediments with a particle size-range<90 mm. In particular,

four LDanalysers (MalvernMastersizer S,Coulter LS200, Fritsch

Analysette22CandHoribaParticaLA-950)wereused.According

to thevariouscriteriaconsidered inGoussensstudy (cumulative

grain-size curve, median diameter, grain-size histograms,

skewness and kurtosis), the LD instruments produced the best

results. Althoughno “ideal”method canbedefinedand thefinal

choice of a grain-size technique depends onmany factors (type

of sediments, quantity of sediment available, speed of

measurement, specific aims of the study, etc.), Goossens (2008)

Page 3: Comparison between grain-size analyses using laser ... · A comparison between laser diffraction method (LDM) and the sieve-hydrometer method ... mined using sieving. The sieve defines

b i o s y s t em s e ng i n e e r i n g 1 0 6 ( 2 0 1 0 ) 2 0 5e2 1 5 207

summarised that instruments based on LDM as offering many

advantages and generally work adequately.

In this paper, following a review of the LDM and some asso-

ciated effects (i.e. ultrasonic duration, pretreatment of the soil

sample and diffraction theory used), we test the method and

then compare the particle size distributions obtained by SHM

andbytheLDM.Wealsopresentsacomparative textureanalysis

using hydrometer measurements as a reference for the LDM.

The analysis is carried out using 228 soil samples, all

sampled in Sicily, representing a wide range of textures and

the Fritsch A22-Economy version of the laser diffraction

analyser. Therefore the paper is also the first comparative

analysis between SHM and LDM measurements carried out

using soil samples collected in Italy.

The results obtained in this paper have to be considered as

being apparatus specific because the measurement accuracy

is dependent on the number of detection cells (e.g. 31 in the

Fritsch instrument and 116 in the Coulter LS 230) even though

Goossens (2008) obtained similar results using different types

of laser analyser.

1.1. Sieving e hydrometer method

The PM or the HM defines a particle diameter as equivalent to

that of a sphere settling in the same liquid with the same

speed as the unknown sized particles, the so-called “Stokes

diameter” (Allen, 1990; Konert & Vandenberghe, 1997). The

sphere is usually assigned the density of quartz.

Hydrometer analysis uses a hydrometer having a gradu-

ated stem and weight bulb, to measure the specific density of

the suspension. The specific density depends on the weight of

soil particles in the suspension at the time of measurement

(Wen, Aydin, & Duzgoren-Aydin, 2002).

The HM is based on Stokes’ law that establishes the

velocity at which particles settle in suspension assuming that:

(1) soil particles are rigid, spherical and smooth; (2) soil

particles have similar densities; (3) particle-to-particle inter-

ference and boundary effects from the walls of the sedimen-

tation column are negligible; (4) particle sizes are small

enough to ensure that the induced fluid flow is well within the

laminar flow regime. A particle size calculated by Stokes’ law

is the quartz equivalent spherical sedimentation diameter

(McCave & Syvitski, 1991)

Deviations from Stokes’ law are expected when particles

are irregular in shape, as most silt particles, or are platy or

tubular in shape as aremost clay particles. The particle-shape

effect is due to the circumstance that the most stable position

of a settling, non-spherical particle is the one in which the

maximum cross-sectional area is perpendicular to the direc-

tion of motion. As a consequence, this position increases the

expected particle drag resistance and reduces the settling

velocity. In other words the particle-shape effect results in

a so-called “overestimation” of the fine size fraction which

depends on at which size the platy particles appear.

The validity of the spherical assumption (1) has been

examined in many papers in the past. Nettleship, Cisko, and

Vallejo (1997) established that the standard hydrometer

analysis should not be recommended for submicron mate-

rials. Vitton and Sadler (1997), examining eleven soil by

hydrometer and laser measurements, found that hydrometer

measurements had higher percentages of fine particles than

LDM. Similarly Konert and Vandenberghe (1997), comparing

the results obtained by pipette analysis and laser-diffraction

technique, concluded that particle size distributions were

comparable for “blocky” quartz particles but significantly

different for “platy” clay particles. Recently, Lu, Ristow, and

Likos (2000) carried out a theoretical analysis for deter-

mining the settling velocity of disk-shaped and rod-shapes

particles. Their analysis showed that for disk-shaped and rod-

shapes particles, in sizes ranging from 0.1 mm to 100 mm,

Stokes’ law underestimates the maximum particles dimen-

sion by up to two orders of magnitude. The experimental

results of Lu et al. (2000), using various techniques, also

confirmed the underestimate errors of particle size inherent

in hydrometer analysis.

For soil and earth materials, particle density is commonly

taken constant and equal to 2.65 Mg m�3 Clifton, McDonald,

Plater, and Oldfield (1999) suggested that density of sediment

particles can vary between 1.66 and 2.99 Mg m�3. A soil is

composed of particles with different densities, which are

mainly determined by their mineral compositions. The

uncertainty of particle density may strongly bias the particle

size distribution (Wen et al., 2002).

The effects due to both particle-to-particle interference and

the columnwalls, which limits the applicability of Stokes’ law

can be avoided limiting the maximum concentration of soil in

the suspension (50 g of dry soil in 1000 ml of suspension).

Assumption (4) from above is verified for an upper limit of the

Reynolds number value ranging from 0.1 to 1 (Allen, 1990;

Bernhardt, 1994); these values correspond to free-falling

spherical quartz particles �2 mm in diameter (Lu et al., 2000).

The classical technique SHM represents a “standard” for

soil particle size analysis and many available relationships,

such as pedotransfer functions, were established using

hydrometer/pipette texture measurements.

1.2. Laser diffraction method

The principle of LDM is that particles of a given size diffract

light througha given angle. The angle of diffraction is inversely

proportional to particle size, and the intensity of the diffracted

beamat any angle is ameasure of the number of particleswith

a specific cross-sectional area in the optical path.

A parallel beam of monochromatic light passes through

a suspension contained in a sample cell, and the diffracted

light is focused onto detectors. For calculating particle sizes

from light intensity sensed by detectors, two diffraction

theories are commonly used: the Fraunhofer diffraction

and theMie theory (Gee & Or, 2002). Both theories assume that

the particles have a spherical shape; in other words, the

particle dimension is the optical spherical diameter, i.e. the

diameter of the sphere having a cross-section area equivalent

to the measured one by laser diffraction.

Fraunhofer theory is based on the approximation that the

laser beam is parallel and the detector is at a distance that is

very large compared with the size of the diffracting particle.

Fraunhofer theory becomes inapplicable when the particle

diameter is close to thewavelength of light (l) as the refraction

of particles in this size range becomes appreciable (Loizeau

et al., 1994).

Page 4: Comparison between grain-size analyses using laser ... · A comparison between laser diffraction method (LDM) and the sieve-hydrometer method ... mined using sieving. The sieve defines

Fig. 1 e Distribution by USDA texture using the percentage

of clay, sand and silt determined by SHM (a) and by LDM

(b).

b i o s y s t em s e n g i n e e r i n g 1 0 6 ( 2 0 1 0 ) 2 0 5e2 1 5208

This circumstance could explain why clay detection is

often problematic for laser grain-size measurements.

The Fraunhofer diffraction model gives inaccurate results

for particles <10 l (de Boer et al., 1987).

Matrices based on Fraunhofer theory are calculated from

diffraction by the particles and differences in absorption and

refraction indices have no effect on the calculated grain-size

distribution. This hypothesis is not completely correct for

organic matter since it may absorb some light.

The Mie theory is a solution of the Maxwell equations

describing propagation of the electromagnetic wave of light in

space. This theory provides a solution for the case of plane

wave on a homogeneous sphere of any size (Eshel et al., 2004).

Mie theory takes into account phenomena of transmission

through the particle and therefore requires knowledge of the

refractive index (RI) of the tested soil. The RI of a material is

a function both of particle size and the composition of the

material. Taking into account that soils are generally multi-

sized and poly-mineralic in nature, this canmake it difficult to

choose a representative RI for a given soil. The RI is a complex

number (Eshel et al., 2004) comprising a real part nr, repre-

senting the change in the velocity of light through the tested

material compared with the velocity of light in vacuum, and

an imaginary term ni which represents the transparency and

absorptivity of the tested material.

According to Konert and Vandenberghe (1997) the

Fraunhofer theory is well suited for non-spherical clay parti-

cles. However, de Boer et al. (1987) suggest that the Fraunhofer

model is not accurate enough for the determination of the

clay-size fraction.

Different authors (Beuselinck et al., 1998; Konert &

Vandenberghe, 1997; Loizeau et al., 1994) have concluded that

the Fraunhofer theory overestimates the clay fraction with

respect to the Mie model. Loizeau et al. (1994) also established

that the Fraunhofer theory detects a significantly larger

proportion of the claymeasured by the sieving-pipettemethod

than does the Mie theory.

The LDM analyses small samples in a short period of time

(5e10 min per sample), so it is suitable for rapid and accurate

analysis of a large number of samples (e.g. soil samples sampled

inabasin, suspensionsamplescaughtduringsoil erosionevents).

LDMalso covers awide range of grain sizes andmay also be

used to analyse non-dispersed samples (Muggler et al., 1997).

Although the fully dispersed size distribution (i.e. the ultimate

grain-size distribution) is important with respect to certain soil

chemical and physical properties, other relevant processes,

such as soil erosion and sediment transport by overland flow,

are dependent on the size distribution of soil aggregates

(effective grain-size distribution) (Buurman et al., 1997; Di Stefano

& Ferro, 2002; Foster, Young, & Neibling, 1985).

2. Materials and methods

Soil samples were taken at various locations in a Sicilian

basin, Imera Meridionale, which has an area of 2000 km2. The

228 samples were selected to represent a large variety of soil

textures based on the SHM (Fig. 1a).

For both the SHM and the LDM, soil samples were dried at

105 �Candweregentlycrushedanddrysievedat2-mmmesh-size.

For each analysed soil sample, 50 g was used for the SHM

analysis and 10 g was used for the LDM. Each sample was

treated with H2O2 (concentration equal to 30%) to assure

complete removal of organic material and was dispersed to

remove aggregates by adding a sodium hexametaphosphate

solution over night (Gee & Or, 2002). A volume of 100 ml of

sodium hexametaphosphate solution, having a concentration

equal to 50 g l�1, was used. The treated sample was mixed

overnight using an end e over e end shaking.

For the SHM analysis the pretreated sample (50 g) was wet

sieved through a 0.075 mm sieve. The fine fraction (<75 mm)

collected after wet sieving was transferred to standard cylin-

ders for hydrometer analysis. The cylinders were inserted into

a water bath at a constant temperature. Corrections for the

temperature effects on density and viscosity of suspension

were carried out. A standard hydrometer, ASTM no. 152 H,

Page 5: Comparison between grain-size analyses using laser ... · A comparison between laser diffraction method (LDM) and the sieve-hydrometer method ... mined using sieving. The sieve defines

Fig. 3 e Cumulative particle size distributions of two

b i o s y s t em s e ng i n e e r i n g 1 0 6 ( 2 0 1 0 ) 2 0 5e2 1 5 209

with Bouyoucos scale (g l�1) was used. The suspension was

mixed using an end-over-end shaking for 1 min (Gee & Or,

2002). The hydrometer analysis was carried out by multiple

readings at 2, 5, 15, 30, 60, 180, 1440 and 2880 min (Gee & Or,

2002). The coarse fraction retained by the 75 mm sieve was

oven-dried at 105�, weighed and sieved at 0.075, 0.106, 0.250,

0.425, 0.85 and 2 mm. The adopted sieve sizes belong to the

series R 40/3 of the standard ISO 3310-1.

For the LDM analysis, in the range 0.1e600 mm, the pre-

treated sample (10 g) was firstly wet sieved through a 710 mm

sieve. A pretreated sub-sample, having a volume of 1.5 ml,

was then introduced into the dispersion unit device of the

laser particle analyser for measurement; it contained 400 ml

of deionised water, for the measurement.

The Fritsch Laser Particle Sizer Analysette 22 e Economy

versionmeasures 31 grain-size classes in the working range of

0.1e600 mm. For the LDM analysis a sub-sample was intro-

duced into the dispersion unit device where, to maintain the

random orientation of particles in suspension, automatic

ultrasonication was applied during the measurement.

Ultrasonication is an efficient dispersionmethod but it can

be critical for the particle size distribution because, although

the clay coatings are quickly removed, the quartz grain can be

also broken up. According to Chappel (1998) a 3-min duration

of ultrasound is appropriate for samples suspended in tap

water. Taking into account that the samples were pretreated

with sodium hexametaphosphate, less than 3-min duration

could be appropriate.

Fig. 2 e Cumulative particle size distributions for samples

22 and 44 corresponding to different durations of

ultrasound.

samples, having a different organic matter content, with

and without H2O2 pretreatment.

In order to prevent the formation of gas bubbles during the

movement of suspension into the dispersion unit device, the

stirrer velocity was set to 60e70 revolutions/s. The suspension

was then pumped through a sample cell placed in the

convergent laser beam where the forward scattered light fell

onto the 31 photosensitive sensor rings. Each run was set for

60 s.

Prior to each run, the detectors were aligned, the back-

ground measured and the sample dilution controlled (to test

that the used sub-sample volume allowed a correct analysis).

All operations were controlled by a personal computer.

3. Results

Some factors affecting the LDMwere tested before comparing

the PSD obtained by the two techniques. In particular the

following effects were considered:

i) the duration of ultrasonification

ii) the pretreatment of the soil sample using H2O2 and

iii) the diffraction theory applied.

Fig. 2 shows, as an example for two tested soil samples

(number 22 and 44), the effect of the duration of ultrasound.

Samples 22 and 44 were selected because they had the highest

Page 6: Comparison between grain-size analyses using laser ... · A comparison between laser diffraction method (LDM) and the sieve-hydrometer method ... mined using sieving. The sieve defines

Fig. 4 e Comparison between clay (a) and silt (b) fractions

with and without H2O2 pretreatment.

Fig. 5 e Comparison between cumulative particle size

distributions obtained by the Fraunhofer model and Mie

theory.

b i o s y s t em s e n g i n e e r i n g 1 0 6 ( 2 0 1 0 ) 2 0 5e2 1 5210

clay content of their data set and their grain-size distribution

could be appreciably affected by clay particle aggregation.

Fig. 2 shows the cumulative particle size distribution, for

each tested sample, corresponding to ultrasound duration of

1, 2 and 3 min. The PSD without the dispersion action of

ultrasound was also measured as a reference. Because no

significant difference was determined between the three

particle size distributions corresponding to ultrasonification

for 1, 2 and 3 min n, a duration of 2 min was used in all the

investigations.

To investigate the effect of a pretreatment of the soil

sample by H2O2, seven samples having different organic

matter contents (0.32, 0.36, 1.64, 2.11, 3.03, 4.03 and 7.18%)

were examined. Fig. 3 shows results from two typical agri-

cultural soils (OM< 4%) and demonstrates that an effect of the

pretreatment can be recognised in the particle size distribu-

tion for soil particles ranging from 0.002 mm to 0.1 mm.

Adding of H2O2 produces a shift in the PSD towards finer

particles; in other words for a given particle diameter d the

particle size distribution corresponding to H2O2 pretreatment

is characterised by a frequency value F(d ) greater than that of

the PSD corresponding to “no H2O2 pretreatment”. Removal of

organic material shows that some soil particles which are

originally aggregated become free from aggregation links.

For the seven considered samples, Fig. 4a clearly demon-

strates that the absence of the H2O2 pretreatment gives

a small underestimation of the clay fraction. Taking into

account that three data pairs of Fig. 4b lie on the 1:1 line, and

that the slope of the relationship is almost equal to one, silt

fraction is assumed not affected by the H2O2 pretreatment.

Taking into account that the effect of the H2O2 pretreatment is

not negligible for the clay fraction, all samples analysed in this

investigation were pretreated.

For testing the effect of the diffraction theory used, the

grain-size distribution was determined using both the

Fraunhofer diffraction model and Mie theory. The first

comparison was carried out using a refraction index charac-

terised by a real part nr assuming two different values typical

for the tested soils (1.5 and 1.6) and an imaginary term, ni,

equal to 0.1. The used, nr, values (1.5 and 1.6) were selected

taking into account that for most minerals a value of

approximately 1.53 is suitable (Eshel et al., 2004). Also, if the

effect of coating clay-sized particles by organic matter and

Page 7: Comparison between grain-size analyses using laser ... · A comparison between laser diffraction method (LDM) and the sieve-hydrometer method ... mined using sieving. The sieve defines

Fig. 6 e Comparison between cumulative particle size distributions obtained by SHM and LDM.

b i o s y s t em s e ng i n e e r i n g 1 0 6 ( 2 0 1 0 ) 2 0 5e2 1 5 211

Page 8: Comparison between grain-size analyses using laser ... · A comparison between laser diffraction method (LDM) and the sieve-hydrometer method ... mined using sieving. The sieve defines

Fig. 7 e Relationship between sand fraction obtained by

LDM and by SHM.

Fig. 9 e Comparison between f percentage estimated by Eq.

(4) and by SHM.

b i o s y s t em s e n g i n e e r i n g 1 0 6 ( 2 0 1 0 ) 2 0 5e2 1 5212

oxides has to be considered a nr value of 1.6 should be

employed (CRC Press, 2002).

Fig. 5 shows that no significant differences could be

detected for the two investigated diffraction models applied to

the selected samples. For the same soil samples, the analysis

showed that the variability of the imaginary term of the

refraction index (0.1e0.2) does not produce appreciable effects

on the cumulative grain-size distribution. Accordingly, the

cumulative grain-size distributions of the investigated samples

were determined using the Fraunhofer diffraction model.

Fig. 6 shows the comparison, as an example for eight soil

samples having a different United States Department of

Agriculture (USDA) texture classifications, between the PSD

determined by SHM (for d < 75 mm by HM and for d � 75 mm by

sieving) and LDM (for d � 600 mm by LD and for d > 750 mm by

Fig. 8 e Relationship between clay fraction obtained by

LDM and by SHM.

sieving). This figure shows that for each sample appreciable

differences were detected between the two methods used to

determine the particle size distribution. In particular, for all

samples, the sand content determined by SHM was similar to

the one obtained by LDMwhile the so-called “overestimation”

of the clay percentage measured by SHM as compared to LDM

was confirmed.

Fig. 7, which compares the sand content determined with

SHM, named SASHM, with the LD measured sand content,

SALDM, shows that the two values can be assumed equal.

SASHMySALDM (1)

The relationship plotted in Fig. 7 is characterised by a root

mean square error (RMSE) equal to 2.16 (expressed as %).

For the clay fraction the following equation was

established:

CLSHM ¼ 1:91CLLDM (2)

where CLSHM and CLLDM are, respectively, the clay percentage

determined by the SHM and the LDM (Fig. 8). The relationship

plotted in Fig. 8 is characterised by RMSE ¼ 9.27.

Use of Eqs. (1) and (2) allows the following estimate of SIE or

silt percentage to be obtained:

SIE ¼ 100� 1:91CLLDM � SALDM (3)

This is characterised by appreciable scatter (RMSE ¼ 9.05).

Taking into account that SHM has been adopted as an inter-

national standard to determine quantitatively the PSD of soils

(Cooper et al., 1984), the use of Eqs. (1) and (2) allows the sand

and clay percentage measured by LDM to be referred to the

SHM standard.

The K soil erodibility factor is an integrated long-term

average soil response to the erosive power of rainstorms. Its

estimation by nomograph of Wischmeier, Johnson, and Cross

(1971) requires knowledge of the soil grain distribution, soil

organic matter, soil structure and permeability. In particular

Page 9: Comparison between grain-size analyses using laser ... · A comparison between laser diffraction method (LDM) and the sieve-hydrometer method ... mined using sieving. The sieve defines

Fig. 10 e Relationship between sand and clay fractions

obtained by LDM and by SHM for the textural group “loamy

sand D sandy loam”.

Fig. 11 e Relationship between sand and clay fractions

obtained by LDM and by SHM for the textural group

“loam”.

b i o s y s t em s e ng i n e e r i n g 1 0 6 ( 2 0 1 0 ) 2 0 5e2 1 5 213

the particle size distribution needed to calculate K is the

percentage f of silt þ very fine sand particles

(0.002mm< d< 0.1mm, being d the particle diameter) and the

percentage g of sand coarser than very fine sand

(0.1mm< d< 2mm) as defined byWischmeier et al. (1971) and

used in their nomograph. Taking into account the definition of

the percentages f and g and Eq. (2), the following equation for

estimating the percentage of siltþ very fine sand particles fE is

obtained:

fE ¼ 100� 1:91 CLLDM � g (4)

Fig. 9 shows the comparison between the percentage of

silt þ very fine sand particles fE estimated by Eq. (4) and the

same percentage f calculated by the measurements carried

out by SHM. This comparison shows that fE is similar to f even

if the scattering of the pairs ( f, fE) is appreciable (RMSE¼ 9.56).

To derive equations useful to transform measurements

obtained from the LDM to the SHM, comparisons between

LDM and SHM measurements were carried out grouping soils

with respect to their USDA classification. Fig. 1b shows the

textural classification of the sampled soils using the silt

content (SI), sand content (SA) and clay content (CL)

percentage measured by LDM.

For comparing the CL percentage measured by the two

different methods the soil samples were merged into three

textural groups: loamy sand þ sandy loam (group 1, 19

samples), loam (group 2, 23 samples), silt loam þ silty clay

loam (group 3, 186 samples). The selected textural groups

represent homogeneous zones of the USDA triangle charac-

terised by sand content SA greater than 50% (loamy

sand þ sandy loam), quasi equal to 50% (loam) and less than

50% (silt loam, silty clay loam).

Figs. 10, 11 and 12 show, for each considered textural

group, the relationship between clay percentage determined

Page 10: Comparison between grain-size analyses using laser ... · A comparison between laser diffraction method (LDM) and the sieve-hydrometer method ... mined using sieving. The sieve defines

Fig. 12 e Relationship between sand and clay fractions

obtained by LDM and by SHM for the textural group “silt

loam D silty clay loam”.

b i o s y s t em s e n g i n e e r i n g 1 0 6 ( 2 0 1 0 ) 2 0 5e2 1 5214

by the two different methods. According to these figures, for

the clay fraction the following equation can be established:

CLSHM ¼ a CLLDM (5)

where a is a coefficient equal to 2.18 for the textural group 1

(SA> 50%), 1.91 for the textural group 2 ðSAy50%Þ and equal to

1.91 for the textural group 3 (SA < 50%).

The relationship Eq. (5) calibrated for each textural group is

characterised by RMSE ¼ 3.1 for the textural group 1,

RMSE ¼ 6.4 for the textural group 2, RMSE ¼ 10 for the textural

group 3 which is lower than or similar to that obtained by Eq.

(2) (RMSE ¼ 9.27). In other words, even if in some case (Figs. 11

and 12) the number of samples used is small, for transforming

clay measurements from the LDM to the SHM a more reliable

estimate of clay percentage can be obtained using a coefficient

specific to each textural group.

As a consequence, the improved estimate of clay

percentage by Eq. (5) allows a more accurate estimate of silt

percentage by use of the following equation:

SIE ¼ 100� aCLLDM � SALDM (6)

and of the percentage of siltþ very fine sand particles fE by the

following equation:

fE ¼ 100� aCLLDM � g (7)

The calibration equations (5) and (6) by particle size

(SA > 50% and SA � 50%) presented in this paper are not

universal. As stated earlier, correlations of the LDM with the

SHM may vary for a variety of reasons related to laser

diffraction analyser used, particle shape, mineralogy, RI, etc.

Poor correlations between LDM results and SHM results may

occur if the calibration equations (5) and (6) are applied

outside the range tested here.

4. Conclusions

Taking into account the fact that LDM provides more infor-

mation and is more efficient than the SHM although the latter

is an accepted and certified method, this paper has tried to

solve the question of how similar are the results from the two

methods.

This study was developed using 228 soils sampled in Sicily,

having a variety of texture and the Fritsch A22-Economy

version laser analyser. Goossens (2008) obtained similar

results using different types of laser analyser, but the results

obtained in this paper have to be considered as being appa-

ratus specific because measurement accuracy for the LDM is

dependent on the number of detection cells.

This study showed that there was no significant difference

in the particle size distribution using different ultrasound

durations. The absence of the H2O2 pretreatment gave a small

underestimation in the clay fraction while the silt fraction can

be assumed not affected by the pretreatment. The choice of

the Fraunhofer or Mie diffraction models for the LDM gave no

appreciable differences for the soils investigated.

Analysis of all samples showed that the sand content

determined by SHM was similar to that obtained by the LDM

while the so-called “overestimation” of the clay percentage of

SHM with respect to LDM was confirmed.

Finally, a set of equations useful to refer LDM measure-

ments to the SHM results, the latter is used as an international

standard, was proposed.

The analysis demonstrated that for improving the trans-

formation of the claymeasurements from the LDM to the SHM

three textural groups (sand content greater than 50% (loamy

sand þ sandy loam), almost equal to 50% (loam) and less than

50% (silt loam, silty clay loam)) have to be distinguished. For

each textural group a more reliable estimate of clay

percentage can be obtained using a specific coefficient.

Even if for transforming the clay measurements from the

LDM to the SHM a more reliable estimate of clay percentage

can be obtained using a coefficient specific for each textural

group, the calibration equations (5) and (6) by particle size

(SA > 50% and SA � 50%) presented in this paper are not

Page 11: Comparison between grain-size analyses using laser ... · A comparison between laser diffraction method (LDM) and the sieve-hydrometer method ... mined using sieving. The sieve defines

b i o s y s t em s e ng i n e e r i n g 1 0 6 ( 2 0 1 0 ) 2 0 5e2 1 5 215

universal. Further measurements carried out contemporane-

ously by the LDM and the SHM could allow the results

obtained in this investigation to be confirmed and the

proposed scale equations to be improved.

Acknowledgements

The research was set up by Prof. V. Ferro and Dr. C. Di Stefano,

the measurements were carried out by Dr. S. Mirabile. All

authors analysed the results and contributed to the writing of

the paper.

The research was supported by a grant of Ministero del-

l’Istruzione, dell’Universita e della Ricerca scientifica, Governo

Italiano, PRIN 2007 “Monitoraggio e modellazione dei processi

erosivi a differenti scale spaziali nell’area sperimentale di

Sparacia” and Progetto FEROS.

r e f e r e n c e s

Allen, T. A. (1990). Particle size measurement (4th ed.). London:Chapman and Hall.

Bah, A. R., Kravchuk, O., & Kirchhof, G. (2009). Fitting performanceof particle-size distribution models on data derived byconventional and laser diffraction techniques. Soil ScienceSociety America Journal, 73, 1101e1107.

Bernhardt, C. (1994). Particle size analysis: Classification andsedimentation methods. London, UK: Chapman and Hall.

Beuselinck, L., Govers, G., Poesen, J., Degraer, G., & Froyen, L.(1998). Grain-size analysis laser diffractometry: comparisonwith the sieve-pipette method. Catena, 32, 193e208.

de Boer, G. B., de Weerd, C., Thoenes, D., & Goossens, H. W. (1987).Laser diffraction spectrometry: Fraunhofer versus Miescattering. Particle Characteristics, 4, 14e19.

Buurman, P., Pape, Th., & Muggler, C. C. (1997). Laser grain-sizedetermination in soil genetic studies. 1. Practical problems.Soil Science, 162, 211e218.

Buurman, P., Pape, Th., Reijneveld, J. A., de Jong, F., & vanGelder, E. (2001). Laser-diffraction and pipette-method grainsizing of Dutch sediments: correlations for fine fractions ofmarine, fluvial and loess samples. Netherlands Journal ofGeosciences, 80, 49e57.

Campbell, G. S., & Shiozawa, S. (1992). Prediction of hydraulicproperties of soils using particle-size distribution and bulkdensity data. InM. T. vanGenuchten, F. J. Leij, & L. J. Lund (Eds.),Indirect methods for estimating the hydraulic properties of unsaturedsoils (pp. 317e328). Riverside: University of California.

Chappel, A. (1998). Dispersing sandy soil for the measurement ofparticle size distributions using optical laser diffraction.Catena, 31, 271e281.

Clifton, J., McDonald, P., Plater, A., & Oldfield, F. (1999). Aninvestigation into the efficiency of particle size separationusing Stokes’ law. Earth Surface Processes and Landforms, 24,725e730.

Cooper, L. R., Haverland, R. L., Hendricks, D. M., & Knisel, W. G.(1984). Microtac particle-size analyzer: an alternative particle-size determination method for sediment and soils. Soil Science,138, 138e146.

CRC Press. (2002). Handbook of Chemistry and Physics (83rd ed.).Boca Raton, FL: CRC Press.

Di Stefano, C., & Ferro, V. (2002). Linking clay enrichment andsediment delivery processes. Biosystems Engineering, 81,465e479.

Eshel, G., Levy, G. J., Mingelgrin, U., & Singer, M. J. (2004). Criticalevaluation of the use of laser diffraction for particle-sizedistribution analysis. Soil Science Society of America Journal, 68,736e743.

Foster, G. R., Young, R. A., & Neibling, W. H. (1985). Sedimentcomposition for nonpoint source pollution analyses.Transactions of the ASAE, 28, 133e146.

Gee, G. W., & Bauder, J. W. (1986). Particle-size analysis. In J. H.Klute (Ed.), Methods of soil analysis. Part 1 (2nd ed.).Agron.Monogr., Vol. 9 (pp. 383e411) Madison, WI: ASA and SSSA.

Gee, G. W., & Or, D. (2002). Particle-size analysis. In: J. H. Dane & G.C. Topp (Eds.), Soil Science Society of America Book Series: Vol. 5,Methods of soil analysis. Part 4. Physical methods (pp. 255e293).Madison, WI.

Goossens, D. (2008). Techniques to measure grain-sizedistributions of loamy sediments: a comparative study of teninstruments for wet analysis. Sedimentology, 55, 65e96.

Konert, M., & Vandenberghe, J. (1997). Comparison of laser grainsize analysis with pipette and sieve analysis: a solution for theunderestimation of the clay fraction. Sedimentology, 44,523e525.

Liu, T. K., Odell, R. T., Etter, W. C., & Thornburn, T. H. (1966).Comparison of clay contents determined by hydrometer andpipette methods using reduced major axis analysis.Proceedings e Soil Science Society of America, 30, 665e669.

Loizeau, J. L., Arbouille, D., Santiago, S., & Vernet, J. P. (1994).Evaluation of a wide range laser diffraction grain size analyzerfor use with sediments. Sedimentology, 41, 353e361.

Lu, N., Ristow, G. H., & Likos, W. I. (2000). The accuracy ofhydrometer analysis for fine-grained clay particles.Geotechnical Testing Journal, GTIODI, 23, 487e495.

McCave, I. N., Bryant, R. J., Cool, H. F., & Coughanowr, C. A. (1986).Evaluation of a laser-diffraction-size analyser for use withnatural sediments. Journal of Sedimentary Petrology, 56,561e564.

McCave, I. N., & Syvitski, J. P. M. (1991). Principles and methods ofgeological particle size analysis. In J. M. P. Syvitski (Ed.),Principles, methods and application of particle size analysis (pp.3e21). Cambridge, UK: Cambridge University Press.

Muggler, C. C., Pape, Th., & Buurman, P. (1997). Laser grain-sizedetermination in soil genetic studies: 2. Clay content, clayformation, and aggregation in some Brasilian Oxisols. SoilScience, 162, 219e228.

Nettleship, I., Cisko, L., & Vallejo, L. B. (1997). Aggregation of clayin the hydrometer test. Canadian Geotechnical Journal, 34,621e626.

Pieri, L., Bittelli, M., & Rossi Pisa, P. (2006). Laser diffraction,transmission electron microscopy and image analysis toevaluate a bimodal Gaussian model for particle sizedistribution in soils. Geoderma, 135, 118e132.

Vitton, S. J., & Sadler, L. Y. (1997). Particle-size analysis of soilsusing laser light scattering and X-ray absorbition technology.Geotechnical Testing Journal, 20, 63e73.

Walter, N. F., Hallberg, G. R., & Fenton, T. S. (1978). Particle sizeanalysis by the IowaStateUniv. Soil SurveyLab. InG.R.Hallberg(Ed.), Standard procedures for evaluation of quaternary materials inIowa (pp. 61e74). Iowa City: Iowa Geological Survey.

Wen, B., Aydin, A., & Duzgoren-Aydin, N. S. (2002). A comparativestudy of particle size analyses by sieve-hydrometer and laserdiffraction methods. Geotechnical Testing Journal, 25, 434e442.

Wischmeier, W. H., Johnson, C. B., & Cross, B. V. (1971). Soilerodibility nomograph for farmland and construction sites.Journal of Soil and Water Conservation, 26, 189e193.