Report to SIM-QSTF Asunción, April 2013

1. QMS supporting CMCs in Chemistry Report to SIM-QSTF Asunción, April 2013

2. Scope of this presentation • QMS supporting CMCs in Inorganic Chemistry (Traces, Metals in Soil, Water) Laboratories in INTI-Quimica • QMS supporting CMCs in Organic Contaminants Laboratories in INTI-Ambiente • Both systems were approved in Santiago, Chile, in March 2008. • So, a 5-years reapproval is needed.

3. Ministery of Industry INTI Board of Directors Advisor Council Presidency General Manager Managers level Regional Assistance Commercial Human Resources International Cooperation Legal Metrology, Quality And Environment Administration & Finances Assistance to social industry Special projects Development Deputy managers level Metrology Environment Quality Dep. Legal Metrology Dep. Scientific & Industrial Metrology 42 R&D centers ……. ……. Química Ambiente INTI Organizational Structure

4. Ministery of Industry INTI Board of Directors Advisor Council Presidency General Manager Metrology, Quality And Environment Managers level Regional Assistance Commercial Human Resources International Cooperation Legal Metrology, Quality And Environment Administration & Finances Assistance to social industry Special projects Development Metrology Quality Deputy managers level Metrology Environment Quality Dep. Scientific & Industrial Metrology Dep. Legal Metrology Dep. Scientific & Industrial Metrology centers …. Química Ambiente 42 R&D centers ……. ……. Química Ambiente Strategic planning and projects Management reviews Maintenance of the Integrated Management System Auditors training Harmonization of procedures, equivalence of results Crossed audits planning Inter-comparisons Technical training planning Maintenance of independent QMSs in each center

5. I. QMS supporting CMCs in Inorganic Chemistry

6. INTI-QUIMICA ORGANIZATIONAL CHART

7. QMS documentation The file INTI-Quimica QMS documentation.pdf contains objectives, scope, responsibilities, organizational charts, contents of the respective Quality Manuals as well as the lists of administrative and technical procedures The Quality Manual is available in INTI-Quimica QM.pdf

8. CMCs Published: Ap A - INTI Quimica CMCs (approved).pdf Metal traces in sediments, soils, ores, and particulates New (under technical review) Ap A - INTI Quimica CMCs (new).xls Metals in different matrices Agreed with the peer reviewer

9. INTI-Química customerfeedback 2012 (surveyto 52 users)

10. Complaints and non conformities 2012 • No complaints were received in 2012 in INTI Quimica. 32 NCs were detected in 2012 in INTI Quimica. All them were managed and closed

11. INTI-Química internal and crossedaudits Management Audit Auditor: Gladys Mastromónaco (INTI-SAI) Date: Sep 28-2012 This audit revealed 5 non-conformities, all resolved to date. Internal Technical audits (2011-2012) The following procedures were audited (September 2011) Determination of Cr in acid solutions (PAAMet-02).Auditor: Pablo Álvarez Non-conformities: 1 – solved Determination de nitrites in calibration solutions. Auditor: Mabel Puelles Non-conformities: 3 – solved Reports and corrective actions in: INTI Quimica internal and crossed audits.pdf Note: Considering that, during 2012, a peer review was held to all the methods related to CMCs, no internal audits were performed then.

12. INTI-Química Management review • Date: October 2012 • Details in: INTI-Quimica MR.pdf • Summary of topics treated: • Summary of preliminary reports • Evaluation of the Period: Policy and Procedure Revision . Audit Results . Independent Entity Evaluations - Interlaboratory Comparison Results Change in Volume and/or Type of Work Customer Feedback - Claims Staff Training • Evaluation of Objectives from the previous review • Improvement objectives for the new period: • expanding the scope of methods • acquire the necessary equipment to expand the range of internal calibrations • optimize maintenance, verification and equipment calibration management. • activities towards tuning up viscosity measurements

13. INTI-Química Peer Review Date:June25‐27 2012, Reviewer:. Heidi Goenaga‐Infante, LGC (UK). Scope: stated CMCs in Ap A Report: INTI Quimica PR report.pdf Results: The reviewer has mentioned 19 recommendations. All of them were considered and actions were defined and were or are being executed. Actions taken in: INTI-QuimicaAction Plan.pdf

14. INTI-Química Peer Review Attestation (extracted from the report) “The INTI has the capabilities and competences to carry out the services it is claiming to deliver to its customers in the scope of the CIPM MRA. The quality system, as far as it could be reviewed, is in compliance with ISO/IEC 17025 and covers the near future claimed CMCs. No Non-Compliances have been found, however a few minor non-compliances have been observed. Those are detailed in further sections of this report. A number of recommendations for further improvements are, therefore, added in the peer review report.”

15. INTI-Química CMCsvitality Evidences included in file: INTI-Quimica vitality evidences.pdf • Summary: • Participation in working groups at CCQM, SIM • Stays at other NMIS • Participation in international technical seminars or congresses • Organizattion of 2 Training courses at INTI-Chemistry during 2010 (by NMI experts) • Organization of 3 proficiency tests in the country (traceability dossemination) • Harmonization of Measurements at different INTI Centres

16. II. QMS supporting CMCs in Organic Contaminants

17. INTI- Ambiente structure Technical Director Secretary Technical Unit Coordination Office Head of Quality Laboratory Management Analysts Test Operators Support Staff

18. QMS documentation The file INTI-Ambiente QMS documentation.pdf contains objectives, scope, responsibilities, organizational charts, contents of the respective Quality Manuals as well as the lists of administrative and technical procedures The Quality Manual is available in INTI-Ambiente QM.pdf

19. INTI-Ambiente customerfeedback 2012 A random sample of 15 users was extracted. The survey results were presented and discussed in the management review

20. INTI-Ambiente NC 2012 3 customer complaints were received in INTI Ambiente in the last period. All of them are related to mistakes in the report of results. Corrective actions were implemented and verified 22 NC were received. All of them were managed according the procedures and closed. In the following tabke, a classification by matters can be shown

21. INTI-Ambiente crossed audits 2012 Management Audit Audit Criteria: QMS requirements in ISO/IEC 17025: 2005 Leader Auditor: Bioq Gladys Mastromónaco Date: Sep 30/31 - 2012 Auditor: Gladys Mastromónaco (INTI-SAI) Date: Sep 28-2012 This audit revealed 1 non-conformity, resolved to date. Technical audit Scope: Aromatic hydrocarbons in metanol (PE 10.39 V2.) Leader Auditor: Bioq Gladys Mastromónaco Auditor Team: Lic. M. Alejandra Rodríguez (technical expert) - Lic. Pablo Sánchez (Observer) Date: Dec 11 2012 This audit revealed 4 non-conformities, all resolved to date. Reports and corrective actions in: INTI Ambiente crossed audits.pdf

22. INTI-Ambiente Management Review • Date: September 2012 • Summary in: INTI-Ambiente MR.pdf • Improvements proposed for 2013: • Improve the supplier evaluation procedure • Improve or implement an effective procedure for the treatment of queries directed to the Centre so that they can become a source of information and feedback to Laboratories. • Train all the employees in complaint reception and management. • Establish procedures to make reagent and equipment purchases for Analytical Service Coordination Laboratories easier and faster. • General Objectives 2013 • Strengthen and expand current metrology capacities based on the start up of the National Metrology Plan. • Reinforce Quality Management notions in the Centre's Technical Assistance areas. • Produce at least two new Standard Materials. • Expand the scope of the QMS with, at least, 5 new tests.

23. Peer review in Ambiente Date: July 2012 Reviewer: Mariana Arce Osuna, CENAM Report in: INTI Ambiente PR report.pdf Scope: stated CMCs in Ap A Results: The reviewer has mentioned 2 non conformities and 21 recommendations. Actions taken in: INTI-Ambiente Action Plan.pdf

24. Extracted form the Executive summary of the peer review report): The results generated by INTI in key comparisons and pilot studies are in general satisfactory, although there are examples in which it became clear that more experience is still needed. However, since the activities in chemistry in INTI still in development and moreover the metrology concepts in measurements in chemistry are not well understood for all staffs, still necessary to include within INTI training program all base chemical metrology concepts. It is observed that Research and Development of Special Organic Contaminants of INTI is making very good progress in the right direction. The Research and Development of Special Organic Contaminants have a large amount of chemical analysis equipment available. The facilities are similar to those in other national metrology institutes. They are suitable for the current activities. In general, the measurement methods applied are adequate. Measurement uncertainty evaluation is based on the GUM and related EURACHEM documents.

25. Extracted form the Executive summary of the peer review report (II) In some cases the claimed uncertainty seems to be on the optimistic side and should be reconsidered, of course taking into account the results of pilot studies and other bilateral comparisons and in particular of key comparisons. Thorough method validation is still necessary addressing all potential uncertainty components. Taking into account some reconsideration as mentioned above, the claimed calibration and measurement capabilities as proposed to become published in the Appendix C of the CIPM MRA are acceptable and seem to be reliable.

26. CMCs vitality Evidences included in file: INTI-Ambiente vitality evidences.pdf Summary: • Participation in working groups at CCQM, SIM • Participations in CCQMK79, CCQM P129, CCQMK55, CCQMK95, AFRIMET QM-K27 • Stays at other NMIS • Participation in international technical seminars or congresses • Organization of national proficiency tests

27. Up to now, the metrological traceability in services related to INTI CMCs is mainly disseminated by means of analytical services to samples supplied by customers, or assignation of reference values in proficiency tests Additionally, INTI is beginning to produce, certify and offer reference materials. Up to know, they are mainly related to measurements in which no CMCs can be stated (for instance, quality of milk parameters) The reviewers have strongly encouraged us to increase this option for CMCs services In that way, ISO Guide 34 is being implemented. Our intention is to have a peer review in the following months and to present the results in the next QSTF meeting Note on the dissemination of traceability in Chemical Metrology:

28. Thank you!