ABSTRACT
The extraction of Nickel (II) from various buffered aqueous solutions was studied using chloroform solutions of Butanoyl-2, 4-Dihydro-5-Methyl-2-Phenyl-3h-Pyrazol-3-One (HBUP). The effect various acids, anions and complexing agents (acetylacetone) on the extraction efficiency of Butanoyl-2, 4-Dihydro-5-Methyl-2-Phenyl-3h-Pyrazol-3-One (HBUP) were also studied investigated and optimized. From the mineral acids studied at various concentrations of 0.1 M, 0.5 m and 1.0 M, the result obtained showed that increase in acid concentration resulted to a steady decrease in the percentage extraction of the Ni2+ ion The results on the effects of anions at similar concentration for the mineral acids on the extraction of Nickel showed that anionic species exhibited similar trend with the mineral acids with increase in their concentrations affecting decrease in the percentage extraction of the Ni2+. Acetylacetone showed an excellent complexing agent when mixed with 4-butanoyl-2,-4-dihydro-5-methyl-2-phenyl-3H-Pyrazol-3-One (HBUP) and the mixture is capable of extracting Ni2+ even in acidic solution.
TABLE OF CONTENTS
Page
Cover page
Title page i
Declaration ii
Certification iii
Dedication iv
Acknowledgments v
Table of contents vi
Abstracts ix
CHAPTER ONE
INTRODUCTION
1.1 Background of the Study 1
1.2 Statement of
problems 3
1.3 Scope of the
study 3
1.4 Aim of the
study 4
1.5 Objectives of
the study 4
CHAPTER TWO
LITERATURE REVIEW
2.1 Historical Facts of Nickel and Its Application 5
2.2 General
Uses and Applications of Nickel 5
2.3 Natural
Abundance of Nickel 6
2.4 Acetylacetone 6
2.5 4-Butanoyl-2,
4-Dihydro-5-Methyl-2-Phenyl-3h-Pyrazol-3-One (Hbup) 7
2.6 Liquid-Liquid Extraction 10
2.6.1 Applications/Uses
of Liquid-Liquid Extraction 12
2.6.2
Factors
Influencing Liquid-Liquid Extraction 14
CHAPTER THREE
MATERIAL AND METHODS
3.1
Materials and apparatus 17
3.2
Methods 18
3.2.1 Preparation of standard solutions
mineral acids 18
3.2.2 Preparation
of standard solutions for anions 18
3.2.3 Preparation
of Metal Standard Solutions 19
3.2.4
Preparation of Stock Solutions of Ligand 19
3.2.5
Preparation of Buffer Solutions for Calibration of pH Meter 20
3.2.6 Preparation
of Buffer Solutions 20
3.2.7
Extraction of Metal Ions from Aqueous Phase at Different pH Values 21
3.2.8
Extractions with Various Metal Concentrations with Ligand 21
3.2.9
Extractions with Various Ligand Concentrations 21
3.2.10 Extraction
in the Presence Of Some Mineral Acids 22
3.2.11 Extraction
in the Presence of Some Anions 22
3.2.12 Extraction
in the Presence of Acetylacetone 22
CHAPTER
FOUR
RESULT
AND DISCUSSION 23
4.1 Absorbance
of Nickel 23
4.2
Effect of Mineral Acids on Nickel 23
4.3
Anions Concentration of Nickel 24
CHAPTER FIVE
5.1 Conclusion 26
5.2 Recommendation 26
Reference 26
Appendices 37
LIST OF TABLES
Table
4.1: Result of Concentration and absorbance of Nickel 23
Table
4.2: Result on effect of mineral acids on Nickel 23
Table
4.3: Anions concentration of Nickel 24
LIST OF FIGURES
Figure
1: shows
the calibration curve used for determining the unknown concentrations of Ni2+
in aqueous raffinate 37
Figure 2: Graph on the effect of acid concentration
on Nickel 38
Figure
3: Graph on the effect of anion concentration on Nickel 39
CHAPTER ONE
INTRODUCTION
1.1 BACKGROUND OF THE STUDY
Heavy metals are a group of trace metals
and metalloids found in the environment, such as arsenic, cadmium, chromium,
cobalt, copper, iron, lead, manganese, mercury, nickel, tin, and zinc. These
metals have a relatively high density of over 4.0 g/ml which is relatively high
compared to water whose density is 1.0 g/ml The metal ions are known to
contaminate the soil, atmosphere, and water systems and are poisonous even in
very low concentrations (Salem et al.,
2000). Although heavy metals are naturally abundant in the earth’s crust,
major environmental contamination and biological exposure arise from human
activities such as mining and extraction operations, domestic and agricultural
use of metals and metal-containing compounds such as pesticides and additives
(He et al., 2005; Goyer, 2001;
Shallari et al., 1998). Industrial sources include metal processing in
refineries, coal burning in power plants, petroleum combustion, nuclear power
stations and high tension lines, plastics, textiles, microelectronics, wood
preservation and paper processing plants (Arruti et al., 2010; Sträter et al.,
2010). Environmental contamination can also occur through metal corrosion
by the atmosphere and water, soil erosion of metal ions and leaching of heavy
metals, sediment re-suspension and metal evaporation from water resources to
soil and ground water (Nriagu, 1989). Natural phenomena such as weathering and
volcanic eruptions have also been reported to significantly contribute to heavy
metal pollution (Fergusson, 1990)
In recent years, heavy metal
contamination has become one of the most topical environmental issues and some
appropriate steps have been taken to reduce heavy metals and metalloids in
water to acceptable levels. Several treatment methods have been developed recently
to adsorb these pollutants and discharge them into systems where they are been
handled safely (Wołowiec, 2019). These methods include chemical precipitation
(Fu and Wang, 2011; Mauchauffée and Meux, 2007), ion exchange (Verma et al.,
(2008). adsorption (Cochrane et al.,
2006; Davarnejad and Panahi,, 2016), membrane
filtration (Landaburu-Aguirre et al.,
2010), reverse osmosis (Mohsen-Nia, et al., 2007). solvent extraction (Lertlapwasin,
et al., 2010). and electrochemical
treatment. Many of these methods suffer from high capital and operational
costs.
Nickel is one of many trace metals widely distributed in
the environment. It is present in the soil, water and air in deferent form.
Nickel is essential element for plant in low concentration but high
concentration is toxic. It is also toxic for human health. Nickel occurs
predominantly as the ion [Ni(H2O)6 ]2+ in
natural waters at pH 5-9 (WHO, 1991). Nickel
sources are steel, non-ferrous alloys, super-alloys, electroplating, alnico
magnets, coinage, microphone capsules, rechargeable batteries, plating on
plumbing fixtures, catalysts, dental and surgical prostheses (Zhang, and
Wang, 2015). Some health
condition that can be acquired through nickel contamination are anemia, diarrhea, encephalopathy, hepatitis, lung and
kidney damage, gastrointestinal distress, pulmonary fibrosis, renal edema, skin
dermatitis (Hoseinian et al.,
2018).
It is has also been observed that relatively low
concentrations of nickel are toxic to a wide variety of plants. Nickel is
usually absorbed in the ionic form (Ni2+), from the soil or the
culture solution. There are a number of reports that nickel is easily absorbed
by the plants when supplied in the ionic form and is not as strongly absorbed
when chelated (Kock and Mitchell, 1956). The absorption of nickel by plants is
depending on the total amount of nickel present in the soil (Roth et al., 1971) and the properties of the
soil, soil pH and the organic matter content (Vergnano and Hunter, 1953). This
accelerated rate of nickel absorption actually does not depend on the net
amount of nickel present, but on the amount of exchangeable nickel present in
the soil. For this reason plants grown in soils rich in exchangeable nickel
have a high content of nickel in their tissues.
Nickel ion can be removed from nickel-containing
wastewater by several techniques: chemical precipitation, ion floatation, ion
exchange, adsorption, membrane filtration, and electrochemical treatments (Barakat, 2011;, Coman
et al., 2013). Chemical
precipitation is currently the most used treatment because the operation is
simple and requires low capital cost. The drawback is the high volume
generation of nickel-containing sludge that may still create environmental
problem if not handled properly (Barakat, 2011).
Electrochemical treatments enable recovery of nickel in the form of pure
nickel, nickel compounds, or concentrated stream that can be reused in
industrial processes (Djaenudin et al., 2017; Robotin et al.,2013). The drawbacks of these
treatments are the high energy consumption and possible fouling in the
processes that use membranes (Barakat, 2011).
Solvent extraction/Liquid-Liquid
Extraction (LLE) proves to be one of the most widely used methods, due to its
relatively high efficiency, low-cost, and ease of operation. The simplicity with which the parameters
controlling extraction, such as pH of the aqueous solution, extractants and
diluent, can be changed is a major advantage of solvent extraction (Vander Hoogerstraete et al., 2013). Solvent extraction technique has been used by
several researchers for extraction and separation transition metals. For instance,
the separation of cobalt and nickel using several extractants such as PC 88A
(Girish et al., 1998), cyanex 272 (Parthi
and Surangi 2008), Aliquat 336 (Nayl, 2010)., N-N ’ -carbonyl difatty
amides (Emad and Khalid, 2011), have
been reported.
This research work involves the extraction of Nickel (II)
ion from wastewater using a mixture of 4-Butanoyl-2, 4-Dihydro-5-Methyl-2-Phenyl-3h-Pyrazol-3-One (HBUP)
and 4-Acylpyrazoline as extractants.
1.2
STATEMENT OF THE PROBLEM
The discharge of industrial effluents
containing appreciably high concentrations of heavy metals such as nickel into
the environment, particularly natural water has constituted environmental
nuisances. The need for the recovery of heavy metals from either their ores or
from industrial effluents has been of great interest to the environmental
analytical chemists. Metals such as cadmium, arsenic, mercury and lead are highly
toxic. Hence, there is urgent need to ensure complete removal of heavy metals
from contaminated water bodies and hence this research work.
1.3
AIM OF THE STUDY
The research is aimed at evaluating the efficiency
of HBUP in liquid-liquid extraction of N2+.
1.4
OBJECTIVE OF THE STUDY
1.
Preparation of various standard solutions of
anions.
2.
Preparation of various standard solution of complex
agents
3.
Preparation of various standard solutions of
mineral acids.
4.
Preparation of 1000ppm solution of metal ions.
5.
Extraction of metal ions from aqueous phase into
organic phase. (Acetylacetone solution of HBUP). Evaluation efficiency of HBUP
in acetylacetone.
1.5
SCOPE OF THE STUDY
The scope of this study covers the determination of
the effect of mineral acids, anions and complexing agents in the extraction of
Ni (II) from waste water using acetylacetone/HBUP as an extractant..
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