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Bioresource Technology 96 (2005) 10291038

Evaluation of sewage sludge, septic waste and sludge


compost applications to corn and forage: Ca, Mg, S, Fe, Mn, Cu,
Zn and B content of crops and soils
P.R. Warman
a

a,b,*

, W.C. Termeer

Coastal BioAgresearch Ltd., 268 Boutiliers Pt Rd, Boutiliers Pt, Canada NS B3Z 1V1
b
Nova Scotia Agricultural College, P.O. Box 550, Truro, N.S., Canada B2N 5E3

Received 5 January 2004; received in revised form 14 September 2004; accepted 19 September 2004

Abstract
This is the second of two papers presenting the data from an experiment on the application of aerobically-digested sewage sludge
(AES), anaerobic lagoon septic wastes (ANS), sewage sludge compost and fertilizer to soils for grass forage and feed corn production at two dierent sites in Nova Scotia. Crop yields, plant tissue and Mehlich-1 extractable soil nutrients were evaluated; 15 elements were analyzed in the plant tissue and 9 elements in the soil extracts. This paper describes the Ca, Mg, S, Fe, Mn, Cu, Zn and B
content of the crops and the Mehlich-1 extractable content of the soils.
The response to the amendments was not consistent at the two sites with the two dierent crops. We found that the septic sludge
(ANS) produced the highest forage Fe, Cu and Zn levels and was equal to compost in elevating corn stover and forage S and the
forage B content. The compost produced the highest forage Ca and corn Zn, the AES produced the highest corn Mn, and fertilizer
produced the highest forage Mn. None of the amendments produced excessive levels of the above nutrients; rather, the amendments
improved the feed quality of the forage and corn stover. Lastly, it was noted that the Mehlich-1 extract only had a signicantly
positive correlation with forage Cu content.
 2004 Elsevier Ltd. All rights reserved.
Keywords: Biosolids; Compost; Corn; Grass forage; Mehlich-1 extract; Sewage sludge

1. Introduction
Land application of sewage sludge (biosolids) has
been a worldwide agricultural practice for many years.
It eectively disposes of a waste product while recycling
valuable nutrients into the soilplant ecosystem; however, too often the dispersal has created environmental
problems that force government agencies to restrict the
amount and type of sewage sludge which can be land*
Corresponding author. Address: Coastal BioAgresearch Ltd., 268
Boutiliers Pt Rd, Boutiliers Pt, Canada NS B3Z 1V1. Fax: +1 902 826
2804.
E-mail address: [email protected] (P.R. Warman).

0960-8524/$ - see front matter  2004 Elsevier Ltd. All rights reserved.
doi:10.1016/j.biortech.2004.09.014

applied. Various processes are employed to reduce any


potential negative eect of sewage sludge application;
composting wastes to stabilize the components is one
process now used more frequently.
The production of corn and grass forage using sewage sludge has been well-documented. Most of the studies have evaluated crop yield, N, P, and K content or
uptake (reviewed in Warman and Termeer, in press),
or heavy metal concentration in crops or uptake from
soils, often following very high rates of biosolids application. Two of the three other macronutrients (specically Ca and Mg) have been assessed in grass forage
amended with sewage sludge (Soon et al., 1978; Tiany
et al., 2000a; Warman, 1986; Zebarth et al., 2000),

1030

P.R. Warman, W.C. Termeer / Bioresource Technology 96 (2005) 10291038

however, there has been little evaluation of S, the sixth


macronutrient, or B, a micronutrient frequently decient in Podzolic soils.
Boron, Fe, Mn, Cu, Zn, Mo and Cl are plant essential micronutrients that are present in sewage sludge
and sewage sludge compost, yet some of these elements
can also be toxic to plants and animals when applied in
excessive amounts. Many researchers have studied the
eects of applied sewage sludge on the levels of Cu
and/or Zn in corn (Bidwell and Dowdy, 1987; Cajuste
et al., 2000; Cripps et al., 1992; Hinesly et al., 1984;
Logan et al., 1997; Rappaport et al., 1988; Reddy
et al., 1989). Along with Cu and Zn, other workers have
also evaluated Mn (Cunningham et al., 1975; Kiemnec
et al., 1990; Lutrick et al., 1982; Ramachandran and
DSouza, 1998), and Mn and Fe (Hernandez et al.,
1991; Juste and Solda, 1985). Fewer studies have looked
at the eect of sewage sludge on grass forage, those evaluating Cu and Zn include MacLean et al. (1987), while
Soon et al. (1980), Warman (1986) and McBride and
Evans (2002) also reported on Mn, and Tiany et al.
(2000b) and Zebarth et al. (2000) also evaluated Fe
and Mn. Investigations of plant Cu and Zn following
sludge compost applications are relatively recent (Sims,
1990; Pichtel and Anderson, 1997; Warman et al., 1995;
Warman and Termeer, 1996; Wen et al., 1999), with
fewer studies involving corn (Cajuste et al., 2000) or forage compared to other crops.
The application of sewage sludge to agricultural land
usually increases the Cu and Zn concentrations of
amended plants and normally the Zn content increases
more substantially than the Cu content. The factors that
aect the bioavailability of an element include soil pH,
plant species and their cultivars, growth stage, biosolid
source, soil conditions and the chemistry of the element.
The NRC (1980) has set the domestic animal mineral
tolerance level for Cu at 100 mg Cu/kg feed (except for
sheep, which is set at 25 mg Cu/kg feed) and for Zn at
300 mg Zn/kg feed (except for Japanese quail, which is
set at 125 mg Zn/kg feed). Based on a review of the literature, Chang et al. (1992) described a methodology for
establishing phytotoxicity criteria for Cr, Cu, Ni and
Zn from agricultural land application of municipal sewage sludges; they found that the Cu concentration in
corn did not rise above the 25 mg Cu/kg feed quality
limit even when 1500 kg Cu/ha was applied. However,
the Zn content in corn leaf tissue can exceed the
300 mg/kg limit if high amounts of Zn are applied by sewage sludge (Hinesly et al., 1984; Lutrick et al., 1982).
Chang et al. (1992) recommended that up to 3500 kg Zn
could be applied per hectare without adverse eects on
plant growth; however, there has been strong criticism
of these recommendations by Schmidt (1997) and others.
Several researchers have shown that the Cu and Zn
applied in sewage sludge remained in the plow layer of
the soil and does not leach downward (Cripps et al.,

1992; Kiemnec et al., 1990; Rappaport et al., 1988).


Therefore, large applications of sewage sludge will
increase total soil Cu and Zn, but not necessarily the
plant available portion. Researchers have used various
multi-element extractants such as DPTA, 0.01 M CaCl2,
Mehlich-1, Mehlich-3, and 0.1 N HCl to estimate plant
available nutrients and other metals in soils with varying
degrees of success. Soil extraction is useful if it can consistently and accurately predict plant uptake of elements
from soil since extraction and analysis is frequently
more rapid than plant tissue digestion. None of the
above extractants, however, has been found to predict
the availability of every element for every dierent crop
and soil.
The study objectives were the comparison of sewage
sludge or septic wastes, and sewage sludge compost to
NPK fertilizer application to two soils and two crops.
Few eld studies compare dierent types of sludges with
compost produced from one of the sludges, and few
studies compare organic amendments (only) with synthetically fertilized crops. The results of the Ca, Mg, S,
Fe, Mn, B, Cu and Zn content of the crops and Mehlich-1 extractable analysis of the soils are included in this
manuscript; a companion paper by Warman and Termeer (in press) documents the yield, N, P and K content
of the two crops and Mehlich-1 extractable P and K.

2. Methods
Two sources of sewage wastes, aerobically-digested
sewage sludge (AES) and anaerobic lagoon septic waste
(ANS), a sewage sludge compost and commercial fertilizer were evaluated for two consecutive years in the
same eld plots. The experiment used two crops (grass
forage [30% P. pratensis L.30% F. elatior L.40% D.
glomerata L.] and feed corn [Zea mays L.]) permitted
by the Nova Scotia Department of Environment and
Labour (NSDEL) for growth on land where sewage
sludge is applied. The aerobic sludge was used to grow
corn in an Acadia silt loam soil; the plots were
10.8 m2. Surface applications were made in the spring
and incorporated within 24 h, a full week prior to planting. The anaerobic septic sludge was used to grow the
grass forage in a Queens silt loam; the plots were
6.0 m2. Surface applications were made twice a year,
once in the spring as the grass started to grow (May)
and again after the rst cut was harvested (July). Sewage
sludge compost was produced in windrows using AES
and horse racetrack bedding as feedstocks (detailed in
Warman and Termeer, 1996). Each amendment was applied at half, full (180 kg N/ha for grass, 150 kg N/ha for
corn), and one and a half times the recommended N
application rate for each crop. The N, P, and K contents
of the organic amendments are shown in Table 1; the
contents of the other plant essential nutrients are found

P.R. Warman, W.C. Termeer / Bioresource Technology 96 (2005) 10291038


Table 1
N, P, and K content (mg/g) of the compost and sewage sludges applied
to the crops
Crop

Year

Compost
N

Grass

1994
1995

Corn

1994
1995

a
b
c

Sewage sludge
P

N
a

12.2
(0.04)b
29.4
(0.05)

5.4
(0.21)
14.1
(2.18)

7.3
(0.40)
16.9
(2.27)

32.5
(0.00)
35.1a
(1.77)

8.7
(0.15)
10.8
(0.51)

2.5
(0.15)
2.7
(0.36)

12.2
(0.04)
29.4
(0.05)

5.4
(0.21)
14.1
(2.18)

7.3
(0.40)
16.9
(2.27)

53.7c
(0.12)
40.0c
(0.05)

16.9
(0.22)
15.6
(0.51)

5.7
(0.05)
4.6
(0.17)

Anaerobic septic sludge (ANS).


Standard error.
Aerobically-digested sludge (AES).

in Table 2. Application rates for the organic amendments assumed 50% of the total N applied was available
to the crop in the year of application. Therefore, the
mean rate of application was 30.6 dry t/ha compost
and 10.7 dry t/ha of ANS to the forage and 25.7 dry t/
ha compost and 6.5 dry t/ha AES to the corn. Synthetic
fertilizer (NPK) was applied according to the Nova
Scotia Department of Agriculture and Fisheries Soil
Test Recommendations. Thus, the mean rate of application was 180 kg N/ha, 110 kg P2O5/ha and 180 kg K2O/
ha to the forage and 150 kg N/ha, 115 kg P2O5/ha and
55 kg K2O/ha to the corn. The experiment also included
a control that received no amendments. The higher elemental analysis of the compost the second year (Table 1)
was due to the higher ratio of sewage sludge used to

1031

make the compost (23 times as high). Each treatment


was replicated four times in a Randomized Complete
Block design.
Corn yields (stover and grain) were taken by hand at
maturity and grass forage yields were taken in early
summer (cut #1) and late summer (cut #2) using a
gas-powered cutting bar. Plant tissue samples were
taken at each harvest and dried at 60 C and ground
to <1 mm. Tissue N was determined by digestion in
H2SO4H2O2. Digests were distilled with 10 M NaOH
into boric acid and quantitatively titrated with HCl. Tissue (as well as sewage wastes and compost) P and K
were determined using a nitric acid digestion procedure
and determined using inductively coupled plasma emission spectrometry (ICP) (Jarrell-Ash 9000 Plasma Spectrometer). At the end of the two years, soil samples were
taken to a depth of 20 cm and extracted for all elements,
except N and S, using the Mehlich-1 double acid procedure (0.05 N HCl0.025 N H2SO4). Tissue (as well as
sewage wastes and compost) P and K were determined
using a nitric acid digestion procedure and determined
using inductively coupled plasma emission spectrometry
(ICP). At the end of the two years, soil samples were
taken to a depth of 20 cm and extracted for all elements,
except N and S, using the Mehlich-1 double acid procedure (0.05 N HCl0.025 N H2SO4). The soil pH of a 1:1
soil:deionized water paste was determined using a glass
electrode.
To determine the eciency of nutrient recovery of the
applied amendments, percent recovery of a nutrient was
determined as follows:

Table 2
Mean elemental analysis (standard error) of the compost and sewage sludges applied to the crops
Crop

Year

Ca (g/kg)

Mg (g/kg)

S (g/kg)

Fe (g/kg)

Mn (g/kg)

Zn (g/kg)

B (mg/kg)

Cu (mg/kg)

Compost
Grass

1994

19.6
(1.00)
25.5
(9.20)

4.2
(0.80)
8.1
(2.29)

7.0
(0.07)
10.0
(3.15)

5.3
(0.40)
18.3
(0.15)

0.39
(0.02)
1.07
(0.14)

0.15
(0.02)
0.29
(0.04)

8.3
(2.00)
26.4
(5.55)

69
(2.0)
229
(4.5)

19.6
(1.00)
25.5
(9.20)

4.2
(0.80)
8.1
(2.29)

7.0
(0.07)
10.0
(3.15)

5.3
(0.40)
18.3
(0.15)

0.39
(0.02)
1.07
(0.14)

0.15
(0.02)
0.29
(0.04)

8.3
(2.00)
26.4
(5.55)

69
(2.0)
229
(4.5)

27.6
(0.34)
20.9
(1.97)

3.0
(0.56)
3.1
(0.25)

9.7
(0.08)
13.0
(1.16)

16.4
(0.46)
15.3
(1.16)

0.45
(0.01)
0.42
(0.04)

1.45
(0.02)
1.34
(0.10)

3.4
(1.92)
25.0
(2.93)

827
(3.1)
853
(58.5)

16.1
(0.30)
5.4
(1.23)

5.7
(0.14)
5.3
(0.45)

4.3
(0.05)
3.7
(0.06)

27.1
(0.05)
23.8
(0.35)

0.81
(0.01)
3.15
(0.08)

0.49
(0.01)
0.39
(0.02)

8.4
(2.80)
5.3
(2.56)

326
(8.5)
316
(6.0)

1995
Corn

1994
1995

Sewage sludge
Grassa
1994
1995
Cornb

1994
1995

a
b

Anaerobic septic sludge (ANS).


Aerobically-digested sludge (AES).

1032

P.R. Warman, W.C. Termeer / Bioresource Technology 96 (2005) 10291038

%Recovery

treatment uptake  control uptake


total amount of nutrient applied

Statistical analysis was performed using Super


ANOVA on a Macintosh computer. Because of the unequal sample size, two sets of comparisons were made;
one test compared the three treatments to each other,
while another test compared the treatments to the control. Comparisons between means were made using linear contrasts and Tukeys multiple range test at p 6 0.05.
For simplicity, the data for all the nine application rates
is not included in this paper; data for the three rates/
treatment are averaged and the means are presented
for nutrient content of the forage and corn stover. However, the nutrient content of the corn grain is from the
high rate treatments only.

3. Results and discussion


3.1. Plant Ca, soil pH and Mehlich-1 extractable Ca
Application of sludge compost and (to a lesser extent)
ANS septic sludge to the forage plots increased the tissue Ca concentration compared to fertilizer and at times
the control plots (Table 3). This response was not surprising since the compost supplied Ca equivalent to 1
2 t/yr of calcitic limestone. The compost and AES
sludge, however, had a small eect on the tissue Ca content of the corn stover or grain.
The consistent increase in forage tissue Ca, up to
10.65 mg/g for cut #2 in 1995, should be considered
when this forage is fed to domestic animals. The NRC
(1980) recommends a Ca:P ratio of 1.52:1 for feed rations and a total dietary calcium of less than 1%
(10 mg/g). The second cut forage tissue from the compost plots in 1995 exceeded both recommended limits;

however, since feed rations consist of dierent components, dietary P could be easily increased to the recommended level. In general, all the amendments improved
the feed quality of the forage and corn compared with
the control, which always produced forage with a Ca:P
ratio greater than 2.1.
None of the amendments changed the soil pH at
either site, which averaged 5.6 at the forage site and
6.2 at the corn site (data not shown). This result was
interesting because neutral composts (the sludge compost had a pH of 7) would be expected to increase soil
pH, even with nitrication of the composts ammonium,
while ammonium-containing fertilizers normally reduce
soil pH.
The compost and sludge increased the Mehlich-1
extractable Ca content of the forage plots but only the
compost increased Mehlich-1 Ca in the corn plots (Table
3). The high initial soil Ca levels likely provided sucient available Ca for the corn crop and masked the
eect of the Ca applied by the compost and AES.
3.2. Plant Mg and Mehlich-1 extractable Mg
Applications of ANS, AES and compost to the grass
forage and corn had little eect on tissue Mg concentrations (Table 4). In 1995, tissue Mg levels in the ANS and
compost-amended forage were higher than the fertilized
samples, but not the control for rst cut samples. For
the second cut, the ANS-amended forage had the highest Mg content of the treated plots, though not higher
than the control. The AES and fertilizer-amended corn
analyzed higher in tissue Mg than the compost and
control plots for the 1994 stover, only. Both sludges
and fertilizer produced higher Mg uptake (yield tissue
content) compared to the compost-amended crops for
the two years.

Table 3
Mean calcium content of grass forage and corn tissue (mg/g) and Mehlich-1 extractable soil Ca (mg/kg)a
Crop

Year

Component

Compost (n = 12)

Sludge (n = 12)

Fertilizer (n = 12)

Zero (n = 4)

Grass

1994

Cut
Cut
Cut
Cut

2.89a
5.69c
6.77c
10.65b

2.99ba
4.67cb
5.35 b
7.70ab

3.22a
3.28a
3.31a
4.96a

2.62
5.62
4.53
8.88

Mehlich-1 Ca

1672c

941ab

722a

618

Stover
Graine
Stover
Graine

1.36a
0.023a
1.62a
0.037a

1.46da
0.023a
1.84b
0.045ab

1.39a
0.024a
1.66a
0.049b

1.40
0.030
1.54
0.047

Mehlich-1 Ca

1649b

1427a

1428a

1520

1995

Corn

1994
1995

a
b
c
d
e

#1
#2
#1
#2

Means with dierent letters in a row are signicantly dierent (p < 0.05).
Anaerobic septic sludge (ANS).
Underlined numbers are signicantly dierent than the zero control.
Aerobically-digested sludge (AES).
Data from the high rate treatment only.

P.R. Warman, W.C. Termeer / Bioresource Technology 96 (2005) 10291038

1033

Table 4
Mean magnesium content of grass forage and corn tissue and Mehlich-1 extractable soil Mg (mg/g)a
Crop
Grass

Year
1994
1995

Corn

1994
1995

a
b
c
d
e

Component
Cut
Cut
Cut
Cut

#1
#2
#1
#2

Compost (n = 12)

Sludge (n = 12)
b

Fertilizer (n = 12)

Zero (n = 4)

1.76a
2.29ca
2.32b
3.11a

1.66 a
2.40a
2.15b
4.38b

1.98b
2.27a
1.89a
3.09a

1.80
3.01
2.29
4.38

Mehlich-1 Mg

205b

153a

141a

143

Stover
Graine
Stover
Graine

1.70a
1.16a
2.04a
1.30a

1.94db
1.09a
2.11a
1.33a

1.87b
1.09a
2.07a
1.30a

1.81
1.08
2.02
1.33

Mehlich-1 Mg

623a

604a

581a

636

Means with dierent letters in a row are signicantly dierent (p < 0.05).
Anaerobic septic sludge (ANS).
Underlined numbers are signicantly dierent than the zero control.
Aerobically-digested sludge (AES).
Data from the high rate treatment only.

Mehlich-1 extractable soil Mg was increased by the


application of sludge compost to the forage plots, but
not by any fertility applications to the corn plots (Table
4). This result was likely due to the high native soil test
rating for Mg that masked the eects of the treatments
to the corn. Based upon the poor relationship between
Mehlich-1 and tissue or Mg uptake (negative or non-signicant correlation coecient), the Mehlich-1 extract
would not be the extract of choice to estimate plant
available Mg.

The higher tissue S content in the ANS and compostamended plots may have been caused by a concentration
factor (plants with lower dry matter yields often have
higher elemental analysis). Even though the fertilizer
produced more forage dry matter (Warman and Termeer, in press), S uptake by the fertilizer and ANSamended grass was the same, which indicates the septic
sludge contributed more S to the rhizosphere than the
fertilizer.
3.4. Plant Fe and Mehlich-1 extractable Fe

3.3. Plant S
The grass forage and corn stover S concentrations
were higher in the compost and ANS-amended plots
than in the synthetic fertilizer plots (except for cut #1
forage in 1994), and one or both the ANS and compost-amended plots often had higher tissue S content
than the control plots (Table 5). Treatment dierences
were greater in the forage plots than in the corn plots.

Although AES and the compost made from it have a


high concentration of iron (Table 2) and considerable
amounts of Fe were applied by the organic amendments
to the forage and corn plots, only the ANS had much of
an eect on tissue Fe concentrations (Table 6). Tissue Fe
levels had high replicate variability in the late summer of
1995 where numerically large dierences between treatments were found in cut #2 forage and corn stover

Table 5
Mean sulfur content of grass forage and corn tissue (mg/g)a
Crop

Year

Component

Compost (n = 12)

Sludge (n = 12)

Fertilizer (n = 12)

Zero (n = 4)

Grass

1994

Cut #1
Cut #2
Cut #1
Cut #2
Stover
Graine
Stover
Graine

1.00ba
2.05c
1.69ab
3.03b
0.72b
0.95a
1.09c
1.29a

1.01ca
1.68b
1.73b
3.64c
0.69db
0.99a
0.94b
1.25a

1.00a
0.98a
1.56a
1.93a
0.61a
0.94a
0.87a
1.25a

0.78
1.88
1.40
3.15
0.61
0.98
0.99
1.38

1995
Corn

1994
1995

a
b
c
d
e

Means with dierent letters in a row are signicantly dierent (p < 0.05).
Underlined numbers are signicantly dierent than the zero control.
Anaerobic septic sludge (ANS).
Aerobically-digested sludge (AES).
Data from the high rate treatment only.

1034

P.R. Warman, W.C. Termeer / Bioresource Technology 96 (2005) 10291038

Table 6
Mean iron content of grass forage and corn tissue (mg/kg) and Mehlich-1 extractable soil Fe (mg/kg)a
Crop
Grass

Year
1994
1995

Corn

1994
1995

a
b
c
d
e

Component
Cut
Cut
Cut
Cut

#1
#2
#1
#2

Compost (n = 12)

Sludge (n = 12)
b

Fertilizer (n = 12)

Zero (n = 4)

26.3a
63.5a
39.4a
96.0a

66.2 b
89.0cb
64.9b
180.7a

31.8a
50.8a
38.6a
60.4a

22.8
59.1
49.4
144.3

Mehlich-1 Fe

22.3a

24.8ab

27.2b

33.5

Stover
Graine
Stover
Graine

33.0a
26.1a
69.1a
42.0a

54.2db
25.5a
86.9a
39.0a

53.0b
24.0a
109.2a
27.0a

53.3
24.7
115.2
27.0

Mehlich-1 Fe

17.3a

21.2ab

22.4b

18.6

Means with dierent letters in a row are signicantly dierent (p < 0.05).
Underlined numbers are signicantly dierent than the zero control.
Anaerobic septic sludge (ANS).
Aerobically-digested sludge (AES).
Data from the high rate treatment only.

and grain. It has been suggested that the forage might


have been contaminated by dust or sludge particles adsorbed to the forage and not removed with the distilled
water wash prior to drying and analysis.
The Fe in the organic amendments had little eect on
Mehlich-1 soil Fe; at both sites, the synthetic fertilizer
plots had the highest extractable Fe. The amended forage soils had less extractable Fe than the control, while
the extractable Fe content of the amended corn soils was
statistically equivalent to the control.
3.5. Plant Mn and Mehlich-1 extractable Mn
The Mn applied in the ANS and compost treatments
had little eect on the Mn content of the grass forage
(Table 7) although the Mn content of the amendments

was quite substantial (Table 2). The synthetically fertilized forage had the highest Mn concentration in the
four cuts of forage; this result is often found in experiments where neutral organic amendments are compared
with ammonium-based fertilizers in acid soils. The fertilizers tend to decrease soil pH and subsequently increase
Mn concentrations in plant tissue. Although the amendments did not reduce the soils pH, the authors believe
that plant Mn is a more sensitive indicator of H+ production than soil pH measurements in naturally acidic
soils.
The application of AES to the corn plots resulted in
higher tissue Mn compared to synthetic fertilizer or
compost applications. Since Mn availability is strongly
aected by the soil oxidation-reduction potential, the response may be the combined eect of high Mn content

Table 7
Mean manganese content of grass forage and corn tissue (mg/kg) and Mehlich-1 extractable soil Mn (mg/kg)a
Crop

Year

Component

Compost (n = 12)

Sludge (n = 12)

Fertilizer (n = 12)

Zero (n = 4)

Grass

1994

Cut
Cut
Cut
Cut

98a
127a
102a
106a

94ca
154ab
110a
109a

119bb
171b
148b
185b

83
116
112
150

Mehlich-1 Mn

80b

71a

71a

76

Stover
Graine
Stover
Graine

19.1a
4.1a
20.9a
4.8a

25.4db
4.2a
29.9b
5.5a

22.2a
4.1a
24.9ab
4.7a

18.5
3.8
18.2
5.6

Mehlich-1 Mn

38a

35a

34a

30

1995

Corn

1994
1995

a
b
c
d
e

#1
#2
#1
#2

Means with dierent letters in a row are signicantly dierent (p < 0.05).
Underlined numbers are signicantly dierent than the zero control.
Anaerobic septic sludge (ANS).
Aerobically-digested sludge (AES).
Data from the high rate treatment only.

P.R. Warman, W.C. Termeer / Bioresource Technology 96 (2005) 10291038

in the AES (especially in 1995) and low oxygen conditions in the sewage sludge clods which lowered the soil
redox potential, causing an increase in stover Mn.
Mehlich-1 Mn was twice as high in the forage soil site
(pH 5.6) compared to the corn soil site (pH 6.2) (Table
7). However, Mehlich-1 extractable Mn was not a good
indicator of plant available Mn because there was poor
correlation between plant Mn or uptake and extractable
Mn (data not shown).
3.6. Plant B and Mehlich-1 extractable B
Sludges and sludge compost have relatively low contents of boron (Table 2); therefore, only small amounts
of B were applied by the organic amendments to the
grass forage and corn plots (on average less than
0.6 kg B/ha). However, the boron applied by ANS and
compost, especially, signicantly increased the forage
B content after the second application (Table 8), and signicantly increased Mehlich-1 soil B in these plots relative to the fertilizer and control. The B applied to the
corn plots by the AES and compost, however, had less
eect on B levels in corn tissue, where soil B levels were
considered adequate for the corn crop; the AES increased the B levels in the corn stover in both years.
The Mehlich-1 extract was not signicantly correlated
with tissue B content or calculated B uptake by either
crop.
3.7. Plant Cu and Mehlich-1 extractable Cu
The ANS used in 1995 had a copper content of
848 mg Cu/kg, which was the highest copper content
of all the amendments (Table 2). Septic sludge applications provided 13.7 kg Cu/ha for the two years, well
below the NSDEL guideline of 150 kg/ha; however, this

1035

application still increased the grass forage Cu concentration (Table 9). The sludge compost applied in 1995 had a
copper content of 238 mg Cu/kg, but the applications
did not increase the Cu concentrations in either the grass
forage or corn tissue. The Cu content of the AESamended corn stover was signicantly greater than the
compost and fertilizer-amended corn in 1994, but was
not signicantly dierent in 1995, possibly due to high
replicate variability.
The minimum recommended Cu concentration for
cattle rations is 9 mg Cu/kg (NRC, 1980); thus, initially,
the forage and corn were Cu decient for animal feed.
Although the NRC tolerance limits for tissue Cu were
never exceeded, continual septic sludge applications to
the forage plots might increase the Cu content beyond
the 25 mg Cu/kg tolerance limit for sheep. However, a
review of the literature suggests this is not likely to happen given that the rates of sludge applications are normally based upon the amendments N or P content.
For example. Soon et al. (1980) reported small increases
in the Cu content of bromegrass and corn grain following ve years of sewage sludge applications of as high as
31 kg Cu/ha, while Kiemnec et al. (1990) recorded only
modest increases in sweet corn leaf and grain Cu content
after seven years of sewage sludge applications of as
high as 62 kg Cu/ha to a silt loam soil.
Mehlich-1 extractable Cu increased in the AES and
ANS-amended plots, but only in the compost-amended
forage relative to the synthetic fertilizer plots (Table 9).
Mehlich-1 Cu was highly correlated with forage tissue
Cu (r = 0.98) but not corn Cu uptake. Calculated plant
uptake of Cu indicated the % recovery in forage or corn
tissue, although less than 1% of applied Cu, was higher
in the sludge compared to the compost-amended plots
(data not shown). This suggests that Cu availability is
higher from sewage sludge than from sludge compost.

Table 8
Mean boron content of grass forage and corn tissue (mg/kg) and Mehlich-1extractable soil B (mg/kg)a
Crop

Year

Component

Compost (n = 12)

Sludge (n = 12)

Fertilizer (n = 12)

Zero (n = 4)

Grass

1994

Cut
Cut
Cut
Cut

#1
#2
#1
#2

4.3a
7.1c
9.5c
8.6c

4.4ca
5.3b
5.9b
6.8b

4.3a
3.5ba
3.2a
3.9a

3.8
6.2
6.1
9.4

Mehlich-1 B

0.42c

0.31b

0.27a

0.24

Stover
Graine
Stover
Graine

5.7ab
1.8a
5.0a
2.4a

6.0db
1.7a
6.0b
2.4a

5.4a
1.9a
5.3a
2.7a

5.8
1.7
5.5
2.6

Mehlich-1 B

0.85b

0.77a

0.80ab

0.80

1995

Corn

1994
1995

a
b
c
d
e

Means with dierent letters in a row are signicantly dierent (p < 0.05).
Underlined numbers are signicantly dierent than the zero control.
Anaerobic septic sludge (ANS).
Aerobically-digested sludge (AES).
Data from the high rate treatment only.

1036

P.R. Warman, W.C. Termeer / Bioresource Technology 96 (2005) 10291038

Table 9
Mean copper content of grass forage and corn tissue (mg/kg) and Mehlich-1 extractable soil Cu (mg/kg)a
Crop
Grass

Year
1994
1995

Corn

1994
1995

a
b
c
d
e

Component
Cut
Cut
Cut
Cut

#1
#2
#1
#2

Compost (n = 12)

Sludge (n = 12)
b

Fertilizer (n = 12)

Zero (n = 4)

3.68a
4.58a
8.96a
10.48a

6.00 c
7.13cb
11.38a
17.69b

4.58b
4.89a
10.38a
7.39a

4.24
6.98
9.18
8.70

Mehlich-1 Cu

0.42b

1.86c

0.21a

0.38

Stover
Graine
Stover
Graine

7.22a
1.62a
12.0a
5.34a

8.90db
1.53a
12.8a
6.13a

7.90a
1.61a
11.8a
5.07a

8.70
1.70
11.7
8.77

Mehlich-1 Cu

0.36a

0.62b

0.41a

0.43

Means with dierent letters in a row are signicantly dierent (p < 0.05).
Underlined numbers are signicantly dierent than the zero control.
Anaerobic septic sludge (ANS).
Aerobically-digested sludge (AES).
Data from the high rate treatment only.

3.8. Plant Zn and Mehlich-1 extractable Zn


Applications of both ANS and compost increased
zinc concentrations in the grass forage tissue (Table
10), but the increase was greater from the ANS, which
is related to its total Zn content (Table 2). Nonetheless,
total Zn applications by ANS to the forage plots for the
two years were well below the NSDEL guideline of
330 kg/ha. The Zn content of the corn stover and grain,
however, was highest in the compost-amended plots,
although the Zn concentration of the compost was below the 500 mg/kg limit for Class I unrestricted compost
as proposed by the CCME (1996) compost standards.
None of the amendments produced tissue Zn levels
above the NRC tolerance limit of 300 mg Zn/kg feed.
Since the minimum recommended Zn content in cattle

rations average 35 mg /kg, and the data in Table 10 show


that most of the crop samples were below that amount,
the addition of ANS, AES or compost appeared to improve the feed quality of both the crops. Although the
longer term studies of Soon et al. (1980) and Kiemnec
et al. (1990) indicated relatively small increases in corn
Zn content, very high Zn applications in sewage sludge
can increase tissue Zn above 300 mg Zn/kg feed.
The % recovery of applied Zn determined that less
than 1% was recovered in the plant, but a relatively large
portion was extractable with Mehlich-1 solution (from
33% to 66% of the applied Zn); however, the correlation
coecients for extractable Zn and Zn uptake were not
signicant. Furthermore, calculations of Zn recovered
in plant tissue indicate the availability of Zn from compost and sludge applications were similar.

Table 10
Mean zinc content of grass forage and corn tissue (mg/kg) and Mehlich-1 extractable soil Zn (mg/kg)a
Crop

Year

Component

Compost (n = 12)

Sludge (n = 12)

Fertilizer (n = 12)

Zero (n = 4)

Grass

1994

Cut
Cut
Cut
Cut

11.7a
6.9a
21.6b
25.8b

18.0bb
23.4cb
31.9c
52.3c

15.2ab
7.4a
16.0a
15.3a

11.4
4.4
12.4
18.1

Mehlich-1 Zn

5.5b

10.6c

1.1a

1.0

Stover
Graine
Stover
Graine

15.6b
18.4a
21.6b
22.8a

13.5dab
17.2a
17.7a
21.0a

11.8a
17.4a
15.9a
21.7a

14.8
18.1
18.7
na

Mehlich-1 Zn

3.8b

3.3ab

2.5a

1.9

1995

Corn

1994
1995

a
b
c
d
e

#1
#2
#1
#2

Means with dierent letters in a row are signicantly dierent (p < 0.05).
Underlined numbers are signicantly dierent than the zero control.
Anaerobic septic sludge (ANS).
Aerobically-digested sludge (AES).
Data from the high rate treatment only.

P.R. Warman, W.C. Termeer / Bioresource Technology 96 (2005) 10291038

4. Conclusions
The response to the amendments was not consistent
at the two sites with the two dierent crops. We found
that the septic sludge (ANS) produced the highest forage
Fe (possibly due to contamination), Cu and Zn levels
and was equal to compost in its benet to plant S and
the forage B content. The compost produced the highest
forage Ca and corn Zn, the AES produced the highest
corn Mn, and fertilizer produced the highest forage
Mn. Lastly, it was noted that the Mehlich-1 extract only
correlated well with forage tissue Cu.
As conrmed by other researchers, it is important to
monitor the Cu and Zn content of plant tissue after a
few years of sewage sludge applications to ensure that
crops will not exceed the tolerance levels for animal feed
or human food. It would be useful to test/develop a soil
extractant which would accurately predict plant metal
uptake from soils with a history of sludge application
in order to ascertain whether additional sludge could
be applied to land without increasing plant metal concentrations beyond safe limits.

Acknowledgement
The authors acknowledge the nancial support of the
Canada/Nova Scotia Cooperation Agreement on Sustainable Economic Development, and the support of
A. Baird of Bairds Septic Tank Pumping Ltd and A.
Forbes of Marshwind Farms.

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