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COMMUNICATIONS IN SOIL SCIENCE AND PLANT ANALYSIS


Vol. 34, Nos. 3 & 4, pp. 547557, 2003

Baseline Concentration of Heavy Metals in Brazilian


Latosols
M. L. Campos, M. A. P. Pierangeli, L. R. G. Guilherme,
J. J. Marques,* and N. Curi
Departamento de Ciencia do Solo, Universidade Federal de Lavras,
Lavras, Brazil

ABSTRACT
Knowledge of baseline concentrations for heavy metals of environmental
and agricultural concern in tropical soils is meager. Latosols are highly
weathered soils that cover ,40% of the Brazilian territory and are by far
the most important agricultural soil order in Brazil. This paper aimed to
compare two methods for heavy metal extraction from soils, and to
provide baseline values of heavy metals for Brazilian Latosols. The soil
samples came from the 0 0.2-m layer of 19 different Latosols from the
various geographic regions of Brazil. The first experiment compared the
USEPA method 3051A (microwave digestion with concentrated HNO3 in
closed vessels) with the aqua regia extraction (hot plate digestion with
concentrated HCl and HNO3, 3:1, in open vessels) regarding Pb
determination. The second analyzed contents of Cd, Cu, Ni, Pb, and Zn,
and for this the USEPA method 3051A was used. Heavy metal contents
were assessed by flame atomic absorption spectroscopy. Although both
*Correspondence: J. J. Marques, Departamento de Ciencia do Solo, Universidade
Federal de Lavras, 37200-000 Lavras-MG, Brazil; E-mail: jmarques@ufla.br.
547
DOI: 10.1081/CSS-120017838
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Campos et al.
methods were highly correlated, the USEPA-3051A rendered Pb contents
29% higher in average than the aqua regia. Average n 57 and
standard deviation values for heavy metals in Brazilian Latosols are
0:66 ^ 0:19 mg Cd kg21 ; 65 ^ 74 mg Cu kg21 ; 18 ^ 12 mg Ni kg21 ;
22 ^ 9 mg Pb kg21 ; and 39 ^ 24 mg Zn kg21 : Considerably variation is
due to the inclusion of Latosols derived from a variety of parent materials.
The values provided could be useful as reference baseline concentrations
for heavy metals in Brazilian Latosols.
Key Words:

Trace elements; Oxisols; Natural concentrations.

INTRODUCTION
Monitoring likely pollution sources is part of the task of maintaining the
agricultural and ecological functions of the soils. Studies have found many
soils around the world are contaminated with Pb, Cd, Hg, and others.[1]
Abnormally high concentrations of heavy metals in soils are caused by
atmospheric deposition and applications of agrochemicals, fertilizers, and
residues to soils. Such applications onto soils are becoming widespread not
only in developed but also in developing countries.[2 4]
The first step of a soil pollution-monitoring program is to establish
background concentrations of unpolluted, pristine soils. Unfortunately, it is
very difficult to assert a given soil is absolutely contaminant-free.[5] Virtually
all the Earth, at variable degrees, has been affected by human activities. Thus
it would be best to use the terms baseline concentrations rather than
background concentrations.[6] Baseline concentration is defined as the
content of a pollutant found in soils during a monitoring program, which will
be used as a reference value for future studies.[6]
Measuring the total content of heavy metals in soils is very useful in soil
genesis and geochemistry studies or even to assess the extent of
contamination. Total content, however, is not a good indicator of heavy
metal bioavailability. On the other hand, it is extremely difficult to choose an
extractor to reliably measure bioavailability. Most extractors, such as
Mehlich-1 (0.05 mol L21 HCl 0.0125 mol L21 H2SO4) and DTPA (Diethylenetrinitrilopentacetic Acid), were developed for measuring bioavailability in
cropland, where heavy metal contents are relatively low. Such extractors are
not suitable for situations wherein heavy metal contents may be in the order of
several hundreds mg kg21.[7] Aqua regia (HNO3 HCl, 1:3) is the
recommended extractor for heavy metal pollutants in European soils and
sludges,[8] whereas the USEPA methods 3050 and 3051A are widely used in

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Heavy Metals in Brazilian Latosols

549

the USA.[9 11] The aqua regia and the USEPA methods 3050 and 3051A,
called total-recoverable methods, are midterms between true total, or total
total, content methods (e.g., x-ray fluorescence, USEPA-3052) and
bioavailability methods.[8,9] The heavy metal contents extracted by such
methods represent the maximum amount of a given heavy metal that may
potentially be either bioavailable or transported to the groundwater under
worst case environmental conditions.[10]
Knowledge of baseline concentrations for heavy metals of environmental
and agricultural concern in tropical soils is lacking.[12] Latosols correspond to
well-drained Oxisols in the Soil Taxonomy.[13] These highly weathered soils
cover , 40% of the Brazilian territory and they are by far the most important
agricultural soil order in Brazil. This paper had two objectives: (i) to compare
a USEPA-recommended method for heavy metal extraction with the
traditional aqua regia extraction, and (ii) to provide baseline values of Cd
and Pb, which are serious pollutants, and Cu, Ni, and Zn, which are also plant
micronutrients, for 19 benchmark Brazilian Latosols.

MATERIALS AND METHODS


Two different experiments were made in this study. The first experiment
compared the USEPA method 3051A with the aqua regia extraction regarding
Pb determination and the second determined baseline contents of Cd, Cu, Ni,
Pb, and Zn for 19 benchmark Brazilian Latosols. The samples came from the
0 0.2-m layer of 19 Latosols from the various geographic regions of Brazil
(Table 1) and were sieved to , 2 mm. The sampling sites belong to a network
of soil erosion studies in Brazil and are used to study soil erosion
modeling.[15,16] A summary of the main physical, chemical, and mineralogical
properties of these soils is presented in Table 2.[18] Complete physical,
chemical, and mineralogical characterization of those soils can be found
elsewhere.[17 19]

Comparison of Methods USEPA-3051A and Aqua Regia


In this experiment, 17 out of the 19 soils listed in Table 1 were analyzed.
Soils 14 and 15 were not analyzed for this experiment. For both methods
described below, Pb was determined by conventional flame (air acetylene)
atomic absorption spectroscopy (FAAS) and all analyses were triplicated.
For method USEPA-3051A,[9 11] , 0,5 g aliquots of soil, ground to
, 0.15 mm, were placed in closed Teflone vessels with 10 mL of

Parent material

Location

Typic Dystrophic Red Latosol


Typic Dystrophic Red Latosol
Typic Dystroferric Red Latosol
Typic Dystroferric Red Latosol
Typic Eutroferric Red Latosol
Typic Dystrophic Red Latosol
Typic Dystroferric Red Latosol
Psammitic Dystrofic Red Latosol
Typic Dystroferric Red Latosol
Typic Dystroferric Red Latosol
Typic Dystroferric Red Latosol
Typic Dystroferric Red Latosol
Typic Dystroferric Red Latosol
Typic Dystroferric Red Latosol
Typic Dystrophic Red-Yellow Latosol
Typic Dystrophic Yellow Latosol
Typic Dystrophic Yellow Latosol
Typic Dystrophic Yellow Latosol
Typic Cohesive Yellow Latosol

Basalt
Basalt
Basalt
Basalt
Diabase
Basalt and sandstone
Clayey sediments
Sandstone
Basalt and sandstone
Gneiss
Clay and siltstones
Clayey sediments
Clayey sediments
Clay and siltstones
Clay and siltstones
Sandstone
Gneiss
Sandy and clayey sediments
Clayey sediments

Iju-RS
Chapeco-SC
Londrina-PR
Dourados-MS
Campinas-SP
Passo Fundo-RS
Ponta Grossa-PR
Paranava-PR
Jaboticabal-SP
Lavras-MG
Sete Lagoas-MG
Goiania-GO
Planaltina-DF
S. Joao Del Rei-MG
S. Joao Del Rei-MG
Ubajara-CE
Lavras-MG
Areia-PB
Tome Acu-PA

Campos et al.

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19

Classification

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Number

Classification[14] and location (town and state) of the studied Latosols.

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550

Table 1.

Clay
(g kg21)

Kaolinite
(g kg21)

Gibbsite
(g kg 2 1)

Hematite
(g kg21)

Goethite
(g kg21)

Organic C
(g kg21)

CEC pH 7
(mmolc kg21)

170
60
60
240
300
470
290
860
660
180
120
360
370
270
170
800
170
550
600

670
790
860
650
600
470
630
139
339
720
850
540
520
691
711
150
720
440
40

421
526
420
402
312
254
344
103
171
190
491
19
360
350
480
69
305
420
327

58
61
225
112
180
95
172
11
141
484
254
448
75
510
375
69
374
0
0

107
71
122
79
61
89
58
9
15
19
73
45
29
26
14
0
0
0
0

10
4
11
11
34
6
42
2
3
16
14
26
17
129
145
10
22
3
6

15
26
8
8
15
18
13
5
17
19
22
17
24
19
16
15
28
25
9

148
158
104
117
86
181
79
41
66
60
41
74
145
68
47
88
64
110
88

551

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1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19

Sand
(g kg21)

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Soil number

Selected physical, chemical, and mineralogical properties of 19 benchmark Brazilian Latosols.[17 19]

Heavy Metals in Brazilian Latosols

Table 2.

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552

Campos et al.

concentrated HNO3. The simplest version of method 3051A, which is


performed without HCl, was used. The vessels were heated to 1758C in a
microwave. It took # 5.5 minutes for the microwave to reach the target
temperature, which remained as such for 4.5 minutes. As the microwave did
not have a temperature sensor, only a pressure sensor, published pressure
temperature data[10,11] was used as indication of which pressure to reach. After
digestion, the contents of each vessel were filtered (Whatman #42) and the
volume made up to 20 mL.
The aqua regia extraction was made according to Ure.[8] About 3 g of fine
earth (, 2 mm), ground to , 0.15 mm, was weighed into an open
Erlenmeyer, adding 2 mL of distilled water and 28 mL of aqua regia solution
(conc. HNO3 conc. HCl at the proportion 1:3). After moderate boiling for
two hours, the mixture in the Erlenmeyer was filtered and washed with 15 mL
of 0.5 mol L21 HNO3. The volume was then made up to 100 mL.

Baseline Contents of Cd, Cu, Ni, Pb, and Zn


For the determination of the baseline contents of Cd, Cu, Ni, Pb, and Zn,
the USEPA method 3051A described previously was used. All 19 Latosols
were analyzed. The contents of Cd, Cu, Ni, Pb, and Zn were determined by
FAAS and all analyses were triplicated.

RESULTS AND DISCUSSION


Comparison of Methods USEPA-3051A and Aqua Regia
Lead content in Brazilian Latosols extracted by the method USEPA3051A ranged from 10 to 49 mg kg21 (Fig. 1). The average value was
23 mg kg21 and the median was at 22 mg kg21. The aqua regia method
rendered contents ranging from 6 to 31 mg kg21, with average and median at
the same value of 18 mg Pb kg21. Although both methods were highly
correlated, the USEPA-3051A had Pb contents 29% higher in average than the
aqua regia (Fig. 1). Link et al.[10] and Chen and Ma[9] compared microwaveand hot plate-digestion methods. They also concluded microwave-based
methods have higher recovery rates. The most likely reasons for such better
result are due to higher temperatures achieved in closed vessels and the
minimal losses due to volatilization during heating. Additionally, microwavebased digestion methods are safer and do not release nearly as many fumes in
the environment as hot plate methods. Microwave methods are, however,

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Heavy Metals in Brazilian Latosols

553

Figure 1. Lead concentrations measured by methods USEPA-3051A and aqua regia


in Brazilian Latosols.

quicker than hot plate methods only when one has few samples to digest. The
small number of samples per microwave run, typically 10 15, greatly limits
lab operations when one has to digest tens of samples per day. A single hot
plate, on the other hand, can heat a much larger number of samples at a time,
80 in our lab. Price is other factor to consider in comparing both methods for
hot plates cost only a fraction of a microwave.
The soil samples were weighed after the digestions and it was found out
their weights had decreased by 30 40%. The solid residues remaining from
the method USEPA-3051A were x-rayed. Although the method preferentially dissolved the finer fractions, it was not able to dissolve all the clay
minerals. Peaks of kaolinite, an ubiquitous clay mineral very abundant in the
studied Latosols, was clearly visible in the x-ray patterns (data not shown).

Baseline Contents of Cd, Cu, Ni, Pb, and Zn


In a recent review about Oxisols of the world, based on limited
information then available in the international literature, it was pointed out
that Brazilian Latosols had heavy metal contents above the world average.[20]

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554

Campos et al.

Average n 57 and standard deviation values for the 19 benchmark


Brazilian Latosols are 0:66 ^ 0:19 mg Cd kg21 ; 65 ^ 74 mg Cu kg21 ; 18 ^
12 mg Ni kg21 ; 22 ^ 9 mg Pb kg21 ; and 39 ^ 24 mg Zn kg21 : Considering
these average values, only Cd and Cu are above world soils average contents,
which are 0.5 mg Cd kg21, 30 mg Cu kg21, 50 mg Ni kg21, 35 mg Pb kg21, and
90 mg Zn kg21.[21] Based on the data now available, one can safely say heavy
metals in Brazilian Latosols are not much different from the average values for
world soils. Buol and Eswaran[20] based their statement on data from Ker,[22]
which happened to analyze mostly soils derived from mafic rocks. Soils
formed from mafic rocks, basalt, gabbro, and others, are known to have higher
heavy metal contents than those ones derived from other rock types.[22 25]
Although their proportion is higher in southern Brazil, where most of the
Brazilian agriculture is located, soils derived from mafic rocks cover , 5% of
Brazils territory.
A trace element survey in 45 soils, mostly Latosols, from the central
area of Brazil, the so-called Cerrado region, has been recently made.[25] That
study found average values of 33 ^ 55 mg Cu kg21 ; 14 ^ 13 mg Ni kg21 ;
10 ^ 6 mg Pb kg21 ; and 38 ^ 54 mg Zn kg21 : Although a technique,
wavelength dispersive x-ray fluorescence, that renders the true total contents
of trace elements in soils has been used,[25] the values obtained in that study
are slightly lower than the ones reported here. The most likely reason is the
inclusion of a greater number of mafic rock-derived Latosols in this study, 7
(soils number 1 6 and 9) out of 19. Comparing the values from this study
(Table 3) with those from Marques[25] and taking into account the parent
material, one sees the values are not much different, indicating good
accuracy. Additionally, the standard deviation values obtained in the present
analyses are relatively low, indicating good precision. Average coefficients
of variation were 23% for Cd, 16% for Cu and Zn, 31% for Ni, and 14% for
Pb, which are not high considering the low concentrations found in these
uncontaminated soils.
Ten of the studied samples had Cd contents above the world average.[21]
However, all samples are , 1 mg Cd kg21, which is the threshold for Cd
contamination in soils.[23] One should notice, however, that Cd was right at the
detection limit of the technique used (FAAS).
It has been postulated that the influence of parent material on soil properties
is long-lasting.[24] It is undeniable that mafic-rock derived soils, even when
highly leached and weathered, have higher contents of heavy metals.[22 25]
However, at the lower end of heavy metals contents in soils, the relation
between parent material and heavy metal content is not so straightforward.
Intense weathering after literally millions of years has leveled off the trace
element contents in such soils. Under intense weathering, only very persistent

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Heavy Metals in Brazilian Latosols

555

Table 3. Contents of Cd, Cu, Ni, Pb, and Zn in benchmark Brazilian Latosols
(mean ^ standard deviation, n 3).
Soil number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19

Cd
(mg kg21)

Cu
(mg kg21)

Ni
(mg kg21)

Pb
(mg kg21)

Zn
(mg kg21)

0.87 ^ 0.06
0.39 ^ 0.32
0.92 ^ 0.02
0.84 ^ 0.14
0.85 ^ 0.14
0.48 ^ 0.08
1.01 ^ 0.03
0.39 ^ 0.14
0.72 ^ 0.23
0.68 ^ 0.10
0.57 ^ 0.14
0.72 ^ 0.16
0.54 ^ 0.14
0.73 ^ 0.23
0.47 ^ 0.17
0.37 ^ 0.09
0.83 ^ 0.17
0.43 ^ 0.07
0.66 ^ 0.12

200 ^ 42
50 ^ 11
238 ^ 61
227 ^ 57
140 ^ 19
40 ^ 7
52 ^ 7
23 ^ 7
17 ^ 2
51 ^ 3
25 ^ 1
43 ^ 6
13 ^ 2
33 ^ 8
37 ^ 1
5^1
16 ^ 0
8^1
3^1

27 ^ 15
9^4
40 ^ 23
45 ^ 19
36 ^ 11
9^4
22 ^ 6
3^1
9^3
17 ^ 1
20 ^ 3
22 ^ 9
14 ^ 2
12 ^ 3
13 ^ 1
10 ^ 3
11 ^ 1
10 ^ 3
5^2

28 ^ 1
27 ^ 8
24 ^ 2
25 ^ 5
26 ^ 1
22 ^ 4
37 ^ 2
17 ^ 2
24 ^ 4
21 ^ 2
49 ^ 2
20 ^ 2
18 ^ 1
13 ^ 4
13 ^ 1
16 ^ 5
17 ^ 1
17 ^ 4
10 ^ 2

96 ^ 18
47 ^ 12
91 ^ 17
79 ^ 15
41 ^ 6
47 ^ 17
49 ^ 5
20 ^ 2
28 ^ 5
23 ^ 2
36 ^ 3
35 ^ 4
25 ^ 3
17 ^ 5
21 ^ 2
24 ^ 5
12 ^ 0
26 ^ 4
12 ^ 2

elements in soils, like Zr and Th, may still keep a relation with their original
contents in the parent material. Soil number 8, for instance is the only soil in the
sampling set derived from sandstone, a rock typically poor in heavy metals.
Nevertheless, it is not the soil that has the lowest amounts of heavy metals
(Table 3).

CONCLUSIONS
The method USEPA-3051A provides equivalent results to the aqua regia
extraction for heavy metals in Brazilian Latosols and may be advantageously
used in several situations. Direct comparison between both methods, however,
must be cautiously done, as USEPA-3051A tends to produce higher values.
Data provided in this paper could be used as reference baseline concentrations
for heavy metals in Brazilian Latosols.

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Campos et al.

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Heavy Metals in Brazilian Latosols

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14.

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