Rapid and simultaneous analysis of dichlorvos, malathion, carbaryl, and 2,4-dichlorophenoxy acetic acid in citrus fruit by flow-injection ion spray ionization tandem mass spectrometry

A simple method for the rapid and simultaneous analysis of dichlorvos (DDVP), malathion, carbaryl, and 2,4-dichlorophenoxy acetic acid (2,4-D) in citrus fruit, which uses flow-injection ion spray ionization tandem mass spectrometry, has been developed for the first time. The method involves the combined use of stable isotopically labeled internal standards (DDVP-d₆, malathion-d₁₀, carbaryl-d₇, and 2,4-D-d₅) and a multiple reaction monitoring technique. The average recoveries for the pesticides at the same concentrations as their tolerance levels (DDVP: 0.1-0.2 μg g⁻¹; malathion: 0.5-4.0 μg g⁻¹; carbaryl: 1.0 μg g⁻¹; 2,4-D: 1.0-2.0 μg g⁻¹) ranged from 90 to 119% with the relative standard deviation (R.S.D.) ranging from 1.0 to 13.1% (n = 5). Analysis time, including sample preparation and determination, was only 15 min. The present method is effective for screening DDVP, malathion, carbaryl, and 2,4-D in citrus fruit.     

Preparation of Metallaiminophosphoranes and Their Reactivity

Treatment of [Cp*(CO) 2 M{P(NHPh)(OMe) 2 }]PF 6 (M = Fe and Ru) with NaNH 2 gives metallaiminophosphoranes, Cp*(CO) 2 M{P(NPh)(OMe) 2 }. The x-ray structures and reactivity of the complexes are reported.     

Effect of Amines on the Selective Bromination of Some β-Substituted-2-Butenoic Esters

The effect of amines on the selective bromination of some β-substituted-2-butenoic esters is described. The bromination of methyl (Z)-4-t-butyldiphenylsilyloxy-3-methylbutenoate 2 in the presence of DIPEA (N, N-diisopropylethylamine) and the successive treatment of the obtained dibromide with potassium t-butoxide afford the desired Z bromide selectively. But the corresponding E bromide forms exclusively when 2, 6-di-t-butyl-4-methylpyridine is used in the bromination.     

Complexation of hydrazine with native cellulose in water and toluene

Adsorption–complexation of cellulose by hydrazine solutions in water and toluene was studied for native cellulose of varied crystallinity. Penetration of hydrazine into cellulose takes place more readily in hydrazine solution of higher concentration and with cellulose of lower crystallinity, but the equilibrium uptake was nearly independent of crystallinity. Complexation from toluene solution takes place at lower hydrazine concentration in toluene than in water, presumably because of the difference in hydrazine–solvent interaction. The adsorption isotherm of hydrazine in water is likely to be sigmoid, implying a cooperative sorption mechanism. It can presumably be ascribed to the disordered structure in the course of complexation.     

Calorimetric evidence for a Fulde-Ferrell-Larkin-Ovchinnikov superconducting state in the layered organic superconductor kappa-(BEDT-TTF)2Cu(NCS)2

The specific heat of the layered organic superconductor kappa-(BEDT-TTF)(2)Cu(NCS)(2), where BEDT-TTF is bisethylenedithio-tetrathiafulvalene, has been studied in magnetic fields up to 28 T applied perpendicular and parallel to the superconducting layers. In parallel fields above 21 T, the superconducting transition becomes first order, which signals that the Pauli-limiting field is reached. Instead of saturating at this field value, the upper-critical-field increases sharply and a second first-order transition line appears within the superconducting phase. Our results give strong evidence that the phase, which separates the homogeneous superconducting state from the normal state is a realization of a Fulde-Ferrell-Larkin-Ovchinnikov state.     

Bleaching effect of a 405-nm diode laser irradiation used with titanium dioxide and 3.5% hydrogen peroxide

A 405-nm diode laser has recently been developed for soft tissue problems in dentistry. A new in-office bleaching agent consisting of a titanium dioxide photocatalyst and 3.5% hydrogen peroxide has proven to react well with light irradiated at a wavelength of around 400 nm. In this study, we evaluated the bleaching efficacy of a newly developed 405-nm diode laser on bovine teeth treated with a bleaching agent composed of titanium dioxide and 3.5% hydrogen peroxide. Sixteen bovine incisors were randomly divided into two groups: Group A, irradiated by the 405-nm diode laser at 200 mW; Group B, irradiated by the 405-nm diode laser at 400 mW. The bleaching agent with titanium dioxide and 3.5% hydrogen peroxide was applied to bovine enamel and irradiated for 1 min. The specimens were then washed and dried, and the same procedure was repeated nine more times. After irradiation, we assessed the effects of bleaching on the enamel by measuring the color of the specimens with a spectrophotometer and examining the enamel surfaces with a scanning electron microscope. L* rose to a high score, reaching a significantly higher post-treatment level in comparison to pretreatment. In a comparison of the color difference (ΔE) between Group A and Group B, the specimens in Group B showed significantly higher values after 10 min of irradiation for the post-treatment. No remarkable differences in the enamel surface morphology were found between the unbleached and bleached enamel. The use of a 405-nm diode laser in combination with a bleaching agent of titanium dioxide and 3.5% hydrogen peroxide may be an effective method for bleaching teeth without the risk of tooth damage.     

Formation and stability of cellulose–copper–NaOH crystalline complex

We investigated the crystal structure of alkali-celluloses, Na-cellulose IIA and II(Cu), formerly known as Na-cellulose IIB, by synchrotron X-ray diffraction. Na-cellulose IIA, formed from cellulose I by high-concentration NaOH treatment, has a fiber repeat of 15 Å and a threefold-like helical conformation. Na-cellulose II(Cu), prepared by treating cellulose I with copper-saturated alkali solution, also has a fiber repeat of 15 Å with threefold helical symmetry. Incorporation of Cu(II) ions into cellulose was confirmed by multiwavelength anomalous diffraction. Monitoring by X-ray diffraction revealed that the formation of this complex from cellulose I is remarkably slow, probably because of the involvement of copper ion. The stability of alkali-cellulose II(Cu) was tested to estimate the influence of the presence of copper in the crystal. Na-cellulose II(Cu) characteristically dissolved in aqueous ammonia solution, indicating strong coordination of copper ion to cellulose.     

Characterization of tension and normally lignified wood cellulose inPopulus maximowiczii

We have investigated unlignified tension wood and normally lignified wood celluloses inPopulus maximowiczii with particular reference to the composition of two crystalline phases I/I (triclinic/ monoclinic). Four independent techniques, which enable us to detect the two phases, CP/MAS¹³C NMR, Fourier transform infrared microscopy, selected-area electron diffraction, and X-ray diffraction were applied. Because of the low crystallinity of wood celluloses, particularly in the case of celluloses in the lignified cell wall, no single method was decisive enough to be able to determine the composition of the two phases as one can with highly crystalline materials. The I dominant structure (monoclinic crystal type) was, however, preferred for both tension and normal wood celluloses.