Chemical Monitoring On Site (CM Onsite) organised by NORMAN Association

and JRC in support of CIS WFD

NORMAN Interlaboratory study (ILS) on passive sampling of emerging pollutants

Branislav Vrana

Water Research Institute, Slovakia

branovrana@gmail.com

Activities of NORMAN network in passive sampling 2009-2011

An expert group meeting in 2009

A position paper “Passive sampling of emerging pollutants in the aquatic environment: state of the art and perspectives” in 2010

An interlaboratory calibrationstudy in 2011

www.norman-network.net

Interlaboratory calibration study in 2011

• present variability in data by comparing results from various passive samplers sent by participating laboratories exposed to water at a single (reference) site

• Target substances:– polar pesticides - 19 participants– Pharmaceuticals – 17 participants– steroid hormones – 15 participants – Triclosan - 8 participants– bisphenol A - 11 participants– PFOA, PFOS - 8 participants– PBDE -16 participants

• 30 participants from commercial, academic and regulatory laboratories

Silicone stripsCONTACT: branovrana@gmail.com

Interlaboratory study DESIGN

• a sampler comparison exercise

• extended to cover individual aspects in the passive sampling process– analytical comparability– comparison with spot sampling

Study design 1. Passive samplers from participants

Coordinator

Participant 1

Participant 2

Participant 3

Participant 4

Sampler 3

Sampler 2

Sampler 1

for selected analyte/analytes

Sampling site -sampler exposure

Sampler 1 Sampler 2

Sampler 3 Sampler 4

Sampler 4

Quasimeme

Report to databaseng/sampler of compound Ang/cm2 sampler of compound Ang/L water of compound Acalculation procedure for compound A

Study design2. Standard solution

Coordinator

Participant 1

Participant 2

Participant 3

Participant 4

send to coordinatorCentral laboratory

S Standard solution

S S SS

purchase standardprepare a QC solutionprepare multiple vials (according to participant registration)check homogeneitysend to coordinator

S

S

S

S

distribute standards

for selected analyte/analytes

Quasimeme

Report to databaseng/ml of substance A

Study design3. Provided passive samplers

Coordinator

Participant 1

Participant 2

Participant 3

Participant 4

for selected analyte/analytes

Sampling site -sampler exposure

ProvidedsamplerProvided

sampler Providedsampler

Providedsampler

Buy

or

pre

pa

re

Providedsampler

Providedsampler

Providedsampler

Providedsampler

Providedsampler

Providedsampler

Providedsampler

Providedsampler

1.

2.

3.

3.

3.

3.

Central laboratory

Providedsampler

3.

Quasimeme

Report to databaseng/sampler of compound Ang/cm2 sampler of compound Ang/L water of compound Acalculation procedure

Report to databaseng/sampler of compound Ang/cm2 sampler of compound Ang/L water of compound Acalculation procedure

Study design4. Water samples

Coordinator

for selected analyte/analytes

Sampling site -sampler exposure

Central laboratory

W water sample

W

WW

WW

Wanalyse water samples

collectwater samplesend to centrallaboratory

Providedsampler Sampler 3

Sampler 2

Sampler 1

Sampler 4

ProvidedsamplerProvided

samplerProvidedsampler

Quasimeme

Report to databaseng/L water of compound A

NOT APPLICABLE FOR HYDROPHOBIC COMPOUNDSPBDE…

Interlaboratory study Steering group

Role Organisation Activity

Coordinator VUVH

Slovakia

coordination, sampling activities, logistics

Central laboratory for pesticides

Cemagref Bordeaux

France

Preparation of QC standards, analysis of provided samplers

analysis of water samples

Central laboratory for pharmaceuticals

ISM-LPTC, University of Bordeaux, France

Preparation of QC standards, analysis of provided samplers

analysis of water samples

Central laboratory for

Steroid hormones

Cemagref Lyon

France

Preparation of QC standards, analysis of provided samplers

analysis of water samples

Central laboratory for PFOS DG JRC IES Preparation of QC standards, analysis of provided samplers

analysis of water samples

Central laboratory for BDE RECETOX + DELTARES Preparation of QC standards, analysis of provided samplersNO analysis of water

Interlaboratory study Steering group

Role Organisation Activity

Central laboratory for

bisphenol A, triclosan

UK Environment Agency Preparation of QC standards, analysis of provided samplers

analysis of water samples

Sampling support Insitute of Public Health Ostrava, Czech Republic

Support at the sampling site

Sampling support

Data interpretation

RECETOX, Masaryk University, Czech rep.

Support at the sampling site

Participant registration

Data interpretation, report preparation

Participant interface for uploading results

Data-assessment and Reporting results

QUASIMEME Setup of the experiment into a database

Setup of sharepointsites

Instruction of laboratories how to get access to the sharepointsite

Introduce the lab specific contact information into the database.

Do the data-assessment

Produce figures and excel sheets of the assessed data.

Produce z-score lists for each individual laboratory.

Help desk facility with respect to data-transfer

Target compounds

Pesticides and their degradation products:

TerbutylazineDesethylatrazineDesethylterbutylazineAtrazineCarbendazimS-metolachlorDiuron

Pharmaceuticals:CarbamazepineDiclofenacIbuprofenNaproxenDiazepamAlprazolamKetoprofenAtenolol

Steroid hormones:

17-alpha-Estradiol17-alpha-Ethinylestradiol17-beta-EstradiolEstriolEstrone

Bisphenol ATriclosan

Brominated flame retardantsBDE 28, 47, 99, 100, 153 and 154

Fluorinated surfactantsPFOA, PFOS

Campaign timing: passive sampler deployment

Campaign number

Class number

Compoundclass

Registration deadline

Deadline for sending samplers + deployment equipment

Sampler exposure

Sampler deployment period

1 1 Pesticides 31.3.2011 16.5.2011 14 days 30.5.-13.6. 2011

2Pharmaceuticals

2 3Steroid hormones 31.3.2011 3.6.2011

14 days20.6.-4.7. 2011

4 PFOA PFOS

5Bisfenol A, Triclosan

3 6 PBDE 31.3.2011 27.6.2011 42 days 11.7.-22.8. 2011

Continuous water sampling

Sampler preparation for deployment

Sampler deployment

Sampler deployment

Sampler recovery

Sampler recovery

Sampler recovery

Onsite sampler cleaning and preparation

Laboratory preparation of provided samplers

Dissemination of results

3 rounds, May-August 2011

2012 – a workshop will be organised to disseminate results.

Study results

Statistics: 30 participating laboratories from Europe, North America and Australia

292 reference samplers for polar compounds distributed 80 reference samplers for PBDE 268 participant samplers for pesticides and pharmaceuticals285 participant samplers for PFOS, steroids, bisphenol A and triclosan132 participant samplers for PBDE

Total: cca. 1057 samplers were deployed at the reference site and distributed for analysis

The reporting deadline for laboratories has been set to 15th December

A dissemination workshop will be organised in 2012 organised by NORMAN + DG JRC