Flammability studies of 3-methyl pyridine/water system

In industrial processes, information on the safety property of chemicals is essentially crucial for safe handling during unit operations. Ensuring the safe use of combustible or flammable substances in processes is unlikely without detailed investigations of their flammability characteristics and related hazards. We studied 3-methyl pyridine (3-picoline), e.g., flammability limits (LFL/UFL), maximum explosion pressure (P _max), maximum explosion pressure rise (dP/dt)_max, minimum oxygen concentration (MOC), vapor deflagration index (K _g), and characterized the influence of inert steam (H₂O) on critical parameters for 3-picoline/water mixtures at 270°C, 1 atm, various oxygen concentrations, and vapor mixing ratios (100/0, 30/70, 10/90 and 5/95 vol.%) with a 20-L-Apparatus in simulated conditions, respectively. The results showed that the flammability characteristics of 3-picoline_(aq) all increased with the oxygen concentration. However, as the composition of inert steam increased, the flammability parameters and the degree of fire and explosion hazards were significantly reduced, instead. This study elucidated the flammability properties of 3-picoline mixed with inert steam. The conclusions could be applied to proactively prevent the relevant processes from incurring fire and explosion accidents.     

Optical measurement of the deformation of giant lipid vesicles driven by a micropipet electrode

We investigate the deformation of giant lipid vesicles driven by a micropipet electrode by use of differential confocal microscopy. This optical technique provides nanometer depth resolution without mechanical contact and hence prevents large tension or perforation of the soft membrane. For dipalmitoyl phosphatidylcholine (DPPC) membranes in the gel phase, we observed deformations of several hundreds of nanometers when the driving voltage was about 0.1 V. The voltage and frequency responses of the vesicle deformation can be explained by the balance between the electroosmotic force inside the micropipet and the membrane tension. We also used DPPC:cholesterol vesicles to check the validity of this model. In the fluid phase, however, the deformation is independent of the modulation signal because micrometer-scale thermal fluctuations dominate the membrane motion.     

Mammalian cell growth studiedin situ by fourier transform infrared spectroscopy

Fourier transform infrared techniques were used to monitor mammalian cell growth plated on attenuated total reflection (ATR) crystals. Consistently, the growth kinetics plots generated from the obtained spectra demonstrated a sigmoidal curve representing a sequence of slow, rapid, then tapering cell growth which correlated well with non-spectral cell growth determinations. Significant advantages over traditional methods of measuring cell growth kinetics are demonstrated. The technique has promising potential to be used to study events in areas such as toxicology and cell biology.     

Analysis of double-stranded DNA by microchip capillary electrophoresis using polymer solutions containing gold nanoparticles

The impact of gold nanoparticles (GNPs) on the microchip electrophoretic separation of double-stranded (ds) DNA using poly(ethylene oxide) (PEO) is described. Coating of the 75-microm separation channel on a poly(methyl methacrylate) (PMMA) plate in sequence with poly(vinyl pyrrolidone), PEO, and 13-nm GNPs is effective to improve reproducibility and resolution. In this study, we have also found that adding 13-nm GNPs to 1.5% PEO is extremely important to achieve high resolution and reproducibility for DNA separation. In terms of the stability of the GNPs, 100 mM glycine-citrate buffer at pH 9.2 is a good buffer system for preparing 1.5% PEO. The separation of DNA markers V and VI ranging in size from 8 to 2176 base pairs has been demonstrated using the three-layer-coated PMMA microdevice filled with 1.5% PEO containing the GNPs. Using these conditions, the analysis of the polymerase chain reaction products of UGT1A7 was complete in 7 min, with the relative standard deviation values of the peak heights and migration times less than 2.3% and 2.0%, respectively. In conjunction with stepwise changes of the concentrations of ethidium bromide (0.5 and 5 microg/ml), this method allows improved resolution and sensitivity for DNA markers V and VI.     

Double-Label Simultaneous Time-Resolved Fluoroimmunoassay of Phenytoin and Phenobarbital

A procedure for the simultaneous time-resolved fluoroimmunoassay for phenobarbital and phenytoin, based on the use of europium- and samarium-labeled haptens, has been investigated. These lanthanide ions are bound to the haptens by means of the anhydride of diethylenetriaminepentaacetic acid. The antibody is immobilized onto immunoplate in which samples are assayed in competitive immunoassay. After the immunoreactions and dissociation with a fluorescence enhancement solution, the fluorescence intensity is measured. The detection limits of the assay are, respectively, 20 ng/ml for phenobarbital and 50 ng/ml for phenytoin. Results obtained with the proposed methods correlate well (CV <10%). The inter-reactions between phenobarbital, phenytoin, and their antibodies are studied.     

Fragmentation processes of methylbutyl trifluoroacetates studied by tandem quadrupole mass spectrometry and isotope labeling

The fragmentation patterns of 3-methyl-2-butyl trifluoroacetate and 2-methyl-2-butyl trifluoroacetate were investigated by GC/MS/MS, with electron impact and collision-induced dissociation, on regular and isotope-labeled (deuterium and ¹⁸O) esters. The atoms found in various fragments could be traced back to specific positions in the parent molecules. In this way, molecular rearrangements potentially occurring during the formation of esters by trifluoroacetolysis of 3-methyl-2-butyl p-toluenesulfonate or trifluoroacetic acid addition to various 2-methylbutenes could be shown. Rearrangements also occurred during the fragmentation, particularly during the expulsion of the small fragments CO, C₂H₄ and F₂CO. For the decompositions of oxygen-containing ions these rearrangements were highly specific. By contrast, alkyl cations lead to fragments that are fully scrambled (statistical label distribution). Alkene radical cations ([C_nH_2n]^{+ ˙}) fragment to daughter ions that are extensively, but less than statistically scrambled. Hydrogen scrambling may also occur in fluoroalkyl cation fragments.     

Dissociation Constants and Chelate Stability Constants of Some Dihalogenated 8-Hydroxyquinaldines

The acid dissociation constants of dihalogenated 8-hydroxyquinaldines and the stability constants of their chelates with Zn[II], Ni[II], Co[II], Pb[II], Cd[II], Mn[II], and Mg[II] have been determined. The Calvin-Bjerrum potentiometric titration technique was used in studying the behavior of these substances. The order of decreasing stability of the metal chelates Zn, Nc>Co>Pb>Cd>Mn>Mg is similar to the stability sequence generally obtained for divalent metals, and the order of decreasing stability of dihalogenated 8-hydroxyquinaldines to form the metal chelates with metal ions is I>Br>Cl. Spot test reactions of dihalogenated 8-hydroxyquinaldines and 8-hydroxyquinolines with the metal ions also have been investigated.     

A Novel Dimeric Coumarin from Clausena lenis

A novel dimeric coumarin (1), a dimeric of seselin named diseselin A, was isolated from the aerial part of Clausena lenis. The structure was elucidated based on the MS, 1D and 2D NMR data.     

金属酞菁化合物在TiO2表面的分散研究

Dispersion of copper(Ⅱ) phthalocyanine (CuPc), copper(Ⅱ) phthalocyaninesulfonate (CuPcS) and cobalt(Ⅱ)phthalocyaninetetrasulfonate (CoPcTS) on the surface of titanium dioxide was investigated by XRD, XPS, FT-IR and UV-Vis techniques. Results show that interaction between CuPc and TiO2 was very weak and CuPc was difficult to disperse on the surface of the support. While partly sulfurized CuPcS could be dispersed on the surface of support through sulfo-groups and its dispersion capacity was determined to be 0.085 g CuPcS/g TiO2. Completely sulfurlzed CoPcTS could also be dispersed on the surface of TiO2 as a monolayer and its dispersion capacity was 0.12 g CoPcTS/g TiO2. Interactions of the sulfo-groups as well as the electrons of CoPcTS with the surface of TiO2 could be evidenced by FT-IR characterization. Therefore, it was suggested that CoPcTS molecules be adsorbed on the surface of TiO2 in a flat-lying mode while CuPcS in a slanting one. UV-Vis spectra show that the dispersed CuPcS and CoPcTS molecules exist in both forms of monomers and dimers.     

Selective Determination of Trace Mercury (II) after Preconcentration with 4-(2-Pyridylazo)-Resorcinol-Modified Nanometer-Sized SiO2 Particles from Sample Solutions

A rapid, selective method that utilize 4-(2-Pyridylazo)-resorcinol (PAR)-modified nanometer SiO₂ (nanometer SiO₂–PAR) as a new solid-phase extractant for preconcentration of trace mercury (II) has been developed. The adsorption property of nanometer SiO₂–PAR for metal ions was studied by selectively extracting different metal ions from aqueous solutions. The results revealed an excellent affinity of the nanometer SiO₂–PAR for mercury (II) in presence of interfering metal ions at pH 4. The main parameters of solid-phase extraction such as shaking time, elution and sample dilution effect were studied. The extractant shows rapid kinetic sorption, and the adsorption equilibrium of mercury (II) on nanometer SiO₂–PAR was achieved in less than 2 min. The adsorbed mercury (II) was easily eluted by 4 mL of 6 mol L⁻¹ HCl. The maximum preconcentration factor was 50. The maximum static adsorption capacity was 276 μmol g⁻¹ at pH 4. The detection limit (3σ) was 0.43 μg L⁻¹ for cold vapor atomic absorption spectrometry (CVAAS), and the relative standard deviation of the eight replicate determinations was 2.4% for the determination of 2.0 μg of Hg(II) in 100 mL water sample. The method was applied to the determination of trace mercury (II) in sample solutions with satisfactory results.