Selective determination of trace arsenic and antimony species in natural waters by gas chromatography with a photoionization detector

Traces amounts of arsenic and antimony in water samples were determined by gas chromatography with a photoionization detector after liquidnitrogen cold trapping of their hydrides. The sample solution was treated with sodium hydroborate (NaBH₄) under weak-acid conditions for arsenic(III) and antimony(III) determination, and under strong-acid conditions for arsenic(III+V) and antimony(III+V) determination. Large amounts of carbon dioxide (CO₂) and water vapor obscured determination of arsine and stibine. Better separation from interference could be achieved by removing CO₂ and water vapor in two tubes containing sodium hydroxide pellets and calcium chloride, respectively. The detection limits of this method were 1.8 ng dm^?3 for arsenic and 9.4 ng dm^?3 for antimony in the case of 100-cm³ sample volumes. Therefore, it is suitable for determination of trace arsenic and antimony in natural waters.     

Biomimetic reactions of some macrocyclic diterpenes

Some macrocyclic diterpenes derived from euphohelioscopin A and euphornin have been stereoselectively converted into the jatropholane- and daphnane-type compounds and the known tricyclic compound which has been treated with phCOCl - pyridine to afford euphohelionone, the new type of diterpene isolated from euphorbia helioscopia L.     

Mean curvature flow through singularities for surfaces of rotation

In this paper, we study generalized “viscosity” solutions of the mean curvature evolution which were introduced by Chen, Giga, and Goto and by Evans and Spruck. We devote much of our attention to solutions whose initial value is a compact, smooth, rotationally symmetric hypersurface given by rotating a graph around an axis. Our main result is the regularity of the solution except at isolated points in spacetime and estimates on the number of such points.     

Flavonol glycosides in leaves of two Diospyros species

Fourteen flavonol glycosides including two new compounds were isolated from the leaves of two Diospyros plants (D. cathayensis and D. rhombifolia). The structures of isolated compounds were determined by spectroscopic analysis. The scavenging activity of 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical of the isolated compounds was also investigated.     

Glycosylidene Carbenes. Part 7. Neighbouring-group participation by the 2-benzyloxy group in the glycosidation of strongly acidic hydroxy compounds

To demonstrate the neighbouring-group participation of the 2-benzyloxy group in the glycosidation of phenols and of strongly acidic alcohols by the diazirine 1 , we examined the glycosidation of 4-nitrophenol, 4-methoxyphenol, (CF₃)₂CHOH, MeOH, and i-PrOH by the diazirine 11 , derived from the 2-deoxypyranose 6 . Oxidation of the oximes 7 yielded (E)- and (Z)- 8 . In solution, (E)- 8 isomerised to (Z)- 8 . Similarly, the (E)-configurated mesylate 9 , prepared from 8 , underwent acid-catalysed isomerisation to (Z)- 9 . Treatment of (Z)- 9 with NH₃, followed by oxidation of the resulting diaziridine 10 with I₂, yielded the desired diazirine 11 . Glycosidation by 11 of the above mentioned hydroxy compounds yielded the glycosides 12–21 . In agreement with the postulated neighbouring-group participation, these glycosidation proceeded without, or with a very low diastereoselectivity, favouring the axial anomers.     

Single-crystalline M-type Sr Hexaferrites studied by <Superscript>57</Superscript>Fe Mössbauer spectroscopy

The ⁵⁷Fe Mössbauer spectra of the single crystalline and the finely ground Sr_1?x La _x Fe_12?y Co _y O₁₉ (x = 0 : y = 0, x = 0.192 : y = 0.152 and x = 0.456 : y = 0.225) samples have been measured to investigate the La-Co substitution effects. All observed spectra at 150 K were well fitted using the five subspectra which correspond to the five crystallographical nonequivalent Fe sites in the M-type hexaferrite, indicating that the valence changes to Fe²⁺ ions in the Fe³⁺ ions were not observed in our Sr_1?x La _x Fe_12?y Co _y O₁₉ samples. In SrFe₁₂O₁₉, the relative absorption intensities in the five subspectra show the large anisotropies in the recoilless fractions at the five Fe sites whereas these anisotropies were not observed in Sr_0.544La_0.456Fe_11.775Co_0.225O₁₉. These results indicate the chemical compositional dependence on the anisotropies of the recoilless fractions at the five Fe sites. The substitution of a Co²⁺ ion for the Fe³⁺ ion changes the center shifts of the Fe³⁺ ions near the Co²⁺ ion by the perturbation of the Fe-O-Co hybridizations. Therefore, the Co²⁺ ions occupy the 4f ₁ and the 4f ₂ sites due to the chemical compositional dependences of the refined magnetic hyperfine field and center shifts of the Fe³⁺ ions.     

Statistical Prediction under an Order Restriction

In this paper, a statistical prediction problem under ordered location and scale parameters are considered. Double-shrinkage predictors are given which use all the available data and improve on single-shrinkage predictors, and hence the best equivariant predictors.     

Reaction of α,β‐unsaturated ketones with cerium(IV) salts in alcohol

Reaction of α,β‐unsaturated ketones with cerium(IV) salts or lanthanide triflates in alcohols gave good yields of the corresponding β‐alkoxy compounds. In the case of 2‐cyclopentenone and 2‐cyclohexenone, the 1,1,3‐trialkoxy acetal derivatives were obtained preferentially accompanied by β‐alkoxyketone, except 2‐cycloheptenone. However, in the reaction of 2‐cycloheptenone with alcohol using cerium(IV) sulfate (CS)‐molecular sieve, 1,1,3‐trialkoxy derivatives were obtained. Also, in the cases of 1‐penten‐3‐one, 4‐hexen‐3‐one and 3‐hepten‐2‐one, 1,1,3‐trialkoxy derivatives were obtained preferentially. Copyright © 2006 John Wiley & Sons, Ltd.