Journal of Sedimentary Research, 2011, v.

81, 600–610
Research Article
DOI: 10.2110/jsr.2011.43

PARTICLE SIZE MEASUREMENT OF DIATOMS WITH INFERENCE OF THEIR PROPERTIES:

COMPARISON OF THREE TECHNIQUES

ROBERT S. PUGH1,2 AND I. NICK MCCAVE1

1
Godwin Laboratory for Palaeoclimate Research, Department of Earth Sciences, University of Cambridge, Downing Street, Cambridge CB2 3EQ, U.K.
2
British Antarctic Survey, Madingley Road, Cambridge CB3 0HT, U.K.
e-mail: mccave@esc.cam.ac.uk

ABSTRACT: Diatom-rich sediments are common in several oceanic regions, especially the Southern Ocean. Some of these are
strongly affected by bottom currents and are expected to be sorted by the flow. Examination of data on diatoms’ response by
instruments commonly used for size measurement is presented here. Diatoms are silt- to fine sand-size, filigree silica structures
of many shapes with high porosity, thus both the bulk density and shape strongly influence the ‘‘size’’ that is calculated from
measurements. We document the particle size of diatoms measured by instruments based on settling velocity (Sedigraph),
electrical resistance pulse counting (Coulter counter), and laser diffraction (Malvern laser sizer). The Malvern laser
consistently measures the largest diameters, followed by the Coulter counter and then settling-based techniques. Relationships
between these inferred sizes (all expressed as quartz-equivalent spherical diameters) have implications for the physical
properties of diatom tests. Earlier work has demonstrated that laser diffraction responds to the particles’ external projected
area. The effects of both low effective density and irregular shape of diatoms (compared with terrigenous grains) on their
settling velocity causes the Sedigraph to indicate relatively small diameters. Shape effects are less pronounced for quasi-
spherical diatom species. The Coulter counter records the diatoms’ solid volume and is relatively unaffected by their density or
shape. The measurement of different physical parameters by these instruments offers a basis for estimation of diatom porosity
(fluid-occupied volume within the test). Measurements of the external diameter and solid volume allow estimates of porosity W.
For (laser) sizes . 20 mm this is W = 75–95%, which can be quite well modeled as a perforated spherical shell of wall
thickness , 1–1.5 mm. For paleocurrent interpretations, a settling-based technique makes Sedigraph measurements of particle
size the most useful, but the visual size is best given by laser.

INTRODUCTION
Nature provides us with some strange particles, glass bubbles of tephra
and perfect cubes of bacterial magnetite among them, but none as
abundant and important in sediments as the beautiful filigree cell walls of
diatoms. For many sedimentary applications we want to know how big
particles are. We have an intuitive idea of what ‘‘how big’’ means when
we look at a particle, but most of the methods of determining size of fine
(silt and clay) particles use a measurement of some other property from
which ‘‘size’’ is inferred. Only (electron) microscopic imaging, measure-
ment, and counting comes close to our intuitive view of size, and that is
not commonly performed, being very time consuming.
Sediment grain size in the silt–clay range has been used as a parameter
from which bottom current strength in the deep ocean may be inferred.
Early studies considered overall silt size as an indication of current
activity (Ledbetter 1984), but more recently the grain size of the 10–63 mm,
or ‘‘sortable silt’’ fraction, has been shown to be a more sensitive index of
bottom current flow speeds (McCave et al. 1995; McCave and Hall 2006).
The sortable-silt mean size (SS) has been used to indicate relative changes
in paleocurrent vigor at a variety of ocean sites (e.g., Hall et al. 2001;
Kuhn and Diekmann 2002; Gyllencreutz 2005). A common step in these
methods has been to remove the biogenic component of the sediments
prior to particle size analysis. Biogenic material has been treated as a
source of noise that interferes with the current-sorting signal acquired by
terrigenous sediment. This is partly because biogenic material may show
up as species-specific size peaks (McCave et al. 1995). However, in the
presence of bottom currents, we would expect biogenic particles above
, 10 mm also to be sorted according to some size-related property,
generally settling velocity. Many workers use instruments that do not use
settling velocity as a basis for inferring size, so we need to understand how
the instruments commonly in use for size measurement record the
dimensions of diatom frustules. In this study, which originates from an
interest in the behavior of currents in the Southern Ocean, we make the
first step to quantify the sizes of diatomaceous material from silica-rich
sediments.
Geologists are not the only group interested in diatom frustules; precise
new data on diatom architecture are emerging from the field of
nanotechnology (Losic et al. 2006; Losic et al. 2009). Diatom properties
are being studied with a view to using them as nano filters, adhesives, and
nanobots (Sterrenburg 2005; Gordon and Parkinson 2005).
Several instruments are available to measure particle size (McCave and
Syvitski 1991). Numerous studies have found large inter-instrument
differences, highlighting the importance of selecting the appropriate
method for the nature of the sediment analyzed and the purpose of the
investigation (Syvitski et al. 1991; Konert and Vandenberghe 1997;
Bianchi et al. 1999; McCave et al. 2006). The density and shape of
diatoms are very different from terrigenous grains. We investigate how
these properties affect their size measurement by three different particle-

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 JSR DIATOM SIZE AND PROPERTIES 601

TABLE 1.— Details of the sediment samples used in this study. Opal wt. % values are based on weight difference after opal removal. Lithological names
follow Dean et al. (1985) and Mazullo et al. (1988).

Core Sample no. Latitude (uS) Longitude (uW) Water depth (m) Region Lithology Opal content (wt. %)
VC324 T1 65.23 56.15 512 Larsen Shelf Diamict , 5
VC326 T2 65.20 56.72 524 Larsen Shelf Diamict , 5
VC340 T3 65.21 55.38 496 Larsen Shelf Diamict , 5
VC344 T4 65.13 55.07 466 Larsen Shelf Diamict , 5
PC072 D1 52.11 41.21 3773 Falkland Trough Diatom ooze 90
PC287 D2 60.31 36.65 1998 Scotia Sea Muddy diatom ooze 69
TC288 D3 59.14 37.96 2864 Scotia Sea Muddy diatom ooze 66
PC290 D4 55.55 45.02 3826 Scotia Sea Diatomaceous mud 44
TC292 D5 52.50 44.24 3404 Scotia Sea Muddy diatom ooze 59

sizing methods (and instruments)—settling velocity (Sedigraph 5100)
(Coakley and Syvitski 1991), electrical sensing zone particle counting
(Beckman Multisizer-3 Coulter counter) (Milligan and Kranck 1991), and
laser diffraction (Malvern Mastersizer Microplus) (Agrawal et al. 1991).
Measuring the Size of Particles
Individual particle size measurement and counting, even when
automated, is far too time-consuming to produce a particle-size
distribution (PSD) for fine material from 100 to below 1 mm. However,
newer methods of high-speed digital imaging (as in the Fluid Imaging
Technologies ‘‘FlowCAM’’) may provide another way of counting and
measuring the external projected dimensions of particles over the 1–
3000 mm range. Most studies require the relatively rapid measurement of
statistically significant numbers of particles. Optical microscope analysis
lacks the resolution at the 1 mm level, and SEM preparation and analysis
is too time consuming. Rapid analyses of sediment samples therefore
measure some property from which particle size is inferred (McCave and
Syvitski 1991).
The classical (and reference standard) method of estimating fine
particle size is to measure settling velocity in pipette analysis and infer the
size via Stokes’ Law (eq. 1) (Krumbein and Pettijohn 1938; ASTM 1983).
Pipette analysis and the Sedigraph use this principle. Spherical particles
are normally assumed, yielding results as equivalent spherical diameters
(dW). In geological applications the density of quartz (2650 kg m23) is
generally assumed. Stokes’ Law gives:
ws ~KDrgdW 2 =18m
where ws is settling velocity, Dr is the density difference between the
particle and fluid, g is acceleration due to gravity, dW is particle diameter,
and m is dynamic viscosity of the fluid. For spheres K 5 1, for other
shapes K , 1 for discs and cylinders using the E shape factor of Janke
(1966) or the Corey Shape Factor (CSF) (Corey 1949) advocated by
Komar and Reimers (1978) and Komar (1980). According to Lerman et
al. (1974) discs are considered to have K , 1, while cylinders have
K . 1.
The Coulter counter is based on the principle that a particle passing
through an electric field in an electrolyte solution causes a change in
voltage when the particle differs in resistivity from the electrolyte
(Milligan and Kranck 1991). In practice dielectric particles are assumed
(zero conductivity). Particles are suspended in a beaker of 1% salt (NaCl)
solution containing an electrode and drawn through a small aperture in
the wall of a tube containing a second electrode. The grain displaces its
volume of liquid in the aperture, momentarily increasing the impedance
of the circuit. A voltage pulse is generated that is directly proportional to
the volume of the particle. The size estimate is therefore a diameter of a
sphere (dV) with the same volume as the solids in the measured particle.
Voltage pulses are sized and counted in a multi-channel analyzer to yield
a particle-size distributions by number (n) or volume (! SndV3).
Laser diffraction analyzers measure the angular distribution of
forward-scattered light from which the most probable particle size
distribution of spherical scatterers is inferred (dL) (Agrawal et al. 1991). A
laser beam of known wavelength is passed through a suspension of the
sample. Detectors measure the angular distribution of intensity of the
light diffracted by the particles. Mie (or Fraunhofer) theory is used to fit a
theoretical model to the diffraction data. When particles are equant there
is good agreement between laser and other sizing methods, but Konert
and Vandenberghe (1997) show that the laser gives a size related to the
projected area of a particle. Irregularly shaped particles with a range of
aspect ratios produce asymmetrical patterns in light diffraction. This is
analogous to the effect of directing a light source through a pinhole
(symmetrical) compared with a slit (asymmetrical). Laser diffraction
sizers cannot distinguish the different axis lengths of irregularly shaped
particles (Kelly and Kazanjian 2006).
Some previous studies (Pudsey and Howe 1998; Buurman et al. 2001)
have alluded to the factors controlling the hydrodynamic properties of
diatoms. As well as having the most dynamical relevance, settling
diameter (dW) is also the measurement most affected by these factors,
mainly density and porosity. Diatoms have external cell walls of hydrated
silica with density around 2000 kg m23. Defining the porosity of the
diatom is not straightforward because the silica walls contain pores of
varying size. The space inside these walls is generally more than 50% of
the overall volume of the particle. We use porosity here to mean the
volume of space occupied by fluid (when immersed) within the outermost
surface of a frustule. We focus here on comparison of dW with dV and dL.
ð1Þ
MATERIAL AND METHODS
Strategy
Our strategy was first to analyze the particle size of sediments on three
different instruments, and then to measure subsamples separated by
settling velocity (SV) on two instruments in order to compare SV with the
response of common instruments. The Sedigraph, Coulter counter, and
Malvern laser analyzer were used first, then the dW of diatomaceous
sediments was compared with Coulter counter and Malvern. Separates of
known dW were obtained by repeated (33) settling and decantation of
diatomaceous sediment to produce ‘‘standards’’ with known values of dW
(see Krumbein and Pettijohn (1938) or Folk (1974) for details of method).
These standards were measured on the Coulter counter and Malvern.
This allows direct comparison of dW, dV, and dL for a range of dW.
Scanning electron microscope (SEM) images of the samples were
obtained to observe the different SV fractions and evaluate their particle
shape.
Sample Material
Diatom-rich ocean sediments from five different sites in and around the
Scotia Sea (between the tip of South America and the Antarctic

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 602 R.S. PUGH AND I.N. MCCAVE JSR

TABLE 2.— Statistics for the particle-size analysis of a range of Southern Ocean sediments by Sedigraph, Coulter Counter, and Malvern laser analyzer.
Samples rich in diatoms are denoted by the letter D, and samples with low diatom content by T (terrigenous). Differences between Coulter and others are
not shown because Coulter does not sense the , 2 mm part of the size range.

Sedigraph (dW) Coulter (dV) Malvern (dL) Difference

Mean MmW Mean MQW Sorting SQW Mean MmV Mean MQV Sorting SQV Mean MmL Mean MQL Sorting SQL MQW–MQL
Sample (mm) (Q) (Q) (mm) (Q) (Q) (mm) (Q) (Q) (Q)
T1 2.82 8.47 1.55 5.23 7.57 1.24 2.81 8.48 1.66 20.005
T2 3.06 8.35 1.67 5.34 7.49 1.37 5.83 7.42 2.08 0.93
T3 2.52 8.63 1.55 4.03 7.89 1.28 4.62 7.76 2.17 0.88
T4 3.14 8.32 1.63 4.99 7.57 1.37 4.7 7.73 1.94 0.58
D1 2.96 8.4 1.32 6.74 7.21 0.86 11.43 6.45 1.85 1.95
D4 3.34 8.22 1.59 8.31 6.9 1.13 9.03 6.79 2.25 1.43
D5 3.86 8.02 1.72 9.41 6.73 1.07 11.3 6.47 2.12 1.55

Peninsula) were selected. Continental shelf sediments (mainly proximal
glacial-marine, hereafter ‘‘till’’) from the east coast of the Antarctic
Peninsula with negligible diatom content were used for comparison. Site
locations for the sample material and its properties are given in Table 1.
Core PC072 was chosen as an example of diatom ooze, containing
approximately 90% diatoms by weight. A glacial-age sample from Core
TC288 was chosen on the basis that its diatomaceous fraction is almost
monospecific within a certain size range. This allowed evaluation of the
impact of differences between species on the size measurement of
diatomaceous material. The other diatomaceous samples were surface
sediments consisting of a mixture of terrigenous material and biogenic
silica.
Sample Preparation
Coarse material (. 63 mm) was removed by wet sieving 15 g of
sediment on a 63 mm mesh. Organic matter was removed by hydrogen
peroxide, which also assists in the disaggregation of fine material.
Observation by light microscope showed the sediments to contain only
negligible amounts of CaCO3. Subsamples of both the diatom-rich and
glacial sediments were taken at this stage for analysis on Sedigraph,
Coulter counter, and Malvern (see procedures below).
Size fractions 8–7.5 Q, 7.5–7 Q, 7–6.5 Q, 6.5–6 Q, and . 6 Q (phi,
Q 5 2log2 d where d is the diameter in mm) of the diatomaceous samples
were then isolated by repeated settling and decantation. Large cylinders
and moderate concentrations were used to reduce the possibility of
hindered settling. Stokes’ Law and quartz density (as a standard basis for
comparison) were assumed during the preparation of the size fractions.
Samples were dried and weighed to determine the yield, then added to
80 ml of 0.1% Calgon dispersant then homogenized and disaggregated on
a rotating carousel for 24 h. A small subsample was taken from each
fraction to mount on stubs for SEM analysis.
Only the total sediment fractions contained sufficient material for
analysis by Sedigraph which requires . 1.5 g (dry). Samples were run at
a constant water temperature of 35uC for an analysis range of 1–70 mm.
For analysis on the Coulter counter, samples were well mixed in
suspension, subsampled with a pipette, and added to a particle-free
electrolyte (Isoton). The aperture size was selected according to the size
fraction analyzed. A 100 mm aperture with a measurement range of , 2–
50 mm (9–4.32 Q) was used to analyze the 8–7.5 Q and 7.5–7 Q fractions. A
200 mm aperture (range 4–100 mm or 8–3.32 Q) was used to analyze the 7–
6.5 Q, 6.5–6 Q, . 6 Q, and total sediment fractions. Each sample run was
preset to measure 50,000 particles. Three measurements per sample were
made to give a total count of 150,000 particles.
The remaining material was then subsampled for analysis by the
Malvern Multisizer. A background reading was taken, then up to 0.3 g of
sample was added until concentration was sufficient for measurement.
After sonication for 15 s, sample PSD was measured. The average of three
runs was taken for each sample.
Biogenic silica (mainly diatoms) was then removed from the sediment
by 6% (w/w) sodium hydroxide on a 95uC water bath for 30 minutes.
Smear slides were viewed under a light microscope to confirm the absence
of biogenic silica. Samples were then again analyzed by Coulter counter
and Malvern laser.
Data Processing
Data comparison was made difficult by the fact that the different
instruments produced PSDs based on dW, dV, and dL in different formats.
The results from the Coulter counter and Malvern laser covered different
measurement ranges and used different bin sizes. To effect the
comparison the PSDs from both instruments were manually transformed
into bin widths of 0.2 Q. Each distribution was then normalized to 100%.
The phi midpoint of the fractions isolated by settling and decantation was
taken as the mean dW to compare with dV and dL.
All statistics calculated are based on the assumption of log-normality.
Means are calculated in phi (and are thus log or geometric means), and
values in mm are their metric equivalents. Sorting is phi standard
deviation. These are calculated in GRADISTAT (Blott and Pye 2001)
which uses the formulae of Krumbein and Pettijohn (1938).
RESULTS
There is far less variation in mean size (MQ) between instruments for
the till samples than for the diatom-rich samples (Table 2). The Q means
for dV and dL of till samples are similar, and both are around 0.75 Q
coarser than dW. However the comparison between dV and other
instrument means is invalid because the Coulter counter does not sense
material , 2 mm. The similarity of dV and dL and dissimilarity between
dW and dL again points up the difficulty with laser sizers and the clay

FIG. 1.—Particle size distributions of the five separate settling velocity fractions of sample D1 by A) Coulter and B) Malvern, fractions of D2 by C) Coulter and D)
Malvern, fractions of D3 by E) Coulter and F) Malvern, fractions of D4 by G) Coulter and H) Malvern, and fractions of D5 by I) Coulter and J) Malvern. (Bimodality is
particularly clear in Parts C (minor mode at 5.5–6.5 Q) and E (minor mode at 6–6.5 Q).

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 604 R.S. PUGH AND I.N. MCCAVE
FIG. 2.—Mean diameter of the terrigenous and biogenic silica fractions of
marine sediment samples D1–D5 as measured by settling and Coulter counter.
Note that the Coulter counter measurements of the terrigenous fraction agree
almost perfectly with settling diameter. Around 5.5 Q (, 22 mm) biogenic and
terrigenous solid volume and settling sizes are about the same, indicating K 5 1
for both (see text).
fraction when related to a settling velocity standard (McCave et al. 1986;
Konert and Vandenberghe 1997). For all the diatom-rich samples dL is
much coarser than dW. Laser sizer data give the poorest sorting (sQL) for
both till and diatom-rich samples.
The prepared standards span discrete intervals of dW because of the
preparation method. Their particle size distributions as measured by
Coulter counter and Malvern are not discrete but show significant
overlap (Fig. 1) These instruments must sense dV and dL to be greatly
different from dW (similar to Blott and Pye (2006) for sand). The broadest
particle size distributions and greatest degree of overlap are found for dL,
demonstrated by their poorer sorting (sQL . sQV ) for all size fractions
(Table 2). Several of the dV distributions are also clearly bimodal. The
finer is usually the more prominent of the two peaks, especially for
samples D2–D3 (Fig. 1C, E). D1 is the only sample that recorded
unimodal dV distributions for all size fractions.
The phi midpoint of the range of dW for each of the prepared size fractions
is taken as its mean (MQW). This assumes that distributions of the dW
separates are log-normally distributed. The midpoint for the , 6 Q fraction
was initially taken as that between 6 Q and the sieving limit (4 Q), i.e., 5 Q, but
plotting it there shows it to fall off the 1:1 line (Fig. 2). Assuming that the
mean value of the 6–4 Q terrigenous fraction should fall on or very close to
the 1:1 line, like all the other terrigenous fractions, yields a value for MQW of
5.6 Q. We use this value of MQW in Tables 3 and 5 and in regression analyses.
For diatom-rich samples, MQV is coarser than MQW, a result that is consistent
for the range of samples and size fractions measured (Table 3). The mean
difference (MQV–MQW) is 0.21 Q. MQL is coarser still than MQV, and the mean
difference (MQL–MQV) is 0.59 Q. The largest discrepancy is therefore between
MQL and MQW, a mean difference of 0.85 Q.
After removing the biogenic silica from the samples, the terrigenous
material was reanalyzed on the Coulter counter and Malvern. As
expected for a sample of diatom ooze, the quantity of terrigenous material
left in sample D1 was too low for further analysis. The mean Coulter sizes
(MQV) for the terrigenous and diatom material for samples D2–D5 are
significantly different (Fig. 2) and is probably the source of the
bimodality observed for the dV size distributions (e.g., Fig. 1C, E), with
the diatoms contributing the coarser mode (attributable to slower settling
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JSR
due to higher porosity, but more solid material thus larger dV).
Terrigenous and diatom mean diameters also plot as separate populations
in MQW–MQL and MQV–MQL space (Figs. 3, 4).
The mean MQV and MQW values for terrigenous material plotted in
Figure 2 fall close to the 1:1 line, indicating that the assumptions of
spherical particles, quartz density, and negligible shape effect are
satisfactory for terrigenous grains. Biogenic dV data approach the 1:1
line at coarser sizes (dW . 6.25 Q), indicating that material of this size
behaves more like equant particles. The dW vs. dV data in Figure 2 show
that at low values of dW the corresponding dV is ‘‘too big,’’ or,
alternatively, dW is too small. The latter case could be due to strong non-
spherical shape effects, while dV ‘‘too big’’ would mean that the particle
appeared larger than its solid volume, perhaps due to occluded porosity.
As this is unlikely because the smaller particles are often fragments with
little porosity, the effect is most likely due to shape such that for
particles , 20 mm, K , 1 in the Stokes equation with diameter dV. So
small biogenic particles are significantly non-spherical with respect to
their Coulter-sensed volume.
For samples of equivalent dW range, diatom mean size MQV is up to
1.00 Q coarser than terrigenous MQV, with an average difference (MQVterr–
MQVdiat) of 0.55 Q (Table 5). The largest differences are observed for finer
size fractions (low dW). For the same samples of equivalent dW range,
diatom MQL is up to 1.72 Q coarser than terrigenous MQL with a mean
difference (MQLterr–MQLdiat) of 1.07 Q (Table 6). The largest differences
are observed for coarser size fractions (high dW). However dW vs. dL of
diatoms in Figure 3 appears to show a clear porosity effect in that
particles of progressively larger dW have even greater dL. At small dW, dL
is still larger but with a smaller porosity effect. If porosity were zero, dW
being smaller than dL would be due to a shape effect, because we know
that for equant terrigenous grains dL < dW (albeit with a constant
offset). This is corroborated by the data in Figure 4, where at small sizes
with negligible porosity dV < dL.
Figure 5A–E shows SEM images of the different size fractions of D1.
This sample has high diatom content, so is particularly useful to view
diatom particles of different dW. Although the proportion of terrigenous
material is low, there are enough silt grains present for a visual size
comparison. The diatoms in all size fractions look several times larger
than the silt grains of equivalent dW.
The smallest silt grains in each image tend to approximate the fraction’s
dW. For example, Figure 5B shows particles with a dW range of 5.5–7.8 mm
(7–7.5 Q). The smaller silt particles in Figure 5B are approximately 4–5 mm
long. Some of the silt particles are larger than this, but their size is small
compared to the size of the diatoms which range from 12 to 44 mm in
diameter, much larger than the dW. In another example, most of the
diatoms in Figure 5D are centric and range in diameter from 24 to 48 mm
(with mean corresponding laser dL of 31.4 mm), but their dW is in the
range 11.0–15.6 mm (6.5–6 Q).
DISCUSSION
The particle size distribution of diatomaceous marine sediments varies
significantly depending on the method of particle-size measurement. The
Malvern measures the largest diameters, followed by the Coulter counter
and then settling-based techniques. Variations in particle size between
methods also apply to the till sediments analyzed in this study, but the
differences for the diatomaceous samples are far more pronounced. The
results show that these inter-instrument variations occur over a range of
size fractions.
Our results are potentially applicable to diatoms in sea-bed sediments
where the organic coatings present in life in surface waters and while
sinking are no longer present. The settling of live particles, with their
frustules intact (both valves present) and of senescent cells, with even
partially intact organic coatings is very different from the hydrogen
 JSR DIATOM SIZE AND PROPERTIES 605

TABLE 3.— Statistics for the particle-size analysis of diatomaceous sediments by settling, Coulter Counter, and Malvern.

Settling (dW) Coulter (dV) Malvern (dL) Differences

Midpoint Mean Mean Sorting Mean Mean Sorting MwV–MwW MwL–MwV MwL–MwW
Sample (MwW) (w) (MmV) (mm) (MwV) (w) (swV) (w) (MmL) (mm) (MwL) (w) (swL) (w) (w) (w) (w)
D1 7.75 6.03 7.37 0.55 6.90 7.18 1.52 20.38 20.2 20.57
PC 072 7.25 8.40 6.09 0.59 11.58 6.43 1.43 20.36 20.46 20.82
6.75 12.37 6.34 0.49 21.28 5.55 1.17 20.41 20.78 21.20
6.25 15.95 5.97 0.46 31.39 4.99 1.01 20.28 20.98 21.26
5.60 21.84 5.52 0.46 44.77 4.48 0.94 20.08 21.04 21.12
D2 7.75 5.53 7.50 0.62 5.67 7.46 1.49 20.25 20.03 20.29
PC 287 7.25 7.23 7.11 0.58 9.52 6.71 1.55 20.14 20.40 20.54
6.75 10.03 6.64 0.59 16.46 5.93 1.53 20.11 20.71 20.83
6.25 13.08 6.26 0.56 24.01 5.38 1.43 0.01 20.88 20.87
5.60 19.12 5.71 0.54 28.49 5.13 1.49 0.11 20.58 20.47
D3 7.75 5.88 7.41 0.69 5.81 7.43 1.55 20.34 0.02 20.32
TC 288 7.25 7.30 7.10 0.54 9.40 6.73 1.61 20.15 20.37 20.52
6.75 11.33 6.46 0.71 14.71 6.09 1.65 20.29 20.38 20.66
6.25 11.89 6.39 0.47 18.02 5.79 1.65 0.14 20.60 20.46
5.60 19.07 5.70 0.52 21.84 5.52 1.50 0.10 20.19 20.08
D4 7.75 6.22 7.33 0.54 7.19 7.12 1.46 20.42 20.21 20.63
PC 290 7.25 8.26 6.92 0.54 12.46 6.33 1.43 20.33 20.59 20.92
6.75 11.89 6.39 0.57 22.66 5.46 1.32 20.36 20.93 21.29
6.25 15.23 6.04 0.55 32.25 4.96 1.19 20.21 21.08 21.30
5.60 20.68 5.59 0.53 34.01 4.88 1.25 20.01 20.71 20.72
D5 7.75 7.00 7.16 0.61 8.34 6.91 1.53 20.59 20.25 20.84
TC 292 7.25 9.28 6.75 0.56 14.21 6.14 1.42 20.50 20.62 21.11
6.75 11.78 6.41 0.56 23.01 5.44 1.30 20.34 20.97 21.31
6.25 14.01 6.16 0.54 31.37 4.99 1.30 20.09 21.16 21.26
5.60 21.6 5.53 0.54 33.51 4.90 1.43 20.07 20.63 20.70
Mean 20.21 20.59 20.80

peroxide-cleaned valves for this trial. In practice, sinking from the upper Eq. 1 (i.e., Ksphere, Kcylinder , Kdiat, etc.):
ocean to the bed is mainly accomplished in aggregates of various types
1
(Schrader 1971; McCave 1975, 1984; Burd and Jackson 2009), to which CSF~c=ðabÞ =2 ð2aÞ
cases the present results are not relevant.
It is immediately obvious from inspection of Figures 2 and 3 that the 


1=2
Coulter volume size converges on settling size as the latter increases, E~c a2 zb2 zc2 3 ð2bÞ
whereas laser projected-area size diverges. We inspect these instructive
cases in turn, but first particle shape factors must be considered. in which a, b, and c are the long, intermediate, and short diameters of a
particle. Their regression analysis gave the empirical relationship
Shape Factors for Diatom Tests
1
As diatom tests are found in a range of shapes (Fig. 5), modified Stokes ws ~ DrgD2n E 0:380 ð3Þ
18m
equations are required to determine their settling velocity. In a series of
experiments on ellipsoidal pebbles and rods settling in glycerine, Komar where Dn is the nominal diameter of a sphere of the same volume; that is,
and Reimers (1978) and Komar (1980) considered the effect of shape on Kdiat 5 E0.38.With the use of SEM images (such as Fig. 5) to inspect
settling rate at Reynolds numbers in the size range down to quartz- diatom shape, the E shape factor can be estimated and used to determine
density fine sand in water (minimum settling Reynolds Number of 0.1, the Kdiat to be employed in Eq. 1. Pennate diatoms such as Fragilariopsis
well into the Stokes region). These authors found the Corey Shape Factor kerguelensis have lengths that are over 10 times their width and depth and
(CSF) (Eq. 2a) to be best for shape effects of ellipsoids, and Janke’s give the lowest Kdiat (typically 0.45–0.6). Length and width are equal for
(1966) E shape factor (Eq. 2b) to be best for cylinders (but also good for centric diatoms (e.g., Coscinodiscus sp.), so the length of the shortest side
ellipsoids) on settling velocity as a factor in the standard Stokes equation, determines Kdiat (0.54–0.75). Eucampia antarctica (Fig. 5F), a species
with three axes of relatively similar lengths, gives Kdiat of 0.75–0.91. The
TABLE 4.—Results of the linear regression analysis for plots in Figures 2 to equivalent Lerman et al. (1974) factors would be, for centrics of 4:1
4. Columns ‘‘m’’ and ‘‘c’’ refer to coefficients in the linear regression diameter to height K 5 0.851, and for equant Eucampia K < 0.9–1.
y 5 mx + c.
Density of Diatom Tests
m c r2 One of the questions surrounding the size measurement of diatoms by
MwW vs MwV diatom 0.684 1.672 0.874 Coulter counter is whether the volume sensed is the solid volume of opal
terrigenous 0.941 0.458 0.989 in the particle alone or whether the cage-like structure of pill-box and
MwW vs MwL diatom 1.467 24.553 0.886 some pennate diatoms occludes the internal water and prevents the
terrigenous 1.041 20.452 0.981 passage of electric current through the porous particle, resulting in its
MwV vs MwL diatom 1.389 23.189 0.713
terrigenous 1.098 20.908 0.979
being sensed as larger than the volume of its solid material but perhaps
smaller than the external projection diameter. The convergence of Coulter

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 606 R.S. PUGH AND I.N. MCCAVE
FIG. 3.—Mean diameter of the terrigenous and biogenic silica fractions of
samples D1–D5 as measured by settling and Malvern laser. The laser represents
the size of terrigenous material as larger than by settling by , 0.2 Q. The greater
the projected area size (dL) of diatoms up to 6.25 Q, the bigger the divergence from
terrigenous settling size, probably due to higher porosity (see Fig. 6).
volume size on settling size noted above (Fig. 3), occurring at around 5.5
Q (22 mm), a size at which visual inspection clearly shows porosity in
frustules, suggests at first sight that any occlusion effect may not be very
large, at least above 20 mm.
In preparing the size fractions and in Sedigraph measurements, quartz
grain density (2650 kg m23) has been assumed for all samples. This is the
usual assumption in settling-velocity analysis, providing a standard based
on a common mineral. The assumption is clearly invalid for many
sediment types, including those rich in opal. The density (ropal) of marine
diatom silica (amorphous opal) is in the range 1980–2010 kg m23 (Hurd
and Theyer 1977) or 1900–2200 kg m23 (Chaika and Dvorkin 2000).
From Eq. 1,





K DrdW 2 qtz ~ K DrdL 2 diat ð4Þ
With Kqtz 5 1, it follows that
Drqtz ðdW =ddiat Þ2 ~ðKDrÞdiat
There are two effects potentially present in (KDr)diat, lower (than quartz)
density difference due to porosity, and non-spherical shape of diatoms.
The finer size classes are dominated by rod-shaped pennate diatoms,
while coarser size classes are dominated by disc-shaped centric diatoms
(Fig. 5). At MQW 5 7– 6.5 Q most particles were disc shaped, and at 7.5–
7 Q they were mixed disc and rod shaped. For a disc of thickness/diameter
ratio 5 1:4, Kdiat 5 E0.38 5 0.634 (Janke 1966; Komar 1980). In
Figure 2 a diatom settling size of 7 Q (7.8 mm) is equivalent to a Coulter
volume size of 6.45 Q (11.44 mm). The terrigenous material points,
however, lie close to the 1:1 line, indicating little extraneous effect of
shape or density for that material. For the two components (terrigenous
and diatoms) at the same settling velocity, and using Eq. 5, with dqtz 5 7
Q (7.8 mm), Kqtz 5 1, Drqtz 5 1650 kg/m3, thus (K Dr)diat 5 772 kg/m3.
If Kdiat 5 1 were assumed, the implied effective density of spherical
diatoms would be , 1772 kg/m3, which is too low. But, taking shape into
account, based on Janke’s E value of Kdiat 5 0.634, gives an effective
density of 2218 kg m23, while Lerman’s K 5 0.851 implies a particle
density of 1903 kg m23. These two values bracket the density of fresh
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JSR
FIG. 4.—Mean diameter of the terrigenous and biogenic silica fractions of
samples D1–D5 as measured by Coulter counter and Malvern. The laser represents
the size of terrigenous material as larger than by Coulter counter by , 0.15–0.35
Q. Around 7.5 Q (5.5 mm) terrigenous and biogenic sizes are about the same,
probably due to the fact that the biogenic material is fragments with zero porosity
(see Fig. 6).
biogenic opal (, 2000 kg m23). (An intermediate shape value of 0.77
yields this opal density.)
We conclude that the result that MQV is coarser than MQW (Fig. 3) for
diatom samples is due to a combination of the density difference (between
opal and quartz) and the shape effects of diatom tests: porosity does not
influence Coulter counter measurements of diatoms, and dV is the
equivalent diameter of an opal sphere.
Porosity of Diatoms
If we accept dV as a measure of the diameter of a sphere having the volume
of the solid opal in the diatoms and dL as the diameter of the total spherical
volume occupied by the particle and its pore spaces, porosity is given by
W~1{ðdV =dL Þ3 ð6Þ
The results of the calculations are rather interesting (Fig. 6). The
ð5Þ porosity is mainly in the range 60–90%, towards the high end of this range
for the larger size fractions, and towards the low end of this range for the
smaller size fractions, dropping to zero around 5 mm. If wall thickness
does not increase as fast as overall size then the porosity goes up with
overall size, as suggested by the results in Figure 6. A simple model for
the porosity is to consider the diatom to be a sphere of radius r, internal
radius (r–d), where d is the wall thickness. The porosity, (internal volume/
external volume), is (r–d)3/r3, which in terms of diameter d (5 2r) and
neglecting cubic-order terms, is thus
W~1{6ðd=d Þz4ðd=d Þ2 ð7Þ
The shape of this function is seen to be similar to the trend of the
estimates in Figure 6 where the wall thickness has been set between 0.5
and 1.0 mm. A value of 0.75 mm shows good agreement, but if the walls
contained 25% holes that would mean actual thickness of , 1 mm and
50% holes implies thickness of 1.5 mm. This range is of the right order for
diatoms, whose size mainly ranges from 10 to100 mm (Burckle 1978; Losic
et al. 2006).
 JSR DIATOM SIZE AND PROPERTIES 607

TABLE 5.— Statistical comparison of the Coulter Counter PSDs for the terrigenous and biogenic silica components of settling-velocity separates of
diatomaceous sediment samples.

Terrigenous Diatom w difference

Mean Mean Sorting Mean Mean Sorting MwVterr–MwVdiat
sample MwW (w) MmV (mm) MV (w) swV (w) MmV (mm) MwV (w) swV (w) (w)
D2 7.75 4.44 7.81 0.44 7.92 6.98 0.47 0.84
7.25 5.97 7.39 0.43 10.75 6.54 0.39 0.85
6.75 8.51 6.88 0.41 13.5 6.21 0.63 0.67
6.25 11.86 6.40 0.42 16.36 5.93 0.61 0.46
5.60 17.05 5.86 0.50 22.49 5.45 0.55 0.41
D3 7.75 4.71 7.73 0.46 9.44 6.73 0.54 1.00
7.25 6.32 7.31 0.41 11.78 6.41 0.35 0.90
6.75 8.89 6.81 0.40 13.29 6.21 0.82 0.61
6.25 12.01 6.38 0.37 11.55 6.44 0.58 20.06
5.60 18.39 5.75 0.47 19.14 5.70 0.50 0.05
D4 7.75 4.85 7.69 0.54 6.73 7.22 0.43 0.47
7.25 6.17 7.34 0.45 9.68 6.69 0.41 0.65
6.75 9.34 6.74 0.52 14.4 6.12 0.4 0.63
6.25 13.47 6.21 0.49 16.42 5.92 0.52 0.29
5.60 18.21 5.76 0.52 23.71 5.39 0.41 0.37
D5 7.75 4.89 7.68 0.56 8.44 6.86 0.54 0.81
7.25 6.39 7.29 0.46 11.45 6.45 0.34 0.84
6.75 8.94 6.81 0.42 15.17 6.04 0.37 0.76
6.25 13.06 6.26 0.46 16.43 5.93 0.58 0.33
5.60 20.72 5.58 0.52 19.16 5.44 1.07 0.14
mean 5 0.55

Saturated Bulk Density Settling, Size, and Species

The saturated density, that is, the density of the test plus its contained
water, rs, can be obtained from
Drs ~Dropal ð1{WÞ
where Dropal 5 1000 kg m23. This is needed in ws 5 KdiatDrsgdL2/18m
to get the settling velocity of diatoms from a laser size measurement, given
the right shape factor Kdiat.
The effect of shape on dW, dV, and dL may vary for different diatom
species, highlighted by the results of sample D3, taken from core TC288.
ð8Þ Differences in particle size measurement of this sample by the three
methods are less pronounced than for other diatom-rich samples. This
result can be explained by the diatom assemblage of TC288, which
contains a large proportion of the species Eucampia antarctica (see
Fig. 5F) (see Burckle 1984). The shape of this diatom is relatively close to

TABLE 6.—Statistical comparison of the Malvern PSDs for the terrigenous and biogenic silica components of settling-velocity separates of diatomaceous
sediment samples.

Terrigenous Diatom W Difference

Mean Mean Sorting Mean Mean Sorting MwLterr - MwLdiat
sample MwW (w) MmL (mm) MwL (w) swL (w) MmL (mm) MwL (w) swL (w) (w)
D2 7.75 4.96 7.65 1.00 7.28 7.10 2.07 0.55
7.25 7.01 7.16 1.06 15.65 6.00 1.88 1.16
6.75 10.11 6.61 1.24 28.41 5.14 1.39 1.48
6.25 13.49 6.20 1.22 38.97 4.68 1.18 1.51
5.60 23.84 5.39 1.19 38.58 4.70 1.83 0.69
D3 7.75 5.10 7.62 1.03 7.66 7.03 2.22 0.59
7.25 7.42 7.07 1.09 15.20 6.04 2.10 1.03
6.75 10.07 6.63 1.16 22.69 5.46 1.88 1.17
6.25 13.35 6.22 1.16 29.88 5.07 2.01 1.16
5.60 22.12 5.50 1.14 21.52 5.54 1.80 20.04
D4 7.75 5.10 7.61 1.01 8.35 6.90 1.58 0.71
7.25 7.65 7.03 1.05 16.89 5.89 1.46 1.14
6.75 10.89 6.52 1.14 33.32 4.91 1.07 1.61
6.25 15.99 5.97 1.20 41.95 4.58 0.97 1.39
5.60 23.94 5.38 1.15 47.90 4.38 1.18 1.00
D5 7.75 5.41 7.53 1.11 11.70 6.42 1.65 1.11
7.25 7.63 7.03 1.11 21.12 5.56 1.30 1.47
6.75 10.70 6.54 1.18 33.20 4.91 1.01 1.63
6.25 14.19 6.13 1.18 46.80 4.42 0.90 1.72
5.60 30.59 5.03 1.22 38.78 4.69 1.98 0.34
mean 5 1.07

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 608 R.S. PUGH AND I.N. MCCAVE JSR

FIG. 5.—SEM photographs of the A) 8–7.5 Q, B) 7.5–7 Q, C) 7–6.5 Q, D) 6.5–6 Q, and E) 6–4 Q fractions of PC072 and F) a close-up of the diatom Eucampia antarctica.
White circles mark individual terrigenous silt grains.

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 JSR DIATOM SIZE AND PROPERTIES
FIG. 6.—Porosities determined by Eq. 6 plotted against Laser size (MmL) with a
theoretical curve for hollow spheres of wall thickness 0.5, 0.75, and 1 mm. The
thickness of 0.75 mm shows good agreement, but if the walls were 25 to 50% holes,
that would mean actual thickness of 1 to 1.5 mm, which is what SEM and atomic
force microscopy reveals (Losic et al. 2006).
a sphere, and it has a much thicker test (greater effective density) than
most species. E. antarctica behaves more like a terrigenous silt grain,
explaining why the dV of terrigenous grains and diatoms of TC288 is
similar. Although E. antarctica is present in the other samples it is greatly
outweighed by the presence of more irregularly shaped diatom tests,
causing more pronounced inter-instrument differences.
High correlation coefficients (r2) show that the regressions summarized
in Table 4 are good approximations for the relationships between dW, dV,
and dL in this inter-instrument comparison. Different diatom species have
different effects on measured PSDs, and the proportion of biogenic silica
contained in different samples also varies. As a result, we cannot
generalize about the offsets between different instruments. Separation of
samples into their component (terrigenous and diatom) size distributions,
as done during this analysis, is required.
CONCLUSIONS
There is far less variation in mean size (MQ) between instruments for
the till samples than for diatom-rich samples. However, dW–dL
discrepancies again reveal the difficulty with laser sizers and the influence
of the clay fraction at sizes well above its nominal diameter when related
to a settling-velocity standard.
The effective density and shape of diatoms causes the relationship
dL . dV . dW of diameters sensed by different methods to be con-
sistent for a range of size classes and a range of diatom-rich sedi-
ment samples. Although both the density and shape of terrigenous silt
grains may vary, the assumptions of quartz grain density and spherical
shape are a fair approximation for these particles but not for diatom tests.
The relatively small dW of diatom tests compared with terrigenous
particles, as measured by Sedigraph, can be explained by their low
effective density (low grain density and high porosity) and irregular
shape. The relatively high dL of diatom tests as measured by Malvern
laser sizer, compared with terrigenous particles, can be explained by their
high porosity.
A plot of dW vs. dL of diatoms shows a clear porosity effect in that
particles of progressively larger dW have even bigger dL. The visual (SEM)
size of diatoms agrees with corresponding laser dL. The porosity is mainly
in the range 60–90%, towards the high end of this range for the larger size
fractions, and towards the low end for the smaller size fractions, dropping
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609
to zero around 5 mm. A simple spherical model for the porosity with d as
the wall thickness yields values of d , 1 to 1.5 mm depending on the area
percentage of holes. This range is of the right order for diatoms.
Coulter volume size converges on settling size as the latter increases,
whereas laser projected-area size diverges. The result that MQV is coarser
than MQW for diatom samples is due to a combination of the density
difference (between opal and quartz) and the shape effects of diatom tests:
porosity does not influence Coulter counter measurements of diatoms,
and dV is the equivalent diameter of an opal sphere. Several of the Coulter
dV distributions of settling-velocity separates are clearly bimodal. The
finer is usually the more prominent of the two, with the diatoms
contributing the coarser mode (attributable to slow settling due to higher
porosity relative to terrigenous, but more solid material thus bigger dV).
Small biogenic particles are significantly non-spherical with respect to
their Coulter-sensed volume.
If we wish to interpret particle size measurements in terms of
paleocurrent strength, the hydrodynamic properties of the particles are
most important. This makes dW as measured by settling the most useful
measure.
It is not yet possible to convert PSDs derived from different
instruments into PSDs based on dW. However a rough guide would be
provided by a Stokes Law assumption with a shape correction of 0.77, use
of a material density of 2000 kg m23, and porosity as shown in Figure 6.
It is unlikely that calibration curves to convert dV or dL to dW could be
applied universally to diatomaceous sediments. Local calibration curves
for sediments with similar species composition and total diatom
percentage would be required.
The methods used here could be employed to determine variation in the
thickness of diatom skeletons in the past, a key variable related to iron
fertilization of the oceans with possible relation to glacial–interglacial
change in atmospheric CO2 drawdown and climate (Hutchins and
Bruland 1998; Takeda 1998). The trick would be to isolate by decantation
a particular fraction, one that was mainly whole diatom tests, ideally of
monospecific centrics, then determine its size by laser and Coulter
counter, proceeding in the manner used to generate Figure 6 here with
modeled wall thickness. One could vary the model for non-spherical
shapes—spheroids, cylinders, etc.—according to the species isolated to
answer the question, ‘‘are iron-fertilized diatoms really thinner?’’ (Boyle
1998).
ACKNOWLEDGEMENTS
This work was completed during RSP’s tenure of a Natural Environment
Research Council Ph.D. studentship at Cambridge (NER/S/A/2003/11321).
Dr. Carol Pudsey (formerly British Antarctic Survey) co-supervised the initial
stages of the project and supplied the sediment samples. We are grateful to
Gillian Foreman and Ian Marshall for laboratory assistance. We would also
like to thank Dr. Claus-Dieter Hillenbrand, Dr. Carol Pudsey, and Prof. Paul
Komar for helpful comments on earlier versions of this manuscript. We are
most grateful for the time and attention paid by reviewers Simon Blott and
Sarah Spaulding and editor Kyle Straub on an admittedly somewhat obscure
topic, which has proved most helpful.
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Received 11 October 2010; accepted 7 March 2011.