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Reprinted from the Journul c$Environmental Quuliiy

Volume 26, no. 1, January-February 1997, Copyright 8 1997, ASA, CSSA, SSSA
677 South Segoe Rd., Madison, WI 5371 1 USA

Chemical Fractionation of Cadmium, Copper, Nickel, and Zinc in Contaminated Soils


Lena Q. Ma* and Gade N. Rao
ABSTRACT mines metal behavior in the environment and its remobili-
Heavy metals are potentially toxic to human life and the environ- zation ability.
ment. Metal toxicity depends on chemical associations in soils. For Selective sequential extraction procedures have been
this reason, determining the chemical form of a metal in soils is commonly used for studying metal mobility and availabil-
.
important to evaluate its mobility and hioavailability Sequential ex- ity in soils. Numerous extraction schemes for soils and
traction was used to fractionate four heavy metals (Cd, Cu, Ni, and sediments have been described in the literature (Gupta
Zn) from nine contaminated soils into six operationally defined groups: and Chen 1975; Stover et al., 1976; Tessier et al., 1979;
water soluble, exchangeable, carbonate, Fe-Mn oxide, organic, and Tessier and Campbell, 1988; Miller and McFee, 1983;
residual. The residual fraction was the most abundant pool for all
Welte et al., 1983; Shuman, 1985; Rauret at al., 1989).
four metals examined. A significant amount (2.4-44%) of Zn was
present in the potentially available fraction: nonresidual fraction. A
The extraction scheme used here is based on operationally
major portion (40-74%)of Cu was associated with the organic, Fe- defined fractions: water soluble, exchangeable, carbon-
Mn oxide, and carbonate fractions in most of the soils. Contamination ate, Fe-Mn oxides, organic, and residual fractions. These
of Cd and Ni in these soils was not as severe as Zn and Cu. Assuming procedures are not entirely specific, and there will be
that mobility and bioavailability of these metals are related to their overlap between the fractions. Despite uncertainties as
solubility and geochemical forms, and that they decrease in the order of to the selectivity of the various extractants and to possible
extractionsequence, the apparent mobility and potential bioavailability problems due to readsorption, extraction procedures pro-
for these four metals in the soils were: Zn > Cu > Cd > Ni. Metal vide qualitative evidence regarding the forms of associa-
distributions in different chemical fractions in these soils depended tion of trace metals and, indirectly, of their bioavailability
on respective total metal concentrations, except for Zn. (Harrison, 1981).
Recently, attempts have been made to assess the bio-
availability of heavy metals in contaminated soils and
C ONTAMINATION of heavy metals in the environment
is of major concern because of their toxicity and
threat to human life and the environment (Purves, 1985).
sediments using sequential extraction (Xian, 1987,
1989). Such assessments assume that metal bioavailabil-
ity decreases with each successive extraction step in
Much research has been conducted on heavy metal con- the procedure. Therefore, metals in water soluble and
tamination in soils from various anthropogenic sources exchangeable fractions would be readily bioavailable to
such as industrial wastes (Haines and Pocock, 1980; the environment, whereas the metals in the residual
Parry et al., 1981; Culbard et al., 1983; Gibson and fraction are tightly bound and would not be expected to
Farmer, 1983), automobile emissions (Lagerwerff and be released under natural conditions (Xian 1989; Clev-
Specht, 1970; Fergusson et al., 1980; Garcia-Miragaya, enger and Mullins, 1982). The procedure of Tessier et
1984), mining activity (Davies and Ginnever, 1979; al. (1979) is one of the most thoroughly researched
Culbard and Johnson, 1984), and agricultural practice and widely used procedures to evaluate the efficacy of
(Colbourn and Thornton, 1978). decontamination treatments (Pardo et al., 1990; Rauret
Based on primary accumulation mechanisms in sedi- et al., 1988; Spevackova and Kucera, 1989; Calvet et
ments, heavy metals can be classified into five categories: al., 1990; Vicente-Beckett et al., 1991).
(i) adsorptive and exchangeable, (ii) bound to carbonate The primary objectives of this study were to investigate
phases, (iii) bound to reducible phases (Fe and Mn the chemical partitioning of Cd, Cu, Ni, and Zn in nine
oxides), (iv) bound to organic matter and sulfides, and contaminated soils and to evaluate the effect of total
(v) detrital or lattice metals (Salomons and Forstner, metal concentrations on metal partition into different
1980). Heavy metals present in these categories have fractions.
different remobilization behaviors under changing envi-
ronmental conditions (Forstner, 1985). Geochemical
forms of heavy metals in soil affect their solubilities, MATERIALS AND METHOD
which directly influence their bioavailability (Xian, Nine contaminated soils collected from various U.S. loca-
1987). Therefore, determining total content of heavy tions were used in this study (Table l). These soils reflect
metals is insufficient to assess the environmental impact various sources of metal contamination,which can be classified
of contaminated soils and sediments (Salomons and Fors- into two broad categories: agricultural activities, such as the
tner, 1980), because it is the chemical form that deter- application of pesticide PbHAs04; and industrial activities,
such as mining and smelting.
The procedure of Tessier et al. (1979), selected for this
Soil and Water Science Dep., Univ. of Florida, Gainesville, FL 3261 1-
0290. Received 17 Nov. 1995. *Corresponding author (qma@gnv.ifas.
study, is designed to separate heavy metals into six operation-
ufl.edu). ally defined fractions: water soluble, exchangeable, carbonate
bound, Fe-Mn oxides bound, organic bound, and residual
Published in J. Environ. Qual. 26:259-264 (1997). fractions. A summary of the procedure is as follows:
259
1

260 J. ENVIRON. QUAL., VOL. 26, JANUARY-FEBRUARY 1997

Table 1. Nine metal-contaminated soils used in the research.


Soil name Abbreviation Location Contamination source PHt SOMS
g 4-’
Burch BU Old apple orchard, WA PbHAs04 5.85 25
Twin Tw Old apple orchard, WA PbHAso4 7.28 23
Burch Loam BL Old apple orchard, WA PbHAso4 5.83 25
East Field 1 EF1 Residential area, MT Smelter site 6.78 21
East Field 2 EEL Residential area, MT Smelter site 6.80 22
FTC PT Oklahoma Smelter site 7.51 61
BPS BP Berks County, PA Battery breaking site 6.14 15
RRS RR Berks County, PA Battery breaking site 7.03 38
AEC 1-1 DA Bridgeport, CT Burning ground 7.51 19
t Measured in 1:2 soil/water suspensions after 24 h.
$ Soil organic matter content.

One gram of each soil is weighed into a 40-mL polycarbonate ground correction and other sources of error. At least one
centrifuge tube and the following fractions obtained. duplicate and one spike sample were run for every 10 samples
Water Soluble. Soil sample extracted with 15 mL of deion- to verify precision of the method. The spike recovery and
ized water for 2 h. precision were found to be within 100 f 10%.
Exchangeable. The residue from water soluble fraction is
extracted with 8 mL of 1 M MgC12 (pH 7.0) for 1 h. RESULTS AND DISCUSSION
Carbonate-Bound. The residue from exchangeable fraction
is extracted with 8 mL of 1 M NaOAc (adjusted to pH 5.0 Soil has long been regarded as a repository for society’s
with HOAc) for 5 h. wastes. Gradually mobilized by biogeochemical pro-
Fe-Mn Oxides-Bound. The residue from carbonate frac- cesses, soil contaminants can pollute water supplies and
tion is extracted with 0.04 M NH20H*HC1in 25% (v/v) HOAc impact food chains. Heavy metals, such as Cd, Cu, Ni,
at 96°C with occasional agitation for 6 h. and Zn, are all potential soil pollutants. Soils consist of
Organic-Bound. The residue from Fe-Mn oxide fraction heterogeneous mixtures of organic and inorganic solid
is extracted with 3 mL of 0.02 M HNO3 and 5 mL of 30% components as well as a variety of soluble substances.
H202(adjusted to pH 2 with HNO,). The mixture is heated
to 85°C for 2 h, with occasional agitation. A second 3-mL Therefore, metal distribution among specific forms varies
aliquot of 30% HzOz (pH 2 with HNO,) is added and the widely based on the metal’s chemical properties and
mixture heated again to 85°C for 3 h with intermittent agitation. soil characteristics (Soon and Bates, 1982). Thus, it is
After cooling, 5 mL of 3.2 M NH40Ac in 20% (v/v) HN03 important to evaluate the availability and mobility of
is added and the samples diluted to 20 mL and agitated continu- heavy metals to establish environmental guidelines for
ously for 30 min. potential toxic hazards and to understand chemical behav-
Residual. The residues from organic fraction are digested ior and fate of heavy metal contaminants in soils (Davies,
using a HF-HCI/HN03 dissolution procedure in a Parr 4745 1980).
acid digestion Bomb (Bernas, 1968). A standard Reference The sequential extraction used in this study is useful
Material (271 1 Montana Soil; National Inst. of Standards and to indirectly assess the potential mobility and bioavail-
Technology, Gaithersburg, MD 20899) was used to verify the
acid digestion method used in this study. The recovery for all ability of heavy metals in the soils. The six chemical
trace metals in the standard was within 100 f 10%. fractions are operationally defined by an extraction se-
After each successive extraction, separation was done by quence that follows the order of decreasing solubility
centrifuging (Beckman Model J2-21) at 14K rpm (15400 x (Xian, 1989; Clevenger and Mullins, 1982; Soon and
g) for 30 min. The supernatants were removed with a pipette, Bates, 1982; Lake et al., 1984). Assuming that bioavail-
filtered with 0.2-pm Nucleopore polycarbonate membrane fil- ability is related to solubility, then metal bioavailability
ters, and analyzed for metals. The residue was washed with decreases in the order: water soluble > exchangeable >
8 mL of deionized water followed by vigorous hand shaking, carbonate > Fe-Mn oxide > organic > residual. This
and then followed by 30 min of centrifugation before the next order is just a generalization and offers only qualitative
extraction. information about metal bioavailability. Based on the
above information, we can further assume that metals
Analytical Methods in the nonresidual fractions are more bioavailable than
All extractions were conducted in triplicate in acid-washed metals associated with the residual fraction. The nonre-
(5% HN03) polycarbonate labware. All chemicals used in this sidual fraction is the sum of all fractions except the
study were of analytical grade or better. Double deionized residual fraction.
water, from a Barnstead NANOpure water system was used.
Total metal concentrations of the supernatants from each Zinc
step were analyzed by atomic absorption spectrophotometer
(Perkin-Elmer 2380) equipped with a graphite furnace atom- Zinc was mostly concentrated in the residual fraction,
izer. Flame atomic absorption was used to analyze metal con- although it was also present in other fractions (Table 2).
centrations >I mg L-’ and graphite furnace atomizer was The percentage of total Zn in the residual fraction ranged
used to measure metal concentrations <1 mg L-’. Multilevel from 55.8% (EF1) to 97.6% (PT). The greater percent-
standards (Fisher Scientific) for all metals were prepared for age of Zn in the residual fraction probably reflects the
each extraction step in the same matrix as the extracting re- greater tendency for Zn to become unavailable once it
agents to minimize matrix effects. Blanks were used for back- was in soils. Similar Zn results were reported for a soil
MA & RAO: CHEMICAL FRACTIONATION OF HEAVY METALS 26 1

Table 2. Zinc concentrations in each fraction of nine contaminated soils.


Total Zn concentrations, mg kg-'
Fractions BU Tw BL EF1 EF2 PT BP RR DA
Water suluble 1.05 f 0.0 0.15 f 0.0 0.90 f 0.0 7.95 f 0.2 1.95 f 0.0 0.15 f 0.0 1.65 f 0.0 0.15 f 0.0 0.60 It 0.0
Exchangeable 20.1 f 2.0 2.80 f 0.2 18.4 f 1.1 133 f 10 46.2 f 2.1 1.60 f 0.0 5.90 f 0.1 12.0 f 0.8 0.8 f 0.0
CarboIUlte 9.84 f 0.3 10.0 f 0.5 12.6 f 0.2 335 f 7.0 116 f 6.8 2.56 f 0.0 5.92 f 0.1 3.36 f 0.1 195 f 13
Fe-Mn oxide 23.2 f 0.5 14.0 f 1.0 15.0 f 1.1 424 f 20 189 f 10.2 8.50 f 0.0 13.6 f 1.0 60 f 3.43 135 f 9.5
Organic 2.40 f 0.0 2.20 f 0.1 2.20 f 0.1 163 f 10 89.4 f 4.8 1.60 f 0.0 6.20 f 0.0 1.40 f 0.0 10.8 f 0.7
Residual 100 f 9.0 90 f 6.2 120 f 7.2 1340 f 30 800f40 560 f 30 55 f 6.0 550 f 42 440f26
Sum of all fractions 157 f 12 119 f 7.9 169 f 9.7 2400 f 77 1240f64 574 f 30 88.3 f 7.2 627 f 46 782 f 48
Nonresidual, % 36.3 24.4 29.0 44.2 35.6 2.40 37.7 12.3 44.1
Residual, % 63.7 75.6 71.0 55.8 64.4 97.6 62.3 87.7 55.9

from tailing dumps (Jordao and Nickless, 1989) and 1.1%) was associated with the organic, exchangeable,
in near-shore sediments (Gupta and Chen, 1975). The and water soluble fractions, and no Cu was extracted
amount of Zn present in the nonresidual fractions ranged from the carbonate and Fe-Mn oxide fractions. Gupta
from 2.4% (PT) to 44.2% (EFl) (Table 2). Among the and Chen (1975) and Hickey and Kittrick (1984) also
nonresidual fractions, the Fe-Mn oxide fraction con- found a majority of the Cu in soils and sediments to be
tained the greatest amount of Zn in all soils except BL and associated with the residual fraction. Although Cu was
DA soils, in which the exchangeable and the carbonate found in all fractions in EFl, EF2, BP, and DA soils,
fractions, respectively, had the greatest amount of Zn it was mostly concentrated in the last four fractions. In
(Table 2). This may be partially due to the high stability the case of EF1 and EF2 soils, the greatest percentage
constants of Zn oxides. Several other workers have also of Cu was associated with the organic fraction (34-
found Zn to be associated with Fe-Mn oxides (Kuo et 35%) (Table 3). Our results were consistent with that
al., 1983; Ramos et al., 1994). Xian (1989) found that of Harrison (1981) who found significant amount of Cu
the sum of the exchangeable and the carbonate-bound in roadside soils associated with the organic fraction.
forms were strongly correlated with Zn uptake by cab- The major association of Cu with the organic fraction
bage plants (Brussicu oleruceu). The sum of Zn in the in these two soils may be due to high formation constants
exchangeable and carbonate fractions in our study ranged
of organic-Cu complexes (Stumm and Morgan, 1981).
from 0.73% (PT) to 25% (DA), which indicates that
the Zn in some of these soils may be highly available In BP soil, the greatest percentage of Cu (58%) was
for plants. The concentrations of the water soluble and present in the residual fraction. The Fe-Mn oxide fraction
organic fractions in these soils was relatively low was the next most important fraction for this soil (BP)
(Table 2). (19.2%), followed by the organic (15.6%), carbonate
Soils used in this study were contaminated from four (12.3%), exchangeable (2.5%), and water soluble frac-
different sources (Table 1). The order of Zn association tion (0.15%) (Table 3). Soil DA had the highest percent-
with various chemical fractions was the same for the age of Cu associated with the Fe-Mn oxide fraction
three soils collected from former smelter sites (EF1, (35%). The residual (30%), carbonate (26%), and or-
EF2, and PT) (Table 2), whereas the trend varied for ganic (10%) fractions also contained a significant portion
the rest of the soils contaminated from other three sources of total Cu in DA soil, whereas Cu in the exchangeable
(Table 2). In general, the association of Zn in these soils (0.08%) and water soluble (0.07%) fractions was negli-
was in the decreasing order of residual > Fe-Mn oxides gible.
> carbonates > organic > exchangeable > water soluble. Of the nine soils studied, four (BU, TW, BL, and
Soils EFl and EF2 were more contaminated than the RR) were not contaminated with Cu, whereas the re-
other soils. Although a large percentage of the total Zn maining five soils (EFl, EF2, DA, PT, and BP) were
was in the residual fraction in these soils, the amount contaminated with Cu (>240 mg kg-'). The normal Cu
of Zn present in the nonresidual fractions was also appre- concentration in soils is 2 to 100 mg kg-' (Lindsay,
ciable from the standpoint of potential Zn mobility and 1979). On the average, percent of total Cu associated
bioavailability. The potential mobility and bioavailability with different fractions in the nine soils was in the follow-
of Zn in these soils would be in the order: EFl > DA ing order: residual > organic > Fe-Mn oxide > carbonate
> BP > BU > EF2 > BL > TW > RR > PT. An attempt > exchangeable > water soluble. As far as the mobility
was made to correlate the effect of total Zn content in and potential bioavailability of Cu in these soils are
soils on the distribution of Zn in the various chemical concerned, the order was as follows as: EF1 > DA >
fractions and found that the distribution was independent EF2 > BP > RR > TW > BL > BU > PT.
of the total amount of Zn present in the soils (Fig. la).
Copper distribution in various chemical fractions de-
pended on the total Cu content of the soils (Fig. lb).
Copper As the total Cu concentration in the soils increased, the
Like Zn, most of the Cu in these soils was present in percent of total Cu in the water soluble, carbonate, Fe-
the residual fraction (Table 3). In BU, TW, BL, PT, Mn oxide, and organic fractions increased and Cu in
and RR soils, >97.6% of the Cu was associated with the exchangeable and residual fractions decreased. Our
the residual fraction. A small percentage of Cu (0.13- results suggest that as the extent of Cu contamination
262 J . ENVIRON. QUAL., VOL. 26, JANUARY-FEBRUARY 1997

Water Exch. Carb. Fe-Mn Organic Res.


100

El 0
-
c
.-
3
0
0

c
L
v)
b
z1

0.1
Water Exch. Carb. Fe-Mn Organic Res. Water Exch. Carb. Fe-Mn Organic Res.
Fractions Fractions

Fig. 1. Distribution of heavy metals in various chemical fractions as a function of total metal content in soils (a)Zn, (b) Cu, (c) Cd, and ( d )
Ni.

in soils increased, more Cu was associated with the nonresidual fractions was much greater than that of the
nonresidual fractions, which increased potential Cu mo- residual fractions (Table 4). Sixty seven percent of the
bility and bioavailability in these soils. Cd in EF1 soil and 57% in EF2 soil was associated with
the exchangeable, carbonate, and Fe-Mn oxide fractions
Cadmium (Table 4), with the exchangeable fraction being the great-
More than 91 % of the total Cd in all soils, excluding est. This suggests that Cd in these two soils was poten-
EFl and EF2, was associated with the residual fraction tially bioavailable because the metals present in the ex-
(Table 4): Cadmium in EF1 and EF2 soils was presented changeable fraction are usually thought to be readily
in all fractions. However, the percentage of Cd in the available for plant uptake (Xian, 1989). These results

Table 3. Copper concentrations in each fraction of nine contaminated soils.


Total Cu concentrations, mg kg-'
Fractions BU Tw BL
~
EFl
~
EFZ
~
FT ~
BP
~ ~
RR
~~~
DA
Water soluble BDLt BDL BDL 1.5 f 0.0 1.05 f 0.0 BDL 0.15 f 0.0 0.15 f 0.0 0.75 f 0.0
Exchangeable 0.5 f 0.0 0.50 f 0.0 0.80 f 0.0 3.10 f 0.2 2.00 f 0.0 0.50 f 0.0 2.50 f 0.0 1.10 f 0.0 0.80 f 0.0
Carbonate BDL BDL BDL 256 f 10 100 f 5.2 BDL 12.3 f 1.0 BDL 261 f 9.2
Fe-Mn oxide BDL BDL BDL 229 f 11 120 f 6.5 BDL 19.2 f 0.5 BDL 352 f 11
ol-pnic BDL BDL BDL 411 f 20 225 f 8.2 0.40 f 0.0 15.6 f 1.1 0.60 f 0.0 99.8 f 6.9
Residual 46.0 f 3.5 20.0 f 1.5 60.0 f 2.4 310 f 12 200 f 7.2 240 f 12 70.0 f 7.3 100 f 7.1 300 f 15
Sum of all fractions 46.5 f 3.5 20.5 f 1.5 60.8 f 2.4 1210 f 52 648 f 27 241 f 12 120 f 6.2 102 f 7.1 1010 f 43
Nonresidual, I 1.10 2.40 1.30 74.4 69.0 0.40 41.7 2.90 70.0
Residual, I 98.9 97.6 98.7 25.6 30.9 99.6 58.3 98.0 30.0
t BDL = below detection limit.
MA & RAO: CHEMICAL FRACTIONATION OF HEAVY METALS 263

Table 4. Cadmium concentrations in each fraction of nine contaminated soils.


Total Cd concentrations, mg kg-l
Fractions BU Tw BL EF1 EM PT BP RR DA
Water soluble BDLt BDL BDL 1.50 f 0.0 0.45 f 0.0 BDL 0.15 f 0.0 0.15 f 0.0 BDL
Exchangeable 1.10 f 0.0 0.80 f 0.0 0.80 f 0.0 50.7 f 4.0 30.0 f 2.1 0.80 f 0.0 1.10 f 0.0 1.10 f 0.0 0.80 f 0.0
Carbonate BDL BDL BDL 36.9 f 1.0 16.4 f 1.0 BDL 0.32 f 0.0 BDL BDL
Fe-Mn oxide 0.20 f 0.0 BDL BDL 25.2 f 2.0 11.4 f 0.2 BDL 1.00 f 0.0 BDL 0.60 f 0.0

I Organic
Residual
Sum of all fractions
BDL
13.0 f 0.9
14.3 f 1.0
BDL
4.0 f 0.4
4.1 f 0.4
BDL
20.0 f 1.2
20.8 f 1.2
4.40 f 0.0
50.0 f 4.5
169 f 12
1.80 f 0.0
40.0 f 2.4
101 f 5.0
BDL
40.0 f 1.2
41.0 f 1.2
0.20 f 0.0
60.0 f 3.0
62.0 f 3.0
BDL
40.0 f 2.0
41.3 f 2.0
BDL
40.0 f 1.7
41.4 f 1.7

I Nonresidual, W
Residual, W
9.00
91.0
2.00
98.0
4.00
%.O
70.0
30.0
60.0
40.0
2.40
97.6
3.20
%.8
3.00
97.0
3.40
97.0
t BDL = below detection limit.

were in agreement with the observations of Harrison CONCLUSIONS


(1981), Miller and McFee (1983), and Kuo et al. (1983). A sequential extraction procedure was used to fraction-
Generally, the Cd association with different fractions
followed the order: residual > exchangeable > carbonate ate Zn, Cu, Cd, and Ni present in nine contaminated
> Fe-Mn oxide > organic > water soluble. It was also soils. Different geochemical fractions are operationally
observed that the distribution of Cd in various chemical defined by an extraction sequence that generally follows
fractions depended on the total Cd content (Fig. lc). the order of decreasing solubility. The residual fraction
Cadmium was present in all fractions when the total Cd was the most abundant pool for all the metals in the
concentration was >50 mg kg-'. It was not present soils studied. However, in most of the soils, a significant
in the organic and carbonate fractions when the total percentage of total metals was associated with the nonre-
concentration was <50 mg kg-'. sidual fractions. Therefore, they should be evaluated
when studying the pollution levels of heavy metals in
Nickel soils.
Like Zn, Cu, and Cd, the residual fraction was by A significant amount of Zn was associated with the
far the most important fraction for Ni in all the soils, nonresidual fractions in soils studied, indicating that this
ranging from 57% (EF1) to 94% (PT) (Table 5). These metal was potentially more bioavailable than other metals
results are consistent with the observations of Gupta and examined. Copper was found primarily in the residual
Chen (1975) and Tessier et al. (1980), who suggested or the organic fractions in most of the soils. Little Cd
that a majority of the Ni in soils and sediments was and Ni were found in these soils. Overall, the order of
detrital in nature. The exchangeable and Fe-Mn oxide contamination was Zn > Cu > Cd > Ni. Among the
fractions contained most of the Ni in the nonresidual nine soils tested, EF1, EF2, and DA soils were the most
fractions (Table 5 ) . Nickel was not detected in the water contaminated soils with the four heavy metals studied.
soluble fraction in any of the soils. Total Ni concentra- The distribution of Zn in various chemical fractions
tions in these soils ranged from 9.0 to 98.7 mg kg-' was independent of the total Zn concentration in soils,
(Table 5 ) compared with the normal soil range of 5 to whereas the distribution of Cu, Cd, and Ni in different
500 mg kg-' (Lindsay, 1979), which suggests little Ni fractions depended on respective total metal concentra-
contamination in these soils. Nickel was found in all tions in the soils.
the fractions, irrespective of the total Ni concentration
(excluding the water soluble fraction) in these soils (Table
5 ) . A decreasing trend in percent of total Ni in the
ACKNOWLEDGMENTS
exchangeable, and an increasing trend in the residual
fractions, was observed with increasing total Ni concen- Approved for publication as Florida Agricultural Experiment
tration (Fig. Id). No clear trend was observed in Ni Station Journal Series No. R-05313.Authors would like to
concentrations present in other chemical fractions as total thank Ms. Angela Choate for partially conducting the experi-
Ni concentrations increased. ments.

Table 5. Nickel concentrations in each fractions of nine contaminated soils.


Total Ni concentrations, mg kg-I
Fractions BU Tw BL EFl EF2 PT BP RR DA
Water soluble BDLt BDL BDL BDL BDL BDL BDL BDL BDL
Exchangeable 3.30 f 0.0 2.80 f 0.1 3.30 f 0.1 3.90 f 0.1 3.30 f 0.16 3.90 f 0.2 3.10 f 0.1 3.10 f 0.0 3.10 f 0.1
CarboMk BDL BDL 0.32 f 0.0 0.88 f 0.0 0.56 f 0.0 0.32 f 0.0 BDL 0.32 f 0.0 0.32 f 0.0
Fe-Mn oxide 0.80 f 0.0 0.20 f 0.0 BDL 2.80 f 0.0 1.60 f 0.0 1.50 f 0.0 1.60 f 0.0 BDL 3.60 f 0.1
Organic BDL BDL BDL 0.80 f 0.0 0.40 f 0.0 BDL 0.60 f 0.0 0.80 f 0.0 BDL
Residual 26.0 f 2.5 6.00 f 0.3 17.0 f 1.3 11.0 f 0.1 14.0 f 0.9 93.0 f 2.0 14.0 f 0.9 26.0 f 0.7 21.0 f 1.5
Sum of all fractions 30.1 f 2.5 9.00 f 0.4 20.6 f 1.3 19.4 f 0.2 20.0 f 1.1 98.7 f 2.2 19.3 f 1.0 30.2 f 0.7 28.0 f 1.3
Nonresidual, % 13.6 33.3 17.5 43.3 30.0 5.80 27.5 14.0 25.0
Residual, W 86.4 66.7 82.5 56.7 70.0 94.2 72.5 86.0 75.0
t BDL = below detection limit.
264 J. ENVIRON. QUAL., VOL. 26, JANUARY-FEBRUARY 1997

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