Determination of traces of fluorine or sulfur by x-ray analysis

New X-ray methods have been developed for the determination of as little as 1 μg of fluorine or as little as 0.1 μg of sulfur. Fluorine as fluoride is precipitated as lanthanum fluoride in 75% ethanol-water mixture and determined by measuring the amount of lanthanum present in the precipitate. Sulfur as sulfate is precipitated as barium sulfate from a barium sulfate saturated 50% ethanol-buffer mixture, using selenate as a coprecipitant, and determined by measuring the amount of sulfur present. Sulfur as sulfide is precipitated as cadmium sulfide and determined by measuring the amount of sulfur or cadmium in the precipitate.     

Dithiocarbamates as Precursors in Organic Chemistry; Synthesis and Uses

Abstract

Organic dithiocarbamates have received great attention due to their interesting chemistry and wide utility as radical precursors and intermediates in organic synthesis. They also have found many of applications, that is, in agriculture and medicine. They are in use as pesticides, as well as in the rubber industries as vulcanization accelerators; and as antioxidants. Because they exhibit strong metal-binding capacity, they can act as in inhibitors of enzymes and have a profound effect on biological systems. Moreover, they have found application in the treatment of cancer and HIV.     

Controlled release of volatiles under mild reaction conditions: from nature to everyday products

Volatile organic compounds serve in nature as semiochemicals for communication between species, and are often used as flavors and fragrances in our everyday life. The quite limited longevity of olfactive perception has led to the development of pro-perfumes or pro-fragrances--ideally nonvolatile and odorless fragrance precursors which release the active volatiles by bond cleavage. Only a limited amount of reaction conditions, such as hydrolysis, temperature changes, as well as the action of light, oxygen, enzymes, or microorganisms, can be used to liberate the many different chemical functionalities. This Review describes the controlled chemical release of fragrances and discusses additional challenges such as precursor stability during product storage as well as some aspects concerning toxicity and biodegradability. As the same systems can be applied in different areas of research, the scope of this Review covers fragrance delivery as well as the controlled release of volatiles in general.     

Application of INAA to the Examination of Art Objects: Research in Poland

Systematic studies on art objects using instrumental neutron activation analysis and neutron autoradiography have been carried out in the Institute of Nuclear Chemistry and Technology in collaboration with the Faculty of Art Conservation and Restoration of the Academy of Fine Arts in Cracow, as well as with other Academies of Fine Arts and museums in Poland. It was possible to accumulate a number of essential data on the concentration of trace elements particularly in chalk grounds and pigments (such as lead white, lead-tin yellow, smalt), Chinese porcelain, Thai ceramics, as well as in the clay fillings of sarcophagi of Egyptian mummies. The above mentioned examination of art objects prior to their conservation helps to determine precisely the materials used in the process of creating art objects, as well as to identify the approximate place of origin of particular materials.     

Ionic liquids and CE combination

This paper reviews and discusses the analytical combination of ionic liquids (IL) with CE. On the one hand, it shows CE as a powerful technique to separate impurities from IL as well as being capable to determine physical and chemical properties of IL. On the other hand, it also shows how IL are employed in CE separations to enhance resolution, peak efficiency and peak symmetry. Specifically, IL are used as additives in CZE, NACE, and MEKC and as support coatings of the capillary wall in electrochromatography. The integrity of the IL in the electrophoretic system as well as the roles of the cations and anions of the IL in the electrophoretic separation are also discussed.     

Photoinduced ionic polymerization. VII. Cationic polymerization of cyclohexene oxide in solid state

Photopolymerization of cyclohexene oxide in the presence of electron acceptors was studied in a bulk system (in liquid as well as in solid states). The polymerization was proved to proceed by a cationic mechanism in both states by the effect of inhibitors. In a liquid phase the light intensity dependence of the rate of polymerization and the molecular weight distribution showed a contribution of a free ionic polymerization. Any discontinuous phenomenon in the rate as well as in the molecular weight was not discerned between liquid(above ?36°C) and plastic crystal (between ?36 and ?81°C) phases. A quantum yield of monomer consumption as high as 8 × 10³ was observed in the plastic crystal phase. Below ?81°C in the normal crystal phase the rate as well as the molecular weight was remarkably suppressed.     

4. Characteristics of cellulose acetates 4.1 Characterization and physical properties of cellulose acetates

An overview is provided of the basic features of cellulose acetate of various degree of substitution in the solid and liquid crystalline state as well as in solution. These features represent a necessity for an understanding of the properties of these cellulose derivatives and further for mixed esters, which are not presented in this paper. Specifically, the crystal structure of cellulose triacetate will be addressed as well as structures in dilute and semi-dilute solutions. Thermal, viscoelastic and further properties in the solid state are discussed as well as flow behavior of solutions and their application in molecular weight determination, including false viscosity of commercial 2.5 cellulose acetates.     

Asymmetric multicomponent reactions (AMCRs): the new frontier

Asymmetric multicomponent reactions involve the preparation of chiral compounds by the reaction of three or more reagents added simultaneously. This kind of addition and reaction has some advantages over classic divergent reaction strategies, such as lower costs, time, and energy, as well as environmentally friendlier aspects. All these advantages, together with the high level of stereoselectivity attained in some of these reactions, will force chemists in industry as in academia to adopt this new strategy of synthesis, or at least to consider it as a viable option. The positive aspects as well as the drawbacks of this strategy are discussed in this Review.     

Aptamers: molecular tools for analytical applications

Aptamers are artificial nucleic acid ligands, specifically generated against certain targets, such as amino acids, drugs, proteins or other molecules. In nature they exist as a nucleic acid based genetic regulatory element called a riboswitch. For generation of artificial ligands, they are isolated from combinatorial libraries of synthetic nucleic acid by exponential enrichment, via an in vitro iterative process of adsorption, recovery and reamplification known as systematic evolution of ligands by exponential enrichment (SELEX). Thanks to their unique characteristics and chemical structure, aptamers offer themselves as ideal candidates for use in analytical devices and techniques. Recent progress in the aptamer selection and incorporation of aptamers into molecular beacon structures will ensure the application of aptamers for functional and quantitative proteomics and high-throughput screening for drug discovery, as well as in various analytical applications. The properties of aptamers as well as recent developments in improved, time-efficient methods for their selection and stabilization are outlined. The use of these powerful molecular tools for analysis and the advantages they offer over existing affinity biocomponents are discussed. Finally the evolving use of aptamers in specific analytical applications such as chromatography, ELISA-type assays, biosensors and affinity PCR as well as current avenues of research and future perspectives conclude this review.     

Synthesis of 3D printing materials and their electrochemical applications

Three-dimensional(3 D) printing, also known as additive manufacturing, has the advantages of low cost,easy structure operation, rapid prototyping, and easy customization. In the past few years, materials with different structures, compositions, and properties have been widely studied as prospects in the field of 3 D printing. This paper reviews the synthesis methods and morphologies of one-, two-and threedimensional micro/nano materials and their composites, as well as their applications in elec...     

Determination of phosphonoformic acid in human plasma and urine by high-performance liquid chromatography with electrochemical detection

Trisodium phosphonoformate (foscarnet) is used in the treatment of cytomegalovirus infections in immunocompromised patients, such as bone marrow and renal transplant recipients, as well as patients with the acquired immune deficiency syndrome. A simple high-performance liquid chromatographic assay is described using an electrochemical detector. The method is accurate, precise and reproducible. Hydrochlorothiazide is used as the internal standard. This assay allows measurement of foscarnet in biological fluids at concentrations as low as 33 microM. This method is being used for the analysis of samples in clinical trials and is important in the evaluation of the pharmacokinetic disposition of the drug.     

Trennung und bestimmung der einzelnen eisenspezies in wässriger lösung mit hilfe der Elektrophorese unter Schutzgasatmosphäre

Electrophoresis in an inert atmosphere with CDTA as complexing agent in the electrolyte system permits the separation of dissolved Fe(II) and Fe(III) as well as that of the colloidal and undissolved Fe(III) in solutions containing strong complexing agents or micro-organisms. The separated iron species are subsequently determined by spectrophotometry or by atomic-absorption spectroscopy after elution, or by direct photometry, plotting absorbance as a function of distance along the electro-phoretogram. The method is suitable for the determination of the iron in two oxidation states in synthetic nutritive fluids containing bacteria as well as in natural waters.     

The Role of Microencapsulation in Food Application

Modern microencapsulation techniques are employed to protect active molecules or substances such as vitamins, pigments, antimicrobials, and flavorings, among others, from the environment. Microencapsulation offers advantages such as facilitating handling and control of the release and solubilization of active substances, thus offering a great area for food science and processing development. For instance, the development of functional food products, fat reduction, sensory improvement, preservation, and other areas may involve the use of microcapsules in various food matrices such as meat products, dairy products, cereals, and fruits, as well as in their derivatives, with good results. The versatility of applications arises from the diversity of techniques and materials used in the process of microencapsulation. The objective of this review is to report the state of the art in the application and evaluation of microcapsules in various food matrices, as a one-microcapsule-core system may offer different results according to the medium in which it is used. The inclusion of microcapsules produces functional products that include probiotics and prebiotics, as well as antioxidants, fatty acids, and minerals. Our main finding was that the microencapsulation of polyphenolic extracts, bacteriocins, and other natural antimicrobials from various sources that inhibit microbial growth could be used for food preservation. Finally, in terms of sensory aspects, microcapsules that mimic fat can function as fat replacers, reducing the textural changes in the product as well as ensuring flavor stability.     

Crayfish Procambarus clarkii shows circadian variations in different parameters of the GSH cycle

The present study investigated the rhythmic changes in glutathione status in midgut gland and hemolymph as well as in glutathione reductase (GR) activity in the crayfish Procambarus clarkii. In order to determine the circadian nature of these rhythms different groups of crayfish were submitted to constant-darkness conditions for 24 or 72 h after they had spent 15 days under light-dark 12:12 cycles. The animals of the different batches were killed at 6 h intervals during a 24 h cycle. Reduced glutathione (GSH) and oxidized glutathione (GSSG) in hemolymph and midgut as well as midgut GR activity were determined in midgut gland and hemolymph by fluorometric and spectrophotometric method. Data analysis by chronogram and single Cosinor revealed circadian rhythmicity for GSH and GSSG concentration in both tissues as well as midgut GR activity. The rhythm parameters revealed oxidative stress induced by light. The possible correlation between the glutathione rhythm and other metabolic and behavioral rhythms of crayfish as well as the importance of the glutathione circadian temporal order in the adaptation of crayfish are discussed.     

Experimental and theoretical challenges in the chemistry of noncovalent intermolecular interaction and clustering

The weak, noncovalent interactions among molecules at long range and as close as van der Waals contact form a crucial contemporary frontier for chemical physics, one with many challenges for experimental as well as theoretical investigation. Certain of these challenges have been met in the last two decades, but as recognition of the complexity of phenomena governed or affected by weak interaction has grown, new challenges have arisen. We discuss a number of these challenges in the context of recent developments and progress, highlighting both disparate objectives of theory and experiment in this area as well as their crucial interplay.     

Recent Progress toward white organic light emitting diodes

An efficient and stable white organic light emitting diode (WOLED) is highly desirable in potential applications such as lighting, background light source, and full color display.A series of highly fluorescent dyes based on a dipyrazolopyridine skeleton,1,7-diphenyl-l,7-dihydrodipyrazolo[3,4-b,4′,3′-e]pyridine, were synthesized and evaluated as emitting as well as charge-transporting material in the fabrication of electroluminescent devices.Several of the blue derivatives are found to be useful as the source of blue emission in fabricating bright white-emitting devices. The choice of dopants, cathode materials, electron-transporting materials as well as the device configurations greatly affect the emission profile, efficiencies, as well as the device lifetime. The latest progress in achieving a more efficient, color stable, durable white light device will be discussed.     

Separation of isomers of acyl glucuronides using micellar electrokinetic capillary chromatography in dynamically coated capillaries

The acyl glucuronide metabolites of endogenous as well as of xenobiotic compounds may undergo isomerization in vitro as well as in the human body. The parent acyl glucuronide and the isomerization products may react with endogenous protein to form products which in worst cases may act as antigens and thus create an allergic response. In the present paper new methods based on micellar electrokinetic or microemulsion electrokinetic chromatography for the separation of all isomerization products as well as the hydrolysis product of acyl glucuronides are described. In order to perform the separation at lower pH values in a reasonable time dynamically coated capillaries were used. This enables the electroosmotic flow to be high and constant even at low pH. The methods were developed using S-naproxen-beta-1-O-acyl glucuronide as the model substance. The assignment of the single peaks in the electropherogram was performed tentatively based on the sequential appearance of the isomerization products with time.     

Spektrochemische schnellbestimmung einiger spurenelemente in der kohlenasche mit alumininmelektroden und verwendung des sichtbaren spektralgebietes

Using an a.c. arc and visible spectral lines a spectrographic method for the rapid determination of traces of Co, Cr, Ga.In, Pb and V in synthetic coal ashes has been worked out, in which the samples are burned in Al electrodes thus avoiding perturbation by cyanogen bands. With the help of intensity-time studies an exposure time of 10 sec was found giving optimum power of detection as well as optimum reproducibility. By a suitable choice of experimental conditions the background density was adjusted to a value which permitted making accurate background corrections and using the background as reference radiation at the same time. Variation of the method included the application of intermediate diaphragms and the use of Fe-lines as well as of the background as reference signals with and without background correction. The standard deviations as well as the tested concentration ranges are reported.     

Simultaneous separation of mercury and lignosulfonate from aqueous solution using supported liquid membrane

This paper presents an experimental investigation on facilitated and simultaneous transport of mercury and lignosulfonate (LS) through a flat sheet supported liquid membrane (SLM) having Nylon 6,6 as support, trioctylamine (TOA) as carrier and dichloroethane as solvent. The experiments were performed at various operating conditions such as strip phase concentration, feed pH, carrier concentration and feed concentration to find the best set of parameters that would yield the maximum separation of pure mercury as well as its mixture with LS. The experiments were performed in co-transport mode using NaOH as the strip phase. It was observed that extraction of mercury as well as its mixture increases with increase in concentration of NaOH up to a certain limit 0.1 M NaOH in case of pure solution and 0.2 M NaOH in case of mixture). Feed phase pH significantly affects the mercury separation process. However, initial feed concentration does not affect the extraction process appreciably. Separation of mixture of mercury and LS behaves in a similar way as their pure solution; however the extraction is low in comparison to pure solution. The extraction of mercury from its pure solution is about 81% in 1 h. The extraction of mercury and LS from their mixture is about 52.6% and 50.2%, respectively at optimum condition and in a period of 2 h.     

Determination of Selenium Species in Environmental Samples

 The essential nature of selenium as well as its toxicity depend on the concentration and the chemical forms in which this element is present in a given sample. Dissolved inorganic selenium can be found in natural water and soil as selenides, selenite and selenate. Organoselenium compounds present in air, soil and plants are volatile methylselenides, trimethylselenonium ion and several selenoamino acids. This review is a summary of recent research on the determination of selenium species in environmental samples such as water, air, soil and plants. Stability of selenium species in solutions and their storage is also discussed. In the metabolic pathway in the body selenide could act as the common intermediate for inorganic and organic Se sources as well as the checkpoint between further utilisation and excretion of selenium. Received May 30, 2001; accepted October 19, 2001; published online July 15, 2002