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land degradation & development

Land Degrad. Develop. 20: 145–155 (2009)

Published online 23 December 2008 in Wiley InterScience (www.interscience.wiley.com) DOI: 10.1002/ldr.888

IMPACT OF LIGNITE WASHERY SLUDGE ON MINE SOIL QUALITY AND


POPLAR TREES GROWTH
Ž. S. DŽELETOVIĆ*, R. M. FILIPOVIĆ, D. DJ. STOJANOVIĆ AND M. M. LAZAREVIĆ
Institute for the Application of Nuclear Energy, PO Box 46, 11080 Zemun, Serbia

Received 20 June 2008; Revised 15 October 2008; Accepted 17 October 2008

ABSTRACT
This paper outlines research on the use of lignite washery sludge as the amendment for reclamation of lignite mine soil and
stimulating poplar trees growth. Sludge is characterized by high total C content (34%) and high C/N ratio (68:1). The sludge
was introduced by ploughing in, down to 20–25 cm depth, in the quantities: 0, 28, 56 and 112 t ha1. We have established that the
N percentage in poplar leaves decreases with introducing increasing quantities of sludge into the mine soil. On the other hand,
the content of B and Cd increased with increasing sludge quantities. The As content in poplar leaves did not correlate with the
applied quantities of sludge, but it did with the P, Fe and Zn content in the leaves. Introducing this sludge can have a positive
effect on annual tree trunk increment, but only in the subsequent phases of growth. In the first few years an increase of total C
content by introducing lignite washery sludge is not sufficient to provide the conditions for faster growth of trees. Copyright #
2008 John Wiley & Sons, Ltd.

key words: reclamation of mine soil; lignite; poplar tree; nitrogen; arsenic

INTRODUCTION
Surface mining is an anthropogenic activity that changes the antecedent soil profile, as well as physical, chemical
and biological properties. The whole layer of soil covering an ore, in mining terms, represents barren soil, which is
removed with powerful machines and deposited at longer or shorter distance from the mining site. Soil disturbance
caused by mining leads to (Shukla et al., 2004) loss of aggregation, decline in soil organic carbon concentration,
loss of soil structure, increased bulk density and reduced porosity. Such soils have markedly low productive
capacity for plant growing, due to lack of nutrients, absence of humus, microbiological activity and influence of
fauna.
Reclamation of disturbed soils is done with the primary objective of restoring the land for agronomic or forest
land use. One of the most important issues for restoration of functional ecosystems in post-mining landscapes is
soil, in which accumulation of organic C in surface layers of the soil material is of crucial importance (Jochimsen,
1996; Bradshaw, 1997). Understanding how to amend mine soils in order to facilitate vegetation recovery
represents an important scientific application.
Soil formation and organic C accumulation in post-mining landscapes depends on the development of vegetation
cover and mineralization of plant debris. Plant growth and mineralization are apparently limited by N and P
deficiencies (Lindemann et al., 1989; Vimmerstedt et al., 1989). Incorporating organic amendments into
reconstructed strip mine soil may provide an alternative to topsoil replacement (Olsen and Jones, 1989). The
addition of organic material to the soil increases fertility and stimulates microbial activity, promotes N
transformation and nutrient cycling and accelerates ecosystem recovery (Coyne et al., 1998). Moreover, organic C
is an energy source for soil biota, which induces decomposition and mineralization of plant residues, thereby

* Correspondence to: Ž. S. Dželetović, Institute for the Application of Nuclear Energy, POB 46, 11080 Zemun, Serbia.
E-mail: zdzeletovic@hotmail.com

Copyright # 2008 John Wiley & Sons, Ltd.


146 Ž. S. DŽELETOVIĆ ET AL.

releasing nutrients. Accumulation of organic C results in changes of physical and chemical properties of the mine
soil, such as water retention and sorption capacities, nutrient content and availability, soil bulk density, buffering
capacity, etc. (Herrick and Wander, 1998). Organic upgrading mediums retain applied nutrients with slight losses,
primarily rinsing losses (Mercuri et al., 2006). The nature of applied upgrading mediums and their concentration
have an impact on heavy metal accumulation, their mobility and storing capacity in plant tissues (Riesen and Feller,
2005).
The utilization of typical, N rich sewage sludge from the purification plants has been most often presented in
scientific and professional literature. Lignite is seldom used as soil amendment, mainly for two reasons. First,
lignite particles often contain a lot of pyrite, causing a strong acidification (Baumann et al., 2006). Second, lignite
particles most often contain only limited organic substances for decomposition and nutrient supply (Rumpel and
Kögel-Knabner, 2004). The results obtained by Fettweis et al. (2005) indicate that the organic carbon, deriving
from lignite and lignite derivatives, can partly compensate the deficiency of soil organic matter in the mine soil.
However, microorganisms can decompose lignite particles only to a certain degree during a longer time period. The
degradation of sludge organic matter is considered to be a significant factor in the release of heavy metals in sludge-
amended soils. Properties of sludge play a critical role in determining the initial release and subsequent availability
of heavy metals in amended soils (Merrington et al., 2003). In time, it has been thought that the sludge properties
would have progressively less impact on metal behaviour and that soil characteristics ultimately control specific
features of metal, irrespective of its peculiarities in the original sludge (Smith, 1996). The time frame over which
this occurs is thought to vary greatly, from less than 12 weeks to over 8 years. The factors that govern this temporal
change have not yet been identified.
Our research aims at establishing the effect of lignite washery sludge on poplar tree plantations (Populus x
euramericana [Dode] Guinier, Cl. I-214) for the purpose of forest biological reclamation of mine soils of lignite
open pit in the mining basin ‘Kolubara’ (Serbia, South-East Europe), during 14 years of sludge application. Sludge
is produced, as by-product, in huge quantities by precipitation of waste water, originating mostly from the facilities
for wet separation and drying of Kolubara lignite. In this study, we assume that the introduction of sludge will have
a positive effect on annual tree trunk increment (radial growth increment) of trees growing on the mine soil. The use
of poplar trees is considered in the context of phytostabilization on mine soils. In addition, the analysis of leaves
from trees should eliminate doubts about some heavy metal accumulation in undesired (high) concentrations by
introducing this sludge.

MATERIAL AND METHODS


Location of the Mining Basin and Basic Climatic-Meteorological Indicators
Lignite basin ‘Kolubara’ is about 50 km to the southwest of Belgrade (capital of Serbia) and covers an area of
approximately 600 km2. The existing four open pits belonging to the mining company ‘Kolubara’ make the latter
the largest lignite producer in Serbia and one of the largest in Europe. Mean annual temperature is 1108C. July is
the warmest month (2078C), and January the coldest (038C). Mean annual precipitation is 6852 mm.

Mine Soil
The properties of mine soil, used in our study, are presented in Tables I and II. Mine soil is characterized by weak
alkaline reaction and very low total C content, total and mineral N content, available P and B. The overall content of
analysed microelements and heavy metals (Table II) has been increased (Cd, Co, Cr, Ni, Zn), relative to usual
content level in agricultural soils (cited by Kabata-Pendias and Pendias, 1989).

Lignite Washery Sludge


The properties of sludge, used in our study, are presented in Tables I and II. It is characterized by neutral pH values,
very high total C content, high total N content, sufficient content of available B, Ca and Mg. Unfavourable
characteristics of the sludge are: low content of mineral N, available P and K; as well as an increased arsenic content

Copyright # 2008 John Wiley & Sons, Ltd. LAND DEGRADATION & DEVELOPMENT, 20: 145–155 (2009)
DOI: 10.1002/ldr
LIGNITE WASHERY SLUDGE 147

Table I. Properties of mine soil and lignite washery sludge (the ISSS particle size distribution has been used)
Properties Mine soil Coal washery sludge

Sand (>002 mm), % 437 474


Silt (0002–002 mm), % 239 342
Clay (<0002 mm), % 324 184
pHH2 O 760  015 685  095
pHKCl 644  007 638  095
Ctot (%) 031  013 3400  885
Ntot(%) 0044  0010 0502  0021
C/N (x:1) 71 677
Nmin(mg N kg1) 0–25 cm 22  4 70  45
25–50 cm 11  3
NO3–N (mg N kg1) 0–25 cm 52 25  15
25–50 cm 31
NH4–N (mg N kg1) 0–25 cm 17  3 45  21
25–50 cm 83
Contents of easily available (mg kg1):
P 101  34 183  127
K 162  28 69  40
Ca 4390  650 9450  1210
Mg 720  130 1450  240
B 014  008 452  078

Table II. Total contents (mg kg1) of trace elements and heavy metals in sludge and minesoil (average  SD)
Coal washery sludge Mine soil (treatments)

þ0 t sludge ha1 þ56 t sludge ha1 þ112 t sludge ha1

As 2160  970 028  012 061  049 089  055


Cd 020  008 032  017 026  007 027  009
Co 106  36 427  76 477  112 440  16
Cr 120  61 571  16 733  241 589  35
Cu 175  08 306  00 462  217 325  33
Mn 196  33 453  12 453  15 460  10
Ni 352  92 1262  21 1508  307 1329  36
Pb 91  30 157  43 130  42 113  18
Zn 307  89 1212  21 1360  186 1225  22
Fe (%) 165  002 173  005 177  005 172  002

(according Serbian regulations). As one of the possible solutions for overcoming the drawbacks of mine soils, as a
substrate for the growth and development of plants, it has recently been suggested to introduce this sludge
(Mihailović et al., 1991). The particles of ‘Kolubara’ lignite are not followed by pyrite, so that the application will
not cause acidification.

Experimental Settings
Due to high organic C content, we have assumed that the sludge can be a suitable material for improving the mine
soil quality. This should result in higher radial increment of trees growing on the mine soil. The experiment is set on
a relatively flat surface, on the inner deposit of the open mine site ‘Field D’. Field experiment has been carried out
with a plantation of hybrid poplars (Populus x euramericana [Dode] Guinier, Cl. I-214). At planting (March, 1990),
2–3 kg of peat, mixed with substrate, was placed into excavated pits. One-year old bare root seedlings were planted.
The distance between seedlings in a row is 4 m and between rows it is 4 m too.

Copyright # 2008 John Wiley & Sons, Ltd. LAND DEGRADATION & DEVELOPMENT, 20: 145–155 (2009)
DOI: 10.1002/ldr
148 Ž. S. DŽELETOVIĆ ET AL.

The beginning of the fourth growth season after planting (April, 1993) was chosen as a convenient time for
sludge introduction. The phase of considerably retarded growth and dying some tree seedlings usually occurs
between 5 and 10 years from planting. At the beginning of the fourth season the poplar roots have not been fully
developed, so that they would not be damaged considerably by sludge plow-in. The experiment was set at random in
a certain area. The sludge in the quantities of 0, 28, 56 and 112 t ha1 was spread evenly across a surface and then
plowed down to 20–25 cm depth. The zero treatment, without sludge introduction, was also plowed in. A single
experimental treatment comprises 30 trees in one row. Each experiment treatment has been repeated three times.
There were two rows of trees between two experimental treatments, there was no sludge spread on the area between
those two rows, that area was neither ploughed nor the trees from these two rows measured. The distance between
some repetitions was at least five rows of trees.

Field Surveying and Collecting Samples of Soil and Plant Material for Laboratory Analyses
Prior to the beginning of every growth season, in March, as from 1993 till 2001, at 1 m height, a tree perimeter was
measured, after which the diameter was calculated according to the expression

P

p
where D is tree diameter (mm); P is measured tree perimeter (mm); p ¼ 314.
After 2001, tree perimeter was measured in 2004 and 2007. By the end of October 1993 (at the end of the first
growth season after sludge introduction) leaves were collected from all poplar crown and branches, from 15–20 m
height, 1 sample at a time from each experimental treatment, on the areas where sludge was applied in the quantities
of 0, 56 and 112 t ha1, for lab analyses. Samples of leaves and barren soil were not collected from the areas treated
with applied sludge of 28 t ha1. Coal washery sludge is not a homogenous material, and for sludge analyses, we
took 9 samples in total from lagoons in which the sludge precipitated (total lagoon area is 10 ha). One sample at a
time was taken from surface layer (depth 0–30 cm) from areas under experimental treatment from which poplar
leaves were collected (9 samples of mine soil in total). Collecting sludge samples was carried out prior to
introduction into the mine soil and mine soil samples after the sludge plough-in. Sludge and mine soil samples were
air dried for 7 days at 20–258C and then screened through a steel sieve of 2 mm mesh size.

Laboratory Methods
pH in H2O and 1N KCl was determined for the ratio soil (sludge): solvent ratio 1:25. We determined the total
amount of organic C using the procedure described by Nikitin (1972): heating barren soil (sludge) samples with a
chromium-sulphuric mixture, followed by spectrophotometrical measurement of optical densities in Visible
spectrophotometer Ultro Spec 2000 (Pharmacia Biotech, UK). Total N content was determined by semi-micro
Kjeldahl digestion with Se, CuSO4 and K2SO4 as the catalysts (Bremner, 1996). Available phosphorus was
measured colorimetrically by ultraviolet/visible light spectrophotometer using the method of Olsen and Sommers
(1982). Available K was determined by flame photometry after extraction with mixture of 0.1 N ammonium
lactate þ 04 N acetic acid solutions. Exchangeable cations (Ca, Mg) were extracted with neutral 1 M ammonium
acetate (Thomas, 1982). After extraction with hot water, available B in the extracts was determined by the curcumin
procedure as modified by Mulford and Martens (1970).
N content in plant material was determined by the Kjeldahl’s method, and foliar P was analysed colorimetrically,
following nitric acid digestion. The content of K, Ca and Mg in solution was determined by flame photometry. The
B content of 500 mg sub-samples of the plant material, ashed for 3 h at 5508C, was determined by a modification of
the curcumin procedure (Mulford and Martens, 1970). Concentrations of Cu, Mn, Zn, Pb and Cd in plant material
were measured by the following procedure. Plant material was washed in de-ionized water, then dried to a constant
weight at 1058C, after which samples were digested with HNO3 at 1258C. After cooling down by 30% H2O2 was
added and digesting was continued until the digest was clear. After being cooled, the samples were diluted in pure
(distilled) water before measurement (Jones and Case, 1990). Metal concentrations were determined using an

Copyright # 2008 John Wiley & Sons, Ltd. LAND DEGRADATION & DEVELOPMENT, 20: 145–155 (2009)
DOI: 10.1002/ldr
LIGNITE WASHERY SLUDGE 149

atomic absorption spectrophotometer Pye Unicam SP-192. Arsenic content was determined by spectrophotometry
after hydrochloric acid digestion of powdered samples (Agget and Aspell, 1976).

Statistical Analysis
The data shown in Tables and figures are the arithmetic means of three replicates of each treatment, namely, of the
corresponding number of analysed sludge samples. Standard deviation value is stated with these data in the Tables.
For the relation between concentrations of some nutrients and heavy metals in different treatments of barren soil
with sludge and their concentrations in poplar leaves, we have used a correlation analysis. Student’s t-distribution
was used for significance levels. We carried out the testing of statistical differences between mean annual
increments of poplar trees by treatments and between cumulative increments of poplar trees by treatments through
regression analysis by means of Fisher-Snedecor’s F-distribution.

RESULTS
It is clear from the data of Table I that this sludge application will have an impact on total organic C content in the
mine soil. The C/N ratio in the sludge is very wide (68:1), and lower in mine soil than in natural soils and is (6–8):1
(Table I). By introducing increasing quantities of sludge in mine soil, the N percentage in leaves is in linear decrease
(Table III; r ¼ 1000; p001). Due to insufficient supply of available P both to mine soil and the sludge, the
P content in leaves is low (Table III) with all three treatments. In addition, the Ca/P ratio in poplar leaves, from land
lots fertilized with sludge, increased (167), relative to this ratio in poplar leaves on controlled land lots, without
sludge introduction (144). For this reason, the relative Ca content in the leaves of poplars fertilized with sludge is
considerably greater (>3%). Thus, the quantity of available Ca in the mine soil negatively correlates with the
quantity of P in poplar leaves (r ¼ 09867).
The concentrations of K, Mg Fe and B in poplar leaves (Table III) are within normal, reference concentration
ranges in plants, stated by Kabata-Pendias and Pendias (1989). By applying increasing quantities of sludge, the B
accumulation in poplar leaves increases (r ¼ 09984; p005), indirectly indicating a positive effect on plant supply
with available B.
The concentrations of heavy metals: Cu, Mn, Zn, Co, Ni, Cr Pb in all analysed plant material samples
(Table III) are within normal, reference plant concentration ranges, stated for these elements by Kabata-Pendias and
Pendias (1989). The Cd content in leaves increases with the application of increasing quantities of sludge
(r ¼ 09681), although the Cd content in the sludge is lower than in the mine soil (Table II).

Table III. Chemical content of poplar leaf growing on minesoil (average  SD)
Treatment: þ0 sludge ha1 þ56 t sludge ha1 þ112 t sludge ha1

N (%) 202  025 181  045 161  059


P (%) 014  001 018  003 017  002
K (%) 069  009 064  010 071  013
Ca (%) 202  028 301  030 311  011
Mg (%) 046  002 046  001 045  019
Fe (mg kg1) 220  44 255  89 234  44
B (mg kg1) 373  118 1010  490 1787  484
Cu (mg kg1) 826  203 1384  1156 764  176
Mn (mg kg1) 1046  255 918  317 1066  76
Zn (mg kg1) 624  136 782  07 709  132
Co (mg kg1) 93  21 87  27 99  01
Ni (mg kg1) 149  23 149  33 159  07
Cr (mg kg1) 45  13 60  18 45  14
Pb (mg kg1) 116  038 128  029 107  062
Cd (mg kg1) 044  008 065  039 073  031
As (mg kg1) 030  018 066  039 046  035

Copyright # 2008 John Wiley & Sons, Ltd. LAND DEGRADATION & DEVELOPMENT, 20: 145–155 (2009)
DOI: 10.1002/ldr
150 Ž. S. DŽELETOVIĆ ET AL.

Figure 1. Average of annual tree trunk increment of poplars in mine soil treated with lignite washery sludge.

The As content in poplar leaves (Table III) does not indicate correlativeness with the application of increasing
sludge quantities thereby creating increasing As content in the mine soil. However, the As content in the leaves
highly and significantly correlates with leaves content: P (r ¼ 09083), Fe (r ¼ 09987) Zn (r ¼ 09942), while the
correlativeness with total Fe and Zn contents in the mine soil, namely with available P content, is low (for Fe and Zn
contents: r ¼ 07963 r ¼ 09412, and for P r ¼ 08322). In the examined barren soil the As content is considerably
below the level that is considered toxic. By applying sludge on the barren soil there is a linear increase of As content
(Table II; r ¼ 09989; p  001).
The growth analyses show that the examined groups of trees respond in a similar way to climatic effects on
annual basis. The annual variability of climatic-meteorological conditions on poplar increment is clearly noticed in
Figure 1. Moreover, the increment intensity decreases in all treatments during the studied time period.
The results of the cumulative increment, presented in Figure 2, show a relatively minor sludge treatment impact.
The mean poplar tree trunk increment on land lots to which sludge was applied in the amount of 28 t ha1 after a
period of 14 years is lower relative to treatment without sludge application, by 75% (Table IV). By introducing

Figure 2. The cumulative tree trunk increment of poplars treated with lignite washery sludge.

Copyright # 2008 John Wiley & Sons, Ltd. LAND DEGRADATION & DEVELOPMENT, 20: 145–155 (2009)
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LIGNITE WASHERY SLUDGE 151

Table IV. Average of annual radial increment of poplars on mine soil (average  SD)
Years 1993–1997 1998–2000 2001–2006 Total tree trunk
increment

Treatment (t sludge ha1) mm y1 % mm y1 % mm y1 % mm %

0 2074  415 1000 1230  246 1000 737  147 1000 1848 1000
28 2008  402 968 1043  209 848 655  130 889 1710 925
56 1974  394 952 1431  286 1163 1074  214 1457 2061 1115
112 2156  431 1040 1150  230 935 845  168 1147 1930 1044

On compare of treatment without added sludge (100%)

56 t ha1, the mean annual radial increment of poplars is higher by 115%, and by introducing 112 t ha1 by 44%,
relative to treatment without sludge introduction.

DISCUSSION
Lignite particles, though relatively inert, seem that they are subject, to a certain degree, to mineralization processes.
Due to the presence of organic C, lignite is considered to be an appropriate means in the humization of lignite mine
soil (Lukina et al., 1990). Lignite use can have a positive effect on agricultural revitalization (Katzur et al., 2003).
Lignite can adsorb nutrients and water, but high pyrite and aluminium content may limit root access to them
(Baumann et al., 2006).
Plantation forest growing for commercial purposes, as a form of utilizing soil surface after ore excavation, is
usually limited by poor nutrient availability in the mine substrates (Mercuri et al., 2006). Deficiency of plant
available N is often a limiting factor in the revegetation and maintenance of disturbed lands, such as strip lignite
mine soils. Vimmerstedt et al. (1989) observe that a long time period is needed (more than 30 years) to increase
total N content in the surface horizon of afforested coal mine barren soils to the level of good N supply. Accretion of
C and N on mine soils will be influenced both by overburden strata, placed on the surface as parent material of the
new soil, and by tree species chosen for planting (Vimmerstedt et al., 1989). It has been established, during several
years of research, that the process of reclamation of lignite mine soil is progressing slower than desired (Veselinović
et al., 1990). Foliage chlorosis was observed on all species, but with different intensities. A mild chlorosis (with
weak intensity) has been established on: Alnus glutinosa, Pseudotsuga menziesii, Betula alba and Quercus rubra;
medium intensity chlorosis on: Acer pseudoplatanus, Betula verucosa, Fraxinus excelsior, Pinus nigra, Pinus
sylvestris, Larix europea, Quercus robur and Tilia tomentosa; while the highest intensity of chlorosis was noticed in
the trees of Pinus strobus L. (Veselinović and Golubović-Ćurguz, 2001).
Experiments on different lignite mine soils have shown that barren soil can supply N (Reeder and Sabey, 1987;
Lindemann et al., 1989). Mineralization of organic N is slower in mine soil than in natural soil (Reeder and Sabey,
1987), and vegetation growing on barren soils takes up less N and produces less biomass than the vegetation
growing on topsoil (Reeder, 1985). Other studies have inferred that slow mineralization of N in mine soils is caused
by low microbial populations, reduced enzymatic activities, narrow microbial diversity and poor N adsorption by
plants (Reeder and Sabey, 1987). It is clear from the data of Table III that N supply to the plants grown on mine soil
will not be improved by this sludge application.
P supply has not even been considerably improved by sludge application. Namely, high Ca and Mg contents is
probably the cause of sludge and barren soil deficiency even in easily available P, because Ca and Mg form hardly
soluble salts with phosphates. Visual deficiency symptoms are manifested in the mean P concentrations in poplar
leaves, being below 016% (van den Driessche, 2000). The P content in poplar leaves, in our experiment, is low:
018% for treatment with 56 t ha1 and 017% for treatment with 112 t ha 1, and for treatment without sludge
introduction it is in the range of values at which deficiency symptoms are manifested (014%).
The results of Ličina et al. (2007) indicate the problem of accumulation of some heavy metals in plants grown on the
lignite mine barren soils. Also, numerous investigations have documented heavy metal uptake by agricultural plant

Copyright # 2008 John Wiley & Sons, Ltd. LAND DEGRADATION & DEVELOPMENT, 20: 145–155 (2009)
DOI: 10.1002/ldr
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species grown in sludge-amended soil (Chaudri et al., 2001; McBride, 2003; Türkmen et al., 2004). Metal behaviour in
soils and plant uptake is difficult to generalize, because it is strongly dependent on the nature of the metal, sludge, soil
properties and crop (McBride, 2003). This results in the heterogeneity of limited values for overall contents of some
elements in the soil, depending on the purpose of their utilization (for agricultural purposes, ecosystems, as well as for
other purposes). However, in mine soils it is usual that the overall contents of some elements exceed specific limited
values, what we can say for the examined mine soil too (Table II). The phytostabilization of mine soils should enable
the removal of pollutants from the environment or making them harmless.
Introducing organic matter (sludge) should, from its side, induce the phytostabilization of the examined mine
soil. Namely, soils with higher organic content show less pronounced response to metal input, although this
tendency is not always consistent (Khan and Scullion, 2000). The Cu, Zn, Ni and Cd ions are strongly bonded in all
soils except in sand soils and are uptaken by plants in greater quantities from sludge treated soils relative to those
that have not been treated. According to Chen et al. (1999), the major factors controlling trace metal concentrations
in soils are clay content, organic C content, pH, CEC and Fe, Al, Ca, Mg and P concentrations. The stated factors
are directly affected by sludge application to the mine soil, which results in the change of concentrations of some
elements in poplar leaves (Table III).
The heavy metal concentration in the plant tops is frequently a linear function of total metal concentration in the
soil (Chaudri et al., 2001; Nan et al., 2002). However, metal concentrations in leaves of metal-accumulating woody
species are not associated with total or labile concentrations in soil (Unterbrunner et al., 2007). In this way, Cd and
Zn are accumulated in poplar leaves from the soil on which they grow (Dos Santos Utmazian et al., 2007;
Unterbrunner et al., 2007), namely, Cd uptake by grown plants from sludge treated soils is usually much higher
compared to uptake from untreated soils, while it appears that phytotoxicity is rarely manifested.
Fast-growing tree species, such as the poplar, could be suitable for treating heavy metal-polluted soils (Dos
Santos Utmazian et al., 2007; Unterbrunner et al., 2007), due to which they are considered very suitable for
phytostabilization contaminated soil (Dos Santos Utmazian et al., 2007). The adaptive features of poplar clones to
various soil conditions is highly estimated (Orlović et al., 1997), and therefore, species belonging to the genus
Populus have been used successfully in forestrial recultivation of mine waste soils in Serbia (Šmit et al., 1996).
In soils formed on coal mine soils, As is considered to be potentially the most hazardous element (Kohel, 1995).
The As concentrations in non-contaminated soils seldom exceed 15 mg kg1, except for the soils derived from
weathered pyrites or quartzite (Smith et al., 1998). The uptake of As by plants from contaminated soils and its
inclusion in the nutrition chain, presents a health hazard. Especially important factors affecting natural background
concentrations of As in soils are total Fe and P quantities (Chen et al., 2002). Organic matter generally has a low
affinity for As.
The As content in poplar leaves (Table III) with treatment without sludge application (030 mg kg 1) is in the
range of usual levels of As content in uncontaminated plant tissues (035 mg kg1 of dry matter); (Kabata-Pendias
and Pendias, 1989). The As content in poplar leaves, treated with sludge, is increased (066 mg kg1 for treatment
with 56 t ha1 and 046 mg kg1 for treatment with 112 t ha1). Madejón and Lepp (2007) have established the As
content of 067–132 mg kg1 in poplar leaves, which appeared by spontaneous revegetation on soil surfaces
contaminated by As. Based on literature data, it can be expected that the As content in leaves adversely correlates
with P and Fe contents in the mine soil. It is evident that in this case, at very low concentrations of available P in the
mine barren soil and sludge and at neutral to alkaline reaction of soil, P and Fe do not hinder As uptake. Thereby, in
our study the As content in the poplar leaves adversely correlates with the content of available Ca in barren soil
(r ¼ 09642), and it also influences the availability of both P and Fe in barren soil.
In the analysis of poplar radial increment on the mine soil one can easily notice three periods that essentially
differ by their values of mean annual increments (Table IV). In the first period (phase I: from 1993 to 1997), the
poplar increment was dynamic and characterized by an inclined ascending line reaching peak values in the seventh
year of the plantation (>20 mm of tree trunk increment). After that, in the phase II (1998–2000) and the phase III
(2001–2006), the poplar increment was much slower.
The values obtained for the phase I radial increment are identical to the values reported by Vučković et al. (2005)
for poplars grown on humofluvisol, a soil considered optimal for growing poplars in Serbia. In this phase, namely,

Copyright # 2008 John Wiley & Sons, Ltd. LAND DEGRADATION & DEVELOPMENT, 20: 145–155 (2009)
DOI: 10.1002/ldr
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in the phase of intensive tree trunk increment, the rates of annual tree trunk increment, stability and good plantation
development on barren soil with N and P deficiency are relatively high. In contrast, Baumann et al. (2006)
established that the formed biomass of Pinus sylvestris and Pinus nigra, grown on the mine soil containing lignite,
was significantly lower.
It is known that Populus spp. typically have a high demand for nitrogen. The C addition to the soil normally leads
to net N immobilization or at least partly lower net N mineralization rates (Magill and Aber, 2000). High C/N ratio
in the sludge and increasing sludge quantities apparently cause, apart from reducing the relative N content in poplar
leaves, a minor reduction in average annual radial increment of the poplars.
In contrast to the values of radial increment in phase I, values obtained in phase II are considerably lower than
reference values for the poplar trees, stated by Vučković et al. (2005). The phenomena of tree dying on barren soils
of ‘Kolubara’ mine are mostly expressed in this phase (Popović and Veselinović, 1988; Šmit et al., 1996). Just in
this phase greater differences (>  5%) appear in the mean annual tree trunk increment. In the phase II of the tree
trunk increment, a marked decrease of increment intensity can be noticed, by 28–50% of the mean tree trunk
increment level in the phase I (Table IV). In the phase III this trend continues, so that tree trunk increments have
been lower compared to the phase II. However, in the phase III the decrease of the tree trunk increment is mostly
expressed in the treatment without sludge introduction (increment decrease by 40%). By introducing 56 t of
sludge ha1 the tree trunk increment decrease relative to the phase II is lower by 25%, and by introducing 112 t of
sludge ha1 by 27%. Briefly, for the entire observed period, from March, 1993 to March 2007 (Table IV), the
introduction of this sludge showed a positive impact on the tree trunk increment only when applying large sludge
quantities (56 and 112 t ha1). A minor sludge quantity (28 t ha1) has, briefly observed, an unfavourable impact on
poplar increment.
The explanation of such different results is problematic, which may lead to confusion, and common results
compared to other similar studies. In this study, sludge introduction results in an increment not being consistent
with similar results obtained elsewhere. In phases II and III of tree trunk increment, the mine soil features, such as
different physical and agrochemical properties, are probably more evident. Regarding biogenicity, ‘Kolubara’ mine
soils have shown less availability of the total microflora, fungi, Clostridium and nitrate bacteria, compared to the
soil of origin (pseudogley) (Rasulić et al., 2002).
By testing statistical differences between mean annual increments of poplar trees by treatments, through
regression analysis (Table V), regression coefficients were obtained, which are statistically very significant. A mean
annual increment for appropriate treatment by sludge introduction changes considerably with the change of mean
annual increment for the treatment without sludge introduction. For the differences between cumulative increments
of poplar trees by treatments, regression coefficients were also obtained, which are statistically very significant.

Table V. Testing of statistical differences between treatments, through regression analysis (n ¼ 10; predictors: results of tree
trunk increment by treatment of 0 t sludge ha1; dependent variable: results of tree trunk increment by treatment: 28, 56, and
112 t sludge ha1)
Parameters: Annual tree trunk increments of poplar Cumulative tree trunk increments of
trees by treatments poplar trees by treatments

28 t ha1 56 t ha1 112 t ha1 28 t ha1 56 t ha1 112 t ha1

Coefficients (Syi ¼ na þ bSx): a 0439 5134 3788 2415 10200 6392


b 0925 0737 0799 0932 1124 0998
Standard error of the estimate 2135 1575 2550 1912 6271 2257
Standard error Sa 1624 1198 1940 1305 4279 1540
Sb 0097 0072 0116 0012 0038 0013
t-test ta 0272 4285 1950 1862 2380 4168
tb 9509 10265 6875 81026 29886 73896
F-value 906 1054 472 66139 8942 57754

For level of significance 005: a ¼ 005 ! F(005, 1, 8) ¼ 532; 001: a ¼ 001 ! F(001, 1, 8) ¼ 1126

Copyright # 2008 John Wiley & Sons, Ltd. LAND DEGRADATION & DEVELOPMENT, 20: 145–155 (2009)
DOI: 10.1002/ldr
154 Ž. S. DŽELETOVIĆ ET AL.

The results of this research do not depend on weather conditions, and certain discrepancy of the results suggests
an unpredictable utilization of sludge with high C content. An increase of total C content in the lignite mine barren
soil by introducing lignite washery sludge is not sufficient to provide the conditions for faster tree increment. It is
hard to expect that simple introduction of C-reached material in unfertile medium can significantly improve plant
growth. Carbon is not nutrient usually supplied by soil or growth medium. Such materials can improve soil
chemical and physical properties, but great time sequence is needed for mine soil quality change.
Thereby, heavy metals (As, Cd, Co, Cr, Cu, Mn, Ni, Pb Zn) neither accumulate in toxic concentrations, by this
sludge introduction, nor in the mine soil and leaves of poplars growing on it. However, compared to other successful
research of sludge application with high C content for reclamation of barren mine soils (Olsen and Jones, 1989;
Coyne et al., 1998), this sludge with high lignite content as a potential C source does not represent an efficient
amendment. The results obtained by this research do not eliminate the results obtained formerly, concerning the
application of other species of waste sludge for reclamation of mine soils.

CONCLUSION
The data from this research on the use of lignite washery sludge to rehabilitate mine soil indicates that heavy metals
(As, Cd, Co, Cr, Cu, Mn, Ni, Pb Zn) are neither accumulated by this sludge application in toxic concentrations in
mine soil nor in poplar leaves growing on it. However, the results of this study show that sludge introduction was not
reflected in higher radial increment of trees growing on mine barren soil in the first few years after the application.
For this reason, we think that the sludge with high lignite content, as a potential C source, does not represent an
efficient amendment for reclamation of barren mine soils.

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