TY - JOUR A1 - Alasonati, E. A1 - Fabbri, B. A1 - Fettig, Ina A1 - Yardin, C. A1 - Del Castillo Busto, M.E. A1 - Richter, Janine A1 - Philipp, Rosemarie A1 - Fisicaro, P. T1 - Experimental design for TBT quantification by isotope dilution SPE-GC-ICP-MS under the European water framework directive N2 - In Europe the maximum allowable concentration for tributyltin (TBT) compounds in surface water has been regulated by the water framework directive (WFD) and daughter directive that impose a limit of 0.2 ng L-1 in whole water (as tributyltin cation). Despite the large number of different methodologies for the quantification of organotin species developed in the last two decades, standardised analytical methods at required concentration level do not exist. TBT quantification at picogram level requires efficient and accurate sample preparation and preconcentration, and maximum care to avoid blank contamination. To meet the WFD requirement, a method for the quantification of TBT in mineral water at environmental quality standard (EQS) level, based on solid phase extraction (SPE), was developed and optimised. The quantification was done using species-specific isotope dilution (SSID) followed by gas chromatography (GC) coupled to inductively coupled plasma mass spectrometry (ICP–MS). The analytical process was optimised using a design of experiment (DOE) based on a factorial fractionary plan. The DOE allowed to evaluate 3 qualitative factors (type of stationary phase and eluent, phase mass and eluent volume, pH and analyte ethylation procedure) for a total of 13 levels studied, and a sample volume in the range of 250–1000 mL. Four different models fitting the results were defined and evaluated with statistic tools: one of them was selected and optimised to find the best procedural conditions. C18 phase was found to be the best stationary phase for SPE experiments. The 4 solvents tested with C18, the pH and ethylation conditions, the mass of the phases, the volume of the eluents and the sample volume can all be optimal, but depending on their respective combination. For that reason, the equation of the model conceived in this work is a useful decisional tool for the planning of experiments, because it can be applied to predict the TBT mass fraction recovery when the experimental conditions are drawn. This work shows that SPE is a convenient technique for TBT pre-concentration at pico-trace levels and a robust approach: in fact (i) number of different experimental conditions led to satisfactory results and (ii) the participation of two institutes to the experimental work did not impact the developed model. KW - Tributyltin KW - Organotin compounds KW - Solid-phase extraction KW - Experimental design KW - Water framework directive KW - Isotope dilution PY - 2015 DO - https://doi.org/10.1016/j.talanta.2014.11.064 SN - 0039-9140 VL - 134 SP - 576 EP - 586 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-32696 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ressel, P. A1 - Hao, P.H. A1 - Park, M.H. A1 - Yang, Z. C. A1 - Wang, L.C. A1 - Österle, Werner A1 - Kurpas, P. A1 - Richter, E. A1 - Kuphal, E. A1 - Hartnagel, H.L. T1 - Pd/Sb(Zn) and Pd/Ge(Zn) Ohmic Contacts on p-Type Indium Gallium Arsenide: The Employment of the Solid Phase Regrowth Principle to Achieve Optimum Electrical and Metallurgical Properties N2 - The development of two metallizations based on the solid-phase regrowth principle is presented, namely Pd/Sb(Zn) and Pd/Ge(Zn) on moderately doped In0.53Ga0.47As (p=4×1018 cm-3). Contact resistivities of 2–3×10-7 and 6–7×10-7 ?cm2, respectively, have been achieved, where both systems exhibit an effective contact reaction depth of zero and a Zn diffusion depth below 50 nm. Exhibiting resistivities equivalent to the lowest values of Au-based systems in this doping range, especially Pd/Sb(Zn) contacts are superior to them concerning metallurgical stability and contact penetration. Both metallizations have been successfully applied for contacting the base layer of InP/In0.53Ga0.47As heterojunction bipolar transistors. KW - Ohmic contacts KW - Indium gallium arsenide KW - InP/InGaAs heterojunction bipolar transistor KW - Solid-phase regrowth KW - Pd/Ge contacts KW - Pd/Sb contacts KW - Backside secondary ion mass spectrometry (SIMS) PY - 2000 DO - https://doi.org/10.1007/s11664-000-0189-y SN - 0361-5235 SN - 1543-186X VL - 29 IS - 7 SP - 964 EP - 972 PB - TMS CY - Warrendale, Pa. AN - OPUS4-7642 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Matthias A1 - Baldan, A. A1 - Beelen, R. A1 - de Boed, E. J.J. A1 - Tuma, Dirk A1 - Kipphardt, Heinrich A1 - Wilke, Olaf A1 - van der Veen, A. M.H. T1 - Primary gas standards for the determination of sulfur-based impurities at trace level in hydrogen N2 - Hydrogen fuel quality needs to comply with ISO 14687:2025 to avoid harmful impact on applications using proton-exchange membrane (PEM) fuel cells. For total sulfur as one of the most impactful contaminants, an amount fraction of 4 nmol/mol has been set as threshold (so-called Grade D quality). In this study, novel gaseous primary gas standards (PGS) of seven sulfur compounds were prepared either gravimetrically at 1000 nmol/mol, 100 nmol/mol, and 10 nmol/mol, or dynamically diluted down to 4 nmol/mol in hydrogen and argon matrices with relative expanded uncertainties well below 10 % (k = 2) and proven stability of at least 9–12 months. Two different cylinder passivation treatments were compared, with one treatment identified as unsuitable since reactions took place within the mixture. By performing a cross-check study, equivalence between both sets of PGS could be demonstrated (≤ 5 % relative deviation for most of the sulfur species). KW - Hydrogen quality KW - ISO 14687 KW - Sulfur impurities KW - Primary gas standards KW - TD-GC/SCD PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656759 DO - https://doi.org/10.1016/j.ijhydene.2026.154461 SN - 0360-3199 VL - 224 SP - 1 EP - 13 PB - Elsevier Ltd. AN - OPUS4-65675 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -