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INTERLABORATORY STUDIES General aspects TYPES OF STUDIES Method performance study Proficiency testing (several methods) Certification of reference materials.

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Presentazione sul tema: "INTERLABORATORY STUDIES General aspects TYPES OF STUDIES Method performance study Proficiency testing (several methods) Certification of reference materials."— Transcript della presentazione:

1 INTERLABORATORY STUDIES General aspects TYPES OF STUDIES Method performance study Proficiency testing (several methods) Certification of reference materials (attribution of values to materials) CONDITIONS Co-ordination Motivation (and competence) of participating laboratories Availability of test materials Statistical evaluation Technical evaluation of results

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3 INTERLABORATORY STUDIES Improvement schemes (method performance studies) The principle followed is similar to a method validation, i.e.analyses of increasingly complex matrices to detect possible errors at the different analytical steps. These schemes have a pedagogic goal and involve technical meetings in the frame of which participants may exchange their experience and discuss weak points of their method(s) as well as source(s) of error(s). S1 S2 M1 M2 Simple solutions (pure substances or mixtures of substances) Solutions simulating the matrix or extracts (spiked or not) « Matrix » reference material similar to the sample, spiked with a known amount of the analyte « Matrix » reference material with a composition close to the sample composition DETECTION DERIVATISATION CLEAN-UP SEPARATION EXTRACTION MINERALISATION OVERALL METHOD

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14 EUROPEAN PROJECTS FOR SPECIATION ANALYSIS ORGANOTIN COMPOUNDS IN THE ENVIRONMENT ( ) JUSTIFICATION Toxicity of tributyltin and triphenyltin to marine biota (fish larvae, molluscs) EVALUATION OF THE STATE-OF-THE-ART DEVELOPMENT OF NEW METHODS PRODUCTION OF CRMS PARTICIPANTS Co-ordinations by the University of Pau, ENEA (Rome) and the Free University of Amsterdam Collaborations with the University of Plymouth, the Joint Research Centre (Ispra) and the CID-CSIC(Barcelona) 23 laboratories from 9 EU countries Two bursaries

15 Test material – TBT spiked sediment Coordination BCR Preparation JRC of Ispra (IT) Collection Lake Maggiore (IT) Drying Air drying then oven drying (120 °C) Sieving 90  m mesh size Sterilization Not performed Homogeneization mixer Storage Brown glass bottles +4 °C Humidity < 4% Certified species None Certification 19 laboratories from 7 Countries

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17 RM 424 Coordination University of Plymouth (UK) Preparation University of Pau (F) and IRMM (B) Collection Sado estuary (PT) Drying Air drying then oven drying (80 °C) Sieving 75  m mesh size Sterilization 120 °C for 1h Homogeneization mixer Storage Brown glass bottles +4 °C Humidity < 3% Certified species None Certification 18 laboratories from 8 Countries

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19 BCR 462 Coordination University of Plymouth (UK) Preparation University of Pau (F) and IRMM (B) Collection Arcachon Bay (France) Drying Air drying then oven drying (120 °C) Sieving 75  m mesh size Sterilization 120 °C for 2h Homogeneization mixer Storage Brown glass bottles +4 °C Humidity < 4% Certified species TBT, DBT Certification 21 laboratories from 9 Countries

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22 BCR TBT AND DBT IN COASTAL SEDIMENT

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25 CompoundCertified value UncertainityUnitSet of accepted results TBT5415  g/kg 5 DBT6812  g/kg 7

26 BCR 477 Coordination ENEA (IT) Preparation ENEA (IT) and JRC of Ispra (IT) Collection La Spezia harbour (Italy) Drying Freeze drying Sieving 125  m mesh size Sterilization Not performed Homogeneization Mixer (15 days) Storage Brown glass bottles –20 °C Humidity < 5% Certified species TBT, DBT, MBT Certification 16 laboratories from 7 Countries

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30 BCR TBT, DBT AND MBT IN MUSSEL TISSUE

31 BCR 646 Coordination IVM (NL) Preparation IVM (NL) and IRMM (B) Collection North Sea Canal at Nauerna (NL) Drying Oven drying (60 °C) Sieving 90  m mesh size Sterilization Pasteurization Homogeneization Mixer Storage Brown glass bottles –20 °C Humidity < 1% Certified species Butyltins, Phenyltins Certification 18 laboratories from 9 Countries

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38 BCR 646 – BUTYL- AND PHENYL-TIN IN FRESHWATER SEDIMENT CompoundCertified value UncertainityUnitSet of accepted results TBT48080  g/kg 14 DBT77090  g/kg 13 MBT  g/kg 10 TPhT2911  g/kg 7 DPhT368  g/kg 8 MPhT6918  g/kg 6

39 BCR 710 Coordination ENEA (IT) Preparation JRC of Ispra (IT) and CNRS (FR) Collection Arcachon Bay (France) Drying Freeze drying Sieving 125  m mesh size Sterilization Not performed Homogeneization Mixer (15 days) Storage Brown glass bottles –20 °C Humidity < 5% Certified species TBT, DBT, CH 3 Hg, AsBet Certification 23 laboratories from 11 Countries

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43 BCR 710 – As, Hg and Sn species in oyster tissue CompoundCertified value Standard deviation UnitSet of accepted results TBT13325  g/kg 10 DBT8217  g/kg 9 AsBet335mg/kg8 CH 3 Hg1158  g/kg 12

44 MethodsNumber of set of results CV Means ± SD Cvmin - CVmax GC-FPD109.0± – 19.6 GC-MS710.8± – 24.3 GC-QFAAS610.3± – 20.0 GC-MIP35.0± – 5.2 HPLC-ICP-MS2-5.1 – 23.9 HPLC-ICP-AES HPLC-Fluorimetry1-6.0 Means and standard deviations of the coefficients of variation as function of the techniques applied during the certification campaigns of TBT in BCR 462 and BCR 646 (sediment materials). R. Morabito and Ph. Quevauviller, Spectroscopy Europe 14, (2002)

45 MethodsNumber of set of results CV Means ± SD Cvmin - CVmax GC-FPD119.1± – 14.3 GC-MS68.1± – 15.9 GC-QFAAS – 20.0 GC-MIP36.5± – 7.8 HPLC-ICP-MS – 25.9 HPLC-ICP-AES HPLC-ID-ICP-MS2-1.5 – 7.7 HPLC/Fluorimetry1-6.6 Means and standard deviations of the coefficients of variation as function of the techniques applied during the certification campaigns of TBT in BCR 477 and candidate BCR 710 (biota materials). R. Morabito and Ph. Quevauviller, Spectroscopy Europe 14, (2002)

46 EUROPEAN PROJECTS FOR SPECIATION ANALYSIS ORGANOTIN COMPOUNDS IN THE ENVIRONMENT ( ) WORK PROGRAMME Two trials (solutions, spiked sediment): Two coastal sediment certifications: Certification of a mussel CRM: Certification of a freshwater CRM: Certification of an oyster CRM: RESULTS Detailed studies of derivatisation methods Systematic studies of extraction recoveries Development of methods (SFE, HPLC-ID-ICPMS) One non-certified (harbour) sediment (RM 424) Two sediment CRMs (CRM CRM 646) One mussel CRM (CRM 477) One oyster CRM (BCR 710) M TBT (sediment) in µg/kg GC-FPD GC-MS GC-MIP-AES HPLC-ICPMS

47 EUROPEAN PROJECTS FOR SPECIATION ANALYSIS ORGANOTIN COMPOUNDS IN THE ENVIRONNEMENT ( ) CONCLUSIONS Establishment of expert laboratory network Improved knowledge of methods Tools for method validation Development of new methods PERSPECTIVES - Development of “rapid” techniques and field methods - - New CRMs - - Laboratory Reference Materials Month Concentration TBT       DBT   MBT     Butyltins at +40 °C in the mussel CRM 477

48 MIGLIORAMENTO DELLE PRESTAZIONI COMPLESSIVE DEI LABORATORI MEDIANTE PARTECIPAZIONE AD ESERCIZI INTERLABORATORIALI ESEMPIO: “MERCURIO IN PESCE” MIGLIORAMENTO DELLE PRESTAZIONI COMPLESSIVE DEI LABORATORI MEDIANTE PARTECIPAZIONE AD ESERCIZI INTERLABORATORIALI ESEMPIO: “MERCURIO IN PESCE” ANNO n° di LABORATORI C.V. 41%36.50%33.50%29.15%24%

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52 MOLTI LABORATORI NON PARTECIPANO A STUDI INTERLABORATORIO IN QUANTO LI RITENGONO UTILI SOLO PER: ANALISI PARTICOLARMENTE COMPLICATE

53 AQUACON - MEDBAS ANALYTICAL QUALITY CONTROL AND ASSESSMENT PROJECT IN MEDITERRANEAN BASIN

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56 MOLTI LABORATORI NON PARTECIPANO A STUDI INTERLABORATORIO IN QUANTO LI RITENGONO UTILI SOLO PER: ANALISTI NON ESPERTI ANALISI PARTICOLARMENTE COMPLICATE

57 IMEP INTERNATIONAL MEASUREMENT EVALUATION PROGRAMME

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59 MOLTI LABORATORI NON PARTECIPANO A STUDI INTERLABORATORIO IN QUANTO LI RITENGONO UTILI SOLO PER: LABORATORI CON STRUMENTAZIONE DI BASSO COSTO ANALISTI NON ESPERTI ANALISI PARTICOLARMENTE COMPLICATE

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61 I benefici derivanti dall'adozione di sistemi di QA sono molteplici: capacità degli analisti di "tracciare" un problema fino alla sua fonte; capacità del laboratorio di fornire dati affidabili; la considerazione degli analisti in loro stessi crescerà dopo aver partecipato con successo ad esercizi interlaboratori; la reputazione del laboratorio risulterà accresciuta; il laboratorio non sprecherà le sue risorse producendo dati senza valore.

62 CONCLUSIONI IL CONTROLLO DI QUALITA’ DEI DATI ANALITICI NON PUO’ ESSERE PIU’ CONSIDERATO COME OPZIONALE ED “ UNA TANTUM” IL CONTROLLO DI QUALITA’ DEI DATI ANALITICI E’ E DEVE ESSERE CONSIDERATO UN PROCESSO CONTINUO

63 CONCLUSIONI LE MISURE CORRETTE COSTANO MOLTO LE MISURE SBAGLIATE COSTANO MOLTO DI PIU’ HARRIS, Quantitative Chemical Analysis (Box 9.1)


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