Juan Mabille

Group B11:
Thomas Moore,
Jude Allen,
Mason Budd and
Juan Mabille
(and for this
experiment only
– Sarah Al
Binsaad).

Electrochemical water treatment

Experiment 3
Group: B11 Experiment 3: Electrochemical Water Treatment 20/10/2022

Experiment 3:
Electrochemical Water Treatment
1.0 Abstract
This experiment shows the effects of fluidization time, regeneration time, and current on the
concentration of acid violet. This was done using Nyex to adsorb the acid violet during fluidization,
then the Nyex would settle to the regeneration zone and a DC power supply was used to regenerate
the Nyex before fluidization again.

For this experiment we first needed to obtain our calibration curve. We prepared a 1L 30mg/L
solution of Acid Violet with Distilled Water. Using this we then diluted it to obtain a range of more
dilute solutions which were all then tested in the UV-Vis spectrometer where absorbance was
measured. This gave our concentration vs absorbance curve.

A 2-litre solution of acid violet at 30mg/L was prepared and poured into the main circulation zone.
Samples were taken every 3 minutes from the circulation zone and then placed in the centrifuge for
8 minutes.

The experimental samples were then also tested in the UV-Vis spectrometer. We compared this with
the calibration absorbance curve which allowed us to determine the concentration of the samples at
any point in time based on the absorbance.

2.0 Context
2.1 Aims and learning outcomes
The aims of the experiment were to purify a solution of acid violet using Nyex in a Y-cell, and
investigate the best way to maximise the rate of change of acid violet concentration, through
variation of factors such as:

• Fluidization time

• Regeneration time

• Current

2.2 Theory
Electrochemical water treatment is a technique that utilises an absorbent to purify effluents through
several cycles of adsorption and electrical regeneration [1,2]. After mixing the effluent and the
absorbent, the pollutants are adsorbed by the adsorbent. The contact between absorbent and
pollutants is increased by using an air pump to improve the efficiency of the adsorption process. In
this experiment, Nyex 1000TM was used, which is a non-porous, highly conductive graphite-based
adsorbent material. Due to its non-porous nature, Nyex has a low adsorbent capacity [4]. However,
the overall efficiency of the treatment is improved by multiple cycles of adsorption. Once Nyex is
fully loaded, it is treated by electricity to restore its adsorbent capacity. In this experiment, Nyex is
processed by anodic regeneration whereby the contaminants captured by the adsorbent are
oxidised by being exposed to an electrical current. Hence, the charged contaminants are released
into the electrolyte after the removal of the electric field [5].

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 Group: B11 Experiment 3: Electrochemical Water Treatment 20/10/2022

2.3 Relevance
The amount of industrial wastewater increased as the chemical processing industry has expanded
over the years. Industrial effluents usually contain diverse types of organic and inorganic pollutants.
They result from various industries such as plastics production, petroleum products,
pharmaceuticals, paint, resins, paper, and disinfectants [1]. Since those pollutants can affect the
surrounding water resources causing severe damage to human health and the environment, water
treatment technologies have been vital to the chemical engineering industry [2-4].

Adsorption technology has been widely used for effluent treatment in the past two decades because
of its affordability and simplicity [2,3]. Once the adsorbent is exhausted, it can be discarded, which is
not economically feasible or environmentally friendly. Therefore, a better alternative was to
regenerate the adsorbent by means of thermal, microwave, ultrasound, biological and
electrochemical processing [3]. Although thermal regeneration is the most common method in the
industry, it is not practical for treating large amounts of effluents since it requires high energy
consumption and causes adsorbent loss due to oxidation [4].

As for electrochemical regeneration, studies on activated carbon, a conventional adsorbent, have

achieved regeneration efficiencies from 70 to 95 % [2]. However, due to the porous nature and poor
conductivity of the activated carbon, the process required a long regeneration time making the
process unfeasible. As a result, a new non-porous, highly conductive graphite-based adsorbent
material was developed, such as Nyex 1000 TM, which is a flake graphite intercalation compound (GIC)
[1]
. Nyex 1000TM has a very low specific surface area of around 1.0 m 2 g-1, which can reduce the
adsorption and regeneration time due to its high intraparticle diffusion [1,4], making the overall
process feasible. Furthermore, Nyex has been commercialised by Arvia Technology Ltd. as a cost-
effective material for various effluents and waste treatment applications [2].

3.0 Experimental work

3.1 Equipment and procedure

Equipment:

Circulation Zone
Electrolyte

Cathode Regeneration Zone

Anode
Power Supply

Air Pump

Figure 1: Y cell

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Group: B11 Experiment 3: Electrochemical Water Treatment 20/10/2022

The Y cell was approximately 1m tall and slightly less than 1m wide at its widest point. The
wastewater containing the dye was in the circulation zone as shown along with the Nyex. The
electrolyte was in a separate zone to the side of the circulation zone. The power supply provided a
current to the Nyex to regenerate it and separate the dye. This current was varied to find the best
value for regeneration and therefore dye separation from the wastewater. The air pump also helped
increase the degeneration of Nyex.

Figure 2: Centrifuge Figure 3: UV-vis Spectrometer

The centrifuge was loaded with 8 test tubes containing the wastewater (along with the dye and the
minimum amount of Nyex we could). The centrifuge had to contain 8 test tubes otherwise it would
not be balanced, and it couldn’t operate properly. This process allowed for the Nyex to sink to the
bottom due to its density, so the wastewater could be properly tested without containing Nyex.
Cuvette samples were obtained from these test tubes and placed into the UV-vis spectrometer and
eventually used to find the concentration of dye still in the wastewater at specific times – therefore
finding the most efficient times for each process and best current value for the separation of dye
from the wastewater.

Procedure:
Calibration Curve:
1. Prepare 1L of 30mg/L Acid Violet solution.
2. Pipette this out into smaller test tubes in small amounts and top off with distilled water to
obtain 10ml of solution with a range of concentrations ranging from 30mg/L to 0mg/L.
3. Add a small amount of each solution into cuvettes.
4. Put each cuvette into the UV-vis spectrometer and measure the absorbance against the
concentration.

Y cell:
First trial: Change in Fluidization Time
1. Prepare 2 litres of acid violet at 30 mg/litre. Add the contaminate water into the circulation
zone.
2. Switch on the air pump and circulate the Nyex through the acid violet for 15 min.

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Group: B11 Experiment 3: Electrochemical Water Treatment 20/10/2022

3. Switch off the air pump and allow the Nyex to settle for 2 min.
4. Switch on the air pump for the fluidization time during 5 min.
5. Switch off the air pump and allow the Nyex to settle for the Settling Time during 3 min.
6. Set the current to 0.5 A and switch on the power supply to regenerate the Nyex for the
Regeneration Time during 5 min.
7. Switch off the power supply.
8. Repeat step 4 to 7 two more times with a Fluidization Time of 10 and 15 min.
9. Samples should be collected in 10 ml centrifuge tubes using a dropper pipette every 3
minutes throughout the process starting at step 4.

Table 1: Time repartition for trial 1.

Fluidization Settling Time Regeneration
Time (min) (min) Time (min)
5 3 5
10 3 5
15 3 5

Second trial: Change in Regeneration Time

 Repeat each step of trial 1 but set a constant Fluidization Time of 10 min throughout the
process and change the Regeneration Time to 5, 10 and 15 min.

Table 2: Time repartition for trial 2.

Fluidization Settling Time Regeneration
Time (min) (min) Time (min)
10 3 5
10 3 10
10 3 15

Third trial: Change in current

 Keeping the same batch, process this trial in the continuity of trial 2 (start at step 4). Repeat
trial 1, however, set a constant Fluidization time and Regeneration Time of 10 min
throughout the process and change the current to 0.5, 1 and 1.5 A.

Table 3: Time repartition for trial 3.

Current Fluidization Settling Time Regeneration
(A) Time (min) (min) Time (min)
0.5 10 3 10
1 10 3 10
1.5 10 3 10

Sample measurement:
1. Put all the samples into the centrifuge at 5000 rpm for 8 min.
2. Pipette the solution from sample 1 into a cuvette, fill to the mark.
3. To calibrate the UV/Vis spectrometer, zero it with nothing in the machine.

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Group: B11 Experiment 3: Electrochemical Water Treatment 20/10/2022

4. Add the cuvette into the UV/Vis spectrometer, run the scan and note the absorbance.
5. Repeat step 2 to 4 for every sample collected.

3.2 Hazards
Table 4: Hazards.
Hazards Risks Precautions
Electrical Risk of electrocution. The equipment should be PAT tested
annually and regularly checked by
electricians.
Water spillage Water/Electric as above. All water systems are checked for
Can lead to slips/trips and falls leakages and spillages are mopped up
and leaks dealt with as soon as they are
hazards. spotted.
Electrolyte and May be harmful if there is a leak Acid electrolyte is prepared before the
chemical or if the fumes are inhaled. lab session by trained Lab support
technician.
No hazards associated with the dye.
Safety glasses, coat and gloves should
be worn.
Centrifuge Entrapments in moving parts. Cannot be opened when in motion.
Risk of electrocution. The equipment should be PAT tested
annually and regularly checked by
electricians.
UV/Vis Risk of electrocution. The equipment should be PAT tested
annually and regularly checked by
electricians.

4.0 Results and discussion

4.1 Observed data
Time (min) Absorbance Time (min) Absorbance
(abs) (abs)
0
Table 5: Data for calibration
Table 6: Sample absorption, trial 1. curve.2.493
Table 7: Sample absorption, trial 2.
0 1.618
Table 8: Sample absorption, trial 3.
Time (min) Absorbance Concentration 3 of Absorbance
2.424 (abs) 3 1.311
(abs) dye (mg/L) 6 2.361 6 1.185
0 2.059 0 9 2.3690.048 9 1.136
3 1.961 2.5 12 2.3470.785 12 1.130
6 1.939 5 15 2.3651.523 15 1.138
7.5 18 2.2142.573 18 1.126
9 1.957
10 21 2.3262.998 21 1.133
12 1.933
15 24 2.126 3 24 0.986
15 1.763
20 27 2.078 3 27 0.888
18 1.720
25 30 2.073 3 30 0.848
21 1.867
30 33 2.075 3 33 0.820
24 1.660
36 2.070 36 0.811
27 1.645
39 2.073 39 0.805
30 1.647
33 1.472 42 1.916 42 0.791
36 1.422 45 1.768 45 0.776
48 1.701 48 0.564
39 1.384
51 1.624 51 0.499
42 1.345
45 1.301 54 1.633 54 0.421
57 1.648 57 0.395
5 48 1.290
60 1.661 60 0.386
51 1.288
54 1.285 63 1.647 63 0.383
66 1.630 66 0.367
69 1.618 69 0.342
Group: B11 Experiment 3: Electrochemical Water Treatment 20/10/2022

4.2 Derived results

Figure 4: Graph of absorbance against concentration for the calibration curve.

10 min
fluidization

5 min
fluidization
15 min
fluidization

Figure 5: Graph of absorbance against time for trial 1.

10 min
fluidization
5 min
fluidization

15 min
fluidization

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Group: B11 Experiment 3: Electrochemical Water Treatment 20/10/2022

Figure 6: Graph of concentration against time for trial 1.

10 min
regeneration

5 min
regeneration
15 min
regeneration

Figure 7: Graph of absorbance against time for trial 2.

10 min
regeneration

5 min
regeneration 15 min
regeneration

Figure 8: Graph of concentration against time for trial 2.

1.0 A
current
0.5 A
current
1.5 A
current

Figure 9: Graph of absorbance against time for trial 3.

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Group: B11 Experiment 3: Electrochemical Water Treatment 20/10/2022

1.0 A
current
0.5 A
current 1.5 A
current

Figure 10: Graph of concentration against time for trial 3.

4.3 Calculations
We used the linear trendline equation from the calibration curve which was: y=0.3075 x +0.0478
in order to calculate the concentration from the absorbance at each time a sample was taken. y was
equal to absorbance and x was equal to concentration. So we rearranged for x to get the equation:
absorbance−0.0478
concentration= and using this data we replotted the data to get graphs of
0.3075
concentration against time.

To calculate the quickest time that the concentration of dye in the wastewater can be reduced from
100mg/L to less than 1mg/L, we looked at the equations for the lines of best fit and needed to find
the one where the gradient is the most negative. In our case it was having a current of 0.5A,
although looking at the graph it looks like an initial large decrease in concentration – so this could be
an anomaly or needing more data. Using this equation y=−0.0576 x+ 4.4242 and using the
gradient which is the change in concentration over time. The time taken to reduce the concentration
of dye from 100mg/L to less than 1mg/L can be worked out:

change ∈concentration 100 mg/ L

Time ( mins )= . Time ( mins )= =1736 minutes. Which is 28.9
0.0576 0.0576
hours to reduce the concentration of dye from 100mg/L to less than 1mg/L. Although if we also took
into account the most negative gradients between the 3 different trendlines for the fluidization
times and the regeneration times, which are 10 minutes for both fluidization time and 10 minutes
for regeneration time then we would be able to decrease this 28.9 hours even further. Our time of
28.9 hours is using 5 minutes for both fluidization time and 5 minutes for regeneration time.

4.4 Error analysis

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Group: B11 Experiment 3: Electrochemical Water Treatment 20/10/2022

5.0 Discussion
It can be seen from figure 6 that for trial 1, as the fluidization time is increased, the rate of change of
concentration remains relatively constant. This is shown by the gradients of each trendline being
very similar. This observation went against the theory as it was expected that the increase of
fluidization time would increase the rate of change of concentration. This is because increasing
fluidization time causes the Nyex to have a larger specific surface area which would result in
increased adsorption of the waste.

For trial 2 as shown in figure 8, as regeneration time is increased, the rate of change of
concentration was relatively constant. It was expected that a higher regeneration time would result
in more removal of AV17 as more Nyex would be regenerated and available to adsorb the waste.
This result could perhaps be explained by the fact that most, if not all, of the Nyex was regenerated
using a regeneration time of 5 minutes.

It can be seen from figure 10 that increasing the current has little to no effect on the rate of change
of concentration, as shown by the similar trendline gradients. This could be explained by the fact
that the Nyex may have already fully regenerated with the initial 0.5A of current, and so increasing it
would not affect the regeneration [6].

Overall, varying current resulted in the most removal of waste. This is shown by comparing the
gradients of the overall trendlines from figures 6, 8, and 10. Although all three gradients were of the
same magnitude, the most negative gradient was from trial 3, varying current. This result was
expected because regeneration of Nyex is caused by the current, so increasing the current would
increase regeneration and so more waste could be adsorbed [6]. It was found that the gradient of the
separate trendlines for each graph were relatively constant. As this result was not expected, it could
be explained by the introduction of errors. For example, human error when taking samples from the
Y-cell as it takes different amounts of time to take a sample each time.

6.0 Conclusion
The study being investigated during this experiment was a method which used the Arvia Gemini rig
to treat wastewater by Manchester Dyes Ltd. It has been shown that water treatment by adsorption
and electrochemical regeneration is an effective method to treat industrial wastewaters. The aims of
this experiment were to find which parameter, if changed, maximises the rate of decrease of
concentration of AV17. It was found that increasing the current was the best way to remove the
waste.

Although the gradients of the separate trendlines for each trial were similar in magnitude, looking at
the graphs of concentration of AV17 against time, there are sudden drops when each of the
parameters were changed. The concentration did drop more when each parameter was at its
highest value, so it can be concluded that keeping each of these parameters at their largest would
result in maximum waste removal. For example, if regeneration and fluidization time were at 15
minutes and current was at 1.5A.

7.0 Further work

The UV/Vis spectrophotometer could not read values of absorption of over 3.000, which meant that
there were fewer data points for the calibration curve. The experiment could have been improved

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Group: B11 Experiment 3: Electrochemical Water Treatment 20/10/2022

by having the spectrophotometer able to read more values as the equation linking adsorption to
concentration would have been more accurate.

A way to improve the experiment can be to repeat it at least 3 times and take the average of the
results. It will provide more data and will be easier to find a general trend and anomalies in the
experiment.

Moreover, the use of equipment with a greater level of precision will help to have a better accuracy
with the results.

Furthermore, as the samples were taken manually. It took approximately 30 seconds to collect them,
so it is not precisely every 3 minutes. It is the same for the change between the fluidization time,
settling time and regeneration time, as the pump and power supply were turn on or off manually a
lack of precision may happen because of the human reaction time. To increase the precision of the
experiment a good way could be to automize those tasks which will provide more accurate results.

8.0 References
[1] Mohammad, H. et al. (2020) “Effect of electrochemical regeneration on the surface of a graphite
adsorbent loaded with an organic contaminant,” International Journal of Environmental
Science and Technology, 17(6), pp. 3131–3142. Available at: https://doi.org/10.1007/s13762-
020-02624-0. (Access date: 24/10/2022)

[2] Asghar, H.M. et al. (2012) “Wastewater treatment by adsorption with electrochemical
regeneration using graphite-based adsorbents,” Journal of Applied Electrochemistry, 42(9),
pp. 797–807. Available at: https://doi.org/10.1007/s10800-012-0439-8. (Access date:
26/10/2022)

[3] Brown, N.W., Roberts, E.P.L., Garforth, A.A. and Dryfe, R.A.W. (2004). Electrochemical
regeneration of a carbon-based adsorbent loaded with crystal violet dye. Electrochimica Acta,
49(20), pp.3269–3281, Online Journal. Available at:
https://doi.org/10.1016/j.electacta.2004.02.040 (Access date: 24/10/2022)

[3] Lv, B. et al. (2021) “Hydrodynamics and adsorption performance of liquid–solid fluidized bed with
granular activated carbon for removal of copper ions from wastewater,” Journal of Cleaner
Production, 328, p. 129627. Available at : https://doi.org/10.1016/j.jclepro.2021.129627.
(Access date: 24/10/2022)

[4] Liu, D. et al. (2016) “Electrochemical regeneration of a graphite adsorbent loaded with acid violet
17 in a spouted bed reactor,” Chemical Engineering Journal, 304, pp. 1–9. Available at:
https://doi.org/10.1016/j.cej.2016.06.070. (Access date: 28/10/2022)

[5] Zhou, W. et al. (2021) “Electrochemical regeneration of carbon-based adsorbents: A review of

regeneration mechanisms, reactors, and future prospects,” Chemical Engineering Journal
Advances, 5, p. 100083. Available at: https://doi.org/10.1016/j.ceja.2020.100083.(Access date:
29/10/2022)

[6] F.M. Mohammed, E.P.L. Roberts, A. Hill, A.K. Campen, N.W. Brown. (2011). Continuous water
treatment by adsorption and electrochemical regeneration. Water Research. Volume 45, Issue
10. Pages 3065-3074. (Access date: 2/11/22)

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