Test procedures and minimum performance requirements to demonstrate equivalency of sulphur dioxide measurement methods for EC compliance monitoring

European Commission Directorate-General For The Environment Directorate-General For The Information Society And Media

Description

Environment policy and protection of the environment
Environmental research

Sujets

• Oxyde
• Sulfur
• Environmental monitoring

Informations

• Publié par: EUROPEAN-COMMISSION-DIRECTORATE-GENERAL-FOR-THE-ENVIRONMENT-DIRECTORATE-GENERAL
• Nombre de lectures: 20
• Langue: English
• Poids de l'ouvrage: 1 Mo

Extrait

EUR. 11143
* *
Commission of the European Communities
environment and
quality of life
Test procedures and minimum
performance requirements to
demonstrate equivalency of sulphur
dioxide measurement methods
for EC compliance monitoring Commission of the European Communities
environment and
quality of life
Test procedures and minimum
performance requirements to
demonstrate equivalency of sulphur
dioxide measurement methods
for EC compliance monitoring
H.J. van de Wiel, H.J. Th. Bloemen
National Institute of Public Health
and Environmental Hygiene
Bilthoven
The Netherlands
Contract No XI-85-B6600-11 -044-11 -N
Directorate-General
Environment, Consumer Protection and Nucle JMfaÉPP- Bib!ioih j
N.C./EUR 11143 EN 1987
CL Published by the
COMMISSION OF THE EUROPEAN COMMUNITIES
Directorate-General
Telecommunications, Information Industries and Innovation
Bâtiment Jean Monnet
LUXEMBOURG
LEGAL NOTICE
Neither the Commission of the European Communities nor any person acting on
behalf of then is responsible for the use which might be made of the
following information
Cataloguing data can be found at the end of this publication
Luxembourg: Office for Official Publications of the European Communities, 1987
ISBN 92-825-7471-7 Catalogue number: CD-NA-11143-EN-C
© ECSC-EEC-EAEC, Brussels • Luxembourg, 1987
Printed in Belgium CONTENTS
Pg.
1. FIELD OF APPLICATION 1
2. DEFINITIONS 2
3. OUTLINE OF THE LABORATORY EVALUATION PROCEDURE 6
GENERAL LABORATORY TEST REQUIREMENTS AND PROVISIONS 7
4.1 Description of the method under test
4-2 Test atmospheres and test solutions
4«3 Data acquisition 8
4.4 Reference conditions
4.5 Preliminary investigation 9
4*6 Miscellaneous
5. LABORATORY TEST PROCEDURES 11
5*1 Classification of the measurement method 1
5.2 Dynamic response characteristics (lag time, rise time,
fall time, response time)
5.3 Calibration experiment5
5.3.1 Detection of outliers7
5«3*2 Variance function
5.3.3 Calibration function , 18
5.3.4 Test on linearity of regression [10,19,20,21]9
5.3.5 Non-linearity 21
5.3.6 Repeatability2
5.3.7 Lower detection limit [25,27]
5.3.8 Measurement threshold (lower limit of determination) 23
5.4 Instability, Drift
5«5 Dependence of influence variables5
5.5.1 Line voltage dependence6
— II — 5.5.2 Temperature dependence 26
5.5.3 Selectivity8
5.6 Miscellaneous characteristics9
5.6.1 Collection efficiency
5.6.2 Effect of storage time 30
6. OUTLINE OP THE FIELD EVALUATION PROCEDURE1
7. GENERAL FIELD TEST REQUIREMENTS AND PROVISIONS 32
7.1 Selection of the test site 3
7.2 Test atmosphere and sample distribution
7.3 Calibration device (automated analysers)
7.4 Environmental test conditions3
7*5 Set-up and start-up
7.6 Data Acquisition (automated analysers)
8. FIELD TEST PROCEDURE 34
9- EVALUATION5
10. DEVELOPMENT OF MINIMUM PERFORMANCE REQUIREMENTS 36
10.1 Objectives
10.2 The TOTAL DEVIATION approach 37
11. REQUIREMENTS ON BIAS AND TOTAL DEVIATION UNDER FIELD CONDITIONS 43
12. REQUIREMENTS ON THE MEASUREMENT RANGE 44
12.1 Upper limit of measurement
12.2 Lower detection limit and measurement threshold5
13. REQUIREMENTS ON THE DYNAMIC PROPERTIES7
14.S ON AVAILABILITY 48
15- SPECIFIED PERFORMANCE REQUIREMENTS FOR AUTOMATED METHODS 49
15-1 Performance limits
— IV — 15.2 Standard field conditions for estimating BIAS and TOTAL
DEVIATION 50
16. SPECIFIED PERFORMANCE REQUIREMENTS FOR MANUAL METHODS (30 MIN AVER.) 52
16.1 Performance limits2
16.2 Standard field conditions for estimating BIAS and TOTAL
DEVIATION4
17. SPECIFIED PERFORMANCE REQUIREMENTS FOR MANUAL METHODS (24 H. AVER.) 55
17-1 Performance limits 55
17.2 Standard field conditions for estimating BIAS and TOTAL
DEVIATION7
18. COMPUTER PROGRAM9
19. REFERENCES 60
APPENDICES3
APPENDIX 1. STEPWISE OUTLINE OF THE LABORATORY EVALUATION 65
APPENDIX 2. PERCENTILES OF THE T- AND F-DISTRIBUTION 7
APPENDIX 3- STEPWISE OUTLINE OF THE ESTIMATION OF BIAS AND TOTAL
DEVIATION UNDER STATIONARY CONDITIONS5
— V — 1. FIELD OF APPLICATION
The test procedures developed are based on:
- (draft) test procedures of the member countries [1-3]
-) tests of foreign countries, ISO and IEC [4-10]
- (common) scientific procedures.
They are applicable to measuring methods:
- with a linear calibration function (linearity may be enforced by
postprocessing of the primary output),
- the instrument reading of which is an average representative of a defined
time Interval,
- the instrument readings of replicated measurements of which constitute a
normal distribution.
The test procedures reflect primarily instrumental methods of measurement.
However, instructions are given to use these procedures also for manual
methods. There is no fundamental distinction between an instrumental
(automated) method and a manual (wet-chemical) method, as long as the
measured value obtained is an average representative of a predefined time
interval.
Minimum performance requirements based on the test procedures are given for
instrumental and manual methods. Compliance with these requirements makes a
candidate method equivalent to the sulfur dioxide reference method for
sampling and analysis in the framework of the EC-directive 80/779/EEC. The
calibration of an equivalent method must be traceable to a primary
standard.
1 -2. DEFINITIONS
performance characteristics
Availability: Ratio of the number of measurements accepted to the total
possible number of measurements of the analyser. It may be expressed in
percent.
Calibration function: Instrument reading as a function of concentration, at
reference conditions [6].
Collection efficiency: Part of the supplied analyte retained in the sample.
Drift: Systematic change in instrument reading over a given period of
unattended operation under reference conditions for a constant pollutant
concentration [6].
Fall time: Difference between response time and lag time in the falling
mode [1,2,3,4,6,8,9].
Instability: Change which takes place in instrument reading over a stated
period of unattended operation for a given pollutant concentration [6].
It is characterized by the variation with time of its mean, specifying
drift, and by its dispersion.
Interference: See Selectivity.
Lag time: Time interval from an instantaneous step change of pollutant
concentration at the input of the analyser to the instant at which the
instrument reading reaches 10% of the final change in instrument output
[1,2,3,4,6,7,8].