Trace Metal Chemistry in Arid-zone Field Soils Amended with Sewage Sludge: I.

Fractionation of Ni, Cu, Zn, Cd, and Pb in Solid Phases1

GARRISON SPOSITO, L. J. LUND, AND A. C. CHANGS
ABSTRACT

of soils employed in short-term laboratory or glasshouse studies. The observed variability in soil trace
metal response to various chemical extractants suggests that, at least for some purposes, sequential extractions of soils may yield more information than
single extractions.
The philosophy and operational aspects of trace
metal extraction and fractionation in soils has been
reviewed recently by Cottenie et al. (1979) and by
Davies (1982). These authors have pointed out that
an extraction procedure generally is judged to be useful if it provides reproducible statistical correlations
between the extracted amounts of trace metal and
plant uptake or growth response. Thus, the criterion
for usefulness places emphasis on correlations with
availability to plants and not on elucidation of the
actual chemical species of trace metals in soil. On the
other hand, the overall goal of predicting accurately
the response of crops to sewage sludge amendments
will not be achieved until the trace metal chemistry
in the amended soil is understood thoroughly. A
knowledge of the trace metal compounds or forms
removed from soil by a given chemical extractant certainly would contribute to this understanding.
Sequential extraction procedures have been applied
to fractionate trace metals in sewage sludges (Stover
et al., 1976; Holtzclaw et al., 1978) and in soils incubated with sludges in the laboratory (Silviera and
Sommers, 1977). The procedure of Stover et al. (1976)
recently was employed by Schalscha et al. (1980, 1981)
to study the solid-phase chemical forms of Cr, Mn,
Ni, Cu, and Zn in the surface horizons of Chilean
Inceptisols that had been irrigated with untreated sewage effluent for up to 50 years. Schalscha et al. (1980,
1981) found that the percentage of the total extracted
metal in exchangeable and adsorbed forms was very
low for all five trace metals. The predominant fractions
for the extracted metals were: Cr, HNO3-extractable;
Mn, EDTA-extractable; Ni, Na4P2O7-extractable; Cu,
Na4P2O7-extractable; and Zn, HNO3-extractable. Thus
Cr and Zn were principally in the "sulfide" fraction,
as designated by Stover et al. (1976), Mn was principally in the "carbonate" fraction, and Ni and Cu
were in the "organic" fraction. However, the quantity
of Mn, Cu, and Zn extracted by Na4P2p7 did not correlate well statistically with the organic C content of
the soil (Schalscha et al., 1981).
In this paper, data are reported for a sequential
extraction technique modeled after that of Stover et
al. (1976) and applied to samples collected from the
surface horizons of two arid-zone soils used for about
four years in field experiments that were conducted
to assess the utility of anaerobically digested sewage
sludge as a soil amendment. The data obtained were
expected to give information about the chemical forms
of trace metals of primary concern, i.e., Ni, Cu, Zn,
Cd, and Pb, as affected by soil properties, the form
of sludge applied, and the rate of application of sludge
to cropped soils.

The surface horizons of two arid-zone field soils that had received
amendments of either liquid or dried, anaerobically digested sewage
sludge for 4 years were sampled to determine the forms of selected
trace metals in the solid phase. The soils had been amended with
sludge twice annually at rates of 0, 22.5, 45.0, or 90.0 tons ha'1
year'1. Barley and sorghum had been grown on the soils in randomized experimental plots. The soil samples were analyzed for total
Ni, Cu, Zn, Cd, and Pb and were fractionated by sequential extraction
to estimate the quantities of these metals in "exchangeable," "sorbed,"
"organic," "carbonate," and "sulfide" forms.
The total contents of the five metals in the two field soils were
governed by the total content of the metals in the sludges applied and
by the rate of sludge application. The accumulation of metals in the
surface horizons of field plots receiving liquid sludge was less than
that in the plots receiving composted sludge, possibly because of a
lesser reduction in soil bulk density resulting from sludge applications.
The percentage of the total metal content in exchangeable and sorbed
forms was very low, averaging between 1.1 and 3.7% for all of the
metals regardless of the type of soil, the form of sludge applied, or
the sludge application rate. The application of sludge tended to reduce
the sulfide fraction and to increase the organic and carbonate fractions
of all five trace metals. At the highest rate of sludge application, the
predominant forms of the metals were: Ni, sulfide; Cu, organic; and
Zn, Cd, and Pb, carbonate.
Additional Index Words: heavy metals, sewage sludge disposal, toxic
metals.
Sposito, G., L. J. Lund, and A. C. Chang. 1982. Trace metal
chemistry in arid-zone field soils amended with sewage sludge: I.
Fractionation of Ni, Cu, Zn, Cd, and Pb in solid phases. Soil Sci.
Soc. Am. J. 46:260-264.

ESEARCH on the possible adverse effects of trace

R
metal accumulation in agricultural soils amended
with municipal sewage sludge has begun to focus on
the chemical forms of trace metals in relation to their
uptake by plants (Chancy and Giordano, 1976; Stover
et al., 1976; Silviera and Sommers, 1977; Latterell et
al., 1978; Mahler et al., 1980). The working hypothesis
in this research has been that trace metal uptake by
crop plants grown in a sludge-amended soil can be
correlated with some extractable fraction of the metal
in the soil. This hypothesis appears to be a useful
guide, but recent work has shown that variability in
trace metal extractability, both with time and with the
chemical extractant employed, must be taken into
account (Chancy and Giordano, 1976; Silviera and
Sommers, 1977; Latterell et al., 1978). The commonly
observed decrease in trace metal extractability with
time indicates that extractions of field soils which have
received sewage sludge and been cropped over extended periods may be of more value than extractions
1
Contribution from the Dep. of Soil and Environmental Sciences,
Univ. of California, Riverside, CA 92521. Received 24 Sept. 1980.
Approved 26 Aug. 1981.
Professor of Soil Science, Associate Professor of Soil Science,
and Associate Professor of Agricultural Engineering, respectively.

260

SPOSITO ET AL.: TRACE METAL CHEMISTRY IN ARID-ZONE SOILS AMENDED WITH SEWAGE SLUDGE: I.

Table 1 Properties of the field soils.

Particle size fractions
Soil series
Domino
Greenfield

Sand
42
62

Silt
35
27

Clay
23
11

CEC

Table 2Total contentst of trace metals in the sludges.

pH
Organic (sat.
paste)
C

meq/100 g
14.0
8.7

261

%
4.3
0.8

Sludge

Application date

Ni

Cu

Zn

Composted

Winter 1975
Summer 1976
Winter 1976
Summer 1977
Winter 1977
Summer 1978
Summer 1976
Winter 1976
Summer 1977
Winter 1977
Summer 1978

303
260
295
275
378
483

829
750
763
712
903
1,042

- Mg/g 2,005
1,785
2,892
2,699
3,060
3,547

531
599
503
535
483

1,493
1,702
1,280
1,103
1,042

4,246
4,643
3,908
4,025
3,547

7.8
7.1

MATERIALS AND METHODS

Soil Samples
Surface horizons (0-15 cm) of two soils in randomized
experimental plots located at the Moreno Field Station of
the University of California, Riverside, were sampled in
September 1979. The experimental plots were employed in
a long-term field investigation by Chang et al. (1979) to
ascertain the utility of anaerobically digested sewage sludge
as a soil amendment. The plots sampled had received either
composted sludge or digested liquid sludge (3.0% total solids) amendments at the rate of 0, 22.5, 45.0, or 90.0 tons
ha~' year~'. The composted sludge was obtained from
the Joint Water Pollution Control Plant operated by Los
Angeles County Sanitation Districts. The source of the liquid
sludge was the same, but the material was not dewatered
prior to its application on the field plots.
The composted sludge had been applied twice annually,
beginning in the winter of 1975, to plots on Greenfield sandy
loam (coarse-loamy, mixed, thermic Typic Haploxeralf) and
on Domino loam (fine-loamy, mixed, thermic Xerollic Calciorthid). These plots had received eight sludge applications
at the time they were sampled for the present study. The
liquid sludge was applied twice annually, beginning in the
summer of 1976, only to plots on Domino loam. These plots
had received seven applications of sludge at the time they
were sampled. During the period of sludge application, all
of the field plots were cropped annually with barley (Hordeum vulgare) and sorghum (Sorghum vulgare). Complete
details of the field experiments are given by Chang et al.
(1979).
Some properties of the surface samples of the two soils
investigated, determined by standard methods (Black, 1965),
are listed in Table 1. Detailed field observations and textural
analyses indicated that soil properties were rather uniform
across each experimental plot and throughout the upper 15
cm of the soil profile. Chemical analyses showed that almost
all (> 90%) of the trace metal accumulation from sludge
applications on the plots was in the upper 15 cm of the soil
profile (Chang et al., 1979). Accordingly, it was expected
that studies of the surface soils in the plots would give
significant information concerning trace metal chemistry.
The metals chosen for study were Ni, Cu, Zn, Cd, and Pb.
The total contents of these metals in the applied sludges are
listed in Table 2 for the applications made from 1975 through
1978. The total contents of the five trace metals are generally
higher in the Los Angeles sludges than in representative
sludges obtained elsewhere in the U.S.A. (see, e.g., Stover
et al., 1976).
Trace Metal Fractionation
The total content of Ni, Cu, Zn, Cd, and Pb in the soil
samples were determined on filtered extracts obtained from
2-g samples which were digested by 12.5 ml 4M HNO3 at
80C overnight. The five trace metals in duplicate 2-g soil
samples were fractionated by a sequential extraction procedure modified after that of Stover et al. (1976). The modified extraction procedure, developed on the basis of studies
with model trace metal compounds (Lund et al., 1980), is
believed to give data concerning the fraction of trace metal
in exchangeable, sorbed, organic, carbonate, and sulfide

Liquid

Cd

Pb

34

1,758

30

1,775

32
57
61

1,475
1,377
1,050
1,797

84
106
73
72
61

1,012
823
997
655
1,797

30

T As determined after digestion with 4AT HNO3 at 80C overnight.

forms. These solid-phase chemical forms were determined

by sequential extractions with 25 g of the following reagents:
0.5M KNO3, 16 hours; deionized water, 2 hours (extract
three times and combine data); 0.5M NaOH, 16 hours;
0.05M Na2 EDTA, 6 hours; 4M HNO,, 16 hours at 80C.
During each extraction, the soil suspension was shaken.
After extraction the suspension was centrifuged and the
resulting supernatant solution was decanted and filtered.
The content of the five trace metals in the filtered solution
was determined by atomic absorption spectrophotometry.
The instrument employed was a Perkin-Elmer model 5000.
Standard solutions for the metals were prepared for each
extraction step in a background solution of the extracting
reagents. The amount of metal extracted by a given extracting reagent was calculated according to this equation:
jug extracted = C x 25 g - C' x M,
[1]
where C is the concentration (/ig/g) of the metal in the
extracted solution; C is the concentration (jug/g) of the
metal in the solution extracted in the preceeding step of the
sequence; and M is the mass of solution (g) carried over
to the present extraction from the preceeding one. Equation
[1] contains a correction for the amount of metal in the
solution entrained in the soil sample after the centrifugation
which follows each extraction. This correction is made in
lieu of washing the sample with deionized water after centrifugation, as suggested by Stover et al. (1976), because
washing may lead to metal losses and, therefore, low recovery of metal from the soil in a given extraction step.
Although the amounts of exchangeable, sorbed, organic,
carbonate, and sulfide forms of trace metals are believed
to correlate well with sequential extraction by KNO3, H2O,
NaOH, EDTA, and fiNO3, it is not critical to the present
study that this con-elation be exact. Therefore, the fractionation of the five trace metals usually will be reported
according to the extracting reagent employed (e.g., KNO3)
instead of the expected soil solid-phase fraction (e.g.,
exchangeable).
RESULTS AND DISCUSSION
Total Metal Contents
The total content of Ni, Cu, Zn, Cd, and Pb in the
soil samples is listed in Table 3. The general conclusion to be drawn from these data is that the trace
metal contents of the two soils, at any level of sludge
application, reflect the trace metal composition of the
sludges. The order of metal content in the composted
sludge is Zn > Pb > Cu > Ni > Cd, and this is the
order of metal content in both the Domino and Greenfield soils regardless of the sludge application rate. In
the liquid sludge, the order of metal content is Zn

262

SOIL SCI. SOC. AM. J., VOL. 46, 1982

Table 3Total content of trace metals in the sludge-amended

field soils.
Rate

Cu

Ni

Zn

Cd

Pb

tons-ha"
year-'
0.0
22.5
45.0
90.0

Extractant

8.9 0.9

19.7 0.1

46.8 0.0

168 1

1.56 0.06

53 1

32.3 0.0

74.3 0.0

293 1

3.13 0.00

89.9 0.6

58.5 0.5

141 2

469 6

6.8 0.3

181.8 0.2

10.2 0.1
21.6 0.2
27.9 0.8

21.0 0.1
46.7 0.9
64 3

42 1

98 7

91.1 0.4 0.1 0.0

169 1
1.75 0.0
232 10
2.8 0.2

8.65 0.05
28.8 0.5
43 3

Ni

Cu

o.ot

Zn
W;/g
3.0 0.1
50.9 0.0
66.5 0.4
89 1
209 1

Sum:

0.5
7.7
5.5
13.9
27.6

Total
content):

23.5 0.5 57.9 0.4 209 2

KNO, + H,O

Domino soil/composted sludge

8.3 LOT 17 2
76 8
<0.05

Domino soil/liquid sludge

0.0
22.5
45.0
90.0

Table 4Distribution of trace metals in Greenfield soils

amended with composted sludge at 45 tons>ha~' year'1.

NaOH
EDTA
HNO,

0.3
0.0
0.4
0.5

1.6
33.5
14.5
14.5
64.1

0.0
0.4
0.2
0.6
0.8

Cd

Pb

0.1 0.0
1.6 0.6
0.7 0.0 3.9 0.1
1.1 0.0 50.8 0.3
0.9 0.0 17.6 0.0
2.8 0.0 73.9 0.7
2.5 0.0

70 2

t Mean deviation of measurements on 2 different extracted soil samples,

t Obtained from Table 3.

Trace Metal Distributions

The experimental precision at any step of the sequential extraction procedure was always better than
5% and the sums of extracted trace metal contents
were always near, though usually systematically higher,
than the total metal contents listed in Table 3. These
features of the extraction procedure are illustrated in
Table 4 with data obtained for the Greenfield soil
amended
with composted sludge at 45 tons ha"1
1
year" . The sequential extraction procedure used by
Stover et al. (1976) on sludges tended to produce sums
of extracted contents of Ni, Cu, Zn, and Cd which

were 15 to 25% below the total metal contents,

whereas the extracted sum of extracted Pb was slightly
above its total content. In the present study, the sums
of extracted Zn, Cd, and Pb in the Domino soil samples and of Zn and Pb in the Greenfield soil samples
were, on the average, equal to the total metal contents
within experimental error, as indicated in Table 5. The
sums of extracted Ni and Cu in both soils and of Cd
in the Greenfield soil tended to be systematically
larger, by about 15%, than the total metal contents.
These small, systematic differences may have been
the result of the 4M HNO3 extraction in the sequential
procedure being more effective than the 4M HNO3
extraction to obtain the total metal content because
of preconditioning of the soil sample by the previous
extractions with NaOH and EDTA in the sequential
procedure.
The amounts of trace metals extracted with either
KNO3 or H2O from the soil samples always were very
small, as illustrated in Table 4. In general, the percent
of the total metal content (in Table 3) extracted by
KNO3 and H2O combined was < 6% for any metal
and any soil sample (see Table 6). Moreover, this
percent showed no trend with the type of sludge or
its rate of application.
The trends in the NaOH-, EDTA-, and KNO3-extractable metal contents with sludge application rate
are illustrated in Fig. 1 to 5 for the case of the Domino
soil amended with composted sludge. The extracted
metal contents are reported as percentages of the total
metal contents given in the first four rows of Table
3. Precisely the same trends as shown in Fig. 1 to 5
were found for the Domino soil receiving liquid sludge
and the Greenfield soil receiving composted sludge.
Figure 1 shows that, as the sludge application rate
increases, the percentage of Ni in the NaOH fraction
increases, while that in the HNO3 fraction drops. The
percentage of Ni in the EDTA fraction increases also,
but not systematically. It appears, therefore, that organic Ni and, to some extent, carbonate Ni are the
principal chemical forms of Ni induced through sludge
applications. However, even at the highest rate of

Table 5Sum of extracted trace metals, as a percent of total

metal content, for 8 Domino soil samples and
4 Greenfield soil samples.

Table 6Trace metal content, as a percent of total metal

content, in the KNO, + H2O fraction for 8 Domino soil
samples and 4 Greenfield soil samples.

360 17

4.8 0.2

72 8

Greenfield soil/composted sludge

0.0
22.5
45.0
90.0

6.3 0.1
15.8 0.5
23.5 0.5
45 2

13.5 0.1
36.3 0.7
57.9 0.4
114 3

66.2 0.6 0.1 0.0

138 1 1.25 0.0
2.50 0.0
209 2
5.3 0.2
376 12

6.15 0.05
40 2
70 2
149 7

t Mean deviation of measurements on 2 different soil samples.

> Cu > Pb > Ni > Cd, which is also the order found
in the Domino soil receiving this sludge.
In the soils amended with composted sludge, the
total content of Ni, Cu, Zn, Cd, and Pb increased
approximately proportionally to the sludge application
rate. However, in the Domino soil amended with liquid sludge, the increase in metal content was less than
proportional to the sludge application rate. This result
does not appear to be caused by migration of the
metals to lower parts of the soil profile after sludge
application, nor by the slightly greater metal uptake
by crop plants grown on the liquid sludge-amended
soil (Chang et al., 1979). Instead, it is probably caused
by differences in soil bulk density. At the same metal
input, the composted sludge application introduced
far greater amounts of organic solids and resulted in
a greater reduction of the soil bulk density. Therefore,
in a given volume of sampled soil, there was a greater
proportion of sludge in the soil treated with composted
sludge. On a mass basis, the metal concentration in
this soil thus would increase at a greater rate.

Soil
Domino
Greenfield

Ni

Cu

Zn

Cd

Pb

111 5t

114 10

102 8

107 9

103 8

117 7J

Il6=t5

105 11

116 4

111 9

t SD for 16 extractions,
j SD for 8 extractions.

Soil
Domino
Greenfield

Ni

Cu

Zn

Cd

Pb

3.6 1.3T
2.4 1.8J

3.7 1.6
3.4 1.4

1.7 0.8
1.6 0.4

1.2 1.2
2.7 2.5

2.8 2.4
1.1 0.3

T SD for 16 extractions.
t SD for 8 extractions.

SPOSITO ET AL.: TRACE METAL CHEMISTRY IN ARID-ZONE SOILS AMENDED WITH SEWAGE SLUDGE! I.
100

263

COPPER

NICKEL

80
(33 NaOH

W
NaOH
II EDTA

80

II EDTA

o 60

&2 HN03

UJ
H

o 60

40

40

20

22.5

22.5

90.0

45.0

SLUDGE A P P L I C A T I O N RATE (ton/ha-yr)

Fig. 1Distribution of Ni among the NaOH, EDTA, and HNO3
fractions of Domino soil amended with composted sludge.

sludge application, the HNO3 fraction amounts to

about one-half the total Ni content, and the order of
fraction content is HNO3 > EDTA > NaOH.
Figure 2 shows that the trend observed for Ni is
even more pronounced for Cu. At the highest sludge
application rate, the NaOH fraction amounts to 60%
of the total Cu content. The order of Cu contents in
the fractions is NaOH > EDTA > HNO3. This ordering is the reverse of that found for Cu in sludges
by Stover et al. (1976), but it is similar to that reported
by Schalscha et al. (1981) and is consistent with the
known affinity of Cu for organic matter ligands.
The trends shown for Zn in Fig. 3 are similar to
those for Ni in that the NaOH fraction increases while
the HNO3 fraction decreases with increasing sludge
application rate. In this case, there is also an increase
in the EDTA fraction, with the result that EDTA >
HNO3 > NaOH at the highest application rate. The
percentage of Zn accounted for in the NaOH fraction
at this rate is almost identical with that of Ni in Fig. 1.
It was not possible to fractionate Cd successfully
in the Domino and Greenfield soils at the zero sludge
100

ZINC
m

SLUDGE A P P L I C A T I O N R A T E (ton/ha-yr)
Fig. 2Distribution of Cu among the NaOH, EDTA, and HNO3
fractions of Domino soil amended with composted sludge.

application rate because the total metal contents were

so small (compare Table 3). Therefore, only fractions
determined in the sludge-amended soil are described
in Fig. 4. The trends shown are similar to those for
Zn, except for variability in the EDTA and HNO3
fractions. This same variability appeared in the Greenfield soil amended with composted sludge and in the
Domino soil amended with liquid sludge. Possibly this
variability is an experimental artifact connected with
the low absolute amount of Cd in the soil-sludge
mixtures.
In the case of Pb, Fig. 5 shows clearly that the
dominant fraction is EDTA regardless of the sludge
application rate. The NaOH fraction undergoes no
significant change with sludge application rate, whereas
the HNO3 fraction may decrease slightly.
CONCLUSIONS
The accumulation of Ni, Cu, Zn, Cd, and Pb in aridzone field soils amended with composted or liquid
sludge was found to be governed by the content of
the metals in the sludges and the rate of sludge application. Soil properties and sludge properties other
than metal content did not appear to play the dominant
role in determining metal accumulation, although the
rate of accumulation in field plots amended with liquid
sludge was less than in plots amended with composted

NaOH

II EDTA

80

80

,1

H
Z
UJ

|_

60

60

CADMIUM

g|| NaOH

(-

90.0

45.0

<

40

40

1 EDTA

& HN03

0
0

20
*

22.5

45.0

90.0

SLUDGE APPLICATION RATE (ton/ha-yr)

Fig. 3Distribution of Zn among the NaOH, EDTA, and HNO,
fractions of Domino soil amended with composted sludge.

IX

22.5

*
\

45.0

j;
90.0

SLUDGE APPLICATION RATE (ton/ha-yr)

Fig. 4Distribution of Cd among the NaOH, EDTA, and HNO,
fractions of Domino soil amended with composted sludge.

264

SOIL SCI. SOC. AM. J . , VOL. 46, 1982

100 "

able with milder reagents, such as dilute NaOH and

EDTA. This shift suggests that sludge applications
would provide the metals in labile chemical forms that
could be more readily available to crop plants than
in the nonamended soils.

LEAD
BS NaOH
CH EDTA

t; so

O HN03

bJ

-,

1-

60

_l
<t
g

40

U_

O
^
^
s
S1
s-

I^

S
s
s-

is

& ^

22.5

45.0

90.0

SLUDGE APPLICATION RATE (ton/ha-yr)

Fig. 5Distribution of Pb among the NaOH, EDTA, and HNO3
fractions of Domino soil amended with composted sludge.

sludge and accumulation was greater in the more

clayey Domino soil than in the Greenfield soil.
The percentage of total Ni, Cu, Zn, Cd, and Pb in
the field soils which was extractable with KNO3 and
H2O was very low, averaging between 1.1 and 3.7%,
regardless of the type of sludge. These results are
comparable with those for water extraction reported
by Bradford et al. (1975) for soil at the bottom of a
sludge-drying pond; in the case of Zn, Cd, and Pb,
with those reported as exchangeable plus sorbed by
Stover et al. (1976); and in the case of Ni, Cu, and
Zn, with those reported by Schalscha et al. (1980,
1981). The low percentages of the metals in the (KNO3
+ H2O) fraction could signify a low availability of the
metals to crop plants, since the readily soluble form
of a trace metal is often regarded as the most bioavailable. However, recent work (Silviera and Sommers, 1977; Latterell et al., 1978) suggests that, e.g.,
KNO3 fractions of trace metals represent potential
mobility more than potential bioavailability in sludgeamended soils. Other extracted fractions, such as the
DTPA fraction, may be better correlated with trace
metal availability to plants.
The application of sewage sludge to the field soils
tended to reduce the HNO3 (sulfide) fraction percentages for all of the trace metals, regardless of the
type of sludge or soil. The application of sludge tended
to increase the NaOH (organic) fraction percentages
for all of the trace metals except Pb, for which there
was no change. Sludge applications also increased the
EDTA (carbonate) fraction percentages for all of the
metals. For Ni, the order of fraction percentages at
the highest sludge application rate was HNO3 >
EDTA NaOH, and for Pb, it was EDTA l> HNO3
> NaOH. These results indicate that the chemical
behavior of Zn, Cd, and Pb in the soils may be similar,
whereas that of Ni and Cu differ both from this group
and from one another.
It is evident that the application of sludge shifted
the solid phases containing Ni, Cu, Zn, Cd, and Pb
in the soils away from those extractable with more
severe reagents, such as 4M HNO3, to those extract-

ACKNOWLEDGMENTS
Gratitude is expressed to Kenneth M. Holtzclaw and John
E. Warneke for assistance in sampling the field plots, and
to Ed Betty, William Emmerich, and Carl Nelson for assistance with the sequential extraction analyses. The research reported in this paper was supported in part by a
grant from the Kearney Foundation of Soil Science and in
part by the Office of Water Research and Technology,
USDI, under the Matching Grant Program of Public Law
95-467, and the University of California Water Resources
Center, as part of OWRT Project no. B-212-CAL and Water
Resources Center Project UCAL-WRC-W-583. The contents of this paper do not necessarily reflect the views and
policies of OWRT, USDI, nor does the mention of trade
names or commercial products constitute their endorsement
or recommendation for use by the U.S. Government.