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ABSTRACT Copolymers of 1,5-dioxepan-2-one (DXO) and e-caprolactone (?-CL), δ-valerolactone (δ-VL) or L-lactide (LLA) have been synthesized and characterized. High molecular weight copolymers were obtained using stannous-2-ethyl hexanoate as catalyst in bulk. Reactivity ratios for the copolymerization of DXO and δ-VL were determined at 110°C as rVL=0.5 and rDXO=2.3. At high conversion, depolymerization of δ-VL occurred, resulting in lower molecular weight and variations in the copolymer composition. Physical properties, such as crystallinity and melting temperature of the DXO-copolymers proved to be strongly dependent on the choice of comonomer and on the molar composition of the copolymers. DXO appears to be incorporated into the poly-?-caprolactone (PCL) crystals and to some extent into the poly-δ-valerolactone (PVL) crystals, resulting in a more gradual decrease in crystallinity with increasing amount of DXO. 相似文献
2.
Stanelle RD Mignanelli M Brown P Marcus RK 《Analytical and bioanalytical chemistry》2006,384(1):250-258
Microbore columns utilizing polypropylene capillary-channeled polymer (C-CP) fibers as the stationary phase in high-performance
liquid chromatography (HPLC) have been investigated. The polypropylene C-CP fiber diameter is ∼50 μm, with eight channels
along the periphery of the fiber ranging in diameter from ∼12 to 35 μm. The polypropylene C-CP fibers were packed into fluorinated
ethylene propylene (FEP) tubing, 1.3 mm inner diameter, with lengths of 500, 750, and 1,000 mm, to examine the effects of
increased column length with regards to plate height, resolution and analysis time. The low backpressures characteristic of
the C-CP fiber stationary phases allow the length of the column to be increased without significantly decreasing the specific
permeability. The high specific permeability (∼5×10−8 cm2) of the C-CP packed microbore columns yields a relatively low backpressure of 2.35 MPa at the highest flow rate of 17 μL/s
(54 mm/s) for a 1,000 mm column. Radial compression of the soft-walled FEP tubing is accomplished by pulling the 1.7 mm o.d.
column through a 1.4 mm diameter orifice. Reducing the inner diameter of the column from 1.3 to 1.0 mm lowered the interstitial
fraction from 47% to 42%, decreased the A-term contributions to band broadening, resulted in a significant decrease in average
plate height (∼30%), and increased resolution (∼36%) at identical linear velocities. Although the lower void volume of the
radially compressed column increased the backpressure from 0.57 to 2.11 MPa at a linear velocity of ∼20 mm/s, the specific
permeability only decreased from ∼7×10−8 to 4×10−8 cm2.
相似文献
3.
RD Harris WS Baker Van Stipdonk MJ RM Crooks EA Schweikert 《Rapid communications in mass spectrometry : RCM》1999,13(14):1374-1380
A suite of keV polyatomic or 'cluster' projectiles was used to bombard unoxidized and oxidized self-assembled monolayer surfaces. Negative secondary ion yields, collected at the limit of single ion impacts, were measured and compared for both molecular and fragment ions. In contrast to targets that are orders of magnitude thicker than the penetration range of the primary ions, secondary ion yields from polyatomic projectile impacts on self-assembled monolayers show little to no enhancement when compared with monatomic projectiles at the same velocity. This unusual trend is most likely due to the structural arrangement and bonding characteristics of the monolayer molecules with the Au(111). Copyright 1999 John Wiley & Sons, Ltd. 相似文献
4.
A Mukherjee M Dasgupta DJ Hinde CR Morton AC Berriman RD Butt JO Newton H Timmers 《Pramana》2001,57(1):195-198
Fusion cross-sections for the 7Li + 12C reaction have been measured at energies above the Coulomb barrier by the direct detection of evaporation residues. The heavy
evaporation residues with energies below 3 MeV could not be separated out from the α-particles in the spectrum and hence their
contribution was estimated using statistical model calculations. The present work indicates that suppression of fusion cross-sections
due to the breakup of 7Li may not be significant for 7Li + 12C reaction at energies around the barrier. 相似文献
5.
LANGLEY J. K. 《中国科学 数学(英文版)》2010,(3)
We determine all real meromorphic functions f in the plane such that f has finitely many zeros, the poles of f have bounded multiplicities, and f and F have finitely many non-real zeros, where F is a linear differential polynomial given by F = f (k) +Σk-1j=0ajf(j) , in which k≥2 and the coefficients aj are real numbers with a0≠0. 相似文献
6.
Nylon-6 capillary-channeled polymer (C-CP) fibers are used as the stationary phase for the hydrophobic interaction chromatography
(HIC) separation of a synthetic protein mixture composed of ribonuclease A, lysozyme, and holotransferrin. Nylon is a useful
polymer phase for HIC as it has an alkyl backbone, while the amide functionality is hydrophilic (in fact ionic) in nature.
The combination of a nonporous polymer surface of the fiber phases and high column permeability yields very efficient mass
transfer characteristics, as exhibited by narrowing of peak widths with increases in mobile phase linear velocity. Retention
factors and resolution were evaluated at flow rates ranging from 0.5 to 9 mL/min (linear velocities of ca. 2 to 15 mm/s) and
at gradient slopes between 3.3 and 20 %B/min. Optimum resolution was achieved by employing fast flow rates (9 mL/min) and
slow gradients (3 %B/min), also resulting in the highest peak capacities. 相似文献
7.
Capillary-channeled polymer (C-CP) fibers extruded from nylon-6 are used as the stationary phase for the ion-exchange/reversed-phase mixed-mode chromatographic separation of a three protein mixture. The nylon-6 C-CP fibers are packed collinearly in a 250 x 1.5-mm i.d. column with an interstitial fraction of approximately 0.6. The effects of four displacing salts at three different pHs are studied with regards to protein retention time, peak width, selectivity, and resolution for a synthetic mixture consisting of myoglobin, ribonuclease A, and lysozyme to determine the optimum mobile phase conditions. The net charge model is found to be inadequate in fully explaining the retention behavior, as the proteins are retained by anion and cation-exchange interactions, as well as hydrophobic interactions with the stationary phase. It is found that pH and displacing salt strength had a significant influence on the retention properties and resolution of the proteins. 相似文献
8.
Mawhinney DB Stanelle RD Hamelin EI Kobelski RJ 《Journal of the American Society for Mass Spectrometry》2007,18(10):1821-1826
A method to enhance the signal intensity and signal-to-noise of several alkyl methylphosphonic acids in negative electrospray ionization liquid chromatography tandem mass spectrometry (ESI LC-MS/MS) is presented. This class of compound represents the initial metabolites and environmental degradants of the nerve agents: VX, rVX (Russian VX), GB (Sarin), GF (Cyclosarin), and GD (Soman). Compared with the post-column addition of the mobile phase, the post-column addition of aprotic solvents and longer chain alcohols enhance the signal intensity and signal-to-noise ratio (S/N) of the chromatographic peaks by factors of up to 60 and 19, respectively. The post-column addition of water, methanol, and ethanol resulted in little or no relative signal enhancement. It is proposed that the post-column addition of these solvents do not result in the same enhancements due to stabilization of analyte solvation through hydrogen bonding. 相似文献
9.
Titanium dioxide was deposited from aqueous suspension onto cellulosic surfaces.Titania was sourced from Degussa (P25TM,70:30 anatase:rutile).Dry uptake of particles was shown to be rapid and dominant with one-third of the deposition occurring in less than 30 s and over one-half in the first minute.Isotherms were recorded to compare the rate of titanium deposition on dry and pre-wetted cotton.In the dry case uptake reached a maximum in 30 min whereas in the pre-wetted case the uptake was seen to continue beyond 180 min.A broad trend of higher deposition occurring at lower pH was seen,corresponding to the region where surface charges were opposite and thus attractive.Dry pickup was less significant at high pH.The response to varying ionic strength was complex and was attributed to the combined effect of charge screening,particle aggregation and consequent particle entrapment or occlusion.Titania deposition into the interstices of woven cotton sheets resulted in the formation of inorganic,nanoparticulate skeletons which could be isolated by controlled combustion of the cellulose and thus cotton was suggested to have potential for the templated synthesis of high surface area semiconductor materials. 相似文献
10.
There are many reports1 of the pyrolysis of fluorinated organic compounds, including the defluorination of cyclic fluorocarbons over iron to give aromatic compounds. Extending this technique we have investigated the flow pyrolysis of some readily accessible unsaturated fluorocarbons, such as I, II, and III, and found these to be synthetically useful routes to fluorinated dienes, cyclobutenes, and furans. Pyrolyses were carried out using a nitrogen flow over platinum, iron or caesium fluoride heated at 430–700°. The various products can all be rationalized in terms of intermediate allylic radicals, and the solid substrate influences which allylic radicals are formed.We are also investigating the chemistry of those now accessible compounds, such as IV, V, and VI, and some of the preliminary results are described. For example the fluoride ion induced dimerisation of IV gave two major products VII and VIII via a particular interesting mechanism. 相似文献
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