Extraction and spectrophotometric determination of zinc in coal fly ash and pond sediments with 2-[2-(3,5-dibromopyridyl)azo]-5-dimethylaminobenzoic acid

An extraction-spectrophotometric method is described for the determination of traces of zinc with 2-[2-(3,5-dibromopyridyl)azo]-5-dimethylaminobenzoic acid. The reagent forms a stable, blue 1:2 zinc/reagent complex that can be extracted into chloroform. The apparent molar absorptivity of the zinc(II) complex is 1.26 × 10⁵ l mol^?1 cm^?1 at 610 nm in chloroform. The reagent is relatively selective; interferences from cobalt, copper and nickel can be masked with dimethylglyoxime and aluminium and iron with a mixture of sodium fluoride and triethanolamine. The method is applied to the determination of zinc in coal fly ash and pond sediments with good precision and accuracy.     

Extraction-spectrophotometric determination of anionic surfactants with a flow-injection system

Anionic surfactants are preconcentrated from 5-ml samples by extraction as the ion-pair with ethyl violet into toluene. The absorbance of aliquots of the toluene phase is measured at 610 nm in a flow-injection system. A phase converter is located prior to the injection valve to convert a water stream to, pumped with ordinary pump tubing, to a toluene stream. The working range was 0.01–1.0 mg l^?1 and the reproductibility (r.s.d, n = 10) was 2% for 0.4 mg l^?1 sodium dodecyl sulphate. The non-aqueous flow-injection system serves to miniaturize the extraction from separatory funnel (200 ml) to test tube (10 ml) scale without loss of precision or validity.     

Search for a simpler synthetic model system for intramolecular 1,3-dipolar cycloaddition to the 5,6-double bond of a pyrimidine nucleoside

In search for a simpler model system for the study of intramolecular thermal reactions between the base and 5'-functionalized sugar moiety in nucleosides, 1-(3-azidopropyl)uracil (2), 1-(4-azidobutyl) pyrimidines (12 and 13) and 1-(5-azidopentyl)-uracil (14) was synthesized through the corresponding ω-benzoyloxy-(6,7 and 8) and ω-hydroxyalkyl-pyrimidines (9,10 and 11). Heating 2 gave 1,N⁶-trimethylene-6-aminouracil (4), while heating 12 and 13 gave N¹-C₆ cleaved addition products. 15 and 16, respectively. 15 was regiospecifically transformed to 1,2,3-triazole derivatives, 17,18 and 19. Heating 1-(4-azidobutyl)-5-bromouracil (20) yielded 3,9-tetramethylene-8-azaxanthine (22). 9 with NBA gave 1,0⁶-tetramethylene-5-bromo-6-hydroxy-5,6-dihydrouracil (24) and the 5-brominated analog of 9 (25). The 4-functionalized butyl side chain proved to serve as a substitute for the 5'-functionalized sugar moiety in pyrimidine ribonucleosides.     

Syntheses of tetraoxaquaterene derivatives

Several new dimethyl and tetramethyl tetraoxaquaterenes, 3d and 3e , have been prepared in order to synthesize the oxygen analogues of porphyrin. The reaction between furan and a ketone using an acidic catalyst gave the cyclic tetramer, tetraquaterene, and oligomers. On the other hand, in the case of furan and an aldehyde, only linear oligomers were isolated. The condensation of furan-containing dimers with carbonyl compounds, both ketone and aldehyde, except formaldehyde, gave the tetraoxaquaterene. In the case of formaldehyde, the yield of cyclic tetramer was negligible.     

Certain algebraic surfaces with Eisenbud‐Harris general fibration of genus 4

We classify the algebraic surfaces with Eisenbud‐Harris general fibration of genus 4 over a rational curve or an elliptic curve whose slope attains the lower bound. The classification of our surfaces is strongly related to the result of the classification for certain relative quadric hypersurfaces in 3‐dimensional projective space bundles over a rational curve and an elliptic curve. We further prove some results about the canonical maps, the quadric hulls of the canonical images and the deformation for these surfaces.     

Eisenbud-Harris special non-hyperelliptic fibrations of genus 4

We define certain index for the degenerate fibers in non-hyperelliptic fibrations of genus 4 but not Eisenbud-Harris general. Furthermore, we investigate the structure of the surfaces which have the pencil as above, and whose sum of the indices is equal to 0 or near 0.     

as-Triazine chemistry. V.The oxidative ring-opening of 5,6-diphenyl-as-triazine-3(2H)-ones with Organic Peracids

The structures of the oxidation products of 5,6-diphenyl-as-triazine-3(2H)-ones (Ia-b) with organic peracids were chemically and spectroscopically reinvestigated and it was concluded that the products were 1,4-dibenzoyl semicarbazide (IIa) and the 2-methyl analogue (IIb).     

Acceleration of the photodimerization of water-soluble anthracenes included by β- and γ-cyclodextrins

The photodimerization of 2-anthracenesulfonate in water was accelerated in the presence of - and -cyclodextrins (CyDs). While four configurational isomers of the photodimer were obtained in the presence of -CyD with similar ratio of the yields to that in the host-free solution, only one of the isomers was obtained in the presence of -CyD. The results were explained by the formation of two guest-one host inclusion complex in the former case and of two guest-two host inclusion complex in the latter. No evidence of an inclusion complex with -CyD was obtained. The inclusion effects of CyD on the photodimerization of other water-soluble anthracenes were also examined.     

Fluorimetric determination of hepatic delta-aminolevulinic acid synthase activity by high-performance liquid chromatography

A fluorimetric method for measuring the activity of delta-aminolevulinic acid synthase (ALAS) in the liver of mice has been developed. The liver homogenate was used as the enzyme source. The final concentration of glycine (substrate) used for the assay was 100 mM. The delta-aminolevulinic acid (ALA) formed during incubation was converted into a highly fluorescent derivative by condensation with acetylactone and formaldehyde (application of the Hantzsch reaction). This derivative was completely separated from other fluorescent substances in the reaction medium, and it was determined using a high-performance liquid chromatograph equipped with a fluorescence monitor (370/460 nm). The activity of ALAS was expressed as nmol ALA formed per gram liver per hour.     

New approach to a novel axially chiral ligand showing spontaneous enrichment of axial chirality

We have synthesized novel axially chiral ligand with two chiral centers, (R)-(R)(2)- and (S)-(S)(2)-2,2'-bis(2,2,2-trifluoro-1-hydroxyethyl)biphenyl (1), which showed a high asymmetric induction when used as ligand. Here, another new approach to 1 by kinetic and thermodynamic resolution is presented which gave these ligands in a much shorter steps, in a higher yield, and in a higher enantiomeric excess.