ABSTRACT

Ten representative soil samples were collected along major gutters within Nkpor
metropolis. The soil samples were digested using mixtures of HF and aqua regia
in ratio1:1. The heavy metals contents of the digested soil samples were
determined via Flame Atomic Absorption Spectrophotometer FAAS. Sample A
had the highest concentration of heavy metal and the trend was Ni > Cr > Hg >
Zn > As ~ Cd, it was followed by sample B with Ni > Cr > Zn > Zn > Cd >g >
As, sample C had Ni>Cr >Zn>Hg>Cd>As, sample E had Ni > Zn > Cd > Cr >
Hg > As. While sample D had Cr > Ni > Zn > Cd > Hg > As. Also the results of
the sequential extraction of each soil sample indicated that Ni had the highest
percentage bioavailability (49.61%), Hg (47. 72%), Cr (42. 19%), Zn (39.66%),
Cd (35.10%), As (0.00%). The high concentration of Hg, Cr and Cd in most areas
of the metropolis indicated gross contamination, which could have resulted from
human activities, hence the need to adequately monitor the release of these toxic
metals to the environment.

TABLE OF CONTENTS

Title Page………………………………………………………………….ii
Approval Page …………………………………………………………………iii
Dedication ………………………………………………………………..iv
Acknowledgement ……………………………………………………….v-vi
Abstract ……………………………………………………………….vii
List of Tables ……………………………………………………………viii
List of Figures ……………………………………………………………ix
Table of contents …………………………………………………………x-xi

CHAPTER ONE
1.0 General Introduction ………………………………1-2
1.1 Scope of study ………………………………………2
1.2 Aims & Objectives of study………….………………3
1.3 Literature Review ……………………………………4-5
1.3.1 Soil pollution ……………………………………. ……5
1.3.2 Soil Pollution and plant growth……………………….. 5
1.3.3 Soil Organism and biochemistry ………………………5
1.3.4 Soil Acidity …………………………………………..5-6
1.3.5 Heavy Metal Pollution …………………………………6
1.3.6 Heavy Metal Relationship to Living Organisms …….6-7
1.3.7 Reported Cases of Environmental Pollution………….7-8
xi 1.3.8 Effects of Cadmium on the Environment………………8
1.3.9 Effect of Antimony on the Environment……………….8-9
1.3.10 Effects of Copper on the Environment…………………9
1.3.11 Effects of Chromium on the Environment…………….9
1.3.12 Effects of Lead on the Environment ……………….9-10
1.3.13 Effects of Mercury on the Environment ………………10
1.3.14 Effects of Nickel on the Environment ………………..10
1.4 Solubility of Heavy Metals in soil …………………10-11
1.5 Phyto Availability of heavy metals in
residual-Treated soil..………………………………….11-12
1.6 Long term environment fate and Bioavailability
of Heavy metals in residual treated soil………………12
1.7 Solute interactions in relation to Bioavailability and
remediation of the Environment…………………..12-14
1.8 A Critical review of the Bioavailability and Impacts
of heavy metals in municipal soil waste Composts….14-15
1.9 Heavy Metals Transport in the soil profiles under
the application of sludge and wastewater ……………15-16

CHAPTER TWO
2.0 Reagents ………………………………………………………..17
2.1 Materials ………………………………………………………..17
xii 2.2 Instrument …………………………………………………….17
2.3 Sample collection and preparation …………………………17,19
2.4 Sequential Extraction …………………………………………..19
2.4.1 Preparation of reagents ……………………………………….19-20
2.5 Analytical procedures …………………………………………20-21
CHAPTER THREE
3.0 Result and Discussions …………………………….…22-41
3.1 Statistical Analysis of the Data …………………………..43
3.1.2 ANOVA (Analysis of Variance) ……………….…….43-44
2.1.3 Correlation of the Fractions. ……………………………..44
CHAPTER FOUR
4.0 Conclusion and Recommendation ………………………………..45
4.1 Conclusion…………………………………………………………45
4.2 Recommendations …………………………………………………45
References ……………………………………………………..46-50

CHAPTER ONE

INTRODUCTION
1.0 GENERAL INTRODUCTION
Minerals, metals and metalloids, toxic or essential, are present in soils or sediments in
various forms with varying bioavailability, toxicities and mobilities. Heavy metals are
natural components of the earth’s crust and the ecosystem with variations in
concentration. They cannot be degraded or destroyed and they enter our bodies via
food, drinking water and air [1].
Unlike organic contaminants, most metals do not undergo microbial or chemical
degradation and the total concentration of these metals in soils persist for a long time
after their introduction [2].
These metals are a cause of environmental pollution (heavy-metal pollution) from a
number of sources. For example lead in petrol, industrial effluents and leaching of
metal ions from the soil into lakes and rivers by acid rain [3].
Living organisms require varying amounts of “heavy metals”. Iron, cobalt, copper,
manganese, molybdenum and zinc are required by humans. Excessive levels can be
damaging to the organisms. Other heavy metals such as mercury, plutonium and lead
are toxic metals that have no beneficial effect on organisms and can cause serious
illnesses (3).
Therefore, with greater public awareness of the implications of contaminated soils on
humans and animal health, there has been increasing interest among scientific
communities in the development of technologies to determine the total concentrations
of these elements of interest in the soil as well as their chemical forms.

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The use of sequential extraction techniques to fractionate metals in soils and evaluate
their potential effects has become very useful and well recognized (4)
1.1 SCOPE OF STUDY
This research covers the analysis of six heavy metals in each of the five selected
drainage pathways or gutters in Nkpor. The heavy metals are mercury (Hg)
Nickel; (Ni), Zinc (Zn), Arsenic (As), Cadmium (Cd), Mercury (Hg)
Soil samples were collected from each of the drainage systems as follows:
Five soil samples each along Nkpor/Enugu Old Road, Nkpor/Obosi Road (site for
Geolis Cables Industry), Limca Road Nkpor, New Market Road Nkpor and
Nkpor/Enugu Express Road.
The samples will be collected at a distance of 10 meters each to avoid bias. A total of
25 soil samples will be analysed to determine the total concentration of each metal in
each sample.

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1.2 AIMS AND OBJECTIVES OF STUDY
Heavy metal content of soil sample in some selected drainage systems in Nkpor
will be investigated. As earlier on stated, heavy metals are dangerous because
they tend to bioaccumulate i.e increase in their concentration over time. Also
heavy metals can enter water supply by industrial and consumer waste or even
from acidic rain and release heavy metal into streams, lakes, rivers and ground
water.
Hence, the study will help in assessing the potential environmental impacts of
these metals by determination of their concentrations in soils as well as the
chemical form of these metals in the soil.
OBJECTIVES OF THIS STUDY
The objectives of this study are:
(a) To determine the total concentration of some selected heavy metals in gutter.
(b) To use sequential extraction technique to fractionate metals in soil samples.

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1.3 LITERATURE REVIEW
A heavy metal is a member of an ill defined subset of elements that exhibit metallic
properties, which would mainly include the transition metals, some metallic
lanthanides and actinides. Many different definitions have been proposed – some
based on density, some on atomic number or atomic weight and some on chemical
properties or toxicity [5]
Pollution is the release of substances which alter the environment and make it
unfavourable to man, animals and plants [6]. Water, air and soil stand the risk of being
polluted.
1.3:1 SOIL POLLUTION
Soil pollution is the introduction of undesirable materials such as solids, liquids or
even gases into the soil, which interfere with its sustenance of plant or animal life [7].
Soil particles may hold chemicals and nutrients making them available for plant roots
and keeping them from moving into lakes or streams or entering the ground water [8].
Metals from soils come from various sources. They may have been present in the
geologic rock, or they may occur as atmospheric additions of copper, mercury, lead
and zinc [9]. Metals also may have been deposited by past industrial activities, such
as; battery productions, brass and steel manufacturing industries, mining and many
different processes involving Nickel, Cadmium, Copper and Lead. Lead is especially
evident in the soil near roadways because of automobile emissions. [10]. Again as
lead paints and some soldered pipes used in houses wear and deteriorate they add lead
to nearby soils [11]. Other on-going sources of metals and organic waste materials in
the soil are landfills [12] and dump sites that are poorly maintained or unregulated

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[13]. Land fill materials eventually decompose and form a highly variable type of
unseen soil. Heavy metals remain in topsoil layer which is a result of chemical
reaction between heavy metals and organic matter [14].
1.3.2 SOIL POLLUTION AND PLANT GROWTH
Metal contamination on a site maybe evidenced by plant growth [15], animal
behaviour [16] or paint flasks containing lead from older building [17]. Many plants
simply cannot grow well where the level of certain metals is high. Other plants grow
well in contaminated soil but fail to set seed or do not grow as well as expected [15].
Absence of plant growth in a locality is a warning sign that a site may be severely
contaminated. Metals may be present at a site but with no risk for gardening or
recreation, depending on the soil properties, drainage and vegetation at the site.
1.3:3 SOIL ORGANISMS AND BIOCHEMISTRY
Soil is made up of mineral particles and organic matter [12] as well as the
decomposed remains of living things [18]. Bacterial fungi and other micro organisms
are largely responsible for breaking down dead plants and animals in the soil. Small
organisms (microbes) have negatively charged sites where soil nutrients and metals
can bond to form soil aggregates and compounds [19]. Earthworms and larger animals
eat and digest organic materials and minerals; transform them into soil aggregates and
deposit them as waste.
1.3:4 SOIL ACIDITY
An acid is a substance that has positive charge and usually yields hydrogen ions when
dissolved in water. The pH scale (1-14) is a common measure of soil reaction [12].
The lower the number, the greater the acidity. The midpoint of the pH scale is neutral

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(7.0) which is a good level for the growth of most plants. Changes in soil reaction, as
measured by pH, have significant effects on metals in soils. Metal toxicity to plants
and animals increases in strongly acid soils with low pH (3.5) [20]. Metals in these
soils are released from negative sites back into soil solution. At a higher pH (8.5), the
metals often are sequestered in the soil [21]. The term ‘sequestered’ indicates that the
positively charged metal ions are bound tightly to negatively charged sites in the soil
[22]. These sites may be on clays, mineral compounds, or organic matter, including
the surfaces of some microorganisms.
1.3:5 HEAVY METAL POLLUTION
These metals are a cause of environmental pollution from a number of sources
including lead in petrol, industrial effluents and leaching of metal ions from the soil
into lakes and rivers by acid rain [3].
Heavy metals occur naturally in the ecosystem with large variations in concentration.
Today, anthropogenic sources of heavy metals ie pollution, have been introduced into
the ecosystem. Wastes derived fuels are especially prone to contain heavy metals so
there should be a central concern in a consideration of their use.
Heavy metal pollution can arise from many sources but most commonly arises from
the purification of metals e.g. the smelting of copper and the preparation of nuclear
fuels. Electroplating is the primary source of chromium and cadmium. Through
precipitation of their compounds or by ion exchange into soils and mud.
1.3:6 HEAVY METAL RELATIONSHIP TO LIVING ORGANISMS
Some metals are necessary for humans in minute amounts (cobalt, copper, chromium,
Nickel etc). Some of them are dangerous to health or to the environment even at low

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concentration (mercury, cadmium, arsenic, lead, chromium etc). Some are harmful in
other ways e.g. Arsenic may pollute catalysts, whilst others are carcinogenic or toxic
thereby affecting, among others, the central nervous system (mercury, lead, Arsenic),
the kidneys or liver (Mercury, lead cadmium, copper) or skin, bones or teeth ( Nickel,
cadmium, copper, chromium) [23]. Certain elements are normally toxic to some
organisms while others may be beneficial e.g. Vanadium, tungsten and cadmium [24].
In medical circle, heavy metals are loosely defined [24] and include all toxic metals
irrespective of their atomic weights. Heavy metal poisoning can occur when excessive
amounts of Iron, Manganese, Aluminum or Beryllium (the fourth lightest element) or
such as semi metal as Arsenic are present in the environment. Early farmers in the
New Zealand suffered from bush sickness which was later discovered to be a
deficiency in cobalt [ 24 ]
1.3:7 REPORTED CASES OF ENVIRONMENTAL POLLUTION
In 1932, sewage containing mercury was released by Chisso’s Chemical works into
Minamata Bay in Japan. The mercury accumulated in sea creatures, leading
eventually to mercury poisoning in the population.
Again, Denis L. Feron and others used a secret discharge pipe to deliberately pump
hundreds of tons of heavy metal wastes into the Mississippi River from 1986 to 1996.
Feron is now an international fugitive and one of the Environmental Protection
Agency’s most wanted man because of the environmental hazards caused by his
pollution of the River.

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In addition to that, the first incidents of mercury poisoning appeared in the population
of Minimata bay in Japan, in 1952. This was caused by consumption of fish polluted
with mercury which brought about over 500 fatalities. [25].
In 1986, in Sandoz, water used to extinguish a major fire carried C. 3ot fungicide
containing mercury into the upper Rhine. Fishes were killed over a stretch of 100km.
The shock drove many Federal Environmental Agency (FEA) projects forward.
Also, toxic chemicals in water from a burst dam belonging to a mine contaminated the
Coto De Danana nature reserve in Southern Spain, C.5 in Southern Spain, C.5 million
M-of mind containing sulphur, lead, copper, zinc and cadmim flowed down the Rio
Guardimar. Experts estimated that Europe’s largest bird sanctuary as well as Spain’s
Agriculture and fisheries suffered permanent damage from this pollution.[25]
1.2.8 EFFECTS OF CADMIUM ON THE ENVIRONMENT.
Cadmium derives its toxicological properties from its chemical similarity to zinc an
essential micro element for plants, animals and humans (25).
In humans, long-term exposure is associated with renal disfunction. High exposure
can lead to lung disease and has been linked to lung cancer. The average daily intake
for humans is estimated as 0.15 mg from air and 1 µg from water. Smoking of 1
packet of 20 cigarettes can lead to the inhalation of around 2.4 µg of cadmium. [25]
1.3:9 EFFECT OF ANTIMONY ON THE ENVIRONMENT.
Antimony is a metal used in the compound antimony trioxide, a flame retardant.
Exposure to high levels of antimony for short period of time causes nausea, vomiting
and diarrhea. There is little information on the effects of long-term exposure, but it is

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a suspected human carcinogen. Most antimony compounds do not bioaccumulate in
aquatic life. [25].
1.3:10 EFFECTS OF COPPER ON THE ENVIRONMENT
Copper is an essential substance to human life, but in high doses it can cause anaemia,
liver and kidney damage. It can also lead to stomach and intestinal irritation. People
with Wilson’s disease are at greater risk from over exposure to copper. Copper
normally occurs in drinking water from copper pipes and also from additives designed
to control alga growth.
1.3.11 EFFECTS OF CHROMIUM ON THE ENVIRONMENT
Chromium is used in metal alloys and pigments for paints, cement, paper and rubber.
Low-level exposure can irritate the skin and cause ulceration. Long-term exposure can
cause kidney and liver damage and damage to circulatory and nerve tissues. It often
accumulates in aquatic environments thereby adding to the danger of eating fish that
may have been exposed to high levels of chromium.
1.3.12 EFFECTS OF LEAD ON THE ENVIRONMENT
Lead is a trace metal that is present naturally in soils and water in trace amounts (26).
In humans, exposure to lead can result in a wide range of biological effects depending
on the level and duration of exposure. Various effects occur over a broad range of
doses, with the developing foetus and infant being more sensitive than adult. High
levels of exposure may result in toxic biochemical effects on humans, which in turn
cause problems in the synthesis of hemoglobin, effects on the kidneys, gastro
intestinal tract, joints and reproductive system and acute or chronic damage to the
nervous system. [25].

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Average daily lead intake for adult in UK is estimated at 1.6 µg from air, 20 µg from
drinking water and 28µg from food. Although most people receive the bulk of their
lead intake from food, in specific populations, other sources may be more important,
such as water in areas with lead piping and air near point of source emissions, soil,
dust, paint flakes in old houses of contaminated land. [25]
1.3.13 EFFECTS OF MERCURY ON THE ENVIRONMENT
Mercury is a toxic substance which has no known function in human biochemistry and
physiology and does not occur naturally in living organisms. Inorganic mercury
poisoning is associated with tumor and/or minor psychological changes together with
spontaneous abortion and congenital malformation.
Monomethyl mercury causes damage to the brain and the central nervous system, it
also gives rise to abortion, congenital malformation and development changes in
young children. [25]
1.3.14 EFFECTS OF NICKEL ON THE ENVIRONMENT
Small amounts of nickel are needed by the human body to produce red blood cells. In
great amounts, it can become mildly toxic. Long term exposure can cause decreased
body weight, heart and liver damage but short-term over exposure to Nickel is not
known to cause any problems. nickel can accumulate in aquatic life, but its presence is
not magnified along food chain. [25]
1.4 SOLUBILITY OF HEAVY METALS IN SOIL.
Solubility of heavy metals is directly related to sorption capacity of residuals and soil.
Soil pH and iron oxides are very important factors controlling metal solubility in these
systems. Sorption is an important chemical process that regulates partitioning of

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heavy metals between solution and solid phases in soils. Recent studies on this have
shown that heavy metal solubility and availability in land applied residuals is
governed by fundamental chemical reactions between metal constituents and soil and
residual components [27].
Iron, aluminum and manganese oxide soil minerals are important sinks for heavy
metals in soil and residual amended soils. Heavy metal cations sorb to soil organic
matter (som) and other forms of humified natural organic matter (NOM). The type of
sorption by NOM affects the environmental fate of heavy metals. Heavy metal cations
form sparingly soluble phosphates, carbonates, sulphides and hydroxides. Sorption
and many metal precipitation processes are highly pH dependent. The pH of the soil
residual system is often the most important chemical property governing sorption and
precipitation of heavy metals. [27]
1.5 PHYTO AVAILABILITY OF HEAVY METALS IN RESIDUAL –
TREATED SOILS.
Application of residuals to soil affects phytoavailability by introducing heavy metal
into the soil and / or redistributing heavy metal into different chemical pools that vary
in phytoavailability (28). Application of biosolids increases heavy metal solubility and
availability in soil. Increases in availability are a function of metal type and metal
loading. Transmission of heavy metal through the food chain is affected by the soil
plant barrier (29). The barrier limits transmission of metal through the food chain
either by soil chemical processes that limit solubility (e.g soil barrier) or by plant
senescence (showing sign of old age) from phytotoxicity (e.g. plant barrier). The soil
plant barrier limits transmission of many heavy metals through the soil-crop-animal

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food chain, except aluminum, zinc, molybdenum, and selenium. Cadmium, which has
lower affinity for metal-sobbing phases (e.g. oxides, NOM), has the greatest potential
for transmission through the food chain in levels that present risk to consumers (30).
1.6 LONG TERM ENVIRONMENTAL FATE AND BIOAVAILABILITY OF
HEAVY METALS IN RESIDUAL TREATED SOILS.
Heavy metals do not degrade in soil and many are considered persistent
bioacumulative toxins (PBTs). The risk to human and ecosystem health from land
application of PBTs in residuals depends on solubility and bioavailabilty of these
contaminants in the residual – treated soil. Uncertainties exist in the effect of
decomposition of soil organic matter complexes that bind metal and uncertainties of
the effect of slower long term reactions between metals adsorbed to inorganic oxide
surfaces in soils on metal solubility and bioavailability. Recent research findings show
that heavy metal is adsorbed to oxide phases of Biosolids (31). Heavy metals
sequestered to oxide surfaces will likely remain sequestered longer than metal
complexed by biosolids NOM. However, the stability of metal sequestered by oxide
depends on the metal and the mineral oxide surface. Long term mineral crystallization
reactions may “eject” metals from the solid phase into solution. The long-term
stability of sequestered metal bounded to metal oxide surfaces remains uncertain.
1.7 SOLUTE INTERACTIONS IN SOILS IN RELATION TO
BIOAVAILABILITY AND REMEDIATION OF THE ENVIRONMENT.
For diffuse distribution of metals (e.g). Fertilizer-derived cadmium input in pasture
soils), remediation options generally include amelioration of soils to minimize the
metal bioavailability.

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The bioavailability of a chemical in the soil environment has been defined as the
fraction of the total contaminant in the interstitial pore water (i.e., soil solution) and
soil particle that is available to the receptor organism [32]. Bioavailability can be
minimized through chemical and biological immobilization of metals using a range of
inorganic compounds such as lime and phosphate (p) compounds (e.g. apatite rocks),
and organic compound such as “exceptional quality” biosolids [33]. Reducing metal
availability and maximizing plant growth through inactivation may also prove to be an
effective method of in situ soil remediation on industrial, urban, smelting and mining
sites.
The more localized metal contamination found in urban environments (e. g chromium
contamination in timber treatment plants) is remedied by metal mobilization process
that include bioremediation (including phyto remediation) and chemical washing.
Bioavailability of metals in soils can be examined using chemical extraction and
bioassay tests. Chemical extraction test includes single extraction and sequential
fractionation [34]. Bioassay involves plants, animals and microorganism [35].
A number of amendments are used either to mobilize or immobilize heavy metals into
soil solution, which is subsequently removed using higher plants. In contrast, in case
of the immobilization technique, the metal concerned is removed from soil solution
either through adsorption, complexation and precipitation reactions, thereby rendering
the metals unavailable for plant uptake and leading to groundwater.
Since one of the primary objectives of remediating contaminated sites is to reduce the
bioavailability of metals, in-situ immobilization using soil amendments that are low in
heavy metal content may offer a promising option. However, a major inherent

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problem associated with immobilization technique is that although the heavy metals
become less bioavailable, their total concentrations in soils remain unchanged. The
immobilized heavy metal may become bioavailable with time through natural
weathering process or through breakdown of high molecular weight organic metal
complexes.
1.8 A CRITICAL REVIEW OF THE BIOAVAILABILITY AND IMPACTS
OF HEAVY METALS IN MUNICIPAL SOIL WASTE COMPOSTS.
The concentration, behaviour and significance of heavy metals in composted waste
materials is important from two potentially conflicting aspects of environmental
legislation in terms of: (a) defining end-of-water criteria and increasing recycling of
composted residuals on land and (b) protecting soil quality by preventing
contamination. All types of municipal soil waste (m s w) compost contain more heavy
metals than the background concentrations present in soil and will increase their
contents in amended soil. [36] Total concentrations of heavy metals in such segregated
and green waste compost are typically below UK PAS100 limits and mechanical
segregated material can also comply with the metal limits in UK PAS100 , although
this is likely to be more challenging [36]. Zinc and lead are the elements presents in
the largest amounts in MSW-compost. Lead is the most limiting element to use of
mechanical segregated compost in domestic gardens, but concentrations are typically
below risk based thresholds that protect human health.
There is general consensus in the scientific literature that aerobic composting
processes increase the complexation of heavy metals in organic waste residuals, and
that metals are strongly bound to the compost matrix and organic matter, limiting their

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solubility and potential bioavailability in soil. Lead is the most strongly bound
element and nickel the weakest, with zinc, copper and Cadmium showing intermediate
sorption characteristics. The strong metal sorption properties of compost produced
from m s w or sewage sludge have important benefits for the remediation of metals
contaminated industrial and urban soils.
The availability of metals in soil depends on the nature of the chemical association
between a metal with the organic residual and soil matrix, the pH value of the soil, the
concentration of the element in the compost and the soil, and the ability of the plant to
regulate the uptake of a particular element.
However, there is good experimental evidence demonstrating the reduced
bioavailability and crop uptake of metal from composted biosolids compared to other
types of sewage sludge. [36] The total metal concentration in compost is important in
controlling crop uptake of labile elements, like zinc and copper, which increases with
increasing total content of these elements in the compost.
1.9.1 HEAVY METALS TRANSPORT IN THE SOIL PROFILES UNDER
THE APPLICATION OF SLUDGE AND WASTEWATER.
The results of packed-column studies may be overly optimistic in predicting soil
immobilization of metals, by pass flow via preferential flow paths in field soils may
allow significant metal transport to ground water (37). The lack of significant metal
deposition in subsoil may not be reliable evidence for immobility of sludge application
metals (38).
Alloway and Jackson (1991) cited several studies reporting some downward metal
translocation in soil, noting a potential correlation with climate (39). Soluble and

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colloidal organics have been shown experimentally to moblize metals (40). Land
application of sludge or compost can have both beneficial and harmful aspects. Its
organic matter content, which constitutes approximately 50% of the solid fraction,
may improve soil physical properties. Nitrogen and phosphorous, ranging from 2 to
8% and 1 to 4% respectively, in sewage sludge and sludge compost are nutrients
essential for growth of crops. Municipal sludge, however, often contain undesirable
chemicals which may be toxic to plants and/or eventually toxic to animals and human
that consume edible parts of such plants (41).
It was concluded that the use of wastewater and sludge application in agricultural
lands, enriched soils with heavy metals to concentrations that may pose, potential
environmental and health risks in the long term.

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