TY - JOUR A1 - You, Yi A1 - Danischewski, Julia A1 - Molnar, Brian A1 - Riedel, Jens A1 - Shelley, Jacob T1 - Manipulation of Gaseous Ions with Acoustic Fields at Atmospheric Pressure N2 - The ability to controllably move gaseous ions is an essential aspect of ion-based spectrometry (e.g., mass spectrometry and ion mobility spectrometry) as well as materials processing. At higher pressures, ion motion is largely governed by diffusion and multiple collisions with neutral gas molecules. Thus, high-pressure ion optics based on electrostatics require large fields, radio frequency drives, complicated geometries, and/or partially transmissive grids that become contaminated. Here, we demonstrate that low-power standing acoustic waves can be used to guide, block, focus, and separate beams of ions akin to electrostatic ion optics. Ions preferentially travel through the static-pressure regions (“nodes”) while neutral gas does not appear to be impacted by the acoustic field structure and continues along a straight trajectory. This acoustic ion manipulation (AIM) approach has broad implications for ion manipulation techniques at high pressure, while expanding our fundamental understanding of the behavior of ions in gases. KW - Ion mobility spectrometry KW - Acoustic KW - Mass spectrometry PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600704 DO - https://doi.org/10.1021/jacs.4c01224 SP - 1 EP - 6 PB - ACS Publications AN - OPUS4-60070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - van Wasen, S. A1 - You, Yi A1 - Beck, S. A1 - Riedel, Jens A1 - Volmer, D. T1 - Quantitative Analysis of Pharmaceutical Drugs Using a Combination of Acoustic Levitation and High Resolution Mass Spectrometry N2 - A combination of acoustic levitation, laser vaporization, and atmospheric pressure chemical ionization mass spectrometry (APCI-MS) is presented in this study that enabled sensitive analysis of pharmaceutical drugs from an aqueous sample matrix. An unfocused pulsed infrared laser provided contactless sample desorption from the droplets trapped inside an acoustic levitator by activation of the OH stretching band of aqueous and alcoholic solvents. Subsequent atmospheric pressure chemical ionization was used between the levitated droplet and the mass spectrometer for postionization. In this setup, the unfocused laser gently desorbed the analytes by applying very mild repulsive forces. Detailed plume formation studies by temporally resolved schlieren experiments were used to characterize the liquid gas transition in this process. In addition, the role of different additives and solvent composition was examined during the ionization process. The analytical application of the technique and the proof-of-concept for quantitative analysis were demonstrated by the determination of selected pharmaceutical drugs in aqueous matrix with limits of quantification at the lower nanomolar level and a linear dynamic range of 3–4 orders of magnitude. KW - Atmospheric Pressure Chemical Ionization KW - Ultrasonic Levitation KW - Mass Spectrometry KW - Laser Desorption PY - 2021 DO - https://doi.org/10.1021/acs.analchem.1c00762 VL - 93 IS - 15 SP - 6019 EP - 6024 PB - ACS AN - OPUS4-52470 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riedel, Jens A1 - Hufgard, Josefin A1 - You, Yi T1 - LIBS at high duty-cycles: effect of repetition rate and temporal width on the excitation laser pulses N2 - Laser-induced breakdown spectroscopy (LIBS) is becoming a more mature technology every year with new variants such as laser ablation molecular isotopic spectrometry, reheating by various discharge techniques, and multiple pulse excitation schemes, in which sometimes lasers of different pulse lengths are used. However, lasers with inherent parameters like pulse length and repetition rate are still almost exclusively employed. Recent years have witnessed the advent of novel high-repetition-rate laser concepts for machining processes, like welding, milling, and engraving. Here, a comprehensive study of single-pulse LIBS spectra of a single aluminum target is presented to showcase the applicability of flexible high duty-cycle master oscillator power amplifier (MOPA) lasers. Although traditional flashlamp-pumped Fabry–Pérot lasers only permit a variation in the pulse energy and are operated at very low duty-cycles, MOPA lasers add repetition rate and pulse length as variable parameters. A thorough analysis of the temporal plasma behavior revealed the emission dynamic to closely match the excitation laser pulse pattern. An aluminum sample’s spectral response was shown to be significantly impacted by variations in both rate and length. Although the spectral emission strength of the elemental lines of Al, Sr, and Ca all peaked at slightly different parameter settings, the strongest impact was found on the relative abundance of molecular AlO bands. Unlike in previous laser ablation molecular isotopic spectrometry (LAMIS) publications, the latter could be readily detected with a good intensity and well-resolved spectral features without any temporal gating of the detector. This finding, together with the fact that MOPA lasers are both inexpensive and dependable, makes for a promising combination for future studies including the detection of diatomic band structures. KW - Laser-induced breakdown spectroscopy KW - LIBS PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583300 DO - https://doi.org/10.3389/fphy.2023.1241533 SN - 2296-424X VL - 11 SP - 1 EP - 8 AN - OPUS4-58330 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - van Wasen, S. A1 - You, Yi A1 - Beck, S. A1 - Riedel, Jens A1 - Volmer, D. A. T1 - Laser Ablation Secondary Electrospray Ionization for In Situ Mass Spectrometric Interrogation of Acoustically-Levitated Droplets N2 - The composition of acoustically levitated droplets was probed by a novel combination of mid-IR laser evaporation and subsequent postionization via secondary electrospray ionization. The combination of microliter samples and subnanoliter sampling provided time-resolved interrogation of droplets and allowed for a kinetic investigation of the laser-induced release of the analyte, which was found to strongly depend on the analytes. The observed substancespecific delayed release of the analytes permitted baseline-separated discrimination of the analytes, ideal for the study of complex samples. The additionally applied postionization scheme was found to enable efficient detection of small volatile compounds as well as peptides. The detection of small molecules and peptides occurred under very different sampling geometries, pointing to two distinct underlying ionization mechanisms. Overall, our results suggest that the experimental setup presented in this study can serve as a widely applicable platform to study chemical reactions in acoustically levitated droplets as model reactors. KW - Acoustic levitation KW - Mass spectrometry KW - Electrospray KW - Laser ablation PY - 2022 DO - https://doi.org/10.1021/acs.analchem.2c03800 SN - 0003-2700 VL - 2022 SP - 1 EP - 5 PB - ACS Publications CY - Washington AN - OPUS4-56531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Yi T1 - MicroPhase: An Open-Source Flexible Ultrasonic Phased Array Based on Microcontrollers N2 - The use of resonant acoustic fields has gained significant attention due to their capability for contactless manipulation of objects in the open air and other media, referred to as ultrasonic levitation. To overcome the limitations in air-coupling efficiency, Langevin-type ultrasonic transducers are often employed, as they can operate at relatively high power, ranging from several tens to thousands of watts. However, such platforms typically lack the ability to move acoustically trapped objects efficiently, often requiring additional mechanical structures for even basic motion control, such as translation. In contrast, ultrasonic phased arrays offer clear advantages by leveraging their inherent beam-forming capabilities, which allows for dynamic shaping of acoustic fields in situ. Unfortunately, phased array control systems are not readily accessible, particularly when specific geometric or performance criteria must be met. Most commercially available phased array controllers are designed to operate in the MHz range; those are suitable only for high acoustic impedance media, such as water. Conversely, platforms for open-air applications typically utilize ultrasonic speakers operating at 40 kHz. In both cases, these systems are built on field-programmable gate arrays (FPGAs). However, interfacing FPGAs with computers and developing FPGA firmware (e.g., in VHDL) can be technically demanding, and analog components such as power amplifiers further complicate the system design. These limitations severely restrained the use of flexible ultrasonic levitations in analytical chemistry. Here, we present a novel platform for controlling ultrasonic phased arrays using single modern microcontrollers. This platform leverages the connectivity features of microcontrollers, allowing straightforward interfacing with computers via common programming languages (e.g., Python). The system employs fast direct memory access (DMA) to control up-to 256 ultrasonic transducers with a resolution of 0.5 µs, which is suitable for air-based applications in the 20-50 kHz range. Additionally, the platform can interface with traditional Langevin-type transducers, enabling their conversion into phased arrays. Optical characterization of acoustic field optimization is also discussed. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Acoustic ion manipulation PY - 2025 AN - OPUS4-64112 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xue, Boyang A1 - Wang, Zhangjun A1 - Zhu, Tao A1 - Gu, Yezhen A1 - Sun, Weihong A1 - Chen, Chao A1 - Li, Zhigang A1 - Riedel, Jens A1 - You, Yi T1 - High repetition-rate laser-induced breakdown spectroscopy combined with two-dimensional correlation method for analysis of sea-salt aerosols N2 - Laser-induced breakdown spectroscopy (LIBS) offers a tantalizing glimpse into real-time, on-the-spot aerosol analysis. Yet, the reliance on traditional lasers, with their limitations in energy and frequency, hampers optimal sample handling, dissociation, and excitation. To address those challenges, we propose a novel tactic: utilize a high repetition-rate (rep.-rate) laser with low pulse energy in combination with the two-dimensional correlation (2D-corr.) technique for sea-salt aerosols analyses. By examining the emission patterns from both the laser pulse train and individual pulses, we recognize distinctive analyte-specific rep.-rate responses, which allowed spectral reconstruction of analytes, avoiding background interferences. This discovery enabled the rep.-rate modulation for a 2D-corr. spectroscopy workflow. Consequently, we successfully differentiated between particle-related and air-species-related spectral components, obviating expensive spectrometers or intensified image detectors. For instance, the Na I at 589 nm stemming from aerosols exhibited an entirely different correlation contribution compared to O I at 777 nm, resulting in reconstructed clean aerosol-spectra without spectral peaks originated from air species. This 2D-corr. aerosol LIBS approach shows promising analytical potential streamlining aerosol particle analysis. KW - LIBS KW - Aerosol PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613392 DO - https://doi.org/10.1016/j.sab.2024.107048 SN - 0584-8547 VL - 221 SP - 1 EP - 8 PB - Elsevier AN - OPUS4-61339 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, Xunyu A1 - Riedel, Jens A1 - You, Yi T1 - Spectrally resolved lithium isotope quantification through high-resolution spatial heterodyne spectrometry N2 - Isotope ratio determination of lithium is increasingly important in fields ranging from geochemistry to battery diagnostics. While mass spectrometry remains the gold standard, it is costly, cumbersome, and incompatible with portable or inline implementations. Optical emission spectroscopy presents an appealing alternative. However, it is traditionally limited by insufficient spectral resolution or resolving power to separate lithium isotope emissions due to their generalized designs for a wide spectral range; this often requires overly complicated algorithms to overcome the instrumental drawbacks. (79) Results Here, we report a high-resolution optical method for lithium isotope quantification using a custom-built spatial heterodyne spectrometer (SHS) combined with a reduced-pressure glow discharge source. This configuration yielded a resolving power of 189,000 and enabled baseline resolution of lithium d-line emission features even without the need for preliminary data processing. Despite the inherent low sensitivity of SHS, a detection limit of 30 pmol was achieved using a standard industrial camera. To improve quantitative accuracy, we introduced a deconvolution-based spectral lineshape recovery technique alongside a bootstrapping-based error propagation strategy. These methods facilitated robust isotope ratio calibration using both peak-height and peak-area metrics. The SHS platform additionally enabled the determination of relative transition probabilities, suggesting the feasibility of calibration-free operation. This work demonstrates the practical viability of SHS for high-specificity, high-resolution lithium isotope analysis. The approach is compact, potentially field-deployable, and adaptable to other elements with optically resolvable isotope shifts, offering a route toward accessible and calibration-free optical isotopic analyses. KW - SHS KW - Isotope KW - High-resolution spectroscopy PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635139 DO - https://doi.org/10.1016/j.aca.2025.344329 SN - 1873-4324 VL - 1368 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-63513 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohan, M. A1 - Prochazka, D. A1 - You, Yi A1 - Riedel, Jens A1 - Gornushkin, Igor A1 - Rocnakova, I. A1 - Papula, M. A1 - Porízka, P. A1 - Kaizer, J. T1 - Investigating plasma morphology at material boundaries under varying ambient pressures N2 - Laser-Induced Breakdown Spectroscopy (LIBS) is a widely used technique for elemental analysis. The analysis of the obtained LIBS spectra generally assumes plasma homogeneity. However, using focused laser beams for interrogation, LIBS probes materials on the microscale and is, thus, prone to artefacts from sample heterogeneities on the micrometer scale. An ablation at a material boundary of two matrices may result in a significant inhomogeneity in the plasma plume, which can severely impact the accuracy of quantitative analysis. Since this propagation of the surface morphology into the plasma plume is driven by the plasma expansion, its final impact is strongly pressure dependent. This study examines the influence of varying ambient pressures (7–1000 mbar) on plasma morphology, spectral characteristics, and key plasma properties such as electron number density at a well-defined Cu–Sn boundary, in comparison with the results obtained using homogeneous alloys. Several approaches of plasma imaging with bandpass filters, spectroscopy, and Radon transform-based 3D reconstruction were employed to analyze elemental distribution, signal-to-noise (SNR) and signal-to-background (SBR) ratios, as well as electron number densities. The 3D reconstructions revealed a pronounced plasma asymmetry for the ablation at the material boundary, in contrast to the near-axial symmetry observed for the ablation of homogeneous alloys. At lower pressures, this distinct elemental separation in plasma persisted, while higher pressures led to an increased collisional mixing and homogenization. SNR and SBR were consistently lower for ablation at the boundary compared to homogeneous samples. These findings highlight how boundary ablation contributes to plasma inhomogeneities in LIBS analysis of heterogeneous materials and emphasize the need to account for these effects when using LIBS for elemental mapping of fine heterogeneous structures. KW - Laser-induced breakdown spectroscopy KW - Plasma inhomogeneity KW - Plasma tomography KW - Radon transform KW - Material boundaries KW - Ambient pressure effects PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634777 DO - https://doi.org/10.1016/j.talanta.2025.128377 SN - 1873-3573 VL - 295 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-63477 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Yi T1 - Differential Mobility Analysis with Acoustic Ion Manipulation (AIM) N2 - Ion mobility analyses provide complementarity to mass spectrometry in analyte ion identification through the introduction of a higher-pressure separation modality. The recently discovered acoustic ion manipulation (AIM) phenomenon, which exploits unique behaviors of ions in acoustic fields, presents a novel, electric-field-free means to distinguish ions by mobility. In one form of AIM, a static pressure field in an ultrasonic resonator causes a displacement of the ion stream toward the node region, when initially directed toward the antinode. When the static field strength falls below the threshold for all ion deflection, the partitioning reflects ion-specific acoustic mobilities or acoustic radiation impedance. This study demonstrates ion-oriented mobility separation with the AIM approach for mass-spectrometric analysis. An Orbitrap mass spectrometer was used to record ion signal variations as a function of acoustic field strength. An acoustic pressure source with a transducer–reflector configuration was used to generate a standing acoustic wave for partial ion deflection. The drive frequency was swept near resonance to modulate the static pressure field. An alternating-current (AC) plasma discharge source was used to produce an ion beam directed toward an antinode of the resonant structure and later deflected into the mass spectrometer inlet with the acoustic field. Several small molecule analytes, including methanol, ethanol, acetone, and toluene, were doped in the discharge gas to distinguish ions formed in the source from those produced in transit to the MS inlet. An ion beam, offset relative to the inlet capillary of the mass spectrometer, yielded minimal ion detection in the absence of the resonant acoustic field. A sweep of the frequency near resonance induced a low–high–low transition in the static pressure within the resonator. Consequently, the total ion signal as a function of drive frequency resembled a horn gain curve, which is commonly recognized as a key characteristic in ultrasonic transducer design. Maximum ion signal was attained at the resonance frequency, while a pronounced minimum occurred at the anti-resonance frequency. Analysis of drive frequency response curves for distinct ion peaks revealed that source-generated ions displayed a congruent pattern to the overall ion count, thereby suggesting the formation of clusters prior to the vacuum region of the mass spectrometer. A finer frequency scan near the resonance region differentiated these clusters. For instance, response curves for toluene-related ions are slightly deviated from those associated with alcohols. Notably, a series of ions, presumably originating from an identical chemical precursor, manifested an entirely distinctive drive frequency response; their maximal signal occurred at a frequency not associated with any characteristic of the acoustic system or its electronics. The frequency response curves of the ions allowed implementation of a modified cross-correlation (mXcorr) algorithm to categorize ions according to chemical origin or clustering. The use of frequency, rather than the transducer voltage/power, offers the advantage of electronically measuring the horn gain curve in tandem with ion-specific analysis. This gain curve subsequently serves as a reference to decode latent chemical information for enhanced analytical accuracy. T2 - ASMS 2025 Conference CY - Baltimore, MA, USA DA - 01.06.2025 KW - Acoustic Ion Manipulation KW - Mass Spectrometry PY - 2025 AN - OPUS4-63512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Jens T1 - LIBs–trends and developments for recycling applications N2 - Recent years have brought up many challenges for an analytical tracing of material flows. While planetary boundaries force end of life material into circular recycling pathways, geopolitical tension creates demands regarding the origin of raw materials. The analytical demands on any instrumentation to tackle the arising challenges of this scenario are straight forward: No sample preparation, precision in the percentage region, and high throughput at comparably low cost. All these demands make LIBS a perfect candidate, why it is time for a re-evaluation of how it exploits the potential possibilities arising from todays’ technology. While being a relatively young technique, the vast majority of conducted LIBS experiments still relies on well established instrumentation, sometimes ignoring the innovations and breakthroughs in the development of its empowering technology sectors such as battery powered compact high repetition rate lasers with tuneable pulse rate and length, low priced cameras with millions of small sized pixels and extremely fast shutter and readout times, optical modulators, galvonometer scanners, and simple robotics. In this talk we will showcase some examples on how the implantation of all these new tools can lead to extremely affordable and compact instrumentation with unprecedented acquisition speed and a spectral resolution sufficient to resolve atomic isotope lines. T2 - Institute Seminar CY - Rostock, Germany DA - 09.01.2024 KW - LIBS KW - Sorting KW - Automatisation PY - 2024 AN - OPUS4-62136 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Palásti, Dávid jenö T1 - Interferometric sensing in the UV range – Investigation and comparison of the all-reflective spatial heterodyne spectrometer designs N2 - Spatial heterodyne spectrometers (SHS) are optical interferometric devices, working in the UV and visible spectral ranges [1]. The most common SHS setup is similar to the Michelson interferometer, both utilizes a beam splitter in the incoming beam path. In case of the SHS the split beams are not aimed towards orthogonal mirrors, but reflective optical gratings, set under a selected angle. These optical gratings diffract the beams, the direction of every wavelength will depend on the grating constant and the angle of the gratings. The wavefronts belonging to different wavelengths are going to cross each other under a unique angle, resulting in a spatial interference, which is recorded by a digital camera. This relatively compact setup provides high resolution and light throughput, which properties were harnessed for tasks requiring good line separation and/or high sensitivity [2]. However, SHS are only applicable on wavelengths for which an adequate transmissive beam splitter is available like the visible range, but not the far UV. To overcome this limitation, different all-reflective designs were introduced [3]. These instruments utilize symmetric optical gratings for the splitting and recombination of the beams. Although these SHS devices solve the main limitations of the traditional ones, they come with their fair share of drawbacks as well, such as more complex arrangement and the requirement for more delicate tuning. The behaviour of the traditional SHS is well documented [4,5], but in regards of the all-reflective ones we have much less available information. In this current study we utilized computational modelling to predict the behaviour of the all-reflective SH spectrometers, with special attention to the effects of the different alignment errors. Later we utilize this knowledge to fine tune an SHS for sensing (LIBS, Raman) in the UV region. Furthermore, we are introducing two new all-reflective SHS setups and compering them to their older counterparts. T2 - 20th European Winter Conference on Plasma Spectroscopy CY - Berlin, Germany DA - 02.03.2025 KW - SHS KW - Spectroscopy PY - 2025 AN - OPUS4-63553 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - You, Yi A1 - Xue, Boyang A1 - Riedel, Jens T1 - Enhancement of LIBS plasma in air with organic solvent vapors N2 - Laser-induced breakdown spectroscopy (LIBS) offers versatile, field-deployable elemental analysis; however, compact, high-repetition-rate nanosecond laser systems typically face constraints in power consumption and size, often compromising emission intensity and thus analytical performance. We demonstrate a significant improvement in LIBS signals through the controlled introduction of common organic solvent vapors into a sheath gas, with a diode-pumped solid-state laser (1064 nm, 2–28 kHz repetition rate, 450–600-μJ pulse energy). Optical and acoustic diagnostics reveal up to ca. 40-fold enhancement of the N II emission line at 567 nm when ambient air serves as the analyte. Maximal enhancement occurs at intermediate repetition rates of ca. 15 kHz, particularly at pulse energies approaching the optical breakdown threshold; this observation suggests a viable strategy for operating LIBS at lower pulse energies and higher repetition rates. Enhancement effects scale jointly with both vapor pressure and ionization energy of the organic species, with acetone and toluene markedly outperforming methanol and isopropanol. These findings provide a rational foundation for significantly improving the analytical performance of portable LIBS instruments without exceeding platform-specific constraints. KW - LIBS PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653758 DO - https://doi.org/10.1016/j.sab.2025.107309 SN - 0584-8547 VL - 236 SP - 1 EP - 6 PB - Elsevier B.V. AN - OPUS4-65375 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hufgard, Josefin T1 - Traveling Wave Acoustic Ion Manipulation (AIM) for Ion Trajectory Alteration N2 - Acoustic ion manipulation (AIM) is a recent discovery reliant on the sound-ion interactions under ambient conditions. Instead of relying upon conventional electric or magnetic fields, this technique initially exploits standing acoustic waves to focus, gate, deflect, and separate ions. Compared to AIM in a standing wave scenario, the transportation of ions and their response to traveling acoustic waves remain less understood. In contrast to standing waves, which establish stationary pressure domains, traveling waves engender continuously propagating pressure variations. Here, we report on AIM effects induced by traveling acoustic waves that occur from a single-transducer setup. The changes in ion trajectory induced by acoustic traveling waves, ion-specific responses to the traveling wave and its analytical applications will be investigated. A home-built alternating-current (AC) plasma source was used to produce a laminar ion stream, positioned ~10 cm from the inlet capillary of an Orbitrap mass spectrometer. A Langevin-type ultrasonic transducer operated at 40 kHz and ~50 W was used to introduce a diverging sound gradient arranged perpendicular to the ion beam direction. Small model analytes, such as methanol, isopropanol, and acetone, were doped in the discharge gas flow as traces produced in the source, to differentiate from ions produced between the source and MS inlet capillary. Aerodynamic information on both the sound field and the gas stream is provided by defocusing shadowgraphy images. T2 - ASMS 73rd Conference on Mass spectrometry and Allied topics CY - Baltimore, Maryland, USA DA - 01.06.2025 KW - Mass spectrometry KW - Acoustic Ion Manipulation (AIM) KW - Traveling acoustic wave PY - 2025 AN - OPUS4-63380 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hufgard, Josefin T1 - Use Your Time (Domain) Wisely: Streamlined Analysis of Complex Mixtures with Pulsed-Laser Techniques N2 - This study aims to streamline complex mixture analysis through the parallel ionization of all analytes without extensive preprocessing. Here, pulsed laser ablation of single droplets is used with modified cross-correlation, a phase-sensitive algorithm. This combined method allows contactless chemical investigation with minimal sample pretreatment, as well as the separation of analytes in mixtures and reconstruction of analyte-specific mass spectra. T2 - SciX 2024 CY - Raleigh, NC, USA DA - 20.10.2024 KW - MS KW - Data analysis KW - Laser ablation PY - 2024 AN - OPUS4-62120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Anwendung von hochauflösender optischer Spektrometrie zur Lithium-Isotopenanalyse N2 - Optische Spektrometrie wird als Alternative zur Massenspektrometrie im Bereich der Lithium-Isotopenanalyse vorgestellt. T2 - 11. Analytische Tage CY - Idstein, Germany DA - 11.05.2023 KW - Lithium KW - Isotopenanalyse KW - Atomabsorptionsspektrometrie KW - Massenspektrometrie PY - 2023 AN - OPUS4-57543 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hufgard, Josefin T1 - Use Your Time (Domain) Wisely: Streamlined Analysis of Complex Mixtures with Pulsed-Laser Techniques N2 - Analyzing complex mixtures with mass spectrometry (MS) usually requires extensive sample preprocessing and separation techniques such as high-pressure iquid chromatography (HPLC). This approach allows for subsequent detection of one analyte at a time but at a cost of throughput. Recently, increasing attention has been put on thesimultaneous ionization of all analytes in complex mixtures without extensive preprocessing, aiming to streamline the analysis process while accepting a compromise in identification. Such methods are commonly referred to as direct mass-spectrometric analysis. Among those, pulsed laser-based ablation, allows for contactless chemical investigation and reaction monitoring in situ, with minimal sample pretreatments. Specifically, the mid-infrared lasers encompass the fundamental vibrational resonances of typical biological matrices and solvents; their use results in efficient material removal from the bulk phase. Interestingly, the resulting analyte chronograms during the ablation process showed that the analytes were not detected concomitantly. Instead, chronograms offered time-domain information by being detected at different timestamps. It is certain that chemical information is encoded in the time domain. However, the analyte-specific chronograms could be difficult to interpret with conventional workflows as they mostly overlap. In this study, we aim exploiting the commonly discarded information in the time domain as an orthogonal dimension to the m/z domain, achieving ategorization and grouping mass-spectral peaks according to their chemical origins. Here, we applied a pulsed diode-pumped solid-state (DPSS) laser at 3-μm wavelength to 10 μL hanging droplets of analyte. A secondary electrospray ionization (SESI) source was built in-house to ionize ablated analytes. With a model sample, i.e. a mixture of two antibiotics, remarkable differences in their chronograms were observed. In fact, the time-domain information reflects the chemical signature of the analytes and can provide an additional data dimension for accurate interpretation. With a phase-sensitive algorithm, the modified cross-correlation (mXcorr), the similarity between chronograms can be gauged. Consequently, mass-spectral peaks that shared the same chronogram features were grouped together, yielding analyte-specific mass spectra that can aid analyte identification. Lastly, the applicability for biological samples, such as peptides, will be discussed. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Mass specrometry KW - Laser Ablation KW - secondary ionization PY - 2024 AN - OPUS4-62733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blume, Simon T1 - Femtosecond vs. Nanosecond Laser-induced XUV Spectroscopy (LIXS) N2 - In contrast to laser-induced breakdown spectroscopy (LIBS), measuring after a delay as long as a few microseconds, laser-induced XUV spectroscopy (LIXS) takes advantage of emissions from the very first instant of the pristine plasma. This process exhibits stable and intense line and recombination emissions in the XUV-range. Therefore, common challenges for precise measurements (e.g. quantification efforts) in LIBS caused by signal intensity fluctuations due to matrix effects and plasma-flicker noise are improved, as shown for ns-pulses. A femtosecond laser (pulse length ~100 fs) interacts fundamentally different with matter than a nanosecond laser. Of the many photons needed for ionization of the sample, less are absorbed via inverse Bremsstrahlung and more in a Franck-Condon multiphoton absorption (MPA) process. In combination with the higher peak power, and therefore higher initial plasma temperature (> 10 eV), atoms are selectively ionized to a higher degree while at the same time thermal dissipation and equilibration is reduced. This specificity in excitation leads to a reduced background and the highly ionized atoms overwhelmingly emit the desired XUV-radiation. Thus, fs-LIXS promises to lead to “cleaner” spectra with sharper separation of the emission lines. The capabilities of a fs-LIXS setup in comparison to ns-LIXS will be discussed. Samples of pure elements (Al, Si, Ni, Fe, Mg), as well as composite samples (CaF, LiF, PTFE, polypropylene) serve as model systems to demonstrate these capabilities. T2 - EMSLIBS 2025 CY - Senlis, France DA - 26.01.2026 KW - Femtosecond KW - LIXS KW - XUV KW - Elemental analysis PY - 2026 AN - OPUS4-65470 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sander, Luise T1 - Multi-Scale Analysis of Commercially Available Sodium-Ion Cells N2 - As the first commercial sodium-ion-batteries (SIBs) are available for purchase, it is possible to investigate material composition. Gaining an insight into the material composition of these SIBs is of interest not only for the classification of possible safety risks and hazards, but also in regards to recycling. Herein we report the preliminary investigations of the chemical and structural composition of first commercial SIB-cells. Two different SIB-cells with different specification were compared regarding electrode size, thickness and further parameters. Furthermore, the composition of the active materials and electrolyte was investigated and compared. T2 - Solid State Ionics (SSI) CY - London, United Kingdom DA - 15.07.2024 KW - Sodium Ion-Cells KW - Multi-Scale PY - 2024 AN - OPUS4-60764 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Palásti, Dávid Jenö T1 - Utilizing modern fiber lasers for LIBS N2 - The development of laser sources plays a very important role in the quick advancements in the field of LIBS. However, the development of fiber lasers went mostly unnoticed by the wider LIBS community. These laser sources, traditionally used in industrial cutting and welding processes, despite their high-power output (hundreds of watts) and are very robust nature, were neglected, because they used to work only in continuous mode. Modern fiber lasers however, offer pulsed output with a couple of mJ-s pulse energy, which can be adequate for certain tasks [1,2]. Furthermore, the pulse duration and the pulse repetition rate can be varied in a reasonably wide range, while their price is a fraction of the ones traditionally used in research. In the recent years, our groups made experiences with modern fiber lasers to evaluate the feasibility of their usage in LIBS. The initial experiments proved that they are not just suitable for standard analytical tasks such as quantitative or qualitative analysis, but their unique set of features makes them capable for fundamental research, like no other laser sources currently on the market. The relatively low energy and elongated profile of the pulses are very efficient in ablation and in the generation of low temperature plasmas [3], which means the ionic lines are less numerous, while the emission is mostly free from the background emission typical for the early stages of the plasma lifetime. It can make spectrometer gating and signal integration much simpler and robust. A thorough set of investigations of single pulse, double pulse and even continuous irradiation experiments was performed. The effects of various parameters, such as energy, duration and shape of the pulse as well as inter pulse delay were investigated on the generated signal focusing mainly the signal intensity, the self-absorption and the width of the peaks as well as the plasma properties. T2 - EMSLIBS 2026 CY - Senlis, France DA - 26.01.2026 KW - LIBS KW - Fiber laser PY - 2026 AN - OPUS4-65561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Soraya T1 - Application of 3,3’,5,5’-Tetramethylbenzidine (TMB) in Amperometric Immunoassays for Mycotoxin Detection N2 - Electrochemical methods make great promise to meet the demand for user-friendly on-site devices for monitoring important parameters. Food industry often runs own lab procedures, e.g., for mycotoxin analysis, but it is a major goal to simplify analysis, linking analytical methods with miniaturized technologies. Enzyme-linked immunosorbent assays, with photometric detection of the horseradish peroxidase (HRP) substrate 3,3’,5,5’-tetramethylbenzidine (TMB), form a good basis for sensitive detection. To provide a straight-forward approach for the miniaturization of the detection step, we have studied the pitfalls of the electrochemical TMB detection. By cyclic voltammetry, it could be shown that TMB electrochemistry is strongly dependent on the pH and the electrode material. It was found that screen-printed gold electrodes and a very low pH value (pH 1) are well-suited to perform the electrochemical detection of TMB, due to the reversible character of the redox reaction under these conditions. Under these conditions, a good signal stability over several measuring cycles is achieved, providing the basis for analyzing multiple samples. In contrast to this, for carbon screen-printed electrodes, it was found that the signal response has changed after the electrochemical reaction with TMB at pH 1. At moderately acidic conditions (pH 4), neither with carbon nor with gold electrodes a reproducible electrochemical detection of TMB could be achieved. Based on these findings, we created a smartphone-based, electrochemical, immunomagnetic assay for the detection of ochratoxin A (OTA) and ergometrine in food samples. A competitive assay is performed on magnetic beads using HRP and TMB/H2O2 to generate the signal. Enzymatically oxidized TMB is quantified after addition of H2SO4 by amperometry with screen-printed gold electrodes in a custom-made wall-jet flow cell. The results are in good correlation with the established photometric detection method, providing a solid basis for sensing of further analytes in HRP-based assays using the newly developed miniaturized smartphone-based, electrochemical, immunomagnetic assay. T2 - 73rd Annual Meeting of the ISE CY - Online meeting DA - 12.09.2022 KW - Cylic Voltammetry KW - Immunoassay KW - Mycotoxins KW - Amperometry KW - Electrochemistry PY - 2022 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-55793 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Soraya T1 - Steps Forward in the Application of 3,3’,5,5’- Tetramethylbenzidine (TMB) in Amperometric Assays N2 - Electrochemical methods make great promise to meet the demand for user-friendly on-site devices for monitoring important parameters. Food industry often runs own lab procedures, e.g. for mycotoxin analysis, but it is a major goal to simplify analysis, linking analytical methods with miniaturized technologies. Enzyme-linked immunosorbent assays, with photometric detection of the horseradish peroxidase (HRP) substrate, 3,3’,5,5’-tetramethylbenzidine (TMB), form a good basis for sensitive detection. To provide a straight-forward approach for the miniaturization of the detection step, we have studied the pitfalls of the electrochemical TMB detection. By cyclic voltammetry it was found that the TMB electrochemistry is strongly dependent on the pH and the electrode material. It was found that screen-printed gold electrodes and a highly acidic pH value (pH 1) are well-suited to perform the electrochemical detection of TMB, due to the reversible character of the redox reaction under these conditions. This set-up provides a good signal stability over several measuring cycles, providing the basis for analysing multiple samples. In contrast to this, for carbon screen-printed electrodes, it was found that the signal response has changed after the electrochemical reaction with TMB at pH 1. At a weakly acidic pH value (pH 4), neither with carbon nor with gold electrodes a reproducible electrochemical detection of TMB could be achieved [1]. Based on these findings we created a smartphone-based, electrochemical, immunomagnetic assay for the detection of ochratoxin A and ergometrine in real samples. Therefore, a competitive assay was performed on magnetic beads using HRP and TMB/H2O2 to generate the signal. Enzymatically oxidized TMB was quantified after addition of H2SO4 by amperometry with screen-printed gold electrodes in a custom-made wall-jet flow cell. The results are in good correlation with the established photometric detection method, providing a solid basis for sensing of further analytes in HRP-based assays using the newly developed miniaturized smartphone-based, electrochemical, immunomagnetic assay. T2 - Electrochemistry 2022 CY - Berlin, Germany DA - 28.09.2022 KW - Cylic Voltammetry KW - Immunoassay KW - TMB KW - Amperometry PY - 2022 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-55876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bayerlein, Bernd A1 - Hanke, T. A1 - Muth, Thilo A1 - Riedel, Jens A1 - Schilling, Markus A1 - Schweizer, C. A1 - Skrotzki, Birgit A1 - Todor, A. A1 - Moreno Torres, Benjami A1 - Unger, Jörg F. A1 - Völker, Christoph A1 - Olbricht, Jürgen T1 - A Perspective on Digital Knowledge Representation in Materials Science and Engineering N2 - The amount of data generated worldwide is constantly increasing. These data come from a wide variety of sources and systems, are processed differently, have a multitude of formats, and are stored in an untraceable and unstructured manner, predominantly in natural language in data silos. This problem can be equally applied to the heterogeneous research data from materials science and engineering. In this domain, ways and solutions are increasingly being generated to smartly link material data together with their contextual information in a uniform and well-structured manner on platforms, thus making them discoverable, retrievable, and reusable for research and industry. Ontologies play a key role in this context. They enable the sustainable representation of expert knowledge and the semantically structured filling of databases with computer-processable data triples. In this perspective article, we present the project initiative Materials-open-Laboratory (Mat-o-Lab) that aims to provide a collaborative environment for domain experts to digitize their research results and processes and make them fit for data-driven materials research and development. The overarching challenge is to generate connection points to further link data from other domains to harness the promised potential of big materials data and harvest new knowledge. KW - Data infrastructures KW - Digital representations KW - Digital workflows KW - Knowledge graphs KW - Materials informatics KW - Ontologies KW - Vocabulary providers PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546729 DO - https://doi.org/10.1002/adem.202101176 SN - 1438-1656 SP - 1 EP - 14 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-54672 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas A1 - Hodoroaba, Vasile-Dan T1 - Correlative Analysis by Raman and other Micro & Nanospectroscopic Imaging Techniques N2 - In the present talk the basics of the Raman spectroscopy and particularly of Raman microscopy are explained. Advantages and disadvantages of the method are highlighted through selected case studies. In the second part of the lecture examples of correlative imaging with electron, X-ray, ion and optical microscopies from micro- to the nanoscale are highlighted. T2 - Charisma School on Raman Harmonisation CY - Turin, Italy DA - 19.10.2022 KW - Raman KW - Correlative Imaging KW - Microscopy KW - Hyperspectral imaging PY - 2022 UR - https://amdgroup.inrim.it/events/vamas-sc-meeting-47/program-sc47 AN - OPUS4-56094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, Xunyu A1 - Riedel, Jens A1 - You, Yi T1 - Determination of broadband-light atomic absorption through interferometric spectrometry with a spatial heterodyne spectrometer N2 - A spatial heterodyne spectrometer (SHS) was combined with a flame atomic absorption (FAA) setup to reveal the analytical potential of SHS to be used as a tool for high-resolution atomic absorption studies. Exploiting the advances in modern computational power, the spectral information encoded in the interferograms was extracted and separated. Consequently, unseeable interferometric ingredients corresponding to narrow-band absorption lines could be recognized. Namely, a single SHS absorption interferogram simultaneously contains both illumination background and absorption information, which can be distinguished through a series of computational steps. In the examples given by this work, we demonstrate the construction of Na absorbance spectra from a single image. The described single-image approach can be used to investigate highly dynamic systems, whereby background collections can be obviated. KW - Optical Spectrometry KW - Spatial Heterodyne Spectrometry KW - Atomic Absorption PY - 2023 DO - https://doi.org/10.1039/D2JA00367H VL - 38 IS - 5 SP - 1088 EP - 1096 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58332 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Erfahrungsaustausch Labor-Robotik N2 - Die BAM setzt in ihren analytischen Labors zunehmend Labor-Robotik ein, um gefähliche oder zeitraubende Routineaufgaben zu automatisieren. Durch Automation kann auch die Reproduzierbarkeit solcher Anwendungen erhöht werden. Im Beitrag werden einige aktuelle Beispiele aus den Analytiklabors diskutiert, wie z. B. die Anwendung für die Herstellung und RFA-Analytik von Gläsern, eine Feinwäge-Robotik für 10-L-Gaszylinder im Rahmen der Herstellung von Primärnormalen oder die Automatisierung von Probenpräsentationen für optische Spektroskopie und chemical Imaging. Auch wird kurz auf den Einsatz von Speicherprogrammierbaren Steuerungen in der modularen Laborautomation und die Virtualisierung von analytischen Laborrechnern eingengangen. T2 - Industrienetzwerk Smartes Labor am Institut für Energie- und Umwelttechnik e.V. (IUTA) CY - Duisburg, Germany DA - 09.11.2022 KW - Laborautomation KW - Labor-Robotik KW - Automatisierung KW - Smartes Labor PY - 2022 AN - OPUS4-56227 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Yi T1 - Acoustic Ion Manipulation (AIM) N2 - The precise control of gaseous ions is a cornerstone in ion-based spectrometry and other disciplines such as materials processing. Traditional high-pressure ion optics rely on electrostatic and magnetic fields that often demand the use of intense electric fields, radio frequency activation, complex geometrical arrangements, or partially transmissive grids. Consequently, the efficiencies of such devices tend to be low or they require large footprints, as ion motions under ambient conditions are governed aerodynamically by collisions and fluid dynamics. However, from a different perspective and holistic reasoning, the limitations posed by collisions, aerodynamics, and other factors that hinder ion control in the open-air suggested an innovative direction for ion manipulation. Our study introduces a novel method that employs low-power standing acoustic waves to effectively manipulate ion beams. We observe that ions distinctively prefer traveling through areas of static pressure within the acoustic field, identified as "nodes." In contrast, neutral gases are unaffected by the acoustic field structure and continue to move along a straight trajectory. We have named this method Acoustic Ion Manipulation (AIM). Initial studies demonstrated selective and efficient manipulations of ion with AIM, including gating, redirection, regional dispersion, and focusing. This technique broadens the scope of ion manipulation strategies at high pressures while enriching our fundamental understanding of ion-acoustic kinetics. The potential applications of this method are vast, promising significant advancements in the fields of analytical chemistry, environmental science, and beyond. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Acoustic ion manipulation KW - Mass spectrometry PY - 2025 AN - OPUS4-64110 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Li, Xunyu T1 - Atomic Isotope Analysis of Lithium with Spatial Heterodyne Spectrometry and Lineshape Recovery through Deconvolution N2 - A spatial heterodyne spectrometer (SHS) was combined with a reduced-pressure glow discharge to demonstrate the analytical utilization of high resolving-power spectral analysis for atomic isotopes. In the experimental illustrations, we will demonstrate the spectra for the lithium isotope ratio through the D-lines featuring 6Li and 7Li. The SHS utilized in our setup boasts single-digit picometer resolution, enabling the precise discrimination of three separate spectral bands in real-time. To further enhance the spectral quality and improve quantification accuracy, we established an innovative approach to recover the natural lineshape, avoiding interferences from the instrumental function that broadens fine features. By understanding the inherent characteristics of an SHS interferogram and leveraging computational capabilities, we will demonstrate the direct extraction of the numerical presentation of the instrumental function from an SHS interferogram; this instrumental function was used for spectral data processing that enables significant improvements in spectral resolution through deconvolution algorithms. The resulting high-quality spectra enabled precise quantitative determination of lithium concentrations and isotope ratios. We aim to showcase the procedures involved in fine-tuning an SHS platform, along with software design strategy to track real-time spectral variations. Meanwhile, the concept of the lineshape recovery through deconvolution will also be discussed. Furthermore, atomic lithium spectra featuring various isotope compositions will be presented to highlight the potential of SHS in real-life applications. T2 - SCIX 2024 Conference CY - Raleigh, NC, USA DA - 20.10.2024 KW - Spatial Heterodyne Spectrometry KW - High-Resolution Spectrometry KW - Isotopic Analysis KW - Line Shape Recovery KW - Instrumental Function PY - 2024 AN - OPUS4-62138 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hufgard, Josefin T1 - Use Your Time (Domain) Wisely: Streamlined Analysis of Complex Mixtures with Pulsed-Laser Techniques N2 - This study aims to streamline complex mixture analysis through the parallel ionization of all analytes without extensive preprocessing. Here, pulsed laser ablation of single droplets is used with modified cross-correlation, a phase-sensitive algorithm. This combined method allows contactless chemical investigation with minimal sample pretreatment, as well as the separation of analytes in mixtures and reconstruction of analyte-specific mass spectra. T2 - Future WINS: Corss-sections and interfaces in science, careers, and communication CY - Berlin, Germany DA - 21.11.2024 KW - MS KW - Data analysis KW - Laser ablation PY - 2024 AN - OPUS4-62124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Jens T1 - Acoustic Ion Manipulation: Electric-field-free Approach to Gate, Focus, and Separate Ions at Atmospheric Pressure N2 - Approaches to control the motion and direction of ionized particles and mole-cules are an essential aspect of ion-based spectrometries, such as mass spec-trometry (MS) and ion mobility spectrometry (IMS). A wide variety of ion optics exist to reflect, focus, separate, gate, and filter ions based on physical proper-ties. Notably all rely on electric and magnetic fields to alter the trajectory of ionized atoms and molecules. While these optics are quite efficient at low pressures due to the large mean free path, diffusion and electrostatic repulsion between ions dominate at higher pressures. Conventional ion optics, that use electric or magnetic fields, can guide ions at atmospheric pressure (AP), but require high field strengths to overcome the dominating aerodynamic effects. Here, we describe a remarkable phenomenon whereby low-power acoustic fields are used to move, shape, gate, and separate beams of gaseous ions at atmospheric pressure. We refer to this approach as Acoustic Ion Manipulation (AIM). Gaseous ions at AP are directed towards and separated by the presence of the acoustic field. To better understand the phenomenon, an ion-detector array provided a measure of bulk ion movement, while mass spectrometry (MS) offered chemical-specific information. As one example of an AIM setup, a standing acoustic wave was formed with two ultrasonic speakers and placed between an ionization source and ion detector. Ion beams preferentially travel through regions of stable pressure gradients (i.e. nodes) and deflect from un-stable regions (i.e. antinodes). Shadowgraphy revealed that the ions are sepa-rated from a neutral gas stream. Specific examples of ion focusing, gating, and separation (based on ion size) will be shown. In addition, experimental findings will be used to postulate a theory to develop a better understand of the behav-ior of gas-phase ions in acoustic fields. This discovery could have profound im-pacts in IMS/MS instrumentation as well as materials processing and charac-terization. T2 - 56. Jahrestagung der DGMS CY - Göttingen, Germany DA - 04.03.2025 KW - Acoustic Ion Manipulation KW - Mass spectrometry KW - Ultrasound PY - 2025 AN - OPUS4-64208 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schröter, Felix T1 - Fluorescence? Not on my Shift! Excitation- Shifted UV Raman Microspectroscopy N2 - Spectroscopic analysis of samples provides elemental information, which is useful when the sample is homogenous. But many samples are not and consequently the creation of maps detailing the spatial composition of materials is needed. Raman microscopy can be used for this exact purpose but suffers a big drawback. The inherently weak Raman scattering results in long measurement times, especially when maps with many data points are created. This is due to the long exposure times needed when visible light lasers are used. A shift to UV-Lasers significantly increases the Raman intensity, as it scales with the fourth power of the inverse of the laser wavelength. But UV excitation often leads to fluorescence which can obscure the relatively weak Raman signal. Consequently, UV-Raman can only be used with specially prepared samples, for example through photo-bleaching, or with samples producing no fluorescence background in the measurement region. A solution is proposed that uses shifted-excitation Raman difference spectroscopy (SERDS) in a confocal microscope to obtain fluorescence-free Raman spectra. This is possible due to the collection of two Raman spectra at different excitation wavelengths. SERDS then allows for the calculation of just the Raman signal from the difference spectrum, which eliminates any fluorescence backgrounds, as they are not excitation wavelength dependent. The presented approach employs a polarized beamsplitter to irradiate the same spot with two lasers of different wavelengths which share the same beam path in the microscope. Consequently, a SERDS UV Raman Microscope is created, which utilizes the speed of UV-Raman without the drawbacks of possible broad fluorescence backgrounds. Here we present the instruments methodology and some first results. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - UV Raman Spectroscopy KW - UV Raman Microspectroscopy KW - Confocal Microscopy KW - Excitation-Shifted Raman Spectroscopy PY - 2025 AN - OPUS4-62734 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blume, Simon T1 - Exploiting Lithium Self-Absorption in a Laser-Induced Breakdown Plasma for Isotopic Analysis via Spatial Heterodyne Spectroscopy N2 - Lithium-ion batteries are ubiquitous in modern life. From powering consumer electronics to enabling electric mobility and energy storage, they are a key building block of a sustainable future. Determination of the ratio of the two naturally abundant stable isotopes, 7Li and 6Li, provides access to a wide variety of information, such as studying the aging processes of lithium-ion batteries or elucidating the isotopic fingerprinting of natural or recycled sources of lithium. However, accurately measuring the lithium isotope ratio in complex samples remains challenging, often requiring either extensive sample pretreatment or specialized equipment, thus impeding in-situ and high-throughput demands of global industries. Recognition and determination of the individual lithium isotopes with conventional laser-induced breakdown spectroscopy (LIBS) setups is nearly impossible. While LIBS offers several advantages, such as obviating time- and resource-intensive sample preparation and enabling rapid measurements, the high temperature (~20,000 K) of the plasma, as well as the Stark-broadening caused by the nascent free electrons spectrally broaden the atomic emission lines to such an extent that the isotopic shift of the lithium doublet at 670 nm cannot be resolved. Since, the excited state energy for this transition amounts to only 14,900 cm-1, lithium exhibits a pronounced self-absorption dip in the emission signal. This self-absorption dip is significantly less affected by the broadening effects, therefore, allowing for the resolution of the isotopic shift from its line shape. Spatial heterodyne spectroscopy (SHS) offers the superior resolution capabilities necessary to differentiate the individual isotopic contributions. To address the generally limited sensitivity of SHS, a high-repetition-rate (>10 kHz) laser allows the accumulation of more than 10,000 lasing events per spectral recording for a sufficient signal-to-noise ratio and gain statistical validity. Optical lithium fluoride serves as a model sample to showcase the analytical performance. Additionally, the impact of the laser parameters on the self-absorption will also be discussed. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Isotopic Analysis KW - Spatial Heterodyne Spectroscopy PY - 2025 AN - OPUS4-63559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Yi T1 - Advanced Repetition-Rate Modulation and Computational Strategies for Background-Free LIBS Using Non-Gated Spectrometers N2 - Laser-induced breakdown spectroscopy (LIBS) is recognized for its rapid, direct elemental analysis capabilities. However, its general adoption is constrained by the reliance on expensive, high-power consumption, gated cameras such as intensified charge-coupled devices (CCDs). These devices, while sensitive, are expensive and possess low frame rates, limiting their efficacy in dynamic or challenging environments. Our study proposes an innovative approach that leverages non-gated spectrometers in conjunction with the framework of correlation spectroscopy to isolate analyte signals responsive to a specific repetition-rate modulation pattern, thereby yielding spectra with zero background. We utilized a diode-pumped solid-state laser, with repetition rates ranging from 10 Hz to 30 kHz, to induce plasma in aqueous solutions containing various alkaline and earth-alkaline metals. With a non-gated single-grating linear CCD spectrometer, we found that the continuum signal plateaued at approximately 7 kHz. In contrast, atomic emissions from the dissolved analytes showed continued increases. Notably, atomic emissions from the solvent (water) were observable only above 8.5 kHz, at a significant high rate of increase. Through computational synthesis of a modulation pattern, we determined an optimized scheme that effectively discriminates continuum and analyte signals; this pattern was optimized with a genetic algorithm. The spectral matrix correlating signal intensity with laser repetition rate and wavelength was used as the input of the model. Meanwhile, the fitness function that extracts the background-free spectra was built in-house and inspired by the Gardner transform, which exploits the power of Fourier transform, allowing for flagging and splitting analyte signal from other undesired features. This approach bypasses the limitations associated with gated cameras, while providing a cost-effective alternative for robust LIBS applications. This advancement is particularly relevant in field, portable and remote applications, aligning with the ongoing demand for accessible, high-performance analytical tools in diverse scientific fields. T2 - SCIX 2024 Conference CY - Raleigh, NC, USA DA - 20.10.2024 KW - LIBS KW - Data Processing KW - High Repetition Rate KW - Repetition Rate Modulation KW - Data-Oriented Experimental Design PY - 2024 AN - OPUS4-62137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Danischewski, Julia L. A1 - You, Yi A1 - Bauer, Lauren A1 - Riedel, Jens A1 - Shelley, Jacob T. T1 - Use of Resonant Acoustic Fields as Atmospheric-Pressure Ion Gates N2 - Ion optics are crucial for spectrometric methods such as mass spectrometry (MS) and ion mobility spectrometry (IMS). Among the wide selection of ion optics, temporal ion gates are of particular importance for time-of-flight MS (TOF-MS) and drift-tube IMS. Commonly implemented as electrostatic ion gates, these optics offer a rapid, efficient means to block ion beams and form discrete ion packets for subsequent analysis. Unfortunately, these devices rely on pulsed high voltage sources and are not fully transparent, even in their open state, which can lead to ion losses and contamination. Here, a novel atmospheric-pressure ion gate based on a resonant acoustic field structure is described. This effect was accomplished through the formation of a resonant, standing acoustic wave of alternating nodes and antinodes. Alignment of an atmospheric-pressure gaseous ion beam with an antinode, i.e. a region of transient pressure, of the acoustic structure acted as a gate and blocked ions from impinging on ion-selective detectors, such as a mass spectrometer and a Faraday plate. The velocity of the ion stream and acoustic power were found to be critical parameters for gating efficiency. In the presence of an acoustic field (i.e., a closed gate), ion signals decreased by as much as 99.8% with a response time faster than the readout of the ion-measurement devices used here (ca. 75 ms). This work demonstrates the basis for a low-cost, acoustic ion gate, which is optically transparent and easily constructed with low-power, off-the-shelf components, that could potentially be used with MS and IMS instrumentation. KW - Acoustic Ion Manipulation PY - 2025 DO - https://doi.org/10.1021/acs.analchem.4c05493 SN - 1520-6882 VL - 97 IS - 5 SP - 2890 EP - 2898 PB - American Chemical Society AN - OPUS4-62648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Anita T1 - Eine sichere Zukunft für Lithium-Ionen Batterien N2 - Eine sichere Zukunft hat eine Technologie dann, wenn sie die Gesellschaft auch von ihrer Sicherheit überzeugen kann. Dies ist insbesondere für Lithiumbatterien von hoher Bedeutung. Die BAM trägt auf den verschiedene Ebenen auf vielfältige Art und Weise dazu bei, diese Sicherheit zu untersuchen und zu verbessern. T2 - 4. Batterieforum Berlin Brandenburg CY - Potsdam, Germany DA - 22.11.2024 KW - LIthiumbatterien KW - Sicherheit PY - 2024 AN - OPUS4-62328 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blume, Simon T1 - Femtosecond Laser-induced XUV Spectroscopy (LIXS) for Elemental Analysis N2 - In a typical laser-induced breakdown spectroscopy (LIBS) setup, emissions from collisional excitation of the atoms in the later stages of the plasma are detected and provide information about the elemental fingerprint of the sample. However, precise measurements, in particular quantification efforts, suffer from fluctuations of the intensity of the detected emission lines due to matrix effects and plasma-flicker noise, as well as significant background noise. In contrast, the early stages of the plasma are dominated by electron-ion recombination and Bremsstrahlung, which lead to sharp and intense x-ray emissions with consistent intensity profiles between laser pulses and suppressed background noise, therefore improving the limit of detection, especially for lighter elements. These emissions are detected in laser-induced XUV spectroscopy (LIXS).[1] Introduction of a femtosecond laser (pulse length ~100 fs) to the LIXS setup fundamentally changes the laser energy absorption and ablation process. The laser pulse energy is absorbed and redistributed by multiphoton absorption and inverse Bremsstrahlung and operates on a time frame faster than the plasma formation. Additionally, the plasma formation itself is accelerated leading to signal generation in the XUV-range before generation of the undesired background emissions. Thus, utilization of a femtosecond laser allows for further suppression of broadband emissions from the plasma allowing for sharper separation of the emission lines and improved limit of detection. This work presents the results of the combination of a LIXS setup with a femtosecond laser and assess the capabilities of this system with a model sample of cathode material from a spent lithium-ion battery. T2 - AMACEE 2025 CY - Brno, Czech Republic DA - 26.8.2025 KW - LIXS KW - Femtosecond laser KW - Instrumentation PY - 2025 AN - OPUS4-64118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Palásti, Dávid jenö T1 - Interferometric sensing in the UV range – Investigation and comparison of the all-reflective spatial heterodyne spectrometer designs N2 - Spatial heterodyne spectrometers (SHS) are optical interferometric devices, working in the UV and visible spectral ranges [1]. The most common SHS setup is similar to the Michelson interferometer, both utilizes a beam splitter in the incoming beam path. In case of the SHS the split beams are not aimed towards orthogonal mirrors, but reflective optical gratings, set under a selected angle. These optical gratings diffract the beams, the direction of every wavelength will depend on the grating constant and the angle of the gratings. The wavefronts belonging to different wavelengths are going to cross each other under a unique angle, resulting in a spatial interference, which is recorded by a digital camera. This relatively compact setup provides high resolution and light throughput, which properties were harnessed for tasks requiring good line separation and/or high sensitivity [2]. However, SHS are only applicable on wavelengths for which an adequate transmissive beam splitter is available like the visible range, but not the far UV. To overcome this limitation, different all-reflective designs were introduced [3]. These instruments utilize symmetric optical gratings for the splitting and recombination of the beams. Although these SHS devices solve the main limitations of the traditional ones, they come with their fair share of drawbacks as well, such as more complex arrangement and the requirement for more delicate tuning. The behaviour of the traditional SHS is well documented [4,5], but in regards of the all-reflective ones we have much less available information. In this current study we utilized computational modelling to predict the behaviour of the all-reflective SH spectrometers, with special attention to the effects of the different alignment errors. Later we utilize this knowledge to fine tune an SHS for sensing (LIBS, Raman) in the UV region. Furthermore, we are introducing two new all-reflective SHS setups and compering them to their older counterparts. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - SHS KW - Spectroscopy PY - 2025 AN - OPUS4-63556 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blume, Simon T1 - Isotopic analysis of lithium via acousto-optically gated high-repetition laser-induced breakdown spectroscopy and spatial heterodyne spectroscopy N2 - Acousto-optically gating the emission signal from a laser-induced breakdown spectroscopy (LIBS) plasma negates some of the line-broadening effects, therefore, improving the signal line shape. However, the remaining influences disallow the differentiation of the contributions of the individual lithium isotopes, even when utilizing a high-resolution spatial heterodyne spectrometer (SHS). Nevertheless, isotopic analysis of lithium with LIBS is still feasible, because lithium exhibits a strong self-absorption dip in the emission signal, which is likewise characterized by the isotopic shift and even benefits from the broad emission lines typically observed in LIBS. The isotopic ration can be resolved from the absorption dip via high-resolution SHS. T2 - SciX 2024 CY - Raleigh, NC, USA DA - 20.10.2024 KW - LIBS KW - SHS KW - Isotopic analysis KW - Lithium PY - 2024 AN - OPUS4-62012 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Palásti, Dávid jenö T1 - The effects of the laser pulse profile on the plasma emission properties N2 - Intense laser pulses create plasmas upon radiation on targets, and the properties of such plasmas are generally determined by both the properties of the target and the laser pulse. In terms of laser intensity, the irradiance and even more importantly the fluence are the critical parameters [1]. Since most lasers emit pulses of a constant pulse duration dictated by the design of the resonator and Q-switch, these two parameters are usually used interchangeably in studies. However, with the emergence of fiber laser based light sources [2], which are capable not just to freely tune the pulse duration, but to generate variable and high pulse repetition rates, up to the MHz range, a new and interesting optimization aspect is given to the laser spectroscopy community. In our study a low alloy steel standard sample (BAS 403/1) was investigated using a variable pulse duration and pulse repetition rate MOPA laser with 80W power of  = 1064 nm emission (JPT M7, VONJAN Technology GmbH, Wessling, Germany). In our experiments the laser was set to pulses with low individual energy (0.4 mJ) at 200 kHz pulse repetition rate, while the pulse duration was varied between 50 and 500 ns. The plasma emission was recorded by an LTB Demon spectrometer in several spectral regions, which included iron, chromium and manganese lines. Utilizing the variable pulse duration of this laser source, it was possible to assess the effects of changing the fluence, while the irradiance was kept at the same value. Among the investigated parameters are the emission intensity, peak width and self-absorption characteristics of major and minor components, as well as the plasma temperature. While the effects for the peak intensity are quite well correlated with the fluence, its interplay with other peak parameters appear to be more complicated. T2 - AMACEE 2025 CY - Brno, Czech Republic DA - 26.08.2025 KW - LIBS KW - Fiberlaser KW - Plasma properties PY - 2025 AN - OPUS4-64218 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - On-line monitoring of polyhydroxyalkanoate extraction process using compact NMR spectroscopy N2 - Portable benchtop NMR spectrometers enable real-time process and reaction monitoring in contrast to conventional laboratory based off-line gas chromatography or high-field NMR measurements. In this study, benchtop NMR spectroscopy is demonstrated as a process analytical technology (PAT) tool for the application of the solvent extraction step in downstream processing of polyhydroxyalkanoate (PHA) biopolymers. These are one of the few thermoplastic polymers synthesized 100 % via biotechnological routes which fully biodegrade in common natural environments. This makes them excellent candidate materials for sustainable replacement of conventional plastic materials. Online NMR experiments were conducted using a fully automated setup, employing commercially available PTFE tubing as a flow-cell assembly. Extraction was carried out in a thermostated stirred batch reactor in lab-scale. Single-scan NMR spectra allowed continuous monitoring of the extraction of the PHA copolymer poly-(hydroxybutyrate-co-hydroxyhexanoate) containing 13.5 mol-% hydroxyhexanoate from Ralstonia eutropha biomass. Extractions were performed in chloroform and acetone across ground lyophilized cell loadings ranging from 20 to 120 g/L. The reproducibility and reliability of compact NMR spectroscopy closely matched with high-field NMR measurements. A strong correlation was observed between online low-field NMR data and offline gas chromatography (GC) analysis. The study highlights the versatility of compact NMR for process monitoring, facilitating endpoint determination and enhancing extraction efficiency by optimizing process parameters. Steady-state conditions were achieved within 6 to 10 minutes for chloroform and acetone, respectively, underscoring the method’s value in supporting downstream process development and optimization for PHA recovery. T2 - 20. Herbstkolloquium Arbeitskreis Prozessanalytik CY - Frankfurt am Main, Germany DA - 03.12.2025 KW - Polyhydroxyalkanoate KW - Process Analytical Technology KW - Downstream processing KW - Benchtop-NMR PY - 2025 AN - OPUS4-65065 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Miliūtė, Aistė A1 - Bustamante, Joana A1 - Karafiludis, Stephanos A1 - Zöllner, Moritz A1 - Eddah, Mustapha A1 - Emmerling, Franziska A1 - Mieller, Björn A1 - George, Janine A1 - Stawski, Tomasz M. T1 - Synthesis and phase purity of the negative thermal expansion material ZrV2O7 N2 - Synthesis of pure, homogeneous, and reproducible materials is key for the comprehensive understanding, design, and tailoring of material properties. In this study, we focus on the synthesis of ZrV2O7, a material known for its negative thermal expansion properties. We investigate the influence of solid-state and wet chemistry synthesis methods on the purity and homogeneity of ZrV2O7 samples. Our findings indicate that different synthesis methods significantly impact the material's characteristics. The solid-state reaction provided high-purity material through extended milling time and repeated calcination cycles, while the sol-gel reaction enabled a “near-atomic” level of mixing and, therefore, homogenous phase-pure ZrV2O7. We confirmed purity via X-ray diffraction and Raman spectroscopy, highlighting differences between phase-pure and multiphase ceramics. These analytical techniques allowed us to distinguish subtle differences in the structure of the material. Based on ab initio simulated phonon data, we were able to interpret the Raman spectra and visualise Raman active atom vibrations. We show that phase purity enables the unbiased characterisation of material properties such as negative thermal expansion. KW - NTE KW - Sol-gel KW - Solid-state KW - Ab-initio KW - XRD KW - Raman PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624013 DO - https://doi.org/10.1039/d4tc04095c SN - 2050-7534 SP - 1 EP - 13 PB - Royal Society of Chemistry (RSC) AN - OPUS4-62401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karafiludis, Stephanos A1 - Kochovski, Z. A1 - Scoppola, E. A1 - Retzmann, Anika A1 - Hodoroaba, Vasile-Dan A1 - ten Elshof, J. E. A1 - Emmerling, Franziska A1 - Stawski, Tomasz Maciej T1 - Nonclassical Crystallization Pathway of Transition Metal Phosphate Compounds N2 - Here, we elucidate nonclassical multistep crystallization pathways of transition metal phosphates from aqueous solutions. We followed precipitation processes of M-struvites, NH4MPO4·6H2O, and M-phosphate octahydrates, M3(PO4)2·8H2O, where M = Ni, Co, or NixCo1–x, by using in situ scattering and spectroscopy-based techniques, supported by elemental mass spectrometry analyses and advanced electron microscopy. Ni and Co phosphates crystallize via intermediate colloidal amorphous nanophases, which change their complex structures while agglomerating, condensing, and densifying throughout the extended reaction times. We reconstructed the three-dimensional morphology of these precursors by employing cryo-electron tomography (cryo-ET). We found that the complex interplay between metastable amorphous colloids and protocrystalline units determines the reaction pathways. Ultimately, the same crystalline structure, such as struvite, is formed. However, the multistep process stages vary in complexity and can last from a few minutes to several hours depending on the selected transition metal(s), their concentration, and the Ni/Co ratio. KW - Non-classical crystallization theory KW - Transition metals KW - Phosphates KW - Amorphous phases KW - Intermediate phases PY - 2023 DO - https://doi.org/10.1021/acs.chemmater.3c02346 SN - 1520-5002 VL - 35 IS - 24 SP - 10645 EP - 10657 PB - American Chemical Society (ACS) CY - Washington D.C. AN - OPUS4-59135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hufgard, Josefin T1 - AIM Forward: Acoustic Ion Manipulation for Efficient Ambient-Pressure Ion Control N2 - In ion-based spectrometry techniques the possibility to manipulate ions is fundamentally important. Currently used ion optics mostly rely on magnetic or electric fields. The electromagnetic forces compete with ion diffusion and are therefore most effective under low-pressure conditions. Therefore, high-pressure ion optics pose challenges related to elevated powers and potentials as well as complex structures and electrode contamination. Acoustic Ion Manipulation (AIM) is a recently discovered phenomenon that relies on the unique interactions between gas-phase ions and acoustic waves. This presentation shows selected patterns of ion manipulation, highlights the flexibility of AIM and discusses its current limitations and potentials. T2 - DGMS Annual Conference 2026 CY - Leipzig, Germany DA - 10.03.2026 KW - Acoustic ion manipulation KW - Mass spectrometry PY - 2026 AN - OPUS4-65680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Henning, Thorsten A1 - Goerdeler, Cornelius A1 - El-Khatib, Ahmed H. A1 - Meyer, Klas A1 - Bruer, Gustav G. A1 - Abraham, Klaus A1 - Monien, Bernhard T1 - Characterization and quantitation of urinary metabolites of 3-monochloropropane-1,2-diol (3-MCPD) in rats N2 - Fatty acid esters of 3-monochloropropane-1,2-diol (3-MCPD) are heat-induced contaminants formed from fats and sodium chloride. The mode of action for the 3-MCPD mediated induction of renal tubule neoplasms in rats is still unclear, which is in part due to lacking metabolism data. In the current study, urinary metabolites were identified by one- and two-dimensional 13C nuclear magnetic resonance spectroscopy and high-resolution mass spectrometry following oral administration of 3-MCPD or [13C3]3-MCPD in rats. In addition to 3-MCPD itself, nine metabolites were identified. Four of those, N-acetyl-S-(2,3-dihydroxypropyl)cysteine (DHPMA), 3-MCPD sulfate, β-chlorolactic acid (β-ClLA) and oxalic acid have been reported before. Five novel metabolites in rat urine were thiodiglycolic acid (TDGA), thionyldiglycolic acid (TNDGA), 3-MCPD glucuronide (at least three isomers), 3-carboxy-2-hydroxypropyl mercapturic acid (CHPMA), and 3-(S-carboxymethyl)mercaptolactic acid (CMMLA). Only three metabolites were excreted at mean dose ratios > 1% (after treatment with 50 mg 3-MCPD/kg body weight in male and female rats), i.e. 3-MCPD (7.3%, 9.7%), DHPMA (3.5%, 1.7%) and TDGA (1.1%, 4.0%). The overall mean dose excretion in urine samples (males: 12.2%, females: 16.3%) supported hypotheses on formation of conjugates/adducts of reactive metabolites and the possibility that dechlorination leads to suitable building blocks for amino acid and fatty acid synthesis. The identification of TDGA indicated the interim formation 2-chloroacetaldehyde, previously identified to mediate specific nephrotoxic effects of the cytostatic ifosfamide in rats. KW - 3-Monochloropropane-1,2-diol KW - 3-MCPD KW - Metabolism KW - Urine PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-657230 DO - https://doi.org/10.1007/s00204-026-04318-x SP - 1 EP - 17 PB - Springer-Verlag GmbH CY - Heidelberg AN - OPUS4-65723 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Benchtop NMR-Spektroskopie im industriellen Produktionsumfeld: Herausforderungen auf dem Weg zur Online-Prozessintegration N2 - Benchtop-NMR Spektrometer erobern erfolgreich seit Jahren die Labore und haben sich als ein vielseitiges analytisches Werkzeug etabliert. Zunächst stark fokussiert auf den Forschungs-bereich, sind sie heute zunehmend auch nahe der Produktion auf dem Vormarsch. Die Zielstellung ist nur selten der Ersatz von klassischer „Hochfeld“-NMR-Spektroskopie. Vielmehr erschließen die kompakten Geräte oftmals neue Anwendungsfelder, beispielsweise in der Online-Reaktionsverfolgung im Labor oder der schnellen at-line Qualitätskontrolle in der chemischen Produktion. Hier kommen die Vorteile der geringeren Anschaffungs- und Betriebskosten, die Möglichkeit des prozessnahen Einsatzes, sowie besonders der einfachen Bedienung zum Tragen. Während es zahlreiche Beispiele von Online-Applikationen im Labor gibt, ist die direkte Einbindung in großtechnische Produktionsanlagen bislang selten. Im Vergleich zu etablierten prozessanalytischen Verfahren, wie z.B. der Nahinfrarot- oder Raman-Spektroskopie ist die Benchtop-NMR-Spektroskopie noch Neuland und es existieren kaum prozesstaugliche kommerzielle Lösungen. Im Rahmen eines gemeinsamen Entwicklungsprojekts zwischen BAM und Evonik wurde eine Einhausung für ein handelsübliches Benchtop-NMR-Spektrometer konzipiert und gebaut. Diese dient nicht nur der Erfüllung sicherheitstechnischer Auflagen wie dem Explosionsschutz, sondern auch der Abschirmung rauer Umgebungseinflüsse auf den Betrieb des Laborgeräts. Eine flexible integrierte Automatisierung ermöglicht die skalierbare Anbindung an übergeordnete Prozessleittechnik im Sinne eines PAT-Moduls. Dieser Vortrag gibt einen Überblick über die Herausforderungen auf dem Weg von der Idee, über die Umsetzung bis hin zur tatsächlichen Prozessintegration. T2 - 47. Praktische Probleme der Kernresonanzspektroskopie CY - Göttingen, Germany DA - 17.03.2026 KW - Prozessanalytik KW - NMR Spektroskopie KW - Feldintegration KW - Explosionsschutz PY - 2026 AN - OPUS4-65705 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karafiludis, Stephanos A1 - Stawski, Tomasz T1 - Deciphering the non-classical Crystallization of transition metal phosphates (TMP) N2 - A crucial aspect of ensuring sustainable raw material utilization to meet global demand lies in the efficient recovery and reuse of critical elements and compounds. Phosphate, PO43-, and many transition metals e.g. Ni and Co are listed as critical raw materials (CRMs) due to their indispensable role in numerous industrial processes. However, these elements can also exert harmful environmental impacts, with phosphorus being a major contributor to anthropogenic eutrophication and transition metal ions acting as toxic pollutants, particularly in ground- and wastewaters. Typically, separate pathways have been considered to extract hazardous substances such as transition metals or phosphate, independently from each other. Here, we report the crystallization pathways of transition metal phosphate (TMP) compounds, M-struvite and M-phosphate octahydrate with M = Ni2+, Co2+, NixCo1-x2+, NH4MPO4∙6H2O, M3(PO4)2∙8H2O from aqueous solutions. The co-precipitation of these particular TMP compounds from industrial and agricultural wastewaters has high potential as a P- and 3d metal recovery route. For efficient extraction and transformation of the TMPs, a comprehensive understanding of their nucleation and crystallization pathways from aqueous solutions is required. While the crystallization mechanisms of magnesium or calcium phosphate-bearing phases have been researched for many decades (e.g. struvite, apatite), investigations into TMP materials are relatively scarce and often focus on the adsorption of transition metals on the surface instead of their actual incorporation in minerals. In our study, we investigated in detail the precipitation process of several Co and Ni phosphates using ex- and in-situ spectroscopic-, spectrometric- and diffraction-/scattering-based techniques. We show that the crystallization behavior of TMPs, indeed deviates from a classical crystallization paradigm and follows a non-classical multi-step pathway. Our work extends the understanding of TMP crystallization by elucidating the formation of amorphous precursors preceding the final crystalline phase This time-dependent transition of the transition metal precursor phases can be observed by electron-imaging/tomography depicting a progressively changing amorphous solids until their ultimate reconfiguration to a crystal (Figure 1). Here, the two-metallic NixCo1-x-mixtures deviated anomalously in their reaction kinetics, crystallization outcome and participation of both metals from their pure endmembers. By measuring the crystallization with in-situ X-ray scattering and pH using a flow-through setup geometry, a complex prolonged interplay among nucleating entities e.g. and amorphous or crystalline solids could be observed in the metal phosphate mixtures reaching equilibrium after almost two and a half hours (Figure 2). Our results provide a holistic perspective on the crystallization behavior of transition metal phosphate phases, shedding light on their unique nucleation and growth kinetics involving structural and chemical transformations of the intermediate phases. T2 - Granada Münster Discussion Meeting 2023 CY - Münster, Germany DA - 29.11.2023 KW - Non-classical crystallization theory KW - Transition metals KW - Phosphates PY - 2023 AN - OPUS4-59007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martins, Ines A1 - Al-Sabbagh, Dominik A1 - Bentrup, U. A1 - Marquardt, Julien A1 - Schmid, Thomas A1 - Scoppola, E. A1 - Kraus, Werner A1 - Stawski, Tomasz A1 - de Oliveira Guilherme Buzanich, Ana A1 - Yusenko, Kirill A1 - Weidner, Steffen A1 - Emmerling, Franziska T1 - Formation Mechanism of a Nano-Ring of Bismuth Cations and Mono-Lacunary Keggin-Type Phosphomolybdate N2 - A new hetero-bimetallic polyoxometalate (POM) nano-ring was synthesized in a one-pot procedure. The structure consists of tetrameric units containing four bismuth-substituted monolacunary Keggin anions including distorted [BiO8] cubes. The nano-ring is formed via self-assembly from metal precursors in aqueous acidic medium. The compound (NH4)16[(BiPMo11O39)4] ⋅ 22 H2O; (P4Bi4Mo44) was characterized by single-crystal X-ray diffraction, extended X-ray absorption fine structure spectroscopy (EXAFS), Raman spectroscopy, matrix-assisted laser desorption/ionisation-time of flight mass spectrometry (MALDI-TOF), and thermogravimetry/differential scanning calorimetry mass spectrometry (TG-DSC-MS). The formation of the nano-ring in solution was studied by time-resolved in situ small- and wide-angle X-ray scattering (SAXS/WAXS) and in situ EXAFS measurements at the Mo−K and the Bi−L3 edge indicating a two-step process consisting of condensation of Mo-anions and formation of Bi−Mo-units followed by a rapid self-assembly to yield the final tetrameric ring structure. KW - Bismuth KW - In situ EXAFS KW - In situ SAXS/WAXS KW - Lacunary Keggin ion KW - Polyoxometalates KW - Self-assembly PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546823 DO - https://doi.org/10.1002/chem.202200079 SN - 0947-6539 VL - 28 IS - 27 SP - 1 EP - 7 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Benchtop-NMR Spectroscopy as a PAT tool in industrial environments – Field integration of a laboratory instrument N2 - Chemical industry is currently in a rapidly changing environment, e.g., due to variability of raw material quality, high energy costs and demand for improving efficiency. Process optimization and new process concepts become more and more important. Flexible chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds like exothermic reactions with high heat dissipation. Highly automated chemical process monitoring along with real-time quality control are prerequisites to such concepts and, thus, should be based on “real-time” chemical information. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as explosion safety, field communication, and robust evaluation of sensor data. Field studies in modular and conventional production plant setups show promising results gaining process knowledge for further optimization. NMR spectroscopy appeared as powerful online analytical method and allows using a modular data analysis approach, which can even serve as reliable reference method for further calibration-dependent PAT applications (e.g., NIR or Raman spectroscopy). Based on experiences from earlier field studies an enhanced field enclosure setup was developed and built, including the option of a secondary analytical method (e.g., optical spectroscopy). Integrated control systems allow for a flexible implementation based on the available automation infrastructure at the chemical plant or pilot plant setup. In the future, modular interconnecting “smart” PAT systems and process equipment have the potential speed up the setup of production equipment for chemicals and pharma-ceuticals and therefore help to reduce the time-to-market. T2 - Analytica Conference 2026 CY - Munich, Germany DA - 24.03.2026 KW - Benchtop NMR spectroscopy KW - Process Analytical Technology KW - Field integration KW - Explosion safety PY - 2026 AN - OPUS4-65771 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -