1 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 Wolfgang Garche Saxony-Anhalt Environmental Protection Agency Department Air Quality Monitoring, Information, Assessment Demonstration of Equivalence for Particle Measurement Methods

2 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 European standards: Reference methods for PM10 and PM2,5 EN12341Air Quality – Determination of the PM10 fraction of suspended particulate matter – Reference method and field test procedure to demonstrate reference equivalence of measurements EN14907 Standard gravimetric measurement method for the determination of the PM2,5 mass fraction of suspended particulate matter A Member State may use an other method for which it can demonstrate gives results equivalent to reference method or displays a consistent relationship to the reference method. In that event the results achieved by that method must be corrected to produce results equivalent to those that would have been achieved by using the reference method.

3 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 Conditioning of the unloaded filters and weighing M 1 Temperature: 20 ± 1 °C Humidity: 50 ± 5 % Air conditioned balance cabinet Sample inlet for PM10 or PM2,5 Conditioning of the loaded filters and weighing M 2 Temperature: 20 ± 1 °C Humidity: 50 ± 5 % P Measurement of volume flow V Filter Reference methods for PM10 and PM2,5 Air conditioned balance cabinet

4 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 Candidate Method: A measurement method proposed as an alternative to the relevant Reference Method for which equivalence has to be demonstrated Reference Method: The principle of a method established by EC legislation for the measurement of a specified ambient air pollutant DEFINITION OF EQUIVALENCE 1.A measurement method that meets the requirements set from the viewpoint of fitness-for purpose for the intended use of the reference method. 2.A measurement method giving results that do not differ from those of the Reference Method within a specified statistical uncertainty. ‘An Equivalent Method to the Standard Method for the measurement of a specified air pollutant, is a method meeting the Data Quality Objectives for continuous or fixed measurements specified in the relevant air quality directive’

5 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 CompoundLimit value (μg/m³) Reference period Expanded Uncertainty (%) Data Capture (%) PM h 1 year PM2, ? 1 year (2015) 1 year (2020) 2590

6 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 Testing of equivalence Tests in laboratory Assessment of the influence of different uncertainty sources Relevant for: -automatically filter changers -different weighing conditions Field test Side-by-side test with the Reference Method (RM) Not relevant if the CM is only a modification of the RM

7 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 Test procedure for the application of automatic filter changes: Check under worst case conditions  storage temperatures  significant fractions of semi volatile materials minimum of 40 samples with significant fractions of semi-volatile materials weighing according to the procedure of the standard exposed the worst conditions of temperature and time reweighing according to the procedure of the standard Largest mass lost shall be used for uncertainty calculation:

8 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 Test procedure for different weighing conditions:  Assessed for blank Filters and samples  Worst case conditions considering hygroscopic and semi volatile materials Minimum 5 blank filters from two batches for each used type Mass changes under the extremes of allowed conditions Largest mass change shall be used for uncertainty calculation:

9 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN samples shall be collected in conditions known to produce significant effects on filter mass First weighing under conditions according to the EN standard second weighing under the new conditions Largest mass difference shall be used for uncertainty calculation:

10 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 Field Test procedure Reference and candidate method side-by-side It shall be determined  between-sampler/instrument uncertainty of the Candidate Method through the use of two samplers or instruments  comparability of the Candidate and Standard Methods

11 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 Experimental conditions: Test sites representative for typical conditions (including possible episodes of high concentrations Minimum 4 comparisons which includes (if appropriate) -high and low fractions of semi-volatile particles, -air humidity and temperature (high and low) -wind speed (high and low) minimum of 40 measurement results for each comparison installation so, that spatial inhomogeneities of the compound concentration can be neglected Both methods shall be operated under normal practical conditions

12 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 Calculation of performance characteristics Between-sampler/instrument uncertainty: Where: yi,1 and yi,2 are the results of parallel measurements for a single 24-hour period i n = number of 24-hour measurement results. The between-sampler/instrument uncertainty shall be determined: - for each of the comparisons separately - for all results together - for two datasets obtained by splitting the full dataset according to PM concentrations: greater than or equal to, or below 50% of the upper assessment threshold Between-sampler/instrument uncertainty have to be ≤ 3µg/m³ !!

13 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 Comparison with the Standard Method Calculation of the between-sampler uncertainty for the standard method  shall be ≤ 2µg/m³ results of parallel measurements the for candidate sampler/instrument are averaged  one result y i for each 24 hours measurement period a linear relation between candidate and reference method is assumed y i = a + bx i Orthogonal regressions (symmetrical treatment of both variables): each of the comparisons separately for all results together for a dataset representing PM concentrations greater than or equal to 50% of the upper assessment threshold

14 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 Uncertainty in the results of the Candidate Method from comparison with the Standard Method: where RSS = the sum of (relative) residuals resulting from the orthogonal regression u(x i ) = random uncertainty of the Standard Method( u bs calculated for the Standard Method may be used) The uncertainty u C_S is calculated for: - each of the comparisons separately - for all results together - for a dataset extracted from all results greater than or equal to 50% of the upper assessment threshold

15 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 For all datasets the combined relative uncertainty of the Candidate Method is calculated : For y i the limit value is used. For all datasets the expanded relative uncertainty of the Candidate Method is calculated : with k = 2 Result: CM is accepted as equivalent CM is not accepted as equivalent

16 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 apply a correction factor or term resulting from the regression equation obtained for the full dataset Case 1:slope b is not significantly different from 1 intercept a is significantly different from 0

17 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 Case 2:slope b is significantly different from 1 intercept a is not significantly different from 0 Case 3:slope b is significantly different from 1 and Intercept a is significantly different from 0

18 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 Excel-Program „test_equivalencev31004.xls“ Link: EQUIVALENCE FIELD TEST INPUT SHEET Insert input into the yellow cells concentration units limit value35,00ug/m3 MethodPM2.5 Expanded Uncertainty Criteria, %25 RM between-sampler uncertainty1,5ug/m3 Reference MethodCandidate Method RM IRM IICM ICM II

19 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09

20 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 PM10 comparison measurements 2003 in Wiesbaden

21 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 Expanded relative uncertainties of gravimetrical methods (Source: U.Pfeffer und R. Beier 40. Messtechnisches Kolloquium Aachen 2005)

22 Saxony-Anhalt State Environmental Protection Agency Wolfgang Garche Bukarest EU-Twinning Project RO 2006 IB EN 09 Many Thanks for your Attention!