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On the Possibilities of Straightforward Characterization of Plasma Activated Water On the possibilities of straightforward characterization of plasma activated water Citation for published version (APA): Hoeben, W., van Ooij, P., Schram, D., Huiskamp, T., Pemen, G., & Lukes, P. (2019). On the possibilities of straightforward characterization of plasma activated water. Plasma Chemistry and Plasma Processing, 39(3), 597-626. https://doi.org/10.1007/s11090-019-09976-7 DOI: 10.1007/s11090-019-09976-7 Document status and date: Published: 02/04/2019 Document Version: Publisher’s PDF, also known as Version of Record (includes final page, issue and volume numbers) Please check the document version of this publication: • A submitted manuscript is the version of the article upon submission and before peer-review. There can be important differences between the submitted version and the official published version of record. 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Link to publication General rights Copyright and moral rights for the publications made accessible in the public portal are retained by the authors and/or other copyright owners and it is a condition of accessing publications that users recognise and abide by the legal requirements associated with these rights. • Users may download and print one copy of any publication from the public portal for the purpose of private study or research. • You may not further distribute the material or use it for any profit-making activity or commercial gain • You may freely distribute the URL identifying the publication in the public portal. If the publication is distributed under the terms of Article 25fa of the Dutch Copyright Act, indicated by the “Taverne” license above, please follow below link for the End User Agreement: www.tue.nl/taverne Take down policy If you believe that this document breaches copyright please contact us at: [email protected] providing details and we will investigate your claim. Download date: 28. Sep. 2021 Plasma Chemistry and Plasma Processing (2019) 39:597–626 https://doi.org/10.1007/s11090-019-09976-7 ORIGINAL PAPER On the Possibilities of Straightforward Characterization of Plasma Activated Water W. F. L. M. Hoeben1 · P. P. van Ooij1,2 · D. C. Schram3 · T. Huiskamp1 · A. J. M. Pemen1 · P. Lukeš4 Received: 31 October 2018 / Accepted: 14 March 2019 / Published online: 2 April 2019 © The Author(s) 2019 Abstract Plasma activated deionized water from a hot arc 150 W PAW synthesizer has been analyzed for nitrite, nitrate and peroxide densities. Observed nitrite and nitrate levels are impressive, reaching several millimoles per liter at few hundred kiloJoules per liter energy input. Nitrate levels appear positively infuenced by the applied energy density, together with a less pro- nounced increase in nitrite levels and limiting energy density for maximum peroxide levels. Active PAW cooling during synthesis appears to be essential for obtaining relevant peroxide levels and connected PAW activity. In addition to established laboratory diagnostics, alterna- tive low access tools have been investigated for applicability of PAW characterization in of- lab situations. Although no unique parameter exists to properly represent PAW activity, pH, oxidizing-reduction potential and electrical conductivity provide important insight, together with aqueous phase nitrite absorption spectrometry. Finally, classic acid-base titration has been applied to fnd access to the complex mixture of acidic reactive nitrogen species. Keywords Plasma activated water · Reactive oxygen species (ROS) · Reactive nitrogen species (RNS) · Reactive oxygen and nitrogen species (RONS) · Wet chemical analysis · Atmospheric plasma liquid interaction · Pulsed power plasma technology Introduction Plasma activated water (PAW) is a versatile medium for both biomedical and agricultural applications. Currently under investigation and promising are its applications e.g plant disease control, plant nutrition, surface disinfection, surgical equipment sterilization, skin * W. F. L. M. Hoeben [email protected] 1 Department of Electrical Engineering, Electrical Energy Systems Group, Eindhoven University of Technology, PO Box 513, 5600 MB Eindhoven, The Netherlands 2 VitalFluid, De Run 8218-C, 5504 EM Veldhoven, The Netherlands 3 Department of Applied Physics, Plasma Materials Processing group, Eindhoven University of Technology, PO Box 513, 5600 MB Eindhoven, The Netherlands 4 Institute of Plasma Physics, The Czech Academy of Sciences (AV ČR), Za Slovankou 1782/3, 182 00 Prague 8, Czech Republic Vol.:(0123456789)1 3 598 Plasma Chemistry and Plasma Processing (2019) 39:597–626 disinfection, wound treatment, dental bleaching and root disinfection, bladder infection and cancer treatment [1–6]. PAW active ingredients comprise transient reactive oxygen and nitrogen species (ROS and RNS, combined abbreviation RONS). The focus of this study has been on investigation of the possibilities of straightforward/ low-access diagnostic tools for PAW characterization, as alternative to reference tools like ion chromatography and peroxotitanyl spectrometry. Simple diagnostic tools would be especially suitable for PAW synthesis process feedback control and also for PAW activity monitoring on locations, where only limited laboratory facilities are available. In compari- son with the reference diagnostics, pH, oxidation reduction potential (ORP), electrical con- ductivity (EC), titrimetry, general UV absorption spectrometry and commercially available indicator strips have been studied. PAW synthesis precedes by application of electric gas discharges in air or nitrogen-oxy- gen mixtures over a water volume [7]. Fundamental plasma phenomena, as will be dis- cussed in "Plasma Fundamental Considerations" section, explain the formation of simple atomic and molecular precursors to the observed liquid phase plasma chemistry, the key 1 research of this study. Involved species are nitrogen oxides based RNS (NO, NO2 , NO3, 2 1 N2O3 , N2O4 , N2O5 ) nitrogen oxoacids based RNS ( HaNbOc ) and ROS ( O3 , O2 , O, OH, HO2 , H2O2 ) [9–13]. PAW solutions typically comprise nitric ( HNO3 ) and nitrous ( HNO2 ) acid and low level transient RNS like e.g. peroxynitrous acid ONOOH / peroxynitrite − ONOO and accompanying ROS. ONOO(H) is generally considered to account for major contribution to PAW activity due to powerful oxidizing and cytotoxic properties [11, 14–18], together with peroxynitric acid − − O2NOOH / peroxynitrate ( O2NOO ), a product from ONOOH and ONOO at near neutral pH conditions [19]. Koppenol [19] and Kissner [20] propose ONOOH decomposition via ⋅ ⋅ the hydroxyl radical in a radical cage pair together with nitrogen dioxide [ NO2 OH ] to nitrate/nitric acid, or directly. The oxidizing potential of ONOOH may also be related to 1 release of singlet oxygen ( O2 ) accompanied by nitroxyl (HNO) [21] upon decomposition. Although the solubility of the higher nitrogen oxides in water is reasonable [22] and acidic conditions thus are easily reached, PAW normally is synthesized at about pH = 3.3. Then, PAW already features impressive disinfection performance, while material corrosion or etching damage in biochemical systems are minimized. Experiments Equipment and Settings All experiments have been performed on PAW, obtained from a 150 W VitalFluid syn- thesizer. VitalFluid is a spin-of company from the Electrical Energy Systems Group at Eindhoven University of Technology, founded in 2014. The power system comprises a dual resonant power modulator switching at 1 MHz [23]. The power (J/s) is modulated by changing the repetition frequency (bursts/s) and the number of cycles per burst (cycles/ burst x J/cycle = J/burst). Small power fuctuations are regulated by the repetition rate, 1 The nitrate radical exhibits minutes to seconds lifetime in atmospheric chemistry [8]. 2 H N O x y z notation has been avoided, because it coincides with ofcial atmospheric chemistry nomencla- NO NO NO = NO + NO NO ture: x = NO+ 2 , y x z , z = reservoir species [8]. 1 3 Plasma Chemistry and Plasma Processing (2019) 39:597–626 599 C1 Kab I1 L1 L2 I2 R1 R2 Fig. 1 VitalFluid PAW synthesizer pulsed power topology 5000 0.2 4000 0.15 3000 0.1 2000 0.05 1000 0 0 Voltage (V) -1000 Current (A) -0.05 -2000 -0.1 -3000 -0.15 -4000 -5000 -0.2 0123456 Time (s) 10-5 Fig. 2 Characteristic voltage and current waveforms at 90 W RF power; burst repetition rate ∼ 23.5 kHz , duty cycle ∼ 0.51 (Color fgure online) while the number of cycles per burst is applied for power level setting. The ignition voltage is up to 100 kV, while the arc voltage is 8 kV peak-to-peak. Schematics and typical wave- forms are given in Figs. 1, 2 and 3, respectively. A few thousand Kelvin arc is produced in the gas phase of a borosilicate 800 mL glass beaker, partially flled with deionized water, typically 400 mL, see also Table 4. The arc is directed into the water vortex, propelled by a magnetic stirrer bar, in order to optimize plasma-water interaction and HaNbOc gas-to-liquid phase mass transfer. The plasma reactor confguration features a DBD topology, the ground electrode situated 1 3 600 Plasma Chemistry and Plasma Processing (2019) 39:597–626 Fig. 3 Characteristic power burst 800 waveform at 90 W RF power 700 600 500 ) 400 300 Power (W 200 100 0 -100 0123456 -5 Time (s) 10 Fig. 4 Typical arc-water vortex interaction; exposure time 1/40 s, aperture f/5 underneath the glass beaker bottom. Figure 4 shows a long exposure photo of the arc in the vortex; a time-resolved CCD picture is given by Fig. 5 [24]. Additionally, a double ◦ wall 600 mL Duran glass beaker has been applied, conditioned at 12 C . Although PAW synthesis using tap water is equally possible, deionized water has been chosen for rea- sons of standardization in process and analytical conditions. The reactor is sealed and purged with fltered compressed air at ambient pressure, unless stated otherwise.
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