Techniques To Measure Grain-Size Distributions of Loamy Sediments: A Comparative Study of Ten Instruments For Wet Analysis

Sedimentology (2008) 55, 6596
doi: 10.1111/j.1365-3091.2007.00893.x
Techniques to measure grain-size distributions of loamy sediments: a comparative study of ten instruments for wet analysis
D IRK GOOSSENS ` mes Atmosphe riques, UMR-CNRS 7583, Universite Paris 12, 61 Laboratoire Interuniversitaire des Syste ne ral de Gaulle, F-94010 Cre teil, France; Physical and Regional Geography Research Group, av. du Ge Katholieke Universiteit Leuven, Geo-Institute, Celestijnenlaan 200E, B-3001 Heverlee, Belgium (E-mail: dirk.goossens@geo.kuleuven.be)
ABSTRACT
Ten instruments for measuring the grain-size distribution of loamy sediments in water were tested in a comparative study. Instruments tested were: the Malvern Mastersizer S, the Coulter LS 200, the Fritsch Analysette 22 (version C), the Horiba Partica LA-950, the Sedigraph 5100, the Atterberg cylinder, the Coulter Multisizer 3, the CIS-100, the EyeTech and the image analysis software Histolab. The rst four instruments use laser diffraction. The Sedigraph and Atterberg cylinder are based on sedimentation. The Coulter Multisizer 3 uses impedance measurements and the last three instruments use optical techniques. Grain-size analyses were carried out on four sediments with median grain diameters of approximately 35, 30, 12 and 9 lm, respectively, and with no particles >90 lm. The laser diffraction instruments produced the best results for the various criteria considered in this study, followed by the Coulter Multisizer 3 (electrical sensing zone technique), the sedimentation techniques and the optical methods. However, the study also showed that there is no such thing as an ideal method because techniques may score differently according to the criterion tested. An appropriate evaluation thus requires that various criteria be considered. Issues to be taken into account are: type of sediment, quantity of sediment available, speed of measurement, complexity of the measurement protocol, processing of the data, reproducibility of the results and the specic aims of the study undertaken. Keywords Clay, grain-size analysis, image analysis, laser diffraction, sedimentation, silt.
INTRODUCTION Grain-size and grain-size distribution are key factors in sedimentology and landscape evolution. These parameters determine the mechanical properties of sediment and provide information on the origin and history of the latter; they also determine by which agent sediment can be eroded, in which physical mode it will be transported, and how it will be deposited. These parameters affect the physical, chemical and biological uxes in sediments and soil, and are thus important parameters in a wide range of environmental disciplines.
Classically, standard methods for grain-size analysis are based on sieving for coarse fractions and sedimentation for ne fractions (Gee & Bauder, 1986). The pipette method has been recommended as a standard for particles <16 lm (Konert & Vandenberghe, 1997), although it has been used frequently for particles of larger sizes. The upper limit for quartz grains analysed in water at laboratory conditions (20 C) is 65 lm, as can be calculated from the ISO 13317 standard, which sets the maximum Reynolds number equal to 025 (International Organization for Standardization, 2001). Other techniques based on sedimentation are, for example, the Atterberg method, 65
2007 The Author. Journal compilation 2007 International Association of Sedimentologists
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D. Goossens Although very useful, many studies show restrictions and, sometimes, errors. A correct comparison of the methods requires that the data they produce be presented in an identical form so that they can be expressed by using the same physical parameters. For example, a direct comparison of Malvern Mastersizer data (based on laser diffraction) and Sedigraph data (based on X-ray attenuation in a settling tube) is somewhat dangerous as the Malvern calculates the data as a volume percentage whereas the Sedigraph uses mass percentages. Because the particle density may vary as a function of the grain-size within a sediment sample, care should be taken when comparing the crude output of both techniques. Similarly, optical measurements cannot be directly compared with the Malvern or the Sedigraph measurements. Many of the studies quoted above neglected to perform the recalculations required for comparison. The results provided by these studies cannot be used for an objective comparison of the techniques, but the diagrams and equations (which were obtained by means of regression analysis) they present can be used to recalculate the numerical results from one technique to another. These studies are thus merely of practical instead of scientic interest. The difference in physical principles on which a measurement is based is only one restriction. Other important issues are: the physical properties of grains, the type of information a technique produces and the denition of grain-size.
the hydrometer method, the hydrophotometer, centrifugal sedimentation and the Sedigraph. Techniques based on other physical principles include electroresistance particle counting (e.g. Coulter Counter), time-of-transition (TOT; e.g. CIS-50 and CIS-100), laser diffraction (various instruments) and optical determination of the particle-size distribution using image analysis. These techniques dene the size of particles in different ways, however, and analytical equipment used to determine the grain-size and associated grain populations can produce variable data from identical samples (Syvitski, 1991). Thus, it can be argued that none of the methods shows true results, as they measure different properties of the same material (Konert & Vandenberghe, 1997). Because of the differences in results, many comparative studies of grain-size techniques have been carried out over the last two decades. These studies include pipette, hydrometer, laser diffraction, Sedigraph, Coulter Counter, optical methods, hydrophotometer and wet sieving. A comprehensive overview of techniques and literature was given in a report by McCave & Syvitski (1991). More recent studies are by: Syvitski et al. (1991) Sedigraph, Coulter counter, pipette, hydrophotometer, laser diffraction; Weber et al. (1991) laser diffraction, Sedigraph; Shillabeer et al. (1992) laser diffraction, sieves; Buchan et al. (1993) Sedigraph, pipette; Zonneveld (1994) sieves, laser diffraction; Duck (1994) pipette, Sedigraph; Loizeau et al. (1994) laser diffraction, pipette; Michoel et al. (1994) Coulter counter, laser diffraction; Bergen & Sukuda (1995) hydrometer, pipette, laser diffraction; Merkus et al. (1995) sedimentation, laser diffraction, Coulter counter; Buurman et al. (1997); Cramp et al. (1997) Sedigraph, Coulter counter, laser diffraction; Konert & Vandenberghe (1997) laser diffraction, pipette; Meyer & Fisher (1997) pipette, Sedigraph; Beuselinck et al. (1998) laser diffraction, pipette; Bianchi et al. (1999) Sedigraph, Coulter Counter; Dalkey & Leecaster (2000) Sedigraph, laser diffraction; Buurman et al. (2001) laser diffraction, pipette; Abee (2002) Sedigraph, pipette, laser diffraction, optical methods; Xu & Di Guida (2003) laser diffraction, Coulter counter, dynamic image analysis; Yamamoto et al. (2004) light scattering, optical measurements; Gao et al. (2005) various optical techniques; Shahin & Symons (2005) optical methods, sieves; and McCave et al. (2006) laser diffraction, Sedigraph.
Physical properties of the grains

Several techniques require detailed information on the physical properties of the grains. Without this information, comparisons between methods are difcult or have only little signicance. Examples of essential grain properties are grain density and grain shape. Knowledge of the grain density (also as a function of the size of the particles) is necessary to compare mass percentages with volume percentages, as explained earlier. Grain shape, on the other hand, is a complex parameter that includes various aspects such as attening, rounding (or angularity) and eccentricity (elongation). These characteristics should be known as a function of the grain-size when data obtained by optical measurements are converted to volume data. Another difculty is that most optical techniques measure the particles in two dimensions only whereas three-dimensional information is needed for accurate volume calculations. Combining data obtained by different
2007 The Author. Journal compilation 2007 International Association of Sedimentologists, Sedimentology, 55, 6596
Grain-size distributions of loamy sediments techniques may be very helpful in this context, as will be illustrated below.
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Type of information
Some techniques produce data based on continuous information whereas others produce data based on discrete information. For example, the Malvern Mastersizer S and Fritsch Analysette 22 calculate the grain-size distribution from the diffraction pattern created by a large number of grains passing through the ow cell. Optical methods, or electroresistance counters (Coulter counter) determine the grain-size for each particle they detect and sum the results when calculating the grain-size distribution. These latter methods generally produce less accurate information for the coarse part of the grain-size spectrum because coarse grains have a much larger volume than ne grains. According to Reid et al. (2003) the greatest particle volume in the coarse mode is usually associated with the largest 1% of particles. The presence of only a few coarse grains in a sample thus makes the grain-size curve irregular, because it evolves stepwise near the coarse end of the grain-size spectrum. Methods based on continuous information suffer much less from this problem.
Denition of grain-size
An important issue is the denition of grain-size. Techniques based on different physical principles dene grain-size in different ways. Laser diffraction and TOT calculate the grain-size in terms of an equivalent volume diameter. Sedimentation techniques calculate the grain-size in terms of an equivalent sedimentation diameter, i.e. the diameter of a sphere settling with the same velocity as that of the particle. Optical techniques apply a wide range of denitions: the most frequently used options are the intermediate diameter (length of the intermediate axis of the best-t ellipsoid), the equivalent surface diameter (diameter of a sphere with the same area as the particle in the plane investigated) and the Feret diameter (measured distance between parallel lines that are tangent to the prole of the particle, in the two-dimensional plane investigated). Converting grain-size data from one diameter to another is not always possible because it may require specic information not necessarily directly available. Binnig et al. (2007) conducted experiments to correlate optical particle diameters to aerodynamic (and volume equivalent)
diameters, but only for particles <10 lm. Such calibrations are sediment-specic, however, and separate tests are required for any new sediment. Here again, combining information obtained by different techniques may be helpful. An important aspect in grain-size analysis is the reproducibility of a measurement. Techniques that analyse only moderate amounts of particles (particle counters, optical image analysers) can be expected to show limited reproducibility. Techniques based on laser diffraction or sedimentation consider many more particles and suffer less from these problems. However, the complexity of the experimental protocol and the associated experimental error, also signicantly affect reproducibility. It is important to note that instruments operating on a same physical principle may produce different results because of technical reasons (see Buurman et al., 2001). For example, the Malvern Mastersizer S, Fritsch Analysette 22, Coulter LS series and Horiba Partica LA series all use laser diffraction, but the number of detectors differs for each instrument. The various parts of the grain-size spectrum are thus measured with a different accuracy for each instrument; this too results in a different reproducibility as a function of the grain-size, as will be illustrated later in this study. The type of sediment also plays a role. Comparing grain-size techniques for different sediments does not produce identical results (Buurman et al., 2001). This situation is understandable because many grain characteristics such as density, attening, angularity, etc., differ for each type of sediment. A comprehensive study of grain-size techniques should thus consider a number of sediments and not just one. A practical issue is the ease with which a technique can be used. This includes: The complexity of the measurement protocol. The less complex, the lower the risk of experimental errors. The complexity of the calculations. Does the technique directly produce the grain-size information desired, or are additional calculations necessary? The amount of sediment required for a measurement. Several techniques require lots of sediment (grams or more), whereas others require only very small samples (order of micrograms or less). The time necessary to perform a measurement. Several techniques take hours (e.g.
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D. Goossens pipette) whereas others require only a few seconds (e.g. laser diffraction). instruments provide the grain-size data as a volume percentage.
Other criteria that can be used in an evaluation are the analytical range (grain-size interval within which measurements are possible) and the measurement resolution (number of grain-size classes measured, and the width of each particular class). Evaluating grain-size techniques is thus a complex operation. Comparative studies published thus far usually considered only a limited number of methods (commonly two or three, rarely more). This study aimed at providing a more complete overview by considering a wide selection of techniques currently available; it also has its restrictions; the most important one is that it considers grain-size analysis in a wet environment only (the sediment is analysed in a water solution). Dry measurements are not considered in this study because of the differences in degree of dispersion of the samples. Another restriction is the particle-size range investigated: only sediments <90 lm were analysed in the current tests. Experiments with coarser sediments should be considered in future studies.
Sedimentation
These techniques help calculate the grain-size from the settling velocity of the particles in a liquid. According to Stokes law, the terminal settling velocity of a spherical particle in a uid is proportional to the square of the diameter of the particles. Thus, coarse particles settle quicker than ne particles. The rate at which the particles settle is calculated by determining the particle mass at a certain depth over time. This information can be obtained by means of several techniques: pipette, Atterberg cylinder, hydrometer, optical sensing and X-ray sensing. Although the International Organization for Standardization considers the pipette as the standard for grainsize analysis, this technique operates slowly and does not always show good reproducibility. The measurement protocol involves sampling of the solution at different times and depths, increasing the risk of experimental error. Because of the rapid sedimentation of coarse grains, the pipette also provides few details for the interval 16 to 65 lm, and no information for the fractions >65 lm (at least, when water is used as the settling medium). A separate analysis with sieves is necessary when details on the latter fractions are required. Because of the capability for quicker analysis and a better suitability for automation, incremental techniques, which measure the change in concentration (or density) of the settling material with time by means of optical or X-ray sensing, have replaced the pipette in many applications. In this test the Sedigraph 5100 (Micromeritics Instrument Corporation, Norcross, GA, USA) was used. This instrument measures the sedimentation rate by determining X-ray obscuration at different levels in a sample cell. The grain-size data are given in percentage of mass. In addition to the Sedigraph, the Atterberg method also was tested. This technique is a slightly modied version of the classic pipette method in that the particles are sampled at a xed height in the sedimentation cylinder, usually near the bottom (see Niedergesa ss et al., 1987 for a detailed description). By diminishing the level of the solution in the cylinder during the settling the correct particle sizes can be sampled and there is no need to put a pipette in the solution. Similar to the Sedigraph, the grain-size
TECHNIQUES AND INSTRUMENTS TESTED Ten instruments, representing ve different measuring principles, were tested:
Laser diffraction
Particles in a laser beam scatter laser light at angles inversely proportional to the size of the particles. Large particles scatter light at small forward angles whereas small particles scatter light at wider angles. Using Fourier and reverse Fourier optics, the scattering is imaged to an array of detectors at the focal plane of the optics. The distribution of the scattered light energy on the detectors can be directly related to the particlesize distribution of the sediment in the laser beam. Mie or Fraunhofer theory is applied to calculate the particle-size distribution. Four laser diffraction particle-size analysers were tested: the Malvern Mastersizer S (Malvern Instruments Ltd, Malvern, UK), the Coulter LS 200 (Beckman Coulter Inc., Fullerton, CA, USA), the Fritsch Analysette 22 C (Fritsch GmbH, IdarOberstein, Germany), and the Horiba Partica LA-950 (Horiba Ltd, Kyoto, Japan). All these
Grain-size distributions of loamy sediments information is provided in terms of percentage of mass.
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Electroresistance particle counting

The Coulter counter instruments operate on this principle. Particles are suspended in an electrolyte solution and sucked through a small aperture. Two electrodes create an electric current through the aperture. When a particle passes through the aperture, it displaces its own volume of electrolyte momentarily, increasing the impedance of the aperture. The pulse created is directly proportional to the volume of the particle. Analysing the pulses enables the size distribution of the suspended sediment to be calculated. In this study, the Coulter Multisizer 3 (Beckman Coulter Inc., Fullerton, CA, USA) was used. This instrument measures the size distribution as well as the number of particles passing through the aperture; it can also calculate the concentration of the particles in the sample.
Time of transition
This technique is based on the detection of particles by a rotating laser beam. The beam, focussed down to a small spot, performs circular scanning by a rotating wedge prism of the sample measurement volume. Interaction signals are generated when the particles within the sample volume are individually bisected by the laser spot. A photodiode detects these signals. Because the beam rotates at a constant speed, the duration of interaction provides a direct measurement of the size of each particle. The grain-size distribution of the sample can then be calculated once sufcient particles have been measured. Similar to laser diffraction analysers, TOT data are delivered as volume percentages. The instrument used in the test is the CIS-100 (Galai Production Ltd, now maintained by Ankersmid B.V., Oosterhout, the Netherlands). The CIS-100 can also perform optical measurements of particles by using dynamic image analysis (DIA), but a new version with more possibilities (called EyeTech; Ankersmid B.V., Oosterhout, the Netherlands) has recently been developed. Thus the EyeTech, rather than the CIS-100, was used to test the DIA application (see below).
analysis software to measure the geometric properties of particles on photographs or other surfaces. A picture of the photograph (or surface) is taken with a video camera and projected on the computer screen. The software scans the picture, and statistics for the whole sample as well as data for individual particles are calculated. DIA uses similar software but is able to measure the characteristics of the particles during their movement through the ow. A high-speed chargecoupled device (CCD) video camera microscope is used to get photographs of the particles as they pass the camera. To ensure high-quality photographs, illumination is provided by a synchronized stroboscopic light source. Histolab software (version 5.14.1; Microvision Instruments, Evry, France) was used in this study to test the possibilities which SIA techniques provide for grain-size analysis. Details on the microscope, the camera and the surface on which the particles were collected are given in the next section. For the DIA application, the EyeTech was tested. As mentioned earlier the CIS-100 can also be used to perform DIA studies, but the EyeTech has more possibilities, including TOT measurements, and also uses different software.
PRESENTATION, SEDIMENTS AND PROCEDURE
Presentation
Data must be expressed in identical form to guarantee correct comparisons of the techniques. Seven of the 10 techniques tested calculate the grain-size distribution as a volume percentage (Malvern, Coulter LS 200, Fritsch, Horiba, Coulter Multisizer 3, CIS-100, EyeTech); two calculate the grain-size distribution as a mass percentage (Atterberg, Sedigraph), and one measures the size of the particles in a plane (Histolab). This study used volume percentages to keep calculation and the experimental error it causes to a minimum.
Sediments General characteristics Four sediment types, collected from a natural excavation in Korbeek-Dijle, Belgium, were used in the tests. Sediment A is a well-sorted silt with a median grain diameter of about 35 lm, a low (<2% to 3%) percentage of clay and no particles above 90 lm. Sediment B is a little ner, with a median diameter around 30 lm and a clay
Image analysis
Two different techniques were tested: static image analysis (SIA) and DIA. SIA uses image
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D. Goossens samples were carried out, as explained earlier. The instruments directly calculate the grain-size distribution as a volume percentage; the data required no further processing.
content of the order of 8%. Moreover, sediment B has no particles >90 lm. Sediment C is much ner, with a median diameter of about 12 lm and clay content around 10%; it is much less sorted than sediments A and B and contains no particles >64 lm. Sediment D, nally, is still ner than sediment C; it has a clay content of about 15% and a median diameter of approximately 9 lm. All numbers are based on an average analysis (average of the 10 techniques tested in this study). The sediments consisted predominantly of quartz, with smaller amounts of feldspars and <5% heavy minerals; they contained no organic matter. All sediments were measured with the techniques described earlier. The analyses were done in water, and 10 repetitions were carried out for each class of sediment. Forty measurements were thus executed with each technique, 400 grain-size analyses in total.
Sample pre-treatment To minimize error, subsampling (to create the 10 samples for the repetition tests) was done very carefully. First, each sediment was mixed carefully. Great care was taken to avoid articially sorting the coarse or ne fractions. Then, many small, random subsamples were taken from the mixed sediment to compose 10 new samples. These 10 samples were then analysed by the instruments. The samples of sediments A and C were not dispersed prior to analysis. The samples of sediments B and D, on the other hand, were dispersed by treating them in an ultrasonic bath for 180 sec. The same ultrasonic bath and the same asks were used for all instruments and for all repetitions; all ultrasonic treatments were performed in equal amounts of distilled water and the degree of dispersion was identical for all dispersed samples of the same type of sediment. No removal of organic matter was necessary because none of the four sediments contained organic matter. Procedure Malvern Mastersizer S, Coulter LS 200, Fritsch Analysette 22, Horiba Partica LA-950 The procedure for these instruments, which all use laser diffraction, was identical. Between 01 and 20 g of sediment (depending on the instrument) was added to the ow circuit of each instrument. To avoid substantial dispersion of the sediments A and C, the grain-size distribution was determined as quickly as possible, usually within a few seconds. Ten repetitions using fresh
Coulter Multisizer 3 This instrument calculates the grain-size distribution in terms of a volume percentage. However, for technical reasons it is unable to measure the entire grain-size spectrum tested (0 to 90 lm) in a single operation. To cover the spectrum, the sediment was analysed by using the following aperture diameters: 30 lm (measuring range: 06 to 180 lm), 100 lm (measuring range: 20 to 600 lm) and 560 lm (measuring range: 112 to 3360 lm). Each sample was therefore analysed in three steps, one aperture per step. The three measurements were then combined, and the total grain-size distribution reconstructed. It should be noted that other aperture diameters can be used (ranging from 20 lm to 2000 lm), depending on the grain-size in the sediment analysed. ISOTON II (Beckman Coulter Inc., Fullerton, CA, USA) was used as the electrolyte in the tests. Sedigraph 5100 This instrument provides the grain-size distribution in terms of a percentage of mass (not of volume). To transfer the data to a percentage of volume, the density of the grains must be known. For natural sediments such as those tested in this study the density may vary with the grain-size. Therefore the density was determined for a large number of grain-size fractions, for all four sediments. The procedure was as follows: rst, sufcient sediment was collected of the following grain-size classes: 64 to 90, 32 to 64, <32, <16, <8, <4 and <2 lm. The samples for the classes 64 to 90 and 32 to 64 lm were obtained by wet-sieving. The samples for the other fractions were obtained by using the Atterberg technique (see below). For each of these seven fractions, a picnometer was used (Blake & Hartge, 1986) to determine the density of the sediment. The density of the fraction 2 to 4 lm can be calculated by using the percentage proportion of the fractions <2 and 2 to 4 lm in the sample of size <4 lm (to ensure objectivity, the average percentage of all 10 tested instruments was used). The same procedure was adopted for the fractions <8, <16 and <32 lm. This procedure allowed the calculation of the density for the following grain-size classes: <2, 2 to 4, 4 to 8, 8 to 16, 16 to 32 and 32 to 64 lm (and, for the sediments A and B, 64 to 90 lm).
Grain-size distributions of loamy sediments Density measurements were repeated up to three times. Figure 1 shows that, for the four sediments used, the density increased with the grain-size up to the class 16 to 32 lm, after which it stabilized (sediments C and D) or even slightly dropped after 64 lm (sediments A and B). By plotting the relationship between the density of the grains and size as a curve (not a histogram), interpolation could be used to reconstruct the grain density for a large number of grain-size fractions. This information was used to recalculate the Sedigraph data (after having been transformed into grainsize classes) to volume percentages.
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Atterberg cylinder As with the Sedigraph all Atterberg data, which were originally obtained as mass percentages, were recalculated to volume percentages. Theoretically, the Atterberg method allows calculation of the percentage proportion of a large number of grain-size fractions. However, because of the rapid sedimentation of the grains >16 lm it is usually not possible to sample many classes between 16 and 64 lm. It is a common procedure to measure only two fractions in this range: 16 to 32 and 32 to 64 lm (see Beuselinck et al., 1998). To obtain more information, grain-size data can
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be reconstructed for intermediate classes by interpolating the cumulative grain-size curve. Such reconstructions are only reliable if the cumulative curve can be adequately reconstructed over the interval 16 to 64 lm, which is not evident as there is usually only one intermediate point (at 32 lm) for which data exist. However, data from other grain-size techniques can help to determine the correct shape of the cumulative grain-size curve. For the sediments C and D all other techniques, except Histolab, produced similar cumulative curves (see section, Results). For these sediments, the Atterberg curves were thus tted using a third-order polynomial function having the same shape. For the sediments A and B the t is more complex. All other techniques (including Histolab) show a cumulative curve with a concave curvature in the ne particle range and a convex curvature in the coarse particle range. These sediments are well-sorted, and their grain-size distribution is close to normal (see section, Results). When calculating the cumulative curves for the sediments A and B, the function y exp()x2) was used to t the data points. Using this function, which describes a normal distribution, ensures that the high degree of sorting of both sediments is guaranteed during the t and that the tted
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Mass density (g cm3)
25 20 15 10 05
1632 m 3264 m 6490 m 816 m <2 m 24 m 48 m
30
sediment A
30 25 20 15 10 05
sediment B
1632 m
3264 m
Grain size class

35 35
Grain size class
25 20 15 10 05
24 m 48 m 1632 m 3264 m 816 m <2 m
30
sediment C
30 25 20 15 10 05
24 m
sediment D
48 m
1632 m
Grain size class
Grain size class
Fig. 1. Mass density for various grain-size classes of the sediments A, B, C and D.
3264 m
816 m
<2 m
00
00
6490 m
816 m
<2 m
24 m
48 m
00
00
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D. Goossens size distribution of the sediment in terms of a volume (so that comparisons with the other techniques tested are possible), the third dimension, i.e. the c-diameter, should also be known. The c-diameter of a grain can be directly determined under a microscope by turning the grain over 90 (see Goossens, 2005; Goossens & Rajot, in press). However, the procedure is very timeconsuming and, because of the difculty in automating the method, it cannot be applied to samples of many thousands of grains. Therefore, the alternative approach described below was followed. First, the a and b-diameters were measured for all grains using Histolab. The only other instrument (tested in this study) that directly measures the volume of individual grains is the Coulter Multisizer 3 (note that laser diffraction instruments do not measure individual grains). By measuring, for all 40 sediment samples, the average grain volume for many grain-size classes with the Coulter Multisizer 3; and by measuring, for the same classes, the a and b-diameters with Histolab, it is possible to calculate, for each grain-size class, the average c-diameter, and thus, also the average degree of attening of the grains. Grain attening is dened in this study as c/(ab)05, which corresponds to the wellknown Corey shape factor (CSF; Corey, 1949). The average CSF is thus calculated for all grainsize classes selected. Sufcient classes should be considered because for natural sediments the attening (and, usually, also the rounding) of a grain usually varies with the grain-size. Using the CSF the volume of any grain measured by Histolab in the ab-plane and in a particular grain-size class can be calculated with a very good approximation. Because Histolab also measures the horizontal cross-section of the grains (in the ab-plane), it is able to calculate the degree of rounding of the grains in that same plane. Accepting that the rounding in the ab-plane is sufciently representative for the whole grain (which is a better option than any other calculable solution), grain rounding can be incorporated into the calculation of the grain volume by using the real cross-section instead of the product abp/4. Summing up the volumes of the individual grains the volume percentage proportion (in the total sample) can be calculated for each grain-size class, producing the grain-size distribution in terms of a percentage of volume. Figure 2 shows, for the four sediments, the CSF values for various grain-size classes. The results
curve will closely approximate the true grain-size distribution of these sediments.
Histolab This technique helps measure the grain-size by using image analysis software. The procedure followed in this study is as follows. First, a pretreated sample of each sediment class was added to a small cylinder lled with de-ionized water. The suspension was carefully mixed to ensure homogeneous distribution of the sediment over the cylinder. The solution was then ltered using a vacuum pump and the grains were retained on a cellulose triacetate lter (diameter: 25 cm). The sediment was very well distributed over the lter, and the amount was small enough to avoid aggregates being formed on the lter (several preliminary tests were carried out to determine the maximum mass of sediment that could be used). The lters were then put on a microscope slide and made transparent by vapourizing acetone over them. In this way, grains will only be detected when analysing the lters under a microscope. The lters were then xed between the microscope slide and a coverglass using EUKITT xation liquid (O. Kindler GmbH & Co., Freiburg, Germany). Several lters were prepared for each of the four sediments; after preparation, they were analysed with the Histolab software. The microscope used was Leica MZ 12 (Meyer Instruments, Houston, TX, USA), and the camera Sony 3CCD Colour Video Camera (Sony Corporation, Tokyo, Japan). From each lter, a large number of image elds (up to 60) were analysed. The elds did not overlap. Each eld contained many hundreds of grains. Several tens of thousands of grains were thus measured for each sample. To produce 10 repetitions per sample (such as for the other techniques tested in this study), the image elds were later combined into 10 groups containing approximately the same number of grains. Each image eld was used only once. The microscope shows the grains in a plane perpendicular to it (in the present case, the plane analysed was horizontal, parallel to the lters). During the collection of particles on a lter, particles are typically oriented such that their minor axis is normal to the substrate (Reid et al., 2003); that is, the largest at side is face down. The grain is assumed to be an ellipsoid with the longest axis a, the intermediate axis b and the shortest axis c. In that case, Histolab measures the particles in the ab-plane. To calculate the grain-
Grain-size distributions of loamy sediments

08 07 06 05
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sediment A
08 07 06 05
sediment B
CSF
04 03 02 01
1015 m 1520 m 2025 m 2530 m 3035 m 3540 m 4045 m 4550 m 5055 m 5560 m <2 m 25 m 510 m
CSF
04 03 02 01
1015 m 1520 m 2025 m 2530 m 3035 m 3540 m 4045 m 4550 m 5055 m 3236 m 5560 m 3640 m <2 m 25 m 510 m
Grain size class

08 07 06 05
Grain size class

08 07 06 05
sediment C
sediment D
CSF
04 03 02 01
24 m 48 m <2 m 812 m 1216 m 2024 m 2428 m 3236 m 1620 m 2832 m 3640 m
CSF
04 03 02 01
24 m 48 m <2 m 812 m 1216 m 2024 m 2428 m 1620 m 2832 m
Grain size class
Grain size class
Fig. 2. Degree of attening (quantied by the Corey shape factor or CSF) for various grain-size classes of the sediments A, B, C and D.
are more or less comparable for the four sediments. The ne grains were distinctly more attened than the coarse grains: note the systematic decrease of the CSF as the particles become ner than approximately 15 lm. The gures also show that for grains >15 lm attening could be considered more or less constant. No data are shown above 60 lm (sediments A and B) and 40 lm (sediments C and D) because the Coulter Multisizer 3 hardly measured any grains coarser than these sizes.
p c p 2 6
where p is the largest axis of the measured ellipse (the cross section of the grain in the ac-plane). Because the orientation of the grains around their c-axis is random (see also Xu & Di Guida, 2003), it is reasonable to assume that, for a sediment composed of many grains, the average value of p (which for each grain is always situated between a and b) will become equal to the geometrical mean (ab)05. Equation (1) then becomes: V p c ab05 2 6 p cab 6
CIS-100, EyeTech These instruments directly calculate the grainsize distribution in percentage of volume. The calculation is based on optical 2D measurements of the grains in the ac-plane. The instruments effectively measure the grains in the ac-plane because the suspension (water + sediment) is in a turbulent ow regime when pumped through the instrument. In such conditions particles have their largest cross-section (i.e. the ab-plane) perpendicular to the ow (Middleton & Southard, 1978; Dietrich, 1982). Both the CIS-100 and the EyeTech calculate the volume V as:
Thus, for a sample composed of many grains, the average volumes measured by the CIS-100 and the EyeTech effectively correspond to the true average grain volume. The only errors that can still occur are those caused by the rounding of the grains. By determining the product cp2 from the true cross-sectional area of the grains (which can be done with the DIA technique but not with the
74
D. Goossens represent the average of the 10 repetitions for each sample. The gure indicates that, for each sediment class, the shape of the curves is more or less identical for the methods tested. Differences occur for a few combinations (in particular, Histolab for the sediments C and D) and there are also minor, more local, irregularities in several other curves. The images also show considerable variation in the horizontal position of the curves in the diagrams. The trends are generally similar for the four sediments: the Sedigraph and CIS-100 curves are always on the left in the pictures (ne part of the grain-size spectrum) whereas those of Histolab and the EyeTech are always on the right (coarse part of the spectrum). The Sedigraph and CIS-100 thus characterized the sediments as ner, whereas Histolab and the EyeTech considered them as coarser than the other six methods did.
TOT technique), it is possible to incorporate the rounding in the volume calculations.
RESULTS This section presents the results without judging the instruments. As noted earlier, each technique denes the size of a particle in a different way, and despite transformation of the data to the same standard (grain-size distribution as percentage of volume) neither method shows true or correct results. An attempt will nevertheless be made in a following section to evaluate the instruments, based on various criteria.
Cumulative grain-size curves

Figure 3 shows the cumulative grain-size curves for all 40 combinations tested. The cumulative curve is a handy tool to display the grain-size distribution in a single graph and it has been frequently used in comparative grain-size studies (e.g. Bergen & Sukuda, 1995; Cramp et al., 1997; Beuselinck et al., 1998). All curves in Fig. 3
100 90
Median grain diameter

Figure 4 shows the median grain diameters for the 40 combinations tested. The ranking of the instruments is almost identical for the four
100 90
Cumulative volume (%)
70 60 50 40 30 20 10 0 0 10 20 30 40 50 60
80
80 70 60 50 40 30 20 10 0
Malvern mastersizer S Sedigraph 5100 Atterberg cylinder Histolab Coulter LS 200 Coulter multisizer 3 Fritsch analysette 22 C CIS-100 (TOT) Eyetech (DIA) Horiba partica LA-950
sediment A
sediment B
70
80
90
10
20
30
40
50
60
70
80
90
Grain size (m)

100 90 100 90
Grain size (m)
70 60 50 40 30 20 10 0 0 10 20 30 40 50 60
80
80 70 60 50 40 30 20 10 0
sediment C
sediment D
70
80
90
10
20
30
40
50
60
70
80
90
Grain size (m)
Grain size (m)
Fig. 3. Cumulative grain-size curves for the four sediments and ten techniques tested. Each curve represents the average of 10 repetitions.

70 70
75
sediment A
sediment B
Median grain diameter (m)
50 40 30 20 10 0
30
H E
H = Histolab E = Eyetech (DIA) P = Horiba partica LA-950 A = Atterberg cylinder C = Coulter multisizer 3
M = Malvern mastersizer S L = Coulter LS 200 F = Fritsch analysette 22 C T = CIS-100 (TOT) S = Sedigraph 5100
60
60 50 40 30 20 10 0
30
H = Histolab E = Eyetech (DIA) P = Horiba partica LA-950 A = Atterberg cylinder C = Coulter Multisizer 3
M = Malvern mastersizer S L = Coulter LS 200 F = Fritsch analysette 22 C T = CIS-100 (TOT) S = Sedigraph 5100
A C
E P A C M L F T
T S
25 20
sediment C
H = Histolab E = Eyetech (DIA) P = Horiba partica LA-950 A = Atterberg cylinder C = Coulter multisizer 3 M = Malvern mastersizer S L = Coulter LS 200 F = Fritsch analysette 22 C T = CIS-100 (TOT) S = Sedigraph 5100
sediment D
25 20 E 15 P 10 5 0 A C M L F T S H
H = Histolab E = Eyetech (DIA) P = Horiba partica LA-950 A = Atterberg cylinder C = Coulter multisizer 3 M = Malvern mastersizer S L = Coulter LS 200 F = Fritsch analysette 22 C T = CIS-100 (TOT) S = Sedigraph 5100
E 15 10 5 0 P A C M L F T S
Fig. 4. Median grain diameter for the four sediments and 10 techniques tested. (Techniques are ranked according to the average numerical result for the four sediments.)
sediments. Histolab and EyeTech produced the coarsest grain-size distributions, followed by the Horiba Partica LA-950, the Atterberg cylinder and the Coulter Multisizer 3. Finer grain-size distributions were measured by the Malvern, Coulter LS 200 and Fritsch. The CIS-100 and Sedigraph, nally, produced the nest grain-size distributions. Moreover notice that, on average, the Malvern, Coulter LS 200 and Fritsch measured nearly identical median grain diameters. The Horiba, which operates on the same principle (laser diffraction), produced somewhat coarser grain-size distributions. Another conclusion is that the two optical methods based on particle image software (Histolab, EyeTech) always measured the coarsest grain-size distributions. The results of the two sedimentation techniques (Atterberg, Sedigraph), on the other hand, were mutually different.
are presented in Table 1, the histograms in Fig. 5. Important differences can be observed within each sediment class. Note how the mode, the sorting of the sediment and the proportion of each grain-size class changes with a technique. Note, in particular, the spectacular differences in the nest grain-size fraction (especially for the A and B sediments, and also for the C and D sediments), the absence of coarse sediments for the CIS-100, and the great difference between Histolab and the other techniques for the sediments C and D.
Skewness and kurtosis

The differences in the histograms can be further quantied by calculating the skewness and kurtosis. Figure 6 shows the skewness of the 40 distributions. All distributions are positively skewed, that is, with scores bunched up on the ner end of the spectrum. The ranking of the methods is almost identical for the sediments C and D but no trends are observed for the sediments A and B. Note however that for these sediments the Sedigraph always scored relatively high, and the Coulter Multisizer 3 very low values, similar to the sediments C and D. Statistical
Grain-size histograms
To analyse the data in greater detail the percentage proportions were calculated for 18 (sediments A and B) and 16 (sediments C and D) grain-size fractions of equal width (5 lm for sediments A and B, 4 lm for sediments C and D). The values
76
Table 1. Numerical data for the 18 (sediments A and B) and 16 (sediments C and D) grain-size classes investigated, for the various techniques and sediments tested.
Sediment A Grain-size class
D. Goossens
Technique 463 123 463 586 338 169 338 507 124 093 124 217 010 049 010 059 422 189 422 611 856 408 856 1265 357 260 357 617 037 142 037 179 004 057 004 061 000 013 000 013 300 886 746 1253 256 473 182 240 399 1010 672 1936 527 1144 625 804 239 300 131 144 575 1460 1145 2398 472 945 345 585 692 1702 588 2524 778 1922 1060 1864 474 774 413 556 863 2323 1497 3895 700 1645 533 1118 967 2669 833 3357 1038 2960 1340 3204 818 1592 890 1447 1041 3364 1563 5458 1268 2913 726 1844 1195 3864 1044 4401 1169 4129 1239 4444 1037 2628 1261 2708 1112 4476 1393 6851 1551 4464 923 2767 1239 5102 1272 5672 1183 5312 1465 5909 1266 3894 1521 4228 1130 5605 1115 7967 1714 6178 938 3705 1195 6297 1219 6891 1059 6371 1226 7134 1391 5285 1459 5688 1022 6627 777 8744 1547 7724 1240 4945 1017 7314 1036 7927 849 7219 1040 8174 1169 6454 1236 6924 865 7492 495 9239 1141 8865 1301 6246 832 8146 828 8756 660 7880 942 9116 1291 7745 920 7844 680 8173 297 9536 641 9506 1006 7252 608 8753 580 9335 526 8406 551 9667 879 8624 673 8517
Per 05 510 1015 1520 2025 2530 3035 3540 4045 4550 5055 5560 6065 6570 7075 7580 8085 8590 lm lm lm lm lm lm lm lm lm lm lm lm lm lm lm lm cent lm lm 545 405 308 224 149 114 083 8717 9122 9430 9654 9803 9917 10000 217 108 068 036 017 017 002 9752 9860 9928 9964 9980 9998 10000 350 106 018 008 005 003 003 9856 9962 9981 9989 9994 9997 10000 705 716 533 389 254 111 039 7957 8674 9207 9596 9849 9961 10000 430 289 197 131 097 068 035 9183 9472 9669 9800 9897 9965 10000 294 147 084 050 023 026 041 9630 9777 9861 9910 9933 9959 10000 444 339 276 214 131 118 073 8850 9188 9465 9679 9810 9927 10000 242 091 000 000 000 000 000 9909 10000 10000 10000 10000 10000 10000 588 400 197 119 072 000 000 9212 9612 9809 9928 10000 10000 10000 511 324 240 164 115 075 054 9028 9352 9592 9756 9871 9946 10000
Malvern Mastersizer S abs cum Sedigraph 5100 abs cum Atterberg cylinder abs cum Histolab abs cum Coulter LS 200 abs cum Coulter Multisizer 3 abs cum Fritsch Analysette abs 22c cum CIS-100 (TOT) abs cum EyeTech (DIA) abs cum Horiba Partica abs LA-950 cum
Sediment B Grain-size class 510 1015 1520 2025 2530 3035 3540 4045 4550 5055 5560 6065 6570 7075 7580 8085 8590 lm lm lm lm lm lm lm lm lm lm lm lm lm lm lm lm lm 926 5473 1113 7602 1351 5334 1615 941 6414 855 8457 1449 6783 1126 843 695 551 440 340 252 179 132 091 066 7257 7951 8502 8942 9282 9534 9712 9844 9935 10000 589 385 228 158 076 042 035 012 012 005 9046 9431 9659 9817 9893 9935 9970 9982 9995 10000 1298 952 525 306 129 008 000 000 000 000 8081 9033 9557 9864 9992 10000 10000 10000 10000 10000 1555 596 522 440 150 281 000 000 000 000
Technique
Per 05 cent lm 1607 406 359 553 756 866 1607 2013 2372 2925 3681 4547 2058 324 644 972 1232 1260 2058 2382 3025 3997 5229 6489 936 126 245 613 851 1214 936 1062 1306 1919 2770 3983 079 228 444 767 1038 1162
Malvern Mastersizer S abs cum Sedigraph 5100 abs cum Atterberg cylinder abs cum Histolab abs
Table 1. (Continued)
Sediment B
Grain-size class 510 1015 1520 2025 2530 3035 3540 4045 4550 5055 5560 6065 6570 7075 7580 8085 8590 lm lm lm lm lm lm lm lm lm lm lm lm lm lm lm lm lm 307 441 1739 403 1019 493 1848 383 811 464 559 187 1669 751 473 2211 750 1769 627 2475 913 1723 483 1042 239 1908 1518 652 2863 622 2391 749 3224 1435 3158 549 1591 489 2397 2556 853 3716 900 3291 949 4173 1605 4763 706 2297 861 3258 3717 1043 4759 1085 4375 1049 5222 1653 6416 936 3232 1113 4371 5332 1076 5835 1225 5600 1036 6258 1403 7819 1114 4347 1260 5631 6457 1028 6863 1170 6770 891 7149 1220 9039 1216 5562 1163 6793 8012 858 7721 1021 7791 715 7864 497 9536 1204 6766 955 7748 8608 697 8418 799 8590 541 8406 272 9808 1169 7936 689 8438 9130 9570 9720 10000 10000 10000 10000 503 354 248 172 114 087 065 8921 9275 9523 9695 9809 9896 9962 609 250 190 095 058 077 072 9199 9449 9638 9733 9791 9868 9940 421 342 263 196 153 102 070 8827 9169 9432 9628 9781 9883 9953 092 100 000 000 000 000 000 9900 10000 10000 10000 10000 10000 10000 881 549 359 212 005 058 000 8817 9366 9724 9936 9942 10000 10000 496 372 233 172 116 081 053 8934 9306 9539 9711 9827 9909 9962 10000 038 10000 060 10000 047 10000 000 10000 000 10000 038 10000
Technique
Per 05 cent lm
cum abs cum Coulter Multisizer 3 abs cum Fritsch Analysette abs 22c cum CIS-100 (TOT) abs cum EyeTech (DIA) abs cum Horiba Partica abs LA-950 cum
Coulter LS 200
079 1297 1297 616 616 1354 1354 428 428 095 095 1482 1482
Sediment C Grain-size class 48 lm 1631 4126 2068 4397 1606 3381 393 475 1643 4141 1678 3183 1605 3981 1109 6598 1362 7526 1204 5989 1000 2300 1146 6688 1676 6554 1142 6527 892 7490 942 8468 1000 6989 1195 3495 918 7606 1186 7741 881 7408 682 8172 610 9078 834 7823 1221 4716 650 8256 1067 8808 697 8105 1363 5489 1767 6164 1405 4786 825 1300 1400 5542 1695 4879 1404 5385 524 8695 373 9451 661 8485 985 5701 464 8719 555 9363 531 8636 812 lm 1216 1620 2024 2428 2832 3236 3640 4044 lm lm lm lm lm lm lm lm 364 9060 256 9707 512 8996 1038 6739 323 9042 328 9690 400 9037 281 9341 125 9832 259 9255 958 7697 235 9277 137 9828 297 9334 205 9545 077 9909 172 9428 659 8356 172 9449 102 9930 208 9542 4448 lm 4852 lm 5256 lm 5660 lm 145 099 074 062 044 9690 9788 9863 9925 9969 043 023 013 005 004 9953 9975 9988 9993 9997 137 102 082 073 080 9565 9667 9749 9822 9902 546 348 250 240 185 8902 9250 9500 9740 9925 127 106 082 084 083 9576 9682 9764 9848 9931 070 000 000 000 000 10000 10000 10000 10000 10000 150 100 075 060 042 9692 9792 9867 9927 9969 6064 lm 031 10000 003 10000 098 10000 075 10000 069 10000 000 10000 031 10000
Technique 2495 2495 2329 2329 1775 1775 082 082 2498 2498 1506 1506 2376 2376
Per 04 cent lm
Malvern Mastersizer S abs cum Sedigraph 5100 abs cum Atterberg cylinder abs cum Histolab abs cum Coulter LS 200 abs cum Coulter Multisizer 3 abs cum Fritsch Analysette abs 22c cum
77
78
Table 1. (Continued)
Sediment C
D. Goossens
Grain-size class 48 lm 812 lm 1216 lm 1620 lm 2024 lm 2428 lm 2832 lm 3236 lm 3640 lm 4044 lm 4448 lm 4852 lm 5256 lm 5660 lm 6064 lm
Technique
Per cent
04 lm
CIS-100 (TOT)
EyeTech (DIA)
Horiba Partica LA-950
abs cum abs cum abs cum
1236 1236 021 021 1497 1497
2605 3841 979 1000 1599 3097
2342 6183 1680 2681 1166 4263
1753 7936 1887 4568 1274 5537
985 8921 1481 6049 1306 6843
419 9341 1083 7132 1078 7921
283 9624 787 7919 764 8685
136 9760 468 8387 497 9183
080 9840 353 8740 312 9494
097 9937 208 8948 197 9691
042 9979 052 9000 116 9806
021 10000 000 9000 072 9878
000 10000 000 9000 053 9932
000 10000 000 9000 030 9961
000 10000 000 9000 024 9986
000 10000 000 9000 014 10000
Sediment D Grain-size class 48 lm 1627 5045 1675 5603 1629 4121 701 927 1789 4778 1716 3921 1762 4666 3341 5918 1132 1364 1581 4041 1214 6258 1342 6945 1392 5513 952 1880 1360 6138 1591 5512 1379 6045 2302 8220 1732 3096 991 5032 924 7183 1099 8044 1138 6651 1055 2935 1041 7179 1366 6877 1048 7093 1157 9377 1567 4664 1046 6079 717 7899 798 8842 918 7569 1298 4233 794 7973 1101 7979 783 7876 534 9911 1412 6076 1082 7161 560 8460 492 9334 702 8271 1194 5426 554 8527 1060 9039 593 8469 082 9993 1041 7116 920 8081 812 lm 1216 1620 2024 2428 lm lm lm lm 2832 lm 3236 lm 3640 lm 4044 lm 4448 lm 4852 lm 5256 lm 5660 lm 6064 lm 012 10000 010 10000 087 10000 000 10000 053 10000 000 10000 017 10000 000 10000 000 9000 017 10000
Technique 3417 3417 3928 3928 2492 2492 226 226 2989 2989 2205 2205 2904 2904 2577 2577 232 232 2461 2461
Per 04 cent lm
Malvern Mastersizer S abs cum Sedigraph 5100 abs cum Atterberg cylinder abs cum Histolab abs cum Coulter LS 200 abs cum Coulter Multisizer 3 abs cum Fritsch Analysette abs 22c cum CIS-100 (TOT) abs cum EyeTech (DIA) abs cum Horiba Partica abs LA-950 cum
425 323 235 184 113 099 061 046 041 8884 9207 9442 9627 9740 9839 9901 9947 9988 275 168 082 057 033 016 012 009 005 9609 9777 9859 9916 9949 9965 9977 9986 9990 534 380 208 142 106 079 073 059 062 8805 9185 9392 9534 9641 9719 9792 9851 9913 1227 1033 620 586 549 295 187 077 000 6654 7687 8307 8893 9441 9736 9923 10000 10000 398 282 206 146 119 079 074 059 057 8925 9207 9413 9559 9678 9757 9831 9890 9947 401 207 237 117 000 000 000 000 000 9439 9646 9883 10000 10000 10000 10000 10000 10000 448 329 241 170 108 080 062 039 036 8917 9246 9487 9657 9765 9845 9908 9947 9983 007 000 000 000 000 000 000 000 000 10000 10000 10000 10000 10000 10000 10000 10000 10000 970 367 269 162 099 016 000 000 000 8086 8453 8723 8885 8984 9000 9000 9000 9000 672 450 290 187 114 073 056 033 027 8753 9202 9492 9679 9794 9867 9923 9955 9983

sediment A
20 15 10 5 0
20 15 10 5 0 20 15 10 5 0 20 15 10 5 0 20 15 10 5 0 20 15 10 5 0 20 15 10 5 0 20 15 10 5 0 20 15 10 5 0 20 15 10 5 0
05 510 1015 1520 2025 2530 3035 3540 4045 4550 5055 5560 6065 6570 7075 7580 8085 8590
79
sediment B
25 20 15 10 5 0 0
sediment C
30 20 10
sediment D
40 30 20 10 0
Malvern mastersizer S
Sedigraph 5100
25 20 15 10 5
Sedigraph 5100
30 20 10
Sedigraph 5100
40 30 20 10 0
Sedigraph 5100
Atterberg cylinder
25 20 15 10 5 0
Atterberg cylinder
30 20 10 0
Atterberg cylinder
40 30 20 10 0
Atterberg cylinder
Histolab
25 20 15 10 5 0
Histolab
30 20 10 0
Histolab
40 30 20 10 0
Histolab
Coulter LS 200
25 20 15 10 5 0
Coulter LS 200
30 20 10 0
Coulter LS 200
40 30 20 10 0
Coulter LS 200
Coulter multisizer 3
25 20 15 10 5 0
30 20 10 0
40 30 20 10 0
Fritsch analysette 22 C
25 20 15 10 5 0
30 20 10 0
40 30 20 10 0
CIS-100 (TOT)
25 20 15 10 5 0
CIS-100 (TOT)
30 20 10 0
CIS-100 (TOT)
40 30 20 10 0
CIS-100 (TOT)
Eyetech (DIA)
25 20 15 10 5 0
Eyetech (DIA)
30 20 10 0
Eyetech (DIA)
40 30 20 10 0
Eyetech (DIA)
Horiba partica LA-950
25 20 15 10 5 0
30 20 10 0
40 30 20 10 0
05 510 1015 1520 2025 2530 3035 3540 4045 4550 5055 5560 6065 6570 7075 7580 8085 8590
04 48 812 1216 1620 2024 2428 2832 3236 3640 4044 4448 4852 5256 5660 6064
Grain size class (m)
Fig. 5. Percentage proportion of 18 (sediments A and B) and 16 (sediments C and D) grain-size fractions.
04 48 812 1216 1620 2024 2428 2832 3236 3640 4044 4448 4852 5256 5660 6064
80
16
D. Goossens
16
sediment A
12
S = Sedigraph 5100 M = Malvern mastersizer S L = Coulter LS 200 T = CIS-100 (TOT) F = Fritsch analysette 22 C A = Atterberg cylinder P = Horiba partica LA-950 E = Eyetech (DIA) C = Coulter multisizer 3 H = Histolab
sediment B
12 S M
Skewness
A 08 S F T P L 04 M E H C 00
30
Skewness
08
T P F A E C
04
00 40
sediment C
25 20 15 S 10 05 00 E A C P 05 H 00 10 M
sediment D
35 30
Skewness
Skewness
25 20 15
L T
F A P E C
Fig. 6. Skewness of the 40 distributions shown in Fig. 5. (Techniques are ranked according to the average numerical result for the four sediments.)
analysis based on the criteria of Tabachnick & Fidell (1996) shows that, despite the differences in the diagrams, all distributions for the sediments A and B do not differ from a normal distribution. The sediments C and D, on the other hand, are much more skewed, except for Histolab and the Coulter Multisizer 3 (and, for sediment C, the CIS-100 and EyeTech). Looking at the kurtosis (Fig. 7) the patterns are generally comparable for the sediments B, C and D (but note the different behaviour of the Sedigraph for sediment C). The pattern for sediment A, on the other hand, is different. Histolab, Coulter Multisizer 3 and EyeTech always showed a negative kurtosis (platykurtic distribution). For the other methods there is no general trend although the Malvern distributions were usually leptokurtic (positive kurtosis) and those of the Atterberg and Horiba platykurtic.
Clay content, sand content, PM20 fraction

Figure 8 shows the percentage proportion of the clay fraction (<2 lm) in the samples. A direct comparison of the data is somewhat risky because the techniques have different ranges at the ne end of the grain-size spectrum (see also Table 2).
The percentages shown in Fig. 8 are those provided by the instruments, and it is useful to examine them because just these data are used by most researchers for further calculations or applications. Figure 8 shows that the trends are comparable for the four sediments. The optical methods based on image analysis (EyeTech, Histolab) measured nearly no clay. This situation is understandable because many clay particles were smaller than the pixels of the images (minimum size of a particle to be measured was 08 lm for Histolab and 07 lm for the EyeTech). The fact that these particles were smaller, restricts the usefulness of these techniques when relatively broad grain-size spectra need to be analysed. For narrow spectra (PM25 or PM10 for instance) optical methods remain useful: images should then be analysed using scanning electron microscopy (SEM) or similar high-resolution technology. On the other hand, the Sedigraph, Malvern, Coulter LS 200 and Fritsch always measured high percentages of clay compared with the other instruments. Studies comparing laser diffraction with sedimentation (more specically, pipette) demonstrated that instruments based on laser diffraction systematically over-estimate the clay content

20 20
81
sediment A
10
M = Malvern mastersizer S S = Sedigraph 5100 L = Coulter LS 200 F = Fritsch analysette 22 C T = CIS-100 (TOT) A = Atterberg cylinder P = Horiba partica LA-950 E = Eyetech (DIA) C = Coulter multisizer 3 H = Histolab
M 10 S
sediment B
Kurtosis
00
Kurtosis
00
10
10
20
40
20
100
sediment C
30 20 M L F 10 00 10 20 S T
sediment D
80 M 60 S
Kurtosis
Kurtosis
40 20
F T A
P E C H
E A P C H
00 20
Fig. 7. Kurtosis of the 40 distributions shown in Fig. 5. (Techniques are ranked according to the average numerical result for the four sediments.)
25
sediment A
4
E = Eyetech (DIA) H = Histolab T = CIS-100 (TOT) C = Coulter multisizer 3 P = Horiba partica LA-950 A = Atterberg cylinder F = Fritsch analysette 22 C L = Coulter LS 200 M = Malvern mastersizer S S = Sedigraph 5100
sediment B
M L F S 20 C
Clay content (%)
Clay content (%)
15
P M A F L
10
A 1 E H T P
5 T 0
45
C E H
0
25
sediment C
20
40 35
sediment D
Clay content (%)
Clay content (%)
M L F S
30 25 20 15 10
S M F L
15
10
A C P
C T E H
5 E H T
5 0
Fig. 8. Percentage of clay (fraction <2 lm) measured by the 10 techniques tested. (Techniques are ranked according to the average numerical result for the four sediments.)
82
D. Goossens grains, sometimes only one, in a sample. This problem is addressed later. To conclude the study of individual fractions, the proportion of PM20 (particles <20 lm) in the samples was considered. Figure 10 shows that, in general, Histolab and EyeTech measured the lowest PM20 whereas the Sedigraph and CIS-100 always measured high PM20. Notice also that the Horiba systematically detected less PM20 than the three other laser diffraction instruments.
compared with the pipette (McCave et al., 1986; Van Dongen, 1989; Konert & Vandenberghe, 1997; Muggler et al., 1997). Figure 8 shows that the same is true for the Atterberg technique (which uses the same principle as the pipette) when compared with the Malvern, Coulter LS 200 and Fritsch. The results of this study also indicate that the Horiba Partica LA-950, which also uses laser diffraction, does not follow this trend. For three of the four sediments the clay content measured by the Horiba was below that measured by the Atterberg technique, and for sediment A the Horiba even measured no clay at all. The Horiba results also deviate substantially from those of the other laser diffraction instruments tested. Looking at the sand fraction (>65 lm), the trends are almost identical for the two sediments that effectively contained sand (Fig. 9). The Sedigraph and (especially) the CIS-100 and Atterberg detected only very little sand, whereas the Malvern and Fritsch detected much more sand. Notice also the difference in behaviour of Histolab in the case of the two sediments. This difference illustrates the sensitivity of this method to the accidental presence of only a few coarse
Reproducibility
Finally, the reproducibility of the techniques is investigated. Ten repetitions were made of each analysis for that purpose. Because several of the techniques do not permit re-use of the sample, 10 subsamples for each sediment were used (see section Presentation, sediments and procedure) and 10 separate analyses were performed for each sample. For Histolab the 10 repetitions were made by dividing the image elds into 10 groups, as explained earlier. Figure 11 shows the 10 cumulative curves for each of the 40 combinations tested. The patterns are similar for the four sediments but signicant differences were observed with respect to the techniques. The instruments based on laser diffraction showed very high reproducibility. This result is further illustrated in Fig. 12, which shows the standard deviations (STD) (for the sediments A and B) and the interquartile ranges (IQR) (for the sediments C and D). Standard deviations were used for the sediments A and B because for these samples the grain-size distribution does not differ statistically from a normal distribution (see earlier). The distributions of the sediments C and D are much more skewed and therefore the interquartile range is used. In Fig. 12 the STD and IQR are shown for: (i) the median grain diameter (upper four diagrams); and (ii) the combination of all 18 (or 16) grainsize fractions analysed (lower four diagrams). The values in the lower diagrams represent the average of the STD (or IQR) of all classes. The trends are identical in all images (local exceptions occur, but are rare); they show high reproducibility (low STD and IQR) for the four laser diffraction instruments, moderate reproducibility for the two sedimentation techniques (Atterberg, Sedigraph) and much lower reproducibility for the four methods based on analysis of individual particles (Coulter Multisizer 3, EyeTech, CIS-100, Histolab). The same trends appear in the cumulative curves (Fig. 11) and
15
sediment A
T = CIS-100 (TOT) A = Atterberg cylinder S = Sedigraph 5100 C = Coulter multisizer 3 E = Eyetech (DIA) L = Coulter LS 200 P = Horiba partica LA-950 F = Fritsch analysette 22 C H = Histolab M = Malvern mastersizer S
Sand content (%)
10
M F P L E C
S 0 12 T A
sediment B
10
T = CIS-100 (TOT) A = Atterberg cylinder S = Sedigraph 5100 C = Coulter multisizer 3 E = Eyetech (DIA) L = Coulter LS 200 P = Horiba partica LA-950 F = Fritsch analysette 22 C H = Histolab M = Malvern mastersizer S
Sand content (%)
8 6 4 2 0
M F L C E H P
S T A
Fig. 9. Percentage of sand (fraction >65 lm for sediments A and B and fraction >64 lm for sediments C and D) measured by the 10 techniques tested. (Techniques are ranked according to the average numerical result for the four sediments.)

50 60
83
sediment A
40
H = Histolab E = Eyetech (DIA) P = Horiba partica LA-950 A = Atterberg cylinder M = Malvern mastersizer S L = Coulter LS 200 F = Fritsch analysette 22 C C = Coulter multisizer 3 T = CIS-100 (TOT) S = Sedigraph 5100
sediment B
50
PM20 content (%)
PM20 content (%)
40 30
S T
30 C 20 M 10 H E A P L F T S
F M P 20 10 0 A H E L C
sediment C
sediment D
100
PM20 content (%)
PM20 content (%)
T E P A M L F C
100 S 80 60 H 40 20 0 E P A M L F C
T S
80 60 40 20 0 H
Fig. 10. Percentage of PM20 (fraction <20 lm) measured by the ten techniques tested. (Techniques are ranked according to the average numerical result for the four sediments.)
they will be discussed in more detail in the next section. An effort was also made to study reproducibility as a function of the grain-size. Relative STD and IQR values were calculated for all 18 (or 16) grainsize fractions, for all techniques. The relative STD and IQR quantify the deviation of a technique relative to the reference technique (dened here as the average of the four physical principles investigated in this study, see the next section for more information) and were obtained by dividing the STD (or IQR) of a class by that of the same class but for the reference technique. Results are depicted in Fig. 13. To facilitate interpretation, the average curve of the four sediments was calculated. Although there is signicant scatter in the pictures the general trends are clear. The pattern is more or less comparable for the four laser diffraction instruments (Malvern, Coulter LS 200, Fritsch, Horiba), which all show a bowl-shaped curve with (relatively) low reproducibility in the nest fractions, higher reproducibility in the intermediate fractions, and (except the Horiba) again lower reproducibility in the coarse fractions. Note that the zone of optimum reproducibility varies slightly by instrument: 30 to 40 lm for the Malvern, 25 to 35 lm for the Coulter LS 200, 30 to 44 lm for the Fritsch, and 40 to 45 lm for the
Horiba. The Coulter Multisizer 3 also shows a bowl-shaped curve, but its reproducibility is much lower than that of the laser diffraction instruments. The minimum in the curve (zone of highest reproducibility) is situated between 45 and 65 lm. The Sedigraph curve closely resembles that of the Horiba although reproducibility is better for the latter than for the former. The CIS-100 curve is more irregular and difcult to interpret, but the reproducibility of this instrument is distinctly worse than that of the laser diffraction instruments and the Sedigraph. Reproducibility of the other two optical methods (EyeTech and Histolab), nally, decreases with increasing grain-size; this trend is very pronounced for Histolab (Fig. 13). Note also the very low reproducibility of this technique for grain-sizes >40 lm. Interpretation of these trends appears in the next section. Because of the difference in behaviour of the Atterberg curves, no average curve was calculated for this technique and no analysis of the reproducibility as a function of the grain-size was made.
EVALUATION AND DISCUSSION Because each technique is based on a particular physical principle, a perfect method for
84
D. Goossens
sediment A
100 80 60 40 20 0 0 100 80 60 40 20 0 0 100 80 60 40 20 0 0 100 80 60 40 20 0 0 20 40 60 20 20 100 80 60 40 20 0 0 100 80 60 40 20 0 0 100 80 60 40 20 0 0 100 80 60 40 20 0 0 20 40 60 20 20
sediment B
100 80 60 40 20 0 0 100 80 60 40 20 0 0 100 80 60 40 20 0 0 100 80 60 40 20 0 0
sediment C
100 80 60 40 20 0 0 100 80 60 40 20 0 80 100 80 60 40 20 0 80 100 80 60 40 20 0 80 0 0 0
sediment D
20 40 60 80 100
20 40 60 80 100
20 40 60 80
20 40 60 80
Sedigraph 5100
40 60 80 100
Sedigraph 5100
40 60 80 100
Sedigraph 5100
20 40 60
Sedigraph 5100
20 40 60 80
Atterberg cylinder
40 60 80 100
Atterberg cylinder
40 60 80 100
Atterberg cylinder
20 40 60
Atterberg cylinder
20 40 60 80
Histolab
80 100
Histolab
80 100
Histolab
20 40 60
Histolab
20 40 60 80
100 80 60 40 20 0 0 100 80 60 40 20 0 0 100 80 60 40 20 0 0 100 80 60 40 20 0 0 100 80 60 40 20 0 0

100 80 60 40 20 0 0 20
100 80 60 40 20 0 0 100 80 60 40 20 0 0 100 80 60 40 20 0 0 100 80 60 40 20 0 0 100 80 60 40 20 0 0

100 80 60 40 20 0 0 20
100 80 60 40 20 0 0 100 80 60 40 20 0 0 100 80 60 40 20 0 0 100 80 60 40 20 0 0 100 80 60 40 20 0 0

100 80 60 40 20 0 0 20
100 80 60 40 20 0 80 100 80 60 40 20 0 80 100 80 60 40 20 0 80 100 80 60 40 20 0 80 100 80 60 40 20 0 80

100 80 60 40 20 0 80 0 20
Coulter LS 200
20 40 60 80 100
Coulter LS 200
20 40 60 80 100
Coulter LS 200
20 40 60
Coulter LS 200
0 20 40 60 80
20 40 60 80 100
20 40 60 80 100
20 40 60
0 20 40 60 80
20 40 60 80 100
20 40 60 80 100
20 40 60
0 20 40 60 80
CIS-100 (TOT)
20 40 60 80 100
CIS-100 (TOT)
20 40 60 80 100
CIS-100 (TOT)
20 40 60
CIS-100 (TOT)
0 20 40 60 80
Eyetech (DIA)
20 40 60 80 100
Eyetech (DIA)
20 40 60 80 100
Eyetech (DIA)
20 40 60
Eyetech (DIA)
0 20 40 60 80

40 60 80 100

40 60 80 100

40 60

40 60 80
Grain size (m)
Grain size (m)
Grain size (m)
Grain size (m)
Fig. 11. Cumulative grain-size curves of the ten repetitions, for the 40 combinations of sediment type and grain-size technique.

40 35
F = Fritsch analysette 22 C L = Coulter LS 200 P = Horiba partica LA-950 M = Malvern mastersizer S A = Atterberg cylinder S = Sedigraph 5100 C = Coulter multisizer 3 E = Eyetech (DIA) T = CIS-100 (TOT) H = Histolab
85
H
45
sediment A
H 40
Standard deviation (m)
30 25 20 15
35 30 25 20 15 10 05 00 25
sediment B
T
T C S
E M S A F L P C
10 05 00 20 18 F M L P A
Interquartile range (m)
16 14 12 10 08 06 04 02 00
sediment C
T
H 20
15
sediment D
10 S 05 F 00 L P M A
E T
P L F M
30 25 20 15 10
35
sediment A
T
30 25 20 15
sediment B
E A
C S
C 10 05 F 00 25 L P S M
05 F 00 25 L P A M
20
C E
15
sediment C
T
H 20
15
sediment D
T C E
10
10 M F 00 L P A S
05 L F 00 M P
05
Fig. 12. Standard deviation STD (sediments A and B) and interquartile range IQR (sediments C and D) for the 10 repetitions. Upper four gures: STD and IQR for the median grain diameter; lower 4 gures: average STD and IQR for the 18 (sediments A and B) or 16 (sediments C and D) grain-size classes shown in Fig. 5. (Techniques are ranked according to the average numerical result for the four sediments.)
86
D. Goossens
Relative STD (sediments A and B) or relative IQR (sediments C and D)
12 10 08 06 04 02 00 0 20 40 60
sediment A sediment B sediment C sediment D average curve
14
15
Coulter LS 200
12
09
06
03
00 80 100 0 20 40 60 80 100
Grain size (m)

10 20
Grain size (m)
08

16
06
12
04
08
02
04
00 0 20 40 60 80 100
00 0 20 40 60 80 100
Grain size (m)

Grain size (m)

24
70
60 50 40 30 20 10 00 0 20 40 60
Sedigraph 5100
20 16 12 08 04 00
80
100
20
40
60
80
100
Grain size (m)

50 70
Grain size (m)
Atterberg cylinder
40
sediment A sediment B sediment C sediment D
Histolab
60 50 40 30 20 10 00
30
20
10
00 0 20 40 60 80 100
20
40
60
80
100
Grain size (m)

60 60
Grain size (m)
CIS-100 (TOT)
50 40 30 20 10 00 0 20 40 60
Eyetech (DIA)
50 40 30 20 10 00
80
100
20
40
60
80
100
Grain size (m)
Grain size (m)
Fig. 13. Relative standard deviation (sediments A and B) and relative interquartile range (sediments C and D) as a function of the grain-size.
Grain-size distributions of loamy sediments determining the true grain-size distribution of sediment does not exist. Evaluating grain-size techniques is thus a subjective operation. However, one objective criterion is reproducibility, and this aspect is investigated in more detail below. Other criteria are analysis time, analytical range, resolution of an analysis and data processing. These criteria are also discussed in this section.
87
Reproducibility
Figures 11 to 13 illustrate the great difference in reproducibility for the 10 techniques. The laser diffraction instruments all score very highly for this criterion. The diffraction patterns are created by an accumulation of a (very) large number of individual grains. It is true that each detector records information for a selected zone of the grain-size spectrum, but that information is also created by a large number of grains. Small variations in the grain-size distribution of a sample will thus create only small differences in the global diffraction pattern. The two sedimentation methods (Atterberg, Sedigraph) also consider a vast amount of grains. A relatively high level of reproducibility can thus be expected, but the experimental protocol of the Atterberg technique is rather complex and this introduces errors. Moreover, for practical reasons the Atterberg technique allows identication of only a limited number of grain-size classes. Interpolation may help to get more information (as illustrated in this study), but it inevitably introduces new error. The Sedigraph, in its turn, executes a vertical scan through the settling solution in the measuring cell. The grain-size data are thus also derived from a large number of particles, but less than in the Atterberg technique. On the other hand, the Sedigraph procedure is fully automated and this helps reduce the error. This study showed higher reproducibility for the Atterberg technique compared with the Sedigraph. The other methods tested (Histolab, EyeTech, Coulter Multisizer 3 and CIS-100) measure individual particles. The grain-size distribution of the sediment is obtained by integrating the results. These techniques always showed low levels of reproducibility. The number of particles analysed during a measurement is lowest for the Coulter Multisizer 3 (for the four sediments tested in this study it varied from a few hundred to a maximum of a few thousands), followed by EyeTech (a few thousands), Histolab (a few tens of thousands) and the CIS-100 (always several tens of thousands
or more). Despite the very low number of particles analysed the reproducibility of the Coulter Multisizer 3 remains reasonable, because the grain volume is directly derived from the impedance measurements. No complex data processing is thus necessary. However, the Coulter Multisizer curves in Fig. 11 show a clear drop in reproducibility in the coarse particle range (especially for the sediments C and D). Similar trends were observed in the EyeTech and, especially, the CIS100 and Histolab curves. Because the data were calculated as volume percentages the coarse grains have a much larger impact on the grainsize distribution than the ne grains. The presence of only a few, sometimes a single, coarse grain(s) in a sample may substantially affect the behaviour of the grain-size curve near the coarse end of the spectrum. The cumulative curves in Fig. 11 illustrate this problem very clearly. The most imprecise technique tested in this study is Histolab. It analyses the grains in two dimensions (ab-plane) only, and the data for the third dimension (c-axis) should be reconstructed by using alternative procedures, which explains the very low level of reproducibility for this method (see Figs 12 and 13). The EyeTech and CIS-100 also measure in two dimensions (ac-plane) but they are less imprecise because the orientation of the grains in the ab-plane (perpendicular to the c-axis) is arbitrary. This study also showed that the reproducibility of the CIS-100 is lower than that of the EyeTech despite the larger number of grains analysed by the former (Fig. 11); especially for the coarse grainsize fractions, the CIS-100 does not operate well.
Analysis time
Although analysis time is a less important factor than reproducibility (especially from a scientic perspective) it can be of considerable practical signicance if many samples are to be analysed. Instruments based on laser diffraction always score highly for this criterion because they take only a few seconds to measure the grain-size distribution. The CIS-100 (TOT), the Coulter Multisizer 3 (electrical sensing zone (ESZ) method) and Histolab (SIA) also work very rapidly, but the latter two methods require signicant extra data processing (see Table 2) and the total time for achieving the nal result is much longer than that for the CIS-100 and the laser diffraction instruments. The Sedigraph and the EyeTech require a few minutes to measure the grain-size distribution, but no complex data
Table 2. Comparison of the techniques. Criterion Resolution of analysis (number of classes) Extra data processing 92 62 64 93 66
88
Technique
D. Goossens
Instrument Excellent Excellent Excellent Excellent Very good Seconds Seconds Seconds Seconds Hours 03752000 011250 0059004 0013000 01655
Working-principle
Reproducibility1
Analysis time2
Analytical range (lm)
Coulter LS 200 Fritsch Analysette 22c Malvern Mastersizer S Horiba Partica LA-950 Atterberg cylinder
Laser diffraction Laser diffraction Laser diffraction Laser diffraction Sedimentation
Sedigraph 5100 220
Sedimentation
Good
Minutes
013007
Coulter Multisizer 3
Impedance measurements Bad Very bad Very bad Seconds Seconds 013600 Depends on microscope used Minutes 07640011 N.A.12 600 N.A.12
Bad
Seconds
0412008
2569
EyeTech
None if desired classes are pre-selected3 None if desired classes are pre-selected3 None if desired classes are pre-selected3 None if desired classes are pre-selected3 If desired, transformation of mass percentages to volume percentages (grain density data required) Interpolation of grain-size data (if information for more than 6 classes is requested) If desired, transformation of mass percentages to volume percentages (grain density data required) Analysis in different steps may be necessary Data of steps should be combined None if desired classes are pre-selected13 None if desired classes are pre-selected3 Measurement of c-diameters Calculation of particle volumes Calculation of grain-size distribution
CIS-100 Histolab
Dynamic Image Analysis10 Time-of-Transition14 Static Image Analysis
Based on the results of this study. Excluding pre-treatment of the samples, rinsing of equipment and processing of the data. 3 Data are calculated from standard classes via interpolation. 4 Standard range (extended range 0053500 lm available). 5 Quartz grains in water (range depends on grain density and uid density). 6 Standard procedure (other options possible). 7 Range depends on grain density and uid density. 8 Range depends on aperture diameter. Minimum diameter is 04 lm (20 lm aperture), maximum diameter is 1200 lm (2000 lm aperture). 9 Per aperture diameter. 10 The EyeTech also has a Time-of-Transition unit. 11 Lower limit depends on lens used; minimum that can be reached is 07 lm. 12 Data are for individual particles. 13 Data are calculated from particle data set. 14 The CIS-100 also has a Dynamic Image Analysis unit.
Grain-size distributions of loamy sediments processing is needed. The slowest method tested in this study is the Atterberg technique. More than two hours are required to complete the sedimentation procedure, and the samples must be dried and weighed after their extraction from the cylinder. This technique is not recommended when there are many samples to process.
89
classes can be measured towards the nest end of the grain-size spectrum).
Extra data processing

Post-analysis data processing differs greatly from instrument to instrument. If volume data are requested, no extra processing is needed for the laser diffraction instruments, the EyeTech and the CIS-100. Sedimentation methods measure the grain-size in terms of mass and a recalculation (using grain density information) is necessary to express the result in terms of volume. The Atterberg technique also requires considerable data interpolation if detailed information is needed for the fractions >16 lm. Considerable data processing (though less than for the Atterberg technique) is also required for the Coulter Multisizer 3, at least if results obtained with different probes are to be combined. No extra processing is needed for this instrument when only a single probe is used. Histolab is the most time-consuming technique tested in this study. Measuring is very fast, but additional measurements of the c-diameter, calculations of the volume of each particle, and the nal calculation of the grain-size distribution are necessary. This method is not recommended for determining the grain-size distribution in terms of volume, or mass.
Analytical range
The analytical range within which grain-size data is measured varies considerably from one instrument to the next. All techniques tested are able to measure particles <1 lm (Table 2), but the maximum size varies from 65 lm (Atterberg cylinder, for quartz in water) to 6400 lm (EyeTech). The widest range is provided by the optical methods (from <1 lm to >3600 lm; Histolab can measure much coarser grains), followed by the laser diffraction method (from <1 lm to 3000 lm), the electrical sensing zone method (from <1 lm to 1200 lm) and the sedimentation methods (from <1 lm to maximum 300 lm). Although the lowest measurable particle size is always <1 lm it differs from instrument to instrument, and this has consequences when the clay content of a sample needs to be measured. It can be expected that the rather high lower limit of the EyeTech and Coulter Multisizer 3 are at least partially responsible for the low percentages of clay that are measured by these instruments (see Fig. 8), but also note that the CIS-100 measures little clay despite a lower limit of 01 lm. The results produced by Histolab depend on the microscope used and even extremely small particles can be measured with this technique if appropriate microscopes such as SEMs are used.
Comparison with a reference technique

An attempt was also made to evaluate how the 10 methods related to a reference technique producing optimum grain-size distributions. Four physical principles were tested in this study (laser diffraction, sedimentation, impedance measurements and optical measurements), but the number of instruments differed for each principle. Taking the average of all 10 techniques as the reference would advantage those instruments that are members of a large physical principle group; therefore, the reference was taken as the average of the four physical principles. In a rst step the average relative deviation of each technique from the reference was checked by calculating the coefcient: n xi 1X 1 R n i1 Xi where xi is the percentage proportion of the idth grain-size class in the total sediment; Xi the percentage proportion of the idth grain-size class measured by the reference method; n the number
Resolution of an analysis
The resolution (number of grain-size classes) varies considerably according to a technique (Table 2). Several instruments allow the operator to pre-select classes freely, but if classes are preselected the instrument interpolates the data from the standard classes it measures directly. The numbers in Table 2 refer to the standard classes. The TOT technique shows the highest resolution (up to 600 classes), followed by the ESZ technique (256 classes, but if measurements with different aperture diameters are combined more classes can be measured), the Sedigraph (220 classes), the laser diffraction technique (between 62 and 93 classes) and the Atterberg technique (six classes in the standard procedure, but more
90
D. Goossens where n is the number of grain-size classes; xi the percentage proportion of the idth grain-size class in the total sediment, measured by technique x; yi the percentage proportion of the idth grain-size class in the total sediment, measured by technique y; calculates the average disagreement between the methods x and y. The higher the C value, the more the grain-size distributions measured by the methods x and y differ from each other. To investigate the behaviour of a method relative to all techniques (not just one other x can be calculated, technique) the average C where Cx is the average of the C-coefcients of all combinations of method x with other methods. In this study 10 methods were tested; the number of combinations for each method is therefore x is thus the average of the nine Cequal to nine. C x , the more the values for method x. The higher C grain-size data measured by method x differ from those of the ensemble of the other techniques. Figure 15 shows the average C-coefcients. This picture resembles that in Fig. 14, but the four laser diffraction instruments now appear in a single group to the left in the gures. Higher x -values were obtained for the Coulter MultiC sizer 3, followed by the sedimentation methods
of grain-size classes (the classes shown in Fig. 5 were used; therefore n 18 for sediments A and B and n 16 for sediments C and D). When the grain-size distribution measured by a technique perfectly coincides with that of the reference method, then R 0; the more it deviates from the reference (regardless of whether the sample is measured as coarser or ner) the higher R becomes. Figure 14 shows the R-coefcients. Differences occur between the sediments, but the instruments based on laser diffraction (Horiba, Fritsch, Coulter LS 200, Malvern) and the Coulter Multisizer 3 generally show the smallest differences with the reference (low R-value). Greater differences were observed for the sedimentation methods (Sedigraph, Atterberg cylinder). Highest R-values were measured for the optical methods (EyeTech, CIS100 and Histolab). Especially, Histolab differs strongly from the reference (see Fig. 14). An alternative way to rank the methods is by studying the grain-size results relative to the combination of all techniques. The coefcient: C
n 1X n i 1
q xi yi 2
12 10
R-coefficient
R-coefficient
08 06 04 02 00 25
P = Horiba partica LA-950 F = Fritsch analysette 22 C L = Coulter LS 200 C = Coulter multisizer 3 M = Malvern mastersizer S S = Sedigraph 5100 A = Atterberg cylinder E = Eyetech (DIA) T = CIS-100 (TOT) H = Histolab
12
sediment A
H 10 08 06 04 02 00 18
M S C
sediment B
M E S A
T H
A E
F P L C
20
R-coefficient
R-coefficient
15
sediment C
16 H 14 12 10 08 06 04
sediment D
T A C M S E
10 S M E A T
L P F
05 P 00 F
02 00
Fig. 14. R-coefcients for the four sediments and ten techniques tested. (Techniques are ranked according to the average numerical result for the four sediments.)
Grain-size distributions of loamy sediments (Atterberg and Sedigraph). The optical methods (EyeTech, CIS-100 and Histolab) showed the least agreement with the other techniques. A clear ranking is thus observed, which is controlled by the physical principle on which a measurement is based. The behaviour of the techniques can also be studied as a function of the grain-size. Figure 16 shows, for the 18 (sediments A and B) or 16 (sediments C and D) grain-size classes, the ratio T xi/Xi (xi and Xi were dened earlier). The gure shows, for each grain-size class, whether a technique overestimates (T > 1) or underestimates (T < 1) the proportion of that class relative to the reference method (average of the four physical principles investigated). The trends are identical for the four sediments except for the Atterberg cylinder, where the results for the sediments A and B differ from those of the sediments C and D. A thorough description of each curve in Fig. 16 would result in a too complex discussion; here only the main points are summarized. The four laser diffraction instruments show similar curves, with higher T-values in the ne and the coarse particle range and lower T-values in the intermediate particle range (but note the low T-value for the Horiba instrument below 15 lm
45 40
91
for sediment A). Moreover, note the pronounced over-estimation of the coarse particle fractions (except the coarsest ones) for Histolab, the prominent under-estimation of these fractions for the CIS-100, and the difference in behaviour (in the same fractions) of the Atterberg technique between the sediments A and B (large underestimation) and the sediments C and D (signicant over-estimation).
Consequences for textural classication

This study has shown that the result of grain-size analysis may vary considerably according to the method or instrument used. It is important to check whether the variety in results can affect the classication of sediment. Natural sediments may be classied according to various criteria, but it is a common procedure to characterize sediment based on its textural composition. Figure 17 shows, for the four sediments tested in this study, the position of each method in a soil texture triangle. The textural classes in the triangle are those of the United States Department of Agriculture (USDA) classication. Other classications exist, but the USDA system is used in many soil studies and it makes a coherent
50
Average C-coefficient
35 30 25 20
H S A C M E T
L = Coulter LS 200 F = Fritsch analysette 22 C P = Horiba partica LA-950 M = Malvern mastersizer S C = Coulter multisizer 3 A = Atterberg cylinder S = Sedigraph 5100 E = Eyetech (DIA) T = CIS-100 (TOT) H = Histolab
sediment A
45 40 35 30 25 20 15 10 05 00 50 45
sediment B
T S M A C E
F L
15 10 05 00 50 45
sediment C
40 35 30 25 20 15 10 05 00
40 35 30 25 20 15 10 05 00
E S M C A
sediment D
T E
S M C A
Fig. 15. Average C-coefcients for the four sediments and 10 techniques tested. (Techniques are ranked according to the average numerical result for the four sediments.)
92
D. Goossens
40 35 30 25
Malvern mastersizer S Fritsch analysette 22 C Coulter LS 200
50
sediment A (part 1)
45 40 35
Sedigraph 5100 Coulter multisizer 3
sediment A (part 2)
CIS-100 (TOT)
Eyetech (DIA) Histolab

Atterberg cylinder
T-ratio
T-ratio
05 m
30 25 20 15
20 15 10
10 05 00
1015 m 1520 m 2025 m 2530 m 3035 m 3540 m 4045 m 4550 m 5055 m 5560 m 6065 m 6570 m 7075 m 7580 m 8085 m 8590 m 510 m
05 00
05 m 1015 m 1520 m 2025 m 2530 m 3035 m 3540 m 4045 m 4550 m 5055 m 5560 m 6065 m 6570 m 7075 m 7580 m 8085 m 8085 m 5660 m 5660 m 8590 m 6064 m 6064 m 8590 m 510 m
Grain size class

40 35 30 25
Grain size class

40
sediment B (part 1)
35 30 25
sediment B (part 2)
CIS-100 (TOT)

Atterberg cylinder
T-ratio
T-ratio
05 m 510 m
20 15 10 05 00
1015 m 1520 m 2025 m 2530 m 3035 m 3540 m 4045 m 4550 m 5055 m 5560 m 6065 m 6570 m 7075 m 7580 m 8085 m 8590 m
20 15 10 05 00
05 m 510 m 1015 m 1520 m 2025 m 2530 m 3035 m 3540 m 4045 m 4550 m 5055 m 5560 m 6065 m 6570 m 7075 m 4852 m 4852 m 7580 m 5256 m 5256 m
Grain size class

40 35 30 25
Malvern mastersizer S Fritsch analysette 22 C Coulter LS 200 Horiba partica LA-950 Atterberg cylinder
Grain size class

80
sediment C (part 1)
70 60 50
sediment C (part 2)
CIS-100 (TOT)
T-ratio
T-ratio
812 m
20 15 10 05 00
04 m 48 m 1216 m 1620 m 2024 m 2428 m 2832 m 3236 m 3640 m 4044 m 4448 m 4852 m 5256 m 6064 m 5660 m
40 30 20 10 00
812 m 04 m 48 m 1216 m 1620 m 2024 m 2428 m 2832 m 3236 m 3640 m 4044 m 4044 m 4448 m 4448 m
Grain size class

50 45 40 35
Grain size class

80
sediment D (part 1)
70 60 50
sediment D (part 2)
CIS-100 (TOT)

Atterberg cylinder
T-ratio
T-ratio
812 m
30 25 20 15
40 30 20
10 05 00
04 m 48 m 4448 m 1216 m 1620 m 2024 m 2428 m 2832 m 3236 m 3640 m 4044 m 4852 m 5256 m 5660 m 6064 m
10 00
812 m 04 m 48 m 1216 m 1620 m 2024 m 2428 m 2832 m 3236 m 3640 m
Grain size class
Grain size class
Fig. 16. T-ratios as a function of the grain-size. To keep the diagrams readable the Malvern, Fritsch, Coulter LS 200, Horiba and Atterberg curves are shown on the left and those of the Sedigraph, Coulter Multisizer 3, CIS-100, EyeTech and Histolab on the right.
93
sediment A
100 90 80 70 60 percent clay 40 30 sandy clay loam 20 sandy loam 10 sand 100 loamy sand 90 80 70 60 50 loam siltloam 90 50 sandy clay clay loam 10 20 30 clay 40 50 silt y cla y silty clay loam 60
sediment B
100 90 80 70 60
percent silt
10 20 30 clay 40 50 silt y cla y clay loam silty clay loam 60 70 80 loam siltloam percent silt
percent clay 40
50 sandy clay sandy clay loam
70
30
80
20 sandy lo am 10
100
S Asilt C H
10
90 100
H
40
MFL CA S EP T
30 20 10
silt
sand 100
loamy sand 90 80 70 60 50 40
M P F L E
30
20
percent sand
percent sand
sediment C
100 90 80 70 60 percent clay 40 30 sandy clay loam 20 sandy loam 10 sand 100 loamy sand 90 80 70 60 50 40 30 20 loam silt loam 50 sandy clay clay loam 10 20 30 clay 40 50 silty clay silty clay loam 60
sediment D
100 90 80 70 60
percent silt
10 20 30 clay 40 50 silty clay clay loam silty clay loam 60 70 percent silt
percent clay 40
50 sandy clay sandy clay loam
70
30
80
20
S M
loam silt loam
80
A silt PC 100 H T E
10
M LF S
90
sandy lo am 10 sand 100 loamy sand 90 80 70 60
LF 90 AP C
silt
T 100 HE
50
40
30
20
10
percent sand
percent sand
Fig. 17. Location of the ten techniques in the soil texture triangle, for the four sediments tested. Textural classes correspond to those of the USDA classication system.
distinction between the most common types of sediment. Figure 17 shows that sediment may be classied differently depending on the grain-size technique adopted. The picture is very clear for the sediments A, B and (especially) D. For sediments A, B and C the techniques are situated in two classes (silt and silt loam) and, for sediment D, in three classes (silt, silt loam, silty clay loam). This study only investigated loamy sediments (sediments composed predominantly of silt and clay particles), but it can be expected that similar trends will occur when other types of sediment are analysed. The selection of a grain-size anal-
ysis technique is thus important: it may well affect the textural classication of sediment.
CONCLUSIONS The most important (though not surprising) conclusion of this study is that there is no optimum technique to measure the grain-size distribution of loamy sediments. Four sediments were analysed with ten techniques, and although the trends were generally similar local differences were observed between the sediments. The choice of a technique thus depends on the type of sediment
94
D. Goossens slowly (up to two hours or more are needed for one analysis) and produces results for only a limited number of grain-size classes. Interpolation of the data is necessary when more detailed information is needed, but this introduces new experimental error. The EyeTech and CIS-100 instruments operate fast, but the results showed less reproducibility compared to the previous techniques. The ne (<5 lm) and coarse (>60 lm) fractions were also less accurately measured (no problems were observed for the intermediate part of the grain-size spectrum). Histolab, nally, is very time-consuming: measurement is fast, but considerable processing of the data is required. Histolab also produced data that differed significantly from that of the other techniques. Although the nal choice of a grain-size technique thus depends on many factors it can be summarized that instruments based on laser diffraction offer many advantages and generally work adequately, whereas instruments based on optical measurements are less recommendable for analysing the grain-size of loamy sediments. However, instruments based on optical techniques permit measuring of the shape of particles and thus provide important complementary information. It should also be noted that the sediments tested in this study contained no particles >90 lm. No information was thus provided for coarser sediments and it is quite probable that, for such sediments, optical methods might score better than they do for silt and clay.
and on other factors. However, the results allowed the grouping of techniques in welldened classes. It is interesting to note that this classication mirrors one based on the physical principle on which the techniques operate. The laser diffraction instruments generally scored the best results for the various criteria checked in this study, followed by the Coulter counter method (ESZ technique), the sedimentation methods and the optical methods. The reasons for these results are: the number of particles analysed (the Coulter counter is an exception), the complexity of the measurement protocol (the more complex, the more experimental error), and the freedom in orientation of the grains during the measurements (very important in the case of optical measurements). The trend is very clear when the reproducibility of an analysis (Figs 11 to 13) or the difference relative to the reference technique (Fig. 14) are considered, or when a technique is compared with the combination of all techniques (Fig. 15). The ten methods also showed great variation when measuring the clay content. The optical methods recorded nearly no clay whereas the other techniques detected much more clay. The limited resolution of the images, an inevitable restriction associated with optical techniques, hampers adequate registration of the nest grains. Laser diffraction instruments generally measured higher clay contents than the Atterberg method, but less than the Sedigraph, which also uses sedimentation; they also measured higher amounts of sand than the other techniques did. Apart from the type and quantity of sediment available, the choice of an optimum grain-size analysis technique will thus also depend on the aim of the study. Different instruments may be recommended according to whether the whole grain-size spectrum or only a part of it is of interest. The complexity of a measurement is another factor, but even more important is the data processing. Laser diffraction instruments are very advantageous because the measurement protocol is very easy, the speed of measurement very high and data processing kept to a minimum (data are directly calculated as a per cent of volume). Instruments based on impedance measurements (Coulter counter technique) also work very fast and the protocol is easy but, to cover the complete grain-size spectrum, it may be necessary to analyse the sediment in different steps using different probe apertures. The Sedigraph technique is also easy but requires more time for an analysis. The Atterberg method works still more
ACKNOWLEDGEMENTS The author wishes to thank the following persons for discussion, permission to use facilities, or technical assistance during this study: A. Gaudichet and A. Chabas (Laboratoire Interuniversi` mes Atmosphe riques, Universite taire des Syste tude Paris 12, France) and G. Petit (Laboratoire dE es, Paris, France) for the des Particules Inhale Histolab measurements; N. Vandenberghe and R. Brepoels (Afdeling Geologie, Katholieke Universiteit Leuven, Belgium) for the Malvern Mastersizer and Sedigraph measurements; J. Gross (Institut fu r Physische Geographie und Landschaftso kologie, Universita t Hannover, Germany) for the Coulter LS 200 measurements; F. Ollevier and A. Wollebrants (Laboratorium voor Aquatische Ecologie, Katholieke Universiteit Leuven, Belgium) for the Coulter Counter measurements; M. Konert and J. Vandenberghe (Faculteit der Aard- en Levenswetenschappen, Vrije Univer-
Grain-size distributions of loamy sediments siteit Amsterdam, the Netherlands) for the Fritsch Analysette measurements; P. Van Der Meeren and H. Saveyn (Vakgroep Toegepaste Analytische en Fysische Chemie, Universiteit Gent, Belgium) and V. De Schepper (Vakgroep Toegepaste Wiskunde, Biometrie en Procesregeling, Universiteit Gent, Belgium) for the CIS-100 measurements; F. Devreese (Ankersmid nv, Wilrijk, Belgium) for the EyeTech measurements; and J.M. Brocas and J. ODonnell (Horiba Jobin Yvon SAS, Longjumeau, France) for the Horiba Partica LA-950 measurements. Software developed at the Vrije Universiteit Amsterdam, the Netherlands (M. Konert) was used for the Fritsch Analysette 22 C. This study was carried out as part of the EU AMMA (African Monsoon Multidisciplinary Analyses) project. Receipt of a CNRS research fellowship for D. Goossens during his stay at LISA is gratefully acknowledged.
95
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Manuscript received 21 December 2006; revision accepted 13 July 2007

Techniques To Measure Grain-Size Distributions of Loamy Sediments: A Comparative Study of Ten Instruments For Wet Analysis

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Techniques To Measure Grain-Size Distributions of Loamy Sediments: A Comparative Study of Ten Instruments For Wet Analysis

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Sedimentology (2008) 55, 6596

2007 The Author. Journal compilation 2007 International Association of Sedimentologists

Physical properties of the grains

Grain-size distributions of loamy sediments information is provided in terms of percentage of mass.

Electroresistance particle counting

PRESENTATION, SEDIMENTS AND PROCEDURE

Mass density (g cm3)

Mass density (g cm3)

Grain size class

Grain size class

Mass density (g cm3)

Mass density (g cm3)

Grain size class

Grain size class

Grain-size distributions of loamy sediments

Grain size class

Grain size class

Grain size class

Grain size class

TOT technique), it is possible to incorporate the rounding in the volume calculations.

Cumulative grain-size curves

Median grain diameter

Cumulative volume (%)

Cumulative volume (%)

Grain size (m)

Grain size (m)

Cumulative volume (%)

Cumulative volume (%)

Grain size (m)

Grain size (m)

Grain-size distributions of loamy sediments

Median grain diameter (m)

Median grain diameter (m)

Median grain diameter (m)

Median grain diameter (m)

Skewness and kurtosis

Sediment A Grain-size class

Grain-size distributions of loamy sediments

Horiba Partica LA-950

abs cum abs cum abs cum

1236 1236 021 021 1497 1497

2605 3841 979 1000 1599 3097

2342 6183 1680 2681 1166 4263

1753 7936 1887 4568 1274 5537

985 8921 1481 6049 1306 6843

419 9341 1083 7132 1078 7921

283 9624 787 7919 764 8685

136 9760 468 8387 497 9183

080 9840 353 8740 312 9494

097 9937 208 8948 197 9691

042 9979 052 9000 116 9806

021 10000 000 9000 072 9878

000 10000 000 9000 053 9932

000 10000 000 9000 030 9961

000 10000 000 9000 024 9986

000 10000 000 9000 014 10000

Grain-size distributions of loamy sediments

Horiba partica LA-950

Horiba partica LA-950

Horiba partica LA-950

Horiba partica LA-950

Grain size class (m)