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Kurzfassung An neun verschiedenen Hardcopygeräten wurden in unterschiedlichen Emissionsmesskammern (zwei verschiedene 1 m³ - Kammern und eine 20 m³ - Kammer) in Kombination mit geeigneten Probenahme- und Analysenverfahren Untersuchungen zum Emissionsverhalten dieser Geräte hinsichtlich Staub, Ozon und VOC (TVOC) durchgeführt. Luftprobenahme und Analytik erfolgten für VOC mittels Tenax TA und anschließender Thermodesorption (TDS) in Verbindung mit GC / MS. Ozon wurde kontinuierlich bestimmt. Der Ozonanalysator arbeitete auf der Grundlage der flammenlosen Reaktion von Ozon mit Ethylen nach dem Prinzip der Chemilumineszenz. Die Staubbestimmung erfolgte gravimetrisch mittels Glasfaserfilter und Ultramikrowaage. Zusätzlich wurde die Partikelemission während des Druckbetriebes mit einem Partikelzähler bestimmt. Aufgrund der technischen Rahmenbedingungen standen nur kurze Druckzeiten von maximal 36 Minuten zur Verfügung. Um die Gleichgewichtskonzentration in der Prüfkammer zu erreichen, wurde die Luftaustauschrate in den 1 m³ - Kammern auf n = 4,0 bis 4,7 pro Stunde erhöht. Zusätzlich zur Prüfung in den Emissionsmesskammern sind verschiedene Papiere mittels Direkt - TDS sowie unter- schiedliche Toner mittels Headspaceprobenahme in Kombination mit GC / MS hinsichtlich ihres Emissionsverhaltens untersucht worden.
Für die untersuchten Geräte wurden Emissionsraten ermittelt. Sie betrugen für TVOC 0,41 bis 22,4 mg pro Stück und Stunde, für Ozon kleiner 0,02 bis 4,6 mg pro Stück und Stunde sowie für Staub 0,10 bis 7,63 mg pro Stück und Stunde. Verglichen mit Frischfaserpapier wurden bei den Untersuchungen mit Recyclingpapier deutlich höhere SVOC - Konzentrationen nachgewiesen. Im Ergebnis der Untersuchungen wurde ein Prüfverfahren entwickelt, das die Basis für Emissionsmessungen im Rahmen der Umweltzeichen RAL UZ 62, RAL UZ 85 sowie des neuen RAL UZ 114 für Multifunktionsgeräte darstellt. Abstract The emission behaviour with regard to dust, ozone and VOC (TVOC) of nine different hardcopy devices in combination with suitable air sampling and analysis procedures was investigated in different emission test chambers (two different 1 m³ - chambers and one 20 m³ - chamber). Air sampling and analysis for VOC were done by means of Tenax TA and subsequent thermal desorption (TDS) in connection with GC / MS. Ozone was determined continuously. The ozone analyser worked on the basis of the flame rid reaction of ozone with ethylene according to the principle of chemiluminescence. The dust determination was done gravimetrically by means of glass fibre filter and an ultra micro - balance. Additional the particle emission during the printing process was measured with a particle counter. The general technical conditions of the tested hardcopy devices were the reason for short printing times with a maximum of 36 minutes. In order to achieve the equilibrium concentration in the test chambers the air exchange rate in the 1 m³ - test chambers had to be increased to a value of n = 4,0 to 4,7 per hour. Additional to the examination of the hardcopy devices in the emission test chambers different papers were investi- gated by means of direct - TDS and different toners were tested by means of head space sampling in combination with GC / MS. For the examined hardcopy devices emission rates were determined. The emission rates for TVOC ranged from 0,41 to 22,4 mg per piece and hour, for ozone from less than 0,02 to 4,6 mg per piece and hour and for dust from 0,10 to 7,63 mg per piece and hour. The comparison between recycling paper and paper produced from primary fibres showed in general higher SVOC emissions from recycling paper. As the result of the investigations a test method for the determination of emissions from hardcopy devices was developed. This test method is the basis for emission tests in the framework of the German Award of the Environmental Label for office devices RAL -UZ 62, RAL -UZ 85 and the new RAL -UZ 114 for multifunctional devices.
In this study 50 construction products were tested in emission test chambers according to the requirements of the AgBB-scheme: 7 acrylic and 6 silicone sealants, 6 paste-like synthetic resin plasters, 13 wood based products, 4 adhesives, 5 lacquers, 6 wall paints and 3 further construction products. VOC and odour emissions were tested on the 1st, 3rd, 10th, and 28th day. In addition to the VOC-measurements, a test procedure was developed to evaluate odour emission of construction products.This test is planned to be implemented into the AgBB-Scheme. A direct evaluation by a sensory panel in the emission test chamber was not possible. So the odour samples were collected in 300- litre tedlar bags which were evaluated later. Odour intensity of the samples was compared with different acetone concentrations. Within this study an interlaboratory comparison was conducted using the newly developed odour test method. Additionally, VVOC emissions, detection of carcinogenic compounds, repeatability of emission test chamber tests, and other issues are presented. This project has shown that construction products can be evaluated in accordance with the AgBB scheme. A sensory evaluation is intended to be introduced in the AgBB scheme. A method for this evaluation is described in this study. The test procedure should be enhanced and validated for practical utilisation.
The aim of this study was the development of a low volume air sampling strategy for biocides and polychlorinated biphenyls (PCB) at low air change rates in modern, air-tight showcases as they are present in museums. Lindane, pentachlorophenol, dichlofluanid, tolyfluanid, isodrin, p,p-dichlorodiphenyl trichloroethane and permethrin were the biocides and PCB 28 and PCB 153 were the PCBs studied, all of which are semi volatile organic compounds (SVOC). Their occurrences in the museum environment originate from various sources e.g. preventive treatment of organic exhibits or organic building materials. Exhibits are long-term exposed to these pollutants due to storing in showcases or other storage equipment at low air change rates. To achieve air sampling under the aforementioned conditions the influences of temperature, air circulation, air change rate and relative humidity on the emission behavior of the selected biocides and PCBs had to be determined. This was carried out with pre-soaked wood samples in low volume air sampling experiments using 27 L test showcases and 23 L and 24 L emission test chambers and also diffusive sampling with glass as the sampling material.
Development of a multi-VOC reference material for quality assurance in materials emission testing
(2015)
Emission test chamber measurement is necessary to proof building materials as sources of volatile organic compounds (VOCs). The results of such measurements are used to evaluate materials and label them according to their potential to emit harmful substances, polluting indoor air. If only labelled materials were installed indoors, this would improve indoor air quality and prevent negative impacts on human health. Because of the complex testing procedure, reference materials for the quality assurance are mandatory. Currently, there is a lack of such materials because most building products show a broad variation of emissions even within one batch. A previous study indicates lacquers, mixed with volatile organic pollutants, as reproducible emission source for a wide range of substances. In the present study, the curing of the lacquer-VOC mixture inside micro-chambers was optimised. Therefore, the humidity and the chamber flow were varied. Typical indoor air pollutants with a wide range of volatilities, for example, styrene, n-hexadecane, dimethyl and dibutyl phthalate were selected. It turned out that, under optimised curing parameters inside the micro-chamber, their emission can be reproduced with variations of less than 10 %. With this, a next important step towards a reference material for emission testing was achieved.
Emission testing of products is currently a rapidly increasing field of measurement activity. Labelling procedures for construction products are based on such emission test chamber measurements and hence measurement performance should be verified. A suited procedure for this purpose is the testing of one unique homogenous material in different laboratories within a Round Robin Test (RRT). Therefore, it is useful to have a reference material which can be used within inter-laboratory studies or as part of the quality management system to ensure comparable results. Several approaches on the development of reproducibly emitting materials have been published. These have in common only to emit a single VOC – toluene. Two further research studies carried out by BAM aimed to develop reference material for emissions testing containing one or more VOC in a single material. The first approach was a doped lacquer with Volatile and Semi-Volatile Organic Compounds (VOC/SVOC) and the second was Thermoplastic Polyurethane (TPU) or a Squalane/Paraffin mixture. Results received with the lacquer based material were presented in more detail.
Since some volatile organic compounds (VOC) are
dangerous to human health whilst others cause harm to the environment by influencing the oxidative capacity of the atmosphere, the overall aim of the KEY-VOCs project is to improve the measurement infrastructure for Key Volatile Organic Compounds in indoor and outdoor air. This is done by providing traceable and comparable reference gas standards and by validating new measurement systems in support to the air monitoring networks.
Design of Reference Materials for Proficiency Tests for Measurements in Emission Test Chambers
(2017)
Emission testing of products is currently a rapidly increasing field of measurement activity. Labelling procedures for construction products are based on such emission test chamber measurements and hence measurement performance should be verified. A suited procedure for this purpose is the testing of one unique homogenous material in different laboratories within a Round Robin Test (RRT). Therefore, it is useful to have a reference material which can be used within inter-laboratory studies or as part of the quality management system to ensure comparable results.
Any commercially available product on the market can be used as reference material, provided it is thoroughly characterised. However, these materials often emit only a few and material specific VOCs and appropriate homogeneity is not given. Therefore, alternative materials should be found.
Several approaches on the development of reproducibly emitting materials have been published. These have in common only to emit a single VOC – toluene. Two further research studies carried out by BAM aimed to develop reference material for emissions testing containing one or more VOC in a single material. The first approach was a doped lacquer with Volatile and Semi-Volatile Organic Compounds (VOC/SVOC) and the second was Thermoplastic Polyurethane (TPU) or a Squalane/Paraffin mixture. Currently, the second approach is not at a level that it could be tested within a RRT.
Important requirements for the production of a reference material were repeatability (homogeneity), reproducibility, long-term stability in terms of compound release and transport stability. The emission rates should be high enough to obtain well measurable chamber air concentrations at standardised test conditions.
The lacquer samples were prepared by weighing portions of a water-based lacquer to which defined amounts of the pure analytes were added. Defined amounts of the lacquer mixture were filled into Petri dishes and cured under standard conditions (23 °C and 50% relative humidity). Reproducible emissions were obtained when the storage time of the cured material was not longer than four weeks. The concentrations were analyzed 7 days after loading of the material into the chamber.
Two RRT were conducted by use of the lacquer system. Here, the laboratories had to identify and also to quantify the compounds. The relative standard deviations obtained were typical for such a kind of test. More than 50 participants reported results.
Recent research into emissions of (semi-)volatile organic compounds [(S)VOC] from solid materials has focused on the development of suitable reference materials for quality assurance/quality control of emission test chamber measurements, which fulfill requirements such as homogenous and reproducible (S)VOC release. The approach of this study was to find a method for preparation of a material with predictable (S)VOC emission rates. AVOC (styrene) and an SVOC (2,6-diisopropylnaphthalene, DIPN), loaded into either vacuum grease or a 1:1 mixture of paraffin/squalane, have been tested. For the prediction of the emission rates, a model using the finite element method (FEM) was created to simulate the (S)VOC emission profiles. Theoretical and experimental results obtained in a Micro-Chamber/Thermal Extractor (μ-CTE™) and in 24 L emission test chamber measurements were in good agreement. Further properties were investigated concerning the material applicability, such as shelf life and inter-laboratory comparability. The maximum relative standard deviation in the inter-laboratory study was found to be 20%.
Since some volatile organic compounds (VOC) are dangerous to human health whilst others cause harm to the environment by influencing the oxidative capacity of the atmosphere, the overall aim of the KEY-VOCs project is to improve the measurement infrastructure for Key Volatile Organic Compounds in indoor and outdoor air. This is done by providing traceable and comparable reference gas standards and by validating new measurement systems in support to the air monitoring networks.
Emission testing of products is currently a rapidly increasing field of measurement activity. Labelling procedures for construction products are based on such emission test chamber measurements and hence measurement performance should be verified. A suited procedure for this purpose is the testing of one unique homogenous material in different laboratories within a Round Robin Test (RRT). Therefore, it is useful to have a reference material which can be used within inter-laboratory studies or as part of the quality management system to ensure comparable results. Several approaches on the development of reproducibly emitting materials have been published. These have in common only to emit a single VOC – toluene. Two further research studies carried out by BAM aimed to develop reference material for emissions testing containing one or more VOC in a single material. The first approach was a doped lacquer with Volatile and Semi-Volatile Organic Compounds (VOC/SVOC) and the second was Thermoplastic Polyurethane (TPU) or a Squalane/Paraffin mixture. Results received with the lacquer based material were presented in more detail.
Emission testing of volatile organic compounds (VOC) from materials and products is commonly based on emission test chamber measurements. To ensure the comparability of results from different testing laboratories, their measurement performance must be verified. For this purpose, Bundesanstalt für Materialforschung und -prüfung (BAM) organizes an international proficiency test (round robin test, RRT) every two years using well-characterized test materials (one sealant, one furniture board, and four times a lacquer) with defined VOC emissions. The materials fulfilled the requirements of homogeneity, reproducibility, and stability. Altogether, 36 VOCs were included of which 33 gave test chamber air concentrations between 13 and 83 µg/m3. This is the typical concentration range to be expected and to be quantified when performing chamber tests. Three compounds had higher concentrations between 326 and 1105 µg/m3. In this paper, the relative standard deviations (RSD) of BAM round robin tests since 2008 are compared and the improvement of the comparability of the emission chamber testing is shown by the decrease of the mean RSD down to 28 % in 2018. In contrast, the first large European interlaboratory comparison in 1999 showed a mean RSD of 51 %.
VOC-emissions and their odours from building products and furnishings present indoors should not have an impact on personal well-being or health. Odours can be measured by applying the standard ISO 16000-28. Indoor air determination of odour emissions from building products using test chambers. One of the described procedures is the assessment of perceived intensity using a comparative scale by a group of panellists. In this paper, the perceived intensity sampling procedure and its evaluation method are investigated and shown to need improvement. New technical developments in the methodology used to increase the reproducibility of measurement results are discussed. Since odour tests are used for labelling, they have a major influence on the assessment of construction products, similar to the procedure of the German Committee for Health Evaluation of Building Products (AgBB). In the original ISO standard, the evaluation is typically performed using a sampling container separated from the emission chamber. For a better sample presentation, an adapter was developed to connect the emission test chamber to the evaluation funnel and thus enable an odour assessment which is comparable to a direct measurement. The investigations show that losses of odourous substances can be greatly reduced, which is very desirable when seeking to obtain reliable results in odour measurement. Another experimental series was carried out to reduce the measurement effort in the evaluation of perceived intensity. Application of the developed greater than or less than/equal to. query could be helpful here. The results show that the query mostly leads to the same result as the evaluation of the perceived intensity using the method according to the standard but is much easier to perform. Overall, the results can contribute to improving the acceptance of the evaluation of perceived intensity using ISO 16000-28 and to determining odours from building materials increasingly more precisely.
Biocides are used to protect materials that might be damaged by fungal, microbial or insect activity. The aim of this study is to develop a method for the measurement of these organic compounds, which generally have low or moderate vapor pressures. The biocides considered in this study are permethrin, dichlofluanid, tolylfluanid, iodpropinylbutylcarbamat, octylisothiazolinone, tebuconazole and propiconazole. The emission from two commercial products (plastic foil, wool carpet) containing biocides and of seven types of biocidal formulations applied to wood or clay tiles were investigated in 20-l glass emission test chambers. Each chamber test was performed over a period of 100200 days, and one investigation was conducted over several years. Compared to volatile organic compounds, low-volatility compounds show totally different emission curves in chamber tests; maximal emission values may be reached in days or weeks. A period of 3 months is sometimes necessary for the determination of area-specific emission rates (SERa's). The SERa's (?g m-2 h-1) from biocide-containing products were determined for permethrin (0.006), propiconazole (0.3), dichlofluanid (2.0), tolylfluanid (1.0), octylisothiazolinone (2.5) and iodpropinylbutylcarbamat (2). In most cases, the SERa stayed at its maximum value or declined slowly over the test period. Additionally, a chamber test begun in 1994 with a piece of wood treated with a typical mixture of biocides dissolved in a technical solvent was continued. SERa's (?g m-2 h-1) for dichlofluanid (0.20), tebuconazole (0.49) and permethrin (0.08) remained detectable after the period of nearly 9 years during which the sample remained continuously in the chamber. This test proved the very slow decrease of emission of low-volatility compounds like permethrin and tebuconazole.
In den Grundsätzen des DIBt zur gesundheitlichen Bewertung von Bauprodukten in Innenräumen ist das Bewertungsschema des Ausschusses zur gesundheitlichen Bewertung von Bauprodukten (AgBB-Schema) als wesentliche Grundlage enthalten.
Dieses Schema bewertet die mit Hilfe einer Prüfkammermessung bestimmten Emissionen von flüchtigen und schwer flüchtigen organischen Verbindungen (VOC und SVOC). Die Prüfkammer dient dabei der Einhaltung standardisierter Klimabedingungen (Temperatur 23°C, relative Luftfeuchtigkeit 50 %) sowie der Einstellung bestimmter Prüfparameter wie Luftwechselrate und Beladungsfaktor. Die Anforderungen an eine Prüfkammer sind in DIN EN ISO 16000-9 beschrieben. Die Analytik und Quantifizierung der VOC geschieht mittels Tenax-Thermodesorption und nachfolgender Gaschromatographie gekoppelt mit Massenspektrometrie und ist in DIN ISO 16000-6 beschrieben.
Probenahmen werden am 3. und 28. Tag der Prüfkammermessung durchgeführt. Am dritten Tag erfolgt eine Bewertung der Emissionen aus dem Bauprodukt anhand des TVOC-Wertes und der Summe der detektierten cancerogenen Stoffe (nach 67/548/EWG, Einstufung als cancerogen der Kategorie 1 und 2). Ein Produkt erfüllt die Kriterien, wenn der TVOC-Wert nach 3 Tagen nicht größer als 10 mg/m³ ist und die Summe der Cancerogene 10 μg/m³ nicht übersteigt. Am 28. Tag wird zusätzlich zum TVOC-Wert und den Cancerogenen die Emission von SVOCs berücksichtigt und eine Einzelstoffbewertung anhand von NIK-Werten vorgenommen. Der TVOC-Wert nach 28 Tagen darf nicht größer als 1 mg/m³ sein, die Summe der Cancerogenen nicht größer als 1 μg/m³. Die Summe an SVOCs darf eine Konzentration von 0,1 mg/m³ nicht überschreiten. Der sogenannte R-Wert, die Summe aller Quotienten aus Einzelstoffkonzentration und dem NIK-Wert des Einzelstoffes, darf einen Wert von 1 nicht übersteigen. Außerdem darf die Summe von Substanzen, die keinen NIK-Wert besitzen, nicht größer als 0,1 mg/m³ sein.
Der Ringversuch, der im Rahmen der Untersuchungen zur Verbesserung der Prüfkammermessungen durchgeführt wurde, hatte vor allem den Zweck, den Einfluss unterschiedlicher Methodenparameter bei der Prüfkammermessung in unterschiedlichen Prüflaboratorien zu erfassen. Anhand der Ergebnisse sollte eine Ursachenforschung für die großen Abweichungen der bisher durchgeführten Ringversuche erfolgen. Durch die drei aufeinander aufbauenden Schritte sollte der Einfluss der Analytik, der Probenahme und der Prüfkammer geklärt werden.
Der Ringversuch diente nicht der Anerkennung der teilnehmenden Prüflaboratorien im Bereich der Bauproduktenprüfung für eine DIBt-Zulassung.
Ausgehend von den Prüflaboratorien, die in der Projektgruppe „Prüf- und Messverfahren zur gesundheitlichen Bewertung von Bauprodukten“ des DIBt mitarbeiteten, wurde der Kreis auf europäische Prüflaboratorien erweitert, die sich ebenfalls mit Prüfkammermessungen an Bauprodukten beschäftigen. Dazu erging ein Einladungsschreiben an alle von vorangegangenen Ringversuchen bekannten Teilnehmer. Insgesamt ergab sich ein Teilnehmerkreis von 29 Instituten, davon 16 aus Deutschland, jeweils zwei aus Österreich, Belgien, Schweden, Dänemark und jeweils eins aus Finnland, Großbritannien, Frankreich, Italien und Portugal. Vor Beginn des Ringversuches waren davon 11 im Zulassungsbereich tätig.
Zur wissenschaftlichen Begleitung wurde durch das DIBt ein Betreuergremium einberufen. In zwei Sitzungen (April und November 2007) wurden die aktuellen Ergebnisse vorgestellt und diskutiert sowie die weitere Vorgehensweise besprochen. Eine Abschlussveranstaltung nach der Auswertung des dritten Schrittes des Ringversuches fand im April 2008 im DIBt statt. Dazu waren alle Teilnehmer eingeladen.
Für die Emissionsmessung von flüchtigen organischen Verbindungen (VOC) aus Materialien mit Hilfe von Emissionsprüfkammern sind bisher nur wenige Ringversuche durchgeführt worden (De Bortoli et al. 1999; Jann et al. 2000; Hansen et al. 2000; Oppl and Winkels 2002; Windhövel and Oppl 2005; Kirchner 2007; Oppl 2008). Dabei zeigten sich meist große Streuungen der Ergebnisse.
Ein großes Problem für die Durchführung solcher Ringversuche ist das Fehlen von Referenzmaterialien mit bekannter Emissionsrate von Zielsubstanzen. Deshalb orientiert man sich für die Auswertung solcher Ringversuche am Mittelwert aller Ergebnisse. Dafür ist die Homogenität des Testmaterials von größter Bedeutung. Diese wurde in früheren Ringversuchen nicht wirklich sichergestellt.
Im hier beschriebenen Forschungsprojekt wurde auf die Homogenität des Probenmaterials besonderen Wert gelegt.
Der gesamte Ringversuch wurde in drei Schritte unterteilt. Die einzelnen Schritte wurden dabei von Schritt zu Schritt immer komplexer. Im ersten Schritt erfolgte die Analyse von flüssigen Lösungen, im zweiten die Bestimmung von VOCs in Prüfkammerluft und im dritten Schritt erfolgte eine komplette Emissionsprüfkammermessung bei den Teilnehmern.
Emissions from building products can considerably impair the quality of indoor air. The AgBB scheme is employed to evaluate the emissions of volatile organic compounds (VOC) from building products. The hygienic evaluation according to the AgBB scheme requires product-specific measuring procedures.
These are available for a range of products. They have been validated in co-operation with several research and testing institutes and have been included in the criteria for awarding the Blue Angel ecolabel.
The evaluation is, however, stricter and generally has lower limits. VOC emissions and odours can cause health problems so testing using sensors is an important element in the evaluation of building products and has – for reasons of precaution – been set down in the AgBB scheme. The main goal of the project was to derive a method of evaluation using sensors and limits for awarding the Blue Angel and for the AgBB scheme. Based on the research conducted (see Chapter 5 Results and Discussion), perceived intensity and hedonics were suggested as a suitable Evaluation method. The derivation of limits for the evaluation using sensors on the 28th day was effected in the present study through the additional questioning of the test subjects on the reasonability of a sample.
For the Blue Angel, there could be different limits of perceived intensity and hedonics for each group of products. A preliminary suggestion for possible limits – for all product groups – is a perceived intensity of 7 pi (5 pi + 2 pi as confidence coefficient, Chapter 5.1.5) and -1 (0+/-0.8, rounded to -1) for the hedonic value.
The labelling of construction products or building materials as “low-emitting” is based on measurements using third-party emission test chambers. Unfortunately there is no method to validate the performance of such test chamber measurements. This might give a Variation of results when testing one material at different laboratories. Therefore it is necessary to hold round robin tests as part of the quality management System to ensure comparable results.
A research project financed by the Federal Environmental Agency focused on the development of an external quality management System for the detection of relevant Chemical compounds from products and in ambient air. The project was structured in four phases (Horn et al., 2009 and 2011; Wilke et al., 2009a) This paper shows results of the fourth phase of the project, which was an inter-laboratory study for VOC-emission testing by means of emission test chambers.