Ion transmission in an electrospray ionization-mass spectrometry interface using an S-lens

We present the design and performance of an in-house built electrospray ionization-mass spectrometry (ESI-MS) interface equipped with an S-lens ion guide. The ion source was designed specifically for our ion beam experiments to investigate the chemical reactivity and deposition of the clusters and nanoparticles. It includes standard ESI-MS interface components, such as nanoelectrospray, ion transfer capillary, and the S-lens. A custom design enables systematic optimization of all relevant factors influencing ion formation and transfer through the interface. By varying the ESI voltage and flow rate, we determined the optimal operating conditions for selected silica emitters. A comparison of the pulled silica emitters with different tip inner diameters reveals that the total ion current is highest for the largest tip, whereas a tip with the smallest diameter exhibited the highest transmission efficiency through the ESI-MS interface. Ion transmission through the transfer capillary is strongly limited by its length, but the loss of ions can be reduced by increasing the capillary voltage and temperature. The S-lens was characterized over a wide range of RF frequencies and amplitudes. Maximum ion current was detected at RF amplitudes greater than 50 V peak-to-peak (p/p) and frequencies above 750 kHz, with a stable ion transmission region of about 20%. A factor of 2.6 increase in total ion current is observed for 650 kHz as RF amplitudes reach 400 V p/p. Higher RF amplitudes also focus the ions into a narrow beam, which mitigates their losses when passing through the ion guide.     

Fibrillar Networks of Glycyrrhizic Acid for Hybrid Nanomaterials with Catalytic Features

Self‐assembly of the naturally occurring sweetening agent, glycyrrhizic acid (GA) in water is studied by small‐angle X‐ray scattering and microscopic techniques. Statistical analysis on atomic force microscopy images reveals the formation of ultralong GA fibrils with uniform thickness of 2.5 nm and right‐handed twist with a pitch of 9 nm, independently of GA concentration. Transparent nematic GA hydrogels are exploited to create functional hybrid materials. Two‐fold and three‐fold hybrids are developed by introducing graphene oxide (GO) and in situ‐synthesized gold nanoparticles (Au NPs) in the hydrogel matrix for catalysis applications. In the presence of GO, the catalytic efficiency of Au NPs in the reduction of p‐nitrophenol to p‐aminophenol is enhanced by 2.5 times. Gold microplate single crystals are further synthesized in the GA hydrogel, expanding the scope of these hybrids and demonstrating their versatility in materials design.     

New isostructural transition metal complexes with a non‐innocent dithiolate ligand

Three new complexes with 3,6‐dichlorobenzene‐1,2‐dithiol (bdtCl₂), namely methyltriphenylphosphonium bis(3,6‐dichlorobenzene‐1,2‐dithiolato‐κ²S,S′)cobaltate(1−), (C₁₉H₁₈P)[Co(C₆H₂Cl₂S₂)₂], (I), bis(methyltriphenylphosphonium) bis(3,6‐dichlorobenzene‐1,2‐dithiolato‐κ²S,S′)cuprate(2−) dimethyl sulfoxide disolvate, (C₁₉H₁₈P)₂[Cu(C₆H₂Cl₂S₂)₂]·2C₂H₆OS, (II), and methyltriphenylphosphonium bis(3,6‐dichlorobenzene‐1,2‐dithiolato‐κ²S,S′)cuprate(1−), (C₁₉H₁₈P)[Cu(C₆H₂Cl₂S₂)₂], (III), have been synthesized and characterized by single‐crystal X‐ray diffraction. The X‐ray structure analyses of all three complexes confirm that the four donor S atoms form a slightly distorted square‐planar coordination arrangement around the central metal atom. An interesting finding for both the Cu^II and Cu^III complexes, i.e. (II) and (III), respectively, is that the coordination polyhedra are principally the same and differ only slightly with respect to the interatomic distances.     

Fire hazard and heat of combustion of sunflower seed hull pellets

This study is concerned with the investigation of the impact of heat flux on the fire hazard and the effective heat of combustion of sunflower seed hull pellets. Pellets produced by pressing common sunflower seed hulls (Helianthus annuus L.) were investigated. The samples were dried on water content of 0 mass% at a temperature of 103 ± 2 °C. The fire hazard and the heat of combustion have been determined via the cone calorimeter and by the testing procedure per ISO 5660-1:2015 at three heat fluxes (25, 35 and 50 kW m⁻²). The peak heat release rate increases with the increasing of the heat flux from 446 (at a heat flux of 25 kW m⁻²) to 601 kW m⁻² (at a heat flux of 50 kW m⁻²). The carbon monoxide yield lies in the interval from 82.50 (at a heat flux of 25 kW m⁻²) to 154.15 g kg⁻¹ (at a heat flux of 50 kW m⁻²). The effective heat of combustion decreases with the increasing of the heat flux from 15.84 (at a heat flux of 25 kW m⁻²) to 14.58 MJ kg⁻¹ (at a heat flux of 50 kW m⁻²).

     

Pore Development during the Carbonization Process of Lignin Microparticles Investigated by Small Angle X-ray Scattering

Application of low-cost carbon black from lignin highly depends on the materials properties, which might by determined by raw material and processing conditions. Four different technical lignins were subjected to thermostabilization followed by stepwise heat treatment up to a temperature of 2000 °C in order to obtain micro-sized carbon particles. The development of the pore structure, graphitization and inner surfaces were investigated by X-ray scattering complemented by scanning electron microscopy and FTIR spectroscopy. Lignosulfonate-based carbons exhibit a complex pore structure with nanopores and mesopores that evolve by heat treatment. Organosolv, kraft and soda lignin-based samples exhibit distinct pores growing steadily with heat treatment temperature. All carbons exhibit increasing pore size of about 0.5–2 nm and increasing inner surface, with a strong increase between 1200 °C and 1600 °C. The chemistry and bonding nature shifts from basic organic material towards pure graphite. The crystallite size was found to increase with the increasing degree of graphitization. Heat treatment of just 1600 °C might be sufficient for many applications, allowing to reduce production energy while maintaining materials properties.     

Stress characterization of elastodynamics with continuously distributed defects

A pure stress formulation of linear nonhomogeneous anisotropic elastodynamics with continuously distributed defects (EcDD) is proposed, and well known solutions of ECDD corresponding to stationary and moving concentrated plastic fields in an infinite body are recovered by direct integration of the stress field equation. A new interpretation of the solutions is given.     

Photokinetic,Biochemical and Structural Features of Chimeric Photoactive Yellow Protein Constructs

Of the 10 photoactive yellow protein (PYPs) that have been characterized, the two from Rhodobacter species are the only ones that have an additional intermediate spectral form in the resting state (λ_max = 375 nm), compared to the prototypical Halorhodospira halophila PYP. We have constructed three chimeric PYP proteins by replacing the first 21 residues from the N‐terminus (Hyb1PYP), 10 from the β4–β5 loop (Hyb2PYP) and both (Hyb3PYP) in Hhal PYP with those from Rb. capsulatus PYP. The N‐terminal chimera behaves both spectrally and kinetically like Hhal PYP, indicating that the Rcaps N‐terminus folds against the core of Hhal PYP. A small fraction shows dimerization and slower recovery, possibly due to interaction at the N‐termini. The loop chimera has a small amount of the intermediate spectral form and a photocycle that is 20 000 times slower than Hhal PYP. The third chimera, with both regions exchanged, resembles Rcaps PYP with a significant amount of intermediate spectral form (λ_max = 380 nm), but has even slower kinetics. The effects are not strictly additive in the double chimera, suggesting that what perturbs one site, affects the other as well. These chimeras suggest that the intermediate spectral form has its origins in overall protein stability and solvent exposure.     

Tellurium delta‐doped InGaP layers grown by metalorganic vapour phase epitaxy

Heavily n‐type doped and several nanometres thick In_0.485Ga_0.515P layers are necessary for various devices. We studied the delta‐doping of this ternary with tellurium; the layers were grown by metalorganic vapour phase epitaxy (MOVPE), and diethyltelluride was used as the precursor. A maximum Hall sheet concentration of 2.75 × 10¹³ cm^–2 was achieved in our samples grown at 560 °C. The Te profiles were analyzed with secondary ion mass spectrometry (SIMS), and a very narrow spectrum with a full width at half maximum of 7.5 nm was measured. This value indicates that the memory effect, referred to in the literature, was practically eliminated with appropriate growth conditions. (© 2013 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)