TY - JOUR A1 - Becker, Roland A1 - Scharf, Holger A1 - Reich, Peter T1 - BAM-Ringversuche "Altlasten" - eine Bilanz PY - 2001 SN - 0942-3818 SN - 1864-8371 IS - 4 SP - 191 EP - 197 PB - Schmidt CY - Berlin AN - OPUS4-1143 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Buge, Hans-Gerhard A1 - Win, Tin T1 - Determination of pentachlorphenol (PCP) in waste wood - method comparison by a collaborative trial N2 - Two independently developed and validated procedures for the determination of pentachlorophenol (PCP) in waste wood were compared by means of a collaborative trial. Both methods foresee quantification of PCP by gas chromatography (GC-ECD) after acetylation and differ with regard to the use of methanol or toluene/sulphuric acid, respectively, as solvent in the sonication extraction step. Test samples with established analyte homogeneity were prepared from a ground “real life” starting material. A total of 23 participating laboratories with experience in wood preservative analysis were instructed to apply both methods to three levels of content in the range of 0.5–20 mg PCP/kg. In case of the toluene/sulphuric acid extraction, lower recoveries and higher interlaboratory dispersion of results at the higher PCP contents were observed. Seen against the background of the Horwitz equation a reproducibility standard deviation of not, vert, similar19% for the methanol extraction at the 4.5 mg/kg level meets the requirement for a sound analytical method. Thus, the sonication extraction procedure with methanol has been annexed as a reference method to the German waste wood regulation. KW - Extraction KW - Derivatisation KW - Sonication KW - Analysis KW - Gas chromatography KW - Regulation PY - 2002 DO - https://doi.org/10.1016/S0045-6535(02)00004-8 SN - 0045-6535 SN - 0366-7111 VL - 47 SP - 1001 EP - 1006 PB - Elsevier Science CY - Kidlington, Oxford AN - OPUS4-1628 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dorgerloh, Ute A1 - Becker, Roland A1 - Freeling, Finnian A1 - Scheurer, Marco A1 - Gökçe, Emine A1 - Strack, Katrin A1 - Sommerfeld, Thomas A1 - Sauer, Andreas A1 - Schneider, Jonas A1 - Härtel, Christoph A1 - Valkov, Vassil A1 - Moser, Lukas A1 - Geiß, Sabine A1 - Junginger, Sabine A1 - Schlittenbauer, Linda A1 - Suess, Elke A1 - Ruth, Katinka T1 - Standardising the quantification of trifluoroacetic acid in water: Interlaboratory validation trial using liquid chromatography-mass spectrometric detection (LC–MS/MS) N2 - The concentration of trifluoroacetic acid in surface and groundwaters and drinking water is subject of increasing concern. Since there is no standardised procedure available, German standardisation body DIN has initiated the first draft standard using liquid chromatography with tandem mass spectrometry (LC–MS/MS) after direct injection for the concentration range between ≥ 0.1 and 3 µg/L. Herein, the interlaboratory comparison as final validation step involving 12 expert laboratories from Germany and Switzerland is described. Two groundwaters, two surface waters, a drinking water, a rainwater, and two fortified groundwater samples displayed relative repeatability standard deviations between 3 and 7% and relative reproducibility standard deviation between 6 and 20% and were included in the draft standard DIN 38407-53. KW - TFA Trifluoroacetic acid KW - LC/MS-MS KW - Validation trial PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-632376 DO - https://doi.org/10.1007/s00769-025-01640-2 SN - 0949-1775 SP - 1 EP - 4 PB - Springer CY - Berlin AN - OPUS4-63237 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 DO - 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 - 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 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 A1 - Koch, Matthias A1 - Lehnik-Habrink, Petra A1 - Nehls, Irene T1 - Quantification of polychlorinated biphenyls in plastic granulates from the recycling of cables - Reference materials and interlaboratory comparison N2 - A procedure for the quantification of the PCB marker congeners 28, 52, 101, 138, 153, 180 in plastic waste form the recycling of cables in the range of content between 0.1 mg kg-1 and 20 mg kg-1 was validated. Representative reference materials for laboratory analyses were produced using granulates from different recycling processes. The method development included aspects of grinding, sieving, homogenising as well as the comparison of extraction methods and chromatographic conditions. The validated procedure foresees grinding of the technical sample to an upper particle size limit of 0.50 mm followed by extraction with an unpolar solvent such as n-hexane and gas chromatographic determination. LOD and LOQ for individual congeners ranged between 0.01 mg kg-1 and 0.08 mg kg-1. Electron capture detection (ECD) and mass selective detection (MS) were equivalent if chromatographic conditions were appropriately selected. The application of MS was advantageous in presence of significant amounts of interfering components which have been found in some cables. Three reference materials containing the marker congeners in the range of 0.1 mg kg-1–5 mg kg-1 were submitted to a final validation intercomparison with 23 selected field laboratories using the developed method. Relative reproducibility standard deviations varied between 15% and 33%. KW - PCB KW - Waste KW - Analysis KW - Method validation KW - Standardisation PY - 2006 DO - https://doi.org/10.1016/j.chemosphere.2006.02.035 SN - 0045-6535 SN - 0366-7111 VL - 65 IS - 9 SP - 1652 EP - 1659 PB - Elsevier Science CY - Kidlington, Oxford AN - OPUS4-14050 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Koch, Matthias A1 - Wachholz, Sigrid A1 - Win, Tin T1 - Quantification of total petrol hydrocarbons (TPH) in soil by IR-spectrometry and gas chromatography - conclusions from three proficiency testing rounds N2 - Due to the utilisation of 1,1,2-trichlorotrifluoroethane (CFE) as extraction solvent the IR-spectrometric determination of total petrol hydrocarbon (TPH) in soil according to ISO/TR 11046 has been replaced by gas chromatography/flame ionisation detection (GC/FID) after extraction with a halogen-free solvent according to ISO/DIS 16703:2001. The results obtained with both methods by field laboratories in three proficiency testing (PT) rounds are compared. The consensus means obtained with GC/FID are typically 10%-20% (ranging between 0% and 25%) higher than those found with IR-spectroscopy. On the contrary, coefficients of variation (CV) are roughly double in case of GC/FID and are briefly discussed against the background of the Horwitz equation. KW - Hydrocarbons KW - Soil KW - IR spectrometry KW - Gas chromatography KW - Interlaboratory comparison PY - 2002 DO - https://doi.org/10.1007/s00769-002-0476-9 SN - 0949-1775 SN - 1432-0517 VL - 7 IS - 7 SP - 286 EP - 289 PB - Springer CY - Berlin AN - OPUS4-1627 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Matthias A1 - Buge, Hans-Gerhard A1 - Becker, Roland A1 - Nehls, Irene T1 - Kalibrierstandard für die Mineralöl (MKW)-analytik mittels GC-FID KW - Kalibrierstand KW - Referenzmaterial KW - MKW KW - GC PY - 2005 SN - 0016-3538 VL - 49 IS - 11 SP - 207 PB - GIT-Verlag CY - Darmstadt AN - OPUS4-11601 LA - deu 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 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 - 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 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 -