TY - CONF A1 - Schultze, Karin A1 - Nehls, Irene A1 - Bremser, Wolfram A1 - Becker, Roland A1 - Win, Tin T1 - Zertifiziertes Referenzmaterial "BAM-U007" - Organochlorpestizide in Boden T2 - ANAKON 2001 CY - Konstanz, Germany DA - 2001-04-04 PY - 2001 SP - 1(?) AN - OPUS4-1314 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Esslinger, Susanne A1 - Becker, Roland A1 - Jung, Christian A1 - Schröter-Kermani, C. A1 - Bremser, Wolfram A1 - Nehls, Irene T1 - Temporal trend (1988-2008) of hexabromocyclododecane enantiomers in herring gull eggs from the german coastal region N2 - Levels of α-, β-, and γ-hexabromocyclododecane (HBCD) were determined in pooled eggs from herring gulls (Larus argentatus) sampled on three bird sanctuaries near the German North Sea coast between 1988 and 2008 (Mellum and Trischen) and the German Baltic Sea coast between 1998 and 2008 (Heuwiese) and archived by the German Environmental Specimen Bank. Pressurized fluid extraction, gel permeation chromatography, and LC–MS/MS using 13C12-labelled isotope standards and a chiral column were applied. α-HBCD was the dominating diastereomer and ranged between 3.7 and 107 ng g-1 lw while β- and γ-HBCD were throughout close to LOQ. The highest α-HBCD concentration was found in eggs from Mellum sampled in the year 2000. Interestingly, HBCD in eggs from the three islands displayed similar time courses with levels increasing to a peak contamination around 2000 and decreasing levels ever since. Chiral signatures of α-HBCD in eggs differed among the islands but indicated a preferential enrichment of the first eluting enantiomer (-)-α-HBCD. KW - Brominated flame retardant KW - Chiral separation KW - HPLC-ESI-MS/MS KW - Enantiomer-specific bioaccumulation PY - 2011 U6 - https://doi.org/10.1016/j.chemosphere.2010.12.047 SN - 0045-6535 SN - 0366-7111 VL - 83 IS - 2 SP - 161 EP - 167 PB - Elsevier Science CY - Kidlington, Oxford AN - OPUS4-23351 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bremser, Wolfram A1 - Becker, Roland A1 - Kipphardt, Heinrich A1 - Lehnik-Habrink, Petra A1 - Panne, Ulrich A1 - Töpfer, Antje T1 - Stability testing in an integrated scheme N2 - ISO Guide 35 deals with RM stability issues and scrutinizes the evaluation of stability testing results under the assumption that either there is no trend at all (a rather rare situation), or any observed deterministic change is insignificant and thus can be neglected. However, market demands for reliable reference materials are obviously not limited to stable or at least seemingly stable materials. In many analytical applications, analytes and measurands under consideration are known, or at least suspected, to be unstable on time scales that may vary widely from measurand to measurand. The Federal Institute for Materials Research and Testing (BAM) has developed (and successfully uses) an integrated approach in its certification practice. The approach is based on an initial stability study and subsequent post-certification monitoring. Data evaluation is model-based and takes advantage of all information collected in the stability testing scheme(s). It thus allows one to deal with any kind of instability observed, to assess limiting time intervals at any stress condition in the range tested, to estimate a final expiry date for materials with detected instabilities or the maximum admissible re-testing interval for seemingly stable materials, and to assess maximum admissible stress loads during delivery of the material to the customer. The article describes (and exemplifies) typical study layout, the model selection, and the integrated data assessment. KW - Certified reference materials KW - Stability KW - Shelf life KW - Arrhenius model KW - ERM PY - 2006 U6 - https://doi.org/10.1007/s00769-006-0152-6 SN - 0949-1775 SN - 1432-0517 VL - 11 IS - 10 SP - 489 EP - 495 PB - Springer CY - Berlin AN - OPUS4-14063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Buge, Hans-Gerhard A1 - Bremser, Wolfram A1 - Nehls, Irene T1 - Mineral oil content in sediments and soils: comparability, traceability and a certified reference material for quality assurance N2 - The performance of twelve laboratories with previously established proficiency in the determination of the mineral oil content in a fresh water sediment is described. The summation parameter total petrol hydrocarbon (TPH) is defined according to ISO 16703:2004 with regard to the sample preparation to be applied, the flame ionisation detection (FID) and the boiling range of C10–C40 to be integrated. Comprehensive tests of homogeneity and stability have been carried out on the candidate material using appropriate models. The outcome of the study served as the basis for the certification of the candidate reference material as ERM-CC015a. The certified mass fraction is 1,820±130mgkg-1 and traceability was established by using an appropriate calibration standard certified for the mass fraction of C10–C40. The interlaboratory scatter of measurement results in this exercise can largely be explained by the variability of the individual calibrations based on this common calibration standard. KW - Total petroleum hydrocarbons KW - Extraction KW - Gas chromatography KW - Calibration KW - Interlaboratory study PY - 2006 U6 - https://doi.org/10.1007/s00216-006-0423-4 SN - 1618-2642 SN - 1618-2650 VL - 385 IS - 3 SP - 645 EP - 651 PB - Springer CY - Berlin AN - OPUS4-12399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dorgerloh, Ute A1 - Becker, Roland A1 - Lutz, A. A1 - Bremser, Wolfram A1 - Hilbert, S. A1 - Nehls, Irene T1 - How to improve reliability in groundwater analysis: over a decade of experience with external quality control in field campaigns on volatile halogenated compounds N2 - The reliability in measurement results obtained during environmental monitoring is crucial for the assessment and further planning of remediation efforts on the respective contaminated sites by the responsible authorities. A case study concerned with groundwater contaminated with perchloroethylene, trichloroethylene and 1,1,2-trichlorotrifluoroethane including their degradation products which involves private contract laboratories and an independent provider of quality assurance (QA) is presented. The experience gained with biannual monitoring campaigns over 14 years indicates that the selection of contractors on basis of accreditation status and successful performance in interlaboratory comparisons are not sufficient. Rather the auditing of the contractors by the QA provider prior to each campaign and the crosschecking of selected monitoring samples by the QA provider led to a lasting improvement of reliability in the contractors' measurement results. A mean deviation of 20% from the reference value determined by the QA provider for the crosschecked samples was reached. KW - Groundwater monitoring KW - External quality management KW - QM KW - VOC PY - 2012 U6 - https://doi.org/10.1039/c1em10460h SN - 1464-0325 SN - 1464-0333 VL - 14 IS - 1 SP - 217 EP - 223 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-25288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Esslinger, Susanne A1 - Becker, Roland A1 - Müller-Belecke, A. A1 - Bremser, Wolfram A1 - Jung, Christian A1 - Nehls, Irene T1 - HBCD stereoisomer pattern in mirror carps following dietary exposure to pure Gamma-HBCD enantiomers KW - Enantiomer-specific determination KW - HPLC-MS/MS KW - Brominated flame retardant KW - Fish feeding experiment KW - Enantiomer fraction KW - Bioisomerization PY - 2010 U6 - https://doi.org/10.1021/jf101469q SN - 0021-8561 SN - 1520-5118 VL - 58 IS - 17 SP - 9705 EP - 9710 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-23173 LA - eng 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 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 U6 - 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 - Zeleny, R. A1 - Voorspoels, S. A1 - Ricci, M. A1 - Becker, Roland A1 - Jung, Christian A1 - Bremser, Wolfram A1 - Sittidech, M. A1 - Panyawathanakit, N. A1 - Wong, W. F. A1 - Choi, S.M. A1 - Lo, K.C. A1 - Yeung, W. Y. A1 - Kim, D.H. A1 - Han, J. A1 - Ryu, J. A1 - Mingwu, S. A1 - Chao, W. A1 - Schantz, M.M. A1 - Lippa, K.A. A1 - Matsuyama, S. T1 - Evaluation of the state-of-the-art measurement capabilities for selected PBDEs and decaBB in plastic by the international intercomparison CCQM-P114 N2 - An international intercomparison involving eight national metrology institutes (NMIs) was conducted to establish their current measurement capabilities for determining five selected congeners from the brominated flame retardant classes polybrominated diphenyl ethers and polybrominated biphenyls. A candidate reference material consisting of polypropylene fortified with technical mixtures of penta-, octa- and decabromo diphenyl ether and decabromo biphenyl, which was thoroughly assessed for material homogeneity and stability, was used as study material. The analytical procedures applied by the participants differed with regard to sample pre-treatment, extraction, clean-up, employed calibrants and type of calibration procedure as well as regarding analytical methods used for separation, identification and quantification of the flame retardant congeners (gas chromatography coupled to an electron capture detector (GC-ECD), gas chromatography-mass spectrometry in the electron ionisation mode (GC-EI-MS), gas chromatography-mass spectrometry in the electron capture negative ionisation mode (GC-ECNI-MS), and liquid chromatography-inductive coupled plasma-mass spectrometry (LC-ICP-MS)). The laboratory means agreed well with relative standard deviations of the mean of means of 1.9%, 4.8%, 5.5% and 5.4% for brominated diphenyl ether (BDE) 47, 183 and 209 and for the brominated biphenyl (BB) congener 209, respectively. For BDE 206, a relative standard deviation of 28.5% was obtained. For all five congeners, within-laboratory relative standard deviations of six measurements obtained under intermediate precision conditions were between 1% and 10%, and reported expanded measurements uncertainties typically ranged from 4% to 10% (8% to 14% for BDE 206). Furthermore, the results are in good agreement with those obtained in the characterization exercise for determining certified values for the flame retardant congeners in the same material. The results demonstrate the state-of-the-art measurement capabilities of NMIs for quantifying representative BDE congeners and BB 209 in a polymer. The outcome of this intercomparison (pilot study) in conjunction with possible improvements for employing exclusively calibrants with thoroughly assessed purity suggests that a key comparison aiming at underpinning calibration and measurement capability (CMC) claims of NMIs can be conducted. KW - Flame retardants KW - Polymer KW - Polybrominated diphenyl ethers (PBDEs) KW - Polybrominated biphenyls (PBBs) KW - International intercomparison PY - 2010 U6 - https://doi.org/10.1007/s00216-009-3314-7 SN - 1618-2642 SN - 1618-2650 VL - 396 IS - 4 SP - 1501 EP - 1511 PB - Springer CY - Berlin AN - OPUS4-22905 LA - eng 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 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 U6 - 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 - JOUR A1 - Scharf, Holger A1 - Becker, Roland A1 - Bremser, Wolfram A1 - Buge, Hans-Gerhard A1 - Lück, Detlef T1 - Certification of the mass fractions of trace elements and pentachlorophenol in an impregnated wood reference material N2 - The resource-saving utilisation of recovered waste wood is a matter of growing concern. In several European countries, this utilisation is governed by regulations and is dependent on the contents of certain trace elements and organic compounds. Thus, for decisionmaking with respect to waste wood management (recycling or combustion), reliable analytical data are needed and, due to their great economic and environmental impact, must be assured by appropriate quality control. To support the improvement in quality assurance in waste wood analysis, for the first time, a wood reference material was certified for its mass fractions of arsenic, cadmium, chromium, copper, lead, mercury, and pentachlorophenol (PCP). These analytes were selected because they represent typical constituents of wood preservatives most widely used in the past. Material preparation and testing of homogeneity and stability were carried out by BAM Federal Institute for Materials Research and Testing. The certification measurements were performed involving selected laboratories with documented expertise in the field of waste wood analysis. The certified values and their corresponding uncertainties were assigned in full compliance with the requirements of ISO Guide 35. The certified mass fractions and their expanded uncertainties (k/i> = 2) are as follows: (3.1 ± 0.5) mg/kg for As, (3.02 ± 0.24) mg/kg for Cd, (36.4 ± 2.6) mg/kg for Cr, (22.9 ± 1.7) mg/kg for Cu, (0.60 ± 0.14) mg/kg for Hg, (39 ± 4) mg/kg for Pb, and (7.9 ± 0.6) mg/kg for PCP. The certified material is available as European Reference Material ERM®-CD100. KW - Waste wood KW - Trace elements KW - Pentachlorophenol KW - Certification KW - European reference material PY - 2010 U6 - https://doi.org/10.1007/s00769-010-0699-0 SN - 0949-1775 SN - 1432-0517 VL - 15 IS - 11 SP - 613 EP - 619 PB - Springer CY - Berlin AN - OPUS4-22392 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 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 -