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Use of suspended and attached growth wastewater treatment systems for the removal of benzotriazoles and benzothiazoles Aikaterini A. Mazioti 1 , Agapi Taka 1 , Evdoxia Chroni 1 , Athanasios S. Stasinakis 1 , Nikolaos S. Thomaidis 2 , Henrik R.

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Use of suspended and attached growth wastewater treatment systems for the removal of benzotriazoles and benzothiazoles

Aikaterini A. Mazioti1, Agapi Taka1, Evdoxia Chroni1, Athanasios S. Stasinakis1, Nikolaos S. Thomaidis2, Henrik R. Andersen3

1 Department of Environment, University of the Aegean, Greece 2 Department of Chemistry, National and Kapodistrian University of Athens, Greece 3Department of Environmental Engineering, Technical University of Denmark, Denmark

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Introduction 2

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Introduction 3

Organic micropollutants in the environment

 Low concentrations  Many compounds – Many sources  Partial removal in Waste Water Treatment Plants (WWTPs)

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Introduction 4

Biological Systems

  • A. Suspended growth systems

(Activated Sludge)

  • B. Attached growth systems

(Moving Bed Biofilm Reactors)

  • C. Hybrid systems

(Combination of A. and B.)

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Introduction 5

BTRs and BTHs

  • Uses: Metal finishing industry (corrosion inhibitors), Brake fluids,

cooling fluids, de-icing fluids, Dishwashing detergents, Tire and rubber manufacturing industries, Biocides and drugs

  • Chemical Properties: Highly soluble in water, Slightly basic

(pKa 7.7-8.9), High polarity - Weak tendency to sorb onto

  • rganic matter

1H-Benzotriazole 2-Hydroxybenzothiazole

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Introduction 6

Occurrence and Removal

Based on recent researches:

  • BTR’s detection frequency in European surface waters,

higher than 90 % Loos et al. (2009) Environ Pollution 157, 561-568

  • BTR’s median detected concentration in European treated

wastewater, higher than 2500 ng L-1

Loos et al. (2013) Water Res 47, 6475-6487

  • BTR’s removal from WWTP in Australia, lower than 60 %

Liu et al. (2012) Environ Pollution 165, 225-232

There is lack of information regarding BTRs and BTHs removal in lab-scale biological treatment systems.

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Introduction 7

Objectives of the study

 To investigate the removal of 5 BTRs (BTR, XTR, CBTR, 4TTR, 5TTR) and OHBTH during biological treatment To operate 4 different biological lab-scale continuous flow treatment systems for the comparison of target compounds removal

I. Activated Sludge system (AS) II. Moving Bed Biofilm Reactor system (MBBR-high)

  • III. Moving Bed Biofilm Reactor system (MBBR-low)
  • IV. Hybrid Moving Bed Biofilm Reactor system (HMBBR)

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Materials and Methods 8

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Materials and Methods 9 System's Name HRT Organic loading SRT Activated Sludge (AS) 26.4h 0.25 kg /m3 d 18d Moving Bed Biofilm Reactor high loaded (MBBR-high) 21.6h 0.77 kg /m3 d ∞ Moving Bed Biofilm Reactor low loaded (MBBR-low) 52.8h 0.30 kg /m3 d ∞ Hybrid Moving Bed Biofilm Reactor (HMBBR) 25h 0.75 kg /m3 d 8d

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Materials and Methods 10

Acclimatization phase: 30-45 days (approx. 3θc )

Raw municipal wastewater was provided. Monitoring of systems.

Experiment with micropollutants: 10 days

Target compounds were spiked, 12 dissolved phase samples were collected and analysed with SPE and HPLC.

Removal was calculated according to: and:

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Results 11

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Results 12

Wastewater quality and micropollutants

Each Target compound (inflow concentration): 20 μg /L

pH 6.6 - 7.4 CODdis ~300 mg /L NH4 -N 50 – 80 mg /L ΝΟ3 -Ν 1 – 9 mg /L TSS 10 – 120 mg /L

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Results 13

Wastewater Treatment Efficiency

COD % removal NH4-N % removal BC1 BC2 Total BC1 BC2 Total AS 90 (±7)

  • 90 (±7)

93 (±12)

  • 93 (±12)

MBBR high 72 (±11) 19 (±9) 91 (±7) 73 (±24) 22 (±15) 95 (±7) MBBR low 81 (±13) 5 (±12) 86 (±11) 78 (±29) 15 (±21) 93 (±13) HMBBR 80 (±16) 7 (±12) 87 (±8) 89 (±11) 9 (±6) 98 (±2)

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Results 14

Biomass concentration

Suspended

(mg/L)

Attached (biofilm) (mg/L) TOTAL (mg/L)

BC1 BC2 BC1 BC2 BC1 BC2 AS 2370 (±590)

  • 2370
  • MBBR

high 1079 (±715) 312 (±108) 138 (±68) 124 (±68) 1217 436 MBBR low 726 100 195 (±81) 131 (±89) 921 231 HMBBR 2914 (±510) 2687 (±524) 1023 (±171) 610 (±203) 3937 3297

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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21

Are the systems able to remove target compounds?

Results 15

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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21

Does a second reactor improves elimination?

Results 16

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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21

Suspended and Attached biomass have the same removal capacity?

Results 17

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Results 18

Comparison of each system’s overall performance

Target Compounds Removal ( >70%) Operational Parameters

OHBTH BTR XTR CBTR 5TTR 4TTR

Organic Loading HRT AS

       

MBBR high

       

MBBR low

       

HMBBR

       

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Conclusions 19

CONCLUSIONS

  • All substances examined can be removed to some extent with

biological treatment (both suspended and attached growth systems)

  • Target compounds were eliminated with the following descending
  • rder regarding % removal

OHBTH>BTR>XTR>CBTR>5TTR>4TTR

  • The addition of a second reactor in series can enhance the removal
  • f more persistent compounds (CBTR, 5TTR, 4TTR)
  • The MBBR systems seems to develop a biomass (biofilm) with

high capacity to remove target micropollutants

  • The HMBBR system was the more efficient, regarding

micropollutants removal and operational parameters (low HRT and high organic loading)

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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20 We Thank AnoxKaldnes for providing the carriers used in the experiments

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

Further information in two recently published articles:

Mazioti, A.A., Stasinakis, A.S., Pantazi Y., Andersen, H.R., 2015, Biodegradation of benzotriazoles and hydroxy-benzothiazole in wastewater by activated sludge and moving bed biofilm reactor systems. Bioresource Technology 192, 627-635. Mazioti, A.A., Stasinakis, A.S., Psoma A.K., Thomaidis N.S., Andersen H.R., Hybrid Moving Bed Biofilm Reactor for the biodegradation of benzotriazoles and hydroxy-benzothiazole in wastewater, Journal of Hazardous Materials (In Press, doi:10.1016/j.jhazmat.2016.06.035).

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21

Use of suspended and attached growth wastewater treatment systems for the removal of benzotriazoles and benzothiazoles

Aikaterini A. Mazioti1, Agapi Taka1, Evdoxia Chroni1, Athanasios S. Stasinakis1, Nikolaos S. Thomaidis2, Henrik R. Andersen3

1 Department of Environment, University of the Aegean, Greece 2 Department of Chemistry, National and Kapodistrian University of Athens, Greece 3Department of Environmental Engineering, Technical University of Denmark, Denmark

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Supplementary Material 22

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Supplementary Material 23

REFERENCES

Mazioti A.A, Stasinakis A.S.,Gatidou G., Thomaidis N. S., Andersen H. R. Sorption and biodegradation of selected benzotriazoles and hydroxybenzothiazole in activated sludge and estimation of their fate during wastewater treatment (2015) Chemosphere,131, 117-123 Mazioti, A.A., Stasinakis, A.S., Pantazi Y., Andersen, H.R., 2015, Biodegradation of benzotriazoles and hydroxy-benzothiazole in wastewater by activated sludge and moving bed biofilm reactor systems. Bioresource Technology 192, 627-635. Mazioti, A.A., Stasinakis, A.S., Psoma A.K., Thomaidis N.S., Andersen H.R., Hybrid Moving Bed Biofilm Reactor for the biodegradation of benzotriazoles and hydroxy-benzothiazole in wastewater, Journal of Hazardous Materials (In Press, doi:10.1016/j.jhazmat.2016.06.035). Loos, R., Carvalho, R., António, D.C., Comero, S., Locoro, G., Tavazzi, S., Paracchini, B., Ghiani, M., Lettieri, T., Blaha, L., Jarosova, B., Voorspoels, S., Servaes, K., Haglund, P., Fick, J., Lindberg, R.H., Schwesig, D., Gawlik, B.M. (2013) EU-wide monitoring survey on emerging polar organic contaminants in wastewater treatment plant effluents .Water Research, 47, 6475-6487 Liu Y.-S., Ying G.-G., Shareef A., Kookana R.S. (2012). Occurrence and removal of benzotriazoles and ultraviolet filters in a municipal wastewater treatment plant. Environmental Pollution 165, 225–232 Loos, R., Gawlik, B.M., Locoro, G., Rimaviciute, E., Contini, S., Bidoglio, G. (2009) EU-wide survey of polar

  • rganic persistent pollutants in European river waters Environmental Pollution, 157, 561-568.

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Analysis of BTRs/OHBTH

Wastewater Sample: 50 mL Filtration pH adjustment : 3.0 ± 0.1 Solid Phase Extraction Conditioning : 10 mL CH3OH Equilibration : 10 mL acidified H2O Washing : 2 × 5 mL acidified H2O Elution: 10 mL CH3OH/ACN Evaporation to dryness Sludge Sample: 100 mg Sonication Mixing : 10 mL CH3OH/ACN Sonication : 45 min (37 oC) Centrifugation : 10 min (4000 rpm) Reconstitution :1 mL CH3OH/H2O 0.05% acetic acid HPLC Analysis with DAD detector Filter

Supplementary Material 24

Mazioti et al. (2015) Chemosphere, 131, 117-123

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Supplementary Material 25

4 8 24 36 48 72 10 20 30

dissolved particulate Time (h) Concentration (μg L-1) Compound Kd (L Kg-1) R2 BTR 220 (± 9) 0.993 4TTR 170 (± 48) 0.870 5TTR 165 (± 14) 0.979 CBTR 242 (± 5) 0.998 XTR 87 (± 17) 0.930 OHBTH 147 (± 29) 0.893

Distribution in dissolved/particulate phase Sorption Coefficients

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

Mazioti et al. (2015) Chemosphere, 131, 117-123

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Supplementary Material 26

Activated Sludge (AS)

 Biomass is suspended and circulating in all parts of the bioreactor (due to aeration)

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Supplementary Material 27

Moving Bed Biofilm Reactor (MBBR)

 Biomass is attached on carriers and forms a stable biofilm  Carriers circulate in all parts

  • f the reactor due to air

supply

Α. High Loading HRT 10.8 ± 1.2 hours (in each reactor)

  • B. Low Loading

HRT 26.4 ± 3.6 hours (in each reactor)

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Supplementary Material 28

Hybrid Moving Bed Biofilm Reactor (HMBBR)

 Biomass is attached on carriers and forms a stable biofilm  Carriers circulate in all parts of the reactor due to air supply  Biomass also exists under suspension in high concentration, similar to those observed in AS systems

HRT 12.4 ± 0.6 hours (in each reactor) SRT 8 days

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Supplementary Material 29

Comparison of operational parameters

~1 day

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Supplementary Material 30

Comparison of operational parameters

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens

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Supplementary Material 31

Comparison of operational parameters

13th IWA Specialized Conference on Small Water and Wastewater Systems, September 2016, Athens