Lipase-catalyzed resolution of 1-hydroxymethyl-2-methylferrocene

±-1-Hydroxymethyl-2-methylferrocene was optically resolved by transesterification with lipases using vinyl esters such as vinyl butyrate, vinyl caproate, vinyl octanoate and vinyl decanoate, as acyl donors.     

Double-sensor method for detection of oscillating electric field

An electric-field sensor consisting of thin copper plates is designed to measure an oscillating electric field produced by charge separations on a plasma column. The sensor installed in a vacuum region around plasma detects charges induced by the electric field on the copper plates. The value of the induced charges depends not only on the strength of the electric field, but also on the design of the sensor. To obtain the correct strength of the electric field, a correction factor arising from the design of the sensor must be known. The factor is calculated numerically using Laplace's equation and compared with a value measured using a uniform electric field in the frequency range of 10-500 kHz. When an external circuit is connected to the sensor to measure the induced charges, the electric field around the sensor is disturbed. Therefore, a double-sensor method for excluding a disturbed component in the measured electric field is proposed. The reliability of the double-sensor method is confirmed by measuring dipole-like and quadrupole-like electric fields.     

Raman spectra of high‐density,low‐density,and linear low‐density polyethylene pellets and prediction of their physical properties by multivariate data analysis

Raman spectra have been measured for pellets of five samples of high‐density polyethylene (HDPE), seven samples of low‐density polyethylene (LDPE), and six samples of linear low‐density polyethylene (LLDPE). The obtained Raman spectra have been compared to find out characteristic Raman bands of HDPE, LDPE, and LLDPE. Principal component analysis (PCA) was applied to the Raman spectra in the 1600–650 cm^?1 region after multiplicative scatter correction (MSC) to discriminate the Raman spectra of the three different PE species. They are classified into three groups by a score plot of PCA factor 1 vs. 2. HDPE with high density and high crystallinity gives high scores on the factor 1 axis, while LDPE with low density and low crystallinity yields negative scores on the same axis. It seems that factor 1 reflects the density or crystallinity. A PC weight loadings plot for factor 1 shows six upward peaks corresponding to the bands arising from the crystalline parts or all‐trans ? (CH₂)_n? groups and seven downward peaks ascribed to the bands of the amorphous or anisotropic regions and those arising from the short branches. Partial least‐squares (PLS‐1) regression was applied to the Raman spectra after MSC to propose calibration models that predict the density, crystallinity, and melting points of the polyethylenes. The correlation coefficient was calculated to be 0.9941, 0.9800, and 0.9709 for the density, crystallinity, and melting point, respectively, and their root‐mean‐square error of cross validation (RMSECV) was found to be 0.0015, 3.3707, and 2.3745, respectively. The loadings plot of factor 2 for the prediction of melting point is largely different from those for the prediction of density and crystallinity. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 443–448, 2002     

Study of Densification Process and Microstructure for Highly Dense Doped MgB2 Bulk Samples

In order to give a contribution in the subject of MgB₂ processing technique to obtain low cost high density bulk samples with improved superconducting properties, studies on dilatometry and on the microstructures of in situ and ex situ MgB₂ bulk samples prepared in the presence of carbon compounds are presented in this paper. The ex situ densification was performed by isostatic pressure followed by high temperature treatment in air, which promoted high density samples compared to the common magnesium diboride in situ samples. It was observed that each carbon compound addition (hydrocarbon??C₈H₁₈, SiC and silicon oil??SiC₂H₆O), corresponds to one microstructure, which can be noticed even after the ex situ process for sintering the pellets. Among the compounds, the SiC showed to present the most irregular structure for the in situ samples. However, this microstructure showed to change completely and reaches higher density (90?%) very rapidly when heat treated in the ex situ process. The X ray diffraction (XRD) analyses also revealed that the presence of spurious phases??like Mg₂Si, Mg₃B₂O₆, MgO and others??for the ex situ samples treated in air at high temperature.     

Formation of bromo-substituted triclosan during chlorination by chlorine in the presence of trace levels of bromide

The side reactions of triclosan (2,4,4'-trichloro-2'-hydroxydiphenyl ether, TC) and chlorine in the presence of sodium chloride were investigated. In the absence of sodium chloride, three chloro-derivatives of TC, 2',3,4,4'-tetrachloro-2-hydroxydiphenyl ether (3-Cl-TC), 2',4,4',5-tetrachloro-2-hydroxydiphenyl ether (5-Cl-TC), and 2',3,4,4',5-pentachloro-2-hydroxydiphenyl ether (3,5-Cl(2)-TC) were formed, whereas in the presence of sodium chloride, 3-bromo-2',4,4'-trichloro-2-hydroxydiphenyl ether (3-Br-TC), 5-bromo-2',4,4'-trichloro-2-hydroxydiphenyl ether (5-Br-TC), (3 or 5)-bromo-2',4,4',(5 or 3)-chloro-2-hydroxydiphenyl ether ((3,5)-(BrCl)-TC), and 3,5-dibromo-2',4,4'-trichloro-2-hydroxydiphenyl ether (3,5-Br(2)-TC) were additionally formed. Radiochemical neutron activation analysis indicated that 1g of commercially available sodium chloride contained 73 microg of bromide and the bromide ion was determined to be the source of the side reactions. The rate of decrease of TC due to reaction with chlorine was greatly accelerated by the presence of bromide ion in the system: the rate with only 1 x 10(-5) M bromide ion was three times the rate in the absence of bromide.     

Enzymatic resolution of planar chiral ferrocene derivatives

Racemic 3-methyl, 2-ethyl, 2-bromo, and 2-trimethylsilyl derivatives of formylferrocene were kinetically resolved by enantioselective reduction with a fermenting baker's yeast. Moreover, 2-methyl, 3-methyl, 2-ethyl, 2-bromo, and 2-trimethylsilyl derivatives of hydroxymethylferrocene were optically resolved with lipases by transesterification using vinyl esters.     

Dry deposition of gaseous radioiodine and particulate radiocaesium onto leafy vegetables

Radionuclides released to the atmosphere during dry weather (e.g. after a nuclear accident) may contaminate vegetable foods and cause exposure to humans via the food chain. To obtain experimental data for an appropriate assessment of this exposure path, dry deposition of radionuclides to leafy vegetables was studied under homogeneous and controlled greenhouse conditions. Gaseous ¹³¹I-tracer in predominant elemental form and particulate ¹³⁴Cs-tracer at about 1 μm diameter were used to identify susceptible vegetable species with regard to contamination by these radionuclides. The persistence was examined by washing the harvested product with water. The vegetables tested were spinach (Spinacia oleracea), butterhead lettuce (Lactuca sativa var. capitata), endive (Cichorium endivia), leaf lettuce (Lactuca sativa var. crispa), curly kale (Brassica oleracea convar. acephala) and white cabbage (Brassica oleracea convar. capitata). The variation of radionuclides deposited onto each vegetable was evaluated statistically using the non-parametric Kruskal-Wallis Test and the U-test of Mann-Whitney. Significant differences in deposited ¹³¹I and ¹³⁴Cs activity concentration were found among the vegetable species.For ¹³¹I, the deposition velocity to spinach normalized to the biomass of the vegetation was 0.5-0.9 cm³ g^− 1 s^− 1 which was the highest among all species. The particulate ¹³⁴Cs deposition velocity of 0.09 cm³ g^− 1 s^− 1 was the highest for curly kale, which has rough and structured leaves. The lowest deposition velocity was onto white cabbage: 0.02 cm³ g^− 1 s^− 1 (iodine) and 0.003 cm³ g^− 1 s^− 1 (caesium). For all species, the gaseous iodine deposition was significantly higher compared to the particulate caesium deposition. The deposition depends on the sensitive parameters leaf area, stomatal aperture, and plant morphology. Decontamination by washing with water was very limited for iodine but up to a factor of two for caesium.     

Production and characterization of plutonium dioxide particles as a quality control material for safeguards purposes

Plutonium (Pu) dioxide particles were produced from certified reference material (CRM) 136 solution (CRM 136-plutonium isotopic standard, New Brunswick Laboratory, Argonne, IL, U.S.A., 1987) using an atomizer system on December 3, 2009 after chemical separation of americium (Am) on October 27, 2009. The highest density of the size distribution of the particles obtained from 312 particles on a selected impactor stage was in the range of 0.7-0.8 μm. The flattening degree of 312 particles was also estimated. The isotopic composition of Pu and uranium (U) and the amount of Am were estimated by thermal ionization mass spectrometry (TIMS), inductively coupled plasma mass spectrometry (ICPMS), and α-spectrometry. Within uncertainties the isotopic composition of the produced particles is in agreement with the expected values, which were derived from the decay correction of the Pu isotopes in the CRM 136. The elemental ratio of Am to Pu in the produced particles was determined on the 317th and 674th day after Am separation, and the residual amount of Am in the solution was estimated. The analytical results of single particles by micro-Raman-scanning electron microscopy (SEM)-energy-dispersive X-ray spectrometry (EDX) indicate that the produced particles are Pu dioxide. Our initial attempts to measure the density of two single particles gave results with a spread value accompanied by a large uncertainty.     

Expression and purification of recombinant human annexin A2 in Pichia pastoris and utility of expression product for detecting annexin A2 antibody

Annexin A2, a Ca2+-dependent phospholipid binding protein, is abundantly expressed in various human organs, which exists as either a membrane-associated, cytosolic or soluble form in serum. We constructed expression systems for recombinant human annexin A2 (rhA2) using Pichia pastoris. The systems are designed to secrete rhA2 as either the N- or C-terminally His6-tagged form to facilitate purification. Both types of rhA2 were overexpressed, but in the N-terminal-truncated form as revealed from the results of N-terminal amino acid sequencing and Western blotting. Therefore, further purification of N-terminally His6-tagged rhA2 was not feasible because of the removal of the N-terminal His6-tag sequence. C-terminally His6-tagged rhA2 was expressed as either a glycosylated or a nonglycosylated form, and the nonglycosylated form was purified using the combination of nickel-immobilized affinity, concanavalin A and cation exchanged column chromatographies. The solid-phase binding of rhA2 was examined by enzyme-linked immunosorbent assay (ELISA), which revealed the specific reactivity of rhA2 against an anti-annexin A2 monoclonal antibody. These results suggest that the expression system using P. pastoris is useful for the preparation of rhA2 that is applicable to the ELISA detection of the anti-annexin A2 antibody.