Studies of tetrazoles as rubber chemicals. II. Reactivities and antioxidation activities of reactive antioxidants based on tetrazoles

The chemical reactivities of novel reactive antioxidants based on tetrazoles for carbon–carbon double bonds of liquid polybutadiene and their antioxidation activities toward isoprene rubber were evaluated. These antioxidants, i.e., 2-substituted phenyl-5-(3′,5′ -di-tert-butyl-4′-hydroxyphenyl)tetrazoles (PHPT), were pyrolyzed in liquid polybutadiene at 160–170°C for 30 min to attach to rubber in extents of 61–85% of the nitrileimines formed from PHPT by 1,3-dipolar addition reaction. The reactivities of PHPT followed the order p-Cl > m-Cl > H > p-CH₃ > m-CH₃, p-OC₂H₅, suggesting that PHPT reacts with diene rubber in electrophilic reaction and p-derivatives exhibit higher contents of binding than m-derivatives due to steric hindrance. From oxygen absorption data, the antioxidation activities of PHPT for isoprene rubber vulcanizates followed the order m-Cl, m-CH₃ > H, p-Cl, p-Cl, p-CH₃ > p-OC₂H₅. Isoprene rubber vulcanizates, obtained after pretreatment with PHPT by heating, were extracted with acetone, followed by aging to show that there was good retention and appreciable antioxidation activities of PHPT, especially, p-CH₃ and p-Cl substituted PHPT.     

Effects of soaking soybeans in dilute acids on biologically active components

Soaking soybeans in dilute acids affected activities of lipoxygenase, trypsin inhibitor and urease. Effects of soaking time, acid concentration and soaking temperature were investigated. Lipoxygenase activity was completely eliminated by soaking in 0.3 M HC1 at either 23°C or 40°C for 8 hr. Less than 50% trypsin inhibitor remained and urease was inactivated to an acceptable level (0.04 ΔpH).     

Ultra-high pressure sterilization of powdery food stuff—a new application of a roller compactor

A new non-heating technique was developed for the sterilization of food stuff. Applying a roller compactor, ultra-high pressure sterilization has experimentally demonstrated its ability to sterilize dry powders, such as corn flour and Chinese herbs, with little quality deterioration. Also, the degree of food sterilization was found correlated well with the linear press forces between the rollers, roller gaps, and number of compaction passes. In comparison to the conventional high pressure sterilization technique, the new dry continuous processing method has the advantage of lower investment cost and is more versatile for sterilizing various food powders.     

k-NN classification of handwritten characters via accelerated GAT correlation

This paper addresses the problem of reinforcing the ability of the k-NN classification of handwritten characters via distortion-tolerant template matching techniques with a limited quantity of data. We compare three kinds of matching techniques: the conventional simple correlation, the tangent distance, and the global affine transformation (GAT) correlation. Although the k-NN classification method is straightforward and powerful, it consumes a lot of time. Therefore, to reduce the computational cost of matching in k-NN classification, we propose accelerating the GAT correlation method by reformulating its computational model and adopting efficient lookup tables. Recognition experiments performed on the IPTP CDROM1B handwritten numerical database show that the matching techniques of the simple correlation, the tangent distance, and the accelerated GAT correlation achieved recognition rates of 97.07%, 97.50%, and 98.70%, respectively. The computation time ratios of the tangent distance and the accelerated GAT correlation to the simple correlation are 26.3 and 36.5 to 1.0, respectively.     

Dynamic Mechanical Properties and Adhesive Joint Strengths of Emulsion Polymers Produced by Power Feed Technique. III. Adhesive Joint Strengths of Grafted Power Feed Copolymer

Power feed copolymers were synthesized using styrene and n-butyl acrylate through non-uniform feeding emulsion polymerization. Poly(vinyl alcohol) (PVA) was used as a protective colloid, onto which vinyl monomers were grafted. Power feed copolymer had a very broad glass transition temperature compared with random copolymer, even if grafting and/or crosslinking were introduced to the system. This tendency was almost the same as the non-grafted power feed copolymer where only low molecular weight surfactant was used.

Adhesive joint strengths of power feed copolymers were evaluated compared with random copolymers. In the case of usual linear power feed copolymer, the adhesive joint strengths were not higher than those of random copolymer, which was considered to be due to the lower film strengths of the power feed copolymer. Power feed copolymer having grafting showed slightly higher adhesive joint strengths over a wide range of temperatures than random copolymer. When crosslinking was introduced to the system, power feed copolymer showed much higher adhesive joint strengths over a wide temperature range.     

Structural analysis of cellulose triacetate polymorphs by two-dimensional solid-state C-C and H-C correlation NMR spectroscopies

For the elucidation of the crystal structures of the two crystalline allomorphs of cellulose triacetate (CTA), namely CTA I and CTA II, two-dimensional (2D) solid-state through-bond ¹³C-¹³C and ¹H-¹³C correlations NMR techniques applied to the two crystalline allomorphs of CTA. As a result, the ¹³C and ¹H chemical shifts of the glucopyranose ring of CTA I and CTA II were completely assigned by the 2D NMR spectra of these allomorphs. On the 2D ¹³C-¹³C correlation spectrum of CTA II, two sets of the ¹³C-¹³C correlations from C1 to C6 were observed. This indicated that the CP/MAS ¹³C NMR spectrum of CTA II can be characterized by its overlapping of the ¹³C subspectra of two kinds of 2,3,6-triacetyl-anhydroglucopyranose units and that there are two magnetically non-equivalent sites in the unit cell of CTA II. In the case of CTA I, the numbers of respective ¹³C and ¹H shifts of CTA I agreed with the those of the glucopyranose residue in the allomorph, strongly suggesting that the asymmetric unit of CTA I is only one glucose residue. In addition, conformational differences in the exocyclic C5-C6 bonds between CTA I and CTA II were strongly suggested by the notable differences in the ¹H and ¹³C chemical shifts at the C6 sites of these allomorphs.     

Skeletonized hybrid liposomes

Summary Giant hybrid liposomes of polymerizable lipid and cholesterol were prepared by the hydration method and were polymerized by UV irradiation. The obtained giant liposomes were freeze-dried and washed with chloroform to skeletonize the frame structure of the polymerized membrane. The skeletonized liposomes were directly confirmed by scanning electron microscopy. The single-layered and fully spherical liposome frame were easily confirmed by the stereo-pair of the obtained micrographs.     

Assessing the capability of code smells to explain maintenance problems: an empirical study combining quantitative and qualitative data

Code smells are indicators of deeper design problems that may cause difficulties in the evolution of a software system. This paper investigates the capability of twelve code smells to reflect actual maintenance problems. Four medium-sized systems with equivalent functionality but dissimilar design were examined for code smells. Three change requests were implemented on the systems by six software developers, each of them working for up to four weeks. During that period, we recorded problems faced by developers and the associated Java files on a daily basis. We developed a binary logistic regression model, with “problematic file” as the dependent variable. Twelve code smells, file size, and churn constituted the independent variables. We found that violation of the Interface Segregation Principle (a.k.a. ISP violation) displayed the strongest connection with maintenance problems. Analysis of the nature of the problems, as reported by the developers in daily interviews and think-aloud sessions, strengthened our view about the relevance of this code smell. We observed, for example, that severe instances of problems relating to change propagation were associated with ISP violation. Based on our results, we recommend that code with ISP violation should be considered potentially problematic and be prioritized for refactoring.     

Reaction Pathways in the Synthesis of Photorefractive gamma-Bi12MO20 (M = Si, Ge, or Ti)

Reaction pathways in the synthesis of three photorefractive silicates—γ-Bi₁₂ SiO₂₀ (BSO), γ-Bi₁₂ GeO₂₀ (BGO), and gamma-Bi₁₂ TiO₂₀ (BTO)—were systematically investigated. The main results were as follows: (i) all the reactions of the form 6Bi₂O₃+ MO₂→> γ-Bi₁₂ MO₂₀ (SR1 for M = Si, SR2 for M = Ge, SR3 for M = Ti) in the solid state seemed to be diffusion-controlled processes and were affected by both temperature and time, where the reaction temperature increases in the order SR1 < SR2 < SR3; (ii) the metastable phases Bi₂ SiO₅ (tetragonal) in reaction SR1, Bi₂ GeO₅ (orthorhombic) in reaction SR2, Bi₄ Ti₃ O₁₂ (orthorhombic) in reaction SR3 may be formed and seemed to greatly accelerate the above-mentioned solid-state reaction processes; and (iii) for a continuous heating process, pure γ-Bi₁₂ SiO₂₀ and γ-Bi₁₂ GeO₂₀ could be produced before melting, whereas pure γ-Bi₁₂ TiO₂0 could not be produced, even if all the mixed phases had melted.     

Fatigue behavior of medium-density polyethylene pipes

A round bar specimen and a square bar specimen cut out from medium-density polyethylene pipes with a notch were made and a fatigue test was conducted to cause a brittle fracture. The initiation and growth of a craze and crack at the tip of a notch was observed. In the range where loading cycles are few and displacement of the specimen does not increase, the craze prior to crack initiation occurs. Also, the effect of frequency was investigated. The pure creep failure and the fatigue failure at low frequency were compared. The lower the frequency, the smaller the reciprocal of the actual loading time T_f becomes. It is also found that this tensile fatigue test is a useful test method to assure the quality of pipes.