4 Material und Umwelt
Filtern
Erscheinungsjahr
- 2018 (12) (entfernen)
Dokumenttyp
- Posterpräsentation (12) (entfernen)
Referierte Publikation
- nein (12)
Schlagworte
- Nano (3)
- OECD (2)
- Additive Fertigung (1)
- Air exchange rate (1)
- Aluminum (1)
- Analytik (1)
- Anodization (1)
- BFR (1)
- Bioactive glass (1)
- Chamber test (1)
Organisationseinheit der BAM
- 4.2 Material-Mikrobiom Wechselwirkungen (12) (entfernen)
Quality Improvement of VOC chamber emission tests observed for 10 years with round robin tests
(2018)
In Europe, the Construction Products Regulation (CPR, 2011/305/EU) sets basic requirements (BR) on how construction works must be designed and built. BR 3 “hygiene, health and the environment” states low emissions of toxic gases, Volatile Organic Compounds (VOCVOCs), particles, etc. from building materials. Meanwhile, a worldwide network of professional Commercial and non-commercial laboratories performing emission tests for the evaluation of products for interior use has been established.
Therefore, comparability of test results must be ensured. The participation in Round Robin Tests (RRTRRTs) is a means to prove a laboratory’s proficiency. Since 2006 BAM offers such proficiency test for emission chamber test every two years.
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. BAM used different materials over the years. Currently, the best suited reference material is a cured lacquer surface which contained several VOCs added to the liquid lacquer system. The round robin tests 2014, 2016 and 2018 were conducted with such a system.
Compounds like Styrene or n-Alkanes like Decane or Tridecane were tested in many of the proficiency test operated by BAM. Up to now the relative standard deviation of these compounds decrease continuously. Starting with values about 30 % in 2008 we reached values for the mentioned compounds 15 to 20 % now. But even for more polar compounds improved results were received.
Over the years the results of a large group of laboratories detected many compounds with much higher accuracy than at the beginning. So, the comparability between results of different laboratories becomes much better.
In addition to previously reported results on the simulated aging of polystyrene samples (PS) containing 1 wt. % hexabromocyclododecane (HBCD), we present the first results of our investigations of polypropylene (PP)-samples containing 0.1 wt. % BDE-209. All studied polymer samples were exposed to a defined weathering schedule in a climate chamber in accordance to regulation EN ISO 4892-3:2006.For the determination of BDE-209 in the collected rain water samples derived from the used climate chamber, the samples were prepared in accordance with a validated protocol. Before the analyses, each sample was spiked with 2 µL of isotopically labeled BDE-209 (13C10-BDE-209) to serve as internal standard (ISTD) in the performed stable isotope dilution analysis. Subsequently the samples were extracted with isooctane, the obtained aliquots of the extracts were concentrated to 200 µL and 2 µL of the resulting solution were injected to the GC/MS for quantification.
Additionally, the total bromine contents are monitored for the aged and untreated samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) as well as X-ray fluorescence analysis (XRF) as non-destructive and rapid method. Furthermore, results from surface analysis using environmental scanning electron microscopy (ESEM) for morphological characterization of the aged and untreated samples were presented and discussed. In general, the resulting data from the accelerated aging will be compared to those from the natural weathering experiments (“atmospheric exposure”, in soil).
The atmospheric exposure was performed by placing the samples on a weathering rack, which is aligned in SW direction (in a 45° angle to the horizon). The weathering data were regularly recorded by Deutscher Wetterdienst at this site. The surfaces of the test specimens (aged and stored references) were analyzed by ESEM as well as by LA-ICP-MS and by XRF. The surface of PS and PP specimens aged outdoors present the aging under real conditions and allow the comparison to the accelerated aged specimens by means of the weathering chamber. This way, we explore the efficiency of the accelerated aging procedure, which provides the advantage of well-defined and reproducible conditions compared to natural weathering, as a tool for testing different plastic materials.
Additionally “in soil” experiments were conducted in-door in a well characterized testing soil. The soil (boulder-clay, sand with 12 % loam, particle size in total 0.2-4 mm) is filled in a free-draining concrete basin inside of an air-conditioned room. In this manner, TOC, water capacity and humidity are recorded parameters. To assure a washing out process from the samples by the raining water, the target water content is calculated to 8%. The actual humidity is measured by a tensiometer, assuring the duration of the raining period. The water content is additionally monitored by weight of the basin, capturing water from raining periods. The correct humidity is a fundamental parameter for biological activity. Samples of PS resp. PP were of dimension 10x1cm and 5 specimens were placed up to the half in the soil per basin. Microbial activity of the soil, monitored by the reference polyurethane, sets HBCD resp. BDE-209 of the samples free and will be leached from the samples by raining water. Thereafter these will be captured by passive samplers placed in a distinct distance to the samples in the soil. The “in soil” experiments are complementary to the weathering experiments due to the biological activity in the soil. These experiments simulate the fate of the brominated flame retardants in the biosphere.
The particle size distribution is considered the most relevant information for nanoscale property identification and material characterization. The current OECD test guideline on particle size and size distribution (TG 110) is not applicable to ‘nano-sized’ objects. In this project we thus develop a new OECD test guideline for the measurement of the size and size distribution of particles and fibers with at least one dimension in the range of 1 - 1000 nm. A fiber is defined as an object having an aspect ratio of length/diameter l/d >3. The width and length of each fiber should be measured concurrently.
In order to measure the particle size distributions, many techniques are available. 9 methods for particles and 2 methods for fibres have been tested in a prevalidation study and appropriate methods will be compared in an interlaboratory round robin test starting in February 2019.
In Vorbereitung einer Restaurierung erfolgten naturwissenschaftliche Untersuchungen zu Schadensphänomenen und Glaszusammensetzungen an mittelalterlichen Gläsern aus der Dorfkirche in Koszewko (Polen)im Environmental Scanning Electron Microscope (ESEM) mit EDX. Die Ergebnisse zeigen, dass die Glasverwitterung schon sehr stark vorangeschritten ist und ein zukünftiger Schutz der mittelalterlichen Glasmalereifelder vor Umwelteinflüssen unbedingt notwendig ist. Es wurde ein Schutzverglasungsystem entwickelt, das speziell auf den langfristigen Erhalt der einzelnen mittelalterlichen Glasmalereifelder ausgelegt ist.
There is a need for an assessment of the emission properties of volatile organic compounds (VOCs) from consumer products. A method comparison was carried out to evaluate adapted and cost-effective procedures for such items. Smaller and automated emission chambers de-picted similar kinetics compared to a 203 L standard chamber. Toy samples made of PVC (Polyvinyl chloride) emitted more VOCs compared to other tested polymeric products. The emissions from 2 selected samples were studied to allow an evaluation of the resulting room concentration and external exposure of a child. Obtained concentrations were not of concern.
Comparison of Formaldehyde Concentrations in Emission Test Chambers Using EN 717-1 and EN 16516
(2018)
For many years EN 717-1 (Wood-based panels - Determination of formaldehyde release - Part 1: Formaldehyde emission by the chamber method) is the standard for formaldehyde emission testing of wooden boards. In 2017 EN 16516 (Construction products - Assessment of release of dangerous substances - Determination of emissions into indoor air) was published as a new harmonised standard for the emission testing of construction products. Because test chamber conditions are different, both standards give different concentrations for formaldehyde. For the determination of a conversion factor four test series were set up with different wooden boards.
Sintered bioactive glass scaffolds of defined shape and porosity, e.g. made via additive manufacturing, must provide sufficient bioactivity and sinterability. As higher bioactivity is often linked to high corrosion and crystallization tendency, a certain compromise between sintering ability and bioactivity is therefore required. Groh et al. developed a fluoride-containing bioactive glass (F3), which allows fiber drawing and shows a bioactivity well comparable to that of Bioglass®45S5.
To study whether and to what extent the sinterability of F3 glass powder is controlled by particle size, coarse and fine F3 glass powders (300-310µm and 0-32µm) were prepared by crushing, sieving and milling. Sintering, degassing and phase transformation during heating were studied with heating microscopy, vacuum hot extraction (VHE), DTA, XRD, and SEM.
For the coarse glass powder, sintering proceeds slowly and is limited by surface crystallization of primary Na2CaSi2O6 crystals. Although the crystallization onset of Na2CaSi2O6 is shifted to lower temperature, full densification is attained for the fine powder. This finding indicate that certain porosity might be tuned via particle size variation. Above 900°C, intensive foaming is evident for the fine powder. VHE studies revealed that carbon species are the main foaming source.
The OECD test guidelines (TGs) for testing chemicals have been widely used for regulatory purposes all over the world since the establishment of the Mutual Acceptance of Data (MAD) principle in 1984. This MAD principle ensures that, if a chemical is tested under the Good Laboratory Practice (GLP) conditions accordingly to an OECD TG, the data should be accepted in all OECD countries. The TGs have been developed, harmonized, internationally validated (round robin tests) and adopted by OECD countries to be used for the physical-chemical characterisation, fate estimation, and hazard identification for risk assessment of various chemicals. In addition to the TGs, OECD Guidance Documents (GDs) usually provide guidance on how to use TGs and how to interpret the results. These GDs do not have to be fully experimentally validated, and hence they are not under MAD, but they are based on relevant published scientific research.
But are the existing TGs and the related GDs applicable and adequate for the regulatory testing of nanomaterials? In general, it is accepted that most of the "endpoints" or more precisely measurement variables are applicable also for nanomaterials. However, for some endpoints new or amended TGs are needed. In addition, several GDs are needed to give more precise advice on the test performance in order to gain regulatory relevant data on nanomaterials.
The poster will present the status quo on recent TGs and GDs development for nanomaterials at OECD level with relevance for physical-chemical characterisation. Emphasis will be given to the proposed OECD TG on particle size and size distribution for manufactured nanomaterials. The development of such a TG is of special importance as particle size and size distribution is considered as major information for nanomaterial identification and characterization. A reliable and reproducible characterisation of particle size and size distribution is also needed for chemicals risk assessment of nanomaterials, for instance to interpret and compare test results and - in future – to forecast interaction and effects of nanomaterials. The presented poster will illustrate the way from the idea for a new TG and new GD to an accepted OECD TG/GD.
The new OECD test guideline will address the following four main steps in the determination of the length and width distributions of fibers: sample preparation, image acquisition, data evaluation and uncertainty analysis. As the sample preparation has to be optimized for each material, general quality criteria will be given in the protocol. For full visibility of a fiber the appropriate resolution has to be chosen. In the data evaluation the length and diameter of each fiber will be determined concurrently to allow for application of different regulatory definitions. The quality of the results critically depends on the sample preparation as well as the data evaluation. In this step the classification rules have to be formulated and followed accurately in order to optimize reproducibility of the method. The SOP will be validated in an international round robin test, which is planned for 2018/2019.