Distal surface of the rat ruffle-ended ameloblasts at the stage of enamel maturation observed by scanning electron microscopy

Distal surface of the rat ruffle-ended ameloblasts was observed by high resolution scanning electron microscopy. Specimens fixed by perfusion with 0.5% formaldehyde and 0.5% glutaraldehyde were decalcified with ethylenediamine tetraacetic acid and freeze-fractured using dimethyl sulfoxide. They were treated with 0.1% osmium tetroxide for 96 hr to remove excess cytoplasmic matrices, dehydrated, and critical-point dried. The present method was useful for observing both surface and intracellular structures simultaneously. The dense lamina lining the distal surface of the ruffle-ended ameloblasts having been dissolved in this preparation, the surface was clearly demonstrated in three dimensions under SEM. The surface was characterized by a complex labyrinth formed by protrusion and invagination of the plasma membrane. At high magnification, two kinds of minute granules are visible: small and larger granules measured as 10-20 nm and 70 nm in diameter, respectively. The former were more numerous than the latter. Furthermore, microfibrils connecting the protrusions of the plasma membrane were observed on the distal surface. The small granules probably connect the dense lamina with the distal surface of the ameloblasts. In addition, a denuded area free from the granules was sometimes recognized on the distal surface. These surface structures of the distal end of the ameloblasts appeared to be concerned with the enamel maturation.     

An improved method of phosphorus analysis in sea water

A reagent for the determination of phosphorus in sea water which contains Mo(VI) plus Mo(V) may be easily prepared by the reduction of Mo(VI) with metallic zinc in acid medium. This reagent is stable in the air for several months, and the development of the molybdenum blue colour is complete in 20 min at about 100°C; the colour is stable for at least a few months. The salt error is approximately 5 per cent with sea water of chlorinity 19 per milli. The interference due to either arsenate or silicate at their concentrations in sea water is negligible.     

Hydrogel of biodegradable cellulose derivatives. I. Radiation‐induced crosslinking of CMC

Radiation crosslinking of carboxymethylcellulose (CMC) with a degree of substitution (DS) from 0.7 to 2.2 was the subject of the current investigation. CMC was irradiated in solid‐state and aqueous solutions at various irradiation doses. The DS and the concentration of the aqueous solution had a remarkable affect on the crosslinking of CMC. Irradiation of CMC, even with a high DS, 2.2 in solid state, and a low DS, 0.7 in 10% aqueous solution, resulted in degradation. However, it was found that irradiation of CMC with a relatively high DS, 1.32, led to crosslinking in a 5% aqueous solution, and 20% CMC gave the highest gel fraction. CMC with a DS of 2.2 induced higher crosslinking than that with a DS of 1.32 at lower doses with the same concentration. Hence, it was apparent that a high DS and a high concentration in an aqueous solution were favorable for high crosslinking of CMC. It is assumed that high radiation crosslinking of CMC was induced by the increased mobility of its molecules in water and by the formation of CMC radicals from the abstraction of H atoms from macromolecules in the intermediate products of water radiolysis. A preliminary biodegradation study confirmed that crosslinked CMC hydrogel can be digested by a cellulase enzyme. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 78: 278–283, 2000     

Synthesis of N-cyclohexylmaleimide for heat-resistant transparent methacrylic resin

N-Cyclohexylmaleimide (CHMI) was synthesized in high yield by dehydration and ring closure of N-cyclohexylmaleamic acid (CHMA) in an organic nonpolar solvent that is immiscible with water in the presence of a catalyst consisting of a mixture of acid and its amine salt. The optimal molar ratio of the acid to the amine is in the range of 1/0.65–1/0.8. N-Cyclohexylaminosuccinic anhydride (CASA), which is a major by-product, was found to induce coloration of the methyl methacrylate/CHMI copolymer. The CASA content could be decreased by distillation under reduced pressure. CHMI contaminated with less than 0.9 wt % of CASA can be used for heat-resistant poly(methyl methacrylate) resin (MMA/CHMI copolymer) free from coloration, as well as for methyl methacrylate homopolymer. © 1997 John Wiley & Sons, Inc.     

High-quality N-substituted maleimide for heat-resistant methacrylic resin

A preparation procedure for colorless, transparent N-substituted maleimide of high quality which can provide heat-resistant transparent methacryl resins was developed. N-Alkylmaleimide, the alkyl substituent of which was composed of 2 to 4 carbons, is employed, giving a polymer with enhanced heat distortion temperature (HDT) because of the higher T_g. The advantages of relatively low melting points and high vapor pressure of N-alkylmaleimide can be used for the preparation of a high-quality product with purification of the monomer by distillation. N-Isopropylmaleimide (IPMI), which fulfills these requirements, is especially useful as a monomer for transparent resins. IPMI was synthesized in a high-yield using a mixture of orthophosphoric acid and orthophosphoric acid-isopropylamine salt as catalyst. IPMI, the purity of which is 99.9 wt % or above, contains 100–200 ppm of N-isopropylmaleamic acid, maleic anhydride, dimethylmaleic anhydride, solvent, and water. IPMI, which solidifies at 25.8°C, is obtained as a colorless liquid and is freely soluble in common monomers such as methyl methacrylate (MMA), styrene (St), and acrylonitrile (AN). The obtained IPMI showed excellent thermal stability, and no quality change was observed after heating for 100 h at 50°C. The copolymer of MMA and IPMI exhibited the same YI value as a measure of coloration, and almost the same transparency as the homopolymer of MMA. An increase in IPMI content in the copolymer by 1 mol % increased the polymer T_g by 0.8°C. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 63: 1055–1062, 1997     

Preparation of silica/poloxamer composite by sol-gel process and pore control of silica gel obtained from the composite

Silica gels that controlled the pore size were prepared by calcination of silica/organic polymer (50/50 wt %) composites prepared by the sol-gel process. Poly(ethylene oxide) (PEO)-poly(propyrene oxide) (PPO)-PEO triblock copolymers, which are called poloxamers, were used as an organic polymer. The pore control of the silica gels was carried out by changing the molecular weight of PEO or PPO in the poloxamers. The silica gels obtained by the above procedure had a dual pore size of around 4 nm and below 2 nm in diameter, and the specific surface area was 500–1000 m²/g. The poloxamer molecules were supposed to be dispersed monomolecularly in the composites. Therefore, the pore structure of the silica gels reflected the structure of the poloxamer and, particularly, the radius of gyration of PPO in the composites. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 64: 763–768, 1997     

Extraction of lanthanide ions from aqueous solution by bis(2-ethylhexyl)phosphoric acid with room-temperature ionic liquids

Extractions of five kinds of lanthanide metal ions by bis(2-ethylhexyl)phosphoric acid (DEHPA) with [1-Cn-3-methylimidazolium][PF₆](Cn = C₂, C₄) or [1-butyl-4-methylpyridinium][PF₆] were carried out under various DEHPA and HNO₃ concentrations from 0 to 1 M and under different temperature conditions from 298 to 333 K. These results were compared with those using the conventional organic solvent, hexane, in terms of their distribution coefficient values. Under all of the conditions in this study, the ionic liquid system shows more than three times greater extractability for lanthanide compared to when hexane was used. The distribution coefficient of lanthanide ions decreased as the length of the alkyl chain increased from the ethyl to the butyl. In addition, the imidazolium cation generally shows a higher distribution coefficient compared to the pyridinium cation in an ionic liquid. The concentration ratio of lanthanides and DEHPA resulted in an extraction affinity transition for lanthanides. Also evaluated in this study were issues related to the selectivity associated with the lanthanide mixture and the dependency of the ionic radius during lanthanide extraction.     

Tyrosine-based poly(m-phenyleneethynylene-p-phenyleneethynylene)s. Helix folding and responsiveness to a base

The Sonogashira-Hagihara polymerization of 3′,5′-diiodo-N-α-tert-butoxycarbonyl-l-tyrosine methyl ester (1) and 3′,5′-diiodo-N-α-tert-butoxycarbonyl-O-methyl-l-tyrosine methyl ester (2) with para-diethynylbenzene (3) was carried out to obtain optically active poly(m-phenyleneethynylene-p-phenyleneethynylene)s [poly(1) and poly(2)] with M_n’s ranging from 9900 to 15,000 in 80-87% yields. Poly(1) exhibited intense CD signals in DMSO and THF, but did not in CH₂Cl₂, indicating that it took a predominantly one-handed helical conformation in the former two solvents. On the other hand, there was no evidence for poly(2) to take a helical structure in these solvents. Poly(1) turned the CD sign at 390 nm from plus to minus in DMSO/H₂O = 9/1 (v/v) by the addition of NaOH. Alkaline hydrolysis of ester moieties of poly(1) and poly(2) gave the corresponding polymers having carboxy groups [poly(1a) and poly(2a)]. Poly(1a) and poly(2a) increased the CD intensity by the addition of NaOH.     

用仿生自组装法制备的新型生物复合材料及表征

通过仿生自组装法在室温下制备了纳米碳酸化羟基磷灰石/胶原（nCHAC）复合材料,并采用X射线衍射（XRD）、热分析（TGA）和透射电镜（TEM）进行了观察和分析.结果表明,该材料具有与天然骨相同的纳米尺度和胶原蛋白无机相,含有（2.8～14.7）w%的碳酸化HA成分;其显微结构是矿化的胶原纤维束,类似于天然骨的分级结构.揭示了碳酸化HA和胶原含量不同的复合材料中,具有微小差别的自组装单元.碳酸的百分含量影响矿物的晶体尺寸和胶原纤维的组装.因此,nCHAC复合材料是有前途的硬组织修复用材料,其所具有的特殊性能要归功于生物仿生制备出的nCHAC材料有与天然骨类似的成分和类似的微观结构.     

Photooxidative degradation of polyethylene containing flame retardants by monochromatic light

Photodegradation of incombustible polymer materials [high-density (HD) and low-density (LD) polyethylene (PE) containing 0.5 to 2.0 phr of decabromodiphenyl ether (DBDE) or tetrabromobisphenol A (TBA) as a flame retardant] were studied using an Okazaki Large Spectrograph (OLS). Samples were irradiated in air at 23°C with monochromatic light of wavelengths at 260, 280, 300, 320, 340, and 360 nm. Ultraviolet and Fourier transform infrared (FTIR) spectra were taken to estimate the chemical changes caused by photoirradiation. Molecular weight change was followed by gel permeation chromatography (GPC) measurements. It was found that the photostability of PE samples was reduced by the addition of flame retardants. The threshold wavelengths of photodegradation are 320 nm and 360 nm for PE–TBA samples and PE–DBDE samples, respectively. Main-chain scission is favored when the irradiation was carried out with the light of wavelength 300 nm for HDPE–DBDE and HDPE–TBA samples. The most effective irradiation wavelengths for crosslinking are found to be 300 nm and 280 nm for LDPE–DBDE and LDPE–TBA samples, respectively. 1995 John Wiley & Sons, Inc.