1. DICLOFENAC Validation according to 17025 requirements
EQS: 0.1 µg/L in surface water
0.01 µg/L in other (coastal) waters
Validation according to
17025 requirements
SPE-LC-MS/MS method
Sample volume: 1L
Limit of detection (0.1 ng/L)
LOD=b+3SD, where b is the mean value of blank samples (n=15)
and SD is their relative standard deviation
Limit of quantification (0.2 ng/L)
LOQ=b+10SD, where b is the mean value of blank samples (n=15)
Linearity
Evaluated by R2 and residual plots of extracted spiked calibration standards on 5 different days
Working range ( ng/L)
Defined by the LOQ and the highest point of calibration curve
Recovery (71.2%)
Trueness
Assessed by significance test (t-test) on 15 replicate quality control samples (QCs) at low (2.91 ng/L) and high (87.3 ng/L) spiking level)
Repeatability and Intermediate Precision
Assessed by one-way ANOVA on fifteen replicate quality control samples (QCs) at at low (2.91 ng/L) and high (87.3 ng/L) spiking level)
Extract stability
Evaluated after one week storage at 4°C in the dark.
The acceptance criteria established requires the concentration fall within 2 SD
Sample stability
Evaluated in water samples stored at 4°C for 38, 83 and 96 days.
Uncertainty budget

2. E2 and EE2 Validation according to 17025 requirements Parameters E2
AA-EQS
400 pg/L
35 pg/L
LOQ (at 1/3 EQS)
Yes No
Recovery
>75%
Sample volume: 1 L
Parameter
Same approach than used for diclofenac method validation
Limit of detection
Limit of quantification
Linearity
Working range
Recovery
Trueness
Repeatability and Intermediate Precision
Extract stability
Sample stability
Uncertainty budget
Validation report for E2 in 1 L water sample foreseen within 2014
EE2 E2

3. Sample volume: 10 L Mariani Box 1 2 3 4 5 6 Parameters E2 EE2 AA-EQS
Battery 12 V
Flow-meter/Counter
Pump (Flow rate: L/min)
Holder-SPE: adsorbent
Water Sampling line
Waste
Mariani Box
Isochronous stability experiment
(0-10 weeks) 1 2 3 4 5 6
30 cm
Parameter
Ad hoc validation scheme considering the complexity of 10 L sample volume manipulation
Limit of detection
Limit of quantification
Linearity
Working range
Recovery
Trueness
Repeatability and Intermediate Precision
Extract stability
Sample stability
Uncertainty budget
Validation report for E2 and EE2 in 10 L water sample foreseen within end of March 2015
In details, my presentation will touch the following topics:
After the presentation of JRC role and mission, I will briefly cite the regulations addressed for our role execution before entering into details of the watch list pilot exercise currently on-going, the presentation of the soft-shell concept, of the European Innovation partnership on water and of the Information Platform for chemical monitoring.
Parameters E2
EE2
AA-EQS
400 pg/L
35 pg/L
LOQ (at 1/3 EQS)
Yes
Recovery
>75%
20 May 2019