Filtern
Erscheinungsjahr
Dokumenttyp
- Vortrag (41)
- Zeitschriftenartikel (26)
- Beitrag zu einem Tagungsband (23)
- Posterpräsentation (5)
- Beitrag zu einem Sammelband (4)
- Forschungsbericht (4)
- Buchkapitel (1)
Schlagworte
- Sewage sludge ash (10)
- Elutionsverfahren (7)
- Resource recovery (7)
- Klärschlammasche (6)
- Phosphorus recovery (6)
- Column test (5)
- Critical raw materials (5)
- Leaching (5)
- Phosphorus (5)
- Batch test (4)
Organisationseinheit der BAM
Eingeladener Vortrag
- nein (41)
Monitoring of PAH in aqueous samples - a comparison of different sample preparation techniques
(2011)
In der Bundes-Bodenschutz- und Altlasten-verordnung (BBodSchV) und im Arbeits-entwurf der Novellierung ist für den Wirkungspfad Boden-Grundwasser eine Sickerwasserprognose vorgesehen, um die Gefahren, die von kontaminierten Stand-orten für das Schutzgut Grundwasser ausgehen, beurteilen zu können. Bei der Sickerwasserprognose kann u.a. auf der Grundlage von Materialuntersuchungen im Labor die Quellstärke kontaminierter Ma-terialen ermittelt werden, welche dann bei Transportmodellierungen Berücksichtigung findet. Der Entwurf der Novellierung der BBodSchV sieht für die Ermittlung der Quellstärke den Übereinstimmungstest des Säulenversuchs nach DIN 19528 bis zu einem Wasser/Feststoff - Verhältnis (W/F) von 2 l/kg für anorganische und organische Stoffe (PAK) oder den Schüttelversuch nach DIN 19529 für anorganische Stoffe und E DIN 19527 für organische Stoffe auch jeweils mit einem W/F von 2 l/kg vor. Die Zulassung beider Elutionsverfahren setzt die Gleichwertigkeit der Ergebnisse beider Verfahren voraus. Im Folgenden werden die Ergebnisse des Vergleichs der Auslaugung von polyzyklischen aromat-ischen Kohlenwasserstoffen (PAK) aus unterschiedlichen Böden mit Hilfe beider Elutionsverfahren vorgestellt.
Mit dem Entwurf der im Januar 2011 vom Bundesumweltministerium vorgelegten Mantelverordnung, welche eine Novelle der Bundes-Bodenschutz- und Altlastenverordnung sowie der Grundwasserverordnung sowie die neue Ersatzbaustoffverordnung (ErsatzbaustoffV) umfasst, werden neue Methoden zur Herstellung von wässrigen Eluaten im Gesetzestext verankert, In der Novelle der BBodSchV werden in diesem Zusammenhang für organische Schadstoffe u.a. Säulen- oder Schüttelverfahren genannt. Bei den Säulenversuchen sollen Perlcolate bis zu einem Flüssigkeits-Feststoffverhältnis von 2 1/lcg entsprechend dem Übereinstimmungstest nach DIN 19528 gesammelt werden. Das Schüttelverfahren soll nach E DIN 19527 („Schüttelverfahren zur Untersuchung des Elutionsverhaltens von organischen Stoffen mit einem Wasser/Feststoff-Verhältnis von 2 1/lcg“) durchgeführt werden.
In der Ersatzbaustoffverordnung wird als Verfahren zur Herstellung von wässrigen Eluaten bisher nur das Säulenverfahren nach DIN 19528 („Perlcolationsverfahren zur gemeinsamen Untersuchung des Elutionsverhaltens von anorganischen und organischen Stoffen“) genannt.
In diesem Beitrag wird ein Vergleich der Ergebnisse von Säulen- und Schüttelverfahren als Übereinstimmungstest für Böden und Bodenmaterialien, welche mit polyzyklischen aromatischen Kohlenwasserstoffen (PAK) und Mineralölkohlenwasserstoffen (MICW) belastet sind, vorgenommen.
Synthetic athletic tracks and turf areas for outdoor sporting grounds may release contaminants due to the chemical composition of some components. A primary example is that of zinc from reused scrap tires (main constituent, styrene butadiene rubber, SBR), which might be harmful to the environment. Thus, methods for the risk assessment of those materials are required. Laboratory leaching methods like batch and column tests are widely used to examine the soil–groundwater pathway. We tested several components for artificial sporting grounds with batch tests at a liquid to solid (LS) ratio of 2 L/kg and column tests with an LS up to 26.5 L/kg. We found a higher zinc release in the batch test eluates for all granules, ranging from 15% higher to 687% higher versus data from column tests for SBR granules. Accompanying parameters, especially the very high turbidity of one ethylene propylene diene monomer rubber (EPDM) or thermoplastic elastomer (TPE) eluates, reflect the stronger mechanical stress of batch testing. This indicates that batch test procedures might not be suitable for the risk assessment of synthetic sporting ground components. Column tests, on the other hand, represent field conditions more closely and allow for determination of time-dependent contaminants release.
Artificial surfaces for outdoor sporting grounds may pose environmental and health hazards that are difficult to assess due to their complex chemical composition. Ecotoxicity tests can indicate general hazardous impacts. We conducted growth inhibition (Pseudokirchneriella subcapitata) and acute toxicity tests (Daphnia magna) with leachates obtained from batch tests of granular infill material and column tests of complete sporting ground assemblies. Ethylene propylene diene monomer rubber (EPDM) leachate showed the highest effect on Daphnia magna (EC50 < 0.4% leachate) and the leachate of scrap tires made of styrene butadiene rubber (SBR) had the highest effect on P. subcapitata (EC10 = 4.2% leachate; EC50 = 15.6% leachate). We found no correlations between ecotoxicity potential of leachates and zinc and PAH concentrations. Leachates obtained from column tests revealed lower ecotoxicological potential. Leachates of column tests of complete assemblies may be used for a reliable risk assessment of artificial sporting grounds.
Ziel des Vorhabens ist es, die Robustheit des Schüttelverfahrens nach E DIN 19527 mit einem Wasser-/Feststoffverhältnis von 2 l/kg für unterschiedliche Bodenarten und Bodenmaterialien zu überprüfen. Gleichzeitig soll bei diesen Untersuchungen das Stoffspektrum auf weitere prioritäre organische Kontaminanten erweitert werden. Dies stellt die Voraussetzung für die Durchführung von Ringversuchen zur Validierung der Norm DIN 19527 dar.
Sulfonamides (SAs) and their metabolites present severe hazards to human health and the environment, mainly because of antibiotic resistance. Knowledge of their bioavailability, including their sorption to soils and their impact on the soil-groundwater pathway, is crucial to their risk assessment. Laboratory batch and column leaching tests are important tools for determining the release potential of contaminants from soil or waste materials. Batch and column tests were carried out with soils differing in particle size distribution, organic matter content and pH, each spiked with sulfonamides (sulfadimethoxine (SDM), sulfaguanidine (SGD), sulfisoxazole (SX)). In order to test the applicability of leaching tests to polar contaminants batch and column tests were also compared. In the column tests, release was found to depend on the properties of both soil and sulfonamides. The fastest release was observed for coarse-grained soil with the smallest organic matter content (MS soil; 100% decrease in concentration until liquid-to-solid ratio (L/S) of 0.9 L kg-1 for all SAs). The slowest release was established for sulfadimethoxine (24.5% decrease in concentration until L/S 1.22 L kg-1). The results of the batch and column tests were comparable to a large extent, with slightly higher concentrations being obtained in the column test experiments of fine-grained soils with a high organic matter content.
Über den derzeitigen und zukünftigen Umgang mit Klärschlamm wird in Deutschland seit Jahren kontrovers diskutiert. Zum einen enthalten kommunale Klärschlamme Nährstoffe, die sinnvoller Weise wieder in die landwirtschaftliche Nahrungsmittelproduktion eingebracht werden sollten. In diesem Zusammenhang steht Phosphor im Vordergrund, da diese Ressource begrenzt ist und deren zukünftig zu erwartende Knappheit neben der geringen Anzahl an Exportländern für Rohphosphate zu unberechenbaren Preissprüngen am Weltmarkt führen können. Zum anderen stellt Klärschlamm die Schadstoffsenke in der Abwasserreinigung dar, was den direkten landwirtschaftlichen Einsatz dieses Abfalls bedenklich macht. Zwar nahm die Konzentration der umweltrelevanten Schwermetalle in Klärschlämmen in den vergangenen Jahren deutlich ab (Wiechmann, Dienemann et al. 2012), die Belastung mit organischen Schadstoffen (z.B. Pharmazeutika, endokrin wirksame Substanzen, persistente organische Stoffe etc.) ist jedoch unüberschaubar und dürfte sich einem sinnvollen „Monitoring“ weitgehend entziehen. Das daraus resultierende Risiko für Mensch und Umwelt ist schwer einschätzbar und wird aufgrund der Beschaffenheit der diffusen Schadstoffquellen (z.B. Eintrag von Pharmaka und deren Metabolite über menschliche Ausscheidungen) unkalkulierbar bleiben.
In Deutschland werden gegenwärtig etwa 53 % der kommunalen Klärschlämme in Mono- und Müllverbrennungsanlagen sowie Kraft- und Zementwerken thermisch und 47 % stofflich, d.h. landwirtschaftlich (30 %) oder in landschaftsbaulichen Maßnahmen u.ä. verwertet (17 %). Bezogen auf die etwa 9,4 Mrd Kubikmeter Abwasser, die pro Jahr in Deutschland anfallen, kann von einem Potenzial von 75000 t Phosphor/a (davon ca. 67500 t P/a im Klärschlamm) ausgegangen werden. Bislang werden in der Literatur ca. 37 Verfahren zur abwasserseitigen Rückgewinnung von Phosphor beschrieben, die im Labor, im Technikumsmaßstab oder in Pilotanlagen erprobt worden sind. Weltweit wurden bisher ca. 12 davon großtechnisch umgesetzt. Etwa vier verschiedene Verfahrenstechniken lassen sich derzeit in Deutschland finden. Einige Verfahren arbeiten mit Ionenaustauschern, zum überwiegenden Teil handelt es sich jedoch um Fällungs- oder Kristallisationsverfahren, bei denen Magnesium-Ammonium-Phosphat (MAP, Struvit) entweder aus den Haupt- oder Nebenströmen einer Kläranlage oder aus dem Schlamm bzw. Schlammwasser gewonnen wird. Für den Nährstoff Phosphor konnte in den Klärschlammaschen ein Gehalt von durchschnittlich 7 % ermittelt werden. Daraus ergibt sich ein Potenzial von etwa 17500 t P/a (Tendenz steigend). Je nach Verfahren kann mit einem Rückgewinnungspotenzial von etwa 60 bis 90 % Phosphor aus der Asche (ca. 55 bis 80 % Pges bezogen auf den Kläranlagenzulauf) gerechnet werden
Sewage sludge ashes (SSA) contain considerable mass fractions of phosphorus (5-10 w-% P) suitable for fertiliser production. Unfortunately, also most of the heavy metals remain in the ashes. A thermochemical process was developed for the treatment of SSA to i) remove heavy metals and ii) transform phosphates into bio-available mineral phases. The technology was already demonstrated in technical scale (capacity of 300 kg/h) and the company OUTOTEC is currently planning the first industrial plant. In order to manufacture a marketable multi-nutrient fertiliser from the thermochemically treated SSA further wastes and industrial by-products were taken into account. Ammonium sulphate occurs as a by-product of the caprolactam production and was chosen as N-carrier (21 w-% N). Straw ash was tested as potassium carrier (11-15 w-% K). Granulation campaigns were carried out with intensive mixers in lab-, medium-and technical scale. NPS-and NPKS-fertilisers were produced that were characterised by suitable particle size distributions and strength.
Sewage sludge ashes (SSA) represent a possible source of phosphorus (P) and technology metals. So far, the sole external source for P, that is indispensable for all animate beings, is rock phosphate, a finite resource. The EU depends completely on the import from possible politically instable regions. Furthermore, rock phosphate is often contaminated with heavy metals like Cd and U, leading to health and environmental hazards. P recovered from SSA might diminish these problems. SSA of German mono incineration facilities are analyzed for their elemental composition. More than 95% of the emerging SSA is monitored, enabling the determination of complete mass flows of the ashes and their components. Initial results indicate a P recovery potential of 16,000 t/a (11% of the annual P demands for fertilizer production). The concentrations of Cd and U in SSA are one to two Orders of magnitude lower than in rock phosphate and could help to reduce possible hazards.
Säulenperkolationsversuche werden u.a. zur Ermittlung der Freisetzung von Schadstoffen aus Böden durchgeführt. Im Entwurf der novellierten Bundesboden-schutz- und Altlastenverordnung ist neben Schüttelverfahren (DIN 19527 und 19529) ein Säulenperkolationsverfahren (DIN 19528) zur Eluatgewinnung aus Böden festgeschrieben. Mit diesem Verfahren kann im Vergleich zu den Schüttelversuchen auch der zeitliche Verlauf der Schadstofffreisetzung erfasst und bewertet werden. Allerdings sind die Verfahren bisher nur für anorganische Stoffe und wenige prioritäre organische Schadstoffe validiert worden (PAK, MKW, PCB, Phenole).
Aber auch Schadstoffe wie perfluorierte Tenside (PFT), die z.B. für die Veredlung von Papier, Textilien und Haushaltsgeräten eingesetzt werden oder Biozide, mit denen Bauprodukte zum Schutz vor mikrobiellem Befall ausgerüstet werden (z.B. Fassadenbeschichtungen und Holz), geraten auf Grund ihrer gesundheits- und umwelt-schädlichen Eigenschaften immer stärker in die Diskussion.
Scrap tyres are widely reused in the form of granules as infill materials or component of sub-base layers in construction of sporting grounds such as synthetic turf areas and athletic track surfaces. The recycled rubber may contain organic and inorganic pollutants due to the presence of vulcanisation catalysts, stabilisers and other additives which can be released into soil and groundwater in the case of outdoor sports facilities. In order to evaluate the amount of potentially mobile pollutants, leaching tests can be employed. This study aimed particularly at the investigation of the feasibility of column tests using complete synthetic surface flooring or turf system assemblies. The release of zinc and polycyclic aromatic hydrocarbons (PAH) leached from components of sports surfaces containing recycled rubber granules was considered. Additionally, batch tests on coated and uncoated styrene butadiene rubber (SBR) granules aged by artificial weathering were performed to indicate its possible influence on the leaching behaviour of zinc and PAH. The chosen approach of column tests simulating typical complete synthetic sports surface installations has been proven to be feasible and robust. The time-dependent leaching behaviour and interactions between single components can be evaluated by column tests. Zinc was the most relevant contaminant in the eluates and its leachability was enhanced after accelerated ageing by artificial weathering. Leachable PAH were found in relatively low but well detectable amounts which increase by ageing as well.
Für die vom Bundesumweltministerium vorgesehene Mantelverordnung sind validierte Unter-suchungsmethoden erforderlich. Dazu gehört auch die Herstellung von wässrigen Eluaten, z.B. zur Beurteilung der Mobilität von Schadstoffen und der Ableitung von Grenzwerten.
Ziel des Vorhabens war es, auf der Grundlage geeigneter Testmaterialien (mit prioritären organischen Schadstoffen kontaminierte Böden und Bodenmaterialien) Ringversuche zur Validierung des Schüttelverfahrens nach E DIN 19527 und des Säulenverfahrens für die Übereinstimmungs-untersuchung nach DIN 19528 durchzuführen. Auf der Grundlage der Untersuchungsergebnisse sollten beide Normen bezüglich der Vorgehensweise präzisiert werden und es sollten die während des Ringversuchs ermittelten Verfahrenskenndatenn zur Validierung der Normen herangezogen werden. Darüber hinaus sollten Säulen- und Schüttelverfahren als Übereinstimmungstest vergleichend bewertet werden.
Es wurden vier geeignete Ringversuchsmaterialien hergestellt und an insgesamt 18 Ringversuchsteilnehmer ausgegeben. Die Auswertung der Ringversuche erfolgte auf der Grundlage klassischer Statistik nach DIN ISO 5725 mit Hilfe der AuswertesoftwareProLab 2011 (quo data).
Auf der Grundlage der Validierungsringversuche wurden die Verfahrenskenndaten für die Norm DIN 19527 ermittelt. Die statistische Auswertung der eingereichten Datensätze war aufgrund der großen Streubreite der Daten schwierig. Die vorgeschriebenen statistischen Methoden zur Datenauswertung adressieren die Behandlung nicht gleichverteilter Datensätze nur ungenügend. Das muss bei der Bewertung der Ergebnisse und deren Zuverlässigkeit berücksichtigt werden.
Generell kann festgestellt werden, dass keine signifikanten Unterschiede zwischen den Ergebnissen der Schüttel- und Säulenelution beobachtet werden. Dabei werden beim Schüttelverfahren tendenziell etwas geringere Gesamtmittelwerte erzielt als beim Säulenverfahren, die berechneten Vergleichsvariationskoeffizienten sind für das Schüttelverfahren meist etwas niedriger. Dennoch erweisen sich beide Elutionsverfahren bei den eingesetzten Ringversuchsmaterialien als gut vergleichbar.
Phosphor ist ein für alle Lebewesen essentielles Element und in seinen Funktionen nicht zu ersetzen. Der Bedarf wird aus der Nahrung gedeckt, daher wird Phosphor letztendlich durch Ackerbau den Böden entzogen. Der Nährstoff muss ersetzt werden, um dauerhafte Landwirtschaft zu ermöglichen. Das geschieht zum einen durch den Einsatz von Wirtschaftsdüngern, aber zu einem großen Teil auch durch Mineraldünger. Das hierfür benötigte Rohphosphat wird bergmännisch aus fossilen Lagerstätten gewonnen. Die entsprechende Reichweite wird auf über 300 Jahre geschätzt. Daher besteht zwar keine unmittelbare Gefahr, dass dieser lebenswichtige Nährstoff zu Neige geht, es bestehen jedoch erhebliche Versorgungsrisiken. Zum einen ist Europa nahezu vollständig von Importen abhängig und damit auch Schwankungen der Weltmarktpreise ausgesetzt. Darüber hinaus liegen Förderung und Reserven von Rohphosphaten entweder in Ländern mit hohem Eigenbedarf (USA, China) oder in politisch instabilen Regionen (Marokko, West Sahara). Außerdem sind viele Rohphosphate mit Schwermetallen wie Uran, Thorium und Cadmium belastet. Das Umweltbundesamt schätzt, dass jährlich mehr als 160 t Uran durch Mineraldünger auf deutsche Ackerflächen ausgebracht werden. Rückgewinnung von Phosphor könnte helfen, diese Probleme zu reduzieren. Ein bedeutendes Potential dafür stellt der Abwasserstrom dar. Die Menge an Phosphor darin wird deutschlandweit auf etwa 70.000 t jährlich geschätzt. Das entspricht etwa der Hälfte der Menge an Phosphor, die derzeit für Mineraldünger benötigt wird. Der Vortrag würde sich mit möglichen Prozessen der Rückgewinnung, deren Wirtschaftlichkeit und Herausforderungen der Analytik befassen:
- in den letzten Jahren wurden zahlreiche Verfahren zur Rückgewinnung von Phosphor aus verschiedensten Phasen der Abwasserreinigung entwickelt (wässrige Phase, Klärschlamm, Klärschlammasche). Ausgewählte Verfahren würden vorgestellt und bewertet.
- für einen Einsatz der so gewonnenen Recyclingphosphate als Düngemittel muss die Schadstofffreiheit und Pflanzenverfügbarkeit der Nährstoffe sichergestellt werden. Dazu ist zu prüfen, ob die zurzeit gängigen Verfahren der Probenvorbereitung und Analytik auch auf Recyclingphosphate anwendbar sind. Das gilt neben der Bioverfügbarkeit von Phosphor besonders für Schadstoffe, da die Recyclingdünger aus Abfallmaterialien gewonnen werden, die stark belastet sein können. Das gilt besonders für die speziesspezifische Analytik von Chrom (Chrom (VI) vs. Chrom (III)) in verschiedenen Matrices.
The annual demand of phosphorus (P) for fertilizer use is more than 550,000 t in Germany. Several of the input streams like mineral fertilizer produced from phosphate rock or sewage sludge are problematic due to contamination with heavy metals and organic pollutants and/or supply risks. Phosphorus recovery from the wastewater stream might help to diminish these problems. Several procedures have been developed to recover P from either sewage sludge ash (SSA) or wastewater via precipitation or crystallization as struvite. This study determined the elemental composition and trace metal mass fractions of 252 SSA samples and 17 struvite samples from wastewater treatment plants (WWTP) to see whether there are differences related to the source of the sludge (municipal/industrial) or the stage of the WWTP where the struvite is produced. Results indicated that there is no clear trend of the elemental mass fractions related to the source of the sludge. All struvite samples show very low heavy metal contents, even though the struvite precipitated from the sludge shows slightly elevated heavy metal mass fractions compared to struvite crystallized from sludge liquor. Struvite is a clean and plant available material for fertilizer production from wastewater streams and has some advantages for the wastewater treatment plant. However, since the P recovery rate of struvite processes is low (7–11%) compared to that from SSA processes (90%), recovery from SSA is necessary for a substantial P recovery from the wastewater stream.
Polycyclic aromatic hydrocarbons (PAH) are severe environmental pollutants that are analyzed frequently. The risk assessment of PAH impact to groundwater can be performed using leaching tests. Therby a liquidsolid separation step including centrifugation may be required, which in turn might lead to loss of analytes due to sorption on the equipment. Thus we determined the PAH recoveries from various container materials (polyethylene (PE), polypropylene (PP), polytetraflourethylene (PTFE), stainless steel (ES), and perflouroalkoxy (PFA)) and compared them to selected PAH properties. We found the best recoveries for PFA (68%) and PTFE (65%) containers. We found good negative correlations (-0.93 and better) between PAH recovery and log partition coefficient organic carbonwater (log KOC) for PFA, PTFE, and ES containers.
There is a growing concern of the direct use of contaminated sewage sludge in agriculture due possible environmental and health hazards. Thus, incineration of the sludge and thus increasing amounts of sewage sludge ashes (SSA) are to be expected in the future. SSA contains considerable amounts of phosphorus (P) and technology metals that might be recovered as secondary raw materials. Since the EU for instance depends completely on the import of rock phosphate needed for fertilizer production, alternative sources for P are in order. Furthermore, rock phosphate is often contaminated with heavy metals like Cd and U, leading to health and environmental hazards. P recovered from SSA might diminish these problems. To determine the possible recovery potential of P and technology metals from SSA, we conducted a survey of German mono incineration facilities and analyzed the respective SSA for their elemental composition. More than 95% of the emerging SSA was monitored. Results indicate a P recovery potential of 18,000 t/a (up to 13% of the annual P demands for fertilizer production). The concentrations of Cd and U in SSA are one to two Orders of magnitude lower than in rock phosphate and could help to reduce possible hazards.
Stir bar sorptive extraction (SBSE) is an equilibrium extraction method used amongst others for the analysis of polycyclic aromatic hydrocarbons (PAH) in aqueous samples. We compared SBSE to liquid–liquid extraction (LLE) for aqueous eluates obtained from batch and column tests of PAH contaminated soils to check whether SBSE might be considered as an alternative sample preparation method. We used soils with different particle size distribution, organic matter content, and resulting eluate turbidity to test the sample preparation methods on eluates with matrices of varying complexity. Furthermore, we studied the influence of diluted organic matter (DOM) on the PAH sorption process to the polymer coating of the stir bar during SBSE. In the majority of cases, we found higher PAH concentrations (up to 288%) with SBSE than with LLE. The turbidity correlates with the difference in PAH results, i.e. the greater the turbidity in the eluate, the more PAH we found with SBSE compared to LLE. We observed no similar trend regarding the amount of total organic carbon (TOC). The presence of DOM in the eluate seems to hamper the SBSE slightly, the PAH recovery varied between 82 and 104%.
Recovery of rare earth elements - optimized elemental analysis of fluorescent lamp shredder waste
(2016)
Rare earth elements (REE) are a crucial component of fluorescence lamps. Several procedures have been developed to recovery these technological important elements. Nevertheless, actual REE recycling from fluorescence lamps is scarce so far (recovery rate of less than 1 %), with current recycling approaches concentrating on glass recovery. Since most recycling processes include several, also wet-chemical steps, a complete knowledge of the actual elemental composition of the respective mass flows is necessary for an efficient REE recovery. We tested seven different reagent mixtures for microwave-assisted digestion of fluorescent lamp shredder, including HF, HClO4, and H2O2. We determined the concentrations of 25 of the most relevant rare earth and other trace elements in the respective dilutions. Two independent digestions, one a mixture of perchlorid/nitric/hydrofluoric acid and the other aqua regia, showed the highest concentrations of 23 of these elements, excluding only Sn and Tb. The REE concentrations in the tested lamp shredder sample (stated in g/kg) were 10.2 (Y), 12.1 (La), 7.77 (Ce), 6.91 (Eu), 1.90 (Gd), and 4.11 (Tb).
Recovery of rare earth elements - optimized elemental analysis of fluorescent lamp shredder waste
(2016)
Rare earth elements (REE) are a crucial component of fluorescence lamps. Several procedures have been developed to recovery these technological important elements. Nevertheless, actual REE recycling from fluorescence lamps is scarce so far (recovery rate of less than 1 %), with current recycling approaches concentrating on glass recovery. Since most recycling processes include several, also wet-chemical steps, a complete knowledge of the actual elemental composition of the respective mass flows is necessary for an efficient REE recovery. We tested seven different reagent mixtures for microwave-assisted digestion of fluorescent lamp shredder, including HF, HClO4, and H2O2. We determined the concentrations of 25 of the most relevant rare earth and other trace elements in the respective dilutions. Two independent digestions, one a mixture of perchlorid/nitric/hydrofluoric acid and the other aqua regia, showed the highest concentrations of 23 of these elements, excluding only Sn and Tb. The REE concentrations in the tested lamp shredder sample (stated in g/kg) were 10.2 (Y), 12.1 (La), 7.77 (Ce), 6.91 (Eu), 1.90 (Gd), and 4.11 (Tb).
Phosphorus is essential for all animate beings and not replaceable in its functions. Recovered phosphorus from secondary sources is expected gain importance in the future due to supply risks and environmental concerns regarding fossil phosphate rock, the single source of phosphorus so far. Existing regulations, standards, and analytical methods are basically configured for well-established organic and mineral fertilizer but not for the emerging recycling products. Consequently, the respective procedures have to be adapted, especially in terms of matrix effects and so far not regulated pollutants like uranium and emerging pollutants of concern.
Die europäische Kommission (Generaldirektion Unternehmen und Industrie) hat kürzlich die Auswirkungen einer harmonisierten europäischen Düngemittelverordnung, einschließlich der technischen Durchführbarkeit und den umweltbezogenen, wirtschaftlichen und sozialen Auswirkungen einer solchen Gesetzgebung untersuchen lassen. Basierend auf diesen Ergebnissen soll nun die EU-Düngemittelverordnung (EG) 2003/2003 revidiert werden. Neben der Vielzahl von bestehenden und neuen Düngemitteltypen wie z.B. Phosphor-Recyclingdüngern soll die neue Verordnung auch organische Düngemittel und somit Matrices wie Klärschlamm, Gärrückstände und Wirtschaftsdünger regeln. Dies bedeutet, dass Parameter und Grenzwerte, die bisher in verschiedenen Verordnungen für verschiedene Matrices geregelt wurden, künftig gemeinschaftlich geregelt werden (Klärschlamm, Düngemittel) und weitere Matrices zusätzlich geregelt werden müssen (Phosphor-Recycling-Produkte, Produkte aus Klärschlamm/-aschen).
Resultierend aus den aktuellen nationalen Entwicklungen insbesondere bezüglich des Ausstiegs aus der landwirtschaftlichen Klärschlammverwertung und im Hinblick auf die Bestrebungen hinsichtlich der Schonung natürlicher Ressourcen (z.B. ProgRess) ist zu erwarten, dass die Anzahl an Düngemitteln, die aus Recyclingmaterialien gewonnen werden, stark zunehmen wird. Recyclingdünger aus dem Stoffstrom Klärschlamm- bzw. Klärschlammasche werden zukünftig einen großen Anteil an diesen neuen Produkten ausmachen.
Vor den angeführten Hintergründen ist es notwendig relevante und insbesondere bereits genormte Verfahren hinsichtlich ihrer Anwendbarkeit auf z.B. Klärschlamm/-aschen und daraus gewonnenen Recycling-Düngern sowie auf kommerzielle P-Düngemittel zu prüfen.
Vor diesem Hintergrund wurde die BAM (FB 4.4) vom UBA mit einer Untersuchung beauftragt:
UFOPLAN FKZ: 3714263200
„Untersuchung der Anwendbarkeit der im Rahmen des CEN-Projekts HORIZONTAL entwickelten Analyseverfahren auf Düngemittel und Klärschlamm/ -aschen“
Laufzeit: 01.07.2014 – 31.01.2017
Phosphorus (P) is essential for all forms of life and cannot be substituted. It is one of the macro nutrients applied in form of mineral or organic fertilizers in agricultural crop production. Mineral P fertilizers are generally based on phosphate rock, a limited resource. Western Europe completely depends on imports as it has no own relevant phosphate mines. The most abundant phosphate deposits are located only in a few countries such as Morocco, China, South Africa and the United States of America. Furthermore, phosphate rock and as a consequence mineral P fertilizers are often contaminated with the toxic elements cadmium and uranium. In Order to substitute phosphate rock P-bearing waste streams are investigated for their potential to be recyded as fertilizers. Wastewater is one of the important P-bearing waste streams that were in the focus of research in the last 10 years. German wastewater is e.g. a carrier of approx. 70,000 t of phosphorus per year.
Phosphorus (P) for fertilizer use can be recovered from sewage sludge ash (SSA). To enhance the bioavailability of P and reduce the heavy metal content of SSA, it can be treated thermochemically with Na2CO3 or Na2SO4 at 950 °C in a rotary kiln using dry sewage sludge or lignite as reducing agent. These processes were investigated by thermogravimetry/differential thermal analysis coupled with gas analysis. Reducing conditions in this experimental setup were provided by 2 % hydrogen in the Ar carrier gas. During SSA + Na2CO3 treatment CO2, CO and water were detected in the off-gas. During SSA + Na2SO4 treatment SO2, some CO2 and water were detected. Heavy metal removal was more efficient for SSA + Na2CO3 compared to the sulfate variant. A SSA + Na2SO4 + lignite variant which also formed CO shifted the heavy metal removal to the results obtained with Na2CO3 which was obviously due to the additional reduction potential. However, Zn evaporation was not achieved with the Na2SO4 variants which were most probably due to immobilization as ZnS.
Klärschlammaschen weisen hohe Gehalte an Phosphor auf, dieser ist allerdings schlecht für Pflanzen verfügbar. Des Weiteren enthalten sie Schwermetalle die vor dem Einsatz als Düngemittel entfernt werden müssen. Vor diesem Hintergrund wurden in den letzten Jahren nasschemische und thermochemische Verfahren entwickelt und zum Teil bereits in Demonstrationsanlagen getestet. Ein thermochemischer Verfahrensansatz wird in diesem Beitrag näher vorgestellt. Klärschlammaschen werden mit Klärschlamm als Reduktionsmittel und Natriumsulfat als Aufschlussmittel im Drehrohrofen thermisch behandelt. Bei diesem Prozess wird pflanzenverfügbares NaCaPÜ4 gebildet, unerwünschte Elemente wie As, Cd, Hg und Pb werden zum Teil über die Gasphase separiert. Die Ergebnisse eines Demonstrationsversuchs werden vorgestellt.
Phosphorous is essential for all living creatures and indispensable in its functions regarding bone structure, energy metabolism, and storage and expression of genetic information. It is removed from the soils through farming and husbandry and has to be replaced. Annually, more than 17 million tons of phosphorous are applied to soils in the form of mineral fertilizer worldwide (Killiches, 2013). In Germany, this accounts for 150,000 t/a. This fertilizer is produced from rock phosphate, which is often contaminated with heavy metals (Dissanayake et al., 2009), especially cadmium and uranium. Cd concentrations are around 30 mg/kg, U around 100 mg/kg, with even higher peak values. Since rock phosphate is treated with acids to make the phosphorous bioavailable, those heavy metals were also mobilized. When the fertilizer is applied to the farmland, the contaminants can pollute the soil and pose an environmental risk. Sewage sludge is another phosphorous source for farming. In Germany, 15,000 t/a phosphorous are applied to farmlands this way. However, there is a growing concern of possible environmental hazards since sewage sludge contains not only inorganic contaminants but also organic pollutants, especially pharmaceuticals and personal care products (Guardia et al., 2004).
Phosphorus fertilizer from sewage sludge ashes by thermochemical treatment - Benefits and challenges
(2015)
Mineral phosphorus (P) fertilizers are solely produced from phosphate rock. Europe completely depends on imports since there are no relevant phosphate rock deposits on the continent. Furthermore, phosphate rock is contaminated with heavy metals such as Cd and U that pollute the farmlands and pose environmental risks. Sewage sludge ash (SSA) might be a promising source for recycling fertilizer since it contains large amounts of P (up to 13 %). However, fertilizer from SSA has to comply with the respective ordinances, particularly the heavy metal limit values stated in the fertilizer ordinance, and requires sufficient P bioavailability. Thus, we conducted a complete survey of SSA from German mono-incineration facilities and developed a thermochemical treatment for SSA to reduce toxic elements and increase P bioavailability.
Sewage sludge incineration is extensively practiced in some European countries such as the Netherlands, Switzerland, Austria and Germany. A survey of German sewage sludge ash showed that the recovery potential is high, approx. 19,000 t of phosphorus per year. However, the survey also discovered that the bioavailability of phosphorus in the sewage sludge ash is poor and that more than half of the ashes cannot be used as fertilizers due to high heavy metal content. A new thermochemical process for sewage sludge ash treatment was developed that transforms the ash into marketable fertilizer products. Sewage sludge ash was thermochemically treated with sodium and potassium additives under reducing conditions, whereby the phosphate-bearing mineral phases were transformed into plant available phosphates. High P-bioavailability was achieved with a molar Na/P ratio > 1.75 in the starting materials. Sodium sulfate, carbonate and hydroxide performed comparably as additives for this calcination process. Potassium carbonate and -hydroxide have to be added in a molar K/P ratio > 2.5 to achieve comparable P-solubility. The findings of the laboratory scale investigations were confirmed by an industrial demonstration trial for an ash treatment with sodium sulfate. Simultaneously, the volatile transition metal arsenic (61% removal) as well as volatile heavy metals such as cadmium (80%), mercury (68%), lead (39%) and zinc (9%) were removed via the off-gas treatment system. The product of the demonstration trial is characterized by high bioavailability and a toxic trace element mass fraction below the limit values of the German fertilizer ordinance, thus fulfilling the quality parameters for a P-fertilizer.
Incineration of sewage sludge is expected to increase in the future due to growing concerns about the direct use of sludge in agriculture. Sewage sludge is the pollutant sink of wastewater treatment and thus loaded with contaminants that might pose environmental hazards. Incineration degrades organic pollutants efficiently, but since the ash is currently mostly disposed of, all valuable component like phosphorus (P) and technologically relevant metals present in the sewage sludge ash (SSA) are removed from the economic cycle entirely. We conducted a complete survey of SSA from German mono-incineration facilities and determined the theoretical recovery potential of 57 elements. German SSA contains up to 19,000 t/a P which equals approximately 13% of phosphorus applied in the German agriculture in form of phosphate rock based mineral fertilizers. Thus, SSA is an important secondary resource of P. However, its P-solubility in ammonium citrate solution, an indicator for the bioavailability, is only about 26%. Treatment of SSA is recommended to enhance P bioavailability and remove heavy metals before it is applied as fertilizer. The recovery potential for technologically relevant metals is generally low, but some of these elements might be recovered efficiently in the course of P recovery exploiting synergies.
The number of different secondary raw materials used for fertilizer production is expected to increase in the future due to newly developed recycling procedures. Thus, more and more different matrices have to be analyzed. Furthermore, the respective legislation and analytical methodology is nonuniform throughout Europe. Therefore, a harmonization of the the regulations and Standards is desirable. We conduct a research project to test the existing analytical methods on their applicability to a broad variety of matrices to support the harmonization process. The project is scheduled tili late spring 2017. Initial results will be presented.
The amount of sewage sludge produced worldwide is expected to further increase due to rising efforts in wastewater treatment. There is a growing concern against its direct use as fertilizer due to contamination of the sludge with heavy metals and organic pollutants. Incinerating the sludge degrades organic compounds almost completely and concentrates heavy metals and phosphorus. However, the sewage sludge ash (SSA) is almost completely disposed of and with it all resources are removed from the economic cycle. Comprehensive knowledge of the composition of SSA is crucial to assess the resource recovery potentials. We conducted a survey of all SSA emerging in Germany and determined the respective mass fractions of 57 elements over a period of one year. The median content of phosphorus was 7.9%, indicating an important recovery potential. Important trace elements were Zn (2.5 g/kg), Mn (1.3 g/kg), and Cu (0.9 g/kg). Mass fractions of technology metals such as V, Cr, Ga, Nb, and rare earths were comparatively low. Considering the possible use of SSA as secondary raw material for fertilizer production it should be noted that its Cd and U content (2.7 mg/kg and 4.9 mg/kg respectively) is significantly lower than that of rock phosphate based mineral fertilizers.
Monitoring of PAH in aqueous samples - a comparison of different sample preparation techniques
(2011)
This study compares the mercury distribution in the vapor phase, the phosphor powder and the glass matrix of new and spent fluorescent lamps. The spent fluorescent lamps were obtained at the collection yards of a public waste management company in Hamburg, Germany. An innovative systematic sampling method is utilized to collect six spent and eight corresponding new, off-the-shelf fluorescent lamp samples. The efficiency of several acid digestion methods for the determination of the elemental composition was studied and elemental mass fractions of K, Na, Y, Ca, Ba, Eu, Al, Pb, Mg, Hg, and P were measured. The study also finds aqua regia to be the best reagent for acid digestion. However, no significant difference in mercury distribution was found in the different phases of the new and spent fluorescent lamps.
Wastewater contains a diverse array of organic and inorganic compounds and its complex composition strongly depends on the location and the connected dischargers. However, municipal wastewater as a carrier of feces and urine generally contains considerable amounts of the main nutrients nitrogen and phosphorus. The latter is in the focus of the discussions about the recovery potential of wastewater due to the relatively high mass flows of phosphorus in wastewater and the finite nature and decreasing quality of phosphate rock reserves. But due to the presence of the whole periodic table of elements, wastewater might contain further valuable components of interest for recovery including those defined as critical raw materials by the European Commission. Phosphorus and most of the other critical raw materials are fixed in the sewage sludge and after incineration in the sewage sludge ash (SSA). This is accompanied by high concentration factors from wastewater via sludge to ash. However, the mass fractions of the majority of elements in sewage sludge are comparable to those of the earth crust, indicating no relative enrichment. Nevertheless, enrichment factors of 100 or higher are given for phosphorus, copper, zinc, cadmium, silver, tin, lead and the platinum group elements indicating an anthropogenic input. An economic value of sewage sludge was estimated to $460,-/t calculated on the basis of the respective market prices for high purity elements – a theoretical value. A German survey of sewage sludge ashes showed that the mass fractions and the mass flows of most of the elements present in SSA are probably too low for an economic recovery. In most cases the mass flows are rather small compared to the imports and the chemical forms are not suitable for recovery. An exception is phosphorus that is present in high mass fractions up to 13% and that bears a high substitution potential. If the application of P-recovery technologies lead to a further concentration of valuable elements e.g. as by-products in side streams of the process, it would probably make also the recovery of other elements of economic interest.
Phosphorus-fertilizers from secondary resources such as sewage sludge ash (SSA) will become more important in the future as they could substitute conventional fertilizers based on the nonrenewable resource phosphate rock. Thermochemical approaches were developed which remove heavy metals from SSA prior to its fertilizer application on farmlands. We analyzed the chemical state of mercury and selenium in SSA before and after thermochemical treatment under different conditions for P-fertilizer production by X-ray absorption near edge structure (XANES) spectroscopy. In some incineration plants the mercury loaded carbon adsorber from off-gas cleaning was collected together with the SSA for waste disposal. SSAs from those plants contained mercury mainly bound to carbon/organic material. The other SSAs contained inorganic mercury compounds which are most probably stabilized in the SSA matrix and were thus not evaporated during incineration. During thermochemical treatment, carbon-bound mercury was removed quantitatively. In contrast, a certain immobile fraction of inorganic mercury compounds remained in thermochemically treated SSA, which were not clearly identified. HgSe might be one of the inorganic compounds, which is supported by results of Se K-edge XANES spectroscopy. Furthermore, the chemical state of selenium in the SSAs was very sensitive to the conditions of the thermochemical treatment.
- Spurenelementanalytik aus Fluoreszenzlampen optimiert
- Königswasseraufschluss Methode der Wahl für REE
- Perchlorsäure-/Flusssäureaufschluss in Kombination mit Königswasseraufschluss für die meisten Elemente geeignet
- Teilweise starke Abhängigkeit der Aufschlusseffizienz vom Element bzw. der vorliegenden Elementspezies
- Nicht aufgelöste Glasmatrix stört die Analytik nicht
The risk assessment of total petrol hydrocarbons (TPH) and polycyclic aromatic hydrocarbons (PAH), two of the most frequent soil and water contaminants, has to include their exposure pathways, especially the soil groundwater pathway. Threshold values have to be aquired for the amendment to the German Federal Soil Protection Contaminated Sites Ordinance. For this purpose, a batch experiment with a liquid to solid ratio (L/S) of 2 L/kg was developed. Aim of this work was to verify the robustness of this leaching procedure for TPH and PAH in different soil types against varying test conditions. Also, stir bar sorptive extraction (SBSE) was tested as alternative sample preparation of eluates for PAH analysis.
In Europa fallen jedes Jahr mehr als 10 Millionen Tonnen Klärschlamm an (Trockenmasse), etwa 2 Millionen davon in Deutschland, Bild 1 zeigt die Entwicklung der Klärschlammentsorgung in Deutschland. Nach dem Deponierungsverbot hat die Verbrennung des Klärschlamms stetig zugenommen. Die Verwendung im Landschaftsbau bzw. als Düngemittel ist nach einem Maximum um die Jahrtausendwende herum zugunsten der Verbrennung zurückgegangen, so dass heute jeweils etwa die Hälfte des Klärschlamms verbrannt und in der Landwirtschaft genutzt wird. Der Anteil an verbranntem Klärschlamm wird in Zukunft vermutlich weiter steigen. Ein wesentlicher Grund dafür ist die zunehmende Besorgnis über Schadstoffe im Klärschlamm, die Mensch und Umwelt schädigen könnten. Neben verschiedenen organischen und anorganischen Schadstoffen handelt es sich insbesondere um Emerging Pollutants of Concern (EMPOC) wie Antibiotika und Kosmetika.
Im Rahmen des EU-Projekts P-REX werden unter anderem die zwei thermischen Verfahren ASH DEC und Mephrec zur technischen Rückgewinnung von Phosphor aus Klärschlamm und Klärschlammaschen für die P-Düngemittelproduktion betrachtet. Die Produkte haben geringe Konzentrationen an Schwermetallen und eine bessere P-Löslichkeit als die nicht behandelten Klärschlammaschen. Die Klärschlammasche wird im ASH DEC-Verfahren mit Natriumverbindungen unter reduzierenden Bedingungen im Drehrohrofen behandelt. Das Verfahren wurde erfolgreich bei einem Demonstrationsversuch getestet. Das Mephrec-Verfahren ist ein metallurgisches Schmelzverfahren und wird unter reduzierenden Bedingungen im Schachtofen durchgeführt. Es ist eine Pilotanlage in Nürnberg geplant.
In order to estimating the amount and kind of emissions from polymeric sporting tracks a laboratory test was developed in BAM that combines artificial weathering and subsequent batch and column tests [1, 2, 3]. The goal consisted in nvestigating a possible change of emissions into soil and groundwater of a new sporting ground as a function of ageing and egradation of the system. At various stages of the weathering, the samples were removed and subjected to especially designed column extraction tests for the solid samples. Both these extracts and the accumulated rainwater run-off of the weathering device were subjected to analytical tests of their ingredients. The overall aim of the test consisted in developing ontrollable, reproducible, and standardisable conditions and methods of investigation that would allow an estimation of the emissions in the course of outdoor application of about five years.
Anticancer drugs (ACDs) exhibit high biological activity, they are cytotoxic, genotoxic, and are constantly released into the environment as a result of incomplete metabolism. Consequently they pose a serious threat to the environment and human health due to their carcinogenic,mutagenic and/or reproductive toxicity properties. Knowledge of their bioavailability, including their sorption to soils and their impact on the soil–groundwater pathway, is crucial for their risk assessment. Laboratory batch and column leaching tests are important tools for determining the release potential of contaminants from soil or waste material. Batch and column tests were carried out with soils differing in physicochemical properties, each spiked with cyclophosphamide (CK) or ifosfamide (IF). Moreover, due to the fact that environmental pollutants may occur as coexisting compounds in the soil themobility evaluation for ACDs in the mixture with metoprolol (MET; β-blocker) as a co-contaminant was performed. In order to assess appropriateness, the batch and column tests were compared. The release depended on the properties of both the soil and the presence of co-contaminants. The faster release was observed for coarse-grained soil with the smallest organic matter content (MS soil: 90% decrease in concentration until liquid-to-solid ratio (L/S) of 0.3 L kg−1 for all tests' layout) than for loamy sand (LS soil: 90% decrease in concentration until ratio L/S of 0.75 L kg−1). ACDs are highly mobile in soil systems. Furthermore, the decrease of mobility of ifosfamide was observed with the presence of a co-contaminant (metoprolol) in both of the soils (in MS soil a decrease of 29%; in LS soil a decrease of 26%). The mobility of cyclophosphamide does not depend on the presence of a contaminant for MS soil, but also exhibits a decrease of 21% in LS soil.
Fluorescence lamps contain considerable amounts of rare earth elements (REE). Several recycling procedures for REE recovery from spent lamps have been established. However, despite their economic importance, the respective recycling is scarce so far, with an REE recovery rate of less than 1%. A reliable analysis of REE and other relevant metals like Yttrium is crucial for a thorough and complete recovery process. This applies both to the solid matter and aqueous phase, since most of the recycling processes include wet-chemical steps. We tested seven different reagent mixtures for microwave-assisted digestion of fluorescent lamp shredder, including hydrofluoric acid, perchloric acid, and hydrogen peroxide. We determined the concentrations of 25 of the most relevant rare earth and other trace elements (Al, P, Ti, V, Cr, Fe, Ni, Cu, Ga, Ge, As, Y, Ag, Cd, Sn, Sb, La, Ce, Eu, Gd, Tb, W, Au, Hg, and Pb) in the respective dilutions. Two independent digestions, one a mixture of perchlorid/nitric/hydrofluoric acid and the other aqua regia, showed the highest concentrations of 23 of these elements, excluding only Sn and Tb. The REE concentrations in the tested lamp shredder sample (stated in g/kg) were 10.2 (Y), 12.1 (La), 7.77 (Ce), 6.91 (Eu), 1.90 (Gd), and 4.11 (Tb).
Complete survey of German sewage sludge ashes - phosphorous and technology metal recovery potential
(2014)
Sewage sludge ashes (SSA) are a possible source for recovery of phosphorous (P) and technology metals. Phosphorous is essential for all animate beings. So far, its sole external source is rock phosphate, which is a finite resource. The EU import dependency on P from regions with high domestic demands or political instabilities is almost complete. Furthermore, rock phosphate often contains high amounts of heavy metals like Cd and U that might lead to health and environmetal hazards. P recovered from SSA might diminish these problems. We analyzed SSA from German mono incineration facilities in terms of their elemental composition and respective recovery potential. More than 97% of the emerging SSA is monitored, enabling the determination of complete mass flows of the ashes and their components. Results indicate a P recovery potential of 19,000 t/a (more than 12% of the annual P demands for fertilizer production). The concentrations of Cd and U in SSA are significantly lower than in rock phosphate and thus might help to reduce possible envrionmental and health hazards.
Determination of chromium (VI) in primary and secondary fertilizer and their respective precursors
(2017)
Hexavalent chromium species (Cr(VI)) are often carcinogenic, of high acute toxicity, highly mobile, and thus pose a severe risk to health and environment. Fertilizers usually contain significant amounts of chromium. Therefore, a reliable analysis of chromium and the fraction of Cr(VI) are crucial for safe use of fertilizers. This problem is expected to increase in the future, since more and more recycled fertilizers emerge due to increasing fertilizer demand and respective supply risks. However, existing analytical methods have been developed for conventional fertilizers and have to be tested whether they are suitable for the new materials. Thus, we performed a wet-chemical extraction for Cr(VI) on several matrices as well as respective quality control experiments including spiking with Cr(III) and Cr(VI)compounds. We found the Cr(VI) amounts to be below 2 mg/kg except for a thermally post-treated sewage sludge ash (SSA) that showed 12.3 mg/kg. The presence of organic matter e.g. in sludge or precipitated struvite caused a reduction of spiked Cr(VI) and thus no satisfying recovery for Quality control. Cr(VI) reduction was also observed for SSA, presumably due to the presence of Fe(II) compounds.
Even though the tested procedure can be hampered in some recycled fertilizer matrices, it might be adapted to be applicable also for these complex samples.
The importance of secondary raw materials for phosphorus (P) fertilizer production is expected to increase in the future due to resource depletion, supply risks, and heavy metal contamination of fossil phosphate resources. Municipal wastewater is a promising source for P recovery. In Germany for instance, it contains almost 50% of the total amount of P that is currently applied as mineral fertilizer. Several procedures have been developed to recover and re-use P resulting in a growing number of recycling fertilizers that are currently not regulated in terms of fertilizer efficiency. We tested various materials and matrices for their total P content, solubility of P in neutral ammonium citrate (Pnac) and water, and performed robustness tests to check if existing analytical methods are suitable for those new materials. Digestion with inverse aqua regia was best suited to determine the total P content. Pnac sample preparation and analyses were feasible for all matrices. However, we found significant time and temperature dependencies, especially for materials containing organic matter. Furthermore, several materials didn’t reach equilibrium during the extractions. Thus, strict compliance of the test conditions is strongly recommended to achieve comparable results.
Leaching experiments on the release of heavy metals and PAH from C&D waste and MSWI bottom ash
(2010)
Leaching tests are fundamental tools for the assessment of long-term impact of
contaminated waste materials on the soil-groundwater pathway. Waste materials should be
tested under conditions equal to their actual application in re-use scenarios to achieve reliable
results. Since the standards for leaching procedures available on international level so far are
either not validated or considered inadequate in respect to coarse grained materials, new
standards had to be developed. Therefore column percolation and batch test procedures have
been standardized and validated to enable their introduction to new German regulations
concerning waste management. Practical aspects of the test procedures as well as the
boundary conditions compared to the already existing standards will be described. Examples
including round robin test results will be given to justify the selection of the new
specifications.