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10 1016@j Elstat 2018 10 002 PDF
10 1016@j Elstat 2018 10 002 PDF
10 1016@j Elstat 2018 10 002 PDF
Journal of Electrostatics
journal homepage: www.elsevier.com/locate/elstat
A R T I C LE I N FO A B S T R A C T
Keywords: Underwater AC diaphragm discharge is energy efficient tool for decontamination of organic compounds from
Underwater diaphragm discharge aqueous solutions. This work is focused on the investigation of the electrical energy dissipation channels of the
Energy dissipation channels underwater AC diaphragm discharge and it chemical efficiency i.e. production of reactive species in aqueous
Reactive species solutions. Experimental results showed that more than 55% of total energy is consumed by heating of a solution
Energetic yields
and around 23% is used for the chemical reactions.
∗
Corresponding author.
E-mail address: avlada5577@gmail.com (A. Khlyustova).
https://doi.org/10.1016/j.elstat.2018.10.002
Received 26 April 2018; Received in revised form 31 August 2018; Accepted 5 October 2018
0304-3886/ © 2018 Elsevier B.V. All rights reserved.
A. Khlyustova et al. Journal of Electrostatics 96 (2018) 76–84
Fig. 1. Underwater AC diaphragm discharge scheme 1 – graphite electrodes, 2 – 3. Results and discussion
quartz ampoule, 3 – plasma zone.
3.1. Electrical characteristics of underwater AC diaphragm discharge
discharge at voltages up to 10 kV. The discharge was excited at different
voltages in the range 2–6 kV at alternating current varied from 20 to High current density (as a result of a small diaphragm size) results in
50 mA depending on the discharge burning regime. All experiments solution overheating and formation of the vapor bubble, which lead to a
were carried out in the non-symmetric H-type cell. In each experiment, break in the electrical circuit. The electromotive force (EMF) of the
a fixed solution volume of 170 mL was used. Two graphite electrodes voltage source and EMF of self-induction is applied to bubbles. The
were immersed into solution in separate parts of the cell. One of was development of a discharge occurs in bubbles. It leads to the collapse of
placed in a quartz ampoule with the hole (diaphragm) with the dia- the bubble with excitation of an acoustic wave (so-called “active
meter of 2 mm. The diaphragm discharge was initiated and propagated phase”). The current and voltage waveforms of the underwater AC
at the hole of the quartz ampoule in the bubble. The values of discharge diaphragm discharge are shown in Fig. 2. The burst of a bubble is ac-
current and voltage drop were recorded using the OWON PDS 5022C companied by the appearance of an additional peak on the current
digital oscilloscope and then processed on a computer. The voltage waveform with a lower current amplitude. This effect has 50 Hz fre-
divider was used to measure the voltage drop. The corresponding re- quency with 3 ms duration of the discharge active stage (pointed by
sistance values were 25 MΩ (R1) and 2.5 kΩ (R2). The temperature of arrows in Fig. 2). Therefore, the discharge operation can be referred to
the solution during the discharge treatment and after discharge off was as pulsed one excited by means of the AC source.
detected by chromel-alumel thermocouple monitored by digital multi- The average power is calculated by equation (1). It was decided to
meter RESANTA DT9208A. integrate over 30 seconds to obtain real value of the dissipated power
Solutions of K4[Fe(CN)6], KMnO4, and K2Cr2O7 were used as the (overcome stochastic discharge operation).
scavengers of OH• radicals, hydrated electrons, and hydrogen atoms, 1
t
77
A. Khlyustova et al. Journal of Electrostatics 96 (2018) 76–84
Table 1
Energy balance in underwater diaphragm discharge.
Input energy Output
78
A. Khlyustova et al. Journal of Electrostatics 96 (2018) 76–84
(reaction rate constants are given from Refs. [52,53] at T = 293 K): O2− + [Fe (CN )6]3 − → [Fe (CN )6]4 − + O2 k = 9 × 102M−1s−1
−
eaq + MnO4− → MnO2 + 2O− k = 3.3 × 1010M−1s−1 (23)
(10)
H2 O2 + 2[Fe (CN )6]4 − → 2[Fe (CN )6]3 − + 2OH− (24)
MnO4− + H • → MnO42 − + H+ k = 3.3 × 1010M−1s−1 (11)
According to our previous data, experiments with ferrocyanide so-
MnO4− + O2− → MnO42 − + O2 k = 8 × 106M−1s−1 (12) lutions did not result in the formation of the hydrogen peroxide [30].
However, there are other pathways to produce H2O2. According to
2MnO4− + 5H2 O2 + 6H+ → 2Mn2 + + 8H2 O + 5O2 (13)
[56], thermal oxidation of ferrocyanide ions by hydrogen peroxide is
It should be noted that the high value of the rate constant for re- very slow in solutions. This reaction takes more than 4 hours. There-
action (11) was obtained in an acid solution (pH = 2) [53]. However, fore, the interaction between [Fe(CN)6]4- ion and H2O2 does not occur.
the contribution of this reaction in reducing the permanganate ion was Interaction of hydrogen atoms with ferricyanide ions leads to the for-
considered. To minimize reduction processes induced by hydrated mation of aquapentacyanoferrate (II) ion (reaction (21)), which has
electrons in H• atoms and OH• radicals detection experiments, several optical absorption at 480 nm [57]. The peak appearance at 480 nm was
experiments were conducted with the flow of N2O through the solution not detected during underwater AC diaphragm discharge. Reaction (22)
(resulted in bubbling). Nitrous oxide is known as the scavenger of the could take place in acid medium and reaction (23) can proceed in alkali
hydrated electrons [54] (reaction 14). The reaction rate for interaction medium, where radical pair HO2•/O2¯ has a pH depended equilibrium
between the H• atom with nitrous oxide is lower than that for reaction [58]. Moreover, the rate constants of reactions (22) and (23) are very
(14) by a factor of 103 [53,54]. low implying that they cannot compete with the much faster reaction
− (20) and ensure that hydroxyl interacts primarily with ferrocyanide
N2 O + eaq → N2 + OH· + OH− k = 9.1 × 109M−1s−1 (14) ions (oxidation mechanism) if similar concentrations of HO2• and OH•
In this case, the reducing process of MnO4‾ ions proceeds through are presented.
the following solution color changes: purple, green, red and brown It should be noted that the concentration of the reactive species in
precipitate appearance. The consequent reactions are: solution is non-uniform. Concentration is higher in the near plasma
regions and negligible in the solution bulk. Thus, all kinetic schemes are
MnVII→MnVI→MnV→MnIV (as MnO2)→Mn2+ (15) described in areas that are near the plasma zone. Applying the sta-
The appearance of MnO2 was observed after 55 minutes of dis- tionary state approximation to these radicals, we have:
− −
charge treatment with N2O. Note that the formation of MnO2 occurred g (eaq ) − k10 [eaq ][MnO4−] − Σki [eaq
−
][Ci] = 0 (25)
after the first minute of treatment without N2O bubbling. Hence, the
main trapping pathway for hydrated electrons is reaction with the g (H •) − k17 [H •][Cr2 O72 −] − Σki [H •][C i] =0 (26)
MnO4¯ ion in the neutral medium (reaction 10). The appearance of
Mn2+ ion in the solution is accompanied by decolorization of the so- g (OH •) − k20 [OH •][[Fe (CN )6]4 − ] − Σki [OH •][Ci] = 0, (27)
lution at a long time of treatment (t > 5 min). whence
− −
4.3. Cr2 O72 − ion g (eaq ) = k10 [eaq ][MnO4−] + ∑ ki [eaq− ][Ci] (28)
H • + [Fe (CN )6]3 − → Fe (CN )5 H2 O3 − + HCN k = 6.0 × 109M−1s−1 curves of CrV ion accumulation had saturation (Fig. 4c). If the transition
(21) of Cr6+ to CrV and then to Cr3+ takes place, the curve of accumulation
would have a maximum. The conditions of our experiments allow ob-
HO2• + [Fe (CN )6]4 − → [Fe (CN )6]3 − + HO2− k=1× 10 4M−1s−1 taining the CrV as the final product (neutral pH, low concentration of
(22) potassium dichromate, low discharge currents). The kinetic scheme for
79
A. Khlyustova et al. Journal of Electrostatics 96 (2018) 76–84
Then the equation for [H•] can express via the initial rate formation:
υ
[H •] = .
k17 [Cr2 O72 −] (34)
V
The initial rates of Cr formation were estimated by the initial parts
of kinetic curves accumulation, which are presented in Table 2.
The production rates for reactive species are calculated by using
equations (28-34). Fig. 5 shows the production rates of reactive species
for various discharge currents. Our results showed that rates of gen-
eration of reactive species are different. We assumed that the increase
of the production rates for reactive species with increasing of a dis-
charge current (input energy) is more pronounced. However, the pro-
duction rate for hydrogen atoms is about 7 × 10−7 M/s and do not
depend on the discharge current for our experimental conditions. It
means that the contribution of ∑ki[H•][Ci] term in Eq. (29) is increased.
This term includes all interaction between H• atoms and other reactive
species in solution. And reactions between hydrogen atoms and hy-
droxyl radicals and hydrated electrons are the main ways for the dis-
appearance of H• atoms by increasing input power at our experimental
conditions.
According to reaction (9), one can suggest that the number of H•
radicals, hydrated electrons, and OH• radicals will be the same within
processes of activation and non-equilibrium dissociation of water mo-
lecules. However, our obtained results are contradicted by this sug-
gestion. On the other hand, this reaction is the scheme of the activation
process. According to data of radiation chemistry, the breaking H-OH
bond results in yielding of the mixture of the radical and molecular
species [53].
−
H2 O → H2 O∗ → 0.028OH·+0. 27eaq + 0.06H·+0.05H2 + 0.07H2 O2
+ 0.27H3 O+ (35)
The reactive nitrogen species did not register in all experiments with
underwater diaphragm discharge. It is not unexpected because the
plasma zone has no contact with air. In the case of H2O2, it should be
noted that hydrogen peroxide is not detected in experiments in pre-
sence of ferrocyanide ions (as the scavenger of OH• radical). In other
experiments, without OH radical scavengers, the accumulation of hy-
drogen peroxide in solution during the plasma treatment was registered
(Fig. 6). Experimental results showed that values of concentration are
lower in comparison with tubular discharge (9 mM) [60] and under-
water capillary discharge (7.5–15.6 mM) [17,18,61].
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A. Khlyustova et al. Journal of Electrostatics 96 (2018) 76–84
Table 2
Steady state concentrations and rates of oxidation and reduction processes by underwater AC diaphragm discharge treatment.
I, mA KMnO4 solution K4[Fe(CN)6] solution K2Cr2O7 solution
−14 −7 • −14
−
[eaq ]ss, 10 M υ, 10 M/s [OH ]ss, 10 M υ, 10−7 M/s [H•]ss, 10−14 M
Table 3
Energy yields (molecules/100 eV) of reactive species in aqueous solutions by
electrical discharge treatment.
Experimental conditions (discharge type, G value (molecule/ Ref.
gas, scavenger) 100 eV)
Hydrated electrons
Glow discharge electrolysis, hydrogen, 0.016 [32]
monochloroacetic acid
Silent discharge, argon, K3[Fe(CN)6]+NaN3 0.06 [33]
Atmospheric pressure glow discharge, air, 0.13 [35]
KMnO4
Underwater AC diaphragm discharge, 0.07 This work
KMnO4
Hydrogen atoms
Silent discharge, Ar, He, Ce(SO4)2 0.6–1.2 [37–39]
Contact glow discharge, air, maleic acid 0.05–0.08 [40]
Underwater AC diaphragm discharge, 0.06 This work
K2Cr2O7
Hydroxyl radicals
Pulsed tubular discharge, Ar, ethanol, 3–5 [29]
TiOSO4
Atmospheric pressure glow discharge, air, 0.17 [30]
K4[Fe(CN)6]
Pulsed corona, air, phenol 0.06 [62]
Fig. 5. Reactive species production rates versus discharge current. Pulsed corona, terephtalic acid, 0.01 [63]
dimethylsulfoxide
Underwater AC diaphragm discharge, K4[Fe 0.03 This work
(CN)6
Hydrogen Peroxide
Underwater DC capillary discharge 0.08 [19]
Pulsed corona in water 0.047–0.091 [63]
Underwater capillary discharge 0.016 [61]
Underwater AC diaphragm discharge 1.06 This work
showed that the yields of reactive species do not depend on the dis-
charge current. The average values are presented in Table 3.
It is difficult to compare the G values obtained by the action of
underwater discharges and discharges above liquids due to different set
reactions in the kinetic schemes. But we can compare the efficacy of our
type of the underwater discharge with other underwater discharge
plasmas. To our knowledge, there is no data on generation rates for
hydrated electrons and H• atoms by underwater discharges. and we can
−
compare with published data for discharges above liquids. The G(eaq )
value has the same order of the magnitude with values of yield by silent
discharge and glow discharge electrolysis [32,33]. The value of yield
for H• atoms is compared with data obtained by DC contact glow dis-
charge [40].
Regarding hydroxyl radicals, one of the reasons for the difference of
Fig. 6. Accumulation of hydrogen peroxide in solutions during underwater
our G value may be explained by using the various scavengers (see
diaphragm discharge treatment in presence of MnO4⁻ ions (1) and Cr2O72− ions
(2) at discharge current of 50 mA. Table 3). The highest value of the OH• radical energy yield of was found
for a pulsed tubular discharge with liquid film in argon (3–5 molecules/
100 eV) [29] which obtained from the H2O2 formation (detected by
where g is the production rate (M/s), NA is Avogadro's number TiOSO4).
(6.02 × 1023 particles/mole), V is the solution volume (0.17 L), e is Regarding hydrogen peroxide, our calculation showed that the en-
charge of electron (1.6 × 10−19 C), < P > is average power of dis- ergetic yield of hydrogen peroxide is higher than for pulsed corona
charge (W) (calculated from eq. (2)). The results of our calculations discharge in water, dielectric barrier discharge in direct contact with
81
A. Khlyustova et al. Journal of Electrostatics 96 (2018) 76–84
Appendix
The oxidation of the potassium ferrocyanide has been successfully used as a dosimeter for OH radicals [30,65]. The use of salicylate ion and
phenol as scavengers of hydroxyl radicals were described in previous works [34,62,66–69]. However, using these compounds for trapping OH•
radicals in solution at pH∼7 requires specific conditions to prevent reduction processes [34,70]. The MnO4‾ ion was used as the scavenger of
hydrated electrons in Ref. [35]. Potassium dichromate solution was chosen as the scavenger for H• atoms. For instance, some works report about
investigations of the reduction kinetics of CrVI to CrIII by various types of gas discharges [51,71–73]. It was noted that in acid and alkali solutions the
reducing CrVI occurs to CrIII through the formation of transient forms of Cr. In acid solution, the reducing process induces by hydrogen atoms
whereas, in alkali solutions, CrVI reduced by hydrated electrons. In a neutral solution, the reducing process can be more complicated owing to the
presence of both H• atoms and hydrated electrons. In spite of this, the dichromate ion can be used as a scavenger of H• atoms.
Kalkar et al. [74] demonstrated that the concentration of permanganate ion greater than 0.4 mM is sufficient to remove all hydrated electrons in a
liquid medium. In the case of OH• radical detection, Gupta and Bluhm [75] established that in order to successfully compete with radical re-
combination (formation of H2O2), 6 mM chemical probe concentration is enough.
The solutions with 0.5 mM of KMnO4 (pH 6.5, conductivity 35 μS/cm) and 0.5 mM of K2Cr2O7 (pH 6.5, conductivity 60 μS/cm) were used as the
scavengers of reductive reactive species. The solution of 1 mM of K4[Fe(CN)6] (pH 7, conductivity 640 μS/cm) was used as the scavenger of hydroxyl
radical. The larger value of ferrocyanide ion concentration is explained by low values of the extinction coefficient of ferricyanide ion in the maximum
of the absorption band (ε = 505 M−1cm−1 at 420 nm) compared with MnO4‾ ion (ε = 2500 M−1cm−1 at 525 nm) and CrV ion (ε = 3150 M−1 cm−1
at 350 nm) [76]. The untreated K2Cr2O7 solution has a maximum absorbance at 360 nm. The appearance of CrV ion in solution leads to a blue shift
and peak appearance at 350 nm (see Fig. A1) [77,78].
Fig. A1. Absorbance spectra of untreated (1) and after 60 s treatment by underwater AC diaphragm discharge (2) of K2Cr2O7 solution.
Hydrogen peroxide accumulation by electrical discharge treatment under various experimental conditions has previously been reported [79]. It
was found that reduction of permanganate ions by hydrogen peroxide in acid solution is thermodynamically favorable since the standard electrode
potential is +1.51 V for MnO4‾ reduction. This potential value is higher than the standard electrode potential for H2O2 oxidation (−0.682 V). The
reduction mechanism of MnO4‾ by H2O2 was described in Ref. [79]. In acid solution, the hydrogen peroxide leads to a direct formation of Mn2+ by
82
A. Khlyustova et al. Journal of Electrostatics 96 (2018) 76–84
reaction (12). Upadhaya and co-workers [80] found that H2O2 reduced only 10% of the permanganate ions. The possibility of reducing reaction with
the participation of H2O2 at pH∼7 was considered in our experiments also. Several experiments on the study of the reduction process of MnO4‾ by
hydrogen peroxide were carried out. The H2O2 was added to the solution (c(H2O2) = 10 mM) without diaphragm discharge ignition. The absorbance
spectroscopy results showed that reducing process is very slow (more than 3 hours). The maximum of absorbance peak shifted on 5 nm in the
shortwave region. It indicates that the MnV ions appeared (as H3MnO4) in solution (reaction (A1)).
KMnO4 + H2 O2 + H2 O → H3 MnO4 + O2 + KOH (A1)
A shift of the absorbance peak by the underwater AC diaphragm discharge treatment was not detected. This indicates that the reducing process of
MnO4‾ ion by hydrogen peroxide did not occur in a neutral solution.
The reduction of MnO4‾ ions by dissolved oxygen in neutral solution is thermodynamically unfavorable because the standard electrode potentials
for MnO4‾ reduction and for O2 oxidation are +0.6 V (pH 7) and +0.815 V (pH 7), respectively.
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