QUALITY OF AIR PROTECTION 2008Workshop –for West Balkan contries

Importance of National References Laboratories for Air Quality role on the

AQ/AC chain

Jiri NovakHead of Central Laboratories for Ambient Air, Czech Republic

Contents

• Introduction - Legislation• QA - Quality Assurance• QC - Quality Control• ISO IEC 17025:2005• Traceabilty chain• National Reference Laboratory/Competent Authority/

associated laboratory of National Metrology Institute• AQUILA• Recomendations to NRL´s

Introduction

• On the tasks specified for the Competent Authority(CA)/National Reference Laboratory in the proposed Directive on the AAQ and CA for Europe:

• Article 3 point(c.): MS shall designate at the appropriate levels the CA and bodies(NRL) for the following:

Ensuring the accuracy of measurements-in the context of DQO

where relevant,the CA/NRL and bodies shall comply

with Section C of Annex I.• Annex 1 Section C.

- CA/NRL shall ensure following:

• all measurement undertaken in relation to the assesment of

AAQ pursuant to Art. 6 and 9 are traceable in accordance with

Introduction – cont.

with the requirements set out in section 5.6.2.2 of the ISO/IEC 17025:2005

• Institutions operating networks and individual stations have an

established QA/QC system

• CA/NRL – taking part in Community-wide intrecomparisions covering

pollutants regulated in this Directive, are accredited according to

EN/ISO 17025 by 2010 for the reference methods referred in

AnnexVI.

• CA can be designated at the political level, but national laboratories

or NRL are designated at the technical level (this distinction is not

clear in the proposed Directive)

Quality Assurance(QA)

• General Principle of QA ISO defines QA as follows Quality Assurance – all planned and systematic actions necessary

to provide confidence that a product, process or service will satisfy given requirements for quality - QA refers to the overall managment of the process involved in obtaining the data–i.e QA relates to measuring process, therefore • QA activities for AQ monitoring networks might include: - Network design - Station siting - Instrument selection - Instrument service and repair

QA – cont.

- Operationl manual

- Instrument calibration (Calibration Laboratory/NRL)

- Site, analyser and calibration audit (CA/NRL)

• In theory, if all of the QA activities are undertaken correctly and

in compliance with relevant CEN standard and detailed local

operating procedures at all times, then there is an expection

that the measurements will fulfil the requirements of the EU

Directives without other checking.

Ongoing QA:

- Calibration of analyser (at least every 6 months)

- Certification of test gases ( at least every 6 months)

QA – cont.

- Zero/Span check (at least every two weeks – better 23 hours)

- Lack of fit (linearity) check (every year + after repair)

- Convertor efficiency for NOx analysers (at least every year)

- Test sample manifold (at least every 3-years)

- Change particulate filter (at least every 3-months – maybe 2 weeks

for very polluted stations!!)

- Test sample lines (at least every 6-months)

- Regular analyser maintenance (as required)

The CA/NRL needs to ensure that procedures are in place for the these

on-going QA check and that results are documented and any

necessary remedial action taken.

Quality Control(QC)

• General Principle of QC

ISO defines QC as follow

Quality Control – operational techniques and activities that are used to fulfil given requirements for quality

QC activities could include:

- Data checking (Data ratification – Plausibility check)

- Quality review and feedback

- Uncertainty requirements

( QC refers to the activities undertaken to check and optimise data

accuracy and precision after collectioon – is concerned primarily

with outputs)

Appendix – CEN Standard Method

• SO2 EN 14212:2005• NOx,NO EN 14211:2005• PM10 EN 12341:1999• PM2.5 EN 14907:2005• Benzene EN 12622:2005• CO EN 14626:2005 , Ozone EN 14625:2005

The CEN standard methods for gaseous pollutants provide details of

the reference method of measurement for each pollutant, specific

analyser tests to be performed and requirements for on-going QA/QC

of analyser. These standards provide a methodology for uncertainty

evalution to enable measurement uncertainty to be directly compared

with specified DQO.

ISO IEC 17025:2005

• Chapter 5.6.2 Specific requirements 5.6.2.1 Calibration• ….that calibrations and measurements made

by • the laboratory are traceable to System of• Units (SI) for gases – mass (mol) AND• A Calibration laboratory established traceability of its own

measurement standards and measuring instruments to the SI by means of an unbroken chain of calibrations or comparisons linking

them to relevant primary standard (for gases Primary Reference Material – PRM) of the SI units of measurement. To link to SI units

may be achieved by reference to national measurements standards. (ozone is exception – reference to Standard Reference Photometer)

Scheme of traceability chain

• Example of traceabilty chain• Calibration Laboratory/National Reference Laboratory/associated laboratory of National Metrology Institute - Czech Republic Primary Reference Material (PRM) – NMi,NPL gases – SO2, NO, CO,BTX - VOC) (Certificated Reference Material – CRM for HM, PAH) Standard Reference Photometer (SRP) for ozone measurement

Scheme of traceability chainPrimární referenční materiál (PRM) KLI Primary Reference Material

Ředění PRM v ředící nádobě referenčním plynem podle stavovérovnice plynů při konst. TeplotěDilution unit

KLI

Pracovní etalon Kalibrátor HoribaPob. lab.

Working etalon Regionallaboratory

Pracovní etalon – analyzátor (PE-A)Working etalon – analyzer KLI

Provozní měřidlo – analyzátor AMSOperational analyzer in AMS

Ředička MCZ + tlaková láhev –směs SO2, NO, CO AMSDilution unit + cylinder (SO2, NO, CO) in AMS

Pracovní etalon -analyzátor (PE-A)Pob.lab.

Working etalon Regional laboratory

Pracovní etalon - tlaková láhev (PE-TL) Pob.lab.Working etalon – cylinder Regional laboratory

Přesný tlakoměr navázanýna národní etalon

KLI

Provozní měřidlo – analyzátorAMS

Operational analyzer in AMS

Pracovní etalon – zdroj kalibra- čního

plynu (PE-TL, PE-Z) (tlaková láhev, kalibrátor) KLIWorking etalon source of calibrationcylinder

Provozní měřidlo – analyzátorAMS

Operational analyzer in AMS

Kalib

račn

í la

bora

toř

imis

í -K

LI

Ca

libra

tionl

ab

ora

tory

AM

S

AMSPobočková laboratoř

Regional laboratory

Calibrationcheck

A),D)

A),D)

A),D) After repair in regional laboratory

A),D) C)

A)

B)

Calibrationone point

A-adjustment zero/spanB-certification ofcalibrations gasesC-zero/span checkD-linearity check

Primární referenční materiál (PRM) KLI Primary Reference Material

Ředění PRM v ředící nádobě referenčním plynem podle stavovérovnice plynů při konst. TeplotěDilution unit

KLI

Pracovní etalon Kalibrátor HoribaPob. lab.

Working etalon Regionallaboratory

Pracovní etalon – analyzátor (PE-A)Working etalon – analyzer KLI

Provozní měřidlo – analyzátor AMSOperational analyzer in AMS

Ředička MCZ + tlaková láhev –směs SO2, NO, CO AMSDilution unit + cylinder (SO2, NO, CO) in AMS

Pracovní etalon -analyzátor (PE-A)Pob.lab.

Working etalon Regional laboratory

Pracovní etalon - tlaková láhev (PE-TL) Pob.lab.Working etalon – cylinder Regional laboratory

Přesný tlakoměr navázanýna národní etalon

KLI

Provozní měřidlo – analyzátorAMS

Operational analyzer in AMS

Pracovní etalon – zdroj kalibra- čního

plynu (PE-TL, PE-Z) (tlaková láhev, kalibrátor) KLIWorking etalon source of calibrationcylinder

Provozní měřidlo – analyzátorAMS

Operational analyzer in AMS

Kalib

račn

í la

bora

toř

imis

í -K

LI

Ca

libra

tionl

ab

ora

tory

AM

S

AMSPobočková laboratoř

Regional laboratory

Calibrationcheck

A),D)

A),D)

A),D) After repair in regional laboratory

A),D) C)

A)

B)

Calibrationone point

A-adjustment zero/spanB-certification ofcalibrations gasesC-zero/span checkD-linearity check

Pracovní etalon – analyzátor (PE-A) KLIWorking etalon - analyzer

Provozní měřidlo – analyzátorAMS

Operational analyzer

Pracovní etalon - analyzátor (PE-A)Pob lab.

Working etalon – analyzer Regional laboratory

Pob

očko

vá la

bora

toř,

AM

S

Re

gio

na

l la

bo

rato

ry

Kal

ibra

ční

labo

rato

ř im

isí

- K

LI

C

alib

ratio

n la

bo

rato

ry

Pracovní etalon – analyzátor (PE-A) KLIWorking etalon - analyzer

Standardní referenční fotometr ozónu (SRP) KLI

Standard Reference Photometer for ozone measurement

kalibrační kontrola

Calibration check

A), B)Multipoint calibration (4-5 point)vícebodová kalibrace (4-5 bodů)

A)-nastavení měřícího rozpětí dle ČSN EN 14625 – 9.5.Zero/span checkB) –ověření linearity dle ČSN EN 14625 – 9.6.3Linearity check

Scheme for Ozone

Calibration Laboratory/National Reference Laboratory - Summary

• Traceability to SI unit• PRM• Dilution units

- Static or Dynamic units

• Working etalon

- analysers

- gas cylinders

• Standard Reference Photometer for ozone measurement

Working etalon + dynamic dilution unit

Working etalon, analysers + gas cylinders

Working etalon, analysers + gas cylinders

Dilution unit – Static manometric injection

Dilution unit – Static manometric injection-PRM

Standard Reference Photometer –SRP No.17, NIST

AQUILA

• There is association of National Reference Laboratories - AQUILA

Air Quality National Reference Laboraqtories

• Meetings cca 2 times per year – JRC Ispra Italy

• min.50% of time – discussion for QA/QC system-program in EU

including Directive, Daugter Directive, tests etc.

Recomendation to NRL´s

1. Ensure that number, distribution and siting of monitoring stations in monitoring network conforms to the Directive requirements

2. Any new analysers purchased to networks used for demonstrating Directive compliance should by type tested to the appropriate CEN procedure – all analysers used in monitoring networks need to be replaced with type tested analysers within 5 years of the implementation of the Directive3. CEN QA/QC procedures need to be introduced into the monitoring networks4. Data uncertainties need to be calculated by the CEN methodology for every analyser, every year5. Obtain the appropriate ISO 17025 accreditation6. Participate in the appropriate EU Commmunity-wide QA programmes7 Examine and review procedures and quality issues on a regular basis to adapt and improve

Recomendations to NRL´s – cont.

8. Ensure that documented QA procedures (SOP) are in place for all

insitutions operating networks and individual stations within the MS

9. Where equivalent analysers are used, ensure that correct

procedures have been followed for the demonstration of

equivalence and that a report has been supplied to the

Commission for approval

10. Ensure that all data reported to the Commission comply with the

Directive requirements and the recomendations of the Data

Exchange Group.