4 Material und Umwelt
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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.
Microbially influenced corrosion (MIC) of iron is usually attributed to sulfate-reducing microorganisms (SRM) which act upon the metal by the reactiveness of hydrogen sulfide, and by withdrawal of the available electrons in electrical contact with the metal. Methanogenic archaea can also cause MIC by directly withdrawing electrons from the iron surface for methanogenesis. However, the mechanistic details and kinetics of the overall process are poorly understood. Precipitation of siderite, a by-product of methanogenesis, (4Fe + 5HCO3 + 5H+ 4FeCO3 + CH4 + 3H2O) can lead to an insulating layer on the metal surface and lower the corrosion rate. Still, the extent of FeCO3 precipitation may be significantly influenced by environmental conditions such as pH and advective processes.
Near-ambient pressure XPS makes it possible to characterise samples not compatible to ultra-high vacuum, and enables the study of liquid-solid, gas-liquid and gas-solid interfaces. NAP-XPS meas-urements of biofilms, suspended nanoparticles and metal-organic frameworks were performed with EnviroESCA developed by SPECS.
An interesting application is surface characterisation of biofilms, which are bacterial communities embedded in a self-produced polysaccharide matrix. Various model systems ranging from pure polysaccharides of alginate to biofilms harvested directly from the growth medium have been char-acterised in humid conditions[1].
NAP-XPS also makes it possible to characterise nanoparticles in solution. Silver nanoparticles in aqueous solution were characterised and the Ag 3d-spectrum compared to spectra obtained of dried nanoparticles in UHV-conditions[2]. The binding energy of the Ag 3d-core level peak was shifted by 0,6 eV towards higher binding energy for suspended nanoparticles compared to the dried sample measured in UHV. This can be assigned to a change in surface potential at the water-nanoparticle interface.
Metal-organic frameworks (MOFs) are suitable materials for gas storage of small molecules due to their nanoporous, crystalline structure. However, instability in humidity remains an issue for many types of MOFs. XPS-measurements of the MOF-structure HKUST-1 were performed in various NAP-conditions to assess the stability of the sample and its interaction with the gas molecules as water, methanol and pyridine.
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.
Synchrotron XPS in the soft-X-ray regime is suitable for the detection of light elements commonly found in biological samples. Various model systems of biofilms have been developed and characterised at synchrotron- and lab-based facilities. By obtaining the chemical composition at various information depths, the vertical distribution of iodine in an artificial biofilm have been determined.
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.
Im Zusammenhang mit dem Horizon2020 geförderten Projekt SCALE (GA°730105) untersuchen wir an der BAM die Scandium Spezies in industriellen Restsoffen wie zum Beispiel Rotschlamm. Dabei kommen Methoden wie Elektronenmikroskopie, LA-ICP-MS und auch X-ray Adsorption near edge structure an Synchrotron-Lichtquellen zum Einsatz. Das Verständnis der Bindungsformen des Scandiums soll im Weiteren helfen, metallurgische Gewinnungsmethoden zu verbessern und anzupassen.
The SCALE Project is a Horizon2020 Project (GA°730105) that aims to develope a secure supply chain for Scandium in Europe. To achieve that, the whole value chain is investigated and new methodologies and techniques are being developed. In BAM we are characterizing potential Scandium-bearing industrial by-products.
Background Bacterial biofilms are regarded as the most common cause of chronic infections and are often associated with medical devices, such as implants and catheters. Bacteria growing in biofilms produce a protective, extracellular matrix, which enables them to tolerate much higher antimicrobial concentrations than free-living bacteria and survive long enough to acquire antimicrobial resistance. Preventive and therapeutic strategies against biofilm infections in clinical settings commonly involve the application of multiple antimicrobials: biocidal coatings on the biomaterials and systemically administered antibiotics. This frequent practice harbors the risk of the development of cross-resistance via shared resistance mechanisms between antimicrobials used in material coatings and administered antibiotics.
Aim Our goal is to determine how bacteria adapt to antimicrobials during biofilm formation on surfaces coated with antimicrobials and how population dynamics within biofilms affect the transmission of resistance mutations. Specifically, we want to identify antimicrobial-antibiotic-combinations that select for and against antibiotic resistance in biofilms by following the population dynamics of resistant and susceptible strains in competition assays on a single cell level.
Methodology To study the effect of antimicrobial-antibiotic exposure on resistance development and population dynamics on bacterial biofilms in a multidrug environment, we will grow Pseudomonas aeruginosa on glass surfaces with and without antimicrobial coatings and expose them to antibiotics. First, we will screen in vitro for combinations of antibiotics and antimicrobials that select for and against antibiotic resistance. Second, effective combinations will be chosen for in-depth investigations during bacterial adhesion and of mature biofilms of resistant and susceptible genotypes. Third, based on the outcome of the screen and the obtained mechanistic understanding we will choose a clinical example in which we study the relevance of our findings in biofilms grown in vivo.
Relevance Studying the biointerfacial interactions between bacterial biofilms and medical devices in terms of population dynamics as well as on single cell level during multidrug selection will help us understand how drug resistance develops and spreads in persistent biofilm infections. Based on our findings we aim to provide clinical recommendations for improved administration of antibiotics/antimicrobials in combination with medical device materials in order to mitigate against biofilm associated antimicrobial resistance.
Background Bacterial biofilms are regarded as the most common cause of chronic infections and are often associated with medical devices, such as implants and catheters. Bacteria growing in biofilms produce a protective, extracellular matrix, which enables them to tolerate much higher antimicrobial concentrations than free-living bacteria and survive long enough to acquire antimicrobial resistance. Preventive and therapeutic strategies against biofilm infections in clinical settings commonly involve the application of multiple antimicrobials: biocidal coatings on the biomaterials and systemically administered antibiotics. This frequent practice harbors the risk of the development of cross-resistance via shared resistance mechanisms between antimicrobials used in material coatings and administered antibiotics.
Aim Our goal is to determine how bacteria adapt to antimicrobials during biofilm formation on surfaces coated with antimicrobials, how antimicrobial resistance mutations are acquired and evolve within mature biofilms, and how population dynamics within biofilms affect the transmission of resistance mutations. Specifically, we want to identify antimicrobial-antibiotic-combinations that select for and against antibiotic resistance in biofilms by following the population dynamics of resistant and susceptible strains in competition assays.
Methodology We will grow biofilms of Pseudomonas aeruginosa on glass surfaces with and without antimicrobial coatings and expose them to antibiotics. Then we will track their physiological properties, evolutionary adaptations, and population dynamics. First, we will screen in vitro for combinations of antibiotics and antimicrobials that select for and against antibiotic resistance. Second, effective combinations will be chosen for in-depth investigations during bacterial adhesion and of mature biofilms of resistant and susceptible genotypes. Third, based on the outcome of the screen and the obtained mechanistic understanding we will choose a clinical example in which we study the relevance of our findings in biofilms grown in vivo.
Relevance Studying the biointerfacial interactions between bacterial biofilms and medical devices in terms of population dynamics as well as on single cell level during multidrug selection will help us understand how drug resistance develops and spreads in persistent biofilm infections. Based on our findings we aim to provide clinical recommendations for improved administration of antibiotics/antimicrobials in combination with medical device materials in order to mitigate against biofilm associated antimicrobial resistance.
Microbially influenced corrosion (MIC) of iron is usually attributed to sulfate-reducing microorganisms (SRM) which act upon the metal by the reactiveness of hydrogen sulfide, and by withdrawal of the available electrons in electrical contact with the metal. Methanogenic archaea are supposed to cause MIC. Because they do not produce hydrogen sulfide, withdrawal of electrons may be their main corrosive mechanism; however, mechanistic details and kinetics of the overall process are poorly understood. Precipitation of siderite (4Fe + 5HCO3 + 5H+ 4FeCO3 + CH4 + 3H2O) can lead to an insulating layer on the metal surface and lower the corrosion rate. Still, the extent of FeCO3 precipitation may be significantly influenced by environmental conditions such as pH and advective processes.
Microbially influenced corrosion (MIC) of iron is usually attributed to sulfate-reducing microorganisms (SRM) which act upon the metal by the reactiveness of hydrogen sulfide, and by withdrawal of the available electrons in electrical contact with the metal. Methanogenic archaea are supposed to cause MIC. Because they do not produce hydrogen sulfide, withdrawal of electrons may be their main corrosive mechanism; however, mechanistic details and kinetics of the overall process are poorly understood. Precipitation of siderite (4Fe + 5HCO3 + 5H+ 4FeCO3 + CH4 + 3H2O) can lead to an insulating layer on the metal surface and lower the corrosion rate. Still, the extent of FeCO3 precipitation may be significantly influenced by environmental conditions such as pH and advective processes.
Biofilm formation on materials leads to high costs in industrial processes, as well as in medical applications. This fact has stimulated interest in the development of new materials with improved surfaces to reduce bacterial adhesion.
We present a flow chamber system to test and quantify bacterial adhesion on materials that are part of antifouling concepts. The adhesion process is standardized and can be adapted to different bacteria in subaquatic of subaerial environments. It is combined with a standardized evaluation procedure based on statistical evidence.
Soil microbes are exposed to different environmental stressors originating from various sources. Biocides used as material preservatives can represent environmental stressors since they are in direct contact with the environment including soil. Microorganism in soils can adapt to stress by different mechanisms; for example, by the evolution of resistance by de novo mutations or acquisition of resistance genes via horizontal gene transfer (HGT). Here, we hypothesize that material preservatives could enhance the evolution of biocide resistance enabling the potential for cross-resistance to antibiotics. Furthermore, we hypothesize that material preservatives can cause increased frequencies of HGT (i.e. altered community permissiveness) facilitating microbial community adaptation to stress. We will culture soil microorganism with increasing concentrations of selected biocides followed by antibiotic susceptibility determination. Moreover, we will incubate soil mesocosms with selected biocides to investigate if these compounds promote HGT of plasmids that carry resistance genes in soil microbial communities. Together these results will elucidate the potential for the evolution of biocide resistance and cross-resistance to antibiotics as well as the effect of biocides on adaptation to environmental stressors in soil microbial communities.
Soil microbes are exposed to different environmental stressors originating from various sources. Biocides used as material preservatives can represent environmental stressors since they are in direct contact with the environment including soil. Microorganism in soils can adapt to stress by different mechanisms; for example, by transferring mobile genetic elements via horizontal gene transfer (HGT). Here, we hypothesize that material preservatives can cause increased frequencies of HGT (i.e. altered community permissiveness) facilitating microbial community adaptation to stress. Furthermore, we hypothesize that soil microbial communities are primed by biocide exposure facilitating the response to different types of stresses. We will incubate soil mesocosms with selected biocides to investigate if these compounds promote HGT of plasmids that carry resistance genes in soil microbial communities. Subsequently, we will prime the soil microbial community with sub-inhibitory concentrations of biocides followed by exposure to toxic biocide concentrations or other types of common environmental stresses including metals, antibiotics, and salt. Using suitable control experiments, a shift in the functional response of the primed as compared to the non-primed community would indicate that biocides prime microbial communities via HGT. Together these results will elucidate the effect of biocides on HGT-mediated adaptation to environmental stressors in soil microbial communities.
Soil microbes are exposed to different environmental stressors originating from various sources. Biocides used as material preservatives can represent environmental stressors since they are in direct contact with the environment including soil. Microorganism in soils can adapt to stress by different mechanisms; for example, by transferring mobile genetic elements via horizontal gene transfer (HGT). Here, we hypothesize that material preservatives can cause increased frequencies of HGT (i.e. altered community permissiveness) facilitating microbial community adaptation to stress. Furthermore, we hypothesize that soil microbial communities are primed by biocide exposure facilitating the response to different types of stresses. We will incubate soil mesocosms with selected biocides to investigate if these compounds promote HGT of plasmids that carry resistance genes in soil microbial communities. Subsequently, we will prime the soil microbial community with sub-inhibitory concentrations of biocides followed by exposure to toxic biocide concentrations or other types of common environmental stresses including metals, antibiotics, and salt. Using suitable control experiments, a shift in the functional response of the primed as compared to the non-primed community would indicate that biocides prime microbial communities via HGT. Together these results will elucidate the effect of biocides on HGT-mediated adaptation to environmental stressors in soil microbial communities.
The halophilic bacterium Halomonas elongata can tolerate salt concentrations above 10% NaCl and uses the accumulation of the compatible solute ectoine as a major osmoregulatory mechanism. Ectoine can be accumalted inside the cell through import from the medium or de novo synthesis and establishes an osmotic equilibrium with the surrounding1. Ectoine also protects proteins from the effects of freezing, drying and high temperatures4 and DNA from ionizing radiation2. These features make ectoine a valuable compound for cosmetics and medical devices.
H. elongata was originally isolated from a solar salt facility, where it thrives under high salt concentrations. It was found that marine prokaryotes, which are exposed to high oxidative stress in their environment, vary glycolytic strategies5. A variation in the use of the glucose metabolic pathways is also assumed for H. elongata.
The halophilic bacterium Halomonas elongata can tolerate salt concentrations above 10% NaCl and uses the accumulation of the compatible solute ectoine as a major osmoregulatory mechanism. Ectoine can be accumalted inside the cell through import from the medium or de novo synthesis and establishes an osmotic equilibrium with the surrounding1. Ectoine also protects proteins from the effects of freezing, drying and high temperatures4 and DNA from ionizing radiation2. These features make ectoine a valuable compound for cosmetics and medical devices.
H. elongata was originally isolated from a solar salt facility, where it thrives under high salt concentrations. It was found that marine prokaryotes, which are exposed to high oxidative stress in their environment, vary glycolytic strategies5. A variation in the use of the glucose metabolic pathways is also assumed for H. elongata.
The Cairo Geniza is an “archive” discovered in the 19th century in Ben Ezra Synagogue in Fustat, a district in Old Cairo (Egypt), located south of the center of modern Cairo. The giant collection of mostly Jewish documents that vary in genres, languages and writing supports contains a large number of early medieval Hebrew manuscripts, mostly in fragmentary form. The larger part of the Cairo Geniza is stored today in the Cambridge University Library (CUL).
The Geniza provides sources for the literary, linguistic, historical studies of the various aspects Jewish life. As the documents attest, at least two Jewish communities co-existed in Fustat up to 11th century: a so-called Babylonian and Palestinian. These communities had different leaders, different traditions and lived independently. The differences seem to manifest themselves also in the paleographical, codicological and some material properties of the manuscripts produced by each community.
The aim of this project is to compare the inks used in the Jewish documents depending on different variables: support (paper, parchment), purpose of the manuscript (legal, private, religious), provenance of the scribe. For the determination of the inks type and composition we had to choose non-invasive, non-destructive and portable techniques to analyse the corpus directly in the CUL.
The analyses were carried out with a mobile energy dispersive micro-X-ray spectrometer ArtTAX® (Bruker GmbH, Berlin, Germany), which consists of an air-cooled, low-power molybdenum tube, polycapillary X-ray optics (measuring spot size 70 µm in diameter), an electrothermally cooled Xflash detector, and a CCD camera for sample positioning (Bronk et al 2001, Hahn et al. 2010). All measurements are executed using a 30 W low-power Mo tube, 50 kV, 600 µA Mo tube, and with an acquisition time of 15 s (live time) to minimize the risk of damage (Fig. 1, 2).
Fig. 1: XRF spectrometer probe above a manuscript fragment
Fig. 2: Typical element profile of a XRF linescan
The Dino Lite digital stereomicroscope (Fig. 3) features built-in LED illumination at 395 nm and 940 nm and a customized external white light source. During use, the microscope is fastened to a small tripod or mounted on a Plexiglas ring holder that incorporates a white light source.
Fig. 3: Dino Lite digital stereomicroscope
Fig. 4: Details of one fragment (T-S 16.124) observed with the Dino microscope (x20). On the left, when illuminated with NIR (Near-Infrared, 940 nm) light, the ink fades, indicating iron-gall ink. On the right, the image under NIR light does not change. It is carbon ink.
On example of these studies is the manuscript T-S 16.124 (Cambridge University Library, Fig. 5) whom belongs to the third corpus. It is a deed, written in Hebrew, dated from 1328 (= 1017 CE) and witnessed by a very high number of people (6) comparing to the standard of similar documents (between 2 and 3), from at least two different Jewish communities in Fustat (trans congregational). The verso is written in Arabic (Bareket 1999).
Fig. 5: Manuscript T-S 16.124 (Cambridge University Library)
To compare the inks, we used the fingerprint model. This method relies on the determination of characteristic elemental compositions and represents the amount of a minor constituent relative to the main component, iron in iron gall ink (Malzer et al. 2004, Hahn et al. 2004, Rabin et al 2014). However, a calculation of a fingerprint based on XRF measurements is not possible in the case of carbon ink since carbon, its main component, cannot be detected with this technique.
Fig. 6: Ink fingerprint T-S 16-124 (recto) normalized to iron (Fe)
Conclusion
We show that using reflectography and XRF analysis it is possible to sort the inks according to their type. In the case of the iron-gall inks, use of the ink fingerprint, i.e. amount of the vitriol components normalized to iron we can make direct comparisons of the ink composition.
We would like also to stress that though the methods of material analysis listed above have been successfully employed in the field of cultural heritage and conservation including ancient and medieval manuscripts they have not yet been used to study fragments from the Cairo Genizah. Therefore, we believe that this research project is a pioneering study that will provide new insights into the history of Hebrew writing materials, their production techniques and materials and, thus, contribute new data to the field of Hebrew paleography.