May 08, 2024

Public workspaceWATER PRODUCTION FOR AWARE (Organic Contaminants) V.1

DOI
dx.doi.org/10.17504/protocols.io.14egn67jql5d/v1
  • 1IIM-CSIC
AWARE Project
Open access
DOI: dx.doi.org/10.17504/protocols.io.14egn67jql5d/v1
Protocol Citation: Antonio Cobelo 2024. WATER PRODUCTION FOR AWARE (Organic Contaminants). protocols.io https://dx.doi.org/10.17504/protocols.io.14egn67jql5d/v1
License: This is an open access protocol distributed under the terms of the Creative Commons Attribution License,  which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited
Protocol status: Working
We use this protocol and it's working
Created: May 08, 2024
Last Modified: May 08, 2024
Protocol Integer ID: 99427
Keywords: water sampling, water processing, water analysis, waste water treatment, advanced tertiary treatment SOP
Funders Acknowledgement:
Horizon Europe
Grant ID: 101084245
Abstract
The protocol summarises the procedures used for analytical control. The protocol describes the Standard Operating Procedure (SOP) for the optimization of advanced tertiary treatment of water, based on a comprehensive quality and risk assessment.
Guidelines
Directive 2008/105/EC of the European Parliament and of the Council of 16 December 2008 on environmental quality standards in the field of water policy.
Materials
ABCDEFGH
ParameterV (mL) x R SProcessingAnalytical methodResultLOD / LOQGoal value
Organic contaminants500 x 2On iceSolid-phase extractionHPLC/MS-TOFPresence/absence-Not present
Materials:
ABCD
Becker cartridges (OASIS HLB 200 mg)
Pre-filterationBuchner flask SPE vacuum pump
PVDF 0.45 µm filters graduated cylinder
trap flask becker
vacuum pump trap flask
SPE vacuum manifold system

Safety warnings
Attention
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Organic Contaminants:
Organic Contaminants:
The water production for AWARE main activities includes three stages – disinfection by ultraviolet C radiation (UVC), storage forDuration12:00:00 -Duration24:00:00 (according to water load and season) and ozonation. The water quality is monitored at these three stages, for the parameters indicated in Figure 1 below.



1d 12h
Sampling, Processing, and Analyses

Water samples are collected (see Figure 2) and processed within aDuration06:00:00 interval, before being shipped for the partner responsible for the analyses (Table 1). In case no processing is needed, samples are frozen and stored atTemperature-80 °C withinDuration03:00:00 .
For each sampling event, the date, day of the week and hour; the temperature and rain. Sampling points, indicated in Figure 2 were designated from A to I:
- Influent of primary treatment (A)
- Influent of biological treatment (activated sludge) (B)
- Treated secondary effluent (C)
- Sand filter effluent (D)
- UVC effluent (E)
- Storage for reuse tank effluent (F)
- Ozonation effluent (1 dose, e.g.,Amount5 mg O3) - MITO3X technology - (G)
- Effluent of the vacuum UV oxidation (VUV) (H)
- Effluent of reactive storage / Influent of the recirculation aquaculture system (RAS) (I) ù



9h
Methods: The section below summarises the procedures used for analytical control – detailed protocols are annexed to this protocol.
Methods: The section below summarises the procedures used for analytical control – detailed protocols are annexed to this protocol.
1d 0h 30m
Organic Contaminants: Analysis: Screening of Organic Contaminants in Water.
Methods: Solid-phase extraction 2.1 Sample filtration (0.45um PVDF).
CollectAmount200 mL of the filtered water sample (e.g. volumetric flask or beaker) and spike with Amount50 µL of an internal standard solution. Produce twoAmount200 mL replicates per sample. Mix well after the internal standard is added.
Cleaning/Conditioning of the cartridges (OASIS HLBAmount200 mg ) 3.1. PassAmount5 mL of MeOH 3.2. PassAmount5 mL of ultrapure water
Pass theAmount200 mL of sample

Rinse the volumetric flask or beaker that contained the sample with 2xAmount10 mL of ultrapure water, which are then passed through the cartridege

Drying the cartridge resin (e.g. N2 flow forDuration00:30:00 )

30m
Store the cartridges in a freezer (Temperature-20 °C ) All samples are to be processed in duplicate. For the cartridge blanks (n=2): start withGo togo to step #2.3 , and then spike directly on the cartridge the same amount of internal standard as for samples (Amount50 µL mix deAmount0 mL ). Then go directly toGo togo to step #2.6 . For the ultrapure water blanks (n=2), the same type of sampling flasks are filled with ultrapure waterDuration24:00:00 before sampling. Then they are treated using the same protocols as for samples. Elution of the loaded cartridges was carried out by gravity usingAmount10 mL of methanol followed byAmount10 mL of dichloromethane. The eluates were concentrated approximately to ca.Amount0.5 mL using a Turbovap II concentrator (Zymark, Hopkinton, MA, USA), then to dryness under a gentle nitrogen stream and finally reconstituted inAmount500 µL of methanol and filtered with aAmount1ug mL GHP‱Thikness13 mm syringe filter (Pall Corporation). The extracts were injected in an Agilent 1290 LC coupled with and Agilent 550 QTOF system.

1d
Parameters framed by Legal and Regulatory Requirements:
Parameters framed by Legal and Regulatory Requirements:
Using the EU Drinking Water Directive:
Organic contaminants - DIRECTIVE 2008/105/EC OF THE EUROPEAN PARLIAMENT AND THE
COUNCIL of 16 December 2008 on environmental quality standards in the field of water policy.
Protocol references
Montes, R.; Méndez, S.; Carro, N.; Cobas, J.; Alves, N.; Neuparth, T.; Santos, M.M.; Quintana, J.B.; Rodil, R. Screening of Contaminants of Emerging Concern in SurfaceWater and Wastewater.
Effluents, Assisted by the Persistency-Mobility-Toxicity Criteria.
Molecules 2022, 27, 3915. https://doi.org/10.3390/molecules27123915