Isotachophoretic determination of stability constants of Ho and Y complexes with diethylenetriaminepentaacetic acid and 1,4,7,10-tetraazadodecane-N,N',N'',N'''-tetraacetic acid

The method of capillary isotachophoresis with conductivity detection was applied for the determination of the physico-chemical characteristics (conditional stability constants log beta') of holmium and yttrium complexes with DTPA (diethylenetriaminepentaacetic acid) and DOTA (1,4,7,10-tetraazadodecane-N,N',N',N'-tetraacetic acid). The log beta' determination is based on the linear relation between the stability constants of lanthanide-DTPA (lanthanide-DOTA) complexes and the reduction of the zone of the complex owing to the bleeding phenomena (liberating free metal ion). The stability constants calculated using this relationship are comparable with the literary data obtained by other methods for both holmium (log beta'(Ho-DTPA)=21.9, log beta'(Ho-DOTA)=24.5) and yttrium complexes (log beta'(Y-DTPA)=21.2, log beta'(Y-DOTA)=24.4). Capillary isotachophoresis was applied for the determination of the optimum composition of the reaction mixture (metal:ligand ratio) as well.     

Deep neural network analysis of nanoparticle ordering to identify defects in layered carbon materials

Smoothness/defectiveness of the carbon material surface is a key issue for many applications, spanning from electronics to reinforced materials, adsorbents and catalysis. Several surface defects cannot be observed with conventional analytic techniques, thus requiring the development of a new imaging approach. Here, we evaluate a convenient method for mapping such “hidden” defects on the surface of carbon materials using 1–5 nm metal nanoparticles as markers. A direct relationship between the presence of defects and the ordering of nanoparticles was studied experimentally and modeled using quantum chemistry calculations and Monte Carlo simulations. An automated pipeline for analyzing microscopic images is described: the degree of smoothness of experimental images was determined by a classification neural network, and then the images were searched for specific types of defects using a segmentation neural network. An informative set of features was generated from both networks: high-dimensional embeddings of image patches and statics of defect distribution.

Defectiveness of carbon material surface is a key issue for many applications. Pd-nanoparticle SEM imaging was used to highlight “hidden” defects and analyzed by neural networks to solve order/disorder classification and defect segmentation tasks.     

IAEA analytical quality assurance programmes to meet the present and future needs of developing countries

For many years the International Atomic Energy Agency (IAEA) has been promoting analytical quality assurance and quality control in its Member States with emphasis on measurands that are amenable to analysis by nuclear and related techniques, i.e. radionuclides, trace elements, and stable isotopes. This paper reviews briefly the rationale for some of these activities, particularly in relation to the needs of participants in developing countries arising out of co-ordinated research programmes, technical co-operation projects and global and regional networks. Emphasis is given to biological and environmental reference materials with a matrix of natural origin. Also described are some activities arising out of the requirements of ISO-25 and other relevant international quality standards.     

Topographical properties of polymer films deposited in capillaries for electrophoretic separations of large organic molecules

Topography and thickness of hydrophilic polymer coatings of fused-silica capillaries for capillary electrophoresis (CE) were investigated using atomic force microscopy (AFM), scanning electron microscopy (SEM), and profilometry. Three hydrogels, poly(2-hydroxyethyl methacrylate) [poly(HEMA)], poly(diethylene glycol monomethacrylate) [poly(DEGMA)], and poly(triethylene glycol monomethacrylate) [poly(TEGMA)], were deposited using two procedures, either by simple physical sorption of the polymers, or by derivatization of the capillary wall surface with glycidyl methacrylate (EPMA) followed by polymerization of the appropriate monomers. The performance of the modified capillaries was tested under CE conditions (decrease in the electroosmotic flow, EOF dependence on pH, separation of milk and standard proteins). It has been found that the most important property of the polymer coating is its thickness, whereas its topography and the degree of its hydrophobicity are less significant. Film deposition by physical adsorption is preferable to polymerization on the derivatized surface.     

Study of perrhenate reduction by capillary electrophoresis

The influence of perrhenate concentration, the concentration of the reducing agent and pH of the reaction mixture on the yield of perrhenate reduction were studied to find a possibility to decrease the stannous chloride concentration in the reaction mixture without negative changes on the yield of perrhenate reduction. Britton-Robinson buffer solutions were selected as the background electrolytes because of their buffering capacity in a wide pH interval. The highest degree of perrhenate reduction was obtained at pH 2 at perrhenate concentrations ranging from 10(-4) to 10(-3) mol/L. The stability of reduced rhenium against pH change from 2 to 5.5 and against dilution of rhenium in the reaction mixture to the concentration suitable for the application in radiotherapy were studied as well. The results obtained by capillary electrophoresis and by thin-layer chromatography with radiometric detection were compared.     

Sulfur Compounds. 183. A Derivative of Perthiocarbonic Acid H2CS4: X-ray structural analysis of bis(triphenylmethyl) perthiocarbonate (Ph3C)2CS4

The molecular structure of Ph₃CSSC(S)SCPh₃ · CS₂ has been determined by X-ray structural analysis. The substance crystallizes in the triclinic crystal system [a = 884.9(2) pm, b = 1 039.5(2) pm, c = 2 064.6(3) pm, α = 75.86(1)°, β = 79.83(2)°, γ = 77.31(5)°, Z = 2, space group P1 ]. The CS₃ group is planar; the S? S-bond (201.4 pm) forms an angle of 5.7° with the CS₃ plane. The torsional angle CSSC equals 96.3°. (Ph₃C)₂CS₄ was obtained by reaction of TosNSCl₂ (Tos = p-MeC₆H₄SO₂) with Ph₃CSH in CS₂ in the presence of triethylamine. The reaction mechanism is discussed.     

Continuous pH monitoring during pretreatment of yellow poplar wood sawdust by pressure cooking in water

Yellow poplar wood sawdust consists of 41% cellulose and 19% hemicellulose. The goal of pressure cooking this material in water is to hydrate the more chemically resistive regions of cellulose in order to enhance enzymatic conversion to glucose. Pretreatment can generate organic acids through acid-catalyzed degradation of monosaccharides formed because of acids released from the biomass material or the inherent acidity of the water at temperatures above 160°C. The resulting acids will further promote the acid-catalyzed degradation of monomers that cause both a reduction in the yield and the formation of fermentation inhibitors such as hydroxymethyl furfural and furfural. A continuous pH-monitoring system was developed to help characterize the trends in pH during pretreatment and to assist in the development of a base (2.0 M KOH) addition profile to help keep the pH within a specified range in order to reduce any catalytic degradation and the formation of any monosac-charide degradation products during pretreatment. The results of this work are discussed.     

Strukturanalyse organischer Sulfide mit Hilfe der Gras-Chromatographie

Zusammenfassung Eine Methode der Identifizierung von Alkyl- und Arylgruppen organischer Sulfide wurde ausgearbeitet, die die Spaltung dieser Stoffe mit Raney-Nickel zur gaschromatographischen Bestimmung der dabei entstandenen Kohlenwasserstoffe ausnützt.

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Summary A method was developed for identifying alkyl- and aryl groups of organic sulfides. The method employs the cleavage of these materials with Raney nickel for the gas chromatographic determination of the resulting hydrocarbons.

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Résumé On a mis au point une méthode d'identification des groupes alkylés et arylés des sulfures organiques exploitant la dissociation de ceux-ci par le nickel Raney pour le dosage par chromatographic en phase gazeuse des carbures d'hydrogène qui se forment.

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Die Autoren danken den Kollegen Dr.M. Veea, Ing.J. Petránek und Ing.J. Gaspari für die Überlassung von Proben organischer Sulfide.     

Characterization of three agave species by gas chromatography and solid-phase microextraction-gas chromatography-mass spectrometry

Steam distillation (SD) extraction-solid-phase microextraction coupled to GC-MS was developed for the determination of terpenes and Bligh-Dyer extraction-derivatization coupled with GC for the determination of fatty acids such as ethyl esters were used. It was found that the three different Agave species have the same profile of fatty acids; the quantity of these compounds is different in each Agave variety. On the other hand, different terpenes were identified in the three Agave plants studied: nine in A. salmiana, eight in A. angustifolia and 32 in A. tequilana Weber var. azul.     

A fast $$(2 + \frac{2}{7})$$ ( 2 + 2 7 ) -approximation algorithm for capacitated cycle covering

Mathematical Programming - We consider the capacitated cycle covering problem: given an undirected, complete graph G with metric edge lengths and demands on the vertices, we want to cover the...