TY - JOUR A1 - Mönch, Bettina A1 - Becker, Roland A1 - Nehls, Irene T1 - Quantification of ethyl glucuronide in hair: effect of milling on extraction efficiency JF - Alcohol and alcoholism N2 - Aim: The objective of the study was to provide conclusive evidence for the effect of particle size reduction as by milling on the extractable content of ethyl glucuronide (EtG) of hair samples. Methods: A number of real case hair samples and two pooled hair materials with EtG contents in the range of 10–30 pg/mg were systematically compared with regard to the extraction yield of EtG after cutting to 2–3 mm length and pulverization with a ball mill. After the respective treatment the samples were submitted to aqueous extraction followed by quantification of EtG using HPLC-MS/MS. Results: It was unequivocally demonstrated that milling of hair samples prior to aqueous extraction significantly increases the extractable EtG content compared with cut hair. The effect ranged between 137 and 230% and was seen to occur regardless of the extent of pulverization. Cooling of samples was not necessary to prevent partial degradation of EtG during the grinding procedure. Conclusion: The options currently employed at choice in analytical practice (cutting or milling) were seen to significantly affect the extractable amount of EtG in hair. This is suspected to influence the degree of equivalence of quantification results obtained in different laboratories as well as their respective classification of a test subject's drinking behaviour on the basis of currently recommended cut-off values. PY - 2013 DO - https://doi.org/10.1093/alcalc/agt059 SN - 0735-0414 SN - 0309-1635 SN - 1464-3502 VL - 48 IS - 5 SP - 558 EP - 563 PB - Univ. Press CY - Oxford AN - OPUS4-28843 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 JF - Acta crystallographica E 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 - Becker, Roland A1 - Jung, Christian A1 - Nehls, Irene T1 - The homogeneity testing of EtG in hair reference materials: A high-throughput procedure using GC-NCI-MS JF - Forensic science international N2 - The validation of a robust quantification procedure for EtG in hair using GC–NCI–MS is presented. Aqueous extraction is followed by complete lyophylization of the extract and derivatization with pentafluoropropionic anhydride (PFPA) under controlled temperature and duration. Clean-up of extracts was dispensable and standard single quadrupole MS displayed sufficient selectivity and sensitivity. The method displayed a wide linearity range and enabled LOD of 0.68 pg/mg, LOQ of 2.4 pg/mg, and precision below 8.12%. Since EtG was seen to display prolonged stability in the aqueous extracts and after derivatization with PFPA this straightforward procedure allows a routine throughput of large quantities of samples with little proneness to procedural scatter of results. The method was applied to demonstrate the homogeneity of two hair reference materials with mean EtG contents of 8.48 pg/mg and 22.0 pg/mg. Aside from the application in homogeneity studies of hair reference materials predominantly in the concentration range of 10–50 pg/mg the method was also designed for daily routine quantification of real-world sample with regard to drinking behavior assessment. KW - Extraction KW - Derivatization KW - High-throughput analysis KW - Reference materials KW - Homogeneity KW - Measurement uncertainty PY - 2013 DO - https://doi.org/10.1016/j.forsciint.2013.01.018 SN - 0379-0738 SN - 1872-6283 VL - 226 IS - 1-3 SP - 202 EP - 207 PB - Elsevier Ltd. CY - Amsterdam [u.a.] AN - OPUS4-27998 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 JF - Acta crystallographica E 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 - GEN A1 - Sauer, Andreas A1 - Scharf, Holger A1 - Becker, Roland T1 - Bericht zum 19. 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 - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-356963 SP - 1 EP - 233 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35696 LA - deu 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 JF - Acta crystallographica E 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 - CONF A1 - Becker, Roland A1 - Mönch, Bettina A1 - Ammann, Dominic A1 - Nehls, Irene T1 - Quantification of ethyl glucuronide in hair: The effect of milling and sonication on the extraction efficiency T2 - 18th Meeting of the Society of Hair Testing T2 - 18th Meeting of the Society of Hair Testing CY - Geneva, Switzerland DA - 2013-08-28 PY - 2013 AN - OPUS4-28722 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Roland T1 - External quality control: a way to improve reliability in hair analysis T2 - 18th Meeting of the Society of Hair Testing T2 - 18th Meeting of the Society of Hair Testing CY - Geneva, Switzerland DA - 2013-08-28 PY - 2013 AN - OPUS4-28723 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 JF - Environmental science : processes & impacts 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 - Becker, Roland A1 - Dorgerloh, Ute A1 - Helmis, M. A1 - Mumme, J. A1 - Diakité, M. A1 - Nehls, Irene T1 - Hydrothermally carbonized plant materials: Patterns of volatile organic compounds detected by gas chromatography JF - Bioresource technology N2 - The nature and concentrations of volatile organic compounds (VOCs) in chars generated by hydrothermal carbonization (HTC) is of concern considering their application as soil amendment. Therefore, the presence of VOCs in solid HTC products obtained from wheat straw, biogas digestate and four woody materials was investigated using headspace gas chromatography. A variety of potentially harmful benzenic, phenolic and furanic volatiles along with various aldehydes and ketones were identified in feedstock- and temperature-specific patterns. The total amount of VOCs observed after equilibration between headspace and char samples produced at 270 °C ranged between 2000 and 16,000 µg/g (0.2–1.6 wt.%). Depending on feedstock 50–9000 µg/g of benzenes and 300–1800 µg/g of phenols were observed. Substances potentially harmful to soil ecology such as benzofurans (200–800 µg/g) and p-cymene (up to 6000 µg/g in pine wood char) exhibited concentrations that suggest restrained application of fresh hydrochar as soil amendment or for water purification. KW - Hydrochar KW - Mass spectrometry KW - Flame ionization detection KW - Phenols KW - Benzenes PY - 2013 DO - https://doi.org/10.1016/j.biortech.2012.12.102 SN - 0960-8524 SN - 1873-2976 VL - 130 SP - 621 EP - 628 PB - Elsevier Applied Science CY - Barking, Essex AN - OPUS4-27616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dorgerloh, Ute A1 - Theißen, H. A1 - Becker, Roland A1 - Nehls, Irene T1 - Das Problem löst sich von selbst: Stabilisierung von Grundwasserproben zur Bestimmung organischer Inhaltsstoffe T2 - Altlastensymposium 2014 N2 - Als Folge der industriellen Produktion und der vielfältigen industriellen Nutzung von organischen Lösungsmitteln sind eine Vielzahl von Edukten, Zwischen- und Endprodukten in die Umwelt eingetragen worden und führen zu massiven Verunreinigungen des Bodens und des Grundwassers. Die Untersuchung und Sanierung des Grundwassers stellt einen aktuellen Schwerpunkt in der Altlastenbearbeitung dar. Vielfach werden klassische pump & treat-Verfahren zur Grundwassersanierung verwendet. Diese aktiven Sicherungs- und Sanierungsmaßnahmen werden jedoch unter dem Gesichtspunkt der Verhältnismäßigkeit häufig als ineffizient eingeschätzt. Als Alternative sollen die natürlichen Abbauprozesse im Grundwasserleiter genutzt oder gezielt verstärkt werden, um auf diesem Weg eine in-situ-Sanierung des Grundwasserleiters zu erreichen. In den letzten Jahren haben sich verschiedene Sanierungsverfahren etabliert, bei denen durch die Zugabe von Hilfsstoffen die mikrobiologische Aktivität des Aquifers erhöht wird bzw. Stoffe zugeführt werden, die mit den Schadstoffen reagieren (in-situ chemische Oxidation bzw. Reduktion, ISCO). An ausgewählten Standorten ist auch die aktive Sanierung (pump & treat, on-site- Sanierung) mit biologischem Schadstoffabbau (Bio-Filter) kombiniert worden. Um den Sanierungsverlauf zu verfolgen und zu optimieren, ist die Beprobung von Grundwasser aus dem Grundwasserleiter oder aus laufenden Anlagen erforderlich. In Fällen der gesteigerten mikrobiologischen Aktivität des Grundwassers treten gehäuft Probleme bei der Stabilisierung der Wasserproben auf. Die forcierten Abbauprozesse der Schadstoffe gehen nach der Probenahme in der Probenflasche weiter, bis die Energiebasis der Mikrobiologie aufgebraucht ist. Durch eine geringe Temperaturerhöhung beschleunigen sich diese Prozesse zusätzlich. In der Folge können die Schadstoffgehalte teilweise innerhalb weniger Stunden stark reduziert werden. Im Analysenlabor wird dann ein Schadstoffgehalt nachgewiesen, der nicht mehr die Verhältnisse im Aquifer bzw. im Ablauf der Reinigungsstufen widerspiegelt. Eine Einschätzung des Sanierungsfortschritts oder der Reinigungsleistung ist unter diesen Bedingungen stark fehlerbehaftet und kann zu groben Fehlinterpretationen führen. Grundwasserproben, die einem Aquifer mit hoher natürlicher oder initiierter mikrobiologischer Abbauaktivität entstammen, müssen daher zusätzlich stabilisiert werden, um den Ist-Zustand zum Zeitpunkt der Probenahme zu erfassen. Die Konservierung von Wasserproben bei der Probenahme von Grundwasser ist in der Normung umfangreich beschrieben: Die EN ISO 5667-3 von 2004 ist im Normausschuss (NA 119-01-03-01-01) überarbeitet und 2012 als Norm verabschiedet worden (EN ISO 5667-3, 03.12, deutsche Fassung DIN EN ISO 5667-3, 03-2013) [1], In Einzelfällen hat sie sich nicht als ausreichend erwiesen, um die Stabilität der organischen Schadstoffe in den oben beschriebenen Wasserproben zu gewährleisten. T2 - Altlastensymposium 2014 CY - Fulda, Germany DA - 20.03.2014 KW - Grundwasser KW - In-situ-Sanierung KW - Probenahme KW - Stabilisierung PY - 2014 SP - 76 EP - 85 AN - OPUS4-30480 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ammann, Dominic A1 - Becker, Roland A1 - Kohl, Anka A1 - Hänisch, Jessica A1 - Nehls, Irene T1 - Degradation of the ethyl glucuronide content in hair by hydrogen peroxide and a non-destructive assay for oxidative hair treatment using infra-red spectroscopy JF - Forensic science international N2 - The assessment of quantification results of the alcohol abuse marker ethyl glucuronide (EtG) in hair in comparison to the cut-off values for the drinking behavior may be complicated by cosmetic hair bleaching. Thus, the impact of increasing exposure to hydrogen peroxide on the EtG content of hair was investigated. Simultaneously, the change of absorbance in the range of 1000–1100 cm-1 indicative for the oxidation of cystine was investigated non-destructively by attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) using pulverized portions of the respective hair samples. Hair samples treated with hydrogen peroxide consistently displayed a significantly increased absorbance at 1040 cm-1 associated with the formation of cysteic acid. The EtG content decreased significantly if the hair was treated with alkaline hydrogen peroxide as during cosmetic bleaching. It could be shown that ATR-FTIR is capable of detecting an exposure to hydrogen peroxide when still no brightening was visible and already before the EtG content deteriorated significantly. Thus, hair samples suspected of having been exposed to oxidative treatment may be checked non-destructively by a readily available technique. This assay is also possible retrospectively after EtG extraction and using archived samples. KW - Hair testing KW - Oxidation KW - Bleaching KW - Cysteic acid KW - HPLC–MS/MS PY - 2014 DO - https://doi.org/10.1016/j.forsciint.2014.07.029 SN - 0379-0738 SN - 1872-6283 VL - 244 SP - 30 EP - 35 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-31755 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Dorgerloh, Ute A1 - Paulke, E. A1 - Mumme, J. A1 - Nehls, Irene T1 - Hydrothermal carbonization of biomass: Major organic components of the aqueous phase JF - Chemical engineering & technology N2 - Process waters obtained from hydrothermal carbonization (HTC) of wheat straw, a biogas digestate derived thereof, and four woody biomass feedstocks were quantified regarding the total organic carbon (TOC) and selected organic compounds. HTC runs revealed that TOC loads were largely unaffected by process severity or type of feedstock whereas the C2–C6 fatty acids, determined by GC, displayed clear effects of temperature and feedstock. HPLC demonstrated simultaneously the initial increase and subsequent consumption of cellulose-derived furfural and 5-hydroxymethylfurfural as well as the increase of the lignin-derived 2-methoxyphenol. 2-Methylbenzofuran, an example for a substance potentially harmful to aquatic biota, was observed in high concentration in the HTC liquor from wheat straw-based feedstocks. KW - Furfurals KW - Gas chromatography KW - Liquid chromatography KW - Phenols KW - Process water KW - Total organic carbon PY - 2014 DO - https://doi.org/10.1002/ceat.201300401 SN - 0930-7516 SN - 1521-4125 VL - 37 IS - 3 SP - 511 EP - 518 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-30333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mönch, Bettina A1 - Becker, Roland A1 - Nehls, Irene T1 - Determination of ethyl glucuronide in hair: a rapid sample pretreatment involving simultaneous milling and extraction JF - International journal of legal medicine N2 - A combination of simultaneous milling and extraction known as micropulverized extraction was developed for the quantification of the alcohol marker ethyl glucuronide (EtG) in hair samples using a homogeneous reference material and a mixer mill. Best extraction results from 50 mg of hair were obtained with 2-mL plastic tubes containing two steel balls (Ø = 5 mm), 0.5 mL of water and with an oscillating frequency of 30 s-1 over a period of 30 min. EtG was quantified employing a validated GC-MS procedure involving derivatization with pentafluoropropionic acid anhydride. This micropulverization procedure was compared with dry milling followed by separate aqueous extraction and with aqueous extraction after manual cutting to millimeter-size snippets. Micropulverization yielded 28.0±1.70 pg/mg and was seen to be superior to manually cutting (23.0±0.83 pg/mg) and equivalent to dry grinding (27.7±1.71 pg/mg) with regard to completeness of EtG extraction. The option to process up to 20 samples simultaneously makes micropulverization especially valuable for the high throughput of urgent samples. KW - Ethyl glucuronide KW - Hair KW - Micropulverized extraction KW - GC-MS PY - 2014 DO - https://doi.org/10.1007/s00414-013-0939-z SN - 0937-9827 SN - 1437-1596 VL - 128 IS - 1 SP - 69 EP - 72 PB - Springer CY - Berlin ; Heidelberg AN - OPUS4-30063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Dorgerloh, Ute A1 - Sauer, Andreas A1 - Hofmann, Andrea T1 - Quality control in extended measurement campaigns: selection of contract laboratories by proficiency testing exemplified for the trace analysis of anilines in groundwater JF - Accreditation and quality assurance N2 - An interlaboratory comparison for the determination of aniline, nine methylated anilines and chlorinated anilines in contaminated groundwater (each compound between 1 µg L-1 and 750 µg L-1) was conducted as proficiency test for the selection of contract laboratories for a groundwater monitoring campaign. For the 13 participants, two different test sample series were prepared from a stabilized real case groundwater. Series A was the groundwater as sampled in the field and series B was prepared from series A by spiking with selected anilines. Homogeneity and stability investigations revealed that contaminated groundwater provides a viable basis for the preparation of ring test samples for the determination of anilines. Analytical procedures were limited to the standardized liquid–liquid extraction or solid-phase extraction in combination with gas chromatography/mass spectrometry (DIN 38407-16:1999). The robust consensus values were evaluated according to the standardized protocol of DIN 38402-45:2013. Robust reproducibility standard deviations ranged largely between 20?% and 60?% depending on the analyte. The proficiency assessment of individual participants combined the qualitative aspect of correct peak identification with the quantitative determination of individual concentrations within set limits in a unified approach. It could be shown that the accreditation status of laboratory and the existence of a standardized analytical procedure do not substitute a problem-related proficiency assessment of potential contractors. KW - Aniline KW - Chloroanilines KW - Methylanilines KW - Groundwater KW - Interlaboratory comparison KW - Proficiency test PY - 2014 DO - https://doi.org/10.1007/s00769-014-1072-5 SN - 0949-1775 SN - 1432-0517 N1 - Geburtsname von Sauer, Andreas: Buchholz, A. - Birth name of Sauer, Andreas: Buchholz, A. VL - 19 IS - 5 SP - 371 EP - 376 PB - Springer CY - Berlin AN - OPUS4-31756 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Roland A1 - Ammann, Dominic A1 - Kohl, Anka A1 - Nehls, Irene T1 - Degradation of Ethyl glucuronide by hydrogen peroxide and a non-destructive assay for oxidative hair treatment using infra-red spectroscopy T2 - 19th Meeting of the Society of Hair Testing T2 - 19th Meeting of the Society of Hair Testing CY - Bordeaux, France DA - 2014-06-11 PY - 2014 AN - OPUS4-30747 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sauer, Andreas A1 - Scharf, Holger A1 - Becker, Roland T1 - Bericht zum 20. 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 - Spurenelemente KW - Chrom(VI) KW - Proficiency testing KW - Soil KW - TPH KW - PAH KW - Trace elements KW - Chromium(VI) PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-356424 SP - 1 EP - 228 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35642 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sauer, Andreas A1 - Scharf, Holger A1 - Becker, Roland T1 - Bericht zum 21. 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 - Spurenelemente KW - Gesamtcyanid KW - Proficiency testing KW - Soil KW - PAH KW - TPH KW - Trace elements KW - Total cyanide PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355586 SP - 1 EP - 234 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35558 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Roland A1 - Dorgerloh, Ute A1 - Nehls, Irene T1 - Analysis of volatile and semi-volatile components in hydrochar: prospects and challenges T2 - International Biochar Symposium 2015 Biochar - Contribution to Sustainable Agriculture T2 - International Biochar Symposium 2015 Biochar - Contribution to Sustainable Agriculture CY - Potsdam DA - 2015-05-28 PY - 2015 AN - OPUS4-33741 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schallschmidt, Kristin A1 - Becker, Roland A1 - Zwaka, H. A1 - Menzel, R. A1 - Johnen, D. A1 - Fischer-Tenhagen, C. A1 - Rolff, J. A1 - Nehls, Irene T1 - In vitro cultured lung cancer cells are not suitable for animal-based breath biomarker detection JF - Journal of breath research N2 - In vitro cultured lung cancer cell lines were investigated regarding the possible identification of volatile organic compounds as potential biomarkers. Gas samples from the headspace of pure culture medium and from the cultures of human lung adenocarcinoma cell lines A549 and Lu7466 were exposed to polypropylene fleece in order to absorb odour components. Sniffer dogs were trained with loaded fleeces of both cell lines, and honey bees were trained with fleeces exposed to A549. Afterwards, their ability to distinguish between cell-free culture medium odour and lung cancer cell odour was tested. Neither bees nor dogs were able to discriminate between odours from the cancer cell cultures and the pure culture medium. Solid phase micro extraction followed by gas chromatography with mass selective detection produced profiles of volatiles from the headspace offered to the animals. The profiles from the cell lines were largely similar; distinct differences were based on the decrease of volatile culture medium components due to the cells' metabolic activity. In summary, cultured lung cancer cell lines do not produce any biomarkers recognizable by animals or gas chromatographic analysis. KW - A549 KW - Honey bees KW - Odour discrimination task KW - Sniffer dogs KW - Solid phase microextraction KW - Volatile organic compounds KW - Volatilome PY - 2015 DO - https://doi.org/10.1088/1752-7155/9/2/027103 SN - 1752-7155 SN - 1752-7163 VL - 9 IS - 2 SP - 027103-1 EP - 027103-10 PB - IOP CY - Bristol AN - OPUS4-34161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schallschmidt, Kristin A1 - Becker, Roland A1 - Jung, Christian A1 - Rolff, J. A1 - Fichtner, I. T1 - Investigation of cell culture volatilomes using solid phase micro extraction: options and pitfalls exemplified with adenocarcinoma cell lines JF - Journal of chromatography B N2 - Three strategies to sample volatile organic compounds (VOC) from lung cancer cell lines cultured in vitro were compared. Headspace solid phase microextraction was applied in situ to culture flasks and alternatively to subsamples of headspace gas or to nutrient solution subsamples followed by gas chromatography–mass spectrometry. The direct quantification of 55 VOC in the headspace of cell cultures was validated and is discussed with respect to reproducibility and system-related interferences. The role of the VOC background from culture media and usually employed polystyrene culture vessels is examined and was seen to invoke potentially misleading conclusions. The commercial A549 and two further adenocarcinoma cell lines displayed largely similar VOC profiles with distinct differences regarding certain individual substances. There is evidence for the inappropriateness of the standard cell culturing methods in the search for volatile cancer markers. KW - A549 KW - Lung cancer cell culture KW - GC–MS KW - SPME KW - VOC KW - Volatilome KW - Alcohol marker KW - Micropulverization KW - HPLC-MS/MS KW - Fortification KW - Long term stability PY - 2015 DO - https://doi.org/10.1016/j.jchromb.2015.10.004 SN - 0378-4347 SN - 1570-0232 SN - 1387-2273 SN - 1873-376X VL - 1006 SP - 158 EP - 166 PB - Elsevier B.V. CY - Amsterdam [u.a.] AN - OPUS4-34991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scharkoi, O. A1 - Becker, Roland A1 - Esslinger, Susanne A1 - Weber, M. A1 - Nehls, Irene T1 - Predicting sites of cytochrome P450-mediated hydroxylation applied to CYP3A4 and hexabromocyclododecane JF - Molecular simulation N2 - This article describes a simple and quick in silico method for the prediction of cytochrome P450 (CYP)-mediated hydroxylation of drug-like compounds. Testosterone and progesterone, two known substrates of CYP3A4, are used to test the method. Further, we apply the procedure to predict sites of hydroxylation of isomers of the flame retardant hexabromocyclododecane by CYP3A4. Within the method, the compound is rotated in the binding pocket of the cytochrome, so that each hydrogen under consideration is placed near the active centre. Afterwards, short molecular dynamics simulations are provided for each step of the rotation. All steps of the simulation are compared concerning the distances between the hydrogens and the active centre and the corresponding energies. The computational results correlate well with experimental results. KW - Predicting sites of metabolism KW - Cytochrome P450 KW - Hydroxylation KW - Metabolism of HBCD PY - 2015 DO - https://doi.org/10.1080/08927022.2014.898845 SN - 0892-7022 SN - 1029-0435 VL - 41 IS - 7 SP - 538 EP - 546 PB - Gordon and Breach CY - New York, NY AN - OPUS4-30492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Nehls, Irene A1 - Schallschmidt, Kristin A1 - Becker, Roland A1 - Fischer-Tenhagen, C. A1 - Johnen, D. A1 - Leschber, G. A1 - Frese, S. A1 - Neudecker, J. A1 - Walles, T. ED - Schüler, C. ED - Püschel, K. T1 - BIOAIR - Ein interdisziplinäres Projekt zur Bestimmung von Krebsmarkern in der Atemluft T2 - Faszinosum Spürhunde - Quo vadis? N2 - Wie viele Forschergruppen, haben auch wir uns das langfristige Ziel gesetzt, einen Beitrag bei der Beantwortung der Frage zu leisten, was Hunde riechen, wenn sie Krebs erschnüffeln. Dabei sollen die Hunde nicht nur anzeigen, ob eine Atemluftprobe positiv oder negativ ist, sondern sie sollen auch aktiv eingebunden werden in den systematischen Suchprozess nach detektierbaren Biomarkern. So ist geplant, dass mittels eines präparativen Fraktionssammlers definierte Schnitte des Gaschromatogramms einzeln oder in möglichen Kombinationen auf das Adsorbervlies gebracht werden, um im Hundetraining eingesetzt zu werden. In analoger Weise könnte auch mit spezifischen Kandidatensubstanzen verfahren werden. PY - 2015 SN - 978-3-8300-8763-2 N1 - Serientitel: Forschungsergebnisse aus dem Institut für Rechtsmedizin der Universität Hamburg – Series title: Forschungsergebnisse aus dem Institut für Rechtsmedizin der Universität Hamburg VL - 30 SP - 93 EP - 101 PB - Dr. Kovac AN - OPUS4-33165 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ammann, Dominic A1 - Becker, Roland A1 - Nehls, Irene T1 - Stability of ethyl glucuronide in hair reference materials after accelerated aging JF - Forensic science international N2 - Two different hair reference materials, one produced from authentic hair displaying an ethyl glucuronide (EtG) content of about 25 pg/mg and one obtained by fortification of blank hair to an EtG level of 85 pg/mg were submitted to accelerated aging between 4 degrees C and 60 degrees C for periods between one and 24 months. Subsequently, the EtG content was determined in the aged samples and untreated reference samples stored at -22 degrees C under repeatability conditions following the so-called isochronous approach. The EtG content remained stable even at 40 degrees C for 24 months and at 60 degrees C over six months. This is in contrast to many organic analytes contained in trace concentrations in diverse matrices. A slight but significant increase of the recovered EtG in case of authentic hair samples having been exposed for 24 months between 4 degrees C and 60 degrees C may be due to a temperature-driven process that allows increased recoveries of the physiologically embedded EtG. KW - Alcohol marker KW - Micropulverization KW - HPLC-MS/MS KW - Fortification KW - Long term stability PY - 2015 DO - https://doi.org/10.1016/j.forsciint.2015.09.015 SN - 0379-0738 SN - 1872-6283 VL - 257 SP - 337 EP - 340 PB - Elsevier Ireland Ldt. CY - Amsterdam [u.a.] AN - OPUS4-34940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Roland A1 - Ammann, Dominic A1 - Mönch, Bettina A1 - Nehls, Irene T1 - Chemische Analytik in der Forensik: Der Alkoholkonsummarker Ethylglucuronid T2 - ANAKON 2015 T2 - ANAKON 2015 CY - Graz (Österreich) DA - 2015-03-23 PY - 2015 AN - OPUS4-32828 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Roland A1 - Schallschmidt, Kristin A1 - Nehls, Irene A1 - Johnen, D. A1 - Fischer-Tenhagen, C. T1 - Odour reference material and training concepts for sniffer dogs T2 - International Conference on Medical Bio-Detection T2 - International Conference on Medical Bio-Detection CY - Cambridge (England) DA - 2015-09-15 PY - 2015 AN - OPUS4-33984 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Roland A1 - Schallschmidt, Kristin A1 - Nehls, Irene A1 - Johnen, D. A1 - Fischer-Tenhagen, C. T1 - Odour reference materials and training concepts for sniffer dogs T2 - International Association of Breath Research Summit 2015 T2 - International Association of Breath Research Summit 2015 CY - Wien (Österreich) DA - 2015-09-14 PY - 2015 AN - OPUS4-33981 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schallschmidt, Kristin A1 - Becker, Roland A1 - Jung, Christian A1 - Bremser, Wolfram A1 - Nehls, Irene A1 - Leschber, G. A1 - Frese, S. A1 - Walles, T. A1 - Neudecker, J. T1 - Comparison of volatile organic compounds from lung cancer patients and healthy controls—challenges and limitations of an observational study JF - Journal of Breath Research N2 - The design and operation of an observational study on the profiles of volatile organic compounds (VOC) in the breath of 37 lung cancer patients and 23 healthy controls of similar age is outlined. The necessity to quantify each VOC considered as potential disease marker on basis of individual calibration is elaborated and the quality control measures required to maintain reproducibility in breath sampling and subsequent instrumental trace VOC analysis using SPME-GC-MS over a study period of 14 months are described. 24 VOC were quantified on basis of their previously suggested potential as cancer markers. The breath concentration levels of aromatic compounds was expectedly increased in smokers while lung cancer patients displayed significantly increased levels of oxygenated VOC such as aldehydes, 2-butanone and 1-butanol. Though sets of selected oxygenated VOC displayed sensitivities and specificities between 80 and 90% using linear discriminant analysis with leave-one-out cross validation the effective selectivity of the breath VOC approach with regard to cancer detection is clearly limited. Results were discussed against the background of the literature on volatile cancer marker investigations and the prospects to link increased VOC levels in patients’ breath with approaches to employ sniffer dogs. Experiences from this study and the literature suggest that the current state of breath VOC based discrimination between cancer patients and healthy controls is hardly improvable. Observational studies tend to observe significant differences mostly in levels of certain oxygenated VOC but without resolution required for practical application. Any step towards practicable exploitation of VOC profile differences for illness detection would have to solve current restrictions set by the low and variable VOC concentrations. Further challenges are the technical complexity of studies involving breath sampling and possibly the limited capability of current analytical procedures to detect instable marker candidates. KW - Breath KW - Volatile organic compounds KW - Marker KW - Cancer KW - Gas chromatography KW - Solid phase microextraction KW - Volatilome PY - 2016 DO - https://doi.org/10.1088/1752-7155/10/4/046007 SN - 1752-7155 SN - 1752-7163 VL - 10 IS - 4 SP - Article 046007, 1 EP - 17 PB - IOP Publishing AN - OPUS4-37801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea A1 - Breitfeld, S. A1 - Sauer, Andreas A1 - Becker, Roland A1 - Kalbe, Ute A1 - Bremser, Wolfram A1 - Braun, Ulrike T1 - A Raman spectroscopic method for the monitoring of microplastics in soil T2 - Tagungsband – 12. Kolloquium Prozessanalytik, Berlin, 28.–30. November 2016 N2 - Due to the increasing presence of microplastic particles (MP) in the Environment and the unknown risks arising from them, there is an urgent need for analytical methods that allow for an efficient identification and quantification of microplastics (MP), i.e. particles < 5 mm, in environmental samples. So far, mostly timeconsuming (micro) infrared or micro-Raman spectroscopic methods are applied. Here an faster alternative Approach is presented based on a Raman processspectrometer with fiber-optical probes in combination with multivariate data analysis. T2 - 12. Kolloquium Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - Raman spectroscopy KW - Microplastics KW - Soil KW - Chemometrics KW - PLS-DA PY - 2016 SP - P10, 59 EP - 60 AN - OPUS4-38392 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 22. BAM-Ringversuch "Altlasten" N2 - Präsentation der Ergebnisse eines Ringversuchs zur Kompetenzbewertung von Prüflaboratorien auf dem Gebiet der anorganischen und organischen Bodenanalytik: Polyzyklische aromatische Kohlenwasserstoffe (PAK) in Boden, Mineralölkohlenwasserstoffe (MKW) in Boden, Elemente in Sediment und Gesamtcyanid in Boden. KW - Eignungsprüfung KW - Boden KW - Spurenelemente KW - Gesamtcyanid KW - MKW KW - PAK PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-398676 SP - 1 EP - 261 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-39867 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bachmann, H. J. A1 - Bucheli, T. D. A1 - Dieguez-Alonso, A. A1 - Fabbri, D. A1 - Knicker, H. A1 - Schmidt, H.-P. A1 - Ulbricht, A. A1 - Becker, Roland A1 - Buscaroli, A. A1 - Buerge, D. A1 - Cross, A. A1 - Dickinson, D. A1 - Enders, A. A1 - Esteves, V.I. A1 - Evangelou, M. W. H. A1 - Fellet, G. A1 - Friedrich, K. A1 - Gasco Guerrero, G. A1 - Glaser, B. A1 - Hanke, U. M. A1 - Hanley, K. A1 - Hilber, I. A1 - Kalderis, D. A1 - Leifeld, J. A1 - Masek, O. A1 - Mumme, J. A1 - Paneque Carmona, M. A1 - Calvelo Pereira, R. A1 - Rees, F. A1 - Rombola, A. G. A1 - de la Rosa, J. M. A1 - Sakrabani, R. A1 - Sohi, S. A1 - Soja, G. A1 - Valagussa, M. A1 - Verheijen, F. A1 - Zehetner, F. T1 - Towards the standardization of biochar analysis: the COST action TD1107 interlaboratory comparison JF - Journal of agricultural and food chemistry N2 - Biochar produced by pyrolysis of organic residues is increasingly used for soil amendment and many other applications. However, analytical methods for its physical and chemical characterization are yet far from being specifically adapted, optimized, and standardized. Therefore, COST Action TD1107 conducted an interlaboratory comparison in which 22 laboratories from 12 countries analyzed three different types of biochar for 38 physical–chemical parameters (macro- and microelements, heavy metals, polycyclic aromatic hydrocarbons, pH, electrical conductivity, and specific surface area) with their preferential methods. The data were evaluated in detail using professional interlaboratory testing software. Whereas intralaboratory repeatability was generally good or at least acceptable, interlaboratory reproducibility was mostly not (20% < mean reproducibility standard deviation < 460%). This paper contributes to better comparability of biochar data published already and provides recommendations to improve and harmonize specific methods for biochar analysis in the future. KW - Biochar KW - Analysis KW - Standardization KW - Ring test KW - Interlaboratory comparison PY - 2016 DO - https://doi.org/10.1021/acs.jafc.5b05055 SN - 0021-8561 SN - 1520-5118 VL - 64 IS - 2 SP - 513 EP - 527 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-35289 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sauer, Andreas A1 - Buttler, Sabine A1 - Scharf, Holger A1 - Becker, Roland T1 - Bericht zum 23. BAM-Ringversuch "Altlasten" N2 - Präsentation der Ergebnisse eines Ringversuchs zur Kompetenzbewertung von Prüflaboratorien auf dem Gebiet der anorganischen und organischen Bodenanalytik: Polyzyklische aromatische Kohlenwasserstoffe (PAK) in Boden, Mineralölkohlenwasserstoffe (MKW) in Boden, Elemente in Sediment und Gesamtcyanid in Boden. KW - Gesamtcyanid KW - Boden KW - Eignungsprüfung KW - MKW KW - PAK KW - Schwermetalle PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-473403 SP - 1 EP - 261 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-47340 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ricci, M. A1 - Shegunova, P. A1 - Conneely, P. A1 - Becker, Roland A1 - Torres, M. M. A1 - Osuna, M. A. A1 - On, T.P. A1 - Man, L.H. A1 - Baek, S.-Y. A1 - Kim, B. A1 - Hopley, C. A1 - Liscio, C. A1 - Warren, J. A1 - Le Diouron, V. A1 - Lardy-Fontan, S. A1 - Lalere, B. A1 - Mingwu, S. A1 - Kucklick, J. A1 - Vamathevan, V. A1 - Matsuyama, S. A1 - Numata, M. A1 - Brits, M. A1 - Quinn, L. A1 - Fernandes-Whaley, M. A1 - Gören, A.C. A1 - Binici, B. A1 - Konopelko, L. A1 - Krylov, A. A1 - Mikheeva, A. T1 - CCQM-K102: Polybrominated diphenyl ethers in sediment JF - Metrologia N2 - The key comparison CCQM-K102: Polybrominated diphenyl ethers in sediment was coordinated by the JRC, Directorate F - Health, Consumers & Reference Materials, Geel (Belgium) under the auspices of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM). Thirteen National Metrology institutes or Designated Institutes and the JRC participated. Participants were requested to report the mass fraction (on a dry mass basis) of BDE 47, 99 and 153 in the freshwater sediment study material. The sediment originated from a river in Belgium and contained PBDEs (and other pollutants) at levels commonly found in environmental samples. The comparison was designed to demonstrate participants' capability of analysing non-polar organic molecules in abiotic dried matrices (approximate range of molecular weights: 100 to 800 g/mol, polarity corresponding to pKow < −2, range of mass fraction: 1–1000 μg/kg). All participants (except one using ultrasonic extraction) applied Pressurised Liquid Extraction or Soxhlet, while the instrumental analysis was performed with GC-MS/MS, GC-MS or GC-HRMS. Isotope Dilution Mass Spectrometry approach was used for quantification (except in one case). The assigned Key Comparison Reference Values (KCRVs) were the medians of thirteen results for BDE 47 and eleven results for BDE 99 and 153, respectively. BDE 47 was assigned a KCRV of 15.60 μg/kg with a combined standard uncertainty of 0.41 μg/kg, BDE 99 was assigned a KCRV of 33.69 μg/kg with a combined standard uncertainty of 0.81 μg/kg and BDE 153 was assigned a KCRV of 6.28 μg/kg with a combined standard uncertainty of 0.28 μg/kg. The k-factor for the estimation of the expanded uncertainty of the KCRVs was chosen as k = 2. KW - Intercomparison KW - Traceability KW - Nation metrology institutes PY - 2017 DO - https://doi.org/10.1088/0026-1394/54/1A/08026 SN - 0026-1394 SN - 1681-7575 VL - 54 SP - 08026, 1 EP - 82 AN - OPUS4-41998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Axel A1 - Becker, Roland A1 - Braun, Ulrike A1 - Dorgerloh, Ute T1 - Einfluss der Alterung auf das Sorptionsverhalten von Mikroplastik, eine Laborstudie mit BTEX und Etherverbindungen T2 - Wasser 2017 Jahrestagung der Wasserchemischen Gesellschaft N2 - Die Präsenz von Mikroplastik in aquatischen Ökosystemen ist ein globales Problem und steht zunehmend im Fokus der Öffentlichkeit. In mehreren Studien konnten Anreicherungen hydrophober, organischer Schadstoffe an MP nachgewiesen werden. Der Einfluss des Alterungszustandes der MP-Partikel auf das Sorptionsverhalten von hydrophoben organischen Substanzen ist nicht hinreichend geklärt. Ziel der vorliegenden Arbeit war die Untersuchung des Sorptionsverhaltens von Schadstoffen mit Bedeutung für limnische Gewässer an künstlich gealterten Partikeln relevanter Polymere. Das Modell verwendete die Aromaten Benzol, Toluol, Ethylbenzol und Xylol (BTEX) sowie Etherverbindungen. Diese Substanzen sind oder waren Bestandteile in unterschiedlichen Kraftstoffen und finden sich daher in vielen aquatischen Ökosystemen weltweit. Als Sorbentien kamen teilkristallines Polypropylen (PP) und amorphes Polystyrol (PS) in Form von Industriepellets zum Einsatz. Die Pellets wurden jeweils sowohl unbehandelt als auch mittels UV-Bestrahlung künstlich gealtert verwendet und mikroskopisch sowie mittels XPS, FTIR und DSC charakterisiert. Die Alterung führte bei PS zu einer verringerten Sorptionskapazität, während bei PP keine Veränderung im Sorptionsverhalten beobachtet wurde. T2 - Wasser 2017 - Jahrestagung der Wasserchemischen Gesellschaft CY - Donaueschingen, Germany DA - 22.05.2017 KW - Mikroplastik KW - Organische Schadstoffe KW - Sorption KW - Polypropylen Polystyrol PY - 2017 SN - 978-3-947197-01-9 SP - 1 EP - 606 PB - Gesellschaft Dt. Chemiker AN - OPUS4-40447 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer-Tenhagen, C. A1 - Johnen, D. A1 - Heuwieser, W. A1 - Becker, Roland A1 - Schallschmidt, Kristin A1 - Nehls, Irene T1 - Odor Perception by Dogs: Evaluating Two Training Approaches for Odor Learning of Sniffer Dogs JF - Chemical Senses N2 - In this study, a standardized experimental set-up with various combinations of herbs as odor sources was designed. Two training approaches for sniffer dogs were compared; first, Training with a pure reference odor, and second, training with a variety of odor mixtures with the target odor as a common denominator. The ability of the dogs to identify the target odor in a new context was tested. Six different herbs (basil, St. John’s wort, dandelion, marjoram, parsley, ribwort) were chosen to produce reference materials in various mixtures with (positive) and without (negative)chamomile as the target odor source. The dogs were trained to show 1 of 2 different behaviors, 1 for the positive, and 1 for the negative sample as a yes/no task. Tests were double blind with one sample presented at a time. In both training approaches, dogs were able to detect chamomile as the target odor in any presented mixture with an average sensitivity of 72% and a specificity of 84%. Dogs trained with odor mixture containing the target odor had more correct indications in the transfer task. KW - dog training KW - herbs KW - reference materials, KW - scent dog KW - smell KW - training model PY - 2017 DO - https://doi.org/10.1093/chemse/bjx020 SN - 1464-3553 SN - 0379-864X VL - 42 IS - 5 SP - 435 EP - 441 PB - Oxford University Press AN - OPUS4-40786 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Elert, Anna Maria A1 - Becker, Roland A1 - Dümichen, Erik A1 - Eisentraut, Paul A1 - Falkenhagen, Jana A1 - Sturm, Heinz A1 - Braun, Ulrike T1 - Comparison of different methods for MP detection: What can we learn from them, and why asking the right question before measurments matters? JF - Environmental Pollution N2 - In recent years, an increasing trend towards investigating and monitoring the contamination of the environment by microplastics (MP) (plastic pieces < 5 mm) has been observed worldwide. Nonetheless, a reliable methodology that would facilitate and automate the monitoring of MP is still lacking. With the goal of selecting practical and standardized methods, and considering the challenges in microplastics detection, we present here a critical evaluation of two vibrational spectroscopies, Raman and Fourier transform infrared (FTIR) spectroscopy, and two extraction methods: thermal extraction desorption gas chromatography mass spectrometry (TED-GC-MS) and liquid extraction with subsequent size exclusion chromatography (SEC) using a soil with known contents of PE, PP, PS and PET as reference material. The obtained results were compared in terms of measurement time, technique handling, detection limits and requirements for sample preparation. The results showed that in designing and selecting the right methodology, the scientific question that determines what needs to be understood is significant, and should be considered carefully prior to analysis. Depending on whether the object of interest is quantification of the MP particles in the sample, or merely a quick estimate of sample contamination with plastics, the appropriate method must be selected. To obtain overall information about MP in environmental samples, the combination of several parallel approaches should be considered. KW - Microplastics KW - FTIR imaging KW - Raman imaging KW - TED-GC-MS KW - SEC KW - Analysis and identification PY - 2017 DO - https://doi.org/10.1016/j.envpol.2017.08.074 SN - 0269-7491 SN - 1873-6424 VL - 231 IS - 2 SP - 1256 EP - 1264 PB - Elsevier AN - OPUS4-42157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mueller, Axel A1 - Becker, Roland A1 - Dorgerloh, Ute A1 - Simon, Franz-Georg A1 - Braun, Ulrike T1 - The effect of polymer aging on the uptake of fuel aromatics and ethers by microplastics JF - Environmental Pollution N2 - Microplastics are increasingly entering marine, limnic and terrestrial ecosystems worldwide, where they sorb hydrophobic organic contaminants. Here, the sorption behavior of the fuel-related water contaminants benzene, toluene, ethyl benzene and xylene (BTEX) and four tertiary butyl ethers to virgin and via UV radiation aged polypropylene (PP) and polystyrene (PS) pellets was investigated. Changes in material properties due to aging were recorded using appropriate polymer characterization methods, such as differential scanning calorimetry, Fourier transform infrared spectroscopy, gel permeation chromatography, X-ray photoelectron spectroscopy, and microscopy. Pellets were exposed to water containing BTEX and the ethers at 130-190 mg/L for up to two weeks. Aqueous sorbate concentrations were determined by headspace gas chromatography. Sorption to the polymers was correlated with the sorbate's Kow and was significant for BTEX and marginal for the ethers. Due to substantially lower glass transition temperatures, PP showed higher sorption than PS. Aging had no effect on the sorption behavior of PP. PS sorbed less BTEX after aging due to an oxidized surface layer. KW - BTEX KW - Polypropylene KW - Polystyrene KW - Sorption KW - Degradation PY - 2018 DO - https://doi.org/10.1016/j.envpol.2018.04.127 SN - 0269-7491 VL - 240 SP - 639 EP - 646 PB - Elsevier CY - Amsterdam AN - OPUS4-44990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dorgerloh, Ute A1 - Becker, Roland A1 - Nehls, Irene T1 - Volatile hydrocarbons in contaminated soil: Robustness of fractional quantification using headspace gas chromatography-mass-spectrometry JF - Soil and sediment contamination N2 - Fuel contamination of soils display complex and variable hydrocarbon mixtures with different volatility and toxicity characteristics. A recently suggested headspace procedure for the structure-based quantification of volatile hydrocarbons is evaluated regarding repeatability, reproducibility, and practical robustness. Three aliphatic and three aromatic fractions covering the boiling range between 69 and 216°C were defined as summation parameters by their respective equivalent carbon number ranges. A standard mixture of 35 aliphatic and aromatic hydrocarbons was used for calibration on basis of selected mass fragments specific for the aliphatics and aromatics, respectively. Two standard soils were fortified with the standard mixture or different fuels, respectively, and submitted to the analytical procedure. Limit of detection (LOD) and limit of quantification (LOQ) were for all fractions lower than 0.1 and 0.3 mg/kg, respectively. Analyte recovery was linear up to between 20 and 110 mg hydrocarbons/kg soil depending on the fraction. Hydrocarbon recovery ranged between 80% and 110% depending on the fraction and the repeatability was typically better than 10%. Finally, the impact of extraction solvent variation, column solid-phase polarity, and alternative summation of fractions were investigated. The procedure was applied to liner samples taken from a site contaminated with aviation fuel and its practicability is discussed. KW - Gasoline KW - Contaminated site KW - Equivalent carbon number KW - Fuel KW - Static headspace PY - 2018 DO - https://doi.org/10.1080/15320383.2018.1418287 SN - 1532-0383 SN - 1549-7887 VL - 27 IS - 1 SP - 1 EP - 12 PB - Taylor & Francis AN - OPUS4-43889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sanchez-Martin, Pedro A1 - Becker, Roland A1 - Toepel, J. A1 - Gorbushina, Anna T1 - An improved test for the evaluation of hydrocarbon degradation capacities of diesel-contaminating microorganisms JF - International Biodeterioration & Biodegradation N2 - The development of a test to evaluate the degradation of semi-volatile fuels as diesel by microorganisms is presented. This method is based on the principles described in the CEC-L-103 Standard procedure that is exclusively meant for testing the biodegradability of non-volatile lubricants. Therefore, significant modifications involve aseptic conditions for testing specific microorganisms and conducting the test in closed vessels avoiding evaporation losses, while fuel quantification using gas chromatography-flame ionization detection (GC-FID) is retained. It is suggested that the modified procedure should enable routine application for semi-volatile hydrocarbon-based fuels. GC-FID provides additionally valuable information on the alteration of fuel component patterns during biodegradation. The procedure was successfully tested using two bacteria (Pseudomonas aeruginosa and Sphingomonas sp.) and two yeasts (Moesziomyces sp. and Candida sp.) isolated from real diesel contamination cases. All tested microorganisms caused a significant degradation of diesel fuel achieving hydrocarbon degradation percentages ranging from 23% to 35%. Specific aspects on the test modification and prospects for further modification regarding targeted investigations in the field of fuel contamination by microorganisms are briefly discussed. KW - Biofouling KW - Bacteria KW - Fungi KW - CEC-L-103 KW - GC-FID KW - Reference organisms PY - 2018 DO - https://doi.org/10.1016/j.ibiod.2018.01.009 SN - 0964-8305 VL - 129 SP - 89 EP - 94 PB - Elsevier AN - OPUS4-44524 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer-Tenhagen, C. A1 - Johnen, D. A1 - Nehls, Irene A1 - Becker, Roland T1 - A Proof of Concept: Are Detection Dogs a Useful Tool to Verify Potential Biomarkers for Lung Cancer? JF - Frontiers in Veterinary Science N2 - Early and reliable diagnostic test is essential for effective therapy of lung cancer. Volatile organic compounds that are characteristic for cancer could serve as valuable biomarkers in cancer diagnosis. Both trace analytical and detection dog approaches give some evidence for the existence of such biomarkers. In this proof of concept, study dogs and trace analysis were implemented in combination to gain more information concerning cancer biomarkers. Two dogs were trained to distinguish between absorbed breath samples of lung cancer patients and healthy persons and succeeded with correct identification of patients with 9/9 and 8/9 and correct negative indications from of 8/10 and 4/10 samples from healthy individuals. A recent observational study found that breath samples from lung cancer patients showed an increase in 1-butanol, 2-butanone, 2-pentanone, and hexanal. Synthetic air samples were therefore fortified with these compounds and adsorbed to a fleece. Tested against breath samples from healthy probands, on presentation to the dogs these synthetic samples provoked an indication in three out of four samples. We were able to demonstrate that a combination of the natural nose of a dog and a trace analytic technique can be a valuable concept in the search for cancer biomarkers. KW - Lung cancer KW - Breath KW - Detection dog KW - Biomarkers KW - Sampling KW - Synthetic air PY - 2018 DO - https://doi.org/10.3389/fvets.2018.00052 SN - 2297-1769 VL - 5 SP - Article 52,1 EP - 6 PB - Frontiers Research Foundation CY - Lausanne AN - OPUS4-44466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Sporkert, F. A1 - Lô, I. A1 - Baumgartner, M. T1 - The determination of ethyl glucuronide in hair: Experiences from nine consecutive interlaboratory comparison rounds JF - Forensic Science International N2 - The increasing request for hair ethyl glucuronide (HEtG) in alcohol consumption monitoring according to cut-off levels set by the Society of Hair Testing (SoHT) has triggered a proficiency testing program based on interlaboratory comparisons (ILC). Here, the outcome of nine consecutive ILC rounds organised by the SoHT on the determination of HEtG between 2011 and 2017 is summarised regarding interlaboratory reproducibility and the influence of procedural variants. Test samples prepared from cut hair (1 mm) with authentic (in-vivo incorporated) and soaked (in-vitro incorporated) HEtG concentrations up to 80 pg/mg were provided for 27–35 participating laboratories. Laboratory results were evaluated according to ISO 5725-5 and provided robust averages and relative reproducibility standard deviations typically between 20 and 35% in reasonable accordance with the prediction of the Horwitz model. Evaluation of results regarding the analytical techniques revealed no significant differences between gas and liquid chromatographic methods In contrast, a detailed evaluation of different sample preparations revealed significantly higher average values in case when pulverised hair is tested compared to cut hair. This observation was reinforced over the different ILC rounds and can be attributed to the increased acceptance and routine of hair pulverisation among laboratories. Further, the reproducibility standard deviations among laboratories performing pulverisation were on average in very good agreement with the prediction of the Horwitz model. Use of sonication showed no effect on the HEtG extraction yield. KW - Ethyl glucuronide KW - Interlaboratory comparison KW - Proficiency testing KW - Society of hair testing KW - Reproducibility KW - Pulverization PY - 2018 DO - https://doi.org/10.1016/j.forsciint.2018.04.025 SN - 0379-0738 SN - 1872-6283 VL - 288 SP - 67 EP - 71 PB - Elsevier AN - OPUS4-44881 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Souza Machado, A. A. A1 - Lau, C. W. A1 - Till, J. A1 - Kloas, W. A1 - Lehmann, A. A1 - Becker, Roland A1 - Rillig, M. C. T1 - Impacts of microplastics on the soil biophysical environment JF - Environmental Science and Technology N2 - Soils are essential components of terrestrial ecosystems that experience strong pollution pressure. Microplastic contamination of soils is being increasingly documented, with potential consequences for soil biodiversity and function. Notwithstanding, data on effects of such contaminants on fundamental properties potentially impacting soil biota are lacking. The present study explores the potential of microplastics to disturb vital relationships between soil and water, as well as its consequences for soil structure and microbial function. During a 5-weeks garden experiment we exposed a loamy sand soil to environmentally relevant nominal concentrations (up to 2%) of four common microplastic types (polyacrylic fibers, polyamide beads, polyester fibers, and polyethylene fragments). Then, we measured bulk density, water holding capacity, hydraulic conductivity, soil aggregation, and microbial activity. Microplastics affected the bulk density, water holding capacity, and the functional relationship between the microbial activity and water stable aggregates. The effects are underestimated if idiosyncrasies of particle type and concentrations are neglected, suggesting that purely qualitative environmental microplastic data might be of limited value for the assessment of effects in soil. If extended to other soils and plastic types, the processes unravelled here suggest that microplastics are relevant long-term anthropogenic stressors and drivers of global change in terrestrial ecosystems. KW - Mikroplastik KW - Einfluß KW - Boden PY - 2018 DO - https://doi.org/10.1021/acs.est.8b02212 SN - 0013-936X SN - 1520-5851 VL - 52 IS - 17 SP - 9656 EP - 9665 PB - American Chemical Society AN - OPUS4-46547 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Andrea A1 - Wander, Lukas A1 - Becker, Roland A1 - Goedecke, Caroline A1 - Braun, Ulrike T1 - High-throughput NIR spectroscopic (NIRS) detection of microplastics in soil JF - Environmental Science and Pollution Research N2 - The increasing pollution of terrestrial and aquatic ecosystems with plastic debris leads to the accumulation of microscopic plastic particles of still unknown amount. To monitor the degree of contamination analytical methods are urgently needed, which help to quantify microplastics (MP). Currently, time-costly purified materials enriched on filters are investigated both by micro-infrared spectroscopy and/or micro-Raman. Although yielding precise results, these techniques are time consuming, and are restricted to the analysis of a small part of the sample in the order of few micrograms. To overcome these problems, here we tested a macroscopic dimensioned NIR process-spectroscopic method in combination with chemometrics. For calibration, artificial MP/soil mixtures containing defined ratios of polyethylene, polyethylene terephthalate, polypropylene, and polystyrene with diameters < 125 µm were prepared and measured by a process FT-NIR spectrometer equipped with a fiber optic reflection probe. The resulting spectra were processed by chemometric models including support vector machine regression (SVR), and partial least squares discriminant analysis (PLS-DA). Validation of models by MP mixtures, MP-free soils and real-world samples, e.g. and fermenter residue, suggest a reliable detection and a possible classification of MP at levels above 0.5 to 1.0 mass% depending on the polymer. The benefit of the combined NIRS chemometric approach lies in the rapid assessment whether soil contains MP, without any chemical pre-treatment. The method can be used with larger sample volumes and even allows for an online prediction and thus meets the demand of a high-throughput method. KW - Microplastics KW - Soil KW - Chemometrics KW - PLS-DA KW - Support vector machines KW - Near Infrared Spectroscopy PY - 2018 DO - https://doi.org/10.1007/s11356-018-2180-2 SN - 1614-7499 SN - 0944-1344 VL - 26 IS - 8 SP - 7364 EP - 7374 PB - Springer AN - OPUS4-45405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian A1 - Iznaguen, Hassan A1 - Traub, Heike A1 - Feldmann, Ines A1 - Köppen, Robert A1 - Witt, Angelika A1 - Jung, Christian A1 - Becker, Roland A1 - Oleszak, Katrin A1 - Bücker, Michael A1 - Urban, Klaus A1 - Reger, Christian A1 - Ostermann, Markus T1 - Bewitterungsszenarien im Vergleich – Veränderungen in der Oberflächenmorphologie von Polypropylen (PP) und Polystyrol (PS) unter dem Aspekt des Austrags von polybromierten Flammschutzmitteln T2 - Umwelteinflüsse erfassen, simulieren, bewerten N2 - Gegenstand der vorzustellenden Arbeiten ist die Prüfung der Umwelt-beständigkeit und -verträglichkeit von Materialien und Produkten hinsichtlich der Emission von potenziellen Schadstoffen in die Umwelt. Hierzu werden chemisch-physikalische Einflüsse (Bewitterung) und mikrobielle Beanspruchungen an Modellmaterialien evaluiert. So werden die Freisetzungsraten von Schadstoffen in Abhängigkeit der Beanspruchung beschrieben. Als Modellmaterialien kommen die Polymere Polystyrol (PS) und Polypropylen (PP) zum Einsatz. Synergistische Effekte der Bewitterungsparameter und der mikrobiologischen Beanspruchung sollen dabei ebenso betrachtet werden, wie die gezielte Alterung. Auch findet eine Beschreibung des Verhaltens der ausgetragenen Schadstoffe in den Umweltkompartimenten Boden oder Wasser statt. Hier sind mit Hilfe der zu entwickelnden Screening- und non-Target-Analyseverfahren die Transformation und der Metabolismus durch Mikroorganismen zu beschreiben. Aus den Ergebnissen sollen Korrelationen zwischen den künstlichen Alterungsverfahren und realen Szenarien abgeleitet werden. T2 - 47. Jahrestagung der GUS CY - Blankenloch-Stutensee, Germany DA - 21.03.2018 KW - Schadstoffaustrag KW - Umweltsimulation KW - Bewitterung PY - 2018 SN - 978-981-18507-2-7 VL - 47 SP - 115 EP - 128 AN - OPUS4-49802 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Roland A1 - Altmann, Korinna A1 - Braun, Ulrike T1 - Querschnittsthema Referenzmaterialien: Planung Ringversuche N2 - Nach einer Erläuterung der international üblichen Definitionen von Referenzmaterialien und Matrix-Referenzmaterialien erfolgt eine Zusammenfassung der spezifischen Anforderungen bei Herstellung und Charakterisierung. Weiterhin werden die unterschiedlichen Anforderungen an die Durchführung von Ringversuchen im Sinne eines Methodenvergleiches, einer Eignungsprüfung von Laboratorien und der Zertifizierung von Matrix-Referenzmaterialien gegenübergestellt. Für den aktuell geplanten ersten Ringversuch zur Quantifizierung von Mikroplastik in Schwebstoffen mittels thermischer Verfahren werden die konkreten technischen Bedingungen zur Herstellung entsprechender Referenzmaterialien einschließlich der Homogenitätsprüfung ihrer Mikroplastikgehalte dargestellt. Die Besonderheiten des Ringversuches vor dem Hintergrund einer Normung der eingesetzten Verfahren werden diskutiert. T2 - Forschungsschwerpunkt „Plastik in der Umwelt – Quellen • Senken • Lösungsansätze“: 2. Workshop des Querschnittsthemas „Analytik und Referenzmaterialien“ CY - Augsburg, Germany DA - 4.7.2018 KW - Mikroplastik KW - Referenzmaterialien KW - Ringversuche KW - Thermische Verfahren KW - Schwebstoffe KW - Methodenvergleich PY - 2018 AN - OPUS4-45681 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sauer, Andreas A1 - Buttler, Sabine A1 - Becker, Roland T1 - Bericht zum 24. BAM-Ringversuch "Altlasten" N2 - Präsentation der Ergebnisse eines Ringversuchs zur Kompetenzbewertung von Prüflaboratorien auf dem Gebiet der anorganischen und organischen Bodenanalytik: Polychlorierte Biphenyle (PCB) in Boden, Mineralölkohlenwasserstoffe (MKW) in Boden, Elemente in Boden und Gesamtcyanid in Boden. KW - Spurenelemente KW - Boden KW - Gesamtcyanid KW - Eignungsprüfung KW - MKW KW - PCB PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-473418 SP - 1 EP - 183 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-47341 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Roland A1 - Altmann, Korinna A1 - Braun, Ulrike T1 - Reference materials for microplastics in environmental matrices N2 - The pollution of marine, limnic and terrestrial environments with plastic waste and the potential impact especially on biota and humans has received increasing attention in recent years. Special focus is on particles smaller than 5 mm, the so-called microplastics. Consequently, possible regulations of emission and remediation efforts require sound information on the occurrence and fate of microplastics in the respective environmental compartments. Microplastics (MP) differ from classical organic pollutants in biota or the environment in that they do not consist of clearly defined low-molecular weight compounds but of polymer particulates with varying sizes and chemical compositions. This leads to specific challenges regarding the analytical techniques to be employed for their identification and quantification. Microplastics are defined as polymer particle in the size range between 1 µm and 5 mm and cover a wide range of polymers such as polyethylene, polypropylene, polystyrene and polyethylene terephthalate in variable geometric shapes. Properties relevant for environmental microplastics are polymer type, particle form and size distribution, surface morphology (aging status) and total mass fraction contained in a given sample. Polymer identification and particle size estimation using optical methods (IR and Raman spectroscopy) are time consuming and complicated by surface characteristics as a result of weathering, soiling, and microbial colonisation. Total mass fractions of MP in environmental samples can be determined by thermo-analytical methods. There are currently no standardised methods for sampling, sampling preparation, or detection of MP in environmental samples. So far, qualitative and quantitative investigations are done by research institutes and have not reached the routine laboratory community. The near future will see harmonisation efforts of MP mass fraction determination in environmental matrices by thermo-analytical procedures. The immediate need for reference materials during method development and comparison is outlined with regard to relevant matrix/polymer compositions, existing regulations and currently achievable detection limits. Examples for solid environmental matrix reference materials are discussed regarding the challenges encountered with matrices and polymer types as well as homogeneity testing and property value characterisation. T2 - BERM 2018 15th International Symposium on Biological and Environmental Reference Materials CY - Berlin, Germany DA - 23 September 2018 KW - Referenzmaterialien KW - Schwebstoffe KW - Sediment KW - Polymer PY - 2018 AN - OPUS4-46209 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholz, Philipp A1 - Wachtendorf, Volker A1 - Elert, Anna Maria A1 - Falkenhagen, Jana A1 - Becker, Roland A1 - Hoffmann, Katrin A1 - Resch-Genger, Ute A1 - Tschiche, Harald A1 - Reinsch, Stefan A1 - Weidner, Steffen ED - Scholz, Philipp T1 - Analytical toolset to characterize polyurethanes after exposure to artificial weathering under systematically varied moisture conditions JF - Polymer Testing N2 - Polyether and -ester urethanes (PU) were exposed to artificial weathering at 40 °C and artificial UV radiation in a weathering chamber. In 3 parallel exposures, humidity was varied between dry, humid, and wet conditions. Material alteration was investigated by various analytical techniques like size exclusion chromatography (SEC), liquid chromatography-infrared spectroscopy (LC-FTIR), thermal-desorption gas chromatography-mass spectrometry (TD-GC-MS), fluorescence mapping and dynamic mechanical analysis (DMA). Our results show that depending on the weathering conditions, different degradation effects can be observed. By means of SEC an initial strong decrease of the molar masses and a broadening of the mass distributions was found. After a material dependent time span this was followed by a plateau where molar mass changes were less significant. A minor moisture-dependent degradation effect was only found for polyester PU. Fluorescence measurements on two materials revealed an increase in the luminescence intensity upon weathering process reaching a saturation level after about 500 h. The changes in the optical properties observed after different exposure conditions and times were very similar. The TD-GC-MS data showed the fate of the stabilizers and antioxidant in the course of weathering. LC-FTIR measurements revealed a change in peak intensities and the ratio of urethane and carbonyl bands. KW - Polyurethane KW - Artificial weathering KW - Moisture KW - Crosslinking KW - Degradation PY - 2019 UR - https://www.sciencedirect.com/science/article/pii/S0142941819303708 DO - https://doi.org/10.1016/j.polymertesting.2019.105996 SN - 0142-9418 VL - 78 SP - 105996, 1 EP - 9 PB - Elsevier CY - Amsterdam AN - OPUS4-48625 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Becker, Roland A1 - Kaiser, Melanie A1 - Dorgeloh, Ute T1 - Hinweis auf den Abbau von FCKW in kontaminiertem Grundwasser bis zur Difluoressigsäure (DFA) N2 - Ein Vergleich der Gehalte von Difluoressigsäure (DFA) und Trifluoressigsäure (TFA) in Regen- und Oberflächenwässern im Berliner Raum ergab ein TFA/DFA Verhältnis in Regenwasser von 10:1. Im Gegensatz dazu wies Grundwasser aus dem Einzugsbereich einer historischen Kontamination durch Fluorchlorkohlenwasserstoffe (FCKW) ein TFA/DFA-Verhältnis von 1:3 auf. Dies und die ungewöhnlich hohe DFA-Konzentration an dieser Stelle wird vor dem Hintergrund der beobachteten mikrobiellen Abbauprodukte des ursprünglichen eingetragenen FCKW 1,1,2-Trichlor-1,2,2-trifluorethan (R113) diskutiert. Eine mikrobielle Umwandlung des bekannten Abbauproduktes Chlortrifluorethylen (R1113) zur DFA wurde bislang nicht in Umweltkompartimenten beobachtet und wird hier auf Basis bekannter Stoffwechselwege vorgeschlagen. TFA wurde in Regenwasser, Oberflächenwasser und Grundwasser in vergleichbaren Größenordnungen von ca. 500 ng/L bestimmt. Im Gegensatz dazu wurde DFA in Grundwasserproben im Bereich der Schadstoffquelle der FCKW-Kontamination mit bis zu 2.000 ng/L nachgewiesen. Die Summe von TFA und DFA im Grundwasser korreliert nicht mit dem Eintrag aus Niederschlag und Oberflächenwasser. Darum liegt die Vermutung nahe, dass es für DFA andere Quellen als den direkten Eintrag oder den möglichen Abbauweg über TFA geben muss. DFA ist vermutlich ein Abbauprodukt von R1113. FCKWs, die im ersten Abbauschritt zu 1,1-Difluorethenen metabolisieren, stehen im Verdacht, in der Folge zu DFA zu hydrolysieren. Entscheidend scheint, dass bereits im Ausgangsprodukt ein CF2-Strukturelement enthalten ist, das dann zur Bildung von DFA führen kann. Somit würde aus dem ursprünglichen Eintrag des Kältemittels R113 über schrittweise Dechlorierung via 1,2-Dichlor-1,2,2-Trifluorethan (R123a) und R1113 die Bildung des beobachteten DFA folgen. Es ist also sinnvoll, DFA in die Diskussion zur Regulierung der Endprodukte des Abbaus fluorhaltiger Kälte- oder Lösungsmittel einzubeziehen. Die Ergebnisse wurden im Normausschuss Wasserwesen (NAW) des DIN vorgestellt und es soll ein Arbeitskreis gegründet werden, der ein Normverfahren zur Quantifizierung von TFA und DFA in Wasser erarbeitet. Interessierte Laboratorien sind herzlich eingeladen, die Normungsarbeit zu unterstützen. T2 - DEHEMA 21. Symposium Strategien zur Sanierung von Boden & Grundwasser 2019 CY - Frankfurt a.M., Germany DA - 25.11.2019 KW - Trifluoressigsäure KW - Difluoressigsäure KW - Grundwasser KW - Fluorchlorkohlenwasserstoffe PY - 2019 AN - OPUS4-49452 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Sauer, Andreas A1 - Bremser, Wolfram T1 - Fifteen years of proficiency testing of total petrol hydrocarbon determination in soil: a story of success JF - Accreditation and Quality Assurance N2 - The total petrol hydrocarbon (TPH) content in soil is determined by gas chromatographic separation and flame ionisation detection according to ISO 16703 in routine laboratories for about 20 years. The development of the interlaboratory variability observed with this analytical procedure over 15 years in a proficiency testing scheme conducted annually with more than 170 participants is evaluated in detail. A significant improvement of the reproducibility standard deviation among participants is observed over the years and attributed to an increasing familiarity with the procedure. Nevertheless, the determination of TPH in the environmentally relevant mass fraction range between 500 mg/kg and 10 000 mg/kg in soils or sediments is far from reaching the reproducibility standard deviations predicted by the Horwitz curve. It is seen that laboratories with sporadic participation tend to report higher bias, while a core group of laboratories participating on a regular basis arrived at reproducibility standard deviations below 20 %. Results from a given laboratory obtained on two different samples tend to be highly correlated in the same PT round indicating a sound repeatability. Expectedly, the within-laboratory correlation between results from consecutive rounds was considerably lower. However, results from consecutive rounds with a temporal distance of 1, 2 or 3 years revealed largely similar correlations which suggests that the within-laboratory reproducibility adjusts to a constant level at least after a period of 1 year. KW - Mineralölkohlenwasserstoffe KW - Boden KW - Ringversuch KW - Gaschromatographie KW - GC-FID KW - Eingnugsprüfung KW - Proficiency Testing PY - 2019 DO - https://doi.org/10.1007/s00769-019-01383-x SN - 0949-1775 SN - 1432-0517 VL - 24 IS - 4 SP - 289 EP - 296 PB - Springer AN - OPUS4-48419 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Souza Machado, A. A. A1 - Lau, C. W. A1 - Kloas, W. A1 - Bergmann, J. A1 - Bachelier, J. B. A1 - Faltin, E. A1 - Becker, Roland A1 - Görlich, A. S. A1 - Rillig, M. C. T1 - Microplastics can change soil properties and affect plant performance JF - Environmental Science and Technology N2 - Microplastics can affect biophysical properties of the soil. However, little is known about the cascade of events in fundamental levels of terrestrial ecosystems, i.e., starting with the changes in soil abiotic properties and propagating across the various components of soil−plant interactions, including soil microbial communities and plant traits. We investigated here the effects of six different microplastics (polyester fibers, polyamide beads, and four fragment types: polyethylene, polyester terephthalate, polypropylene, and polystyrene) on a broad suite of proxies for soil health and performance of spring onion (Allium fistulosum). Significant changes were observed in plant biomass, tissue elemental composition, root traits, and soil microbial activities. These plant and soil responses to microplastic exposure were used to propose a causal model for the mechanism of the effects. Impacts were dependent on particle type, i.e., microplastics with a shape similar to other natural soil particles elicited smaller differences from control. Changes in soil structure and water dynamics may explain the observed results in which polyester fibers and polyamide beads triggered the most pronounced impacts on plant traits and function. The findings reported here imply that the pervasive microplastic contamination in soil may have consequences for plant performance and thus for agroecosystems and terrestrial biodiversity. KW - Mikroplastik KW - Boden KW - Pflanzenwachstum PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-484181 DO - https://doi.org/10.1021/acs.est.9b01339 SN - 0013-936X SN - 1520-5851 VL - 53 IS - 10 SP - 6044 EP - 6052 PB - ACS AN - OPUS4-48418 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dorgerloh, Ute A1 - Becker, Roland A1 - Kaiser, M. T1 - Evidence for the formation of difluoroacetic acid in chlorofluorocarbon-contaminated ground water JF - Molecules N2 - The concentrations of difluoroacetic acid (DFA) and trifluoroacetic acid (TFA) in rainwater and surface water from Berlin, Germany resembled those reported for similar urban areas, and the TFA/DFA ratio in rainwater of 10:1 was in accordance with the literature. In contrast, nearby ground water historically contaminated with 1,1,2-trichloro-1,2,2-trifluoroethane (R113) displayed a TFA/DFA ratio of 1:3. This observation is discussed versus the inventory of microbial Degradation products present in this ground water along with the parent R113 itself. A microbial Transformation of chlorotrifluoroethylene (R1113) to DFA so far has not been reported for environmental media, and is suggested based on well-established mammalian metabolic pathways. KW - Fluoroacetic acid KW - DFA KW - TFA KW - Rainwater KW - Ground water KW - Degradation of refrigerants PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475569 DO - https://doi.org/10.3390/molecules24061039 SN - 1420-3049 VL - 24 IS - 6 SP - 1039, 1 EP - 6 PB - MDPI CY - Basel AN - OPUS4-47556 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Altmann, Korinna A1 - Sommerfeld, Thomas A1 - Braun, Ulrike T1 - Quantification of microplastics in a freshwater suspended organic matter using different thermoanalytical methods – outcome of an interlaboratory comparison JF - Journal of Analytical and Applied Pyrolysis N2 - A sedimented freshwater suspended organic matter fortified with particles of polyethylene (PE), polypropylene (PP), polystyrene (PS), and polyethylene terephthalate (PET) was employed in an interlaboratory comparison of thermoanalytical methods for microplastics identification and quantification. Three laboratories performed pyrolysis gas chromatography-mass spectrometry (Py-GC-MS), three others provided results using thermal extraction desorption followed by gas chromatography coupled to mass spectrometry (TED-GC-MS). One participant performed thermogravimetry-infrared spectroscopy (TGA-FTIR) and two participants used thermogravimetry coupled to mass spectrometry (TGA-MS). Further participants used differential scanning microscopy (DSC), a procedure based on micro combustion calorimetry (MCC) and a procedure based on elemental analysis. Each participant employed a different combination of sample treatment, calibration and instrumental Settings for polymer identification and quantification. Though there is obviously room for improvements regarding the between-laboratory reproducibility and the harmonization of procedures it was seen that the participants Performing Py-GC-MS, TED-GC-MS, and TGA-FTIR were able to correctly identify all polymers and to report reasonable quantification results in the investigated concentration range (PE: 20.0 μg/mg, PP: 5.70 μg/mg; PS: 2.20 μg/mg, PET: 18.0 μg/mg). Although for the other methods limitations exists regarding the detection of specific polymers, they showed potential as alternative approaches for polymer quantification in solid environmental matrices. KW - Interlaboratory comparison KW - Microplastics KW - Suspended organic matter KW - Pyrolysis PY - 2020 DO - https://doi.org/10.1016/j.jaap.2020.104829 VL - 148 SP - 1 EP - 6 PB - Elsevier B.V. AN - OPUS4-50977 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland T1 - Non-invasive cancer detection using volatile biomarkers: Is urine superior to breath? JF - Medical Hypothesis N2 - In recent years numerous reports have highlighted the options of chemical breath analysis with regard to noninvasive cancer detection. Certain volatile organic compounds (VOC) supposedly present in higher amounts or in characteristic patterns have been suggested as potential biomarkers. However, so far no clinical application based on a specific set of compounds appears to exist. Numerous reports on the capability of sniffer dogs and sensor arrays or electronic noses to distinguish breath of cancer patients and healthy controls supports the concept of genuine cancer-related volatile profiles. However, the actual compounds responsible for the scent are completely unknown and there is no correlation with the potential biomarkers suggested on basis of chemical trace analysis. It is outlined that specific features connected with the VOC analysis in breath – namely small concentrations of volatiles, interfering background concentrations, considerable sampling effort and sample instability, impracticability regarding routine application - stand in the way of substantial progress. The underlying chemicalanalytical challenge can only be met considering the severe susceptibility of VOC determination to these adverse conditions. Therefore, the attention is drawn to the needs for appropriate quality assurance/quality control as the most important feature for the reliable quantification of volatiles present in trace concentration. Consequently, the advantages of urine as an alternative matrix for volatile biomarker search in the context of diagnosing lung and other cancers are outlined with specific focus on quality assurance and practicability in clinical chemistry. The headspace over urine samples as the VOC source allows adapting gas chromatographical procedures well-established in water analysis. Foremost, the selection of urine over breath as non-invasive matrix should provide considerably more resilience to adverse effects during sampling and analysis. The most important advantage of urine over breath is seen in the option to partition, dispense, mix, spike, store, and thus to dispatch taylor-made urine samples on demand for quality control measures. Although it is still open at this point if cancer diagnosis supported by non-invasively sampled VOC profiles will ultimately reach clinical application the advantages of urine over breath should significantly facilitate urgently required steps beyond the current proof-of-concept stage and towards standardisation. KW - VOC KW - Breath KW - Urine KW - Lung cancer KW - Volatile organic compounds PY - 2020 DO - https://doi.org/10.1016/j.mehy.2020.110060 VL - 143 SP - 110060 PB - Elsevier Ltd. AN - OPUS4-51066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dorgerloh, Ute A1 - Becker, Roland A1 - Riedel, Juliane A1 - Hofmann, Andrea T1 - Comparison of gas- and liquid chromatography-mass spectrometry for trace analysis of anilines in groundwater JF - International Journal of Environmental Analytical Chemistry N2 - Three chromatographic procedures were investigated regarding their potential for the quantification of aniline and 19 of its methylated and chlorinated derivatives in groundwater. These methods were based on liquid-liquid-extraction in combination with gas chromatography and single quadrupole mass spectrometry (GC/MS) according to German standard DIN 38407-16:1999 and its extension using tandem mass spectrometry (GC/MS-MS), both following liquid-liquid extraction, and as third alternative the direct injection of the water sample into a liquid chromatograph coupled to tandem mass spectrometry (LC/MS-MS). Results were compared using fortified water and real-world contaminated groundwater used in an interlaboratory comparison. It could be shown that GC/MS and GC/MS-MS yielded results deviating less than 10% from each other while all three procedure displayed quantification results deviating less than 15% from the intercomparison reference values in case of each analyte in the concentration range between 1 and 45 µg L-1. Though GC/MS-MS displays a ten-fold higher sensitivity than single quadrupole GC/MS, the precision of both methods in the concentration range was similar. LC/MS-MS has the advantage of no further sample preparation due to the direct injection and leads for methylanilines and meta-, para- substituted chloroanilines to results sufficiently equivalent to the standardised GC/MS method. However, LC/MS-MS is not suitable for ortho-chloroaniline derivates due to significantly lower ion yields than meta- and para-substituted chloroanilines. KW - Interlaboratory comparison KW - Aniline KW - Chloroanilines KW - Methylanilines KW - Groundwater KW - GC/MS KW - GC/MS-MS KW - LC/MS-MS PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-535793 DO - https://doi.org/10.1080/03067319.2021.1987423 VL - 103 IS - 19 SP - 8465 EP - 8477 PB - Taylor & Francis CY - London AN - OPUS4-53579 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Heyn, L. A1 - Jung, Christian T1 - Indoor exposure to airborne polycyclic aromatic hydrocarbons: A comparison of stir bar sorptive extraction and pump sampling JF - Engineering Reports N2 - Stir bar sorptive extraction (SBSE) was compared with standardized pump sampling regarding the prospects to assess airborne levels of polycyclic aromatic hydrocarbons (PAHs) in indoor environments. A historic railway water tower, which will be preserved as a technical monument for museum purposes, was sampled with both approaches because the built-in insulationmaterial was suspected to release PAHs to the indoor air. The 16 PAHs on the US EPA list were quantified using gas chromatography with mass spectrometric detection in filters from pump sampling after solvent extraction and on SBSE devices after thermal desorption. SBSEwas seen to sample detectable PAHmasseswith excellent repeatability and a congener pattern largely similar to that observed with pump sampling. Congener patterns were however significantly different from that in the PAH source because release from the insulation material is largely triggered by the respective congener vapor pressures. Absolute masses in the ng range sampled by SBSE corresponded to airborne concentrations in the ng L−1 range determined by pump sampling. Principle differences between SBSE and pump sampling as well as prospects of SBSE as cost-effective and versatile complement of pump sampling are discussed. KW - Polycyclic aromatic hydrocarbons KW - Adsorption KW - Extraction KW - Indoor air PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537427 DO - https://doi.org/10.1002/eng2.12419 VL - 3 IS - 12 SP - 1 EP - 10 PB - John Wiley & Sons Ltd. AN - OPUS4-53742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ogrinc, N. A1 - Rossi, A. M. A1 - Durbiano, F. A1 - Becker, Roland A1 - Milavec, M. A1 - Bogozalec Kosir, A. A1 - Kakoulides, E. A1 - Ozer, H. A1 - Akcadag, F. A1 - Goenaga-Infante, H. A1 - Quaglia, M. A1 - Mallia, S. A1 - Umbricht, G. A1 - O'Connor, G. A1 - Guettler, B. T1 - Support for a European metrology network on food safety Food-MetNet JF - Measurement: Sensors N2 - This paper describes Food-MetNet, a coordinated preparatory initiative to establish the European Metrology Network on Food Safety (EMN-FS). Food-MetNet aims to establish a long-term ongoing dialogue between the metrology community and relevant stakeholders, in particular, European Union Reference Laboratories (EURLs), National Reference Laboratories (NRLs) and the Joint Research Centre (JRC). This dialogue is meant to support the collection of needs from stakeholders, the take-up of metrological research output and the development of the roadmaps needed to navigate future research. KW - Network KW - Metrology KW - Food KW - Safety KW - Stakeholders PY - 2021 DO - https://doi.org/10.1016/j.measen.2021.100285 VL - 18 SP - 1 EP - 4 PB - Elsevier AN - OPUS4-53740 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sichler, Theresa Constanze A1 - Adam, Christian A1 - Becker, Roland A1 - Sauer, Andreas A1 - Ostermann, Markus A1 - Barjenbruch, M. T1 - Phosphorus determination in sewage sludge: comparison of different aqua regia digestion methods and ICP-OES, ICP-MS and photometric determination JF - Environmental Sciences Europe N2 - Phosphorus recycling from sewage sludge will be obligatory in Germany from 2029. Phosphorus content determination in sewage sludge is crucial to assess the prescribed recycling rates. Currently, German law regards sample preparation using aqua regia digestion in a microwave or under reflux conditions as well as instrumental phosphorus determination by ICP-OES, ICP-MS, or photometric determination with ammonium molybdate as equivalent. However, it is questionable whether these methods are indeed equivalent regarding phosphorus quantification in sludges near the limit of 20 g/kg for mandatory recycling. To answer this question, 15 sewage sludges of 11 different wastewater treatment plants were investigated with all permitted method (digestion and measurement) combinations. Moreover, one sewage sludge was also examined in an interlaboratory comparison (ILC) with 28 participants. This study shows that the above-mentioned methods differ in some cases significantly but across all method combinations and sludges, phosphorus recovery was between 80 and 121% after normalization to the grand mean (average of 15 sludges between 85 and 111%). The ILC and the examination of 15 sludges produced largely similar results. There is a tendency to higher phosphorus recovery after microwave digestion compared to reflux digestion and ICP-OES measurements determine higher phosphorus contents than ICP-MS and photometric phosphorus determination. As a result, the authors recommend ICP-OES determination of phosphorus in sewage sludge after microwave digestion. KW - Sewage sludge KW - ICP-OES KW - Phosphous recovery KW - ICP-MS KW - Photometric P determination KW - Interlaboratory comparison PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-558869 DO - https://doi.org/10.1186/s12302-022-00677-1 VL - 34 IS - 99 SP - 1 EP - 14 PB - Springer AN - OPUS4-55886 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Scholz, Philipp A1 - Jung, Christian A1 - Weidner, Steffen T1 - Thermo-Desorption Gas Chromatography-Mass Spectrometry for investigating the thermal degradation of polyurethanes JF - Analytical Methods N2 - Thermo-Desorption Gas Chromatography-Mass Spectrometry (TD-GC-MS) was used to investigate the thermal degradation of two different polyurethanes (PU). PU samples were heated at different heating rates and the desorbed products were collected in a cold injection system and thereafter submitted to GC-MS. Prospects and limitations of the detection and quantification of semi-volatile degradation products were investigated. A temperature dependent PU depolymerization was found at temperatures above 200 °C proved by an increasing release of 1,4-butanediol and methylene diphenyl diisocyanate (MDI) representing the main building blocks of both polymers. Their release was monitored quantitatively based on external calibration with authentic compounds. Size Exclusion Chromatography (SEC) of the residues obtained after thermodesorption confirmed the initial competitive degradation mechanism indicating an equilibrium of crosslinking and depolymerization as previously suggested. Matrix-Assisted Laser Desorption Ionization (MALDI) mass spectrometry of SEC fractions of thermally degraded PUs provided additional hints on degradation mechanism. KW - Thermo-desorption KW - Mass spectrometry KW - Polyurethanes KW - Thermal degradation PY - 2023 DO - https://doi.org/10.1039/D3AY00173C SN - 1759-9660 SP - 1 EP - 6 PB - Royal Society for Chemistry AN - OPUS4-57307 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lisec, Jan A1 - Recknagel, Sebastian A1 - Prinz, Carsten A1 - Vogel, Kristin A1 - Koch, Matthias A1 - Becker, Roland T1 - eCerto—versatile software for interlaboratory data evaluation and documentation during reference material production JF - Analytical and Bioanalytical Chemistry N2 - The statistical tool eCerto was developed for the evaluation of measurement data to assign property values and associated uncertainties of reference materials. The analysis is based on collaborative studies of expert laboratories and was implemented using the R software environment. Emphasis was put on comparability of eCerto with SoftCRM, a statistical tool based on the certification strategy of the former Community Bureau of Reference. Additionally, special attention was directed towards easy usability from data collection through processing, archiving, and reporting. While the effects of outlier removal can be flexibly explored, eCerto always retains the original data set and any manipulation such as outlier removal is (graphically and tabularly) documented adequately in the report. As a major reference materials producer, the Bundesanstalt für Materialforschung und -prüfung (BAM) developed and will maintain a tool to meet the needs of modern data processing, documentation requirements, and emerging fields of RM activity. The main features of eCerto are discussed using previously certified reference materials. KW - Reference material KW - Statistics KW - Software KW - Collaborative trial PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591851 DO - https://doi.org/10.1007/s00216-023-05099-3 SP - 1 EP - 9 PB - Springer Science and Business Media LLC AN - OPUS4-59185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Groschke, Matthias A1 - Becker, Roland T1 - Comparison of carrier gases for the separation and quantification of mineral oil hydrocarbon (MOH) fractions using online coupled high performance liquid chromatography-gas chromatography-flame ionisation detection JF - Journal of chromatography A N2 - On-line coupled high performance liquid chromatography-gas chromatography-flame ionisation detection (HPLC-GC-FID) was used to compare the effect of hydrogen, helium and nitrogen as carrier gases on the chromatographic characteristics for the quantification of mineral oil hydrocarbon (MOH) traces in food related matrices. After optimisation of chromatographic parameters nitrogen carrier gas exhibited characteristics equivalent to hydrogen and helium regarding requirements set by current guidelines and standardisation such as linear range, quantification limit and carry over. Though nitrogen expectedly led to greater peak widths, all required separations of standard compounds were sufficient and humps of saturated mineral oil hydrocarbons (MOSH) and aromatic mineral oil hydrocarbons (MOAH) were appropriate to enable quantitation similar to situations where hydrogen or helium had been used. Slightly increased peak widths of individual hump components did not affect shapes and widths of the MOSH and MOAH humps were not significantly affected by the use of nitrogen as carrier gas. Notably, nitrogen carrier gas led to less solvent peak tailing and smaller baseline offset. Overall, nitrogen may be regarded as viable alternative to hydrogen or helium and may even extend the range of quantifiable compounds to highly volatile hydrocarbon eluting directly after the solvent peak. KW - Mineral oil hydrocarobons KW - Food KW - Liquid chromatography KW - Gas chromatography KW - MOSH/MOAH PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601450 DO - https://doi.org/10.1016/j.chroma.2024.464946 SN - 0021-9673 VL - 1726 SP - 1 EP - 7 PB - Elsevier CY - New York, NY AN - OPUS4-60145 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -