Improved sample preparation method for environmental plutonium analysis by ICP-SFMS and alpha-spectrometry

A rapid and simple sample preparation method for plutonium determination in environmental samples by inductively coupled plasma sector field mass spectrometry (ICP-SFMS) and alpha-spectrometry is described. The developed procedure involves a selective CaF₂ co-precipitation for preconcentration followed by extraction chromatographic separation. The proposed method effectively eliminates the possible interferences in mass spectrometric analysis and also removes interfering radionuclides that may disturb alpha-spectrometric measurement. For ²³⁹Pu, ²⁴⁰Pu and ²⁴¹Pu limits of detection of 9.0 fg·g⁻¹ (0.021 mBq), 1.7 fg·g⁻¹ (0.014 mBq) and 3.1 fg·g⁻¹ (11.9 mBq) were achieved by ICP-SFMS, respectively, and 0.02 mBq by alpha-spectrometry. Results of certified reference materials agreed well with the recommended values.     

Dipyrrolo[1,2-a;2',1'-c]pyrazines. 6. Electrophilic Substitution in a Series of Dipyrrolo[1,2-a;2',1'-c]pyrazine and 5,6-Dihydrodipyrrolo[1,2-a;2',1'-c]pyrazine Derivatives. Phosphorylation of Dipyrrolo[1,2-a;2',1'-c]pyrazines

We have studied the behavior of asymmetrically substituted dipyrrolo[1,2-a;2',1'-c]pyrazines and their 5,6-dihydro analogs under phosphorylation reaction conditions.     

Chiral separation of pyrethroic acids with single isomer permethyl monoamino beta-cyclodextrin selector

Enantiomers and diastereomers of chrysanthemic, permethrinic, and deltamethrinic pyrethroic acids were separated from each other, using positively ionizable permethyl monoamino beta-cyclodextrin (PMMAbetaCD). The highest chiral resolution value was 20.0. The optimum conditions of separation were found to be 16 mM PMMAbetaCD concentration and pH 6.5, where analytes and selector were in oppositely ionized states. Selectivity of PMMAbetaCD proved to be the best among the cyclodextrin derivatives studied.     

Phytoecdysteroids of plants of the genusSilene XIV. Brahuisterone fromSilene brahuica

A new ecdysteroid with the composition C₂₇H₄₄O₆ which has been called brahuisterone has been isolated from the epigeal part of the plantSilene brahuica Boiss. Its chemical and complete spatial structures have been established by spectral studies and the x-ray structural method (diffractometer, Cu-K radiations, 996 reflections, direct method, R=0.119).Institute of the Chemistry of Plant Substances, Academy of Sciences of the Uzbekistan Republic, Tashkent. Translated from Khimiya Prirodnykh Soedinenii, No. 4, pp. 553–558, July–August, 1993.     

Electrophilic addition of lead tetraacetate to 2-carene in an acidic medium

Oxidation of 2-carene by lead tetraacetate in acetic acid afforded p-menth-1(10),2-dien-7-ol, 2-acetyl-6,6-dimethylbicyclo[3.1.0]hexane, p-menth-2-ene-1,7-diol, p-menth-1-ene-3,7-diol, and 2-(m-tolyl)propanol-2.Deceased.A. M. Butlerov Scientific Research Chemical Institute, V. I. Ul'yanov-Lenin Kazan' State University, 420008 Kazan. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 1, pp. 147–150, January, 1992.     

Synthesis and properties of benzyl-substituted thiiranes

The reaction of phenyl- and p-tolylmagnesium bromides, as well as di, tri, and tetramethylbenzene, with epichlorohydrin was used to synthesize the corresponding chlorohydrins, which were then converted to various benzyl-substituted oxiranes and thiiranes.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 5, pp. 598–602, May, 1988.     

Polargraphic adsorptive waves of alkaline-earth metal complexes with thymolphthalexone

Sensitive derivative polarographic adsorption waves have been observed for alkaline-earth metal-TP complexes in 0.15M potassium hydroxide containing 3 x 10(-5)M thymolphthalexone (TP). The limit of detection for calcium, strontium and barium was 7.5 x 10(-7)M and for magnesium 4.0 x 10(-6)M. The proposed method has been used successfully for determining trace amounts of calcium in natural waters and hair samples. The composition of the complex has been shown to be 1:1 alkaline-earth metal:TP and various experiments have confirmed that the wave is an adsorption wave. The reaction mechanism has been studied by a number of methods.     

Synthesis and stereochemical studies of 6-substituted 1H,3H,6H,7aH-3,3-dimethylimidazo-[1,5-c]thiazol-5-one-7-thiones

The reaction of (4S)-5,5-dimethyl-4-thiazolidine-carboxylic acid 1 with alkyl and aryl isothiocyanates 2 gave bicyclic thiohydantoins 3 . The (2R,4S)- and (2S,4S)-mixtures of 2-substituted 5,5-dimethyl-4-thiazolidine-carboxylic acids 4 and 8 containing two centers of chirality in the analogous reaction afforded thiohydantoins 7 and 10 , respectively, with (1R)-configuration. In some cases we managed to isolate the thioureido acid intermediates 6 and 9 or their triethylamine salts which afforded the corresponding bicycles 7 and 10 under thermal cyclization or acidification. The stereochemistry has been elucidated by high resolution ram studies, optical rotation measurements and X-ray crystallography.