Experiment 3 – Electrochemical Water Treatment 28/2/2017

Group B18

Second Year Laboratory Report

Experiment 3 – Electrochemical Water Treatment (Arvia Water Treatment)
Group B18: Members: Jun Ying Liew 9829359
Ming Wei Chua
Beatrice May Ter Liew
Brenda Wiputeri

Table of Contents Page

1.0) Abstract……….……………………………………………………......2
2.0) Context
2.1) Introduction……...………………………………………………2
2.2) Aims and learning outcomes…………...……………………......2
2.3) Relevance……………………………………………....………..2
3.0) Literature Review……………………………………………………....4
4.0) Theory………………………………………………………………......5
5.0) Methodology…………………………………………………………....9
6.0) Core Work……………………………………………………………..10
7.0) Equipment used………………………………………………………..11
8.0) Hazards………………………………………………………………...11
9.0) Results
9.1) Observed Data…………………………………………………..12
9.2) Derived Results...…………………………………………….....15
9.3) Calculations……………………………………………………..
10.0) Discussion
10.1) Interpretation of results………………………………………...
10.2) Comparison with theory………………………………..............
10.3) Limitations……………………………………………..............
10.4) Conclusion……………………………………………..............
11.0) Nomenclature………………………………………………................
12.0) References…………………………………………………………….

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1. Abstract
2. Context
2.1 Introduction
Different approaches have been developed in order to treat and dispose of industrial wastewaters.
They include physical, chemical and biological methods. In this experiment, we are focusing on the
adsorption method, which is one of the physical method being developed. The adsorption method that
we are currently looking to investigate is a method developed by Arvia Technologies, which utilizes
the properties of Nyex 1000 as the adsorbent. The purpose of this experiment is to determine the
relationship between different parameters – fluidization time, regeneration time, regeneration current
density, and conclude on the most cost-effective parameters to use in order to treat 7m3 of waste water
containing 100mgL-1 of Acid Violet 17 (AV17). The cost incurred and the time required to treat 7m3
of wastewater is also taken into account when determining the optimum set-up.

2.2 Aims and learning outcomes

The experiment was carried out so that a suitable wastewater treatment of Acid Violet 17 (AV 17) can
be designed for Manchester Dyes Ltd to reduce concentration of Acid Violet 17 from 100 mg L-1 to
1 mg L-1 before discharging 7 𝑚3 of waste into sewages daily. The understanding of the Arvia process,
which is used for wastewater treatment and involves fluidizing, settling, and electrochemically
regenerating Nyex 1000 in a batch operation is gained. Using graphical methods, the relationship
between concentration of the dye with fluidization time, regeneration time and magnitude of current
were evaluated to determine parameters which can be used to optimise the operating conditions of
Arvia process. The experience of using laboratory equipment such as centrifuge and
spectrophotometer and understanding of their working principles were gained. The collected dye
samples were analysed using a spectrophotometer, where the amount of light absorbed by the sample
was measured. Absorbance readings are used to determine the greatest rate of change in concentration
of dye, which allows the observation of the most suitable current, fluidization and regeneration time
that could be used to treat Acid Violet 17 to a concentration below 1 mg L-1 .

2.3 Relevance
Many of our everyday products have colour, and the textile industry is the largest consumer of dyes
[1]. To date, there are more than ten thousand different types of dye available and approximately one
thousand tonnes of dyes are used annually [1]. A substantial amount of dye does not bind to the
material during the colouring process and is lost as part of the effluent. As the dyeing industry is one
of the most water consuming industries, the effluent carrying colour compounds and other chemicals
being discharged into the sewage could cause water pollution on a large scale [2]. Dyes have high
water solubility, and may also undergo degradation to form carcinogenic and toxic compounds which
can jeopardize both aquatic and human lives [1]. Also, dyes do not decompose in the presence of light
and they are resistant to biological digestion [3].
There are a number of efficient methods for water treatment to remove toxic compounds such as
coagulation, filtration with coagulation, precipitation, adsorption, ion exchange, reverse osmosis and
advanced oxidation processes [3]. However, most of these processes have high capital and operational
costs, and they are not economically feasible in the long run. Adsorption has the advantage of
requiring a lower cost due to its simpler design and its ability to remove both organic and inorganic
compounds from wastewater [3]. Activated carbon is an adsorbent that is widely used in water
treatment due to its high surface area, high adsorption capacity and its ability to be regenerated [4].
However, it is an expensive adsorbent not only due to its high initial cost but also the cost for off-site
regeneration, which accounts for 75% of the total operating and maintenance cost of a granular

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activated carbon packed bed [4]. Not only that, there is also high material loss during regeneration.
There are also adsorbents available at low cost such as sewage treatment plant biosolids, clay,
brewery waste, activated rice husk and wood-shaving bottom ash, where they each have different
adsorption capacity and ability [3]. However, all of these adsorbents could not be regenerated or
recovered, making them unsuitable to be used on a large scale commercially. Graphite-based
adsorbent known as Nyex 1000 is highly electrically conductive and non-porous but has small
adsorption capacity [4]. A better understanding of Nyex 1000 ability to electrochemically regenerate
and methods to improve its performance in water treatment process should be investigated to improve
on its commercial viability.

Figure 1: Benefits of the Arvia Water Treatment Process.

Other than colour removal, there are other issues in water treatment processes which could be
addressed by using Arvia process. The presence of antibiotics and drugs in the environment are
usually due to discharge of wastewater from hospitals, pharmaceutical industries and human waste,
where sewage plants do not detect or remove these antibiotics residue [5]. Hospital wastewater could
contain antibiotic levels than are almost 100 times greater than regular sewage plants [6]. Antibiotics
pose a threat to aquatic and soil organisms and if they were recycled into drinking water, they might
lead to carcinogenic or allergic reactions in the human body [5]. Another major concern is that
microorganisms in these wastewaters become more antibiotic resistant, which would contribute to the
proliferation of drug resistant infections [6]. Arvia process could remove an average of 90% of
pharmaceutical residues, including antibiotics, prescription and non-prescription drugs, which could
greatly reduce antibiotic residues in wastewater [6].
Also, Arvia water treatment could be used to treat microbiological contamination of water which
could cause many diseases such as diarrhoea, typhoid and cholera [7]. In three of the four water
treatment classes, which are B (disinfection of borehole water), C (standard treatment for reservoir
and lowland rives) and D (special treatment for industrial and urban development water sources),
disinfection of water is a part of the treatment [9]. Chlorine is the most commonly used disinfectant
but alternative disinfectants are being looked into as Chlorine could chemically react with organics to
produce by products that are potentially carcinogenic such as trihalomethanes [9]. In the Arvia
process, Nyex could adsorb microorganisms and electrochemically disinfect the water from
microorganisms such as Escherichia coli [7]. Disinfection occurs during electrochemical regeneration
and the mechanisms could include direct electrochemical disinfection, which deactivates the
microorganisms due to passage of electrons through the microbial and electrochlorination, which is
due to high concentration of chlorine produced at the cathode during oxidation of chorine [7].

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Metaldehyde pellets are a very common form of pesticides used to control population of slugs and
snails but they are long lived in the environment and have a solubility of 20 mg L-1 at 20 ℃ [6]. This
means that the leaching of Metaldehyde into water sources could easily occur and affect the quality of
drinking water since adsorption on activated carbon and advanced oxidation processes have proven
ineffective [8]. Nyex has been proven to be able to effectively remove and destroy 96% of
Metaldehyde from drinking water, reducing the concentration of Metaldehyde from 11 𝜇𝑔 L-1 to a
concentration less than EU/UK regulatory limits [8].

3. Literature Review

One of the methods to remove Acid Violet 17 using adsorption was investigated by R. Sivaraj et al. in
a Waste Management 21 (2001) article. In the experiment, the adsorbent used was powdered orange
peels and the study was carried out using batch adsorption with a control volume of Acid Violet 17 of
50 mL [1]. The author studied the effect of agitation time interval, initial dye concentration, pH and
adsorbent concentration on the performance of orange peels as adsorbents [1]. The author’s analysis
method was similar to our procedure in this experiment, which involves initially separating powdered
orange peels from the dye using a centrifuge at 10000 rpm and adsorption of light was measured by a
UV-visible spectrometer [1].

Figure 2: The effect of agitation time on the amount of Acid Violet 17 removed [1].

From Figure 2, it can be observed that for an adsorbent concentration of 100 mg/ 50 mL and dye
concentrations of 10,20,30, and 40 mg L-1, of 50 mL, the average mixing time required to reach the
saturation point of the adsorbent is 80 minutes [1]. Comparing this result to our fluidization time of
around 5 minutes to reach saturation of Nyex 1000, the time taken for maximum adsorption of Acid
violet 17 is much longer for orange peels. This could be because the rate of adsorption of dye onto the
orange peel is very low. From Figure 2, it can be observed that the amount of dye removed increases
with the concentration of dye. However, removal of dye was not enough to lower the concentration of
dye in the solution to the specification of 1 mg L-1. A maximum of 87% removal of dye from 10 mg
L-1 of Acid Violet 17 was achieved at a pH of 2 with an orange peel concentration of 600 mg/ 50 mL
[1]. This data indicates that a very large amount of powdered orange peels would be needed for
100 mg L-1 of Acid Violet 17. It was reported that the orange peels may be reused as desorption of
dye from adsorbent was possible through agitation of adsorbent with distilled water at different pH for
the same amount of time it takes for the adsorbent to be saturated [1]. From our experiment,

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regeneration time for Nyex 1000 is much shorter at 3 minutes. The use of orange peels as an
adsorbent may be economical and environmentally friendly, but it is very time consuming and they
could achieve a concentration of dye as low as Nyex 1000.

4. Theory
Methods of water treatment can be divided into three categories: physical, biological, and chemical
methods.
Physical methods of water treatment
Physical methods of water treatment usually involve filtration techniques capable of separating
suspended solids, such as sand filtration, multi-media filtration and membrane filtration [1]. Another
common physical method is reverse osmosis (RO), whereby contaminants are filtered out by means of
an applied pressure to force water through a semi-permeable membrane. Another well-known
mechanism classified under physical methods of water treatment is adsorption, which was the
mechanism employed during the experiments in this report.
Chemical methods of water treatment
Chemical methods of water treatment are also known as chemical unit processes. One of the many
notable chemical unit processes is coagulation-flocculation, which utilises two methods. Coagulation
method intends to neutralise the charges on the particles in the solution to be treated, causing small-
suspended particles to conglomerate and form microflocs. Here, a rapid and energetic mix is needed
to properly disperse and increase particle collisions. Following this, flocculation is deployed, whereby
gentle mixing is required to bring microflocs into contact with each other. Collisions from this stage
cause microflocs to bond and form visible flocs. Prolonged flocculation leads to formation of
macroflocs until they reach their optimum size. Physical separation methods such as sedimentation or
filtration can now be deployed to separate the macroflocs [2].
Biological methods of water treatment
Biological methods of wastewater treatment are relatively complicated and not fully understood
compared to many physical and chemical water treatment processes, although biological methods are
more effective and economical. These methods utilise bacteria, nematodes, or other microorganisms
for the decomposition of organic wastes via typical cellular processes. The intent of these biological
methods would be to create a system that enables the collection of the decomposition results for
proper disposal [3].
Adsorption
The focus of this experiment is based on the adsorption process for water treatment. This process
refers to the ability of retention of certain desired molecules (adsorbate) on a surface of a material
(adsorbent) in a more or less reversible manner [4]. A commonly-used adsorbent is activated carbon.
One form of activated carbon is granular activated carbon (GAC) that forms a filter bed through
which the water to be treated passes, while the impurities are adsorbed on the surfaces of the GAC [4].
Another form of activated carbon is powdered activated carbon (PAC), which will be mixed with the
solution to be treated for a short time period, then removed. During this mixing period is when
contaminants will be adsorbed [5].

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Figure 3: Infographic of Different Methods of Water Treatment.

Although commonly used as a process of water treatment, adsorption would be best suited when the
substance to be removed is sparingly soluble in water. A number of organic substances possess very
few ionizable groups per unit mass of substance, which will form hydrogen bonds with water
molecules. These hydrogen bonds are strong enough to retain organic molecules in the solution.
However, this could be overcomed by a good adsorbent that will reverse the solvation process. This is
due to the greater sum of all chemical bonds after adsorption than before adsorption [6].
Adsorption equilibria
During adsorption, adsorbates will coat the adsorbent surface until equilibrium is achieved between
the adsorbate molecules and the same type of molecules still present in the solution. Whether the
equilibrium could be achieved either with a single layer or multiple layers of the adsorbate on the
adsorbent, depends on the properties of both the adsorbate and adsorbent.
Obtaining the relationship between the adsorbate concentration in solution after equilibrium and the
quantity of adsorbate adsorbed per unit mass of adsorbent requires the plotting of an isotherm. To
construct an isotherm, a standard laboratory procedure could be carried out. Samples of wastewater
containing the adsorbate (may be a specific chemical compound or a group of compounds), are placed
into flasks and added to them are different quantities of adsorbent either in granular form or powder
form. The flasks are then shaken together in a device at constant temperature until all the contents of
the flask have reached equilibrium. This can be seen when the concentration of adsorbate no longer
changes with time. Then, a plot of adsorbate concentration in solution after equilibrium against the
quantity of adsorbate adsorbed per unit mass of adsorbent can be constructed.
One standardised isotherm model developed by Langmuir is as follows:
𝑞𝑚 𝐾𝑎 𝐶
𝑞= 1+𝐾𝑎 𝐶
(Eq. 1)
where 𝑞 is the mass of adsorbate adsorbed, 𝑞𝑚 is the mass of adsorbate adsorbed if a complete layer
of one molecule thick is adsorbed, 𝐾𝑎 is a constant and 𝐶 is the equilibrium concentration of
adsorbate in the solution [6].
Several assumptions of the Langmuir isotherm model are [6]:
1. Only a layer of adsorbate molecules will adsorb onto the adsorbent.
2. Adsorbate is immobile once adsorbed.

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3. Enthaly of adsorption for all adsorbate molecules are equal.

Factors affecting physical adsorption

An increase in temperature would decrease the degree of physical adsorption. At higher temperatures,
adsorbed molecules will have higher levels of vibrational energies, resulting in the molecules being
more likely to desorb from the surface of the adsorbent. The experiments in this report were done at a
stable ambient temperature in the laboratory so it can be said that the effect of temperature would be
negligible [5].

Figure 4: Factors Affecting Adsorption.

Typically, adsorption would increase with the increase in surface area of the adsorbent. This applies to
both the external surface area and the internal surface area of the adsorbent. However, large adsorbate
molecules will not be able to adsorb onto much of the internal surface area of the adsorbent. The
solution for this would be to reduce the particle size of the adsorbent [5].
Adsorption would also depend highly on the nature of the adsorbate-adsorbent bond. In a more
technical and quantitative term, it refers to the free energy of interaction between the adsorption sites
and the contact surface area of the adsorbed molecule [4].
The solvent molecules would also compete with the activated carbon surface to attract the adsorbent
molecules, proving that the type of solvent used would affect the degree of adsorption as well. It is
known that organic solvents would compete less with organic adsorbates compared to aqueous
solvents [5].
Researches have shown that it is possible to increase the degree of adsorption of organic adsorbates
onto carbon-based adsorbents using inorganic salts such as sodium chloride and sodium sulphate.
However, care should be taken to not add large amounts of inorganic salts during water treatment
indiscriminately. Appropriate amounts of organic ions adsorbed on the carbon-based adsorbent
surface will cause the repulsion force between adjacent organic ions on the adsorbent surface to be
decreased [5].
Nyex™, the absorbent
It is worth mentioning that despite its desirable properties, AC is expensive and frequently replacing
the saturated AC would be uneconomical. To circumvent this problem, AC would need to be
regenerated so that a continuous process can take place [4]. One way to do this is by supplying an

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electrical current to the GAC to oxidise the adsorbates on the surfaces of the AC [7]. Nyex™, the
carbon-based adsorbent in the Arvia Organics Destruction Cell (ODC), has a non-porous nature that
facilitates rapid adsorption of the contaminants [8]. It is also highly-conductive to facilitate the
passage of electric current across its surface for regeneration. Such characteristics reduce the time
needed for both equilibrium and regeneration to be achieved. A significant downside of Nyex™ is of
its reduced adsorbent capacity due to small internal surface area. Nyex™ is a graphite bi-sulphate
intercalation compound, made from flake graphite and a strong oxidising medium with sulphuric acid
present. To provide some context, graphite intercalation compounds are modified compounds of
graphite in which other chemical species have been inserted into the carbon layers of graphite,
resulting in increased distance between the carbon layers, while the characteristic planar structure of
graphite is maintained.
Activated carbon undergo two principal mechanisms to remove contaminants: adsorption and
catalytic reduction. A reason to why the adsorption mechanism is chosen for the activated carbon in
this experiment is for the removal of organic contaminants, for which the catalytic reduction
mechanism would be useless. Organic contaminants adsorb well onto activated carbon due to the
stronger attractive forces between the activated carbon surface (non-polar) and the contaminants (non-
polar), compared to that between the contaminant molecules and water molecules (polar) [9].
Spectrophotometry
Chemical compounds absorb, transmit or reflect light over specific ranges of wavelength. Via
spectrophotometry, the degree of absorbance of light of a certain wavelength can be determined by
measuring the intensity of light when the light beam passes through the sample solution [10].
Spectrophotometry is based on two laws, one of which is called Beer’s Law, which states that the
absorbance of a tested sample is linearly proportional to its concentration [10]:
𝐴 = 𝜀𝑐𝑋 (Eq. 2)
where 𝐴 is the absorbance of the sample, 𝜀 is the molar absorptivity, 𝑐 is the uniform concentration of
the sample, and 𝑋 is the path length where the sample solution is confined within.
This equation also states that it is possible to plot a straight line of 𝐴 against 𝑐. This plot is called a
calibration curve, and could be used in estimating the concentration of a sample solution. Beer’s Law
operates under a few assumptions [11]:
1. The radiation is monochromatic and strikes the cuvette at a normal incidence (90ᴼ).
2. Scattering and reflection of the radiation occurs at a minimal, so there are no uncompensated
losses.
3. No molecular interactions between the absorber and other molecules in the sample solution.

Dilution
Dilution, according to Chemistry-Dictionary.com, is the process in which the concentration of a solute
in a solution is reduced, typically done by adding and mixing the existing solution with more solvent
[12]. This concept was crucial in the experiments in this report for the construction of the calibration
curve that would enable the concentration of Acid Violet 17 solutions sampled throughout the
experiments to be easily estimated. The following equation was used:
𝐶1 𝑉1 = 𝐶2 𝑉2 (Eq. 3)
where 𝐶1 is the concentration of the stock AV17 solution, 𝑉1 is the volume of the stock solution used
to make the diluted solution, 𝐶2 is the final concentration of the diluted solution and 𝑉2 is the final
volume of the diluted solution [13].

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5. Methodology
Acid Violet 17 with a concentration of 200 mg L-1 was used in the experiment because the time taken
for this concentration to be cleared is sufficient to show the gradual change in concentration of acid
violet 17 through the process of fluidization, settling and regeneration. The concentration of Acid
Violet 17 discharged by Manchester Dyes Ltd is half of the experimental concentration used and it is
not suitable to be used because a concentration of 100 mg L-1 is cleared up in a short time in the Arvia
process. This would make it difficult to determine the effect of regeneration and fluidization time on
the change in concentration of dye.
A small volume of deionized water was initially added into the volumetric flask to avoid Acid violet
17 from sticking to the bottom of the flask, which would affect the concentration of solution produced.
Different concentrations of Acid Violet 17 within the range of 200 mg L-1 to 20 mg L-1, at every
interval of mg L-1 were produced and their corresponding absorbance was read using the spectrometer
so that a calibration line can be plotted. The graph is plotted to relate absorbance to concentration,
which is required to determine the unknown concentrations of dye samples taken from the Arvia rig
from their absorbance reading. A clean dropper was used every time a sample was taken and when the
sample was transferred from the centrifuge tubes to the cells to prevent cross contamination, which
would affect the concentration of sample read.
The Arvia rig has two compartments where one contains catalyst and the other compartment contains
Nyex 1000. The Nyex 1000 compartment is connected to an air pump and an external power supply is
connected to the cathode in the Nyex 1000 compartment and anode in the catalyst compartment. The
air pump was used to pump air through the Nyex 1000 in the dye solution to fluidize the Nyex 1000,
which promotes mixing of the adsorbent with the dye and facilitates the adsorption of organics on
adsorbent surface. The effect of fluidization time on the change in concentration of dye was
investigated to determine the optimum amount of time for maximum adsorption of dye. This can be
achieved by using fluidization time of 5 and 15 minutes, which is 5 minutes deviation from the
standard time, as this would give a range that takes both longer and shorter times into account. The
range could also indicate the saturation point of the adsorbent, which is the time when concentration
of dye does not change when mixing occurs. Any additional fluidization time beyond the time taken
for Nyex 1000 to be saturated is unnecessary and this reduces the amount of time it takes to clear the
dye. After fluidization, the air supply was switched off to allow sedimentation of Nyex 1000 due to
gravitational force. A compact Nyex 1000 bed reduces electrical resistance between electrodes
significantly. This is because when Nyex 1000 cluster together to form a bed, it has a high electrical
conductivity of 0.16 Ω−1 𝑐𝑚−1 , which improves electrochemical oxidation [3]. During regeneration,
Acid Violet 17, which is a triphenylmethane compound, is oxidized into carbon dioxide and hydrogen
gas, which is a harmless compound is produced at the cathode [3]. This removes the triphenylmethane
compound from saturated Nyex 1000, and the adsorbent is ready to be reused again. The current from
DC power supply was varied from the standard current of 1 Ampere to 0.5 and 2 Ampere to determine
the effect of the magnitude of current on the rate of regeneration of the adsorbent. If a lower current
can be used to achieve the same amount of regeneration over different periods of time, then the utility
cost of running the process can be lowered at the cost of more time required. Also, the amount of time
used for regeneration is also varied from standard time to 3 and 7 minutes to determine the
relationship between regeneration time and the amount of adsorbent regenerated. This relationship is
important as it indicates the optimum time for regeneration where all of the dye compounds have been
removed from the adsorbents, and this could reduce overall time taken for the treatment of dye.
The samples collected from the Arvia rig have to be centrifuged using a centrifuge before their
reading is taken by the spectrophotometer. During fluidization, the adsorbent is well mixed with the
dye, causing them to be collected together in the sample. A centrifuge is used to separate the mixture
of dye solution from Nyex 1000 collected in the centrifuge tubes because presence of Nyex 1000

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would affect the amount of absorbance of light in the spectrophotometer and hence affect the
concentration of dye obtained. The centrifuge will spin the tubes at high speed of 5000 rpm to create a
strong centripetal force that will cause the denser material, which is Nyex 1000 to move outwards,
hence they accumulate at the bottom of the tube [1]. However, diluted solutions used for calibration
does not need to be centrifuged as they do not contain Nyex 1000.
67 Series Spectrophotometer measures the absorbance of light at a wavelength of 540 nm by the
sample when a beam of radiation is passed through the dye sample. The reference point for the
spectrophotometer is taken with pure deionized water, which gives each sample reading an
absorbance value relative to deionized water, where absorbance is taken as zero. To ensure that the
results are accurate and consistent, reference point is always taken at pure deionized water before
another sample was read. Depending on the sample, different amount of light may be absorbed and
this is calculated from the negative logarithm of the difference between the intensity of light exiting
and entering the dye sample [2]. The calibration line gives the corresponding concentration of dye
sample from their absorbance value given by the spectrophotometer. The change in concentration of
dye with time is used to determine the effect of varying the magnitude of current, regeneration time
and fluidization time on the overall water treatment process.

6. Core Work
The experimental procedure can be divided into four main parts: sample preparation, dilution for the
calibration curve, the Arvia process, and spectrophotometry.
Preparation of 200 mg L-1 of Acid Violet 17
400 mg of Acid violet 17 was weighed on an electronic balance and poured into a 2 L volumetric
flask which contains a small volume of deionized water initially. The flask was swirled to dissolve the
Acid Violet 17 and deionized water from the dispenser was added until the level was near the
volumetric mark. Then a dropper was used to add deionized water carefully until it reached the
2 𝐿 mark on the volumetric flask.
Dilution of 200 mg L-1 of Acid Violet 17
To dilute the solution to 20 mg L-1, a 50 mL measuring cylinder was used to measure out 5 mL of 200
mg L-1 of Acid Violet 17. A dropper was used to add deionized water into the measuring cylinder until
the level of solution reaches 50 mL. The dilution step was repeated to produce different
concentrations of 40, 60, 80, 100, 120, 140, 160, and 180 mg L-1by varying the volume of 200 mg L-
1
Acid Violet 17. 5 mL of each solution with different concentration from the range of 20-200 mg L-
1
was measured into centrifuge tubes with a dropper.

Figure 5: Infographic of the Arvia Process.

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Figure 6: The Arvia Process Experiment Set-Up.

The Arvia process
2L of 200 mg L-1 Acid Violet 17 was poured into the Arvia rig, the pump was turned on and the
stopwatch was started. A 5 mL sample was taken from the Arvia rig and added into a centrifuge tube
with a dropper immediately after the stopwatch was started, and this step was repeated at every 2
minute interval throughout the experiment. The experiment was initially carried out at standard
conditions with fluidization time of 10 minutes. Then, the pump was turned off and the Nyex 100 was
allowed to settle for two minutes. After the settling time, the power supply was turned on and the
current was set at 1 Ampere for 5 minutes for the regeneration of Nyex 100. After turning off the
power supply, the process of fluidization, settling and regeneration was repeated until the solution in
the Arvia rig was clear. The water treatment procedure was repeated with one of the conditions varied
in each case, while other parameters were set at standard conditions. This was carried out with 5, 15,
and 20 minutes fluidization time, a current at 0.5 and 2 A, and with 3 and 7 minutes regeneration time
for Nyex 1000.

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Spectrophotometer readings The spectrophotometer was turned on and the photometric option was
selected, where the wavelength was set to 545 nm. Deionized water was filled into a cell with a
dropper and was placed into a cell holder at the back of the spectrophotometer, where the direction of
the clear side of the cell with a triangle was facing the right side. The zero button was selected on the
spectrophotometer. A clean cell was filled with a sample of 200 mg L-1 of Acid Violet 17 from a
centrifuge tube with another clean dropper. After calibration of the spectrophotometer, the cell with
deionized water was removed and was replaced with the cell filled with the sample of 200 mg L-1. The
read button was selected and the absorbance reading on the spectrophotometer was recorded. This was
repeated for diluted solutions of Acid Violet 17 at 20, 40, 60, 80, 100, 120, 140, 160, and 180 mg L-1.
Zero reading on the spectrophotometer was taken with the deionized water cell each time before
another sample reading was taken. The tubes containing samples from Arvia rig were placed into a
centrifuge, which was set to 5000 rpm with a capacity of 16 tubes. After the samples in the centrifuge
tubes were centrifuged, the process of calibrating, filling a cell with the sample and recording the
reading of the sample were repeated for all the tubes containing samples from obtained from 2
minutes interval throughout each experiment.

Figure 7: The centrifuge machine.

8. Hazards
Ensured that any spillage of Acid Violet 17, Nyex 1000 or water was cleaned up immediately to avoid
slipping. Ensured that safety goggles, laboratory coat and rubber gloves were worn at all times to
protect skin and eyes from Acid Violet 17 and Nyex 1000 dust, which can cause irritation. Handled
Nyex 1000 with care especially around electrical items such as DC power supply and the sockets
because Nyex 1000 is electrically conductive. Ensured that hands or gloves were not wet when using
electrical equipment such as power supply, Centrifuge, and Spectrophotometer to prevent
electrocution from occurring. Was aware that one of the by-products of electrochemical process is
Hydrogen gas, which is very flammable and could form explosive mixture in air and made sure that
the experiment was carried out in a well ventilated area.

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9. Observed Data
9.1 Observed Data
The first step of the experiment is to collect data to plot a calibration curve to correlate absorbance in
relative to the concentration of dye in the deionized water. The results are collected by varying
different concentration of dye from 0 𝑚𝑔 𝐿−1 to 200 𝑚𝑔 𝐿−1 with a step size of 20 𝑚𝑔 𝐿−1 (Table 1).
The calibration curve is plotted with the data collected (Figure 8), with a line of best fit going through
the origin. To make calculating the concentration easier, an equation for the curve is derived (𝐶 =
63.221𝐴𝑏 ). After plotting the calibration curve, it is then time to perform an experiment with the
standard conditions, they are: starting with 10 minutes of fluidization, then sedimentation for 2
minutes, then start regeneration at a current of 1A for 5 minutes, repeat the steps until the fluid is clear
(Table 2).

Table 1: Relative Absorbance data collected from various concentrations of dye.

Concentration / 𝑚𝑔𝐿−1 Relative Absorbance
0 0.000
20 0.246
40 0.483
60 0.812
80 1.295
100 1.472
120 2.037
140 2.321
160 2.607
180 2.877
200 3.000

250

200
C = 63.221Ab
Concentration (mg L-1)

150

100

50

0
0.000 0.500 1.000 1.500 2.000 2.500 3.000 3.500
Relative Absorbance

Figure 8: Calibration Curve plotted from data of concentration and relative absorbance.

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Group B18

Table 2: Data collected from the experiment with standard conditions.

Time / Concentration / Time / Concentration /
𝑚𝑖𝑛𝑢𝑡𝑒𝑠 Absorbance 𝑚𝑔𝐿−1 𝑚𝑖𝑛𝑢𝑡𝑒𝑠 Absorbance 𝑚𝑔𝐿−1
0 2.477 156.60 36 0.555 35.09
2 1.926 121.76 38 0.590 37.30
4 1.919 121.32 40 0.501 31.67
6 1.741 110.07 42 0.423 26.74
8 1.744 110.26 44 0.455 28.77
10 1.612 101.91 46 0.445 28.13
12 1.702 107.60 48 0.488 30.85
14 1.683 106.40 50 0.462 29.21
16 1.731 109.44 52 0.470 29.71
18 1.270 80.29 54 0.203 12.83
20 1.069 67.58 56 0.177 11.19
22 0.998 63.09 58 0.179 11.32
24 0.902 57.03 60 0.181 11.44
26 1.116 70.55 62 0.197 12.45
28 1.040 65.75 64 0.331 20.93
30 1.139 72.01 68 0.223 14.10
32 0.991 62.65 70 0.111 7.02
34 0.753 47.61 72 0.090 5.69

180.00

160.00

140.00

120.00
Concentration (mg L-1)

100.00

80.00

60.00

40.00

20.00

0.00
0 10 20 30 40 50 60 70
Time

First Cycle Second Cycle Third Cycle Fourth Cycle

Figure 9: Graph of Absorbance vs Time plotted from the standard conditions.

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Group B18
With the data in hand, a graph is then plotted and an equation of the curve is generated based on the
trend (Figure 9).
For the standard experiment, four batches of reaction have been done to purify the water. In this case,
each batch reaction are 17 minutes each (including fluidization time, settling time and regeneration
time). The trend can be seen for each cycle of reaction. However, the steepness of the curves for each
batch seems to be decreasing as the reaction goes on, see figure 9 above.

180

160

140
Concentration (mg L-1)

120

100

80

60

40
y15 = 151.6e-0.022t
20
y5 = 145.6e-0.055t y10 = 156.6e-0.039t
0
0 10 20 30 40 50 60 70 80 90 100
Time (minutes)

Fluidization Time = 5minutes Fluidization Time = 15minutes

Fluidization Time = 10 minutes Expon. (Fluidization Time = 5minutes)
Expon. (Fluidization Time = 15minutes) Expon. (Fluidization Time = 10 minutes)

Figure 10: Graph of Absorbance vs Time for different fluidization time.

The steps are then repeated by varying either the fluidization time, the regeneration time, and the
current. A graph of absorbance vs time is plotted for different fluidization time (5 minutes, 10 minutes,
and 15 minutes) (Figure 10). Equations of the trend line are generated to ease the process of finding
the concentration at a specific time.
A graph of absorbance vs time is also plotted for different current (0.5A, 1A, and 2A) (Figure 11).
Lastly, a graph of absorbance vs time is plotted for different amount of regeneration time (3 minutes,
5 minutes, and 7 minutes) (Figure 12). The experiment for 7 minutes of regeneration stopped halfway,
due to the fact that the concentration of the dye is observed to changing too slow, hence it would be
impractical to continue. Then, calculations are done based on the equation generated to find the time
required to get a fluid of 1𝑚𝑔𝐿−1 for different parameters (different fluidization time, different
magnitude of current, and different regeneration time).

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Group B18

180.00

160.00

140.00
Concentration (mg/L)

120.00 y2 = 162.64e-0.042t

100.00

80.00

60.00

40.00 y1 = 156.6e-0.039t
20.00
y0.5 = 90.46e-0.042t
0.00
0 10 20 30 40 50 60 70 80
Time (minutes)

Current = 2A Current = 1A Current = 0.5A

Expon. (Current = 2A) Expon. (Current = 1A) Expon. (Current = 0.5A)

Figure 11: Graph of Absorbance vs Time for different magnitude of current.

180

160

140
Concentration (mg L-1)

120

100

80

60

40
y15 = 151.6e-0.022t
20
y5 = 145.6e-0.055t y10 = 156.6e-0.039t
0
0 10 20 30 40 50 60 70 80 90 100
Time (minutes)

Fluidization Time = 5minutes Fluidization Time = 15minutes

Fluidization Time = 10 minutes Expon. (Fluidization Time = 5minutes)
Expon. (Fluidization Time = 15minutes) Expon. (Fluidization Time = 10 minutes)

Figure 12: Graph of Absorbance vs Time for different amount of regeneration time.

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Group B18
9.2 Derived Data

Table 3: Table of Calculation for the amount of time required for 2 litres of purification of water
and its number of cycles respectively.
Fluidization Regeneration Current Time Required / Number of Cycles
Set-Up Time / minutes Time / minutes /A hours Required
1 5 5 1 1.51 8
2 10 5 0.5 1.79 6
3 10 5 2 2.02 7
4 10 5 1 2.16 8
5 10 3 1 2.37 9
6 15 5 1 3.80 10
7 10 7 1 5.66 18

The time required to purify the solution to 1𝑚𝑔𝐿−1 concentration is calculated for each set-up based
on the equation that has been derived for each experiment. Although the equation derived might not
exactly describe the trend, it serves as a good approximation to determine the time required to get the
concentration required. These times required are tabulated above (Table 3) for each set-up conditions.
The rates for electricity consumption can be calculated for each set-up to determine the feasibility and
the cost for each set-up (Table 4). A few assumptions are made in order to calculate the cost incurred
for the purification of 7000 L of wastewater, they are: Assuming the price of Electricity for Industrial
uses to be 12.58p/kWh [1], the power output for a common fluidized bed reactor is 140 Watt [2], the
voltage used is constant throughout the experiment and is equal to 5V, and the plant operates 24 hours
a day. The cost is calculated and tabulated below for economic analysis of the feasibility and the
optimum set-up is considered based on the cost and the efficiency of the set-up.

Table 4: Tabulated Data for the Calculation for Cost Estimation for Economic Evaluation.
Total Power
Consumption
for All Cycles
Amount for 7000
of Water Power Power Litres of
Total Time Number of Each Consumption Consumption Water for Total Power
Required for Reactors Reactor for for each Reactor Consumption
7000 L / Required Purifies / Fluidization / Regeneration / per Day / for Every Total Cost /
hours for 7000 L litres kWh kWh kWh Reactors £
5282.67 221 31.67 0.012 0.00042 1.44 319.1611111 40.15
6256.83 261 26.82 0.023 0.00021 1.99 519.8692402 65.40
7071.75 295 23.73 0.023 0.00083 2.04 603.1786765 75.88
7558.83 315 22.22 0.023 0.00042 2.01 633.6080882 79.71
8285.67 346 20.23 0.023 0.00025 2.26 781.6145556 98.33
13314.00 555 12.61 0.035 0.00042 2.32 1286.011364 161.78
19810.00 826 8.47 0.023 0.00058 1.81 1496.176316 188.22

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Group B18

25000.00 200.00
180.00
20000.00 160.00
140.00
15000.00 120.00
Hours

100.00

£
10000.00 80.00
60.00
5000.00 40.00
20.00
0.00 0.00
1 2 3 4 5 6 7
Axis Title

Total Cost Total Time Required For 7000 Litres

Figure 11: Cost and Time required for each set-up.

As can be seen from Figure 11, set-up 1 requires the least amount of time and cost. The trend is the
longer it takes, the more power is consumed and more number of reactors are required for 7000 litres
of water purification, and hence the amount of cost incurred is higher.
References for Derived Data:

[1]https://www.gov.uk/government/statistical-data-sets/gas-and-electricity-prices-in-the-non-
domestic-sector

[2]https://www.alibaba.com/product-detail/laboratory-fluidized-bed-glass-
reactor_60503327389.html

10. Calculations
10.1 Derived Data Calculations
The following section provides specimen calculations for the derived experimental data.
A solution of AV17 dye dissolved in water with a concentration of 200 mg L -1 were diluted with
different volumes of water to prepare the calibration samples with varying concentrations. Equation 3
is used to determine the volume of water required to dilute the 200 mg L-1 AV17 dye solution into the
desired concentration for a volume of 50 mL. For instance, for a diluted concentration of 120 mg L-1:
𝐶1 = 𝐶2 𝑉2 /𝑉1
𝐶2 𝑉2 120 𝑚𝑔 𝐿−1 × 0.05 𝐿
𝑉1 = = = 0.03 𝐿 ≈ 30 𝑚𝐿
𝐶1 200 𝑚𝑔 𝐿−1
The absorbance detected by the spectrometer is converted into concentration by using the best-fit line
equation of the calibration curve (Figure 8). For instance, from the results in Table 2 at time = 0 min:
𝑚𝑔
𝐶 = 63.221𝐴𝑏 = 63.221 × 2.477 = 156.60 𝑚𝑔 𝐿−1
𝐿

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Group B18
10.2 Error Calculations
The y-error bars corresponding to the uncertainty of concentrations in Figure 8 are derived from
propagation of errors. The concentration is calculated by Equation X, and so the propagated errors are
calculated as follows:
1/2
∆𝐶2 2 ∆𝑉2 2 ∆𝑉1 2
∆𝐶1 = 𝐶1 × (( ) +( ) +( ) )
𝐶2 𝑉2 𝑉1

For instance, for C= 80 mg L-1:

2 1/2
𝑚𝑔 ±0.001 𝑚𝑔 𝑚𝐿−1 ±1 𝑚𝐿 2 ±1 𝑚𝐿 2
∆𝐶1 = 80 × (( ) +( ) +( ) ) = ± 4.32 𝑚𝑔 𝐿−1
𝐿 0.2 𝑚𝑔 𝑚𝐿−1 50 𝑚𝐿 20 𝑚𝐿

The y-error bars representing the uncertainty of concentrations in Figures 9, 10, 11, and 12 are derived
from propagating the error of the absorbance recordings.
𝑚𝑔
∆𝐶 = 63.221 × ∆𝐴𝑏 = 63.221 × ± 0.001 = ± 63.221 × 10−3 𝑚𝑔 𝐿−1
𝐿
11. Conclusions
11.1 Interpretation of Results and Comparison with Theory
Overall,
The calibration curve depicted by Figure 8 shows a linear relationship between absorbance and
concentration. The linear relationship is justified by Beer’s law (Eq. 1). Figure 1 plots concentration
as a function of relative absorbance, with a best-fit line equation of C = 63.221Ab. This function is
1
simply a rearrangement of Beer’s Law, with the slope of 63.221 corresponding to 𝜀𝑋 . The best-fit line
equation is used for deriving the sample concentrations based on the absorbance recorded by the
spectrometer. The first data point corresponding to 0 absorbance at 0 mg L-1 concentration is
reasonable since it is pure water, and therefore no light in the spectrometer is absorbed by the dye.
However, not all the data points in Figure 1 are perfectly aligned with the linear curve, indicating
random errors in the experiment. Conducting more trials of the experiment and averaging the
observations would diminish the effect of random errors on the experimentally derived linear best-fit
line equation. Section X further evaluates the effects of errors on this experiment.
In general, there is a decaying trend of the AV 17 concentration in the as a function of time in this
batch Arvia Water Treatment process. An example of the trend is illustrated in Figure 9. The observed
continuous decay in concentration of AV 17 throughout a number of cycles justifies the ability of
Nyex to undergo multiple cycles of adsorption and regeneration with minimal reduction in its
adsorptive capacity.
https://www.dropbox.com/s/ii4g1de9emaxl21/Adsorption%20of%20Organics%20in%20Wastewater
%20on%20NYEX%20and%20Electrochemical%20Regeneration%20-
%20Development%20of%20a%20Process.pdf?dl=0
Literature findings also observe a relatively stable trend for the regeneration efficiency (90-100%) of
Nyex after multiple cycles of adsorption and regeneration.
https://www.escholar.manchester.ac.uk/api/datastream?publicationPid=uk-ac-man-
scw:283011&datastreamId=FULL-TEXT.PDF# pg 105

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Group B18
The AV 17 concentration decays with a relatively steep slope during the fluidization process. It then
decelerates during sedimentation and becomes gradually constant during the regeneration process.
The concentration declines at its fastest rate during the fluidisation period because the Nyex particles
are being distributed and agitated throughout the solution. This increases the active contact area
between Nyex and AV 17 dye in the solution, which effectively improves the adsorption rate. As the
Nyex particles settles and begins reforming the bed in the sedimentation period, the active contact
area of Nyex with AV 17 dye decreases, consequently declining the adsorption rate. During the
regeneration period, the electric current passing through the Nyex bed removes and destroys the
adsorbed AV 17 dye, which is why the AV 17 concentration of the solution remains relatively
constant. Despite not producing a smooth decay curve between cycles, the decay in concentration of
an entire experiment batch can be approximated with an exponential best-fit line. The exponential
best-fit line equations are useful to generalise the rate of decay and predict the times required to
achieve an AV 17 dye concentration of 1 g L-1 for each tested conditions.
The experimentally derived data depicted in Figure 3 illustrates the comparison of treatments with
varying fluidisation times. A shorter fluidisation time (5 minutes) yields a steeper slope, whereas a
longer fluidisation time (15 minutes) shows a more gradual decay. The observed trend indicates that a
shorter fluidisation time enables the removal of AV 17 dye to be achieved at a faster rate. This
contradicts literature that observes an increase in AV 17 dye removal with increasing agitation time,
which in this case corresponds to the fluidisation time (R.SIVARAJ REFERENCE).With a longer
period of fluidisation, the effective contact time for adsorption between AV 17 and Nyex particles
should have increased, and therefore should have contributed to an improvement to the rate of AV 17
removal. However, the experiment results show otherwise. A reason for this might be that the
maximum adsorption capacity of Nyex had already been achieved by using 5 minutes fludisation time.
As a result, increasing the fluidisation time does not allow more AV 17 to be adsorbed. This prolongs
the fluidisation process more than the effective period required, consequently making the process less
time-efficient. However, it is observed that the slopes of the three experiment curves have already
been distinct since the initial period (from t = 0 – 5 minutes), despite in theory it should be similar
because all three experiments held the same conditions during this period. This indicates potential
random errors in the experimental data, which may have been cause by not regenerating in between
experiment sets. Section X further evaluates random errors.
Figure 10 compares the effect of varying currents to the removal of AV17 dye. It is observed that a
higher current produces a steeper decay, and thus a faster rate of AV17 dye removal. However, it
must be noted that there is only a minor difference in rate between the experiment using a current of
2A and 1A.
https://www.dropbox.com/s/ii4g1de9emaxl21/Adsorption%20of%20Organics%20in%20Wastewater
%20on%20NYEX%20and%20Electrochemical%20Regeneration%20-
%20Development%20of%20a%20Process.pdf?dl=0 (Figure 9.4)
http://ac.els-cdn.com/S0013468604002804/1-s2.0-S0013468604002804-
main.pdf?_tid=a4825aa2-04fd-11e7-ba17-
00000aacb362&acdnat=1489087489_6cbae3ba308847db0efd4f26cc30bad6 (Fig. 5) !!! Some
useful info
According to a research by Nigel Brown, the
regeneration efficiency approaches a
maximum after a certain charge density. The
regeneration efficiency is the adsorptive
capability of regenerated in ratio to new Nyex
tested under the same conditions. The
experiment data coupled with this literature

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knowledge implies that an increase in current from 1A to 2A does not have a significant impact on the
regeneration efficiency and consequently the rate of AV17 dye removal, which is because the charge
density approaches its maximum regeneration efficiency. However, it is observed that the starting
concentration of the experiment set with 0.5 A current starts at 90.46 mg L-1, which is substantially
lower than the starting concentrations of other experiment sets (~160 mg L-1). This is a significant
indication of random error in this particular experiment set, which most likely occurred during the
sample preparation stage. Despite an initial concentration that is off, the rate of decline in
concentration for the experiment set with 0.5 A current is still reasonable because it is slower than the
rates for 1A and 2A.
From the experiment findings in Figure 10, it can be deduced that an increase in current densities
improves the time efficiency of the treatment process to a certain extent, which relates to the findings
from literature (reference). However, using higher currents require higher power consumption. Thus,
it is important to select a current density with the best trade-off between the costs of power utility and
time efficiency. With the basis of a constant cell voltage, the power consumption of using 2A current
is twice than using 1A. In the scale of this experiment, assuming a cell voltage of 5V and average
household price of electricity at 14 pence/kWh, it costs 0.14 pence to reduce the AV17 concentration
to 1g/L using 1A current, whereas it costs 0.30 pence using 2A current. This means that the cost of
using 2A current is approximately 110% more expensive than using 1A. Therefore, for this
experiment, 1A current is the more economically efficient and sensible option.
Based on Figure 11, there is only a minor difference in the rate of AV17 dye concentration removal
between the experiments using a 3 minutes and 5 minutes regeneration time. A research by Dun Liu
suggests that the regeneration efficiency also approaches maximum after a certain regeneration time.
The minor difference in rate of AV17 between 3 and 5 minutes regeneration time can therefore be an
indication that this period of regeneration time approaches the time corresponding to maximum
regeneration efficiency. Increasing the regeneration time beyond a certain point does not improve the
adsorbing capacity and consequently also the removal efficiency.
https://www.escholar.manchester.ac.uk/api/datastream?publicationPid=uk-ac-man-
scw:283011&datastreamId=FULL-TEXT.PDF
It is also observed that the decline in AV17 dye concentration of the treatment with a regeneration
time of 7 minutes is substantially slower than treatments using 3 minutes and 5 minutes regeneration
time. Due to time constraints, the experiment was ended mid-way. If the trend continues at that rate, it
will take a significantly long period for the AV17 dye concentration to drop below 1 g L -1, which is
inefficient and impractical especially if applied to an industrial scale. It is a reasonable observation
that the AV17 dye removal process takes longer with 7 minutes regeneration time because 7 minutes
regeneration time may have well exceeded the effective time corresponding to the maximum
regeneration efficiency. Due to this, an excess regeneration time causes a reduction in time-efficiency
because it is prolonging the process beyond the necessary effective duration. However, in the period
between t = 0 min to t = 12 min, the process was fluidisation and settling, which supposedly held the
exact same conditions for all three experiments with different regeneration times. This should have
resulted in a similar initial slope during this period for all three experiment sets. However, it is clearly
seen that the initial decay (until t = 12 min) for 7 minutes regeneration time was already substantially
slower than the other two experiment sets. This deviation, similar like to that of Figure 10, is an
indication for random error in the experiment.
Based on the exponential best-fit line equations, the times required to reduce the AV17 dye
concentration to 1 g L-1 for each experiment set-up conditions were extrapolated and tabulated in
Table 3. The fastest time corresponds to Set-Up 1, which is for 5 minutes fluidization time, 1A current,
and 5 minutes regeneration time. In contrary, the slowest time corresponds to Set-Up 7, with the
conditions of 10 minutes fluidization time, 1A current, and 7 minutes regeneration time. Further

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Group B18
deductions made on the basis of several assumptions also enabled an estimated economic evaluation
to be derived, which is tabulated in Table 4. The results also show that Set-Up 1 is the most
economically efficient set-up to treat 7 m3 of waste water, whereas Set-Up 7 is the least economically
efficient

 https://www.escholar.manchester.ac.uk/api/datastream?publicationPid=uk-ac-man-
scw:283011&datastreamId=FULL-TEXT.PDF pg 105
 Efficiency of Nyex compared to GAC http://waset.org/publications/8027/development-of-
composite-adsorbent-for-waste-water-treatment-using-adsorption-and-electrochemical-
regeneration
 http://www.jese-online.org/Articles/OLF/jESE_0019.pdf
 http://ac.els-cdn.com/S0013468605014106/1-s2.0-S0013468605014106-
main.pdf?_tid=b2f1930a-04fd-11e7-807a-
00000aab0f6c&acdnat=1489087513_78d77703640eaa6f4c9e8ff6da35a23a
 http://www.sciencedirect.com/science/article/pii/S0043135411001345 continuous water
treatment
 https://www.escholar.manchester.ac.uk/api/datastream?publicationPid=uk-ac-man-
scw:283011&datastreamId=FULL-TEXT.PDF

11.2 Limitations and Suggestions for Improvements

Uncertainties and deviations in experimental data represent errors in the experiment. The digital
scales of the digital balance, spectrometer, stopwatch, and ammeter are sources of systematic error.
Table ? tabulates the systematic errors corresponding to equipment used in the experiment.
Table 5 - Systematic Errors of Equipment

Equipment Variable Uncertainty

Digital Balance Mass ± 0.001 g
Spectrometer Absorbance ± 0.001
Stopwatch Time ±1s
Ammeter Current ± 0.1 A
Measuring Cylinder Volume ± 1 mL

When preparing the calibration solutions, parallax error occurs when taking readings from the
measuring cylinder. Parallax error can be reduced by having a second individual to check the reading
and taking repeated measurements. Inadequate calibration of the spectrometer is also a source
systematic error that affects the absorption readings. The analogue scale of the measuring cylinder
also imposes systematic error. Systematic errors affect the accuracy of experimental data and can be
reduced by calibrating the equipment and opting for equipment with better scales.
Random errors affect the precision of experimental data and are sourced from unpredictable
fluctuations in the experiment conditions. For this experiment, a number of random errors are
observed and are explained below.

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The AV17 dye solution was prepared by weighing a relatively exact 0.4 g mass of AV17 dye powder
and dissolving it into deionised water. However, there were residual traces of AV17 dye powder on
the plastic sheet and in the volumetric flask used for sample preparation, indicating that not the entire
0.4 g mass of AV17 dye powder were mixed into the solution. Although minor, this is a potential
source of random error because it affects the concentration of the AV17 dye solution actually being
treated in the Arvia process. Furthermore, the AV17 dye solution was not thoroughly mixed during
the sample preparation process. This leads to a non-homogenous mixing and varying concentrations
throughout the solution. Nevertheless, it is expected that the fluidisation stage will promote the
general mixing of the solution.
Due to the limited availability of resources, the pipettes, sample tubes, and spectrometer vials, were
reused throughout the experiment, only being rinsed with water after each use. This implies that they
were not completely sterile for next usages, leading to contamination and affecting the concentrations
of the latter sample intakes, which is leads to random errors in the absorbance data.
When pipetting the samples from the rig during fluidisation mode, some Nyex are inevitably carried
along with the sample. This would affect the absorbance level of the solution detected by the
spectrometer. Also, the absorbance of the samples was not immediately measured, since it needs to
undergo centrifugation and also wait for the availability of the spectrometer. This time delay enables
the residual Nyex on the surface of the sediment in some of the samples to continue adsorbing the
AV17 dye as much as it can hold, altering the actual concentration from when the sample was initially
pipetted. These two points are random errors affecting the detected absorbance of the samples.
Furthermore, the samples are designed to be taken every 2 minutes. However, there were instances
when there is a time delay from human response when taking these samples, which is a source of
random error. The same human error also applies when switching modes such as from fluidisation to
settling, or settling to regeneration, or regeneration to fluidisation. Thus, the systematic error of time
from the stopwatch (± 1 s) is minor in comparison with the random error sourced from time delay of
human response, which can range between ± 10 - 20 s.
Upon completion of an experiment set, the treated AV17 solution was syphoned from the rig, saving
the Nyex bed for subsequent experiments. However, the solution was never well syphoned from the
rig, resulting in some volume to remain in the rig. This residual volume will contaminate the
concentration of the solutions prepared for subsequent experiments, which is a source of random error.
Since the Nyex bed is reused for all experiment sets, another source of random error is not
regenerating the Nyex bed in between experiment sets because not all the experiments were finished
during the regeneration phase. Due to this, some Nyex particles are still covered in traces of AV17,
which decreases its adsorptive capacity at the start of the latter experiment set. Although a very low
concentration of AV17 is expected at the end of each experiment, and so the effects of residual AV17
in subsequent experiments are minor, actions still need to be taken to tackle this random error.
Therefore, it must be ensured in the experiment design that the Nyex bed should always be
regenerated between experiment sets. Another better but more costly option would be to use a fresh
bed of Nyex for each experiment set.
Other unpredictable fluctuations in the environment conditions may also have been sources of random
error. Due to time constraints, the experiment was only performed once, which means that there is
only one set of data recorded. This limits the ability to quantify random errors and analyse precision
in the experimental data. Repeating trials of the experiment would generate more sets of observed
data, which enables better statistical evaluation of random errors, reduces the effect of random errors,
and improves data precision.

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Gaps in the Nyex bed leads to ineffective regeneration because the electric charge are not conducted
homogeneously throughout. This is a source of random error because some Nyex are not regenerated
and so has residual AV17 dye still adsorbed on the surface of the particles.

Nomenclature:

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