CORDIS Archive

Organic contaminants in water.

1. CONFORMITY WITH THE WORK PROGRAMME

This topic falls under the Competitive and Sustainable Growth Programme, generic activity Measurement and Testing. Specifically, it is related to Objective GROW-2000-6.3. Support to the Development of Certified Reference Materials for which expressions of interest have been called.

2. KEYWORDS

Water quality, EU Water quality Directives, Monitoring, Feasibility study, Quality Assurance, Quality Control, European Certified Reference Materials, Performance Testing

3. SUMMARY OF OBJECTIVES AND JUSTIFICATION

The objective of the project is the development of the ability to produce and certify reference materials related to the monitoring of organic contaminants in water quality measurements. These CRMs are required to ensure the comparability and traceability of measurements of analytical test laboratories.

The intended CRMs should be adequate for measurements relevant to levels and methods used in support of European legislation.

This feasibility study should determine the conditions and processes that are necessary to produce and certify key organic contaminants in water reference materials, which will directly benefit both users of such materials and the general public in giving assurance on health and consumer safety concerns.

4. BACKGROUND

In 1998, Council Directive 98/83/EC on the quality of water intended for human consumption was adopted. This directive is an update of Council Directive 80/778/EC and its revision is in response to the scientific and technological progress made since 1980, on the need to monitor water intended for human consumption. The new directive creates a more flexible and transparent legal framework for Member States to address failures to meet the standards.

To ensure comparability and traceability of these measurements the regular use of reference materials is one of the cornerstones for achieving accurate analytical measurements. Such measurements may have huge economic impact in areas such as health, environment, trade and law enforcement, and it is in these areas that reference materials have been described as 'strategic tools for the European Union'.

Although this project has as its major objective the investigation and eventual production of reference materials for organic contaminants in water to meet the needs of Council Directive 98/83/EC, the study will also support other regulatory programmes within the environmental monitoring area.

With the imminent expansion of the community by the accession countries - the first six new members may join the EU from 2003, they will require assistance from the EU to ensure that they are able to comply with the requirements of analytical quality measurements. The availability of suitable reference materials will be a necessity if these programmes are to be successfully implemented.

Literature studies have shown that only a few matrix reference materials for water are available. In a Dutch study, 28 examples of CRMs were found, however, the materials were mainly for inorganic parameters 1. Other studies have highlighted that the need for aqueous reference materials is even more acute and that their inclusion in monitoring and research programmes that support European legislation is substantial 2.

A recently published (1999) report by the European Environment Agency (EAA) on the water quality of lakes and reservoirs in the EAA area 3, confirms that there is an urgent need for reference materials as the data presented appeared to be incomplete and outdated. This lack of comprehensive information may have its origin in how the EAA and the National Focal Points gather these data, and in the very different situations experienced on a country by country basis, but it may well indicate the scarcity of comparable data and measurements being carried out. On this basis there is a strong argument that a European wide Proficiency testing scheme is also needed and that any materials identified and subsequently produced from this programme would offer suitable samples for measurement.

The Council Directive 98/83/EC lists a large number of organic parameters that should be determined. For purposes of clarity it is considered necessary to define the parameters within "groups" based on distinct chemical and/or physico-chemical behaviour.

Two additional "groups" of organic contaminants are also considered to be important. Although not specifically defined, they could be considered to fall under the Article 1 objective which states that " The objective of this Directive shall be to protect human health from the adverse effects of any contamination of water intended for human consumption by ensuring that it is wholesome and clean".

"Group 2" being : Chlorophenols , Phthalates - (including ethoxylates and nonylphenol)

"Group 3" :
Consideration will also be given to the class of parameters defined as "pesticides", although some generic grouping is given in the directive i.e. organic insecticides, herbicides, fungicides, nematocides etc. The major problem is likely to be the diversity of analytical techniques and extraction procedures required for such a wide indistinct group of organic materials. Problems will also result from the "compound mixtures" that may be required by the analytical community, to meet the specific needs of the local area (i.e. different pesticides will be used in different areas depending upon the type of agricultural practices of the region).

The selection of parameters and/or groups of substances also goes a long way to meeting a recent proposal on Priority substances in the aquatic environment from the European Parliament and a Council Decision which establishes, in the context of the Water Framework Directive, an initial list of 32 priority substances (or groups of substances) believed to pose a risk to aquatic ecosystems and consequently to human health. 4

5. ECONOMIC AND SOCIAL BENEFITS

The project will contribute to the improvement in the quality of water used for human consumption and will provide tangible evidence on traceability and comparability of data throughout the community.

The project has direct relevance to the implementation of EU Directives aimed at improving water quality. It has particular benefit to the protection of human health, the environment and to the costs related to the maintenance and improvement of water quality throughout the European community.

To quantify and to provide accurate information on the possible economic benefits arising from the project is extremely difficult, although examples of pollution incidents that have occurred indicate that in monetary terms figures such as 250billion Euros could be involved. The social impact of such incidents is also difficult to estimate with accuracy, but in the consumer society any adverse situations often lead to significant problems.

The project also considers the special situation of the Accession Countries. The participation of representative laboratories from these countries will help in their approach towards meeting the requirements of European quality standards and existing EU-legislation. The project will also provide a measure, and allow evaluation of the current situation within the EU in relation to the "state-of-the art" in water analysis. This has implications in respect to international trade relationships dealingwith the quality of water for human consumption e.g. export/import of bottled waters, efficiency of water treatment processes, etc.

6. SCIENTIFIC AND TECHNOLOGICAL OBJECTIVES

The work arising from this project will have a number of scientific and technological objectives. There will need to be a thorough review of current practices used by the European analytical community for the analysis of organic pollutants in water. Data currently produced and reported to the community will require evaluation and the use of the European PT-database currently under development at BAM is seen as one of several possible ways of assessing the current stature of measurement comparability for the organic compounds specified by the Directive.

In parallel to the above study, desk research and limited practical work will be undertaken either by a reference laboratory or by a core group of expert laboratories, to obtain information on the feasibility of producing suitable matrix reference materials. Following the feasibility study, information will be obtained on the homogeneity, stability, storage conditions, packaging, etc., for the range of materials considered suitable for development into full-scale reference materials.

The work should lead to the ability to produce and certify reference materials with the following specification:
- A between sample homogeneity of < 2%
- A long term stability of > 10 years
- Certification of concentrations with uncertainties (k=2) < 5%

7. IMPORTANT ADDITIONAL INFORMATION

An addendum giving general information related to the development of CRMs in the sense of the proposal is attached.

1. NNI-ANVM PD206- development of reference materials for ground-, surface- and wastewater containing organic compounds. - A feasibility study. D Verkuil NMi February 2000.
2. Development of reference and test materials for organic contaminants in water, David E Wells, The Analyst, 1998, (005), 983-989.
3. General considerations on the preparation of water certified reference materials, M.J.Benoliel, P. Quevauviller, The Analyst, 1998, (005), 977-979.
4. European Inquiry on the Use and Needs for Reference Materials organised by the European Commission' Standards, Measurements and Testing Programme, P. Quevauviller, 1998
5. QUASIMEME project - Quality Assurance of Information for marine environmental monitoring in Europe, Sponsored by the commission of the European Communities. Marine Pollution Bulletins Issues 1-5
6. Biological and Environmental Reference Materials conferences. BERM-5, 6 and 7 conferences. (Keulen 1992, Hawaii 1994 and Antwerp 1997.
7. Equate - Equal quality of Water related analyses throughout Europe, R.A.L. Peerboom, W.P Cofino, IVM, RIZA, E-99/11 May 1999
8. Reference materials: an inquiry into their use and prospects in Europe, P. Quevauviller, European Commission, Trends in Analytical Chemistry 1999 Vol 18 No.2
9. New certified reference materials for the quality control of groundwater monitoring. P. Quevauviller, M.J. Benoliel, K. Andersen, J.Merry, Trends in Analytical Chemistry 1999, Vol 18 No 6 pp376-383
10. Proposal for a European Parliament and Council Decision. COM(2000)47,2 Feb 2000.
11. Water Quality of lakes and reservoirs in the EAA area. J. Leonard (Office International de l'Eau) and P. Crouzet (Institut Francais de l'Environnement) 1999.

Research in support of the development of CRMs is an objective of the Growth Programme. The modality for this research is a shared cost action on RTD (cf work programme Competitive and Sustainable Growth). The guidelines for the submission of the proposal are laid down in the Guides for Proposers.

In addition to the requirements for research on a specific topic that are laid down in the supporting document*, there are general requirements for the development of CRMs. These requirements are described below and are in addition to the general requirements for shared cost actions, as described in the guides for proposers and the model contract.

The requirements have been divided in 2 major parts:

I) Description of the work

Research on CRMs consists of the development of the ability to produce and certify reference materials. The actual production of the CRM is not part of the research but is part of the exploitation of the result(s).

In the first phase of the research project the certification strategy should be elaborated (development of the materials and methods for characterisation), in the second phase of the research project the ability to produce and certify should be demonstrated and finally the specifications for the final CRM should be set.

The development of a CRM normally consists of 4 major parts:

1. Development of the know-how required to produce (and package) the future CRM

• specify the sort of material that is most likely to meet both the targets laid down in the supporting document and be suitably homogeneous, stable, safe to handle, and acceptable in cost
• identify the options available for selecting / preparing such a material
• take into account special storage and / or transport requirements existing for certain types of materials
• develop of methods for production / selection and preparation, homogenisation, stabilisation, protection and packaging of material as required, to enable the production of a CRM which will be fit for purpose
• if a material needs to be altered substantially (e.g. freeze drying), or when it is artificially spiked with the substance of interest, it is necessary to check if the material behaves in the same manner as the routine samples when applying the relevant methods of measurement.
• Ensure the availability of a suitable reconstitution procedure if a material will need reconstitution

2. Development of the methods needed for future certification of the material

Certification can be performed according to different criteria. The research will define which certification route, following internationally recognised quality requirements and standards, will be followed.

Certification on the basis of pure substances

• If the CRM is a pure substance the preparation methods should be such that the presence of impurities are reduced to a minimum. Additionally the substance should be tested for impurities by carefully selected methods at least in two laboratories.

Certification on the basis of preparation data

• When dealing with a synthetic CRM and a quantity which is directly related to (or depends in a well-established way on) composition, examine if preparation under metrological conditions and certification on that basis (e.g. using gravimetric data) is possible
• Identify nevertheless a method of measurement that can be used as an independent check for large errors

Certification on the basis of measurements - method-dependent quantities

• If the quantity to be certified is defined on the basis of a specific (standard) sample treatment or method of measurement, certification will be based on statistical processing of results produced by a sufficient number of laboratories (e.g. 12 - 15), which follow strictly the standard protocol but include all variability which is allowed by the protocol (do not use common sources of calibrants, reagents, ... unless these will be available to the future CRM users and prescribed in the protocol). Such protocol may have to be developed
• Work may be necessary to achieve an acceptable level of reproducibility

Certification on the basis of measurements - method-independent quantities

• As error-free, matrix-independent, calibration-independent methods are exceptional, the basis for certification will usually be an agreement between different methods and different laboratories, applied under conditions of independence which rule out the risk of a common systematic error. Methods with a high potential for matrix-independence and/or calibration-independence (e.g. IDMS for determining polyisotopic elements) should be included if available
• it may be necessary to perform a substantial collaborative method improvement (to achieve the required level of agreement between methods and between laboratories), or even research (method development) to achieve the required ability to measure. Guidance for collaborative method improvement is given in the BCR Guidelines*

3. Demonstration of the feasibility of the CRM production

• prepare a small batch of material, similar to that intended to be prepared as a CRM, using the method intended to be used to prepare the actual reference material
• Check the fitness for purpose:

Guidance for homogeneity and stability testing is given in the BCR Guidelines.

• Use the test batch to mimic the certification of a future CRM in a measurement campaign, designed as a certification exercise (see BCR Guidelines)
• If the results show that a CRM prepared and certified as in the test round is not good enough, then the development work (1. or 2. above) must be recommended

4. Reporting of detailed and realistic specifications for the future CRM

The reporting requirements are set in the guidelines for reporting. In addition to the Final Technical Report the coordinator should prepare an overview of all the results, as foreseen in the Technical Implementation Plan. In this report the outcome of the research that sets the boundaries for the future CRM production should be given preferably in the form of a technical data sheet. It should contain the following information:

- form / type of samples (with preference for individually packed portions for single use)
- lyophilisation and reconstitution procedures
- specify bottling, labelling, packing, storage and transport requirements
- identify any legal restrictions on the transport of such material and need for safety labelling, collect data for material safety data sheets
- magnitude of the quantity of interest (acceptable range)
- acceptable uncertainty on the certified value for an individual sample (this includes at least: acceptable uncertainty on the mean value for the entire batch, and acceptable level of inhomogeneity of the batch)
- method requirements (if the CRM is method dependent)
- acceptable magnitude of other quantities
- an estimate of the quantity of CRM that should be produced as well as an estimate of the production costs.

II) Implementation of the objectives of the research

As for all shared cost contracts the contractors are obliged to exploit the knowledge arising from the project. In the case of research on CRMs the contractors are, among others, obliged to assure that the CRM is produced and certified within a reasonable time limit (article 10 of Annex II General Conditions of model contract).

The "Technological Implementation Plan" (TIP), which has to be prepared in any RTD project of the 5th Framework Programme, shall explain the actions planned to assure that results of the project will be exploited. In case of CRMs this TIP has to outline the strategy for the CRM production, certification and marketing within a reasonable time frame, at a reasonable cost and according to internationally recognised quality requirements. A draft TIP has to be available at the project mid-term. Options, ranging from production by the consortium to production by a third party or the Commission, will be explored in consultation with the Commission Services.