Volume 8, Issue 1, January – 2023 International Journal of Innovative Science and Research Technology

ISSN No:-2456-2165

The Impact of Heavy Metals on the Soil in Calabar

Metropolis Lemna Area
Udie Linus Ugbong Offiong Effanga Offiong
Department of Pure & Applied Chemistry, University of Department of Pure & Applied Chemistry, University of
Calabar, Calabar, Cross River State Calabar, Calabar, Cross River State

Etuk Marvelous Christopher Anjorin Ayodele Ebenezer

Department of Zoology and Environment Biology, Department of Pure & Applied Chemistry, University of
University of Calabar, Calabar, Cross River State Calabar, Calabar, Cross River State

Abstract:- Soil samples were collected from the dumpsite metals in soil, which evaluates the actual potential
soil located at Lemna Road, Calabar Municipality, Cross mobility in metals and according to Bashir et al.. (2013).
River State, Nigeria to investigate the speciation and The understanding of metal bioavailability and mobility
bioavailability of some trace metals namely: iron, in soil is important for eva luati ng its potential
cadmium, copper, zinc and lead. Extract from the soil environmental and health effects. Environmental
were obtained by sequential extraction. This involved reports have also shown that, pollution of soil
Acid extractable fraction, Oxidisable fraction, Reducible envi ronment is ascertained by ca lculating the enrich men t
fraction and Residual fraction. These fraction were then factor, the contami nation factor/degree of contamination
analyzed for Pb, Cd, Cu, Fe and Zn using acetylene and i ndex of geoa ccumution . However, previous studies
flame atomic absorption spectrophometer. The results in dumpsite soils wi thin the area concentrate on the
obtained, showed that the metals occurred with the determination of total metal con tent without assessing the
following percentage bioavailability: Fe (33.57%), Zn polluting status of the dumpsite and metal. These elements
(43.59%), Cd (67.23%), Cu (82.98%) and Lead are usually associated with the principle component of
(69.96%). Acid extractable 5.57% reducible fraction the sam ples (Carbonates, Organic Matter, Fe –Mn Oxides
accounted for over 9.33% of the total fractions, metal and Minerals) and they are available to living organism
bound to residual and oxidisable fraction accounted for when the dissolved i n environ mental materials. The
10.90% and 13.05% respectively. Fe has the highest information about the physiocochemical properties of the
distribution in all the fractions followed by Zn while Cd elements is required for understanding their environment
has the least in all the fractions. The results of these behavior, including mobility and bioavailability, the
findings indicates that the trace metals with exception of determination of total metal content in the samples after
Cd were readily bioavailable in the dumpsite soil digestion with aqua regia does not provide sufficient
therefore, phytoremediation is advocated. criteria for estimating their ecological and biological
effects. The sampling area was mainly influenced from
I. INTRODUCTION three sources natural phenomenon, namely industrial,
traffic and natural sources. The mobilization of metal, in
Contamination of the soil by trace metal is a far more particular toxic heavy metals has caused the increase of
serious problem than either water or air pollution because their concentrations in the environment. Investigation of
they are usually tightly bound by the soil and may persist for metal contents of the dust samples of car parking areas
centuries depending on the conditions. Hence the are vital for heavy metal pollution originated from traffic
environmental problem of soil pollution by trace metals has particularly lead and recently the elements of platinum
received increasing attention in the past decades in both group, used in catalytic convertors for the purpose of
developed and developing countries of the world. Metal reducing the pollutants coming from automobile
toxici ty though dependent on their chemic a l forms, emissions. Th i s study aimed at using metal speciation to
can cause s e v e r a l diseases affecting almost all the vital identify the forms, mobility, bioavailability toxicity and
organs and functions of the human body· However, trace sources of trace metals in Lemna dumpsite soils. It is also
metals such as Zn, Cu, Cr, Fe, and Mn are required by aimed at establishing the pollution status of the Lemna dumpsite
the body i n small amount, but can be toxic i n larger soil and its environ and compared result obtained at control site
quantities. It has been reported that the determi nation of with that of Lemna dumpsite soil thereby stressing the possible
total trace metal content in soil cannot indicate the factor, and effect for any difference observed.
comprehensive pollution status of the environment but
metal speciation can identify the bioavailability, mobility Nowadays soil p o l l u t i o n is ma i n problem t o
and toxicity of trace metal i n soils. Unlike the single agriculture. Soil pollution may arise and mainly y from
extraction tech nique, sequential extraction gives i ndustrial waste, sewage water, pesticides, fertilizers
information about both mobile and stable fraction of (chemical based), mining and smelting, fuel production,

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Volume 8, Issue 1, January – 2023 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165
automobile les etc. Industrial activities are also caused of profile into ground water via leaching or by colloid-
land pollution like chemical i ndustries, paper and pulp facilitated transport, precipitated as solid phases, diffused in
mills, steel industries, pharmaceuticals industries, mining porous media such as soils.
industries, refineries. pesticides and fertilizer industries.
thermal and nuclear power plants, food processing This r esearch work was carried out in the dumpsite
industries, tanneries. textile industries etc. releases their soil at L emna Road, Calabar, Cross River State, Niger
effluents direct into lands. Delta region of Nigeria. The state is located in the coastal south-
south part of the country, lying between S' 45°N 8'30°E I 5.
Srinivas N. et al., (2005). reported the concentration of 750°N 8.SOO'E. The state has basically two distinct seasons
Pb. Zn. Ni and Cu in air, soil and vegetables analyzed by namely the dry and the wet. The wet season fasts between 8
using ICP-ES. The work done mainly in indust rial areas, sub to 9 months starting from mid-march till the end of
urban and rural areas of Vishakhapatnam. The P b November. The dry season has a short duration of between
c o n c e n t r a t i o n (1.46µg/m3) is higher in industrial the last week of November or early December and last
area. Th e Ni, Zn and Cu concentrations is higher in semi till early march. This study was undertaken during April
urban area than with ind ustrial area. The concentration of when the rain was not yet much to avoid the
Pb in vegetable rural area 0.88 to l.02µgis and sub urban area leaching of the heavy metals to the soil. During the
3.55µg/g. sampling the surface soil samples were obtained from
the following location within the dumpsite at Lemna
Metalsin the en vironment maybe present in the solid, liquid Road, Calabar.
or gaseous state. They may be presen t as individual elements
and as organic and inorganic compound s. The movement of Table 1 Coordinates Samples Location
metal between environmental reservoirs may or may not S/N Locations Coordinate
involve changes of state. The geosphere is the original sourceof 1 Location 1 N 5°01’59.4’’ E8°21’59.3
al l meta l (except thosethat entered the atmosphere in the form of 2 Location 2 N5°01’59.7’’E8°21’49.9’’
meteorites andcosmicdust.) Wi thin the geosphere, metals may 3 Location 3 N5°01’57.2’’ E8°2157.5’’
be present in minerals, glasses and melts. In the 4 Location 4 N5°01’58.7’’E8°21’58.8’’
hydrosphere metals occur as dissolved ions and 5 Location 5 N5°02’ 1.7’’ E8°21’59.3’’
complexes, colloids and suspended solids. 6 Location 6 N5°02’ 1.9’’ E8°21’47.6’’
I n t he atmosphere, metals maybe present as gaseous II. SAMPLE COLLECTION AND TREATMENT
elements and compounds and as particulate and aerosols
(Nriagu; 1 989).Gaseous and particulate metals may be Top soil (0-15 cm) samples were collected at six (6)
inhaled and solid and liquid (aqueous-phase) metals may be different locations including the control sample. A W-shape
ingested or absorbed, thereby entering the biosphere. In format was employed in collecting samples in order to
addi tion to being the original source of all terrestrial cover a transverse of the dumpsite soil while the soil auger
metals. The atmosphere and hydrosphere also constitute was use to pick samples at six (6) different location.
si nks for metals however, from a geological perspective,
they are more likely to be considered as agents of  All samples were air d r i e d for three (3) days and
transport. grounded to pass through a 2rnm mesh. While trace
metals speciation was done using 3.3 procedures for
The main source for metal input to plants and soils is optimized BCR sequential extraction of trace metals
atmospheric deposition. Volatile metalloids such as As, Hg, were as described by Rauret et al, (2000) and Umoren
Se, and Sb can be transported over long distance in et al., ( 2 0 1 4 ) .
gorgeous form or enriched in particles, while trace metals
such as Cu, Pb, Zn are transported in particulate phases  Acid extractable fraction: 40ml of 0.11rnol/L acetic
(Adriano, 200l. Adriano et of .. 2005) in terrestrial (CH3COOH) was added to 1 g of dry soil sample in
ecosystem, soils are the major recipient of metal a 50ml polypropylene tube. The mixture was shaken
contaminants. while i n aquatic systems sediments are the overnight (16hr) in an end to end mechanical
major sink for metals (Spark. 2005). Freshwater system are shaker at room temperature. The mixture was
contami nated due to runoff and drai nage via sediments or centrifuged at 3000rpm for 20mins to separate the
disposal, while groundwater is impacted through leaching or extract from residue.
transport via mobile colloids (Adriano, 200l). A number of
biological processes take place at the heterogeneous interface
 Reducible fraction: 40ml of 0.5mol/L hydroxyl
between the rock, soil, water, air and living organisms. (Spark.
ammine hydrochloride (NH20H..HCI ) c o n t a i n i n g
2005). The process or interaction ill turn controls the solubility,
2..5ml 2m HN03 (pH = 1 . 5 ), was added to
mobility. bioavailability and toxicity of metals (Sparks, 2005).
residue from step 1, shaken for 16hr at 22 ± 50c
Metals are found in solution as free ions or complexestoinorganic
.The mixture was centrifuged as per step 1.
or organic liquids. Both the free ions and the metal· ligand
complexes can be; taken up by plants, retained on minerals,
natural organic matter, microbes, transport through the soil

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Volume 8, Issue 1, January – 2023 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165
 Oxidisable fraction: the residue from step two (2) was IV. RESULT
treated twice with 10ml of 8..8mol/Lhydrogenperoxide (H101) and
allowed to digest for one (1) hour with intermittent manual Table 2 Total Concentration of Trace Metal Ions (M/Kg) in
mixing. The mixture was evaporated to dryness, then 50ml Calabar Dumpsite Soil and Control.
of 1 mol/dm3 ammonium acetate (NH4 OAC) adjusted to Location Pb Cd Cu Fe Zn
pH = 2 with 2m HNO3 was added, shaken for 16hr at 22 A 238.25 1. 32 37.40 2506.01 1169.47
± 50C and centrifuged to separate the extract from B 241.07 1.45 43.26 2495.39 1246.32
residue. C 225.63 1.23 40.38 2673.85 1072.38
D 232.94 1.29 36.74 2594.17 1350.53
Residual fraction: To the residue from step iii, 5ml Control 5.78 0.42 4.72 306.55 12.06
16mol/L HCI on a hot plate cooled for 2hr and filtered
through Whatman no. 50 filter paper into a volumetric flask for
Table 3 Different Fractions of Lead
analysis. Determination of total trace metal 1g of sieved soil
sample was digested with 5ml conc. HNO3 and 15ml conc. Location Acid Reducible Oxidisable Residual
HCI on a hot plate. After cooling, the digest was filtered extractable
using (Whatman type 50 filter paper) into a 100ml volumetric A 66.85 98.30 33.48 37.62
flask and diluted to the mark with distilled water. B 67.52 99.01 34.15 38.27
Concentration of Cd, Cu, Fe, Zn, and Pb, in the extract from C 63.65 95.16 30.32 34.46
both sequential extraction method and total metal extracts D 65.52 96.73 32.18 36.16
were determined using air acetylene flame atomic Control 1.37 2.11 1.24 0.92
absorption spectrophotometer ( U n i c a m 939/ 959 model )
Rauret et al., 1999,Mmolawa et al., 2011; Udousoro et al., Table 4 Different Fractions of Cadmium
(2010). Location Acid Reducible Oxidisable Residual
extractable
III. CHEMICAL ANALYSIS A 0.50 0.35 0.23 0.19
B 0.51 0.37 0.26 0.22
All the supernatant solution from stage (i) to (iii) C 0.47 0.33 0.21 0.17
and the residual digest (iv) were analyzed for the D 0.48 0.34 0.22 0.18
following trace metals: Lead (Pb), Cadmium (Cd), Control 0.16 0.10 0.07 0.06
Copper (Cu), iron (Fe), and Zinc (Zn) using air acetylene
flame atomic absorption spectrophotometer (Unicam Table 5 Different Fractions of Copper
939/959 model). Location Acid Reducible Oxidisable Residual
extractable
 Apparatus / Equipment used in the project. A 4.92 14.24 10.28 6.21
 Soil auger B 7.54 16.36 11.41 6.12
 Crucible C 6.82 15.62 9.69 6.40
 Filter D 5.91 14.69 9.78 4.49
 Filter funnel Control 0.90 1.82 1.12 0.82
 Mechanical shaker
 Centrifuge / fume cupboard Table 6 Different Fractions of Iron
 Atomic Absorption Spectrometer (AAS). Location Acid Reducible Oxidisable Residual
 Viii) Conical flask extractable
 Reagent bottle
A 315.21 492.12 614.30 1012.32
 Beaker
B 312.51 489.40 611.58 1009.62
 3.5 Chemical / Reagents
C 357.13 534.02 656.20 1054.24
 Acetic Acid (CH3 COOH)
D 337.21 514.10 636.28 1034.32
 Polypropylene tube
Control 47.75 61.06 78.23 114.51
 Hydrogen peroxide (H2 O2 )
 Nitric acid (HNO3 )
Table 7 Different Fractions of Zinc
 Hydroxyl ammonium chloride (NH2 OH.HCl)
Location Acid Reducible Oxidisable Residual
 Ammonium acetate (NH4 OAC) extractable
 Aqua regia (tri-oxonitrate and nitric acid)
 Hydrochloric acid (HCl) A 179.18 304.03 407.20 224.25
B 198.39 323.24 426.38 243.42
C 155.00 279.75 382.83 199.89
D 224.43 349.28 425.35 269.43
Control 1.87 3.13 4.38 2.06

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Volume 8, Issue 1, January – 2023 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165
Table 8 Percentage Concentration of Metal Ions in Different Fractions
S/N Fractions Pb Cd Cu Fe Zn
1 Acid extractable 0.66% 0.005% 0.063% 3.31% 1.89%
2 Reducible 0.97% 0.003% 0.15% 5.07% 3.14%
3 Oxidizable 0.33% 0.002% 0.10% 6.30% 4.17%
4 Residual 0.37% 0.0019% 0.06% 10.28% 2.34%

Table 9 Shows the Mean Value, Total Concentration and % Bioavailability

S/N Pd Cd Cu Fe Zn
1 Mean value 234.47mg/kg 1.32mg/kg 39.45mg/kg 2567.36mg/kg 1209.68mg/kg
2 Total conc. 2.34% 0.013% 0.39% 25.67% 12.10%
3 %bioavailability 69.96% 67.23% 82.98% 33.57% 43.59%

V. DISCUSSION  In the metals bound to organic matter (oxdisable), Fe also

had the highest concentration in all locations followed by
The tables above shows the result t of partitioning Zn in all the locations.
or trace metals in the soil sa mple. Fi gures 1-5 also  For the selected trace metals evaluated, they occurred in
represent the percentage composition of each trace metal the fraction in the order: for iron; Residual > Oxidisable
accumulated in t he four fractions. Taking location I as a > Reducible > Acid extractable. For zinc; Oxidisable >
case study the total conc. of tr a ce metals are partitioned Reducible > Residual > Acid extractable. For lead;
in the sediment in the order : Fe>Zn> Pb> Cu> Cd which Reducible > Acid extractable > Residual > Oxidisable.
followed same for all the location. I r o n have the total For cadmium; Acid extractable > reducible > Oxidisable
concentration of trace metal which was > Residual. For copper; Reducible > Oxidisable >
2506.0 1mg/kg and percentage concentration of 33.57% Residual > Acid extractable.
while cadmium have the lowest concentration with  I n acid ex tractable the occurrence of the Cd is least
1.32mg/kg. Both the oxidizable and residual fraction followed by Cu and Pb, while in reducible fraction
of lead (Pb) are closely related to values obtained for the Cd is still the l east widely fol l owed by Cu and Pb. Fe
same metal by Tessier et al , (1999) (0.8µg/0.81g/g) and is the highest in the entire fraction that shows the h igh
Horowi tz (l .3µg/g,0.8µg.lg) in the Ruzin sediment concentration of iron i n the Lemna dumpsite soil.
leachates. The concentration of lead i n residual fraction was  Also in o.xidisble fraction the percentage occurrence of
0.37%. The high value may not pose any threat to human and Cd is the lowest (0.002%) followed by Cu (0.1%) and Pb
its en vironment considering. the fact that metals in this (0.33%). Fe had the highest with (6.30%).
form are not readily released into solution b u t  In residua l fraction, Fe still had the highest occurrence
incorporated in the crystal lattices of clay minerals and with 10.28% with a high margin from closest Zn, which
silicate. Conversely, the distribution of lead in acid had 2.34%.
extractable (0.66°/o) and 0Kidi1.ablc (0.33%) forms. which
are known as the major contributors to the mobility and VI. CONCLUSION AND RECOMMENDATION
bioavailability of the metals in the soil were very high. Copper
had the highest percentage bioavailability o f 8 2 . 9 8 % The result obtai ned and pr e s e n t e d in this project
widely foll owed by lead 69.96% and has the least value of revealed that the concentrat ion of Fe and Zn i n the
33.57%. Percentage bioavailability fraction range from dumpsite soil at Lemna Road, Calabar is high. The high
35.57% to 82.98%. The values were moderate but most concentration of Fe and Zn could be as a result of iron
parts of the trace metals were absorbed or found in scraps and zinc metals which when rust and decompose
t h e exchangeable fractions. This small amount entering increased the concentration of the dual i n the area. The mean
biota may not pose immediate en vironmental hazards. It value concentration of zinc, though essential to maintain the
was also found that the percentage bioavailability or metabolism of organism, has to be monitored, because at high
trace metals studied followed the order Cu (82.98%) > Pb concentration. It can lead to poisoning and may cause anemia
(69.96%) > Cd (67.23%) > Zn (43.59%) > Fe (33.57%). The and copper deficiency as a result of bioavailability. The total
percentage bioavailability of Fe was found to be 33.57%. The concentration of cadmium in the fractions though minimal must
result of this investigation was on high side when compared also be monitored considering the fact that it is relatively mobile
with the findings of distribution pattern of Fe in the top soil in solution and has no nutritional benefit to both animal
within Awkuzu area of Anarnbra State, Nigeria as reported and plant. Soluble in anoxic environment and readily
by Omuku et al., (2009). available to biota Reducible metals which arc the most
important scavengers represented only a minor fraction of the
 The concen tration of trace metals evaluated i n residual sediment (0.003%). Bound to organic matter fraction also
form were relatively high. Fe had the highest bounded small portion of the trace metals i nstigated. Residual
concentration of 2 506.01mg/kg, Cd had concentration metals, that is those that bound to crystal lattices and
of 1.32mg/kg, and this value is low and tolerable but should silicates, were found to be 10.28%. This portion is not easily
be monitored. released into ecosystem over a time frame, therefore the

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Volume 8, Issue 1, January – 2023 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165
easy of bioavailability is negligible. The continuous [8]. Culbard, E. B. and L.R. Johnson. (1984). An
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