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Table1. Cumulative
biosolids andheavymetalIoadingson the 1-9 plots at the Rosemount
Experimental
Station.
Cumulativeloads
Years
Treatment applied Biosolids Cd Cr Cu Ni Pb Zn
-~
Mgha -~
kg ha
Low 1977-1979 60 9 48 41 16 54 106
Med 1977-1979 120 17 91 83 26 97 220
High 1977-1979 180 25 141 127 43 173 343
CPLRlimit’~ 39 3000 1500 420 300 2800
Cumulative Pollutant LoadingRate limit established by the USEPA
(1993).
1314 J. ENVIRON.QUAL., VOL. 27, NOVEMBER-DECEMBER
1998
Table 2. Croppingand fertilizer history of I-9 field plots during and after biosolids applications.
Year Crop Variety Fertilizerappliication
1977 Cornt Pioneer 3780 Dewateredsludge
1978 Corn Pioneer 3780 Dewateredsludge + 1112 kg K -1
ha
1979 Corn Pioneer 3780 Dewateredsludge
1980 Corn Pioneer 3780 None
1981 Corn Pioneer 3780 None
1982 Corn Pioneer 3780 92 kg ha-1 N
1983 Corn Pioneer 3780 92 kg ha-1 N
1984 Corn Pioneer 3780 160 + 98 kg ha-~ N-t+ K
1985 Oat~ Ogle 35 + 15 + 29 kg ha N + P + K
1986 Alfaifal[ None
1987 Oat None
1988 Alfalfa Pioneer 532 129 kg ha-~ K
1989 Alfalfa Pioneer 532 None
1990 Alfalfa Pioneer 532 112 kg ha-1 K
1991 Corn None
1992 Corn Dekalb 421 115 kg ha-t N + manure
1993 Corn NK4242 40 + 112 kg ha-1 N + K
1994 Soybean§ Evans None
1995 Corn NK4242 83 kg ha-I N
~ Zea mays.
~ Avena sativa L.
¶ Medicagosativa L.
§ Glycine max.
biosolids loadings on surface soil OC(0-0.30 m) <1 at the 120 and 180 Mgha -1 loading rate. However,
after the third and final biosolids application (1979) and the similarity of the regression lines for 1979 and 1995
16 yr after application (1995). Less than 1 yr after the suggests there were only small changes in soil OCfor
third and final biosolids application (1979), soil OCwas the control and biosolids treatments during the 16 yr
linearly correlated to cumulative loading rate (r = 0.61). after cessation of biosolids applications.
The same relationship was still apparent in 1995 (r The greatest rate of OCmineralization in biosolids-
0.56), 16 yr after the last biosolids application. treated soils occurs within 7 to 11 d after applications
Significant increases in soil OCwere expected due to (Lerch et al., 1992; Wisemanand Zibilske, 1988). After
the addition of relatively large amountsof biosolids to this initial period of rapid mineralization, biosolids-
the soil (i.e., up to 180 Mgha-l). A more relevant ques- treated soils continue to exhibit greater OCmineraliza-
tion is the fate of biosolids-applied organic matter in tion rates than untreated soils (Boyle and Paul, 1989;
the soil with time. Beckett and Davis (1978) suggested Linden et al., 1994). However, the rate of OCdecompo-
a possible "time bombeffect" where leaching of heavy sition decreases greatly with time if no additional biosol-
metals would increase with time due to decomposition ids applications are made. Logan et al. (1997) observed
of biosolid organic matter. For the individual treatments the greatest decrease in soil OCduring the first 2 yr after
in our study, there were no statistically significant biosolids applications with only small changes during the
changes in soil OCcontent between 1979 and 1995. This next 3 yr. Boyle and Paul (1989) suggested that total
was due in part to high levels of variability, especially soil OCin biosolids-treated soils after 3 yr of field de-
composition might be more recalcitrant than native soil
45 OC. In our study, biosolids were applied over a 3-yr
1976:Prior to application period with the largest application being madethe first
-1
year. Annual applications rates for the 180 Mg ha
1979: Y = 20.35 + 0.05X; r= 0.61"*
1995: Y = 21.8 + 0.04X; r = 0.56** cumulative loading were 90, 45, and 45 Mgha -1 yr -1
for 1977, 1978, and 1979, respectively. Consequently,
when soil OCwas measured in 1979, 50°,/0 of the total
biosolids load had decomposed for more than 2 yr and
75%for more than 1 yr. Lack of significant decreases
in soil OCfrom 1979 to 1995 suggests that the period
of most rapid decomposition had already occurred and
subsequent rates of decomposition were much lower.
The addition of an estimated <1 Mgha-1 dairy manure
in 1992 ( Table 2) was too small to significantly affect
soil OC.
0 60 120 180
"1
BIOSOLIDSLOADING,Mg ha Vertical Translocation of Heavy Metals
Fig. 2. Soil OCas a function of total biosolids Ioadings for the last Sixteen years after cessation of biosolids applications,
year of application (1979) and16 yr after applications (1995). Bars all heavy metals exhibited a similar pattern of distribu-
showsoil OClevels before first biosolids application (1976). Error
bars represent _+1 standard deviation of the treatment means. tion with depth in the well-drained Waukegansilt loam
**Significant at the 0.05 level of probability. soil (Fig. 3). Biosolids-applied heavy metals were mostly
SLOAN ET AL.: RECOVERYOF BIOSOLIDS-APPL1ED HEAVYMETALS 1315
Cd Ni Zn
0.00
:--.
0.30 .,,,....
0.45 /
NS NS NS
0.60 Itl i NS ~lz NS ~ 0
E 0.75 ~l.qNS
- NS
0.90 ’ : : ~, : i"~
O. 0 2 4 6 8 5 10 15 0 30 60 90 120
IU --~-- 120
Cr Cu Pb
.a
o.oo ± --~-- 180
", ""
NS
0.45 ~-
0.66
0.90 ~
0 10 20 30 20 40 0 20 40 60 80
METAL CONCENTRATION, 4
mg kg
Fig. 3. Distributionof Cd, Cr, Cu, Ni, Pb, andZn in the profile of a well-drained,TypicHapindoll16 yr after biosolidsapplications.*, **, ***
Significant effect of biosolids loading at 0.05, 0.01, and 0.001 level of probability, respectively.
concentrated in the upper 0.30 mof soil. Metal concen- 0.45 m depth. Movementof heavy metals to the 0.30 to
trations at the 0 to 0.15 m depth were similar to those 0.45 m depth maybe attributed to co-transport with soil
at the 0.15 to 0.30 m depth. At the 0.30 to 0.45 msoil colloids and/or bioturbation by soil organisms. There is
depth, metal concentrations in biosolids-treated soils no indication that significant amounts of heavy metals
were slightly elevated above the control (P < 0.05). have migrated to depths >0.45 m.
Below 0.45 m, biosolids-applications had no effect on
heavy metal concentrations. These heavy metal distribu- Heavy Metal Recovery
tion patterns are similar to those reported by McGrath
and Lane (1989) 24 yr after applying biosolids at a rate Since biosolids applications had no effect on soil metal
of 30.6 Mgha -~ yr -~ for 20 yr. Chang et al. (1983) concentrations below 0.45 m (Fig. 3), only the upper
reported that more than 90% of biosolids-applied Cd 0.60 m of soil was used to calculate heavy metal recover-
and Zn (50 and 2000 kg ha-~, respectively), remained ies. In general, >90%of biosolids-applied Cd, Cu, Ni,
in the 0 to 0.15 m soil layer after applying biosolids at Pb, and Zn were present in the upper 0.30 m of soil
90 Mgha-1 yr -~ for six consecutive years. Studies that (Table 3). This finding agrees with various studies that
examined heavy metal concentrations with depth in bio- found about 95%of Cd, Cu, Pb, and Zn were retained
solids-treated soils generally report increased metal con- in the 0 to 0.30 m depth after application of sewage
centrations to a depth of 0.30 m, but no measurable sludge to soil (Sidle and Kardos, 1977; Sidle et al., 1977;
increases below 0.40 m (Chang et al., 1982, 1983; Dowdy Parker et al., 1978). In fact, if soils are sampledwithin
and Volk, 1983; Kelling et al., 1977; McGrathand Lane, 1 to 6 yr after biosolids application, more than 90%of
1989; Parker et al., 1978; Sidle and Kardos, 1977; Sidle heavy metals are found in the 0 to 0.15 mdepth (Chang
et al., 1977; Williamset al., 1984, 1985). etal., 1983).
The six heavy metals examinedin this study (Cd, Cr, In the present study, metal concentrations at the 0 to
Cu, Ni, Pb, and Zn) have different chemical properties 0.15 m depth were approximately equivalent to those
due to their atomic structures. Consequently, each metal at the 0.15 to 0.30 mdepth (Fig. 3). Metal concentrations
reacts differently with biosolids and soil solids (McLean at the 0.15 to 0.30 mdepth 16 yr after biosolids applica-
and Bledsoe, 1992). Their association with soil solids tions were generally within 10%of the concentrations
ranges from easily-extracted exchangeable forms for Cd extracted with 1 M HNO3by Dowdy and Volk (1983)
to more resistant oxide and strongly-bound organic and at the 0.10 to 0.20 mdepth <1 yr after applying biosolids.
inorganic forms for Cr and Pb (Sloan et al., 1997). With The concentrations measured by Dowdy and Volk
this in mind, it is somewhatsurprising to see similar (1983) at the 0.10 to 0.20 m depth are equivalent to 51,
patterns of distribution in the soil profile for each of 50, 54, and 37%of biosolids-applied Cd, Cu, Ni, and
these metals (Fig. 3). This suggests that physical, rather Zn, respectively. Assuming equal amounts of metals
than chemical, processes are primarily responsible for were present in the 0 to 0.10 m depth, nearly 100%of
heavy metal distribution in this soil. Biosolids were orig- biosolids-applied heavy metals were present in the up-
inally surface-applied and incorporated to a depth of per 0.20 mof soil 1 to 3 yr after the biosolids applications.
0.15 to 0.20 m with a moldboard plow. During the 16 The fact that 16 yr after biosolids applications, >90%
yr since biosolids were applied and soil samples for this of Cd, Cu, Ni, Pb, and Zn are present in the upper 0.30
study were collected (Table 2), annual tillage operations m of soil and 100% are present in the upper 0.45 m
have facilitated the movementof heavy metals to the indicates the heavy metals migrated very slowly into the
0.15 to 0.30 m depth and to a lesser extent, the 0.30 to soil profile and consequently, there was little risk of
1316 J. ENVIRON. QUAL., VOL. 27, NOVEMBER-DECEMBER 1998
Table 3. Percent of biosolids-applied heavy metals extracted (1 M HNO,) from the upper 0.60 m of a Typic Hapludoll.
0-0.15 0.15-0.30 0.30-0.45 0.45-0.60 0-0.60
Sludge
Metal load Mean SDt Mean SD Mean SD Mean SD Mean
Mg ha"1 Of
of total metals applied ———
Cd 60 44 11 49 9 10 3 2 2 105
120 49 2 45 7 4 3 1 0 99
180 51 10 55 13 5 2 0 0 111
Cr 60 19 1 23 3 6 3 4 2 52
120 27 0 27 6 3 2 2 1 59
180 25 5 31 14 2 1 1 0 59
Cu 60 43 10 49 7 10 3 6 3 108
120 54 1 52 9 6 3 3 1 115
180 51 9 62 20 5 2 1 0 119
Ni 60 45 13 49 13 1 5 0 0 95
120 48 3 42 13 0 0 0 0 90
180 48 4 56 7 10 5 0 0 114
Pb 60 40 11 44 8 8 6 7 5 99
120 48 1 43 7 3 2 3 2 97
180 47 14 47 15 6 5 2 0 102
Zn 60 37 9 42 10 9 2 5 3 93
120 46 2 44 8 3 3 1 1 94
180 43 8 49 13 5 3 1 0 98
f Standard deviation of the treatment mean.
groundwater contamination. It should be noted that amounts in the 0.30 to 0.45 m layer. Biosolids applica-
these results are valid for the soil type used in this study tions had little or no effect on heavy metal concentra-
and for other soils with similar composition, structure, tions below 0.45 m. Approximately 100% of biosolids-
and management history. The results may not be the applied Cd, Cu, Ni, Pb, and Zn were recovered from
same for soils with different composition and structure the upper 0 to 0.45 m of soil. The 1 M HNO3 extractant
and that exist under different climatic conditions. used in this study was unable to extract 100% of bio-
Percent recovery of biosolids-applied Cd, Cu, Ni, Pb, solid-applied Cr.
and Zn was close to 100% for all biosolids loadings The results of this study suggest that biosolids-applied
(Table 3). Chromium was the exception to this trend. organic matter decomposes slowly when applied to a
Biosolids-applied Cr exhibited the same distribution in well-drained silt loam soil in a temperate climate. Con-
the soil profile as the other heavy metals (Fig. 3), but sequently, rapid release of biosolids-derived heavy met-
percent recoveries ranged from 52 to 59%. Low recov- als followed by leaching and plant uptake is unlikely to
ery of Cr was probably due to incomplete extraction by occur. Complete recovery of biosolids-applied heavy
1M HNO3. During an earlier study, soils from a different metals is possible when plot size is large enough to
location at the 1-9 site were extracted for 16 h with hot prevent cross-mixing of treated soils during tillage oper-
4 M HNO3 (Sloan et al, 1997). The amounts of Cr ations and when sediment losses due to erosion are
extracted from those soil samples with hot 4 M HNO3 minimal. The long-term immobility of biosolids-applied
(data not shown) were four to nine times greater than heavy metals in this soil suggests that the risk of ground-
the amounts extracted with 1 M HNO3 from soils in the water contamination is minimal in a well-drained, silt
present study. A comparison of DTPA vs. 1 M HNO3 loam agricultural soil.
extractable Cr also provides evidence of the chemical
resistance of soil Cr. For the soils used in the present
study, concentrations of DTPA-extractable Cd, Cu, Ni,
Pb, and Zn (data not shown) were 69, 37, 37, 30, and
46% of 1 M HNO3 values, respectively. In contrast,
DTPA-extractable Cr was <1% of 1 M HNO3 values.
Kelling et al. (1977) also found that DTPA was able to
extract Cd, Cu, Ni, and Zn, but not Cr from a biosolids-
treated soil.
CONCLUSIONS
Soils were sampled with depth 16 yr after three annual
biosolids applications. Soil OC concentrations in the
soil surface were linearly correlated to biosolids loadings
and were not significantly different from the levels mea-
sured 1 yr after the final biosolids application. Biosolids-
applied Cd, Cr, Cu, Ni, Pb, and Zn were concentrated
primarily in the upper 0.30 m of soil with smaller
SLOAN ET AL.: RECOVERY OF BIOSOLIDS-APPLIED HEAVY METALS 1317