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Preliminarily Comparative Performance of Removing Bisphenol-S by Ferrate Oxidation and Ozonation ✉ Shaoqing Zhang 1, Jia-Qian Jiang 1 and Michael Petri2

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Preliminarily Comparative Performance of Removing Bisphenol-S by Ferrate Oxidation and Ozonation ✉ Shaoqing Zhang 1, Jia-Qian Jiang 1 and Michael Petri2 www.nature.com/npjcleanwater BRIEF COMMUNICATION OPEN Preliminarily comparative performance of removing bisphenol-S by ferrate oxidation and ozonation ✉ Shaoqing Zhang 1, Jia-Qian Jiang 1 and Michael Petri2 Bisphenol-S (BS) has recently raised public concerns for its adverse effect on the health safety and ecological security. BS concentrations were detected in many water resources, ranging from 10 ng L−1 to 300 μgL−1, so that various purification techniques have been sought to remove BS. This study investigated the performance of ozonation and ferrate oxidation in the degradation of BS since they are both promising oxidants with high redox potential among water treatment chemicals. It was observed that both ozone and ferrate can achieve over 99% of BS concentration reduction and up to 22.5% of DOC reduction for dosing 0.036 mM of either ferrate or ozone. The vibrio fisheri toxicity exhibited a decline in the treated samples after ozonation or ferrate oxidation. According to the mass spectra analyzed, the degradation pathways were proposed and oxidation products (OPs) were identified. BS degradation by ozonation and ferrate oxidation followed a similar route and four common OPs (OP-249; OP-497- a; OP-497-b, and OP-201) were detected. While ferrate treatment produced one more intermediate (OP-217), ozonation did not, which is attributed to the intensified decomposition of BS by ozonation. The major impact of this study is that ferrate treatment is comparable to the ozonation in removing BS, and further research continuing from this study is necessary to explore the BS removal in various waters with more complex matrixes (e.g., high natural organic matter contents), to investigate BS degradation mechanisms in depth, and to conduct pilot-scale and full-scale trials to establish operational database in running ferrate oxidation 1234567890():,; and/or ozonation for the treatment of BS in practical world. npj Clean Water (2021) 4:1 ; https://doi.org/10.1038/s41545-020-00095-x INTRODUCTION homogeneous and heterogeneous chemical oxidation techniques Endocrine disrupting chemicals (EDCs) have received major public have been tested including the activated persulfate with concerns in terms of their adverse effects on the water quality and CuCo2SO4 and permanganate coupled with iodide, which all public health. For human population exposed to EDCs, many show the acceptable performance in the removal of BS but with 15–17 endocrine-related diseases and disorders have been reported, for limitations . And then, the alternative treatment technologies example, the incidence of genital malformations has increased are still sought to tackle the BS pollution issues. over time at an unexpectedly high rate1,2. Bisphenol-A was once Ferrate (Fe(VI)) is a promising cleaning chemical for water and world widely used in industry but after its reorganization as one of waste water treatment, which predominantly attributed to its high EDCs, it has been phased out in the commercial use. Bisphenol-S oxidation capacity and coagulation function after its rapid 18–20 (BS, or 4,4-sulfonyldiphenol) is then regarded as a safe replace- decomposition and dissociation in water . The ferrate treat- ment to bisphenol-A due to its higher thermal stability and ment is highly recommended due to its less adverse effect on proposed high biodegradability3–5, and has been widely used in human and ecosystems18,21, and has been studied to clean the the production of epoxy resins and also used as a chemical H2S odor, remove turbidity, color and heavy metals and to additive to produce colourfast agents, leather tanning agent, dye inactivate lethal bacteria22,23. Currently, the water treatment by dispersants and fiber improvers6. However, based on fatal mouse ferrate is receiving more attention at the prospect of removing tests, recent researches showed that BS exhibits high endocrine residuals of pharmaceuticals, EDCs and personal care products in negative effect on human and aquatic species and the studies water and waste water effluents18,19,24. suggested that BS possesses higher toxicity than bisphenol-A and On the other hand, ozone is acknowledged as a strong reagent other bisphenol analogs3,4,7,8. In addition, BS concentrations were applied in water treatment25, which has greater oxidation capacity detected in a range from 10 ng L−1 to 300 μgL−1 in many water than permanganate, chlorine dioxide, chlorine gas, oxygen and resources including raw water and waste water effluent9–11, which hypochlorite26,27. As an oxidant in water treatment, ozone not only has caused concerns on the BS adverse effects on the aquatic plays main role in disinfection27, but can react with unsaturated environment and human health. bonds and aromatic and amino groups and then degrade various Several cleaning techniques have been tested for the removal organics27,28. The mechanism of ozonation is the formation of various of BS. For example, the activated sludge reactor and constructed reactive oxygen species (ROS) and free radicals when ozone is wetland have shown high efficiency of removing BS but their decomposed, which hold fairly high redox potentials, especially the performance was uncontrollable due to varying metabolisms hydroxyl radical can exert maximum redox potential of 2800 mV27. when the ambient conditions changed12,13. The adsorptive Table 1 shows the basic information of ferrate and ozone. technique can be considered as one of options, with 50–80% Due to the problematic issues caused by BS, this study aimed to removal achievable but the optimized performance was achieved conduct the comparative study of BS removal with ozonation and under relatively high restricted conditions14. Besides, many ferrate oxidation. Specifically, we investigated at bench scale, (1) 1Department of Civil Engineering and Environmental Management, Glasgow Caledonian University, Glasgow G4 0BA Scotland, United Kingdom. 2Qualitaetssicherung und ✉ Forschungslabor, Zweckverband Bodensee-Wasserversorgung, Suessenmuehle 1, 78354 Sipplingen, Germany. email: [email protected] Published in partnership with King Fahd University of Petroleum & Minerals Table 1. Basic properties of ozone and ferrate potassium26,27,36,37. Parameters Ozone Ferrate Molecular formula O3 K2FeO4 2− Oxidative species O3 molecule FeO4 − Free radicals generated as decomposition of ozone HFeO4 and H2FeO4 + + + Reaction mechanism O3 + 2H ⇄ O2(g) + H2O H3FeO4 ⇄ H +H2FeO4 − • −• + − O3 + HO2 → HO2 + O3 H2FeO4 ⇄ H +HFeO4 • + −• − + 2− HO2 → H + O2 HFeO4 ⇄ H +FeO4 Redox potential (V) 2.07–2.80 0.7–2.2 Table 2. Comparative reduction of EDCs with ferrate oxidation and ozonation. Ferrate oxidation EDC Sample condition Ferrate dosage Removal (%) Reference Tetrabromobisphenol-A Deionised water 0.025 mM 100 38 0.018 mM 17α-ethinylestradiol (EE2) Deionized water 0.05 mM 99 39 0.01 mM Bisphenol-A Deionised water 0.002 mM >95 40 0.002 mM Octylphenol Natural water 0.7 μM 100 41 7.5 μM 1234567890():,; Bisphenol-S Natural water 36 μM 99.95 This study 10 µg L−1 99.99 100 µg L−1 Ozonation Chemicals Sample condition Ozone dosage Removal (%) Reference Sulfolane Spiked groundwater 20 mg.L−1 200 mg.L−1 82 42 Bisphenol-A Spiked Milli-Q water 0.9 mg.L−1 1.4 mg.L−1 99 43 Spiked distilled water 0.509 mM 0.35 mM 87 44 levonorgestrel Spiked natural water 2mg.L−1 88 28 2.3 μg.L−1 Bisphenol-S Natural water 36 μM 99.99 This study 10 µg L−1 99.99 100 µg L−1 the reduction of BS concentrations, (2) mineralization efficiency of Mineralization of BS (DOC removal) BS, (3) resulting toxicity after the treatment, (4) the potential DOC removal indicates the extent of mineralization of BS in water oxidation products (OPs) formation, and (5) the degradation samples. Figure 1 shows that comparing to the concentration pathways of BS, by ozonation and ferrate oxidation. reduction of BS, the DOC removal of BS was relatively lower; 17.2 ± 1.91% and 22.5 ± 1.93%, respectively, by ozonation and ferrate treatment at a dose of 0.036 mM. Toxicity assessment RESULTS Figure 2 shows the comparative toxicity in untreated BS samples Reduction of BS concentration and in the BS samples after treatment by ozonation and ferrate. Table 2 shows that the ozonation and ferrate oxidation both The resulting toxicity of BS solution decreased after the treatment. achieved the high BS reduction, together with removal efficiency It can be observed that the toxicity declined more with ferrate of other EDCs by ferrate oxidation and ozonation. In this study, for treatment compared with that by ozonation, the average resulting −1 −1 its original concentrations of 10 µg L and 100 µg L , respec- toxicity was reduced by 23% after ozonation and by 69% after tively, BS was reduced >99% by either ozonation or ferrate ferrate treatment. treatment for a chemical dose of 0.036 mM at pH 7. The dose of The toxicity results in this study were consistent to a reported 0.036 mM of ferrate at pH 7 was chosen for the comparison with study29, where the resulting toxicity was significantly reduced the performance of ozonation since doses of ferrate greater than after BS was treated by the peroxymonosulfate with the addition 0.036 mM would not increase the BS reduction further (Supple- of Fe-SBA-15 under UV photolytic conditions. However, in another mentary Fig. 1) and neutral pH conditions produced similar BS study16, the toxicity increased when decreasing in BS concentra- reduction to that at the acidic condition but high reduction than tion after BS was treated by peroxydisulfate with sonolysis, that at the alkali condition (Supplementary Fig. 2). suggesting the more toxic oxidation products were generated. S. Zhang et al. 3 Fig. 1 DOC removal from BS spiked Lake Constance water with ozonation and ferrate treatment. [BS] = 1000 μgL−1,pH= 7. The error bars inserted were based on the standard deviation (s.d., n = 3).
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