Synthesis and Properties of Thermosensitive Poly(N-Isopropylacrylamide)/Waterborne Polyurethane Graded Concentration Hybrid Films

Temperature-sensitive hybrid films were synthesized with a concentration gradient by casting and UV curing of N-isopropylacrylamide (NIPAAm) monomers (0%–70%) on the free surface of waterborne polyurethane (WPU) films on a Teflon substrate. The surface hardness and contact angle of the free surface with a water drop increased asymptotically with the addition of NIPAAm, whereas those on the substrate side were virtually unchanged. The diffusion coefficient (D), rates of swelling at 20°C (below the lower critical solution temperature (LCST) of poly(N-isopropylacrylamide) (PNIPAM)) and deswelling at 50°C (above the LCST) increased with increasing NIPAM content, showing favorable thermosensitivity. In addition, the glassy state modulus and glass transition temperature (Tg) of the film increased with increasing NIPAM content, whereas the rubbery modulus decreased due to the increased molecular weight between the crosslinks. In addition, as the NIPAM content increased, the film showed a positive yield with an increased yield and fracture stress and decreased ductility. Above 50% NIPAM, the film became brittle, showing a linear stress–strain relationship.     

Simultaneous determination of 75 abuse drugs including amphetamines,benzodiazepines, cocaine,opioids, piperazines,zolpidem and metabolites in human hair samples using liquid chromatography–tandem mass spectrometry

A liquid chromatography–tandem mass spectrometric method for the simultaneous determination of 75 abuse drugs and metabolites, including 19 benzodiazepines, 19 amphetamines, two opiates, eight opioids, cocaine, lysergic acid diethylamide, zolpidem, three piperazines and 21 metabolites in human hair samples, was developed and validated. Ten‐milligram hair samples were decontaminated, pulverized using a ball mill, extracted with 1 mL of methanol spiked with 28 deuterated internal standards in an ultrasonic bath for 60 min at 50°C, and purified with Q‐sep dispersive solid‐phase extraction tubes. The purified extracts were evaporated to dryness and the residue was dissolved in 0.1 mL of 10% methanol. The 75 analytes were analyzed on an Acquity HSS T3 column using gradient elution of methanol and 0.1% formic acid and quantified in multiple reaction monitoring mode with positive electrospray ionization. Calibration curves were linear (r ≥ 0.9951) from the lower limit of quantitation (2–200 pg/mg depending on the drug) to 2000 pg/mg. The coefficients of variation and accuracy for intra‐ and inter‐assay analysis at three QC levels were 4.3–12.9% and 89.2–109.1%, respectively. The overall mean recovery ranged from 87.1 to 105.3%. This method was successfully applied to the analysis of 11 forensic hair samples obtained from drug abusers.     

Pericyclic reactions in the synthesis of new 5-aryl-5,6-dihydroquinolino[2,1-b]quinazolin-12-ones

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MAO‐free and extremely active catalytic system for ethylene tetramerization

The original Sasol catalytic system for ethylene tetramerization is composed of a Cr source, a PNP ligand, and MAO (methylaluminoxane). The use of expensive MAO in excess has been a critical concern in commercial operation. Many efforts have been made to replace MAO with non‐coordinating anions (e.g., [B(C₆F₅)₄]^?); however, most of such attempts were unsuccessful. Herein, an extremely active catalytic system that avoids the use of MAO is presented. The successive addition of two equivalent [H(OEt₂)₂]⁺[B(C₆F₅)₄]^? and one equivalent CrCl₃(THF)₃ to (acac)AlEt₂ and subsequent treatment with a PNP ligand [CH₃(CH₂)₁₆]₂C(H)N(PPh₂)₂ ( 1 ) yielded a complex presumably formulated as [ 1 ‐CrAl (acac)Cl₃(THF)]²⁺[B(C₆F₅)₄]^?₂, which exhibited high activity when combined with iBu₃Al (1120 kg/g‐Cr/h; ~4 times that of the original Sasol system composed of Cr (acac)₃, iPrN(PPh₂)₂, and MAO). Via the introduction of bulky trialkylsilyl substituents such as –SiMe₃, –Si(nBu)₃, or –SiMe₂(CH₂)₇CH₃ at the para‐position of phenyl groups in 1 (i.e., by using [CH₃(CH₂)₁₆]₂C(H)N[P(C₆H₄‐p‐SiR₃)₂]₂ instead of 1 ), the activities were dramatically improved, i.e., tripled (2960–3340 kg/g‐Cr/h; more than 10 times that of the original Sasol system). The generation of significantly less PE (<0.2 wt%) even at a high temperature is another advantage achieved by the introduction of bulky trialkylsilyl substituents. NMR studies and DFT calculations suggest that increase of the steric bulkiness on the alkyl‐N and P‐aryl moieties restrict the free rotation around (alkyl)N–P (aryl) bonds, which may cause the generation of more robust active species in higher proportion, leading to extremely high activity along with the generation of a smaller amount of PE.     

Effect of irradiation for sterilization on beverage reference materials for the analysis of food additives

Accreditation and Quality Assurance - Reference materials for proficiency testing (PT) were prepared for 6&nbsp;years. The target analytes were food additives, sorbic acid, benzoic acid, and...     

LGP pattern design with single LED light source

We investigated optimize pattern design of a LGP for TFT-LCD with single LED. For the purpose, we introduced new concepts of pattern design most appropriate design for single light source, density adjustment design and radius adjustment design. And than compared the LGP output intensity distribution of the two cases with that of the uniform density pattern. As the result, above two types pattern design given a good result. Especially, the radius adjustment pattern design enhanced intensity uniformity definitely.