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Chapter one 1.1 Introduction Organic pollution is the term used when large quantities of
organic compounds. It originates from domestic sewage, urban run-off, industrial
effluents and agriculture wastewater. sewage treatment plants and industry including
food processing, pulp and paper making, agriculture and aquaculture. During the
decomposition process of organic pollutants, the dissolved oxygen in the receiving
water may be consumed at a greater rate than it can be replenished, causing oxygen
depletion and having severe consequences for the stream biota.

Wastewater with organic pollutants contains large quantities of suspended solids which
reduce the light available to photosynthetic organisms and, on settling out, alter the
characteristics of the river bed, rendering it an unsuitable habitat for many invertebrates.
Organic pollutants include pesticides, fertilizers, hydrocarbons, phenols, plasticizers,
biphenyls, detergents, oils, greases, pharmaceuticals, proteins and carbohydrates.[1]
Toxic organic pollutants cause several environmental problems to our environment. The
most common organic pollutants named persistent organic [2] pollutants (POPs).

POPs are compounds of great concern due to their toxicity, persistence, long-range
transport ability and bioaccumulation in animals,[3] travel long distances and persist in
living organisms. POPs are carbon-based chemical compounds and mixtures (twelve
pollutants) that include industrial chemicals such as polychlorinated biphenyls (PCBs),
polychlorinated dibenzo-pdioxins and dibenzofurans (PCDD/Fs), and some
organochlorine pesticides (OCPs), such as hexachlorobenzene (HCB) or dichloro-
diphenyl-trichloroethane (DDT), dibenzo-p-dioxins (dioxins) and dibenzo-p-furans
(furans).[4] PCDD/Fs are released to the environment as byproducts of several processes,
like waste incineration or metal production.[5] Many of these compounds have been or
continue to be used in large quantities and due to their environmental persistence, have
the ability to bioaccumulate and biomagnify.[6] Efficient techniques for the removal of
highly toxic organic compounds from water have drawn significant interest.

A number of methods such as coagulation, filtration with coagulation, precipitation,

ozonation, adsorption, ion exchange, reverse osmosis and advanced oxidation processes
have been used for the removal of organic pollutants from polluted water and
wastewater. These methods have been found to be limited, since they often involve high
capital and operational costs. On the other hand ion exchange and reverse osmosis are
more attractive processes because the pollutant values can be recovered along with
their removal from the effluents.

Reverse osmosis, ion exchange and advanced oxidation processes do not seem to be
economically feasible because of their relatively high investment and operational cost.
Among the possible techniques for water treatments, the adsorption process by solid
adsorbents shows potential as one of the most efficient methods for the treatment and
removal of organic contaminants in wastewater treatment. Adsorption has advantages
over the other methods because of simple design and can involve low investment in
term of both initial cost and land required.

The adsorption process is widely used for treatment of industrial wastewater from
organic and inorganic pollutants and meet the great attention from the researchers. In
recent years, the search for low-cost adsorbents that have pollutant –binding capacities
has intensified. Materials locally available such as natural materials, agricultural wastes
and industrial wastes can be utilized as low-cost adsorbents. Activated carbon produced
from these materials can be used as adsorbent for water and wastewater treatment.

[7] The adsorption technique has become more popular in recent years for wastewater
treatment owing to its efficiency in the removal of pollutants too stable for biological
methods (Figure 1). Dye adsorption is a result of two mechanisms (adsorption and ion
exchange) and is influenced by many factors such as dye/adsorbent interaction,
adsorbent’s surface area, particle size, temperature, pH and contact time. The main
advantage of adsorption recently became the use of low-cost materials, which reduces
the procedure cost. / Figure 1. Works published for “adsorption” and various
environmental (Data after search in Scopus).(7.1) However, following the economic
boom in the 1970s—where the procedure cost was not such a big problem (or had not
been taken into account)—the economic crisis of the 2000s arose and led researchers to
turn their interest to other fields with lower procedure costs. Therefore, different
materials were tested as possible wastewater adsorbents.

The selection for the most appropriate adsorbent would be based on some major
characteristic properties such as: (i) the low-cost along with the satisfactory adsorption
properties (capacity, reuse, industrial-scale use etc.) and (ii) the environmentally-friendly
nature of each adsorbent. It is fundamental to use only materials which either have the
lowest impact on environmental balance or are absolutely environmentally-friendly
(from abundant natural sources, biodegradable, non-toxic etc.).

, a new term will be introduced in this study, which is called “green adsorption”. Under
this term, it is meant that the low-cost materials originated from: (i) agricultural sources
and by-products (fruits, vegetables, foods); (ii) agricultural residues and wastes and (iii)
low-cost sources from, which most complex adsorbents will be produced (i.e., activated
carbons after pyrolysis of agricultural sources Therefore).

These “green adsorbents” will be expected to be inferior (regarding their adsorption

capacity) than the super-adsorbents of literature (complex materials as modified
chitosans, activated carbons, structurally-complex inorganic composite materials etc.),
but their cost-potential makes them competitive. 1.2 Objective By studying the literature
survey and the previous works, the investigation on the removal of phenol from waster
by adsorption using walnut shell as adsorbent was carried out. The objectives of the
research work are as following. Collection of walnut shell Washed Crushed in a crusher
(FRITSCH industry.8 6580 Idar Oberstein). Sieved into particule size of 0.1mm, using a
sifter (Analysensieb-retsch-5657 HAAN W).

Characterization of the prepared adsorbent. Preparation of synthetic wastewater. Batch

studies for adsorption of phenol on the adsorbent. Optimization of operating
parameters using design of experiments. Conduction of isotherm and kinetic studies
and to calculate the adsorption capacity. 1.3 Methodology The walnut shell (50 g) were
initially powdered to remove any earthy matter. It is washed with distilled water to
remove all the dirt and impurities. It is dried in hot air oven (Serve well instruments
Private Limited H024DF) at 110°C for 1h to remove the moisture content. The 50 g of
sample was mixed with 95 mL of 0.1 M sulphuric acid for 15- 20 minutes.

Then the mixture was kept in a muffle furnace (Shital Scientific EMF-34) at 450oC for 1.5
h. After the heating process, the mixture was cooled and mixed with distilled water in
2000 ml beaker and allowed to settle for overnight. The process was continued and 0.1N
Sodium hydroxide was added, till the pH of the chemically treated carbon comes in the
range of 6-7. Then it is once again dried in hot air oven for 24 hour and ground to fine
particles passing through 300 mesh sieves. Finally the prepared powder was stored in air
tight containers. The batch experiments were conducted in 250mL conical flasks
containing 200mL of phenol solution of various initial concentrations. The equilibrium
time for the phenol adsorption was evaluated.
The variation of operating parameters such as adsorbent dosage, pH and initial
concentration were optimized and studied. The kinetic studies were conducted under
optimum conditions. The flasks were agitated in the shaker and the samples were
collected at regular interval of time. The samples were filtered using vacuum pump and
the remaining phenol concentration was measured using UV spectrophotometer at a
wavelength of 270 nm with the help of calibration chart prepared.

The isotherm studies were conducted by agitating the solutions of different

concentrations 40, 60, 80, 100, 120, 140, 160 and 180 mg/L till the equilibrium time. At
the end of equilibrium time, the concentration of the samples were determined using
UV Spectrophotometer.[7.1]

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