1. 2nd CHEMICAL MONITORING AND EMERGING POLLUTANTS (CMEP) PLENARY MEETING Task 3.1E (co-chaired by JRC and IT) Survey on available PTs, RMs and other QC tools

2. Task 3.1e Survey on available PTs, RMs and other QC tools
Task with contribution from:
EC-JRC-IRMM, Italy, FI, FR, SE, LU, BG, LT
The objective of Task 3.1E is to inform WG E about the status of presently available QC tools for laboratories dealing with the implementation of the WFD with regard to monitoring requirements (QA/QC-Directive 2009).
- Proficiency Testing schemes
- Certified Reference Materials
- Standard methods of analysis

3. QA/QC tools Proficiency testing schemes
“external assessment”
(Certified) Reference Materials
Traceability
Measurement uncertainty
Tools for QA/QC of analytical data
Compliance with the monitoring duties will imply the delivery of reliable measurements which accuracy poses a considerable challenge, considering the generally very low EQSs.
The tools needed for such purpose include appropriate CRMs, use of internationally recognised and validated methods and also participation in proficiency testing schemes, for an external assessment of performance.
Unfortunately, not all these tools are available for all priority substances
“Standardised methods”
prescribed methods/procedures
(sampling, method-defined parameters)

4. Mandate of 3.1e in short
First focus on the existing Priority substances
Future (soon) extension to “new” PSs (the list should be finalised and approved later this year)
Revision of EQS for some “old” PS foreseen + extension to other matrices (biota, sediment).
Always keeping in mind the requirements of the QA/QC Directive 2009…

5. New survey on available CRMs
Previous lists of this kind date back to 2003 (JEM article) and 2006 (D15 EU FP6 EAQC-WISE project).
All WFD relevant matrices included: not only water, but also sediment and biota CRMs.
We targeted an exclusive inclusion of CRMs* with some compromise (certificate had to be available, but uncertainty and metrological traceability were not always provided).
Marine water, sediment and biota CRMs have also been included for a more general overview and to account for the limited number of matrix-matched CRMs.
* definition given in ISO Guide 30/Amd 1 (2008)

6. New survey on available CRMs
Inclusion of the 8 other pollutants not categorised as PS but having nevertheless an EQS
Table with matrix CRMs
Table with discontinued matrix CRMs
No (!) Table for pure compounds or solutions CRMs
List of CRMs producers and/or distributors

7. Some highlights (1) ? No water CRMs for organics
common approach used is the “reconstitution”
mimicking the real matrix
To start soon: EMRP ENV08, Traceable measurements
for monitoring critical pollutants under the WFD
Biota CRMs for organics
Available from different producers, based on aquatic plants
or animals
So far, only for two PS, HCB and HCBD, EQS are established in
prey tissue (10 µg/kg, EQS directive 2008).
Two frozen fish tissues (SRM 1946 and 1947) available from
NIST are certified around the EQS value.
Primary issue for biota RMs is the "commutability“ =
close mimic to the routine sample. ?
NIST was the first producer introducing fresh-frozen CRMs (early 1990s)
QUASIMEME program is providing wet PT samples
IRMM is also working in producing fresh texture-improved CRMs.
CRM
123

8. Some highlights (2) Sediment CRMs for organics
Available from different producers
Absolute number of CRMs is higher than for the biota,
but number of PS covered about the same
NRC-CNRC and NWRI, producers from Canada, discontinued the largest number of sediment matrix CRMs (over the past five years).
This gap was only recently covered by materials from WEPAL, but with informative values
and almost always no uncertainty.

9. Some highlights (3) water CRMs for priority metals
EQSs refer to the dissolved concentration
General situation much more comfortable than for organic PS.
For Hg at or below the level of the EQSs
(0.05 µg/L as AA and 0.07 µg/L as MAC),
only 3 CRMs are available
ERM-CA615 (JRC-IRMM)
BCR-579 (JRC-IRMM)
ORMS-4 (NRC-CNRS)
ERM-CA615, groundwater with a certified value of ± µg/L
BCR-579, coastal seawater with a certified value of 1.9 ± 0.5 ng/kg,
NRC-CNRC, ORMS-4, river water with a certified value of 22 ± 1.6 pg/g
CRM

10. Some highlights (4) biota CRMs for priority metals
Large number of CRMs
EQS is established in prey tissue for Hg as 20 µg/kg (EQS directive 2008).
at least a couple of CRMs are available from NIST around this content
level, both freeze-dried
SRM 1974b (mussel tissue)
SRM 1566b (oyster tissue)
sediment CRMs for priority metals
Sufficient number of representative sediment CRMs

11. WATER CRMs

12. BIOTA CRMs

13. SEDIMENT CRMs

14. Pure compound/solution CRMs
The compilation of a similar list to the matrix CRMs
turned out to be a “mission impossible”
Compared to the previous survey, a number of pure PS
finally appeared on the market
PBDEs by NIST in 2006
SCCPs by Chiron in
Several standard CRMs are provided by the CERI.
Among others, calibrants for benzene, 1,2-dichloroethane,
dichloromethane, DEHP, nonyl and octylphenols.
Purity issue

15. Isotope Pure compound/solution CRMs
All organic PSs (except chlorfenvinfos and SCCPs) are now available also as labelled compounds (from Aldrich, Fluka, LGC, C/D/N Isotopes, CIL…).
“Inorganic spikes” used in inorganic isotope dilutions applications, are also widely available.

16. Next CMEP meeting November 2011 JRC-IRMM, Geel, Belgium
JRC-IRMM location
Next CMEP meeting
November 2011
JRC-IRMM, Geel, Belgium

17. Looking forward to welcome you all!