Analytische Chemie
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Organisationseinheit der BAM
- 1 Analytische Chemie; Referenzmaterialien (1480)
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Paper des Monats
- ja (29)
Die Probenpräparation ist ein wichtiger Schritt für die Qualität der Massenspektren in MALDI-TOF MS. Es werden Polymerproben, die lösungsmittelbasiert und lösungsmittelfrei präpariert worden sind, verglichen. Dabei werden die Intensitätsverhältnisse von ternären Mischungen von PEG-, PS- und PMMA-Polymeren beachtet.
Ergot alkaloids (EAs) formed by Claviceps fungi are one of the most common food contaminants worldwide, affecting cereals such as rye, wheat, and barley. To accurately determine the level of contamination and to monitor EAs maximum levels set by the European Union, the six most common EAs (so-called priority EAs) and their corresponding epimers are quantified using high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). The quantification of EAs in complex food matrices without appropriate internal tandards is challenging but currently carried out in the standard method EN 7425:2021 due to their commercial unavailability. To address the need for isotopically labeled EAs, we focus on two semi-synthetic approaches for the synthesis of these reference standards. Therefore, we investigate the feasibility of the N6-demethylation of native ergotamine to yield norergotamine, which can subsequently be remethylated with an isotopically labeled methylating reagent, such as iodomethane (13CD3-I), to yield isotopically labeled ergotamine and its C8-epimer ergotaminine. Testing the isotopically labeled ergotamine/-inine against native ergotamine/-inine with HPLC coupled to high-resolution HR-MS/MS proved the structure of ergotamine-13CD3 and ergotaminine-13CD3. Thus, for the first time, we can describe their synthesis from unlabeled, native ergotamine. Furthermore, this approach is promising as a universal way to synthesize other isotopically labeled EAs.
Bei der Erhaltung von Stahlbetonbauwerken ist der Chloridgehalt im Beton ein wichtiger Parameter zur Festlegung geeigneter Instandsetzungsmaßnahmen. Die bisher etablierten Verfahren basieren auf der nasschemischen Analyse einer Probe, Bohrmehl oder aufgemahlener Segmente eines Bohrkerns. Das Verfahren liefert einen Chloridgehalt je Tiefensegment, was mit einer starken Homogenisierung der Probe einhergeht, wodurch detaillierte Informationen zu Chloridunterschieden im Millimeterbereich verloren gehen. Eine alternative Methode ist die laserinduzierte Plasmaspektroskopie (LIBS), die nicht nur die quantitative ortsaufgelöste Bestimmung des Chloridgehalts im Bezug zur Zementmasse ermöglicht, sondern auch simultan detaillierte Informationen über die Verteilung vieler anderer chemischer Elemente liefert. Die räumliche Auflösung liegt in der Regel im Bereich von einigen Millimetern, kann aber bei Bedarf auf 0,1 mm oder weniger erhöht werden. Das neue Merkblatt B14 „Quantifizierung von Chlorid in Beton mit der laserinduzierten Plasmaspektroskopie (LIBS)“ der Deutschen Gesellschaft für Zerstörungsfreie Prüfungen (DGZfP) regelt und vereinheitlicht erstmals die zuverlässige und reproduzierbare Ermittlung des Chloridgehalts mit LIBS. In diesem Beitrag wird das Merkblatt vorgestellt und anhand praktischer Anwendungsbeispiele das Potenzial von LIBS für Fragestellungen in der Betonerhaltung verdeutlicht.
The use of ashes from municipal solid waste incineration as secondary building materials is an important pillar for the circular economy in Germany. However, leaching of potential toxic elements from these materials must be at environmentally acceptable levels. Normally, a three-month ageing period immobilizes most hazardous heavy metals, but antimony (Sb) and vanadium (V) showed previously unusual leaching. In order to clarify the mechanisms, we analyzed the Sb and V species in various bottom and fly ashes from municipal waste incineration by XANES spectroscopy. Antimony oxidizes from Sb(+ III) species used as flame retardants in plastics to Sb(+ V) compounds during waste incineration. However, owing to the similarity of different Sb(+ V) compound in the Sb K- and L-edge XANES spectra, it was not possible to accurately identify an exact Sb(+ V) species. Moreover, V is mainly present as oxidation state + V compound in the analyzed ashes. However, the coarse and magnetic fraction of the bottom ashes contain larger amounts of V(+ III) and V(+ IV) compounds which might enter the waste incineration from vanadium carbide containing steel tools. Thus, Sb and V could be critical potential toxic elements in secondary building materials and long-term monitoring of the release should be taken into account in the future.
Soil certified reference material (CRM), UME EnvCRM 03 was produced by a collaborative approach among national metrology institutes, designated institutes and university research laboratories within the scope of the EMPIR project: Matrix Reference Materials for Environmental Analysis. This paper presents the sampling and processing methodology, homogeneity, stability, characterization campaign, the assignment of property values and their associated uncertainties in compliance with ISO 17034:2016. The material processing methodology involves blending a natural soil sample with a contaminated soil sample obtained by spiking elemental solutions for 8 elements (Cd, Co, Cu, Hg, Ni, Pb, Sb and Zn) to reach the level of warning risk monitoring values specified for metals and metalloids of soils in Europe. Comparative homogeneity and stability test data were obtained by two different institutes, ensuring the reliability and back up of the data. The certified values and associated expanded uncertainties for the total mass fractions of thirteen elements (As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Pb, Sb, V and Zn) are established. The developed CRM can be used for the development and validation of measurement procedures for the determination of the total mass fractions of elements in soil and also for quality control/assurance purposes. The developed CRM is the first example of a soil material originating from Türkiye.
In this work, the electrochemical behavior of 4-phenylurazole (Ph-Ur) was studied and the latter was used as a molecular anchor for the electrochemical bioconjugation of tyrosine (Y). Cyclic voltammetry (CV) and controlled potential coulometry (CPC) allowed the in-situ generation of the PTAD (4-phenyl-3 H-1,2,4-triazole-3,5(4 H)-dione) species from phenylurazole on demand for tyrosine electrolabeling. The chemoselectivity of the reaction was studied with another amino acid (lysine, Lys) and no changes in Lys were observed. To evaluate the performance of tyrosine electrolabeling, coulometric analyses at controlled potentials were performed on solutions of phenylurazole and the phenylurazole-tyrosine mixture in different proportions (2:1, 1:1, and 1:2). The electrolysis of the phenylurazole-tyrosine mixture in the ratio (1:2) produced a charge of 2.07 C, very close to the theoretical value (1.93 C), with high reaction kinetics, a result obtained here for the first time. The products obtained were identified and characterized by liquid chromatography coupled to high-resolution electrospray ionization mass spectrometry (LC-HRMS and LC- HRMS2). Two products were formed from the click reactions, one of which was the majority. Another part of this work was to study the electrochemical degradation of the molecular anchor 4-phenylazole (Ph-Ur). Four stable degradation products of phenylurazole were identified (C7H9N2O, C6H8N, C6H8NO, C14H13N4O2) based on chromatographic profiles and mass spectrometry results. The charge generated during the electrolysis of phenylurazole (two-electron process) (2.85 C) is inconsistent with the theoretical or calculated charge (1.93 C), indicating that secondary/parasitic reactions occurred during the electrolysis of the latter. In conclusion, the electrochemically promoted click phenylurazole-tyrosine reactions give rise to click products with high reaction kinetics and yields in the (1:2) phenylurazole-tyrosine ratios, and the presence of side reactions is likely to affect the yield of the click phenylurazole-tyrosine reaction.
Volatile organic compounds (VOCs) emitted by furniture and building materials can cause health issues. For an improvement of indoor air quality low emitting materials should be used. Quality assurance and –control (QA/QC) measures require an emission reference material (ERM) with a predictable emission rate of VOCs. The idea is to use porous materials as ERM, which store the VOCs inside their pores and emit them constantly.
Volatile organic compounds (VOCs) emitted by furniture and
building materials can cause health issues. For an
improvement of indoor air quality low emitting materials
should be used. Quality assurance and –control (QA/QC)
measures require an emission reference material (ERM) with a
predictable emission rate of VOCs. The idea is to use porous
materials as ERM, which store the VOCs inside their pores and
emit them constantly.
Isotope analysis plays a critical role in various disciplines, including environmental science, archaeology, and forensic investigations. Traditional methods such as mass spectrometry provide precise isotopic data but often require complex, costly setups and extensive sample preparation. As an alternative, optical spectrometry has emerged as a versatile and less invasive technique. This presentation explores the advancements and applications of optical spectrometry methods in isotope analysis, emphasizing their benefits and challenges.
Lithium (Li), Boron (B), Nitrogen (N), Magnesium (Mg), and Calcium (Ca) are pivotal elements across various spheres such as the hydrosphere, biosphere, and lithosphere, significantly impacting (bio-) geochemical and physiological processes. These elements exhibit stable isotopes with substantial roles in geological, environmental, and biological studies. The traditional method for measuring isotope amount ratios has been through mass spectrometry, which, despite its accuracy, comes with high operational costs, the need for skilled operators, and time-consuming sample preparation processes.
Combining optical spectroscopy with chemometrics introduces an innovative, cost-effective approach by the hand of high-resolution continuum source atomic and molecular absorption spectrometry (HR-CS-AAS and HR-CS-MAS) for the analysis of isotope ratios in Li, B, N, Mg, and Ca. By analyzing the atomic or molecular absorption spectrum of the in-situ generated cloud of atoms of diatomic molecules (e.g., Li, BH, NO, MgF, CaF) during the electronic transition from the fundamental state, this method allows for the rapid determination of isotope ratios directly from sample solutions without the need for complex sample preparation.
For each element, the respective atomic or molecule's absorption spectrum was deconvoluted into its isotopic components using partial least squares regression or machine learning algorithms. Robust calibration models were developed, calibrated with enriched isotope, and validated against certified reference materials. Spectral data underwent preprocessing to optimize the modeling to determine the optimal number of latent variables.
The findings showcase that this optical spectrometric method yields results that agree with those obtained via inductively coupled plasma mass spectrometry (ICP-MS), offering a promising, cost-effective, and rapid alternative for isotope analysis with precisions as low as ± 0.2‰. This approach is a significant advancement in analytical chemistry, providing a new way to study isotope variations in biological, environmental, and geological samples.
What does GD-OES reveal about the aging and manufacturing processes of lithium-ion batteries?
(2024)
Glow-Discharge Optical Emission Spectroscopy (GD-OES), a powerful analytical technique, sheds light on the two critical aspects of lithium-ion batteries (LIBs): manufacturing and aging 1, 2. We optimized cell production in manufacturing by adjusting parameters, including cathode doping, electrolyte concentration, and pressing force. GD-OES provided in-depth elemental composition and homogeneity analysis, which is crucial for identifying optimal manufacturing conditions. These findings were validated by electrochemical impedance spectroscopy, confirming the quality of the manufactured batteries.
Shifting the focus to aging, we use GD-OES for fluorine depth profiling, a key element in understanding polymer and electrolyte degradation. However, fluorine presents analytical challenges. We addressed this by substituting argon with a neon:argon mixture, which significantly enhanced fluorine detection sensitivity. This advancement not only improves accuracy but also holds the potential to guide sustainable and cost-efficient manufacturing strategies.
Through its versatility, GD-OES has proven to be a powerful tool for not only optimizing LIB manufacturing processes but also gaining deeper insights into their aging mechanisms. This research extends beyond academic interest, offering tangible benefits for the industry by translating into improved battery quality, extended lifespan, and overall performance.
Im Rahmen der von der BAM und anderen Partnern ins Leben gerufenen Initiative „Digitale Qualitätsinfrastruktur“ liegt der Fokus u.a. auf der Entwicklung von neuen Zertifizierungsworkflows. Dabei ist eine besondere Bedeutung dem Zusammenführen von Operational Technology (OT) und Informationstechnik (IT) beizumessen. Zur Datenintegration aus der Sensor-Feldebene einer Versuchs-wasserstofftankstelle wurde eine solche Infrastruktur zunächst in einer Laborumgebung aufgebaut.
Faecal contaminants in water are considered serious threats for human health, due to the presence of viruses, bacteria and other harmful microorganisms.1 Urobilin (UB) is a well-known faecal pigment and can be used as a marker for faecal matter in water.2 UB is commonly present in the urine of all mammals as the catabolic end product of bilirubin degradation.2 As the only simple chemical approach to its detection, Schlesinger’s test is usually used to enhance the weak fluorescence of UB in alcoholic media by complexation with Zinc.2, 3 The major limitation of this method is the only weak enhancement of the intrinsically weak UB fluorescence in aqueous media.3 This work presents an approach to introduce different Zn salts for improved fluorescence response, where we found a clear dependence of the fluorescence yield of UB-Zn(II) complexes on the counterion of the salt in water. By employing a combination of fluorescence parameters like transition energy, fluorescence intensity, and fluorescence lifetime, a photophysical understanding of the structure and conformation of the UB-Zn(II) complexes responsible for the fluorescence enhancement in water could be gained. The possibilities of developing a sensitive analytical method based on the acquired understanding are also discussed.
Therapeutic monoclonal antibodies are the fastest-growing group of biological agents which generated a yearly turnover of USD 210 billion in 2022 and whose sales are expected to grow by 10% annually over the next 10 years. With steadily increasing market importance, analytical methods for reliable quantification of therapeutic antibodies also become more and more relevant. Liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) has become the main technology for antibody quantification. This approach, however, requires enzymatic digestion of the intact protein into peptides, for which a wide range of different protocols exists that often lead to different results depending on the digestion procedure or trypsin variants used. In particular, the amount and type of detergents added for protein unfolding prior to digestion is known to create significant bias in measurement results. The overall goal of the presented project is the application of novel thermostable and surface-functionalized trypsin particles for improved antibody digestion. Specifically, a trypsin-variant described in the literature exhibiting increased activity and thermal stability above 80°C, will be examined. The application of this enzyme should allow to perform digestion at elevated temperatures where the protein is naturally unfolding thereby increasing enzyme accessibility without the need for detergents. Furthermore, we will immobilize the thermostable trypsin onto the surface to further enhance enzyme stability, prevent self-digestion, and enable separation of trypsin from target peptides before LC–MS/MS analysis. As an immobilization platform, cheap and non-porous corundum particles will be used as these show high chemical stability and low levels of interaction of matrix proteins with the functionalized surface. adsorption. In a multidisciplinary collaboration with the SALSA Photonics Lab, we will investigate the characteristics of covalent enzyme binding and unspecific peptide binding using an interface-sensitive analytical tool, vibrational sum-frequency generation (VSFG) spectroscopy. The insights gained will not only lead to new competencies in peptide and enzyme surface analysis using VSFG spectroscopy in SALSA but will also significantly contribute to optimizing antibody quantification.
In this study, we demonstrate the applicability of nitrogen microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) for Ca, Fe, and Se quantification in human serum using isotope dilution (ID) analysis. The matrix tolerance of MICAP-MS in Na matrix was investigated, uncovering that high Na levels can suppress the signal intensity. This suppression is likely due to the plasma loading and the space charge effect. Moreover, 40Ca and 44Ca isotopic fractionation was noted at elevated Na concentration. Nine certified serum samples were analyzed using both external calibration and ID analysis. Overestimation of Cr, Zn, As, and Se was found in the results of external calibration, which might be resulted from C-induced polyatomic interference and signal enhancement, respectively. Further investigations performed with methanol showed a similar enhancement effect for Zn, As, and Se, potentially supporting this assumption. The mass concentrations determined with ID analysis show metrological compatibility with the reference values, indicating that MICAP-MS combined with ID analysis can be a promising method for precise Ca, Fe, and Se determination. Moreover, this combination reduces the influences of matrix effects, broadening the applicability of MICAP-MS for samples with complex matrix.
Antikörper sind in der medizinischen Welt nicht mehr wegzudenken. Ihr Einsatz-Repertoire als Therapeutika für die Behandlung diverser Krankheiten und Infektionen weitet sich von Jahr zu Jahr mehr aus. Dabei basiert ein Großteil der verwendeten Antikörper zu diesem Zeitpunkt auf monoklonalen Antikörpern auf Basis von Hybridomazellen. Doch hier könnten rekombinante Antikörper aufgrund ihrer Vektor-basierten Expression eine vielversprechende und womöglich sogar revolutionierende Alternative bieten. So ergeben sich neue Optimierungsoptionen für Merkmale wie Affinität, Stabilität und Kompatibilität über Anpassungen auf genetischer oder posttranslationaler Ebene. Allerdings ergibt sich kein Anwendungszweck ohne die vorhergehende detaillierte Charakterisierung der Antikörper. Denn nur mit spezifischem Wissen über die diversen Eigenschaften und Wechselwirkungen kann eine effektive und präzise Verwendung in der Diagnostik und Therapeutik gewährleistet werden und auf diese Weise Leben retten.
Aus diesem Grund beschäftigt sich diese Masterarbeit mit der Vertiefung der rekombinanten Antikörper-Thematik. Dazu soll ein Anti-Tetanus-Antikörper erstmals rekombinant in verschiedenen Zelllinien hergestellt und anschließend über umfangreiche analytische Verfahren mit einem Fokus auf die Einflussanalyse der unterschiedlichen posttranslationalen Glykosylierungen charakterisiert werden. Zu diesem Zweck wurden als Grundlage einerseits zwei P1316-Dual-Expressions-Vektoren mit variierenden Insert-Positionen der schweren und leichten Kette durch Gibson-Assembly sowie individuellen pRK5-Plasmide für eine separiert Expression der Antikkörperketten mithilfe Restriktionsfragment-Ligation generiert. In einer Gegenüberstellung der der Expressionsausbeuten stellte sich die Überlegenheit der P1316-Plasmid-Konfiguration heraus, in der das Leichtketten-Insert an der ersten Expressionsstelle positioniert ist. Deshalb wurde dieser Vektor als Ausgangspunkt für die anschließende hochskalierten Herstellung des Anti-Tetanus-Antikörpers in Expi293F-GnTI- und ExpiCHO-S-Zellen verwendet. Ein ELISA bestätigte die Bindungsaktivität der rekombinanten Antikörper am Tetanus-Toxoid unabhängig vom Expressionssystem. Nach einer folgenden Optimierung der für die Aufreinigung verwendeten Protein-A-Affinitätschromatographie, wurde über weitere Charakterisierungsmethoden wie Größenausschlusschromatographie und dynamische Lichtstreuung eine vergleichbare Aggregation aufgrund der sauren Elution aufgezeigt. In diesem Kontext wurde die Notwendigkeit einer Zweistufen-Präparation mit Affinitäts- und Größenausschlusschromatografie für den Erhalt monodisperser Proben verdeutlicht. Zudem wurden die verschiedenen intakten Massen mitsamt ihrer spezifischen Glykan-abhängigen Streumaßen in Relation zum monoklonalen NISTmAB-Referenzantikörper bestimmt. Dabei konnte den Erwartungen nach sowohl die geringere Masse als auch die uniformere Glykosylierung der in Expi293 GnTI- exprimierten Immunoglobuline in Relation zum ExpiCHO-S-Antikörper nachgewiesen werden. Anschließend wurde das Stabilitätsverhalten mittels thermischer Entfaltung und dynamischer Lichtstreuung über einen ausgeweiteten Zeitraum sowie verschiedenen Temperaturen dokumentiert. Grundlegend wurde eine höhere thermische Stabilität der zweiten konstanten Schwerketten-Domäne des aus ExpiCHO-S-Zellen stammenden Antikörpers nachgewiesen. Außerdem konnte eine problemlose Lagerungsfähigkeit beider unterschiedlich glykosylierter Antikörper bei Raumtemperatur für mindestens 4 Wochen festgestellt werden. Des Weiteren wurde die Langzeitlagerung im Rahmen der Auswirkung von Gefrier-Auftau-Zyklen mit gleichbleibenden Methoden sowie zusätzlicher Größenausschlusschromatographie erprobt. Hierbei stellte sich der Erhalt der strukturellen Integrität nach bis zu 15 Zyklen heraus. Allerdings geht die Monodispersität bereits nach wenigen Zyklen verloren, wobei die geringfügiger glykosylierten Expi293F-GnTI-Anti-Tetanus-Antikörper eine stärkere Beeinträchtigung durch multiple Gefrier-Auftau-Zyklen aufwiesen.
This technical note highlights the fact that CF-LIBS algorithms work in mole fractions, while results of spectrochemical analysis are usually reported in mass fractions or mass percent. Ignoring this difference and not converting mole fractions to mass fractions can lead to errors in reported concentrations determined by the CF-LIBS method and inadequate comparison of these concentrations with certified concentrations. Here, the key points of the CF-LIBS algorithm are reproduced and the formulae for converting a mole fraction to a mass fraction and vice versa are given. Several numerical examples are also given, which show that the greater the difference between the molar mass of an individual element in a sample and the average molar mass, the greater the discrepancy between the mole and mass fractions.
Solvent-free sample preparation offers some advantages over solvent-based techniques, such as improved accuracy, reproducibility and sensitivity, for matrix-assisted laser desorption/ionization (MALDI) analysis. However, little or no information is available on the application of solvent-free techniques for the MALDI analysis of polymer blends. Solvent-free sample preparation by ball milling was applied with varying sample-to-matrix ratios for MALDI time-of-flight mass spectrometry analysis of various polymers, including polystyrenes, poly(methyl methacrylate)s and poly(ethylene glycol)s. The peak intensity ratios were compared with those obtained after using the conventional dried droplet sample preparation method. In addition, solvent-assisted milling was also applied to improve sample homogeneities.
Depending on the sample preparation method used, different peak intensity ratios were found, showing varying degrees of suppression of the signal intensities of higher mass polymers. Ball milling for up to 30 min was required to achieve constant intensity ratios indicating homogeneous mixtures. The use of wet-assisted grinding to improve the homogeneity of the blends was found to be disadvantageous as it caused partial degradation and mass-dependent segregation of the polymers in the vials.The results clearly show that solvent-free sample preparation must be carefully considered when applied to synthetic polymer blends, as it may cause additional problems with regard to homogeneity and stability of the blends.
Die Angabe von Unsicherheiten bei zertifizierten Werten von Referenzmaterialien ist von entscheidender Bedeutung. Die korrekte Einbindung der Unsicherheiten zur Berechnung von Verfahrensmessunsicherheiten ist wesentlich für die Gewährleistung der Genauigkeit und Zuverlässigkeit von Messungen. In diesem Vortrag werden die verschiedenen Einflussfaktoren auf die Unsicherheit zertifizierter Werte gemäß ISO Guide 35 dargestellt. Dabei werden insbesondere die Charakterisierung, Homogenität und Stabilität als entscheidende Faktoren für die Bestimmung der Unsicherheit eines Referenzmaterials betrachtet. Abschließend wird das Konzept anhand eines konkreten Beispiels veranschaulicht, um die praktische Anwendung und die Auswirkungen auf die Berechnung von Verfahrensmessunsicherheiten zu verdeutlichen.
This is a set of use examples for the HDF5Translator framework. This framework lets you translate measurement files into a different (e.g. NeXus-compatible) structure, with some optional checks and conversions on the way. For an in-depth look at what it does, there is a blog post here.
The use examples provided herein are each accompanied by the measurement data necessary to test and replicate the conversion. The README.md files in each example show the steps necessary to do the conversion for each.
We encourage those who have used or adapted one or more of these exampes to create their own conversion, to get in touch with us so we may add your example to the set.
qNMR - The handbook
(2023)
Quantitative NMR (qNMR) has been around for a long time, but also has great potential to solve future problems in any quantitative analysis. As a primary method, it differs fundamentally from chromatographic methods: it is better described as a quantum mechanical balance. Succesful implementation of qNMR requires certain attention to detail. "qNMR - the handbook" is intended to be a guide for analysts to help understand the fundamental principles of NMR and the significant points relating to its implementation for quantitation. Regulatory considerations of qNMR adoption are explained. NMR fundamentals are explained to provide understanding. Together with many useful examples, the book is a compelling addition to the laboratory's reference library, providing all the tools that any practitioner should know to successfully implement qNMR.
The authors are qNMR pioneers and come from a variety of backgrounds including business, government and academia.
In situ chemical analysis of duplex stainless steel weld by laser induced breakdown spectroscopy
(2024)
The high corrosion resistance and good mechanical properties of duplex stainless steel (DSS) are due to its special chemical composition, which is a balanced phase ratio of ferrite (α) and austenite (γ). Many industrial applications require the integration of DSS components. For this, Gas tungsten arc welding (GTAW) is an excellent choice, as it allows an automated operation with high reproducibility. However, when the weld pool solidifies, critical ratios of α- and γ- phases can occur, which lead to solidification cracking, increased susceptibility to corrosion, and a decrease in ductility and critical strength. Previous studies have shown that these defects can be caused by the accumulation of manganese and chromium in the heat affected zone (HAZ), requiring ongoing monitoring of this accumulation. A suitable method for such monitoring is laser-induced breakdown spectroscopy (LIBS), which can be used in two operating modes: calibration using standard reference samples and calibration-free. Unlike conventional quantitative LIBS measurements, which require reference samples to generate a calibration curve, calibration-free LIBS (CF-LIBS) allows chemical compositions to be determined solely from the emission spectrum of the plasma. Numerous publications show that CF-LIBS is a fast and efficient analytical method for the quantitative analysis of metal samples. In this work, CF-LIBS is applied to spectra obtained during GTAW DSS welding and the result is compared with those obtained by PLS analysis. A good correlation was found between both types of analysis, demonstrating the suitability of the CF-LIBS method for this application. The CF-LIBS method has a significant advantage over conventional LIBS due to the rapid in situ measurement of concentrations of major alloying elements without calibration procedure. This, combined with fast feedback and appropriate adjustment of welding parameters, helps prevent welding defects.
Die Pulskompression wird in der Radartechnik eingesetzt, um den Signal-Rausch-Abstand zu erhöhen. Das Ziel ist es die Entdeckungswahrscheinlichkeit eines Nutzsignals bei gleichbleibender Auflösung zu erhöhen. Durch den Einsatz von Barker Codes oder komplementären Golay Codes werden Sendesignale von Luftultraschallanwendungen pulscodiert. Dies ermöglicht in der zerstörungsfreien Prüfung die Inspektion von dickeren Bauteilen, da die Signalenergie durch zeitlich gestreckte Sendesignale bei gleicher Auflösung vergrößert wird.
In dieser Arbeit wird die Pulskompression durch die Einführung von unipolaren Sequenzen zur Pulscodierung für thermoakustische Ultraschallwandler ermöglicht. Der Signal-Rausch-Abstand wird in der Anwendung der Pulscodierung und anschließenden Filterung mit einem signalangepassten Filter in Luftultraschallmessungen mit dem thermoakustischen Wandler und Wandlern aus zellulärem Polypropylen erhöht.
Heterogeneous sandwich immunoassays are widely used for biomarker detection in bioanalysis and medical diagnostics. The high analyte sensitivity of the current “gold standard” enzyme-linked immunosorbent assay (ELISA) originates from the signal-generating enzymatic amplification step, yielding a high number of optically detectable reporter molecules. For future point-of-care testing (POCT) and point-of-need applications, there is an increasing interest in more simple detection strategies that circumvent time-consuming and temperature-dependent enzymatic reactions. A common concept to aim for detection limits comparable to those of enzymatic amplification reactions is the usage of polymer nanoparticles (NP) stained with a large number of chromophores. We explored different simple NP-based signal amplification strategies for heterogeneous sandwich immunoassays
that rely on an extraction-triggered release step of different types of optically detectable reporters. Therefore, streptavidinfunctionalized polystyrene particles (PSP) are utilized as carriers for (i) the fluorescent dye coumarin 153 (C153) and (ii) hemin (hem) molecules catalyzing the luminol reaction enabling chemiluminescence (CL) detection. Additionally, (iii) NP labeling with hemin-based microperoxidase MP11 was assessed. For each amplification approach, the PSP was first systematically optimized regarding size, loading concentration, and surface chemistry. Then, for an immunoassay for the inflammation marker C- eactive protein (CRP), the analyte sensitivity achievable with optimized PSP
ystems was compared with the established ELISA concept for photometric and CL detection. Careful optimization led to a limit of detection (LOD) of 0.1 ng/mL for MP11-labeled PSP and CL detection, performing similarly well to a photometric ELISA (0.13 ng/mL), which demonstrates the huge potential of our novel assay concept.
SWIR luminescent nanomaterials – key chemical parameters for bright probes for in vivo bioimaging
(2024)
A current challenge for studying physio-pathological phenomena and diseaserelated processes in living organisms with non-invasive optical bioimaging is the development of bright optical reporters that enable deep tissue penetration, a high detection sensitivity, and a high spatial and temporal resolution. The focus of this project are nanomaterials, which absorb and emit in the shortwave infrared (SWIR) between ~900–2500 nm where scattering, absorption, and autofluorescence of the tissue are strongly reduced compared to the visible and NIR.
The frequency-domain (FD) method provides an alternative to the commonly used time-domain (TD) approach in characterizing the luminescence kinetics of luminophores, with its own strengths, e.g., the capability to decouple multiple lifetime components with higher reliability and accuracy. While extensively explored for characterizing luminophores with down-shifted emission, this method has not been investigated for studying nonlinear luminescent materials such as lanthanide-doped upconversion nanoparticles (UCNPs), featuring more complicated kinetics. In this work, employing a simplified rate-equation model representing a standard two-photon energy-transfer upconversion process, we thoroughly analyzed the response of the luminescence of UCNPs in the FD method. We found that the FD method can potentially obtain from a single experiment the effective decay rates of three critical energy states of the sensitizer/activator ions involved in the upconversion process. The validity of the FD method is demonstrated by experimental data, agreeing reasonably well with the results obtained by TD methods.
Four donor-acceptor boron difluoride complexes based on the carbazole electron donor and the [1,3,5,2]oxadiazaborinino[3,4-a][1,8]naphthyridine acceptor were designed, synthesized, and systematically spectroscopically investigated in solutions, in the solid states, and dye-doped polymer films. The dyes exhibit an intense blue to red solid-state emission with photoluminescence quantum yields of up to 56% in pure dye samples and 86% in poly(methyl methacrylate) films. All boron complexes show aggregation-induced emission and reversible mechanofluorochromism. The optical properties of these dyes and their solid state luminescence can be tuned by substitution pattern, i.e., the substituents at the naphthyridine unit. Exchange of CH3- for CF3-groups does not only increase the intramolecular charge transfer character, but also provides a crystallization-induced emission enhancement.
Antibacterial photodynamic therapy (a‐PDT) has emerged as a promising non‐invasive therapeutic modality that utilizes the combination of a photosensitive agent, molecular oxygen, and excitation light to generate reactive oxygen species (ROS), demonstrating remarkable activity against multidrug‐resistant bacterial infections. However, the effective use of conventional photosensitizers is significantly limited by a number of their shortcomings, namely, poor water solubility and low selectivity. Herein, we present a novel biocompatible water‐soluble nanocomposite based on hydrophobic tetraphenylporphyrin (TPP) molecules and hydrophilic ternary AgInS2/ZnS quantum dots incorporated into a chitosan matrix as an improved photosensitizer for a‐PDT. We demonstrated that TPP molecules could be successfully transferred into chitosan solution while remaining primarily in the form of monomers, which are capable of singlet oxygen generation. We performed a detailed analysis of the Förster resonance energy transfer (FRET) between quantum dots and TPP molecules within the nanocomposite and proposed the mechanism of the singlet oxygen efficiency enhancement via FRET.
A poly(L-lactide) with a trifluoroethyl ester end group and an average degree of polymerization (DP) of 50 was synthesized by ROP of L-lactide initiated with trifluoroethanol. Small-angle X-ray scattering (SAXS) in combination with differential scanning calorimetry (DSC) measurements revealed an average crystal thickness of 13 nm, corresponding to 45 repeat units. This suggests that most crystallites were formed by extended PLA chains, and both flat surfaces were covered by CF3 groups. The crystalline PLAs were annealed at 140 or 160 °C in the presence of two catalysts: tin(II) 2-ethylhexanoate, (SnOct2) or dibutyltin bis(pentafluorophenoxide) (BuSnPhF). The chemical reactions, such as polycondensation and cyclization, proceeded in the solid state and were monitored by matrix-assisted laser desorption/ionization time-offlight (MALDI TOF) mass spectrometry and gel permeation chromatography (GPC) measurements. Under optimal conditions a large fraction of linear chains was transformed into crystallites composed of extended cycles. Additionally, MALDI TOF MS analysis of GPC fractions from samples annealed for 28 or 42 days detected chain elongation of the linear species up to a factor of 20.
In einer Versuchsreihe im Realmaßstab wurden drei Flüssigwasserstofftanks (LH2) unterfeuert. Hierbei sollte unter anderem geklärt werden, ob es, analog zu druckverflüssigten Gasen, zu einem BLEVE (Boiling Liquid Expanding Vapor Cloud Explosion) kommen kann. Die Experimente wurden auf dem Testareal Wasserstoffsicherheit des Testgeländes Technische Sicherheit der Bundesanstalt für Materialforschung und -prüfung (BAM-TTS) im Rahmen einer Forschungskooperation zwischen der BAM und Gexcon, als Teil des SH2IFT-Programms durchgeführt. Es handelte sich um doppelwandige, vakuumisolierte Tanks von 1 m³ Volumen. Die zylindrischen Tanks unterschieden sich durch ihre Ausrichtung (horizontal oder vertikal) und das verwendete Isoliermaterial (Perlit oder Mehrschichtisolierung (MLI). Der Füllgrad der Tanks betrug bei jedem der durchgeführten Tests etwa 35-40 %. Die Brandlast wurde homogen durch ein propangasbetriebenes Brennersystem erzeugt. Gemessen wurden die Bedingungen im Behälter (Temperaturen und Druck) sowie äußere Randbedingungen und Auswirkungen beim Versagen (Wärmestrahlung, Druckwellen, Flammenballentwicklung und Fragmentierung). Mit Bolometern wurde die Wärmestrahlung gemessen, die sowohl durch das Propanfeuer als auch durch einen möglichen Feuerball/BLEVE erzeugt wurde. Zur Messung der durch das Bersten von Behältern/BLEVEs erzeugten Druckwellen wurden sog. Pencil-Probes verwendet. Des Weiteren wurden mehrere Kameras zur Überwachung der Experimente eingesetzt: Normalbildkameras, Infrarot (IR)-Kameras und Hochgeschwindigkeitskameras, sowohl bodengestützt als auch mittels einer Drohne. Zwei der untersuchten Tanks, ein horizontaler und der vertikale, die beide mit Perlit isoliert waren, hielten der Brandbelastung stand, ohne dass es zu einem Behälterversagen kam. Der mit MLI isolierte horizontale Behälter barst nach 1 Stunde und 6 Minuten und erzeugte dabei einen Feuerball, Trümmerflug und eine Druckwelle. Neben der Beschreibung der Auswirkungen eines kritischen Versagens eines LH2-Tanks sind weitere Ziele der Arbeit die Identifizierung kritischer Behälterzustände sowie die Erstellung eines umfassendes Datensatzes der Trümmer des geborstenen Tanks. Die größten Abstände für kritische Abstände ergaben sich durch Fragmentwurf. Hier sollen 3D-Scans für die Verwendung in CAD und FEM Anwendungen bereitgestellt werden. Umfassende Daten zu den Fragmentwurfweiten, -massen und -positionen wurden bereits publiziert. Damit soll die Voraussetzung geschaffen werden, um vorhandene Wurfweitenmodelle, die bisher nur für einschalige Behälter konzipiert wurden auf ihre Eignung für mehrschalige Behälter zu überprüfen oder mögliche Anpassungen anhand der realen Daten vornehmen zu können.
Zudem wurde damit begonnen die nicht geborstenen Tanks zu vermessen und zu zerlegen, um u.a. die Perlit-Schüttung auf Beeinträchtigungen durch den Transport und die Unterfeuerung zu untersuchen.
In einer Reihe von Experimenten wurden die möglichen Folgen der Freisetzung von verflüssigtem Wasserstoff (LH2) auf, bzw. unter Wasser untersucht. Die Experimente zielten darauf ab, eine unbeabsichtigte Freisetzung von LH2 (z.B. durch Schlauchabriss) insbesondere bei der Betankung eines Schiffes zu simulieren. Für verflüssigtes Erdgas (LNG) wurden dabei sog. RPT’s (rapid phase transition) nachgewiesen, bei denen die spontane Verdampfung relevante Druckwellen erzeugt. Es kann nicht ausgeschlossen werden, dass RPTs auch im Falle von LH2 möglich sind. Die Versuche wurden auf dem Testareal Wasserstoffsicherheit auf dem Testgelände Technische Sicherheit der Bundesanstalt für Materialforschung und -prüfung (BAM-TTS) in Horstwalde, im Rahmen einer Forschungskooperation zwischen der BAM und Gexcon im Rahmen des SH2IFT-Programms durchgeführt. Die LH2-Freisetzungen erfolgten direkt aus einem LH2-Tanklastwagen über eine lange, flexible, vakuumisolierte Transferleitung. Während die Freisetzung oberhalb und unterhalb der Wasseroberfläche jeweils vertikal orientiert war, wurde bei der Unterwasserfreisetzung zusätzlich eine horizontale Ausströmung, parallel zur Wasseroberfläche realisiert. Zur Bestimmung des Massenstromes, wurde ein Wägesystem unter dem Tankwagen eingesetzt. Spezielle Drucksensoren wurden verwendet, um die durch die Freisetzungsvorgänge erzeugten Stoßwellen sowohl im Wasser als auch in der Luft zu messen. Die Gaskonzentrationen über dem Wasserbecken wurden an verschiedenen Positionen gemessen. Hochgeschwindigkeits-, Infrarot- (IR) und normale Kameras wurden eingesetzt, um die Phänomenologie der Freisetzung aufzuzeichnen und das Verhalten der Gaswolke im Zeitverlauf zu verfolgen. Neben den fest installierten Systemen an Land, kamen auch Unterwasserkameras sowie eine Drohne mit Normal- und IR-Kameras zum Einsatz.
Zwei Wetterstationen wurden zur Messung von Windgeschwindigkeit, Windrichtung, Temperatur und Luftfeuchtigkeit während aller durchgeführten Tests eingesetzt. Des Weiteren kamen Bolometer zur Wärmestrahlungsmessung zum Einsatz. Zwar führten die Freisetzung zu einer hochturbulenten LH2/Wasser Mischzone, jedoch zu keinen nennenswerten Überdrücken durch RPT. Im Gegensatz dazu wurde unerwartet, aber reproduzierbar, eine Zündung der Gaswolke in freier Luft in einiger Entfernung von den Instrumenten und dem Ort der Freisetzung beobachtet. Die daraus resultierenden Gaswolkenexplosionen führten zu relevanten Überdrücken und zur Wärmeabstrahlung in die Umgebung.
Trinamic TMCL IOC is a Python package designed for controlling stepper motors connected to a Trinamic board using the TMCL language (all boards supported by PyTrinamic should now work, has been tested on the TMCM 6110 and the TMCM 6214). Since it is implementing the TMCL protocol, it should be easy to adapt to other Trinamic motor controller boards. This package assumes the motor controller is connected over a machine network via a network-to-serial converter, but the underlying PyTrinamic package allows for other connections too.
This allows the control of attached motors via the EPICS Channel-Access virtual communications bus. If EPICS is not desired, plain Pythonic control via motion_control should also be possible. An example for this will be provided in the example.ipynb Jupyter notebook.
This package leverages Caproto for EPICS IOCs and a modified PyTrinamic library for the motor board control, and interfaces between the two via an internal set of dataclasses. Configuration for the motors and boards are loaded from YAML files (see tests/testdata/example_config.yaml).
The modifications to PyTrinamic involved extending their library with a socket interface. This was a minor modification that should eventually find its way into the official package (a pull request has been submitted).
Technische Regeln im Arbeitsschutz – wie TRBS für die Betriebssicherheitsverordnung und TRGS für die Gefahrstoffverordnung – sind nicht zwingendes Recht, sondern konkretisierende Empfehlungen mit Vermutungswirkung. In Gerichtsurteilen werden sie eher selten herangezogen. Wie diese – und Branchenregelungen von Verbänden – von der Rechtsprechung diskutiert werden, zeigt ein Urteil des Verwaltungsgerichts Münster.
A novel distributed acoustic sensing technique is proposed that exploits both phase and amplitude of the Rayleigh backscattered light to quantify the environmental variation. The system employs a wavelength-scanning laser and an imbalanced Mach-Zehnder interferometer to acquire the reflection spectra and the phase of the detected light, respectively. Fading-free and low-frequency measurements are realized via the crosscorrelation of the reflection spectra. The discrete crosscorrelation is used to circumvent the nonlinear frequency sweeping of the laser. Based on the phase of the backscattered light, it is possible to quantify fast environmental variations. The whole system requires no hardware modification of the existing system and its functionality is experimentally validated. The proposed system has the potential to monitor ground motion/movement at very low frequency band like subsidence around mining areas and at high frequency band like earthquakes and vibrations induced by avalanches.
The development of new fluorescent organic probes effective in the NIR-II region is currently a fast-growing field and represents a challenge in the domain of medical imaging. In this study, we have designed and synthesized an innovative series of aza-boron dipyrromethenes emitting in the NIR-II region. We have investigated the effect of different water-solubilizing groups not only on the photophysical properties of the compounds but also on their in vitro and in vivo performance after bioconjugation to the antibody trastuzumab. Remarkably, we discovered that the most lipophilic compound unexpectedly displayed the most favorable in vivo properties after bioconjugation. This underlines the profound influence that the fluorophore functionalization approach can have on the efficiency of the resulting imaging agent.
Metabolomics
(2024)
The BAM Data Store
(2023)
As a partner in several NFDI consortia, the Bundesanstalt für Materialforschung und -prüfung (BAM, German federal institute for materials science and testing) contributes to research data standardization efforts in various domains of materials science and engineering (MSE). To implement a central research data management (RDM) infrastructure that meets the requirements of MSE groups at BAM, we initiated the Data Store pilot project in 2021. The resulting infrastructure should enable researchers to digitally document research processes and store related data in a standardized and interoperable manner. As a software solution, we chose openBIS, an open-source framework that is increasingly being used for RDM in MSE communities.
The pilot project was conducted for one year with five research groups across different organizational units and MSE disciplines. The main results are presented for the use case “nanoPlattform”. The group registered experimental steps and linked associated instruments and chemicals in the Data Store to ensure full traceability of data related to the synthesis of ~400 nanomaterials. The system also supported researchers in implementing RDM practices in their workflows, e.g., by automating data import and documentation and by integrating infrastructure for data analysis.
Based on the promising results of the pilot phase, we will roll out the Data Store as the central RDM infrastructure of BAM starting in 2023. We further aim to develop openBIS plugins, metadata standards, and RDM workflows to contribute to the openBIS community and to foster RDM in MSE.
Angesichts der zunehmenden Digitalisierung und dem Einsatz datenintensiver Methodiken in der Wissenschaft stehen Forschende vor der Herausforderung, stetig wachsende Datenmengen nachvollziehbar zu dokumentieren, langfristig zu speichern und für Dritte nachnutzbar zu machen. Um diesen Anforderungen gerecht zu werden, bietet sich die Nutzung von Software-Lösungen an, welche Forschungsdatenmanagement mit der digitalen Dokumentation von Laborinventar und Experimenten in elektronischen Laborbüchern (engl. electronic lab notebooks (ELN)) verknüpfen.
Oxidative degradation processes of tetrabromobisphenol A (TBBPA), a brominated flame retardant (BFR) in wood, plastics and electronics, were investigated by electrochemistry (EC) coupled online to electrospray ionization mass spectrometry (ESI/MS). Oxidative phase I and II metabolites production was achieved using an electrochemical flow-through cell equipped with a boron doped diamond electrode. Structural elucidation and prediction of oxidative metabolism pathways of TBBPA according to type II ipso-substitution were based on retention time, m/z ratio in negative mode and fragmentation pattern. Using the data obtained through high resolution MS analysis and the identification of single electron transfer (SET) as the initial step of a two-electron oxidation provided the necessary information to propose a mechanism for the electrochemical oxidation of TBBPA. Oxidation reactions involving aromatic hydroxylation and β-scission were the main degradation observed when studying the electrochemical behavior of TBBPA. Computational chemistry experiments using density functional theory (DFT) allowed to identify mono-hydroxylated reaction intermediate and dismissed the mechanism involving two concurrent hydroxylation. TBBPA oxidation products were compared to known metabolites of its biological and environmental degradation confirming the ability of electrochemistry to simulate β-scission reactions.
Plastic pollution is the biggest environmental concern of our time. Breakdown products like micro- and nanoplastics inevitably enter the food chain and pose unprecedented health risks. In this scenario, bio-based and biodegradable plastic alternatives have been given a momentum aiming to bridge a transition towards a more sustainable future. Polyhydroxyalkanoates (PHAs) are one of the few thermoplastic polymers synthesized 100 % via biotechnological routes which fully biodegrade in common natural environments. Poly(hydroxybutyrate-cohydroxyhexanoate) [P(HB-co-HHx)] is a PHA copolymer with great potential for the commodity polymers industry, as its mechanical properties can be tailored through fine-tuning of its molar HHx content. We have recently developed a strategy that enables for reliable tailoring of the monomer content of P(HB-co-HHx).
Nevertheless, there is often a lack of comprehensive investigation of the material properties of PHAs to evaluate whether they actually mimic the functionalities of conventional plastics. We present a detailed study of P(HB-co-HHx) copolymers with low to moderate hydroxyhexanoate content to understand how the HHx monomer content influences the thermal and mechanical properties and to link those to their abiotic degradation. By increasing the HHx fractions in the range of 2 – 14 mol%, we impart an extension of the processing window and application range as the melting temperature (Tm) and glass temperature (Tg) of the copolymers decrease from Tm 165 ◦C to 126 ◦C, Tg 4 ◦C to − 5.9 ◦C, accompanied by reduced crystallinity from 54 % to 20 %.
Elongation at break was increased from 5.7 % up to 703 % at 14 mol% HHx content, confirming that the range examined was sufficiently large to obtain ductile and brittle copolymers, while tensile strength was maintained throughout the studied range. Finally, accelerated abiotic degradation was shown to be slowed down with an increasing HHx fraction decreasing from 70 % to 55 % in 12 h.
With the reduction of large oil spills because of stricter regulations and safety measures, the question of how to manage smaller oil spills arises. Few on-site analytical tools are available for first responders or other law enforcement personnel to rapidly test for crude oil in the early management of localized polluted areas. The approach reported here relies on well-described computer-assisted multivariate data analysis of the intrinsic fluorescence fingerprints of crude oils to build a multivariate model for the rapid classification of crude oils and the prediction of their properties. Thanks to a dedicated robust portable reader, the method allowed classification and accurate prediction of various properties of crude oil samples like density (according to API, the American Petroleum Institute and viscosity as well as composition parameters such as volume fractions of paraffins or aromatics. In this way, autonomous operation in on-site or in-the-field applications becomes possible based on the direct (undiluted and untreated) measurement of samples and a rapid, tablet-operated readout system to yield a robust and simple analytical test with superior performance. Testing in real-life scenarios allowed the successful classification and prediction of a number of oil spill samples as well as weathered samples that closely resemble samples collected by first responders.
As part of the development of a new standard testing procedure, a round robin study was conducted by six participating laboratories. This study involved the measurement of both the maximum explosion pressure and the maximum rate of pressure rise for hybrid mixtures comprising dust and vapor. Measurements were performed using a modified 20L-sphere. The primary objective of this collaborative effort was to assess the accuracy, reliability, and consistency of analytical and measurement methods across multiple laboratories, thereby increasing confidence in the obtained results. The method and protocol were developed as part of the NEX-HYS project and documented in a technical specification by the German Institute for Standardization Registered Association (DIN). The study revealed that precise pre-ignition pressure rise (PIPR) measurements and the use of a leak-free test apparatus significantly influenced the results of the measured maximum explosion pressure and maximum pressure rise rate.
This document constitutes the Strategic Research Agenda (SRA) for the European Metrology Network for Mathematics and Statistics in Metrology (EMN Mathmet). The EMN Mathmet is an alliance of European National Metrology Institutes (NMIs), Designated Institutes (DIs) and an EMN Partner that aims to strengthen research and cooperation in the field. The SRA has been developed within a European project (EMPIR 18NET05 MATHMET) to promote and support the network. The SRA was developed based on a consultation process with stakeholders and the strategies of individual NMIs and DIs, and in alignment with the EURAMET 2030 strategy.
As a key result, the SRA defines a long-term research goal: the EMN Mathmet will coordinate research to strengthen the trust in algorithms, software tools and data to underpin digital transformation. For this purpose, new emerging research topics where algorithms, software tools and data play a significant role were identified: (i) Artificial Intelligence and Machine Learning, and (ii) Computational Modelling and Virtual Metrology. The foundation for the development of these new topics is given by the traditional focus on (iii) Data Analysis and Uncertainty Evaluation. The SRA characterises the future needs and challenges in the field of mathematics and statistics in metrology and provides an outline of how the EMN Mathmet can meet these new emerging requirements.
In industrialised countries more than 80% of the time is spent indoors. Products, such as building materials and furniture, emit volatile organic compounds (VOCs), which are therefore ubiquitous in indoor air. VOC in combination may, under certain environmental and occupational conditions, result in reported sensory irritation and health complaints. Emission concentrations can become further elevated in new or refurbished buildings where the rate of air exchange with fresh ambient air may be limited due to improved energy saving aspects. A healthy indoor environment can be achieved by controlling the sources and by eliminating or limiting the release of harmful substances into the air. One way is to use (building) materials proved to be low emitting. Meanwhile, a worldwide network of professional commercial and non-commercial laboratories performing emission tests for the evaluation of products for interior use has been established. Therefore, comparability of test results must be ensured. A laboratory’s proficiency can be proven by internal and external validation measures that both include the application of suitable emission reference materials (ERM). For the emission test chamber procedure according to EN 16516, no artificial ERM is commercially available. The EU-funded EMPIR project MetrIAQ aims to fill this gap by developing new and improved ERMs. The goal is to obtain a material with a reproducible and temporally constant compound release (less than 10 % variability over 14 days). Two approaches were tested: the impregnation of porous materials with VOC, and the encapsulation of VOC in polymer microcapsules. Impregnation is performed with help of an autoclave and supercritical CO2. The encapsulation is done by interfacial polymerisation on VOC droplets. For both approaches, synthesis and/or material parameters were varied to obtain an optimal ERM. Findings about the optimisation of ERM generation, as well as performance of the best emission reference materials, will be presented.
The principles of (Hard) X-ray photoelectron spectroscopy and some application in the field of (core-shell) nanoparticles will be presented. The presentation should answer hoe to get reliable results. Furthermore, examples of the correlation between physical-chemical measurments and toxicological results are given which are crucial for the risk assessment of nanoparticles.
Capillary electrophoresis (CE) is a powerful and sensitive tool for speciation analysis when combined with inductively coupled plasma mass spectrometry (ICP-MS); however, the performance of this technique can be limited by the nature of pneumatic nebulizers. This study compares two commercially available pneumatic nebulizers to a newly introduced vibrating capillary nebulizer (VCN) for on-line coupling of CE with ICP-MS. The VCN is a low-cost, non-pneumatic nebulizer that is based on the design of capillary vibrating sharp-edge spray ionization. As a piezoelectrically driven nebulization source, the VCN creates an aerosol independent of gas flows and does not produce a low-pressure region at the nebulizer orifice.
To compare the systems, we performed replicate analyses of sulfate in river water with each nebulizer and the same CE and ICP-MS instruments and determined the figures of merit of each setup. With the CE-VCN-ICP-MS setup, we achieved around 2–4 times lower sensitivity compared to the commercial setups. However, the VCN-based setup provided lower noise levels and better linear correlation from the analysis of calibration standards, which resulted in indistinguishable LOD and LOQ values from the in-house-built VCN-based and commercial setups for CE-ICP-MS analysis. The VCN is found to have the highest baseline stability with a standard deviation of 3500 cts s−1, corresponding to an RSD of 2.7%. High reproducibility is found with the VCN with a peak area RSD of 4.1% between 3 replicate measurements.
We report an analytical methodology for the quantification of sulfur in biological molecules via a speciesunspecific postcolumn isotope dilution (online ID) approach using capillary electrophoresis (CE) coupled online with inductively coupled plasma−mass spectrometry (online ID CE/ICP−MS).
The method was optimized using a mixture of standard compounds including sulfate, methionine, cysteine, cystine, and albumin, yielding compound recoveries between 98 and 105%. The quantity of sulfur is further converted to the quantity of the compounds owing to the prior knowledge of the sulfur content in the molecules. The limit of detection and limit of quantification of sulfur in the compounds were 1.3−2.6 and 4.1−8.4 mg L−1, respectively, with a correlation coefficient of 0.99 within the concentration range of sulfur of 5−100 mg L−1. The capability of the method was extended to quantify albumin in its native matrix (i.e., in serum) using experimentally prepared serum spiked with a pure albumin standard for validation. The relative expanded uncertainty of the method for the quantification of albumin was 6.7% (k = 2). Finally, we tested the applicability of the method on real samples by the analysis of albumin in bovine and human sera. For automated data assessment, a software application (IsoCor) which was developed by us in a previous work was developed further for handling of online ID data. The method has several improvements compared to previously published setups: (i) reduced adsorption of proteins onto the capillary wall owing to a special capillary-coating procedure, (ii) baseline separation of the compounds in less than 30 min via CE, (iii) quantification of several sulfur species within one run by means of the online setup, (iv) SI traceability of the quantification results through online ID, and (v) facilitated data processing of the transient signals using the IsoCor application. Our method can be used as an accurate approach for quantification of proteins and other biological molecules via sulfur analysis in complex matrices for various fields, such as environmental, biological, and pharmaceutical studies as well as clinical diagnosis.
Sulfur is an essential element in living organisms, where it plays important roles in various biological processes, such as protein synthesis, enzyme activity, and antioxidant defense. However, the biological effects of different sulfur species can vary widely, and imbalances in sulfur speciation have been observed in a range of diseases, including cancer, Alzheimer’s disease, and diabetes.1−3 The accurate quantification of sulfur and its species in biological samples requires sensitive and selective analytical techniques. In recent years, separation techniques coupled online with inductively coupled plasma−mass spectrometry (ICP−MS) have emerged as powerful online analytical tools complementary to molecular spectrometric methods for speciation analysis of biological compounds.
External calibration4−9 and isotope dilution (ID)10−15 are common calibration approaches applied for online quantification of sulfur species in complex samples. The ID analysis is advantageous over.
An observation of the fracture process in front of the crack tip inside a dentin sample by means of ex-situ X-ray computed tomography after uniaxial compression at different deformation values was carried out in this work. This ex-situ approach allowed the microstructure and fracturing process of human dentin to be observed during loading. No cracks are observed up to the middle part of the irreversible deformation in the samples at least visible at 0.4μm resolution. First cracks appeared before the mechanical stress reached the compression strength. The growth of the cracks is realized by connecting the main cracks with satellite cracks that lie ahead of the main crack tip and parallel its trajectory. When under the stress load the deformation in the sample exceeds the deformation at the compression strength of dentin, an appearance of micro-cracks in front of the main cracks is observed. The micro-cracks are inclined (~60°) to the trajectory of the main cracks. The further growth of the main cracks is not realized due to the junction with the micro-cracks; we assume that the micro-cracks dissipate the energy of the main crack and suppressed its growth. These micro-cracks serve as additional stress accommodations, therefore the samples do not break apart after the compression test, as it is usually observed under bending and tension tests.