The importance of sampling strategy, sample handling and storage for emission testing
27/06/2012 The importance of sampling strategy, sample handling and storage for emission testing F. Maes 27/06/2012 © 2011, VITO NV 1 Summary » Product emission testing: why – what? » » » » » » Indoor air Construction Products Directive (CPD) Emission test chamber experiments - general Evaluation protocols – product labels Consumer products / electronic devices emission testing SVOC emission testing 27/06/2012 © 2011, VITO NV 2 Indoor air pollution » Indoor air pollution is the presence in buildings of toxic or other substances which may directly or indirectly be a cause of occupant ill health or discomfort. » Sources of pollution: contaminants in the outdoor air and those released from products or by activities of occupants » Formaldehyde and VOCs are key pollutants emitted from construction products D. Crump, European concepts to identify and limit emissions from construction products 27/06/2012 © 2011, VITO NV 3 Construction Products Directive » CPD (European Council Directive 89/106/EEC) » Recently: Regulation (EU) No 305/2011, replaces CPD from July 2013 » Goal: removing trade barriers for construction products in the common market of the European Union and permitting the free movement of goods, if they are “fit for their intended use” » Products have to fulfill essential requirements (Annex I CPD) 1. Mechanical resistance and stability 2. Safety in case of fire 3. Hygiene, health and the environment 4. Safety in use 5. Protection against noise 6. Energy economy and heat retention 27/06/2012 © 2011, VITO NV 4 Construction Products Directive 1. Mechanical resistance and stability 2. Safety in case of fire 3. Hygiene, health and the environment 4. Safety in use 5. Protection against noise 6. Energy economy and heat retention » “The construction work, must be designed and built in such a way that it will not be a threat to the hygiene or health of the occupants or neighbours, in particular as a result of any of the following: » » » » » the giving-off of toxic gas, the presence of dangerous particles or gases in the air, the emission of dangerous radiation pollution or poisoning of the water or soil, faulty elimination of waste water, smoke, solid or liquid wastes, » the presence of damp in parts of the works or on surfaces within the works.” 27/06/2012 © 2011, VITO NV 5 Beginning of emission measurements » To promote development of low emitting building materials » 1990: GuT – association of environmentally friendly carpets, voluntary labelling system with respect to VOC emissions » 1995: DICL (Danish Indoor Climate label), products representing large surface areas in indoor environment » 1995: Finnish emission classification » … » 1997: European collaborative action: IAQ and its impact on man Report No 18: “Evaluation of VOC emissions from building products” =basic testing scheme for flooring materials =basis for German AgBB, French AFSSET,… 27/06/2012 © 2011, VITO NV 6 Standardisation of emission testing » 1999: EN 13419 » -1: test chamber » -2: test cell » -3: sample preparation » Revised and published as EN ISO 16000 Indoor Air standards » » » » ISO 16000-3: Formaldehyde and other carbonyl compounds in air analysis ISO 16000-6: Volatile organic compounds in air analysis (VOC: C6-C16) ISO 16000-9: Operation of emission test chamber ISO 16000-10: Operation of emission test cell - FLEC » ISO 16000-11: Preparation of test specimens » ISO 16000-25: Determination of the emission of semivolatile organic compounds (SVOC: > C16) by building products — Micro-chamber method » WD: ISO 16000-31: Measurement of flame retardants and plasticizers based on organophosphorus compounds -- Phosphoric acid ester 27/06/2012 © 2011, VITO NV 7 Sampling of the material Transport of the sample Storage of the sample before testing ISO 16000-11 Test specimen preparation Testing age and conditioning of the test specimen Measuring technique ISO 16000-3 -6 Analyses Evaluation procedure AgBB, Afsset,… Reporting, labelling Building material emissions to indoor air, Opportunities/consequences for Belgian companies, M. Lor 27/06/2012 © 2011, VITO NV 8 Evaluation Standardisation of emission testing » 1999: EN 13419 » -1: test chamber » -2: test cell » -3: sample preparation » Revised and published as EN ISO 16000 Indoor Air standards » ISO 16000-3: Formaldehyde and other carbonyl compounds in air analysis » ISO 16000-6: Volatile organic compounds in air analysis » ISO 16000-9: Operation of emission test chamber » ISO 16000-10: Operation of emission test cell » ISO 16000-11: Preparation of test specimens » EN 717-1: formaldehyde emission testing for wooden products » US: California section 1350 and ASTM D5116 27/06/2012 © 2011, VITO NV 9 Emission test chamber operation R. Oppl, New draft harmonized CEN standard on emissions from construction products principles common with ISO 16000 and EN 717-1 and differences 27/06/2012 © 2011, VITO NV 10 Emission test chamber operation R. Oppl, New draft harmonized CEN standard on emissions from construction products principles common with ISO 16000 and EN 717-1 and differences » Started from ISO 16000, addition of specifications for improving reliability of testing when more than one lab is involved » Pending validation project » Differences: tried to find compromise » Allows integrating several testing purposes into one test setup 27/06/2012 © 2011, VITO NV 11 Emission test chamber operation » » » » Test chamber simulates reference room conditions ISO 16000-9: 7 m² surface; 2.49 m high New CEN standard: 3 x 4 m surface, 2.5 m high, one door and one window These dimensions determine loading factors » Flooring material: 12 m² / 30 m³ = 0.4 m²/m³ » … 27/06/2012 © 2011, VITO NV 12 Different sizes of test chambers » ISO 16000-9 » ISO 16000-10 ISO 16000-25 Determination of the emission of semi-volatile organic compounds by building products -- Micro-chamber method 27/06/2012 © 2011, VITO NV 13 Emission test results » Result of an emission test: compound in µg/m³ » Different sizes, different loading factors,… » => specific emission rate • AER = 0.5 h-1 ; ASAFR = AER/loading factor [m³/hm²] • SER = concentration [µg/m³] x ASAFR; [µg/hm²] » Comparison of results possible between emission tests in different test chambers 27/06/2012 © 2011, VITO NV 14 Sampling of the material Transport of the sample Storage of the sample before testing ISO 16000-11 Test specimen preparation Testing age and conditioning of the test specimen Measuring technique ISO 16000-3 -6 Analyses Evaluation procedure AgBB, Afsset,… Reporting, labelling Building material emissions to indoor air, Opportunities/consequences for Belgian companies, M. Lor 27/06/2012 © 2011, VITO NV 15 Evaluation ISO 16000-11 » Sampling of test material » Preparation of test material » Building material emissions to indoor air, Opportunities/consequences for Belgian companies, M. Lor International Conference „Construction Products and Indoor Air Quality“, W. Misch 27/06/2012 © 2011, VITO NV 16 Sampling and analysis » Active air sampling: actively drawing air (pump – mass flow controller) through sorbent-filled tube =sampling followed by offline analysis » Aldehydes ISO 16000-3: active air sampling on DNPH cartridges, followed by HPLC-UV » VOC: ISO 16000-6: active air sampling on Tenax tubes, followed by TD-GC-MS » Online analysis: THC analyser, no identification, just sumparameter 27/06/2012 © 2011, VITO NV 17 Sampling and analysis » Active air sampling: actively drawing air (pump – mass flow controller) through sorbent-filled tube =sampling followed by offline analysis » Aldehydes ISO 16000-3: active air sampling on DNPH cartridges, followed by HPLC-UV » VOC: ISO 16000-6: active air sampling on Tenax tubes, followed by TD-GC-MS » Online analysis: THC analyser, no identification, just sumparameter 27/06/2012 © 2011, VITO NV 18 Sampling and analysis 27/06/2012 © 2011, VITO NV 19 Sampling and analysis » PM sampling » Offline: sampling on filters and weighing » Online: Grimm monitor – optical measurement » SVOC sampling » PUF – Soxhlet extraction…: high flow – long sampling time » High flow: test chambers have flow restrictions! » PDMS/Tenax: » » » » Low flow (indoor air – test chamber air (flow restriction) – personal sampling) gaseous and on PM fraction No sample preparation Validated for PAHs, exploration ongoing for other SVOCs Improved accuracy in the determination of polycyclic aromatic hydrocarbons in air using 24 h sampling on a mixed bed followed by thermal desorption capillary gas chromatography–mass spectrometry, Eric Wauters, VMM 27/06/2012 © 2011, VITO NV 20 Sampling of the material Transport of the sample Storage of the sample before testing ISO 16000-11 Test specimen preparation Testing age and conditioning of the test specimen Measuring technique ISO 16000-3 -6 Analyses Evaluation procedure AgBB, Afsset,… Reporting, labelling Building material emissions to indoor air, Opportunities/consequences for Belgian companies, M. Lor 27/06/2012 © 2011, VITO NV 21 Evaluation AgBB evaluation protocol Mandatory for flooring materials 1st step: identification and assessment of chemical composition 2nd step: testing of VOC and SVOC emissions 27/06/2012 © 2011, VITO NV 22 Afsset evaluation protocol 27/06/2012 © 2011, VITO NV 23 Products may only be made available on the market if they are accompanied by a label, applied to the product or its packaging, indicating their emissions of volatile pollutants 1st september 2011 for products placed on the market 1st september 2013 for all products 27/06/2012 © 2011, VITO NV 24 Evaluation schemes and labels Building material emissions to indoor air, Opportunities/consequences for Belgian companies, M. Lor 27/06/2012 © 2011, VITO NV 25 Testing consumer products cleaning agents, personal care, air fresheners, … Use scenario’s, use conditions 27/06/2012 © 2011, VITO NV 26 Testing electronic equipment ISO 16000-9: general requirements for emission test chamber measurements Electronic devices: ‘active’ emissions sources => special aspects taken into consideration: Duration of testing, sampling times and testing parameters Electrical power => heat => higher levels of emissions Equipment using consumables: printers (ink,…) Equipment not using consumables: PC, TV,… Size of equipment => 1 m³ test chamber 27/06/2012 © 2011, VITO NV 27 SVOC emission testing » No special emission measurements have been standardized for investigating SVOC emissions of electronic devices » Sink effect: released components partially adsorb at chamber walls => determined emission rate is incorrect » Caused by chamber itself => use of appropriate materials (stainless steel) » Also from sample itself: materials are good sinks for the substances emitted by them e.g. porous building materials or foams Uhde et al., Influence of molecular parameters on the sink effect in test chambers, Indoor Air 2006; 16: 158–165 Time to reach equilibrium concentration in the test chamber can be considerably higher compared with VOC measurements 27/06/2012 © 2011, VITO NV 28 SVOC emission testing » Principal compound analysis (PCA) reveals that sink effect essentially depends on a compound’s boiling point (Uhde et al., 2006) » Assessment of sink effects: introduction of pure standards of high boiling compounds into test chamber = recovery test (as described in ISO 16000-25 for the micro-chamber) » Assessment of SVOC in chamber testing: » Sampling during test itself; then » Device out of chamber and » Heating of test chamber and simultaneously sampling, or » Rinsing of the test chamber walls with appropriate solvent » In addition: use of a cooled ‘fogging plate’ for the deposition of SVOC emissions from electronic devices. 27/06/2012 © 2011, VITO NV 29 SVOC emission testing – fogging device •First used in testing of automobile interiors: SVOC condense as a ‘fogging’ film on the inner side of the windscreen •After sampling, film is washed of wtih solvent and analysed •Value in µg is characteristic for SVOC quantity to condense on cold indoor surfaces Wensing M. Emissionen elektronischer Gerate. Neuere Entwicklungen bei der Messung und Beurteilung der Luftqualitat, VDI Berichte, vol. 1443. VDI-Verlag; 1999b. p. 765–74. 27/06/2012 © 2011, VITO NV 30 SVOC emission decay Ref. 2 Ref. 1 » SVOC emissions increase with increasing operating time (> 1 week) These emissions cannot be measured using short-time measuring methods » Due to sink effects and material properties of the studied device 27/06/2012 © 2011, VITO NV 31 VOC emission decay Wensing et al., Emissions from electronic devices: examination of computer monitors and laser printers in a 1 m³ emission test chamber, proceedings of the 9th international conference on indoor air and climate » VOC emissions: » rapid increase in emission strength after turn-on » Then slow decay over time 27/06/2012 © 2011, VITO NV 32 PANDORA, prof. Marc Abadie, Univ. La Rochelle, France 27/06/2012 © 2011, VITO NV 33 27/06/2012 © 2011, VITO NV 34 To conclude » ESR3 Borislav Lazarov: start October » Research work: determination of emission factors of FR » Input for ESR4 (modelling indoor emissions) » ESR2 secondment to VITO, ESR3 secondment to UB » Visits to IVL, SU, VU, UA » Questions? » Now or » frederick.maes@vito.be ; Boeretang 200, 2400 Mol, Belgium » Thanks for your attention! 27/06/2012 © 2011, VITO NV 35 Interesting lecture - references 1. 2. 3. 4. 5. Plastics additives in the indoor environment—flame retardants and plasticizers, Wensing et al., science of the total environment 339 (2005) 19-40 Emissions of organophosphate and brominated flame retardants from selected consumer products and building materials, Kemmlein et al., Atmospheric environment 37 (2003), 5485-5493 Influence of molecular parameters on the sink effect in test chambers, Uhde et al., Indoor Air 2006; 16: 158-165 Emission of flame retardants from consumer products and building materials, BAM (http://www.umweltdaten.de/publikationen/fpdfl/2386.pdf) Organic indoor air pollutants, edited by Salthammer and Uhde, ISBN 978-3-527-31267-2, 2009 27/06/2012 © 2011, VITO NV 36
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