TITLE: WATER PRODUCTION FOR AWARE (Organic Contaminants)
AUTHORS: Celia Manaia

[DESCRIPTION]
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.

[STEPS]
SECTION: Organic Contaminants:
1. The water production for AWARE main activities includes three stages – disinfection by ultraviolet C radiation (UVC), storage for720 min-1440 min(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.

 

SECTION: Organic Contaminants:
1.1. Sampling, Processing, and Analyses 

Water samples are collected (see Figure 2) and processed within a360 mininterval, before being shipped for the partner responsible for the analyses (Table 1). In case no processing is needed, samples are frozen and stored at-80 °Cwithin180 min.

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.,5 mgO3) - MITO3X technology - (G) 
- Effluent of the vacuum UV oxidation (VUV) (H) 
- Effluent of reactive storage / Influent of the recirculation aquaculture system (RAS) (I) ù

 

SECTION: Methods: The section below summarises the procedures used for analytical control – detailed protocols are annexed to this protocol.
2. Organic Contaminants: 

Analysis:  Screening of Organic Contaminants in Water.
SECTION: Methods: The section below summarises the procedures used for analytical control – detailed protocols are annexed to this protocol.
2.1. Methods:  Solid-phase extraction 

2.1 Sample filtration (0.45um PVDF). 
SECTION: Methods: The section below summarises the procedures used for analytical control – detailed protocols are annexed to this protocol.
2.2. Collect200 mLof the filtered water sample (e.g. volumetric flask or beaker) and spike with 50 µL of an internal standard solution. Produce two200 mLreplicates per sample. Mix well after the internal standard is added.  
SECTION: Methods: The section below summarises the procedures used for analytical control – detailed protocols are annexed to this protocol.
2.3. Cleaning/Conditioning of the cartridges (OASIS HLB200 mg) 
 
3.1. Pass5 mLof MeOH 

3.2. Pass5 mLof ultrapure water 
SECTION: Methods: The section below summarises the procedures used for analytical control – detailed protocols are annexed to this protocol.
2.4. Pass the200 mLof sample

SECTION: Methods: The section below summarises the procedures used for analytical control – detailed protocols are annexed to this protocol.
2.5. Rinse the volumetric flask or beaker that contained the sample with 2x10 mLof ultrapure water, which are then passed through the cartridege 

SECTION: Methods: The section below summarises the procedures used for analytical control – detailed protocols are annexed to this protocol.
2.6. Drying the cartridge resin (e.g. N2 flow for30 min)

SECTION: Methods: The section below summarises the procedures used for analytical control – detailed protocols are annexed to this protocol.
2.7. Store the cartridges in a freezer (-20 °C) 


All samples are to be processed in duplicate.


For the cartridge blanks (n=2): start with , and then spike directly on the cartridge the same amount of internal standard as for samples (50 µLmix de ).  Then go directly to .
For the ultrapure water blanks (n=2), the same type of sampling flasks are filled with ultrapure water1440 minbefore sampling. Then they are treated using the same protocols as for samples.


Elution of the loaded cartridges was carried out by gravity using10 mLof methanol followed by10 mLof dichloromethane. The eluates were concentrated approximately to ca.0.5 mLusing a Turbovap II concentrator (Zymark, Hopkinton, MA, USA), then to dryness under a gentle nitrogen stream and finally reconstituted in500 µLof methanol and filtered with a1ug mLGHP‱ syringe filter (Pall Corporation). The extracts were injected in an Agilent 1290 LC coupled with and Agilent 550 QTOF system. 

SECTION: Parameters framed by Legal and Regulatory Requirements:
3. 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.