Page 100

Chapter 3
MINERAL FRACTIONATION FOR SOILS
Particle size distribution of mineral species, a measure of chemical
weathering and a control of chemical activity through specific surface
Contents:
................................................................ Page
Size limits employed (Fig. 3-1) ............................................101,103
Fractionation aids qualitative and semi-quantitative analysis...............102,104
Fractionation aids size function of species ..................................105
Equivalent spherical diameter ................................................110
SEPARATION OF MINERALS BY SIEVE AND BEAKER SEDIMENTATION..........................110
Flow sheet for mineral segregation (Fig. 3-2) ................................111
Fraction sizes (Table 3-1) ...................................................113
Time for gravity sedimentation (Table 3-2);
nomograph (Fig. 3-3).......................................................114,115
Procedure
.................................................................123
Tabulation of results. .......................................................126
SEPARATION OF MINERALS BY TUBE CENTRIFUGE ........................................127
Time required for sedimentation (Table 3-4);
nomograph (Fig. 3-6)...................................................... 128,130
Procedure
.................................................................139
Angle head centrifuge........................................................144
SEPARATION OF MINERALS BY THE SUPERCENTRIFUGE ....................................152
Elutriation principle in Sharples supercentrifuge ...........................154
Flow rate for Sharples supercentrifuge; nomograph (Fig. 3-12)............... 155,158
Procedure
.................................................................161
QUESTIONS
.................................................................166
3-1.
The mineralochemistry of soils is made complex by the occurrence of numerous mineral
species, amorphous inorganic substances, and organic complexes mixed together in
various proportions in different soils. This situation is analogous to the complexity
of the organochemistry of soil, arising also because of the complex mixture of
molecular species and variously altered or polymerized organic substances mixed
together in soil organic matter (Chapter 12). The approach to mineralochemical analysis
is to separate the mineral series or species as much as possible prior to application
of various soil analytical techniques. Selective dissolution of various oxides (Chapter
2) helps with mineral dispersion and segregation into size fractions. The latter
segregation of size fractions, with resultant concentration of mineral series or
species, aids X-ray diffraction analysis (Chapter 4), thermal analysis (Chapter 6),
specific surface interpretation (Chapter 7), examination with the electron microscope
(Chapter 9), examination by means of the polarizing microscope (Chapter 10), and
further selective dissolution of mineral species as well as the allocation of chemical
elements to mineral species (Chapter 11).

Page 101
32.
Size limits employed. The colloid chemistry of several fine fractions of soils has
*
been studied. The use of a 0.2um limit being given preference to the 0.lum limit for
reasons stated as follows: In the first place the determination is quick, involving
rotation at 3500 revolutions for about 45 min in the centrifuge used . Secondly, this
point falls into line with the other points chosen for ordinary mechanical analysis,
being 0.1 of 2 um. Thirdly, there are good grounds for choosing 200 nm as the upper
limit of the truly colloidal matter of clays, i.e., colloidal matter as the colloidal
chemist understands the term. Lastly, as will be shown in the paper which follows, at
<200 nm the figures obtained using various alkali cations to saturate the clays show no
appreciable variation, whereas at 100 nm and 50 nm the lyotrope series is often in
evidence. Various clay fractions finer than the 2um limit had previously been employed
for elemental analysis of soil colloids for purposes of characterization, separation
#
being effected by ion settling or supercentrifugation. Differences in refractive
indexes were noted** in minerals of the finer clay fractions. Three to 7 times greater
##
exchange capacity was found in the clay less than 0.2um than in the coarse clay (2 to
***
In our
0.2um in diameter). Separation at 0.2um diameter limits has been advocated.
###
found to be most valuable for Xray
laboratory, the size fractions equivalent
diffraction analysis and other minera1ochemical procedures are the following:
1. Coarser sands...................................... 100+ um (microns)
2. Very fine sand..................................... 100 to 50 um
3. Coarse silt........................................ 50 to 20um
4. Medium silt........................................ 20 to 5 um
5. Fine silt ......................................... 5 to 2 um
6. Coarse clay........................................ 2 to 0.2 um
7. Medium clay........................................ 0.2 to 0.08 um
8. Fine clay ......................................... 0.03 um (80 um)
____________________________________________________________
*Marshall, C. E. (1931) J. Soc. Chem. Ind., 50T:444.
#
Bradfield R . (1923) Mo. Agr. Exp. Sta. Res. Bul. 60; Brown and Byers (1932) U.S.D.A.
Tech. Bul. 319.
**
Marshall, C. E. (1930) Trans. Faraday Soc., 26:173.
#
Truog, E. et al. (1937) S.S.S.A. Proc. , 1:175.
***
Nagelschmidt (1939) J. Agr. Sci., 29:477.
###
The size fractions are greatly affected by turbidity currents (Fig. 38) and density
decreases by hydration (Table 36), and so the values given are arbitrary
equivalent spherical diameters (para 38)

Page 102
102
3-2a.
The coarser sands may be further subdivided by sieving at the U.S.D.A.# or
International limits (Fig. 3-1). Although narrower and more numerous size fractions
have been obtained** (Fig. 3-1), seldom is additional minera1ochemical information
obtained by the separation of more fractions than the 8 fractions listed above. Types
of fractionation other than size segregation generally are best applied to the size
fractions rather than the whole soil. Thus the separation of minerals of heavy specific
gravity for study with the polarizing light microscope (Chapter 10) is most frequent-1y
applied to the very fine sand fraction (100 to 50 microns).
3-3.
Studies made in this laboratory of subdivisions of the clay fraction at 0.1, 0.08,
0.06, 0.04, and 0.02u indicate that a separation at the 0.08u limit achieves as much
segregation of minerals as generally can be obtained by more size-segregation in this
range. Little increase in mineralochemical information is gained by determination of
particle size distribution within the fraction less than 0.08u in diameter. The 0.08u
separation is relatively fast and convenient with either a supercentrifuge or high
speed angle head centrifuge. Departure from a logarithmic interval in the choice of the
0.08u limit is fully justified by the distribution of minerals found by
experimentation. A relatively small part of the clay fraction occurs below 0.02u. The
##
thinnest montmorillonite particles seen in the electron microscope were estimated to
be 0.002u thick, but the width of the thin platy particles gives a fairly large
equivalent diameter (para 3-8).
3-4.
Use of the three fractions in the silt size range and of the three fractions in the
clay size range is consistent with the abundance and importance in soils of these
fractions, especially in comparison to sands which are often fractionated into more
than three fractions. The use of these three subfractions of silt and clay is strongly
supported as optimum by many workers reporting on minera1ochemical and weathering
interpretations. The silts are very important quantitatively, frequently making up 60
to 85% of a silt loam, The 20u point divides the silt fraction of soils developed on
loess and some tills about equally. The 50u point is important as the approximate upper
limit of soil material of loessial origin. The 50-20u silt subfraction is excellent for
***
Zr measurements.
3-5.
Fractionation aids qualitative analysis. Separation of mineral species out into as
simple as possible mixtures provides for as few sets of diffraction peaks as possible
in each diffraction pattern, thus facilitating qualitative analysis (para 4-136), The
diffraction intensity from each component, relative
______________________________________________________
#
Knight, S.S.S.A. Proc., 2:592 (1938).
**
Steele and Bradfield, Soil Surv. Assoc. Bul., 15:88 (1934); White-side and Marshall,
S.S.S.A. Proc., 4:100 (1940).
##
Shaw, J. Phys. Chem., 46:1032 (1942).
***
Fanning, D. S., and Jackson, M, L. (in manuscript).

Page 103
Thinnest Montmorillonite plates Shaw (1942)

Page 104

to the total, is greater and each peak is as specific as possible, For

example, feldspars can be determined better in the coarse clay (20.2 micron
fraction) than in the whole clay fraction below 2 microns. X-radiation of
fractions of wide size distribution has often resulted in the erroneous
attribution of the diffraction analysis of the coarser size particles to the
entire fraction including the finer fractions. Some interstratified layer
silicates of the 1:1, 2:1, and 2:2 families have low (00L) diffraction
intensity, and this phenomenon can best be recognized and the minerals
identified and estimated if they are concentrated into fractions exclusive of
more perfectly crystallized minerals such as quarts, kaolinite, and mica,
which give strong diffraction patterns and mask the diffraction of the
interstratified layer silicates (para 4152). Also, montmorillonite series
minerals often (though not always) occur abundantly in the fraction less than
0.08 microns in diameter, but have often been overlooked in diffraction
patterns of the whole fraction of soil particles less than 2 microns in
diameter. Studies of Bray* and coworkers
...showed the inadequateness of the usual clay examination where
fractionated material is not used. Minerals were found which were
not originally indicated by ordinary methods, because they were
masked by the larger amounts of the dominant minerals present.
Neither the petrographic nor xray studies of the whole clay (C2u)
indicates, for example, the presence of beidellite (series) when
either the sericitelike clay mica (illite series) or kaolinite is
the dominant mineral.
The nondetection of significant amounts of montmorillonite in 2u clay, which
was abundant in illite, was noted also in soils by the author and coworkers#.
Large amounts (up to 40% of the clay fraction**) of hydrous micas of poorly
resolved basal spacings may not be detected in large amounts of
montmori1lonite or kaolinite.
36.

Fractionation aids quantitative analysis. The criterion of quantitative xray

diffraction analysis of soil minerals is the measured intensity of diffraction
at angles which are characteristic for each mineral. The intensity of
diffraction is a function of the mineral concentration in a mixture, but is a
function also of the particle size and degree of crystal perfection (freedom
from distortion) of each individual mineral. Finer particles have weaker
diffraction intensities which cannot be evaluated accurately in the presence
of stronger diffraction intensities of larger particles of the same mineral
species. The only way to obtain a weighted average analysis from diffraction
intensity is to xradiate each relatively narrow size fraction separately. If
each individual mineral series could be segregated into a single discrete
physical fraction, each could be identified by x-ray diffraction, regardless
of variation in diffraction intensity per unit weight as influenced by
particle size and crystal perfection of sample and standard##. The amount
present in a monomineral fraction could be determined quantitatively by
weighing. Segregation of amorphous material (Chapter 11) along with one of the
separated crystalline series would have to be detected. In practice,
segregation of minerals is not complete enough to produce monomineral
fractions. Obviously, segregation of mineral series and species as much as
possible into separate fractions is a great advantage to quantitative
a1location of elemental analysis (Chapter 11). For example, having two layer
_______________________________________________________________
*
Bray J., Am. Ceram. Soc., 20:257 (1937), who is summarizing work also of Grim
and Bray, J. Am. Ceram. Soc., 19:307 (1936), and Bray, Grim, and Kerr, Bul.
Geol. Soc. Am., 46:1909 (1935)
#
Jackson and Hellman, S.S.S.A. Proc., 6:133 (1942): Pennington and Jackson,
Ibid., 12:452 (1948); Jackson, Natl. Acad. Sci.Natl. Res. Council Pub. 327,
p. 218 (1954).
**
Hellman,, et al., S.S.S.A. Proc., 7:194 (1943).

Page 105
si1icate fractions, one higher in K content (often obtained in the coarse clay) and the
other lower in K content (often obtained in the fine clay) is a distinct analytical
advantage over having a single fraction with an intermediate content of K. Similar
advantages of mineral segregation and concentration into different fractions accrue to
CEC, thermal, surface, and microscopic analysis.
3-7.
Fractionation aids study of size function of mineral species. The size distribution of
each mineral species gives information about the extent and processes of geochemical
weathering* of minerals in soils and rocks. Soils which are only slightly weathered may
have significant amounts of primary minerals such as albite in the fine clay fraction.
In soils of somewhat greater weathering, montmori1lonite and (or) mica may be the most
abundant minerals in the fine fraction. In more highly weathered soils, oxides and
hydroxides of Fe, Al, Mn, and Ti are concentrated in the fine fraction. Amorphous
aluminosilicates and oxides often separate into the fine fraction and this increases
the precision of diffraction analysis of the coarser fractions. In the medium clay
fraction, kaolin, mica, and vermiculite are concentrated together with lesser amounts
of quartz, chlorite, and interstratified layer silicates. Concentration of kaolin in
#
the medium clay of montmorillonitic soils has been reported Quartz, kaolin, and mica
minerals (giving a 10A diffraction peak in the presence of glycerol) typically occur in
the coarse clay fraction. Little separation of minerals species has been found to occur
through the separation at l um; also, the long interval from 2 to 0.2 um includes a
satisfactory percentage of the clay. Quartz, feldspars, vermiculite, chlorite and mica
occur in the fine silt. Highly weathered soils, such as Ferruginous Humic Latosols,
have crystals of geochemical secondary minerals such as hematite, gibbsite, and anatase
which have grown sufficiently large to fall in the silt size range. The particle size
**
limit below which the feldspars and quartz disappear, the size extinction function ,
is characteristic of the degree of weathering. In Gray Brown Podzolic soils of the
North Central Region of United States, the feldspars tend to become extinct at a
particle diameter of 1 or 2 um, while quartz tends to become extinct at a particle
diameter of 0.1 um. In Latosols, wherein weathering has been more extensive, quartz
may occur as particles of 10 to 50 um, but becomes extinct at particle diameters of 5
or 2 um.
____________________________________________________
*
Jackson and Sherman (1953) Adv. Agron., 5:219#
Coleman and Jackson (1946) S.S.S.A. Proc., 10:381**
Jackson et al. (1948) J. Phys. Coll. Chem., 52:1237-

Page 110

3-8.
Equivalent spherical diameter. Soil particles are often plate-shaped. According to
convention, the particle diameter referred to herein is the equivalent spherical
diameter of the particles. For diameters smaller than 20 um this refers to spheres
having the same settling velocities, according to Stokes law for streamline flow (para
3-13), as the actual particles. For particle sizes of 50 um and above, the equivalent
spherical diameter refers to the nominal sieve opening size. Because the particle
densities vary from one mineral species to another, only an average density can be
employed for a given size separation. The density is taken as 2.65 for all diameters
down to 0.2 um. For finer sizes the density, given in tables, is based on the mineral
density in a heavy liquid such as tetrabromoethane, which of course is greater than the
mineral density when the mineral is highly solvated in a water suspension. The
diameters referred to therefore are equivalent spherical diameters of particles
having the stated density. Particles of greater density, such as of hematite, will be
separated at smaller actual diameters than stated. Particles of lower than the assumed
density will be separated at diameters greater than the stated diameter. Each fraction
has an upper and a lower "limiting diameter." The upper size limit in sedimentation is
determined by the maximum size of particle which, starting at the top of the
suspension, can remain in suspension during the sedimentation time.

SEPARATION OF MINERALS BY SIEVE AND BEAKER SEDIMENTATION

3-12.
The sieve type of separation of cleaned mineral particles can be employed down to a
particle diameter of about 50 um (Fig. 3-2). Wet sieving involves some decrease in
nominal sieve opening (Table 31) of the sieve, and the final sizing is therefore done
by dry-sieving.
3-13.
The settling times (Table 3-2) have been calculated by means of Stokes law for
streamline or viscous flow about a falling spherical body, wherein the resistance to
fall is 3 Dnv, in which D is the particle diameter in cm, v is the settling velocity
in cm/sec, and n is the viscosity in poises. This law is combined with the differential
specific gravity, delta-s = sp-s1 (particle relative to liquid), and the gravitational
2
constant, g, the value of which is 980 cm/sec , thus giving the working form of Stokes
law,

g (s p s1 )D 2
18n

= k1 D 2 (3-1)

Since v = h/t, in which h is the depth of fall in cm and t is the time in seconds,
(3-2)

t=

18nh
k
= 22
2
g ( s p s1 ) D
D

The nomograph (Fig. 3-3)

gives in more detail the time for
sedimentation (Table 3-2) for various sizes of particles.

Page 111
Fig. 3-2.

Page 113

Table 3-1.
Sand, silt, and c1ay fractions obtained for analysis by diffraction thermal,
microscope and other methods
Fraction
Size range,
microns

Name

Sand

Silt

Clay

Technique of obtaining
fraction

Very coarse sand

2000-1000

Sieve round-hole, on 1mm, through 2-mm

Coarse sand

1000-500

Sieve, round-hole, on
0.5mm

Medium sand

500-250

Sieve, screen, on 0.25 mm

(60 meshes per inch)

Fine sand

250-100

Sieve screen, on 0.1mm

(140 meshes per inch)

Very fine sand

l00-50

Sieve, screen, on 0.05mm

(300 meshes inch)

Coarse silt

50-20

Sieve, decantation

Medium silt

20-5

Decantation, centrifuge

Fine silt

5-2

Decantation, centrifuge

Coarse clay

2-0.2

Decantation, centrifuge

Medium c1ay

0.2-0.08

Decantation,
supercentrifuge

Fine clay

-0.08

Decantation,
supercentrifuge

Page 114

Table 3-2.
#

Time required at various temperatures for gravity sedimentation of soil particles, a

specific gravity of 2.65 being assumed and a 5-cm suspension depth being employed.
Particle
Time required for sedimentation at a suspension temperature of
limiting
diameter
20C
25C
30C
Microns
Hr
Min
Sec
Hr
Min
Sec
Hr
Min
Sec
Hr
50
--2
--20
--17
-20
-2
20
-2
5
-1
50
-5
-37
30
-33
20
-29
10
-2
3
50
-3
30
-3
3
-2
*Sedimentation times for a more extensive range of partic1e
sizes and temperatures are given in the accompanying nomograph.

35C
Min
-1
25
28

Sec
15
40
50
--

Page 115

Fig. 3-3.
Nomograph of
particle
settling time
under gravity
acceleration.
From Tanner
and Jackson,
S.S.S.A. Proc.
(1947) 12:60
(1948).

Page 123

Apparatus
3-29.
Needed apparatus includes a large funnel supporting a 50micron (300 meshes per inch)
sieve (figure 34); 1-liter, 600-ml, and tall form 100-mi beakers; water washing bottle
equipped with a coarse tip; sieve set (table 3-1) for separation of sand fractions; 8
cm evaporating dishes; glazed paper; and sample vials.

Reagents
3-30.
Reagents needed for the segregation procedure include distilled water; an 18-liter
stock of dilute Na2CO3 solution of pH 9.5 in distilled water (about 2 gm of Na2CO3 in
18 liters of water); and acetone in a wash bottle.

Procedure*
3-31.
The flow-sheet for the mineral segregation procedure should be consulted (figure 3-2).
The soil has been thoroughly dispersed by H2O2 treatment, removal of reduction soluble
iron oxides, and by saturation with Na (para 2-65g; 2-72).
332.
Separation of sands from silts and clays (at 50u). To facilitate the separations of
the various finer size fractions by centrifugation later, the total sand fraction
(grains greater than 50 microns in diameter) are removed from the suspension of
dispersed soil by wet sieving. First, the soil in the centrifuge tube or beaker is
thoroughly dispersed by shaking and tituration until all visible aggregates are broken
up and the individual particles seem discrete. A 50micron sieve is supported on a
glass funnel, so as to deliver into a 600-ml beaker (figure 3-4). The thoroughly
dispersed and freshly stirred soil suspension is allowed to stand (exactly) 40 seconds
for each 10 cm (4 inches) of its depth, and is then decanted through the sieve. The
purpose of this action is to permit particles greater than 50 microns to have settled
50u
are decanted through the
out so as not to obstruct the sieve as particles less than
sieve. This procedure is remarkably effective compared to use of either a longer or
shorter settling time. When most of the suspension has been poured through, the sands
are vigorously stirred in more distilled water, another 4 second per cm settling is
permitted, and the particles less than 50u are poured through the sieve as before. The
sands are then swirled in more distilled water, and the mixture quickly poured into one
side of the sieve. All grains are then washed onto the sieve, by means of a coarse jet
of water and with the aid of a policeman. The remaining silt and clay are washed from
the sand on the sieve by means of a coarse jet of water, as the sand is displaced from
one side of the sieve to another. Finally, the bottom of the sieve is washed clean
with a jet of water.
3-33.
After the sands are washed clean of silt and clay, as indicated by a clear washing
solution coming through the sieve and funnel (and complete absence of aggregates on the
screen), the sieve and sands are washed with two or three small portions of acetone
delivered from a wash bottle. A few silt particles less than 50 microns lodge in the
sieve and will not
____________________________________________________
*
Portions of this procedure have been published elsewhere, Jackson et al S.S.S.A. Proc.
14:77 (1950).

Page 123

50micron

sieve openings (300 meshes per inch)

Suspension of particles
diameter (silt and clay)

less

than

50

microns

Fig. 3-4.
Apparatus for wet-sieving of dispersed soil
suspension to effect the 50-micron separation,

in

Page 125

pass in the wet condition because of the decreased effective diameter of the sieve
openings due to its being wet. The sieve therefore is dried in an oven for a few
minutes and then tapped over the same funnel to pass the remaining silt particles. The
silt and c1ay particles are washed from the funnel into the beaker and the funnel is
removed.
334.
The sands (greater than 50u) remaining on the sieve are carefully transferred to a
glazed paper and then to a weighed bottle, are dried and weighed, and set aside for x
ray diffraction, light microscope analysis (Chapter 10) , and selective dissolution
analysis for quartz, feldspars and micas (Chapter 11). The sands dry to constant weight
at l00oC in a few minutes. The weight of the sand fractions is recorded (table 3-3) and
the percentage is calculated later on the basis of the total recovered mineral portion
of the sample (particles less than 2 mm) . In preparation for petrographic or
diffraction analysis, the sands are further subdivided into coarse and fine sub
fractions by means of well cleaned sieves (outlined in table 3-1) and then into heavy,
medium and light fractions by the heavy liquid specific gravity technique (Chapter 10).
3-35.
Separation of coarse silt (50 to 20u). The suspension of silt and clay (particles less
than 50 microns) contained in the 600-ml beaker, is next separated at the 20-micron
particle diameter limit. To do this, the suspension is stirred and then allowed to
stand quietly for at least five minutes (but not over 10 minutes) for each 10 cm (4
inches) of depth. The supernatant liquid is then decanted into a 1-liter beaker, care
being exercised to prevent the decantation of any of the settled particles. This and
the combined subsequent decantates are labeled less than 20u. The sedimented portion
is brought into suspension again by the addition of dilute Na2CO3 solution of pH 9.5
(solution of pH 8 to 10.3 NaOH are used if needed to disperse Latosols, rich in
kaolinite, halloysite, gibbsite, and iron oxide; for soils high in allophane, HCl
dispersion is employed; para 2-78). This suspension is then quantitatively transferred
to a tall-form l00-ml beaker having a mark encircling it at a height of 5 cm from the
bottom, inside measurement. The suspension is diluted to a depth of exactly 5 cm. This
suspension is again allowed to settle, this time for 3 minutes, and the supernatant
liquid decanted as before. The sediment is again dispersed in Na2CO3 solution, to a 5
cm depth, and the suspension is allowed to settle for about two minutes, the exact time
for the 20micron limiting diameter at the existing temperature being obtained from
table 3-2 or more precisely by means of a nomograph (figure 33).
3-36.
Sedimentation and decantation are continued until the finer silt and clay are separated
from the coarse silt in the l00-ml beaker, usually requiring five or more decantations.
For the last two times, the resuspension is made in pure distilled water, so as to
rinse all of the Na2CO3 (or HCl in allophanic soils) from the sediment consisting of
coarse silt. The coarse silt, remaining in the tall-form beaker, is washed into an
evaporating dish. The particles are allowed to settle, the excess liquid decanted, and
the coarse silt fraction dried and weighed. The weight of coarse silt is entered in
table 3-3

Page 126

Table 33.
Recovery of mineral fractions, expressed in grams and calculated as percentage of
mineral portion, of mineral plus oxide portion , aid of original sample weight of soil
and the percentage based on the mineral portion of soil less than 2 mm is calculated.

Page 127

J. Am. Chem.Soc. , 45 : 2910 ( 1923) ; also given by D Steel and Bradfield, Am. Soil
Survey Assoc. Bul., 15:88 (1934).

Page 128

Table 3-4.
Time required* at various centrifuge speeds and temperatures for sedimentation of
particles, an International No. 2 centrifuge with No. 240 head being employed with
l00ml tubes, a 10-cm suspension depth, a 1-cm of sediment, and a 9-cm net depth of
fall.

Page 129

With 1 cm of sediment, the International No. 2 centrifuge, R = 25 cm and. = 16 cm. At

25C n = 0.00894. One of the values in Table 34 may be recalculated. as an exercise in
the use of equation 37. More detailed information on sedimentation times is given in
the nomograph (figure 36). Equations 36 and 37 hold for the regular tube centrifuge
(para 349) , for the angle-head centrifuge (para 371), for the supercentrifuge (para
380) , and also for the 2layer method (para 373). The procedure given (para-349)
is the single layer method. of separation by centrifugation (figure 35) . The
principles of limiting diameter (para 38) applicable to this method are the same as
for beaker decantation with gravity sedimentation (para 335). The suspension density
increases with depth owing to partial sedimentation of particles and this stabilizes
the column against mechanical mixing The twolayer method of separation (para 373)
carries differential density a step further. A number of alternative formulas for the
supercentrifuge have been developed. (para 399).
343.

The centrifuge nonograph (figure 36) is prepared for a temperature of 20C

and. a particle specific gravity of 2.5. A specific gravity of 2.5 is found to
be about right for siliceous soil in the particle size range of approximately
0.2 microns, as judged by the specific gravity found for particles of about
this diameter by means of a heavy liquid. In the finer fraction, the observed
specific gravity in heavy liquids falls to about 2.2. In water dispersion the
colloidal particle specific gravity would necessarily be even lower. The
picnometer specific gravity of dried layer silicate colloids is 2.6 to 2.8,
but this is not applicable to highly hydrated colloidal particles which
sediment with interlameller water attached. In the coarser sizes, the
specific gravity of 2.65 is appropriate. Corrections, CT to various particle
specific gravities for use at varied temperatures may be made by means of
Table 35, as follows :
(3-8)
Centrifugation time (at wanted
=
Centrifugation time
CT
specific gravity, temperature)
from nomograph

Apparatus
3-47.
Apparatus needed for the size segregation procedure includes an International No. 2
centrifuge (International Equipment, Boston, Mass.) with No. 240 head, speed indicator,
time clock; and a rack of eight l00-ml centrifuge tubes fitted with rubber stoppers (a
shaker* for the rack of centrifuge tubes is a great convenience); glass rod with rubber
ball plunger (figure 21, page 34); glass rod with policeman; and a 6-liter flask.

Reagents
34-8.

Needed reagents include distilled water, Na2C03 solution of pH 9.5.

Page 130

Page 131

Page 139
Procedure*
3-49.
The centrifuge separation procedure to be followed removes the clay particles less than
2u from the medium and fine silt, then the medium silt is separated from the fine silt.
The flow sheet (figure 32) may profitably be reviewed in this connection.
350.
Separation of silt from clay at 2u. The suspension of silt and clay consisting of the
combined decantates in the lliter beaker, resulting from the 20u separation (para 3
36) , is allowed to stand undisturbed for more than eight hours for each 10 cm (4
inches) of depth. An excess of 50% over the limiting time is employed for the first
sedimentation. Or, to avoid the necessity of waiting for eight hours for each 10 cm,
the entire suspension may be centrifuged as in the following paragraph. After the
sedimentation period, the clay fraction (particles less than 2u in diameter) is
decanted or siphoned into a 6liter flask. This decanted suspension is labeled less
than 2u
351.
The sedimented solids remaining after decantation of the clay from the 1-liter beaker
are brought into suspension again in the pH 9.5 Na2CO3 solution and transferred to
centrifuge tubes, to a suspension depth of 10 cm. The suspension is centrifuged for a
time 50% in excess of 2.7 minutes at 750 rpm (International No. 2 Centrifuge with No.
240 head) . The supernatant suspension, remaining after centrifuging, is decanted into
the 6liter flask, being combined with the first decantate (para 3-50 The sediment in
the bottom of each tube is suspended into a small portion of the pH 9.5 Na2CO3
solution, by means of shaking or with the aid of a rubber plunger on a glass rod. The
plunger is lowered in the suspension carefully and the sediment tapped gently with
short strokes to avoid splashing the suspension over the top of the tube. The
suspensions of one sample in the several tubes are combined by transfer to fewer
centrifuge tubes or if possible to one tube as the successive centrifugation and
decantations progress. The particles adhering to the stopper and plunger are washed
into the suspension and the suspension depth is brought exactly to the 10cm mark.
Next, the tube is centrifuged at exactly 750 rpm for 2.7 minutes (table 34).
Centrifuge speeds corresponding to various temperatures and other speeds can be found
on the accompanying nomograph or by direct calculation (para 342).
352.
The processes of resuspension, centrifugation, and decantation are continued until the
supernatant suspension is fairly clear after the centrifuging periods. Usually five to
eight times are given in all. It has been found experimentally in unpublished studies
by Dr. N. N. Hiellman and the author that over 90% of the clay yield is obtained in the
first 3 centrifugings and that 97 to 99% of the clay yield is obtained in the first 5
centrifugings. Certainly never over 10 centrifugings should be required. Because of the
gradual breaking up of the finer silt particles, particularly of mica and kaolinite
during the process of resuspension, the suspension does not become entirely clear, even
with a very large number of centrifugings. Segregation of
_________________________________________________________________
*Portions of this procedure have been published, Jackson, et al.,
S. S. S. A. Proc., 14:77 (1950).

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various minerals into separate fractions is probably more complete if the number of
repetitions is limited to 5 to 8 so as to keep the physical fracture of the particles
at a minimum.
353.
The silt fraction (particles 20 to 2u in diameter) makes up the sediment. The medium
silt is now to be segregated (flow sheet, figure 3-2) from the fine silt according to
para 3-54; further separation of the clay fraction in the 6liter flask is to be made
according to para 357.
354.
Separation of the medium from fine silt at 5u via centrifuge.The solids medium and
fine silt particles 20 to 2u in diameter) remaining in the centrifuge tube are
suspended in the pH 9.5 Na2CO3 solution as before, to a suspension depth of 10 cm. The
separation of 5u may be accomplished either by centrifugation or by gravity
sedimentation, but usually is effective by the centrifuge because of the shorter
sedimentation time. (Under gravity, a 5u particle falls 5 cm in about 30 minutes, table
32.)
3-55.
The suspension is promptly centrifuged at 300 rpm for the appropriate time,
approximately 2.7 minutes (the exact time is given in table 3-4 or the accompanying
nomograph). The supernatant liquid is immediately decanted into a 600ml beaker.
Resuspension, centrifugation, and decantation are repeated until the separation is
completed, usually requiring five centrifugation Water is substituted for Na2CO3
solution for the last two centrifugations. The medium silt (particles 20 to 5u in
diameter) remains in the centrifuge tube, and is washed into a weighed bottle, dried,
weighed, and kept for x-ray diffraction analysis. The yield is calculated as percentage
of the minerals particles less than 2 um in diameter (table 33).
356.
The suspension of fine silt (particles 5 to 2u in diameter) is allowed to stand in the
600-ml beaker for 8 hours per 10 cm (4 inches) suspension depth, and the supernatant
1iquid is then decanted and combined with the clay fraction in the 6 liter conical
flask (or discarded if perfectly clear). The fine silt is washed into a 125-m1 conical
flask and kept in the moist condition for xray diffraction analysis. A small aliquot
of the fine silt is washed in 0.05 N HCl, dried, and weighed. The percentage of fine
silt is calculated on the basis of the mineral particles less than 2 min in diameter
(table 33).
357.
Separation of the coarse clay (2 to 0.2u) via centrifuge. The suspended 2u clay
fraction (sometimes known as the total clay fraction) has been decanted into a 6liter flask in the previous two separations. Two alternatives are available:
(a) To proceed with the separation at 0.2 with the entire suspension volume (para 3
59) (most efficacious if the suspension volume of 2u clay is only 1 or 2 liters).
Because eight 100ml tubes hold a total working volume of only about 500 ml, the first
separation at 0.2u requires two 35minute runs per liter of suspension.
(b) To reduce the suspension volume by means of a preliminary separation at 0.08u
(para 3-58) prior to beginning the separation at 0.2u (most efficacious when the total
volume exceeds 2 liters).

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(c) Reduction of the volume can also be accomplished by flocculation of the clay
suspension and decantation, but washing out the electrolyte used to produce
flocculation is more time consuming than the preliminary separation by the
supercentrifuge.
358.
The Preliminary separation of the fraction less than 2u, is made at 0.08u by means of
the supercentrifuge to reduce the suspension volume (in accordance with para 385,
broken line in flow sheet, figure 32). The resulting effluent containing the fine clay
particles less than 0.08u is then set aside while the separation at 0.2u (para 359) is
completed on the sediment on the supercentrifuge bowl liner. The preliminary separation
is at 0.08u instead of 0.2u because the accumulated large suspension volume would
otherwise have to be passed through the supercentrifuge a second time for the 0.08u
separation.
359.
To begin the separation at 0.2u, the suspension of clay less- than 2u (from 6liter
flask, para 353, or bowl liner, para 3-90) is transferred to l00ml centrifuge tubes
with suitable policing and washing to effect complete recovery of the clay. The
suspension, brought to a 10cm depth in the tubes, is centrifuged in the international
No. 2 centrifuge for the appropriate time at 2400 rpm, the time being about 30 minutes
(table 34). The time and temperature relations for various centrifuge speeds may be
obtained from the accompanying nomograph and further adjusted, if desired, for particle
specific gravities (table 35).
360.
The supernatant liquid is decanted into a 3liter flask and labeled less than 0.2u.
The sediment in the bottom of the tubes is dispersed in pH 9.5 Na2CO3 (pH 8 to 10.3
NaOH in the case of kaolinitic clays or Latosols) , and the suspensions are then
combined into fewer or one centrifuge tube. (Recentrifuging of more than one tube as
before may be necessary to reduce the volume of suspensions so as to go into one tube.)
The particles adhering to the stopper or plunger are washed into the tube and the
suspension depth again brought to exactly the 10cm mark. The tube is centrifuged as
before. The processes of resuspension, centrifugation, and decantation are continued
until the supernatant liquid is fairly clear, after centrifugation Usually five
centrifugations suffice. This process is essentially identical to that of separation of
the clay fraction at 2u (para 3-51) except for higher centrifugation speed and longer
time. The degree of completeness of separation ion as centrifuging progresses is about
the same as for total clay (para 352).
361.
The coarse clay (particles 2 to 0.2u), remaining in the bottom of the centrifuge tube,
is washed into a 125 ml conical flask and labeled; it is now ready for xray
diffraction analysis. A small aliquot of clay is washed in 0.05 N HCl and dried to
calculate the percentage of coarse clay (table 33). The decanted suspension of the
medium and fine c1ay is further separated 4 or more times at 0.08u (para 385).