TY - JOUR A1 - Becker, Roland A1 - Dorgerloh, Ute A1 - Theißen, H. A1 - Nehls, Irene T1 - Stabilisation of groundwater samples for the quantification of organic trace pollutants N2 - The concentration of contaminants in groundwater samples can be decreased by degradation in the time course between field sampling and quantification in the laboratory, especially in samples from sites where degradation activity is enhanced by remediation measures. The sampling sites covered a variety of priority organic pollutants such as volatile aromatic and chlorinated compounds, phenols and petroleum hydrocarbons and different remediation strategies such as anaerobic and aerobic microbial in situ degradation, in situ chemical oxidation, and on-site purification with biological treatment. The stability of the contaminants' concentration was investigated over a time range of several hours without cooling in the autosampler of the analytical equipment (short term) and over several days of storage until analysis (long term). A number of stabilisation techniques suggested in international standards ISO 5667-3:2013 and ASTM D6517:2000 were compared both with regard to short term and long term stabilisation of the contaminants and their practicability for field sampling campaigns. Long term storage turned out to be problematic for most compound groups even under cooling. Short term stability was problematic also for volatiles such as benzenic aromates, naphthalene and volatile organic halogenated compounds to be analysed by headspace gas chromatography. Acidification (pH <2) was sufficient to prevent degradation of benzenic aromates, naphthalene, phenols and petrol hydrocarbons for up to seven days. The use of acids was not applicable to stabilise volatiles in waters rich in carbonates and sulphides due to stripping of the volatiles with the liberated gases. The addition of sodium azide was successfully used for stabilisation of volatile organic halogenated compounds. KW - Groundwater KW - Sampling KW - Organic pollutants KW - Stabilisation KW - Analysis PY - 2013 DO - https://doi.org/10.1039/c3em00332a SN - 2050-7887 SN - 2050-7895 VL - 15 IS - 12 SP - 2329 EP - 2337 PB - RSC Publ. CY - CambridgeRSC Publ. AN - OPUS4-29689 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nehls, Irene A1 - Hanebeck, Olaf A1 - Becker, Roland A1 - Emmerling, Franziska T1 - N-(beta-carboxyethyl)-alpha-isoleucine N2 - The title compound, {2-[(2-carbamoylethyl)amino]-3-methylpentanoic acid}, C9H18N2O3, is of interest with respect to its biological activity. It was formed during an addition reaction between acrylamide and the amino acid isoleucine. The crystal structure is a three-dimensional network built up by intermolecular N–H···O and O–H···N hydrogen bonds. KW - Acrylamid KW - Isoleucin KW - Derivatisierung PY - 2013 DO - https://doi.org/10.1107/S160053681205146X SN - 1600-5368 VL - 69 IS - Part 2 SP - o172-o173, sup-1 - sup-7 PB - Munksgaard CY - Copenhagen AN - OPUS4-27573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mönch, Bettina A1 - Emmerling, Franziska A1 - Kraus, Werner A1 - Becker, Roland A1 - Nehls, Irene T1 - n-Propyl 2,3,4,6-tetra-O-acetyl-beta-D-glucopyranoside N2 - The title compound [systematic name: (2R,3R,4S,5R,6R) 2-(acetoxymethyl)-6-propoxytetrahydro-2H-pyran-3,4,5-triyl triacetate], C17H26O10, was formed by a Koenigs-Knorr reaction of 2,3,4,6-tetra-O-acetyl-α-D-glucopyranosyl bromide and n-propanol. The central ring adopts a chair conformation. The crystal does not contain any significant interactions such as hydrogen bonds. PY - 2013 DO - https://doi.org/10.1107/S1600536812051495 SN - 1600-5368 VL - 69 IS - Part 2 SP - o158, sup-1 - sup-7 PB - Munksgaard CY - Copenhagen AN - OPUS4-27439 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mönch, Bettina A1 - Emmerling, Franziska A1 - Kraus, Werner A1 - Becker, Roland A1 - Nehls, Irene T1 - Isopropyl 2,3,4,6-tetra-O-acetyl-beta-D-glucopyranoside N2 - The title compound, C17H26O10, was formed by a Koenigs-Knorr reaction of 2,3,4,6-tetra-O-acetyl-α-D-glucopyranosyl bromide and propan-2-ol. The central ring adopts a chair conformation. The crystal does not contain any significant intermolecular interactions. PY - 2013 DO - https://doi.org/10.1107/S1600536812051483 SN - 1600-5368 VL - 69 IS - Part 2 SP - o157, sup-1 - sup-7 PB - Munksgaard CY - Copenhagen AN - OPUS4-27572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sauer, Andreas A1 - Scharf, Holger A1 - Becker, Roland T1 - Bericht zum 18. BAM-Ringversuch "Altlasten" N2 - Präsentation der Ergebnisse eines Ringversuchs zur Kompetenzbewertung von Prüflaboratorien auf dem Gebiet der anorganischen und organischen Bodenanalytik. KW - Eignungsprüfung KW - Boden KW - MKW KW - PAK KW - Gesamtcyanid KW - Spurenelemente KW - Proficiency testing KW - Soil KW - TPH KW - PAH KW - Total cyanide KW - Trace elements PY - 2012 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-357399 SP - 1 EP - 226 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35739 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dorgerloh, Ute A1 - Becker, Roland A1 - Lutz, A. A1 - Bremser, Wolfram A1 - Hilbert, S. A1 - Nehls, Irene T1 - How to improve reliability in groundwater analysis: over a decade of experience with external quality control in field campaigns on volatile halogenated compounds N2 - The reliability in measurement results obtained during environmental monitoring is crucial for the assessment and further planning of remediation efforts on the respective contaminated sites by the responsible authorities. A case study concerned with groundwater contaminated with perchloroethylene, trichloroethylene and 1,1,2-trichlorotrifluoroethane including their degradation products which involves private contract laboratories and an independent provider of quality assurance (QA) is presented. The experience gained with biannual monitoring campaigns over 14 years indicates that the selection of contractors on basis of accreditation status and successful performance in interlaboratory comparisons are not sufficient. Rather the auditing of the contractors by the QA provider prior to each campaign and the crosschecking of selected monitoring samples by the QA provider led to a lasting improvement of reliability in the contractors' measurement results. A mean deviation of 20% from the reference value determined by the QA provider for the crosschecked samples was reached. KW - Groundwater monitoring KW - External quality management KW - QM KW - VOC PY - 2012 DO - https://doi.org/10.1039/c1em10460h SN - 1464-0325 SN - 1464-0333 VL - 14 IS - 1 SP - 217 EP - 223 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-25288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Durmaz, V. A1 - Weber, M. A1 - Becker, Roland T1 - How to simulate affinities for host-guest systems lacking binding mode information: application to the liquid chromatographic separation of hexabromocyclododecane stereoisomers N2 - A novel approach for the simulation of host.guest systems by systematically scanning the host moleculefs orientations within the guest cavity is presented along with a thermodynamic strategy for determining preferential binding modes and corresponding optimal interaction energies between host and guest molecules. By way of example, the elution order of hexabromocyclododecane stereoisomers from high performance liquid chromatography separation on a permethylated β-cyclcodextrin stationary phase has been computed using classical molecular dynamics simulations with the explicit solvents water and acetonitrile. Comparison of estimated with experimental separation data reveals remarkable squared coefficients of correlation with R2=0.87 and a very high correlation RLOO2 . 0:72 using the leaveone-out cross-validation method and water as solvent. In particular, the approach presented shapes up as very robust in terms of the evaluated time range under consideration, reflecting well thermodynamic equilibria. These and further observations correlating with experimental results suggest the suitability of the underlying force fields and our multi-mode approach for the estimation of relative binding affinities for host–guest systems with unknown binding modes. KW - Molecular simulation KW - Molecular dynamics KW - Binding affinity KW - Elution order KW - Beta-cyclodextrin PY - 2012 DO - https://doi.org/10.1007/s00894-011-1239-5 SN - 1610-2940 SN - 0948-5023 VL - 18 IS - 6 SP - 2399 EP - 2408 PB - Springer CY - Berlin; Heidelberg AN - OPUS4-26112 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Roland T1 - Solid and liquid products of hydrothermal carbonizsation: Patterns of volatile organic compounds T2 - Third International Symposium on Green Chemistry for Environment, Health and Development CY - Skiathos, Greece DA - 2012-10-03 PY - 2012 AN - OPUS4-26632 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mönch, Bettina A1 - Gebert, Antje A1 - Emmerling, Franziska A1 - Becker, Roland A1 - Nehls, Irene T1 - Koenigs-Knorr reaction of fusel alcohols with methyl (1-bromo-2,3,4-tri-O-acetyl-alpha-D-glucopyranosid)uronate leading to the protected alkyl glucuronides-crystal structures and high resolution 1H and 13C NMR data N2 - Crystal structures and high resolution 1H and 13C NMR spectral data for methyl (alkyl 2,3,4-tri-O-acetyl-β-D-glucopyranosid)uronates (alkyl = methyl, ethyl, n-propyl, i-propyl, n-butyl, sec-butyl, i-butyl, n-pentyl, 2-methyl-1-butyl and 3-methyl-1-butyl) are presented. KW - D-Glucuronic acid derivates KW - X-ray analysis KW - High resolution NMR KW - Anomeric configuration KW - Synthesis PY - 2012 DO - https://doi.org/10.1016/j.carres.2012.01.002 SN - 0008-6215 SN - 1873-426X VL - 352 SP - 186 EP - 190 PB - Elsevier CY - Amsterdam AN - OPUS4-25759 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sauer, Andreas A1 - Scharf, Holger A1 - Becker, Roland T1 - Bericht zum 17. BAM-Ringversuch "Altlasten" N2 - Präsentation der Ergebnisse eines Ringversuchs zur Kompetenzbewertung von Prüflaboratorien auf dem Gebiet der anorganischen und organischen Bodenanalytik. KW - Eignungsprüfung KW - Boden KW - PAK KW - MKW KW - AOX KW - Spurenelemente KW - Gesamtcyanid KW - Proficiency testing KW - Soil KW - PAH KW - TPH KW - Trace elements KW - Total cyanide PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-357785 SP - 1 EP - 212 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35778 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Roland T1 - Hydroxylierte Derivate des Flammschutzmittels Hexabromcyclododecan: Beiträge zu Charakterisierung und Analytik in Biota T2 - ANAKON 2011 (ETH Zürich) CY - Zurich, Switzerland DA - 2011-03-22 PY - 2011 AN - OPUS4-23000 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moser, H. A1 - Roembke, J. A1 - Donnevert, G. A1 - Becker, Roland T1 - Evaluation of biological mehtods for a future methodological implementation of the hazard criterion H14 'ecotoxic' in the European waste list (2000/532/EC) N2 - The ecotoxicological characterization of waste is part of its assessment as hazardous or non-hazardous according to the European Waste List. For this classification 15 hazard criteria are derived from the Council Directive 91/689/EEC on hazardous waste. Some of the hazard criteria are based on the content of dangerous substances. The criterion H14 'ecotoxic' lacks of an assessment and testing strategy and no specific threshold values have been defined so far. Based on the recommendations of CEN guideline 14735 (2005), an international round robin test (ring test) was organized by the German Federal Environment Agency in order to define suitable test methods for the biological assessment of waste and waste eluates. A basic test battery, consisting of three aquatic and three terrestrial tests, was compiled. In addition, data were submitted for ten additional tests (five aquatic (including a genotoxicity test) and five terrestrial ones). The tests were performed with three representative waste types: an ash from an incineration plant, a soil containing high concentrations of organic contaminants (polycyclic aromatic hydrocarbons) and a preserved wood waste. The results of this ring test confirm that a combination of a battery of biological tests and chemical residual analysis is needed for an ecotoxicological characterization of wastes. With small modifications the basic test battery is considered to be well suitable for the hazard and risk assessment of wastes and waste eluates. All results and documents are accessible via a web-based data bank application. KW - European waste list KW - Waste legislation KW - Bio test battery KW - Ring test structure KW - Interlaboratory comparison KW - Waste ecotoxicity PY - 2011 DO - https://doi.org/10.1177/0734242X10367844 SN - 0734-242X SN - 1096-3669 VL - 29 IS - 2 SP - 180 EP - 187 PB - Sage CY - London AN - OPUS4-23271 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Esslinger, Susanne A1 - Becker, Roland A1 - Jung, Christian A1 - Schröter-Kermani, C. A1 - Bremser, Wolfram A1 - Nehls, Irene T1 - Temporal trend (1988-2008) of hexabromocyclododecane enantiomers in herring gull eggs from the german coastal region N2 - Levels of α-, β-, and γ-hexabromocyclododecane (HBCD) were determined in pooled eggs from herring gulls (Larus argentatus) sampled on three bird sanctuaries near the German North Sea coast between 1988 and 2008 (Mellum and Trischen) and the German Baltic Sea coast between 1998 and 2008 (Heuwiese) and archived by the German Environmental Specimen Bank. Pressurized fluid extraction, gel permeation chromatography, and LC–MS/MS using 13C12-labelled isotope standards and a chiral column were applied. α-HBCD was the dominating diastereomer and ranged between 3.7 and 107 ng g-1 lw while β- and γ-HBCD were throughout close to LOQ. The highest α-HBCD concentration was found in eggs from Mellum sampled in the year 2000. Interestingly, HBCD in eggs from the three islands displayed similar time courses with levels increasing to a peak contamination around 2000 and decreasing levels ever since. Chiral signatures of α-HBCD in eggs differed among the islands but indicated a preferential enrichment of the first eluting enantiomer (-)-α-HBCD. KW - Brominated flame retardant KW - Chiral separation KW - HPLC-ESI-MS/MS KW - Enantiomer-specific bioaccumulation PY - 2011 DO - https://doi.org/10.1016/j.chemosphere.2010.12.047 SN - 0045-6535 SN - 0366-7111 VL - 83 IS - 2 SP - 161 EP - 167 PB - Elsevier Science CY - Kidlington, Oxford AN - OPUS4-23351 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Esslinger, Susanne A1 - Becker, Roland A1 - Maul, Ronald A1 - Nehls, Irene T1 - Hexabromocyclododecane enantiomers: microsomal degradation and patterns of hydroxylated metabolites N2 - The degradation of the enantiomers of α-, β-, and γ-hexabromocyclododecane (HBCD) by phase I metabolism was investigated using induced rat liver microsomes. HBCD isomers were quantified using HPLC-MS/MS (ESI-) after separation on a combination of a reversed phase and a chiral analytical column. The degradation of all six isomers followed first-order kinetics and the estimated half-lives ranged from 6.3 min for both β-HBCD enantiomers to 32.3 min in case of (+)-γ-HBCD. (+)-α- and (–)-γ-HBCD displayed significantly shorter half-lives than their corresponding antipodes. It could be shown that this degradation led to a significant enrichment of the first eluting enantiomers (–)-α- and (+)-γ-HBCD. Individual patterns of mono- and dihydroxylated derivatives obtained from each α- and γ-HBCD enantiomer were seen to be distinctly characteristic. The patterns of monohydroxylated HBCD derivatives detected in liver and muscle tissues of pollack, mackerel and in herring gull eggs were largely similar to those observed in the in vitro experiments with rat liver microsomes. This enabled individual hydroxy-HBCDs to be assigned to their respective parent HBCD enantiomers. KW - Brominated flame retardant KW - Cytochromes KW - Phase I metabolism KW - Hydroxylation KW - HPLC-MS/MS PY - 2011 DO - https://doi.org/10.1021/es1039584 SN - 0013-936X SN - 1520-5851 VL - 45 IS - 9 SP - 3938 EP - 3944 PB - ACS Publ. CY - Washington, DC AN - OPUS4-23837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Roland T1 - Bewertung von HTC-Kohle für ihre Eignung zur Verbesserung von Bodeneigenschaften T2 - First INTERREG NSR Biochar conference - Biokohle - Klimaretter oder Mogelpackung? Biochar - Climate Savior or Bluff Package? 72. Symposium des ANS e. V., FU BErlin CY - Berlin, Germany DA - 2011-10-05 PY - 2011 AN - OPUS4-24456 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Roland T1 - Phase I Oxidation of alpha- and gamma-Hexabromocyclodeodecane by Cytochrome P450 Enzymes: Simulation of the Stereoisomerism of Hydroxylated Metabolites T2 - DIOXIN 2011, 31st International Symposium on Halogenated Persistent Organic Pollutants CY - Brussels, Belgium DA - 2011-08-21 PY - 2011 AN - OPUS4-23823 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Roland T1 - Determination of the proteinaceous binder component and soluble nylon preservative in Central Asian mural paintings using GC-MS T2 - "Auf Grünwedels Spuren - Restaurierung und Forschung an zentralasiatischen Wandmalereien" (Ausstellung des Museums für Asiatische Kunst, Berlin) CY - Berlin, Germany DA - 2011-12-10 PY - 2011 AN - OPUS4-24703 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scharkoi, O. A1 - Esslinger, Susanne A1 - Becker, Roland A1 - Weber, M. A1 - Nehls, Irene T1 - Phase I oxidation of alpha- and gamma-hexabromocyclododecane by cytochrome P450 enzymes: simulation of the steroisomerism of hydroxylated metabolites T2 - DIOXIN 2011 CY - Brussels, Belgium DA - 2011-08-21 KW - Bromierte Falmmschutzmittel KW - Hexabromcyclododecan KW - Cytochrom KW - Metaboliten KW - HPLC KW - Simulation PY - 2011 UR - http://www.dioxin20xx.org/pdfs/2011/1810.pdf SN - 1026-4892 VL - 73 SP - 730 EP - 733 AN - OPUS4-27263 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riddell, N. A1 - Becker, Roland A1 - Chittim, B. A1 - Emmerling, Franziska A1 - Köppen, Robert A1 - Lough, A. A1 - McAlees, A. A1 - McCrindle, R. T1 - Preparation and X-ray structural characterization of further stereoisomers of 1,2,5,6,9,10-hexabromocyclododecane N2 - Technical 1,2,5,6,9,10-hexabromocyclododecane (HBCD) consists largely of three diastereomers (α-, β-, and γ-HBCD) produced by the trans addition of bromine to cis,trans,trans-cyclododeca-1,5,9-triene (CDT). However, another seven diastereomers are theoretically possible and may be produced by trans addition of bromine across the double bonds of the other three isomers of 1,5,9-CDT. There are indications that small amounts of the minor HBCD isomers may be present in commercial HBCD mixtures or in products containing this brominated flame retardant (BFR). Such minor components may indeed derive from traces of other 1,5,9-CDTs in the cis, trans, trans starting material, however their formation may also be possible through isomerizations during the processing of this BFR or by bioisomerization subsequent to its release into the environment. Two of the seven additional diastereomers (δ- and ε-HBCD) were synthesized previously from trans,trans,trans-CDT. We now report the preparation of the remaining five diastereomers, ζ-, η-, and θ-HBCD from cis,cis,trans-CDT and ι- and κ-HBCD from cis,cis,cis-CDT, and their characterization by 1H NMR spectroscopy and X-ray crystallography. The availability of these further diastereomers of HBCD should aid in determining if the minor isomers are present in commercial samples of this BFR, in products containing HBCDs, or in environmental samples. We have also carried out an X-ray crystal structure determination on ε-HBCD, so that crystal structures are now available for all 10 HBCD diastereomers. KW - Brominated flame retardants KW - HBCDs KW - Minor isomers KW - X-ray PY - 2011 DO - https://doi.org/10.1016/j.chemosphere.2011.06.014 SN - 0045-6535 SN - 0366-7111 VL - 84 IS - 7 SP - 900 EP - 907 PB - Elsevier Science CY - Kidlington, Oxford AN - OPUS4-24298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Roland T1 - Time courses of HBCD levels and enantiomeric signatures in herring gull eggs from the German coast T2 - 30 th International Symposium on Halogenated Persistent Organic Pollutants (Dioxin 2010) CY - San Antonio, TX, USA DA - 2010-09-12 PY - 2010 AN - OPUS4-21600 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -