4 Material und Umwelt
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Organisationseinheit der BAM
- 4 Material und Umwelt (440)
- 4.4 Thermochemische Reststoffbehandlung und Wertstoffrückgewinnung (93)
- 4.1 Biologische Materialschädigung und Referenzorganismen (91)
- 4.3 Schadstofftransfer und Umwelttechnologien (81)
- 4.2 Material-Mikrobiom Wechselwirkungen (77)
- 4.5 Kunst- und Kulturgutanalyse (66)
- 4.0 Abteilungsleitung und andere (46)
- 6 Materialchemie (30)
- 1 Analytische Chemie; Referenzmaterialien (27)
- 6.1 Oberflächen- und Dünnschichtanalyse (16)
In Deutschland ist ab 2029 eine Phosphorrückgewinnung aus Klärschlamm verpflichtend. Ausgenommen sind Klärschlämme mit weniger als 20 g P/kg TM. Für die Phosphorbestimmung sind verschiedene Methoden nach Klärschlammverordnung als gleichwertig zugelassen: Der Königswasseraufschluss in der Mikrowelle und am Rückfluss sowie die Messung an ICP-OES, ICP-MS und die photometrische Bestimmung mittels Ammoniummolybdaten. An der BAM wurden die unterschiedlichen Methodenkombinationen aus Aufschluss- und Messmethode an 15 Klärschlämmen überprüft und in einem Ringversuch mit einem Klärschlamm getestet. Die Ergebnisse werden in diesem Vortrag zusammengefasst. Als Folge der Untersuchungen wird für die Phosphorbestimmung in Klärschlamm die ICP-OES-Messung nach Königswasseraufschluss in der Mikrowelle empfohlen.
Agricultural sewage sludge utilization becomes less important in Germany. In 2017, new fertilizer and waste laws caused the agricultural sewage sludge utilization to collapse by more than a quarter. From 2029, in German wastewater treatment plants (WWTPs) phosphorus (P) must be recovered from sewage sludge ifit contains more than 2 wt % P. Agricultural utilization will be prohibited for large WWTPs > 100,000 population equivalents (pe) from 2029 and > 50,000 pe from 2032. In Germany, each federal state must annually report amounts and quality of agriculturally utilized sewage sludge which was 17 % of the total disposal in 2019. The reports of 10 States were evaluated for 2016 and 2017 representing approx. 60 % ofthe total agriculturallyused sludge volume. Whereas phosphorus recovery is mandatory this does not apply to other nutrients. However, many P recovery processes recover other nutrients, too. Considering three differentscenariosfor future German sewage sludge disposal shows that 70 - 77 % ofthe P load in sewage sludge will probably be recovered in the future. At the same time, this applies for about 0 - 16 % of nitrogen, 36 - 52 % of calcium, 31-53 % of potassium, and 40 - 52 % of magnesium. However, these recovered nut rient loads can substitute only 1 % or less ofthe commercial fertilizer demand except from phosphorus which is about 45 % ofthe demand.
Die Ergebnisse des extraWERT-Vorhabens wurden Vertreter*innen des Umweltministeriums von Bund und Ländern vorgestellt und im Zusammenhang mit dem Vollzug der AbfKlärV diskutiert. Es ging um die Phosphorschwankungen in kommunalem Klärschlamm und eine Empfehlung der Untersuchungshäufigkeit, um den Phosphorgehalt rechtssicher festzustellen. Des weiteren wurde die Performance verschiedener nach Verordnung gleichwertiger Analyseverfahren für Phosphor in Klärschlamm diskutiert anhand von Ringversuchsergebnissen und Eigenuntersuchungen an 15 Klärschlammproben.
Gleichwertigkeit der nach AbfKlärV zulässigen Verfahren zur Phosphorbestimmung in Klärschlamm
(2021)
In dem Meeting wurde den Notifizierern und Ausrichtern des jährlichen länderübergreifenden Ringversuchs Klärschlamm die Ergebnisse zu Untersuchungen hinsichtlich der Gleichwertigkeit verschiedener nach AbfKlärV zulässiger Verfahren zur Phosphorbestimmung in Klärschlamm vorgestellt. Die Untersuchungen an 15 Klärschlammproben ergaben die höchsten Ergebnisse für das Messverfahren ICP-OES und das Aufschlussverfahren in der Mikrowelle. Diese Ergebnisse wurden im Ringversuch bestätigt.
Die landwirtschaftliche Klärschlammverwertung ist in der Bundesrepublik Deutschland seit Jahren rückläufig. Neben den Risiken durch Schadstoffeinträge gibt es in Deutschland Regionen mit einem stark erhöhten Nährstoffüberschuss. Um die Grundwasserbelastung zu verhindern wurde u.a. das Düngerecht verschärft, was die Flächenkonkurrenz zwischen Klärschlamm und Wirtschaftsdünger vergrößern wird.
Es ist davon auszugehen, dass sich die neuen Regelungen im Düngerecht und der Klärschlammverordnung massiv auf die landwirtschaftliche Verwertung von Klärschlamm und damit auf die Kreislaufwirtschaft verschiedener Nährstoffe auswirken werden. In diesem Beitrag werden erste Ergebnisse des Projekts extraWERT vorgestellt.
Es wurden erste Ergebnisse des Projekts extraWERT vorgestellt. Im Projekt werden monatlich Klärschlammproben von 10 kommunalen Kläranlagen untersucht, deren P-Gehalt im Grenzbereich der AbfKlärV liegt zwischen 1,7 und 2,3%. Die ersten Ergebnisse lagen zu fünf Kläranlagen vor, es wurden Daten zum TS-Gehalt, zur oTS und zu den Nährstoffgehalten präsentiert.
New developments in legislation and technology development for P-recovery were presented with focus on the situation in Germany.
Im Projekt extraWERT geht es um die Ermittlung von Nährstoffpotenzialen in Abwasser und Klärschlamm. Neben kommunalen Kläranlagen soll auch die Industrie als Quelle für nährstoffreiche Abfallströme betrachtet werden. Mit dem Vortrag sollten Mitglieder des MIV zu einer Projektbeteiligung bewegt werden. Es sollen rohes und gereinigtes Abwasser von direkt einleitenden Betrieben auf Makronährstoffe untersucht werden, neue Erkenntnisse werden insbesondere für die Nährstoffe Calcium und Magnesium erwartet.
Vorstellung des REFOPLAN-Projekts extraWERT Erhebung zusätzlicher Wertstoffpotenziale in Klärschlamm
(2019)
Auf dem Regionalgruppentreffen wurden erste Projektergebnisse vorgestellt und die Probenahmestrategie diskutiert. Vorgestellt wurde eine Rückberechnung der mittleren Wertstoffgehalte aus dem Klärschlamm-Monitoring 2014 (Krüger und Adam) und erste Auswertungen der Klärschlammbericht-Rohdaten aus NRW und Hessen.
For centuries, churches, secular buildings and museums have been furnished with valuable works of art. Many works of art are UV- and light-sensitive. It is well known that especially UV radiation causes damage and discoloration in paintings, textiles, plastics, wood and other materials. In particular, the wavelengths between 280 and 410 nm cause color changes, embrittlement or destruction of e.g. plastics over time. Therefore, strongly UV-absorbing glasses are advantageous for architecture and are necessary for the protection of cultural assets. As restorers in all disciplines become more and more aware, the demands placed on buildings and their furnishings in terms of climate are becoming increasingly detailed and precise. The aim in each case is to preserve the valuable artwork.
For some years now, the industry has been offering the protection of cultural objects by installing special UV-protective glasses. Currently, UV protection for church buildings is realized by laminated safety glass equipped with appropriate UV-protective plastic films. Technically, this always means a second pane of glass in front of the windows, which is installed outside the building. This creates climatic gaps that are difficult to control and deterioration due to ageing effects can be expected. At the same time, this protective glazing is not invisible and has a considerable aesthetic influence on the interior and exterior appearance of the building. Meanwhile, the preservation of historical monuments accepts such aesthetic cuts on buildings in order to protect the artwork in the interior from UV light. To this day, however, the long-term durability of UV protection provided by inserted plastic films is still controversial.
To date the only available alternative on the market is a mouth-blown UV protection glass which uses a so-called overlay to provide UV protection. This shows that UV protection can also be achieved by glasses without plastic films thus realizing an exclusive inorganic protection which normally is more stable than a polymeric one. So far there are not enough studies to prove long-term durability.
The aim of this project is to provide existing glazing or new glazing to be created with a highly transparent layer that ensures this UV-protective filter function below 400 nm. The glass coating is to be applied to the glass over a large area and fired into the surface like a classic ceramic enamel paint with the same technics. In addition, it should be long-term durable in its function. It means, that the glass has to be fused at temperatures below 630 °C during the firing process, its chemical durability has to be high, its coefficient of thermal expansion has to be as close as the one of the substrate (usually float glass) and the glass has to absorb the UV-radiation within a thin thickness (thinner as 100 µm).
In this project, the long-term durability of commercial UV-protective glasses is examined. New low melting glasses containing UV-absorbing ions are being developed. Their UV-absorption as a thin layer is analyzed as well as their chemical durability and their thermal properties.
We are grateful to BMWI for the financial support in the frame of the Central Innovation Programme for SMEs (ZIM).
Today glass is broadly used in modern architecture. For applications indoor it is possible to produce decor glass by using enamel colors and glass painting techniques without any problems. However, this is more limited for applications outdoor. Humidity and environmental pollution attack the surface of the coating and damage it strongly. There are only few colors on the market which are resistant towards acids and bases until now. Additionally, most of those colors are opaque. In order to extend the color palette, chemically resistant colored glasses are being developed which are transparent, relatively low melting and intensively toned even in thin coat thickness. To achieve such ambitious aim, many parameters have to match which act in complex manner. Metal oxides were used to color the glasses. A lead-free glass composition was developed to avoid an exposition of heavy metals to the environment. The glasses were characterized, in particular in terms of their thermal properties, their crystallization and corrosion behavior as well as their chemical and environmental durability. Different practical applications will be shown.
Quantitative chemical analysis of airborne particulate matter (PM) is vital for the understanding of health effects in indoor and outdoor environments, as well as for enforcing air quality regulations. Typically, airborne particles are sampled over long time periods on filters, followed by lab-based analysis, e.g., with inductively coupled plasma mass spectrometry (ICP-MS). Within the EURAMET EMPIR AEROMET project, cascade impactor aerosol sampling was combined for the first time with on-site total reflection X-ray fluorescence (TXRF) spectroscopy to develop a tool for quantifying particle element compositions within short time intervals and even on-site. This makes variations of aerosol chemistry observable with time resolution of only a few hours and with good size resolution in the PM10 range. A proof of principles of this methodological approach and the comparison to standard methods within the scope of a field campaign will be presented. Secondly, aerosol sampling and TXRF analysis seems suitable for the quantification of elements in indoor aerosols as well and may provide an important enhancement of existing methods for the analysis of organic species in aerosols (such as sampling and TD-GC/MS). As an example, the TXRF analysis of particles emitted from laser printers under controlled conditions in an environmental test chamber will be presented.
Quantitative chemical analysis of airborne particulate matter (PM) is vital for the understanding of health effects in indoor and outdoor environments and required by EU air quality regulations. Typically, airborne particles are sampled on filters, followed by lab-based analysis, e.g., with inductively coupled plasma mass spectrometry (ICP-MS). Within the EURAMET EMPIR AEROMET project, cascade impactor aerosol sampling was combined with on-site total reflection X-ray fluorescence (TXRF) spectroscopy. The study aimed at a proof of principles for this new mobile and on-size tool for the quantification of aerosol element compositions and element mass concentrations within short time intervals of less than 12 h. In a field campaign the method’s technical feasibility could be demonstrated. The TXRF results were traced back to a stationary, reference-free XRS setup in the laboratory of the German national metrology institute PTB at the BESSY II electron storage ring in Berlin, Germany. Simultaneous PM10-filter sampling, followed by standardized lab-based analysis, allowed for a comparison of the field campaign data of both methods. As Fig. 1 shows, the correspondence between PM10 filter sampling and ICP-MS, and on the other hand, cascade impactor sampling and TXRF is quite encouraging. However, for some of the analysed elements, e.g. V and Pb, the observed deviations are higher than expected and this highlights the fact, that spectral deconvolution strategies for TXRF on cascade impactor samples still need some improvement.
This work was supported by the EMPIR programme, co-financed by the Participating States and from the European Union’s Horizon 2020 research and innovation programme, through grant agreements 16ENV07 AEROMET and 19ENV08 AEROMET II
Measurements of aerosol particles are vital for enforcing EU air quality regulations to protect human health, and for research on climate change effects. Although metrics such as PM10 and PM2.5 are currently in use, the level of uncertainty of aerosol metrics is too high and the traceability is insufficient. The project AEROMET, which has been started in June 2017 aims at implementing improvements in a) the uncertainty of particle mass, size and number concentration measurements and b) in the characterization of regulated components in airborne particles. Both are demanded by existing networks within the EU as well as by global atmospheric research.
On-site measurement campaigns
One of the objects is the application of mobile x-ray spectroscopy techniques combined with aerosol sampling techniques for quantifying particle compositions in the field for real time analysis. During two in-field measurement campaigns in Budapest, Hungary in May 2018 and Cassino, Italy in September 2018 the size dependent mass concentrations of specific elements in ambient aerosols were monitored under dynamic conditions.
Typically, airborne particles are sampled on filter substrates. During this project new sampling methods with specially designed substrate holders for an in-situ TXRF analysis were developed and applied for the first time. This approach allows a direct time and size resolved analysis without laborious digestion steps and a reduced risk of contamination.
Aerosol particles were sampled in a 13-stage DLPI impactor - size range from 0,03 µm to 10 µm - which was equipped with special adapters for acrylic discs of 30 mm diameter, serving as substrates. TXRF analysis was performed on site with the transportable spectrometer S2 PICOFOX (Bruker Nano GmbH) equipped with a Mo X-ray tube and a 30 mm² Silicon Drift Detector (SDD). Excitation conditions were 50 kV, 600 µA, measurement time 1000 s. Quantification was based on internal standardization using 50 ng of Y in solution, which was pipetted into the centre of the discs prior to sampling.
At moderate air pollution levels, i.e. PM10 ~ 20 µg/m³, sampling times of less than 2 hours were enough for the detection of elements in different particle size bins. The in-situ approach and the high sensitivity of TXRF enables the observation of rather quick changes in the quantity and distribution of elements in an ambient aerosol on the day of sampling, as the below example from the Cassino field campaign on 11 Sept. 2018 shows: The analysis of the morning and afternoon sampling shifts reveals the occurrence of the elements Fe, Ca and Si in different size bins as well as their significant temporal change in respective mass concentrations over the day while the distributions of several other elements in the aerosol remain unchanged.
The validation of these results by backup measurements is planned.