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Society for Applied Spectroscopy (SAS) Atomic Section Student Award.
Magnesium is a major element in the hydrosphere and biosphere and plays important roles in (bio-) geochemical and physiological cycles. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg. It is due to their relatively large mass difference (~8% between) that isotope fractionation leads to slight variations of isotope amount ratios in biological, environmental and geological samples. Traditionally, isotope ratios are measured by mass spectrometric methods. Their drawbacks include the high costs for instruments and their operation, experienced operators and elaborate time-consuming chromatographic sample preparation.
Recently, optical spectrometric methods have been proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS), and laser ablation molecular isotopic spectrometry (LAMIS).
For the determination of Mg isotope ratios in selected rock reference materials, the molecular spectrum of the in-situ generated MgF and MgO molecules were studied and their results compared with MC-ICP-MS. By HR-CS-MAS, samples were dissolved by acid digestion and Mg isotopes analyzed with and without matrix. The absorption spectrum was recorded for MgF for the electronic transitions X 2Σ → A 2 Πi, and X 2Σ → B 2Σ+. In the case of LAMIS, we investigated the MgF molecule for the electronic transition A 2Πi → X 2Σ, as well as direct analysis by the MgO molecule for the electronic transition A 1Π+ → X 1Σ. The MgF and MgO spectra are described as the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF for the MgF and 24MgO, 25MgO, and 26MgO for the MgO. The isotope analysis was done by deconvolution of the MgF spectrum by partial least square regression (PLS) calibrated with enriched isotope spikes. Results were accurate with precisions ranging between 0.2 ‰ and 0.8 ‰ (2 SD, n= 10) for HR-CS-GFMAS. No statistically significant differences were observed for samples w/o matrix extraction. On the other hand, LAMIS allows the direct analysis of solid samples with the extended possibility of direct analysis, however the precision is lower due the lack of solid isotopic calibration standards.
Magnesium is a major element in the hydrosphere and biosphere and plays important roles in (bio-) geochemical and physiological cycles. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg. It is due to their relatively large mass difference (~8% between) that isotope fractionation leads to slight variations of isotope amount ratios in biological, environmental and geological samples. Traditionally, isotope amount ratios are measured by mass spectrometric methods. Their drawbacks include the high costs for instruments and their operation, experienced operators and elaborate time-consuming chromatographic sample preparation. Recently, an optical spectrometric method has been proposed as faster and low-cost alternative for the analysis of isotope ratios: high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS).
For the determination of Mg isotope ratios in selected rock reference materials, the high-resolution molecular absorption spectrum of in-situ generated MgF molecule was studied applying multivariate analysis and the results compared with MC-ICP-MS. Samples were dissolved by acid digestion and Mg isotopes analyzed with and without matrix. The absorption spectra were recorded for MgF for the electronic transition X 2Σ → B 2Σ+. The MgF spectrum is described as the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF. The isotope analysis was done by deconvolution of the MgF spectrum by partial least square regression (PLS). A PLS model was built and calibrated with enriched isotope spikes and certified reference materials. Spectra data was preprocessed by a derivate of second order and venetian blinds cross-validation was employed for finding the optimum latent variables. Finally, the model was refined by a genetic algorithm which identified the best subset of variables for a precise and accurate regression. Results are compatible with those obtained by MC-ICP-MS with an accuracy of ± 0.3‰ with uncertainties ranging between 0.02 to 0.6‰.
Magnesium is a naturally occurring element that can be found in several mineral forms in the earth crust. This element presents three stable isotopes 24Mg, 25Mg and 26Mg with a natural abundance of 79%, 10%, and 11% respectively. It is due to their relatively large mass difference (~8% between 24Mg and 26Mg) that isotope fractionation leads to slight isotope amount ratio variations n(26Mg)/n(24Mg) in biological and geological samples. Traditionally, isotope amount ratios have been measured by mass spectrometric methods. However, drawbacks of these methods include the high costs for instruments and their operation, experienced operators and elaborate chromatographic sample preparation which are time-consuming. Recently, optical spectrometric methods have been proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) and laser ablation molecular isotopic spectrometry (LAMIS). For the determination of Mg isotope amount ratios, the molecular spectrum of the in-situ generated MgF and MgO molecules were studied. In the case of HR-CS-GFMAS, the absorption spectrum was recorded for MgF for the electronic transitions X 2Σ → A 2 Πi and X 2Σ → B 2Σ+ around wavelengths 358 nm and 268 nm respectively. In the case of LAMIS, it was studied the MgF molecule for the electronic transitions A 2Πi → X 2Σ as well as the MgO molecule for the electronic transition A 1Π+ → X 1Σ around 500 nm. The MgF and MgO spectra are composed by the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF for the MgF and 24MgO, 25MgO, and 26MgO for the MgO (F is monoisotopic, and the isotope composition of O is assumed as constant). By HR-CS-GFMAS the analysis of Mg was done by deconvolution of the MgF spectrum by a partial least square regression (PLS) calibrated with enriched isotope spikes. The isotope amount ratios in rock samples with and without matrix separation were analyzed. Resulting delta values were obtained with precisions ranging between 0.2-0.5 ‰. On the other hand, LAMIS allows the direct analysis of solid samples with the extended possibility of in-situ analysis. Main advantages, limitations, and scopes of both optical techniques are going to be discussed and compared with MC-ICP-MS.
Mass spectrometric Methods MC-ICP-MS and TIMS) are without doubt the working horse of stable isotope analysis. However, drawbacks of these methods include the high costs for instruments and their operation, experienced operators and elaborate chromatographic sample preparation which are time consuming.
Optical spectrometric methods are proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS) and laser ablation molecular isotopic spectrometry (LAMIS). First, stable isotope amount compositions of boron (B) and magnesium (Mg) were determined based on the absorption spectra of in-situ generated heteronuclear diatomic molecules (MH or MX) in graphite furnace HR-CS-MAS. The use of a modular simultaneous echelle spectrograph (MOSES) helps to find the maximal isotope shift in the diatomic molecular spectra produced in a graphite furnace by using isotopic spike solutions. Isotopes of boron (10B and 11B) were studied via their hydrides for the electronic transition X 1Σ+ → A 1Π. The spectrum of a given sample is a linear combination of the 10BH molecule and its isotopologue 11BH. Therefore, the isotopic composition of samples can be calculated by a partial least square regression (PLS). For this, a spectral library was built by using samples and spikes with known isotope composition. Boron isotope ratios measured by HR-CS-MAS are identical with those measured by mass spectrometric methods at the 0.15 ‰ level. Similar results were obtained for a multiple isotope system like Mg (24Mg, 25Mg, and 26Mg), where isotope shifts of their isotopologues can be resolved in the MgF molecule for the electronic transition X 2Σ → A 2 Πi. Finally, the application of molecular spectrometry via emission by LAMIS is compared and discussed.
Arraying of single cells for mass spectrometric analysis is a considerable bioanalytical challenge. In this study, we employ a novel single cell arraying technology for quantitative analysis and isotopic fingerprinting by laser ablation inductively coupled plasma time-of-flight mass spectrometry (LA-ICP-TOF-MS). The single cell arraying approach is based on a piezo-acoustic microarrayer with software for automated optical detection of cells within the piezo dispense capillary (PDC) prior to arraying. Using optimized parameters, single cell occupancy of >99%, high throughput (up to 550 cells per hour), and a high cell recovery of >66% is achieved. LA-ICP-TOF-MS is employed to detect naturally occurring isotopes in the whole mass range as fingerprints of individual cells. Moreover, precise quantitative determination of metal-containing cell dyes is possible down to contents of ∼100 ag using calibration standards which were produced using the same arrayer.
Tandem mass spectrometry represents an important analytical tool to unravel molecular structures and to study the gas-phase behavior of organic molecules. Besides commonly used methods like collision-induced dissociation and electron capture or transfer dissociation, new ultraviolet light–based techniques have the potential to synergistically add to the activation methods. Here, we present a new simple, yet robust, experimental design for polychromatic activation of trapped ions using the 115–160 nm output of a commercially available deuterium lamp. The resulting continuous dissociative excitation with photons of a wide energy range from 7.7 to 10.8 eV is studied for a comprehensive set of analyte classes in both positive and negative ion modes. While being simple, affordable, compact, and of low maintenance, the new setup initiates fragmentation of most precursor ions via their known dissociation pathways. Additionally, some new fragmentation patterns were discovered. Especially, electron loss and electron capture reactions with subsequent fragmentations were observed. For oligonucleotides, peptides, carbohydrates, and organic dyes, in comparison to collision-induced dissociation, a significantly wider fragment distribution was obtained, resulting in an information increase. Since the individual photons carry enough energy to post-ionize the nascent fragments, a permanent vacuum ultraviolet light exposure inside the ion trap potentially goes along with a general increase in detection capability.
A fast and simple method for sulfur quantification in crude oils was developed by using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). For this, heavy crude oil samples were prepared as microemulsion (shake) and injected into a graphite furnace (shut). Finally, the concentration of sulfur was determined by monitoring in situ the transient molecular spectrum of GeS at wavelength 295.205nm after adding a germanium solution as molecular forming agent (and go). Zirconium dioxide in the form of nanoparticles (45–55nm) was employed as a permanent modifier of the graphite furnace. Calibration was done with an aqueous solution standard of ammonium sulfate, and a characteristic mass (m0) of 7.5ng was achieved. The effectiveness of the proposed method was evaluated analizing, ten heavy crude oil samples with Sulfur amounts ranging between 0.3 and 4.5% as well as two NIST standard reference materials, 1620c and 1622e. Results were compared with those obtained by routine ICP-OES analysis, and no statistical relevant differences were found.
Advances in laser-induced plasmas have enabled various rapid and simple analytical applications. Especially, their uses in the analyses of condensed-phase samples have drawn significant attention in the past few decades. Depending on the laser energy per pulse, various analytical goals can be achieved. Laser-induced airborne plasmas allow direct analysis of species in ambient air. Importantly,
all of these applications are based on a fundamental understanding of the laser–medium interaction. Recent developments of diode-pumped solid-state lasers offer an alternative to conventional powerful, yet bulky lasers, which can specifically operate at high Repetition rates. Although these lasers deliver much lower power per pulse (mJ compared to mJ), the outstanding repetition rates offer significant improvement to meet statistical needs in some cases. In the present work, a mJ-laserinduced airborne plasma was characterized through optical emission analysis. By using a ns-timegated image detector coupled with specific bandpass filters, spatially, temporally, and spectrally resolved plasma images were recorded. Compared to conventional mJ-laser-induced plasmas, the one induced by mJ-lasers demonstrated unique features during its evolution. Specifically,
measurements of the distribution of ionic and atomic species revealed distinctive energy/matter transfer processes during early ignition of the plasma. Meanwhile, dynamic investigations suggested subsequent matter transport in the later stage.
Sustainability means meeting the needs of today without compromising the needs of the next generations. How can we meet the needs of the next generations, if we do not even know what these needs are? If we do not listen to the next generation and learn from them? Do we even meet the needs of today for everyone on earth?
The efficiency, relatively low cost and eco-friendly nature of hydrogen peroxide-assisted photocatalysis treatment procedures are significant advantages over conventional techniques for wastewater remediation. Herein, we evaluate the behaviour of g-cyclodextrin (g-CD) immobilised on either bare or chitosan (CS)–functionalised Fe3O4 nanoparticles, for photodegrading Bisphenol A (BPA) in ultrapure water and in real wastewater samples. The BPA removal efficiencies with Fe3O4/g-CD and Fe3O4/CS/g-CD were compared with those of Fe3O4/b-CD, and were monitored under UVA irradiation at near-neutral pH. The addition of H2O2 at low concentrations (15 mmol L-1) significantly increased BPA photodegradation in the presence of each nanocomposite. The highest catalytic activity was shown by both Fe3O4/g-CD and Fe3O4/CS/g-CD nanocomposites (,60 and 27%BPA removal in ultrapure water and real wastewater effluent, respectively). Our findings reveal the superior performance of g-CD-functionalised Fe3O4 relative to that of Fe3O4/b-CD. The use of CD-based nanocomposites as photocatalytic materials could be an attractive option in the pre- or post-treatment stage of wastewaters by advanced oxidation processes before or after biological treatment.
An airborne high repetition rate laser-induced plasma was applied as a versatile ambient ionization source for mass-spectrometric determinations of polar and nonpolar analytes in solution. The laser plasma was sustained between a home-built pneumatic nebulizer and the inlet capillary of an Orbitrap mass spectrometer. To maintain stable conditions in the droplet-rich spray environment, the plasma was directly fed by the fundamental output (λ = 1064 nm) of a current state-of-the-art diode-pumped solid-state laser. Ionization by the laser-driven plasma resulted in signals of intact analyte ions of several chemical categories. The analyte ions were found to be fully desolvated since no further increase in ion signal was observed upon heating of the inlet capillary. Due to the electroneutrality of the plasma, both positive and negative analyte ions could be formed simultaneously without altering the operational parameters of the ion source. While, typically, polar analytes with pronounced gas phase basicities worked best, nonpolar and amphoteric compounds were also detected. The latter were detected with lower ion signals and were prone to a certain degree of fragmentation induced during the ionization process. All the described attests the laser-induced microplasma by a good performance in terms of stability, robustness, sensitivity, and general applicability as a self-contained ion source for the liquid sample introduction.
Digital Analytical Sciences
(2019)
Based on inductive reasoning scientific inquiry in Analytical Sciences has a long tradition. The talk addresses in which way the digital transformation will change the scientific paradigm in Analytical Sciences to a data-driven discipline. Three main areas, integration, instruments, and methods, are discussed in their transformation through machine learning and other digital tools. Finally, some shortcomings and pitfalls in the deployments of algorithmic shortcuts are illustrated.
Xenobiotics and their reactive metabolites are conjugated with native biomolecules such as glutathione and glucoside during phase II metabolism. Toxic metabolites are usually detoxified during this step. On the other hand, these reactive species have a potential health impact by disrupting many enzymatic functions. Thus, it is crucial to understand phase II conjugation reactions of xenobiotics in order to address their fate and possible toxicity mechanisms.
Additionally, conventional methods (in vivo and in vitro) have limitation due to matrix complexity and time-consuming. Hence, developing fast and matrix-free alternative method is highly demandable. In this work, oxidative phase I metabolites and reactive species of chlorpyrifos (insecticide) and fluopyram (fungicide) were electrochemically produced by using a boron-doped diamond electrode coupled online to electrospray mass spectrometry (ESI-MS). Reactive species of the substrates were trapped by biomolecules (glutathione and glucoside) and phase II conjugative metabolites were identified using liquid chromatography (LC)-MS/MS, and/or Triple time of flight (TripleTOF)-MS. Glutathione conjugates and glucosylation of chlorpyrifos, trichloropyridinol, oxon, and monohydroxyl fluopyram were identified successfully. Glutathione and glucoside were conjugated with chlorpyrifos, trichloropyridinol, and oxon by losing a neutral HCl. In the case of fluopyram, its monohydroxyl metabolite was actively conjugated with both glutathione and glucoside. In summary, seven bioconjugates of CPF and its metabolites and two bioconjugates of fluopyram metabolites were identified using electrochemistry (EC)/MS for the first time in this work. The work could be used as an alternative approach to identify glutathione and glucosylation conjugation reactions of other organic compounds too. It is important, especially to predict phase II conjugation within a short time and matrix-free environment.
Acoustic levitators generate acoustic standing waves between a transducer and a concave reflector. These acoustic waves are separated by multiple integer numbers of half wavelengths. Thus, acoustic levitation is the effect that a small volume (5 nL-10 μL) of sample can be levitated in a contact-free manner. Until now, levitation in analytical chemistry has primarily been associated with optical techniques such as Raman, X-Ray or UV/Vis spectroscopy. Less common applications are combinations of acoustic levitation with mass spectrometry. One reason for this being that the acoustic field surrounding the droplet effectively shields the sample, thus making it inaccessible to most ambient ionization techniques. Any effective investigation of acoustically-levitated droplets therefore requires the physical removal of some of the sample from the confine region of the acoustic trap before analysis.
Metal tags find application in a multitude of biomedical systems and the combination with laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) offers an opportunity for multiplexing. To lay the foundation for an increase of the signal intensities in such processes, we herein present a general approach for efficient functionalization of a well-defined metal oxido cluster [Bi6O4(OH)(4)(SO3CF3)(6)(CH3CN)(6)].2 CH3CN (1), which can be realized by selecting 7mer peptide sequences via combinatorial means from large one-bead one-compound peptide libraries. Selective cluster-binding peptide sequences (CBS) for 1 were discriminated from non-binders by treatment with H2S gas to form the reduction product Bi2S3, clearly visible to the naked eye. Interactions were further confirmed by NMR experiments. Extension of a binding peptide with a maleimide linker (Mal) introduces the possibility to covalently attach thiol-bearing moieties such as biological probes and for their analysis the presence of the cluster instead of mononuclear entities should lead to an increase of signal intensities in LA-ICP-MS measurements. To prove this, CBS-Mal was covalently bound onto thiol-presenting glass substrates, which then captured 1 effectively, so that LA-ICP-MS measurements demonstrated drastic signal amplification compared to single lanthanide tags.
The meeting was organised by the European Commission’s Joint Research Centre and held at the JRC-Geel site on 22–23 February 2018. It was a follow-up of a similar meeting held in 2009. The objective of the meeting was to exchange information about ongoing publicly funded reference material (RM) production, identify areas of interest for future specific RMs, including certified reference material (CRM) developments, investigate potential areas of collaboration, and to identify areas which may be of a lower importance in the future for a specific RM producer. The benefit of exchanging such information is to avoid duplication of efforts in RM production, make better use of public funds by potentially matching competencies, and to address problems that are common to publicly funded RM producers.
Analytical Sciences has developed from Ostwald’s “unentbehrlichen Dienstmagd” to a chemical discipline at the core of many of today’s fundamental and applied scientific problems and innovations. An atomic or molecular understanding of basic processes in chemistry, soft matter physics, materials and life science is enabled only through new analytical methods and instrumentation. Similar observations can be found for pressing sociopolitical conflicts of the future: A rational discussion of global climate change or new energy sources is only possible with reliable analytical results. Progress in Analytical Sciences is only possible if the underlying interdisciplinary character is acknowledged and valued. The talk will illustrate the scope of modern Analytical Science through examples from process analysis relevant to modern process intensification and industry 4.0 to bioanalysis and the use of synchrotron radiation to elucidate fundamental reactions materials.
Estrone (E1), a metabolite of the estrogenic hormones 17β-estradiol (β-E2) and 17α-estradiol (α-E2), is itself a potent estrogen which can have a significant impact on the hormonal balance. Due to ist high potential for adverse effects on human health and aquatic life even at pg/L to ng/L levels, its appearance in water should be monitored. E1 has also been considered a marker substance for the presence of other estrogens. This study presents a newly developed direct competitive enzymelinked immunosorbent assay (ELISA) for quantification of E1 in environmental water samples using new monoclonal antibodies.
The quantification range of the ELISA is 0.15 μg/L to 8.7 μg/L E1, and the limit of detection is around 60 ng/L for not pre-concentrated water samples. A pre-concentration step after careful selection of suitable phases for SPE was developed, too. The influence of organic solvents and natural organic matter on the ELISA was assessed. The high selectivity of the monoclonal antibody was demonstrated by determining the cross-reactivity against 20 structurally related compounds.
For the assessment of matrix effects, a concept (“LC–ELISA”) is thoroughly exploited, i.e., separating complex samples by HPLC into 0.3 min fractions and determination of the apparent E1 concentration. Furthermore, fractions with interferences for nontarget/suspected-target analysis can be assigned. A dilution approach was applied to distinguish between specific interferences (cross-reactants) and non-specific interferences (matrix effects). In the determination of 18 environmental samples, a good agreement of the E1 concentration in the respective fractions was obtained with mean recoveries of 103 % to 132 % comparing ELISA to LC–MS/MS.
The interaction of hydrogen with various tungsten-inert-gas-welded austenitic stainless steels’ (AUSS) microstructure is studied by means of desorption/absorption analysis and microstructure observations. One of the limitations of welding is created by the presence of hydrogen in the weld, which can shorten the steel’s service life. The local hydrogen concentration, trapping, and its distribution along the welded samples were studied by thermal desorption spectrometry and were supported by X-ray diffraction (XRD) and electronic microstructural observations. Hydrogen content demonstrated a dependence on the welding zone. It was found that hydrogen distribution, and accepted microstructure during welding, played a significant role in the trapping mechanism of 316L AUSS. XRD analysis revealed residual stresses which were caused due to the presence of hydrogen in c-phase. It was shown that the austenite microconstituents inside 316L can have a crucial effect in preventing hydrogen-assisted cracking phenomenon. The effects of AUSS microstructure on hydrogen absorption and desorption behavior are discussed in detail.
Iron nanoparticles (NPs) metabolism is directly associated to human health due to their use as anemia treatment and should be studied in detail in cells. Here we present a speciation strategy for the determination of the metabolic products of iron oxide nanoparticles coated by tartaric and adipic acids in enterocytes-like cell models (Caco-2 and HT-29). Such methodology is based on the use of SDS-modified reversed phase high performance liquid chromatography (HPLC) separation using inductively coupled plasma-mass spectrometry (ICP-MS) as Fe selective detector. Post-column isotope dilution analysis is used as quantification tool by adding Fe-57 as isotopically enriched standard. To assess the separation capability of the method, two different iron nanostructures: iron sucrose nanoparticles -Venofer®- used as model suspension and iron tartrate/adipate-modified nanoparticles, both of about 4 nm (core size) were evaluated. The two nanostructures were injected into the system showing good peak profiles and quantitative elution recoveries (>80%) in both cases. In addition, both nanoparticulate fractions could be based-line separated from ionic iron species, which needed to be complexed with 1mM citrate to elute from the column. Exposed cells up to 0.5mM of iron tartrate/adipate-modified nanoparticles were specifically treated to extract the internalized NPs and the extracts examined using the proposed strategy. The obtained results revealed the presence of three different fractions corresponding to nanoparticle aggregates, dispersed nanoparticles and soluble iron respectively in a single chromatographic run. Quantitative experiments (column recoveries ranging from 60 to 80%) revealed the presence of the majority of the Fe in the nanoparticulated form (>75%) by summing up the dispersed and aggregate particles. Such experiments point out the high uptake and low solubilization rate of the tartrate/adipate NPs making these structures highly suitable as Fe supplements in oral anemia treatments.
The mechanism of action of zirconium permanent modifiers on graphite surfaces was investigated in order to understand its influence on the analytical signal in atomic and molecular absorption spectrometry (AAS/MAS). For this, the molecule formation of CaF was studied, which is used for the indirect analytical determination of fluorine in high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). The kinetics of this reaction was established by monitoring its molecular spectrum at different atomisation temperatures. An Arrhenius plot showed a pseudo-first order reaction with respect to fluorine (n = 1). An intermediate state was isolated, and its structure was elucidated by spectroscopic methods: scanning electron microscopy with energy dispersive X-ray spectroscopy (SEMEDX), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XANES and EXAFS), and Raman microspectroscopy. We propose here a mechanism, where ZrO2 acts as a heterogeneous catalyst: after a pyrolytic step, an intermediate state of ZrO(OCaF) is activated, and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface. No evidence of the formation of zirconium carbide was found. Consequently, as the CaF formation is catalysed by a heterogeneous catalyst, surface modifications with ZrO2 nanoparticles and ZrO xerogels were investigated in order to increase the surface area. Their influence was evaluated in the molecule formation of CaF, CaCl, CaBr, and CaI. Graphite furnace modification with zirconium oxide nanoparticles proves to be the best choice for fluorine analysis with a signal enhancement of more than eleven times with respect a non-coated graphite furnace. However, the influence of zirconium modifications in the analytical signals of Cl, and I is lower than the F signals or even negative in case of the Br. Understanding zirconium modifiers as heterogeneous catalysts offers a new perspective to AAS and MAS, and reveals the potential of surface analytical methods for development of improved permanent modifiers and graphite furnace coatings.
Identifying the fate of agrochemicals is important to understand their potential risk for living organisms. We report here new photodegradation products (PPs) of the fungicide fluopyram. The PPs were produced by irradiating a fluopyram standard in 0.1% acetonitrile aqueous media by a 150-W medium pressure Hg-lamp that emits wavelengths between 200–280 nm. The structural elucidation of PPs was achieved by combining the retention time, isotopic pattern, targeted fragmentation, and accurate mass measurements using liquid chromatography-tandem mass spectrometry (LC-MS/MS) and high resolution-MS (HRMS). In addition to previously known PPs, seven new PPs of fluopyram were identified in this work: mainly dihydroxyl and hydroxylimide fluopyram as well as mono, di, and trihydroxyl lactam. Additionally, two PPs were found to be formed by rearrangement after the loss of H2C=CH2. Hence, the results of the work contribute to extending the current knowledge regarding the photoinduced fate of agrochemicals, and fluopyram in particular.
LA-ICP-MS is increasingly used for single cell analysis in two different detection modes using either the imaging mode with subcellular resolution or alternatively single spot analysis of cells with a larger laser spot size. This study compares the analytical figures of merit of both detection modes (signal to noise, precision, accuracy, throughput), as well as ease of operation and data evaluation. Adherent 3T3 fibroblast cells were stained with two metal dyes (mDOTA-Ho, Ir-DNA-intercalator) and several dozen cells were measured using both modes. We found a ten times higher throughput for single spot analysis, which has as well a straightforward data analysis, shortening the total analysis time further. The signal to noise ratio for single spot analysis was found to be slightly better compared to the signal to noise of pixels in imaging. The mean metal intensity per single cell differed by only 10% between both modes and obtained distributions were found to show no statistically significant differences. Using matrix matched calibration based on standards spotted onto nitrocellulose membrane, we achieved detection limits (10s) of 12 fg for Ir and 30 fg for Ho and quantified 57 +/-35 fg Ir and 1192 +/- 707 fg Ho per single cell.
Compared to a conventional ICP-MS measurement of a digest of about 60000 cells, 54% of Ir content and 358% Ho content was found using quantitative LA-ICP-MS. The difference might be a consequence of the two metal dyes binding to different structures of the cell and therefore might behave differently in sample preparation for conventional and LA-ICP-MS.
Laser-induced plasma (LIP) has drawn significant amount of attentions in the past decades, particular in elemental analyses for solid or liquid samples. Through proper focusing of the highly energetic laser beam, the plasma can also be ignited in the ambient air, where airborne analytes can be ionized. Such an effect enabled the use of airborne LIP as an ambient ionization source for mass spectrometric analyses. In contrast to other ambient desorption/ionization sources, airborne LIP does not require a specific discharge medium or expensive gas stream. Meanwhile, the airborne LIP produces reagent ion species for both proton-transfer and charge-transfer reactions in addition to the vacuum ultraviolent photons that are capable of promoting single photon ionization, which can be utilized to ionize polar and non-polar analytes. In order to gauge the analytical performance of airborne LIP, it is critical to understand the undergoing chemistry and physics during and after the plasma formation.
Due to the ambient nature of airborne LIP, the variations of air composition and flow strongly affect the plasma behaviors. Preliminary result suggested the addition of a laminar flow of nitrogen gas favored the formation of protonated species (MH+) against the molecular ones (M+). Although the gas addition approach cannot fully tune the ionization process towards the specific production of pseudo-molecular species versus molecular ones, the alternation of molecular ion formation can be used for analyte recognitions through post processing of the ion patterns. The pulsed character of the used lasers makes the reagent ion equilibrium both transient- and highly fluid-dynamically controlled. The acoustic shock-waves induced by the airborne LIP get affected by an applied gas streams towards the plasma center, influencing the molecular-ion and ion-ion interactions in the near proximity of the plasma.
To understand the airborne LIP formation, the temporally and spatially resolved optical emission spectra were recorded. The results will be correlated to time-resolved mass-spectrometric investigations of the ion profile during different stages of the plasma formation. As one example, the formation of pyrylium ion originating from aromatic compounds will be highlighted.
Polyethylene (PE) frits were used to quantify sulphur in copper and its alloys by isotope dilution combined with LA-ICP-MS as an alternative approach to conventional sample preparation: the copper samples were spiked, the spiked samples were dissolved, the resulting solutions were absorbed in the PE frits and finally the PE frits were analysed by LA-ICP-MS. A prerequisite for such a support material is a low sulphur blank and thus PE was selected for this purpose. The absorption efficiency of the PE frits was studied for varying sulphur amounts ranging from 2 mg S to 80 mg S showing that more than 99.5% of the loaded sulphur was absorbed by the frit. The so prepared PE frits were measured by LA-ICP-MS and yielded a good linearity (R2 ¼ 0.999) for the sulphur ion intensities corresponding to sulphur amounts up to 40 mg S; the associated sensitivity is approximately 3.4 x 10⁴ cps μg⁻¹ for ³²S. For the validation of the developed procedure the reference materials BAM-M376a, BAM-228 and BAM-227 were applied such that 2 μg S, 5 μg S and 11 μg S were absorbed in the PE frits, respectively. These samples were pre-quantified for the adsorbed sulphur amount by external calibration LA-ICP-MS yielding sulphur amounts of 0.9 μg, 5.1 μg and 8.5 μg (quantified for ³²S only), respectively. Relative Standard deviations of the isotope ratios were below 5% in average (n ¼ 3 lines) in all cases (except for the pure spike solution). These samples were then analysed by LA-ICP-IDMS and the measurement results were validated by comparing them with the results obtained by conventional ICP-IDMS. The obtained relative expanded measurement uncertainties ranged between 10% and 26%. Pearson's coefficient was used to express the correlation between both techniques; the obtained value was 0.999 demonstrating a strong correlation. Contrary to most published LA-ICP-IDMS procedures, the developed procedure enables SI-traceability for the measurement results. The metrological traceability to the SI for the sulphur mass fractions in copper was established by an unbroken chain of comparisons, each accompanied by an uncertainty budget. Thus, the measurement results are considered reliable, acceptable and comparable within the stated measurement uncertainty. The metrological traceability chain from the kg down to mass fraction in the samples obtained by LA-ICP-IDMS is presented as well.
The development and improvement of new ionization techniques for mass spectrometry often requires dedicated, specific sampling approaches. Recently, a novel ionization scheme for ambient MS has been introduced based on a quasi-continuous laser-induced plasma, which was ignited directly before the MS inlet. This setup combines the general advantages of ambient ionization, provides electro neutrality, sufficient duty cycle and a ubiquitous plasma medium.
A high repetition rate DPSS laser (Conqueror 3-LAMBDA, Nd:YVO4, 1 - 500 kHz, average output power: 12 W at 50 kHz, Compact Laser Solutions GmbH, Germany) and the corresponding optomechanical system were installed on an optical breadboard above the inlet of a LCQ DecaXP ion trap mass spectrometer. The quasi-continuous airborne plasma was ignited inside the sprayed sample in front of the inlet via focused laser irradiation.
The introduction of liquid samples into laser-induced plasmas requires higher plasma power during solvent evaporation as compared to gaseous samples. This increased demand was approached via a two-fold strategy: Firstly, an alternative, more powerful, laser plasma driven by the fundamental instead of the second harmonic wavelength was implemented, which provided a 10-fold increase of signal intensity, while maintaining the same reagent ion pattern as the previous plasma. Protonated water clusters [(H2O]nH]+, NH4+ as well as charge transfer promoting ion O2+, dominated the reagent ion mass spectrum. Secondly, a miniaturized nebulizer was used to minimize the size of the plasma quenching solvent droplets. The result of these improvements was a new and very stable ion source for direct microfluidic coupling. A variety of samples demonstrated the performance of the ion source.
A laser-driven plasma was shown to be a powerful ion source for gaseous and solid samples. For the first time, liquid samples were examined using the novel source. In addition to demonstrating an improved strategy for igniting the laser plasma, this contribution also covers the miniaturization of the spray source for enhanced ionization, while minimizing sample consumption via a microfluidic spray systems.
Quantification of sulphur in copper metals by isotope dilution LA-ICP-MS using polyethylene frits
(2018)
Sulphur is one of the relevant impurities in copper and its alloys affecting their material properties. To ensure the quality of copper products, fast direct solid sampling techniques are very attractive. However, for the calibration suitable matrix reference materials are required. For the certification of such reference materials appropriate, SI-traceable analytical methods are essential. Therefore, a procedure was developed to quantify total sulphur in copper by combining the classical isotope dilution (ID) technique and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS).
Here, for the first time, polyethylene (PE) frits were used to prepare appropriate solid samples for the sulphur quantification in copper metals (alloyed/unalloyed) by isotope dilution LA-ICP-MS. The properties of the PE frit meet the requirements as porous material with high absorption efficiency, thermal and chemical resistance as well as low sulphur blank. Different copper reference materials were used to develop and validate the procedure. The copper samples were spiked with 34S, digested with nitric acid and then the digests were absorbed on PE frits. After drying, the frits were analysed by LA-ICP-IDMS using a Nd:YAG laser at 213 nm coupled to an ICP sector field mass spectrometer. It could be demonstrated, that the sample solution dispersed on the frits did not influence the 32S/34S ratio significantly even though the sulphur intensities were fluctuating along the scanned lines. Relative standard deviations of the isotope ratios were below 5 % in average between three line scans (except for the pure spike solution and procedure blank). The measurement results were validated by comparing them with the results obtained by conventional ICP-IDMS after analyte-matrix separation. Plotting the mass fraction of sulphur in copper obtained by LA-ICP-IDMS versus those obtained by ICP-IDMS yields a linear curve with a correlation coefficient of 0.9999 showing a strong agreement between both techniques.
The metrological traceability to the SI from the kg down to the sulphur mass fraction in copper is established by an unbroken chain of comparisons, each accompanied by an uncertainty budget. Thus, the measurement results are considered reliable, acceptable and comparable within the stated measurement uncertainty.
Selected resonance states of the deuterated formyl radical in the electronic ground state X^2A´ are computed using our recently introduced dynamically pruned discrete variable representation [H. R. Larsson, B. Hartke, and D. J. Tannor, J. Chem. Phys. 145, 204108 (2016)]. Their decay and asymptotic distributions are analyzed and, for selected resonances, compared to experimental results obtained by a combination of stimulated emission pumping and velocity-map Imaging of the product D atoms.
The theoretical results show good agreement with the experimental kinetic energy distributions. The intramolecular vibrational energy redistribution is analyzed and compared with previous results from an effective polyad Hamiltonian. Specifically, we analyzed the part of the wavefunction that remains in the interaction region during the decay. The results from the polyad Hamiltonian could mainly be confirmed. The C=O stretch quantum number is typically conserved, while the D-C=O bend quantum number decreases. Differences are due to strong anharmonic coupling such that all resonances have major contributions from several zero-order states. For some of the resonances, the coupling is so strong that no further zero-order states appear during the dynamics in the interaction region, even after propagating for 300 ps.
Singlet oxygen generation potential of two novel free-base-porphyrin photocatalysts was investigated. The freebase-porphyrin-sensitized Fe3O4 magnetic nanoparticles (MNPs) were tested for the degradation of the model pollutant Bisphenol A (BPA) in aqueous solution, for the first time. MNPs with either cubic or spherical shape were synthesized using the sonochemical approach, followed by sensitizing with photoactive 4,4′,4′′,4′′′- (Porphine-5,10,15,20-tetrayl)tetrakis(benzoic acid) (TCPP). The resulted photocatalysts were characterized in detail by scanning and transmission electron microscopy, Brunauer–Emmett–Teller analysis, spectral techniques and vibrating sample magnetometry. The electron spin resonance experiments have confirmed the high activity of the photocatalysts through the efficient formation of singlet oxygen in solution. The optimum operational parameters for BPA degradation were established as follows: 1.0 μmol L−1 BPA, 1.0 g L−1 of photocatalyst, 100 μmol L−1 H2O2, under UVA irradiation. In these conditions, the results for both photocatalysts revealed that after only 10 min of reaction, over 64% and ca. 90% of BPA have been removed from solution in the absence and presence of H2O2, respectively. Whereas after 60 minutes of treatment, only 24% of BPA in real wastewater effluent samples were removed under UVA irradiation in the absence of H2O2, showing the high complexity of real wastewater. Moreover, both photocatalysts were successfully used for BPA removal in three consecutive runs, without significant loss of catalytic features.
Die Bundesanstalt für Materialforschung und -prüfung (BAM) ist eine Ressortforschungseinrichtung, die zum Schutz von Mensch, Umwelt und Sachgüter, forscht, prüft und berät. Im Fokus aller Tätigkeiten in der Materialwissenschaft, der Werkstofftechnik und der Chemie steht dabei die technische Sicherheit von Produkten und Prozessen. Dazu werden Substanzen, Werkstoffe, Bauteile, Komponenten und Anlagen sowie natürliche und technische Systeme erforscht und auf sicheren Umgang oder Betrieb geprüft und bewertet. Schwerpunkt des Vortrages sind multimodale Polymeranalytik, nanoskalige Sensormaterialien und die Charakterisierung von technischen Eigenschaften von Polymeren sowie ihre Alterung und Umweltrelevanz.
Cost-effective water cleaning approaches using improved Treatment technologies, for instance based on catalytic processes with high activity catalysts, are urgently needed. The aim of our study was to synthesize efficient Fenton-like photo-catalysts for rapid degradation of persistent organic micropollutants in aqueous medium. Iron-based nanomaterials were chemically synthesized through simple procedures by immobilization of either iron(II) oxalate (FeO) or iron(III) citrate (FeC) on magnetite (M) nanoparticles stabilized with polyethylene glycol (PEG). Various investigation techniques were performed in order to characterize the freshly prepared catalysts. By applying advanced oxidation processes, the effect of catalyst dosage, hydrogen peroxide concentration and UV-A light exposure were examined for Bisphenol A (BPA) conversion, at laboratory scale, in mild conditions. The obtained results revealed that BPA degradation was rapidly enhanced in the presence of low-concentration H2O2, as well as under UV-A light, and is highly dependent on the surface characteristics of the catalyst. Complete photo-degradation of BPA was achieved over the M/PEG/FeO catalyst in less than 15 minutes. Based on the catalytic performance, a hierarchy of the tested catalysts was established: M/PEG/FeO > M/PEG/FeC > M/PEG. The results of cytotoxicity assay using MCF-7 cells indicated that the aqueous samples after treatment are less cytotoxic.
The development and enhancement of new ionization techniques for mass spectrometry often needs to be custom-tailored for specific sampling approaches. Here, a direct sampling ionization technique is presented for ambient mass spectrometry. Ambient mass spectrometry based techniques are typically used to analyze samples in their native states without sample pretreatment. This new design is based on a quasi-continuous airborne plasma which is ignited inside the particulate air via a focused laser irradiation. Desorption and ionization of the analyte molecules are achieved by the laser plasma without reaching the plasma. The ionization process is induced by interaction with nascent ionic fragments, electrons and ultraviolet photons in the plasma vicinity. Previously, this method was solely used for the characterization of solid and gaseous analytes. The sample introduction was occurred via thermal desorption and headspace analysis. This study focuses on the potential applicability of liquid samples. In comparison to previous approaches, the usage of liquid samples has an impact on the stability of typically used plasma of 532 nm. It was necessary to realize an alternative plasma using light of the fundamental wavelength of 1064 nm. That new plasma resulted in a significant more stable and bright plasma and the first laser plasma ionization spectrum was recorded for an analyte in the condensed phase with a mass spectrometer of type LCQ DecaXP.
A versatile ionization scheme for atmospheric pressure MS is presented. It is based on a quasi-continuous laser-induced plasma (LIP), generated by a 26 kHz pulsed DPSS-laser, which is ignited in front of the MS inlet. Analytes are determined with different sampling regimes, comprising either an ambient desorption/ionization mechanism, a liquid-phase or gas-phase sample introduction.
The MS signal closely resembles the ionization behavior of APCI-like plasma-based sources, such as DBD or DART. Though LIPs are known to efficiently atomize/ionize any sample material, mass spectra of intact molecular ions are recorded, exhibiting low fragment-ion content. To understand this contradictory behavior, the plasma properties are investigated that lead to the formation of molecular ions. Comprehensive studies include optical emission spectroscopy, shadowgraph imaging and mass spectrometry diagnostics.
The results show that the ionization of analyte does not occur in the plasma itself, but in the cold adjacent gas layer. The pulsed character of LIPs induces an expanding shockwave, which concentrically expands around the plasma core and sweeps the molecules toward the plasma edges, where they are ionized either directly by the self-emission of the hot core or via interaction with secondary reactants. However, this unidirectional transport causes a rarefaction inside the plasma center, which leads to a decrease in plasma intensity and number density. Thus, a restoration of the former gaseous medium by other dynamically equilibrated diffusion processes would be favorable. Besides gas replenishing, we demonstrate the beneficial use of an acoustical standing wave inside an ultrasonic resonator on the performance of the LIP.
Optical elemental analysis in the gas phase typically relies on electrically driven plasmas. As an alternative approach, laser-induced plasmas (LIPs) have been suggested but have so far been only scarcely used.
Here, a novel signal enhancement strategy for laser-based airborne plasma optical Emission spectroscopy for gas phase analytics is presented. In contrast to an electrically driven plasma, in the laser-induced analogue dynamic matter transport equilibrium builds up. The latter results in a rarefied density regime in the plasma core itself, surrounded by an area of compressed matter. The central rarefaction leads to a decrease in plasma intensity and analyte number density, both of which are detrimental for analytical purposes. Since the repetitive ignition of LIPs is a transient process, a restoration of the former gaseous medium by other dynamically equilibrated diffusion processes would be favourable. The presented combination of an airborne LIP and an ultrasonic acoustic resonator yields a fourfold signal enhancement while the Background contribution of ubiquitous air is at the same time effectively suppressed. Since the entire enhancement effect occurs without contact, no additional sources for abrasive sample contamination are introduced.
Because of the globally increasing prevalence of diabetes, the need for accurate, efficient and at best miniaturized automated analytical systems for sugar detection in medical diagnostics and the food industry is still urgent. The development of molecular probes for sugars based on boronic acid receptors offers an excellent alternative to the kinetically slow enzyme-based sugar sensors. Moreover, by coupling such chelating units with dye scaffolds like BODIPYs (boron–dipyrromethenes), highly fluorescent sugar sensing schemes can be realized. In this work, a boronic acid-functionalized BODIPY probe was developed, which binds selectively to fructose’s adjacent diols to form cyclic boronate esters. Placement of an amino group in direct neighborhood of the boronic acid moiety allowed us to obtain a broad working range at neutral pH, which distinguishes the probe from the majority of systems working only at pH > 8, while still meeting the desired sensitivity in the micro-molar range due to a pronounced analyte-induced fluorescence increase. To enhance the applicability of the test in the sense described above, integration with a microfluidic chip was achieved. Here, fructose was selectively detected by fluorescence with similar sensitivity in real time on chip, and an assay for the straightforward detection of sugar in (colored) sodas without sample clean-up was established.