CMA-3 CMA-3

Support to StandardisationSupport to Standardisation66thth CMA Plenary Meeting CMA Plenary Meeting

under the German Presidencyunder the German Presidency

Berlin, 02Berlin, 02ndnd May 07 (modified: 03 May 07 (modified: 03rd rd May 07)May 07)modified according to discussions at the meeting,modified according to discussions at the meeting,

and further data supplied by B, A, DE are considered and further data supplied by B, A, DE are considered

Ulrich Borchers and Peter Lepom Ulrich Borchers and Peter Lepom

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Agenda

Introduction on Requirements for Methods From the WFD From the EQS Daughter Directive From the QA/QC COM decision

State of the Art of standardised analytical methods Modified AMPS table / Substance guidance sheets CEN/UBA enquiry 2005 / Comments NL, UK Ongoing standardisation activities

Definition of needs and further steps Standards for the WFD Annex V Research needs (new methods) Revision and optimisation of existing methods

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CMA 2007 – 2009 – Tasks and Deliverables

CMA-1Exchange of best practices

STRATEGIC CO-ORDINATION GROUP

PLENARY CMA(GW, SW/MW)

CMA-2QA_QC

CMA-3Standardisation

(CEN TC/230)

• Sharing best practices• Identification of gaps and needs• Analytical methods, sampling• Practical exercises• Sediment and biota

• Follow-up of COM decision• Discussion of common strategy (EAQC-WISE)

• Identification of standards• Follow-up of CEN work• Links with RTD

WG C or WG E(joint meetings)

WG E

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CMA-3 Core Activities

Identification and evaluation of standardisation needs and appropriate actions related to them Discussion on standardisation needs

related to WFD chemical monitoring Establishment of lists of

Existing standards fit for purpose Standards that need to be revised Standards that need to be developed

Proposal of a) Existing standards for adoption b) Development of new standards mandated to CEN

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WFD Requirements for analytical methods

Article 8.3 Technical specifications and standardised methods for

analysis and monitoring of water status shall be laid down in accordance with the procedure laid down in Article 21

Annex V, paragraph 1.3.6 the provision of chemical data by MS shall be ensured by

analytical methods that conform to relevant international or national

standards or to other national or international standards

or alternatively by analytical methods that are not standardised but provide data of equivalent or better scientific quality and comparability than standard analytical methods

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Requirements from the EQS Daughter Directive*

EQS values (Article 2) In conjunction with Limit of Quantification (LOQ) requirements

in the QA/QC COM decision

Monitoring based on annual averages … and as a maximum allowable concentration

That means: time integrating sampling methods (e.g. passive samplers) offer important and new possibilities

But these methods are not directly intended for compliance checking in whole water samples

Matrix “Whole water”, SPM, sediment, biota

Indicator parameters* Proposal for a Directive of the European Parliament and of the Council on environmental

quality standards in the field of water policy and amending Directive 2000/60/EC

key point 1

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Requirements from QA/QC COM decision

Sampling and sample treatment … shall follow recommendations of relevant

international guidelines and standards, including relevant parts of ISO 5667

Limit of quantification (LOQ) … equal or below a value of 0.3 of the relevant

quality standards (EQS) LOQ versus Lower Limit of Application (LLOA)

LOQ = lab specific performance value LLOA = method specific performance value

Relative Target Uncertainty … a relative target uncertainty of 50% measured at

the level of the relevant EQS

key point 2

key point 3

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Agenda

Introduction on Requirements for Methods From the WFD From the EQS Daughter Directive From the QA/QC COM decision

State of the Art of standardised analytical methods Modified AMPS table / Substance guidance sheets CEN/UBA enquiry 2005 / Comments NL, UK Ongoing standardisation activities

Definition of needs and further steps Standards for the WFD Annex V Research needs (new methods) Revision and optimisation of existing methods

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State of the Art of standardised analytical methods

Basis of information on the performance of methods AMPS table accepted by EAF-7

modified by JRC IES and EAQC-WISE in March 2007 CEN/UBA enquiry on performance criteria (LOQ etc.)

among labs from Europe A problem of the statistical evaluation was that the

responses of labs were not balanced regarding the MS Emphasis on labs in F, Scandinavia and D

At the time being: some further enquiries among labs in DE (Friederike Vietoris, LAWA), UK (John Batty, EA) and NL (Joan Staeb, RIZA) A (Karin Deutsch) B (Peter van Caeter)

concerning performance criteria of standard methods

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Table of methods and their performance

Data from: CEN D UK B A NL TotalOK

questionablenot possible marine

waters

not possible

Priority Substance Status Status Status Status Status Status Status

considering LOQ, U, SPM

Alachlor 1 1 1 2 1

Anthracene 2 1 2 2 1

Atrazine 1 1 1 1 1 1

Benzene 1 1 1 1 1 1

Pentabromodiphenylether 4 4 4 4 4 3

Cadmium and its compounds

Class 1: < 40 mg/l CaCO3 1 1 3 2 3 1 1

Class 2: 40 to < 50 mg/l CaCO3 1 1 3 2 3 1 1

Class 3: 50 to < 100 mg/l CaCO3 1 1 3 2 3 1 1

Class 4: 100 to < 200 mg/l CaCO3 1 1 3 2 3 1 1

Class 5: > 200 mg/l CaCO3 1 1 3 2 3 1 1

C10-13-chloroalkanes 4 4 4 2 3

Chlorfenvinphos 2 1 1 1 2 1

Chlorpyrifos (-ethyl, -methyl) 2 1 1 1 2 1

1,2-Dichloroethane 1 1 1 1 2 1

Dichloromethane 1 1 1 1 2 1

Di(2-ethylhexyl)phthalate (DEHP) 2 1 3 1 2 1

Diuron 1 1 1 1 1 1

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Table of methods and their performanceEndosulfan 3 3 3 4 3 4 3a

Fluoranthene 2 1 2 1

Hexachlorobenzene 2 1 1 3 2 1

Hexachlorobutadiene 2 1 1 2 1 2 1

Hexachlorocyclohexane 2 3 3 2 3 3 3a

Isoproturon 1 1 1 1 1 1

Lead and its compounds 1 1 1 1 1

Mercury and its compounds 1 1 3 2 3 1 1

Naphthalene 1 1 3 2 1 1

Nickel and its compounds 1 1 1 1

Nonylphenols 2 1 1 1 1

Octylphenols 3 3 1 2 3a

Pentachlorobenzene 3 3 1 3 3 3 3a

Pentachlorophenol 2 1 1 1 1

Polyaromatic Hydrocarbons (PAH´s)

Benzo(a)pyrene 2 1 1 1 2 1

Benzo(b)fluoroanthene 2 1 1 3 2 1

Benzo(k)fluoroanthene 2 1 1 3 2 1

Benzo(g,h,i)perylene 3 3 3 4 4 3

Indeno(1,2,3-cd)-pyrene 3 3 3 4 4 3

Simazine 1 1 1 1 1 1

Tributyltin compounds 3 3 3 4 4 3

Trichlorobenzenes 1 1 1 2 1 2 1

Trichloromethane 1 1 1 1 1 1

Trifluralin 2 2 1 3 2 2

DDT 2 1 3 2 1

para-para-DDT 2 1 2 2 1

Aldrin 2 2 2 2

Endrin 3 2 3 2 2

Isodrin 3 2 3 2 2

Dieldrin 3 2 3 2 2

Carbontetrachloride 1 1 1 1 1

Tetrachloroethylene 1 1 1 1 1

Trichloroethylene 1 1 1 1 1

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State of the Art of standardised analytical methods

Lack of sensitivity of some methods (LLOA) and/or LOQ to high

Statements in the standards Practical experience in many labs

See various enquiries

Published LOQs and U are sometimes Too optimistic (determined in ultraclean sample) Too pessimistic (better with modern equipment) In any case they are lab specific

We have no LOQ’s and U in the standards Lack of reliable data on Measurement Uncertainty (U) There is a need to assess realistic LOQ and U values

but mainly in cases of doubts In labs from different MS

e.g. by in house tests or by ring tests

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State of the Art of standardised analytical methods

Pre-condition Normal accredited and well qualified laboratories

should be able to perform the monitoring

Lack of representativeness of the Validation trials in the existing standards Matrix of tested waters not suitable Concentration range much above EQS values

No or not clear statements on the suitability of the methods for “whole water samples” Water with remarkable SPM content

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Summary (41 substances)

1st cat.: Everything is OK for about 10 substances

2nd cat.: Lack of data for LOQ, U,or SPM at the time beingbut high probability that collected data will be OK

for about 20 substances

it is likely that for about 30 substances we can show in due course that they are fit for purpose

only those methods should be mentioned where suitability is commonly agreed!

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Summary (41 substances)

3rd cat.: Existing standards are not suitable:(there is at least 1 of 3 criteria not OK: LOQ, U, SPM)

Problems with compliance checking for all waters TBT PAHs (6-ring-PAH) Triflualin

Problems mainly for marine waters HCH (4 relevant isomers) Octylphenol Endosulfan (a+b) Pentachlorobenzene Aldrin, Dieldrin, Eldrin, Isodrin

4th cat.: Standardised method does not exist: C10-13-chloroalkanes (SCCP) Pentabromodiphenylether (PDBE)

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Ongoing standardisation activities with WFD relevance

Polyaromatic Hydrocarbons (PAH´s) GC MS method new pre-treatment steps for waters containing SPM ISO TC 147 / SC 2 / WG 19 (convenor: Van Zonen, NL)

ISO/CD 28540

Organochloropesticides (OCP) e.g. DDT, Pentachlorobenzene Aldrin, Endrin, Isodrin, Dieldrin ISO TC 147 / SC 2 / WG 53 (convenor: Van Zonen, NL)

only first WD and some experiments available no ISO project number at the time being

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Agenda

Introduction on Requirements for Methods From the WFD From the EQS Daughter Directive From the QA/QC COM decision

State of the Art of standardised analytical methods Modified AMPS table / Substance guidance sheets CEN/UBA enquiry 2005 / Comments NL, UK Ongoing standardisation activities

Definition of needs and further steps Standards for the WFD Annex V Research needs (new methods) Revision and optimisation of existing methods

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Definition of needs and road map (adjusted time table according to comments of PQ)

Task 1: Discussion of the modified AMPS table(s), the list with performance

data from UK, NL, DE, A, B (and others), the suitability of methods for SPM containing samples in CEN TC 230 / WG1 report with relevant conclusions 15th June 2007, Vienna meeting

Drat list of methods with consolidated data for adoption by CMA Plenary

30th June 2007 Task 2:

Proposal of a list of standards for Annex V Only those methods where suitability and performance criteria are

commonly agreed at CEN and CMA level Comments by relevant groups until end of July 07 Adoption of the proposal at next CMA plenary meeting

Identification of methods for further discussion / collection of further information 16th October 2007, Brussels

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Definition of needs and road map (adjusted time table according to comments of PQ)

Task 3: Definition and agreement on the list of methods to be

developed and or revised in 3 parts: 1) New methods

pre-normative research 2) Methods with enhanced sensitivity

optimisation / revalidation 3) Methods with proved suitability for SPM

containing waters (if relevance for analysis of SPM fraction is given)

optimisation of pre-treatment / revalidation

31th July 2007, Commenting by e-mail

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Definition of needs and road map (adjusted time table according to comments of PQ)

Task 4: Definition and agreement on

a new ISO standard (or TS) on passive sampling techniques

On the basis of BSI PAS 61:2006 Launching of a NWIP at ISO

TC 147 / SC 6

Technical discussion on 15th June 2007, Vienna CEN meeting

Submission of NWIPto ISO CS 31st July 2007

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Definition of needs and road map (adjusted time table according to comments of PQ)

Task 5: Adoption of standards and mandates to CEN

Proposal of existing suitable standards to the WFD Committee for adoption by comitology and

Mandate on the development of new or revised standards involving pre- or co-normative research

mandated to CEN, followed by adoption by comitology

31st July 2007