New micro-flow pumping system for liquid chromatography

This paper deals with the development of practical approaches to a new liquid-delivery system for capillary liquid chromatography. Under different chromatographic conditions, the factors affecting liquid-delivery performance are theoretically described, and the new liquid-delivery system without any splitter is evaluated with its flow-rate accuracy and precision using a variety of solvents. The experimental results demonstrate that the liquid-delivery system is capable of generating accurate, reproducible and conditions-independent micro- and nano-flows.     

Mannich-type reaction with trifluoromethylated N,O-hemiacetal: facile preparation of beta-amino-beta-trifluoromethyl carbonyl compounds

On treatment of silyl enolates and an N,O-hemiacetal, derived from trifluoroacetaldehyde ethyl hemiacetal and p-anisidine, with GaCl(3) (0.2 equiv) and C(6)H(5)COCl (0.2 equiv) in propionitrile, Mannich-type reaction took place smoothly to afford beta-amino-beta-trifluoromethyl carbonyl compounds in high yields.     

In-process monitoring and control of doping gas concentration during vapor phase silicon epitaxial growth by using a flame photometric detector

An in-process monitoring and control method of the doping gas concentration during epitaxial growth of Si was developed. A flame photometric detector (FPD) can be used as a monitor for the PH₃ and B₂H₆ dopant concentrations in the injected doping gases. A combination of this dopant monitor with an automatic control system of the silicon source (SiHCl₃) gas concentration using an infrared spectrophotometer as a monitor, makes possible an automatic in-process control of the concentrations of dopant and of silicon source gas supplied to the reactor. The present system provides an accurate and reproducible control of impurity concentrations in Si epitaxial layers. Good correlation between the monitored signal (or the doping gas concentration) and the impurity concentration incorporated into the growth layers was confirmed for PH₃ (n-type) and B₂H₆ (p-type) doping. For the B₂H₆ doping, a divergence from the linear relationship between the doping gas concentration and the impurity concentration in the layers was observed in the level of acceptor concentration below about 10¹⁵ atoms/cm³. The transient response of the present system was measured by growing epitaxial layers with increasing and decreasing step-changes in the dopant gas flow during continuous deposition of the layers. Some interesting, but complicated, transient responses of impurity concentration in the growth layer were observed. The responses are different between the PH₃ doping and the B₂H₆ doping, and also different between increasing and decreasing steps especially for the B₂H₆ doping.     

Controlled Polymerization of Protic Ionic Liquid Monomer by ARGET‐ATRP and TERP

The direct synthesis of structurally well‐defined protic polymeric ionic liquid (PIL) with controlled molecular weight and molecular weight distribution is examined using N,N‐diethyl‐N‐(2‐methacryloylethyl) ammonium bis(tri‐fluoromethylsulfonyl)imide (DEMH‐TFSI) as a monomer. Three polymerization methods, namely, atom transfer radical polymerization (ATRP), activators regenerated by electron transfer (ARGET)‐ATRP, and organotellurium‐mediated living radical polymerization (TERP) are employed in this study. While the polymerization by ATRP is slow and does not reach high monomer conversion that under ARGET‐ATRP and TERP proceeds smoothly and affords structurally well‐defined poly(DEMH‐TFSI)s. TERP is especially efficient for the control and poly(DEMH‐TFSI)s with low to high molecular weights ( = 49 100–392 500) and narrow molecular weight distributions (/ = 1.17–1.46) are obtained. These results represent the first example of synthesis of a structurally well‐defined protic, ammonium PIL by direct polymerization of the protic ionic liquid monomer. The polymerization of N,N‐diethyl‐N‐(2‐methacryloylethyl)‐N‐methylammonium bis(trifluoromethylsulfonyl)imide (DEMM‐TFSI), which possesses a quaternary ammonium salt, also proceeds in a highly controlled manner under TERP conditions. A diblock copolymer, polystyrene‐block‐poly(DEMH‐TFSI), is also successfully synthesized by TERP.

     

Cyclotron resonance and mass enhancement by electron correlation in KFe2As2

Cyclotron resonance (CR) measurements for the Fe-based superconductor KFe(2)As(2) are performed. One signal for CR is observed, and is attributed to the two-dimensional α Fermi surface at the Γ point. We found a large discrepancy in the effective masses of CR [(3.4±0.05)m(e) (m(e) is the free-electron mass)] and de Haas-van Alphen results, a direct evidence of mass enhancement due to electronic correlation. A comparison of the CR and de Haas-van Alphen results shows that both intra- and interband electronic correlations contribute to the mass enhancement in KFe(2)As(2).     

Cryogenic plasmas for controlled processing of nanoporous materials

Plasma processing at cryogenic temperatures tremendously suppresses the depth penetration of plasma radical species within nanoporous materials. We demonstrate that this confining effect is surprisingly unrelated to changes in the phase diffusivity of radical species gas, but is determined by the increase of the sticking coefficient and the radical recombination and reaction factors, favoring an early irreversible surface adsorption of the plasma radical species.