Analysis of mussel standard reference material by inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry

A method for the analysis of mussel standard reference material by inductively coupled plasma atomic emission spectrometry( ICP-AES) and inductively coupled plasma mass spectrometry(ICP-MS) was developed. K, Na, Ca, Mg, P, Al, Fe, Zn, Mn and Sr were determined by ICP-AES and As, B, Cd, Co, Cr, Cu, Ga, Ge, Mn, Mo, Ni, Pb, Se, Sr, U and V by ICP-MS, The interference coefficients at the Mn-55, Se-78, Cu-63, Co-59, Ni-58, Ni-60, As-75, Se-77, V-51, Cr-53 and Cr-52 originating from polyatomic ion of the matrix elements (KO)-K-39-O-16, K-39(2), (ArNa)-Ar-40-Na-23, (CaO)-Ca-43-O-16, (CaO)-Ca-42-O-16, (CaO)-Ca-44-O-16, (PO2)-P-31-O-16, (ArCl)-Ar-40-Cl-35, (ArCl)-Ar-40-Cl-37, (ClO)-Cl-35-O-16, (ClO)-Cl-37-O-16 and (ArC)-Ar-40-C-12 were determined under the selected operation parameters. The major matrix elements, such as K, Na and Ca, result in the suppression of analytes signals. The apparent concentration at the significant biological element which was produced by the different digestion methods, (.) HNO3 + H2O2 (3 + 2), HNO3 + HClO4 (3 + 0.5) and HNO3 + H2SO4 (3 + 0.5),was determined. The sample digested by HNO3 + H2O2 did not give rise to interfere on the analyte, and the backgrounds of Se-77, Ga-69, Zn-67, As-75, V-51, Cr-53 and Cr-52 were increased by HNO3 + HClO4 digestion method, that affected the determination of these elements, especially the monoisotope As and V. Sample digested by HNO3 + H2SO4 increased the backgrounds at Cu-65, Zn-64 and Zn-67. Detection limits of ICP-AES are 0.001 similar to 0.75 mg/L and those of ICP-MS are 0.005 similar to 1.01 mu g/L. The relative standard derivations of ICP-AES and ICP-MS are 2.7% similar to 12.8%, 3.4% similar to 24.8%, respectively.

High resolution electron microscopy study of single chain single crystals of gutta percha

Single chain single crystals (SCSC) of gutta percha (GP) were prepared by a dilute-solution spraying method. Electron diffraction (ED) patterns revealed that the single chain single crystal was of a new crystalline modification, the delta form. The images of SCSC of GP obtained with a high resolution electron microscope (HREM) showed a two dimensional periodic structure. Most of the images consisted of lattice fringes derived from the (001) zone. This is the first time that the single chain single crystal images of GP have been observed at a molecular level. Micrographs were image processed using optical filtering methods to improve the signal-to-noise ratio, and were compared with computer-generated simulations of the images. From the viewpoint of the defects seen in high resolution images, the crystal formation and melting processes are discussed. (C) 1998 Elsevier Science Ltd. All rights reserved.

High resolution solid-state NMR and DSC study of poly(ethylene glycol) silicate hybrid materials via sol-gel process

Hybrid materials incorporating poly(ethylene glycol) (PEG) with tetraethoxysilane (TEOS) via a sol-gel process were studied for a wide range of compositions of PEG by DSC and high resolution solid-state C-13- and Si-29-NMR spectroscopy. The results indicate that the microstructure of the hybrid materials and the crystallization behavior of PEG in hybrids strongly depend on the relative content of PEG. With an increasing content of PEG, the microstructure of hybrid materials changes a lot, from intimate mixing to macrophase separation. It is found that the glass transition temperatures (T-g) (around 373 K) of PEG homogeneously embedded in a silica network are much higher than that (about 223 K) of pure PEG and also much higher in melting temperatures T-m (around 323 K) than PEG crystallites in heterogeneous hybrids. Meanwhile, the lower the PEG content, the more perfect the silica network, and the higher the T-g of PEG embedded in hybrids. An extended-chain structure of PEG was supposed to be responsible for the unusually high T-g of PEG. Homogeneous PEG-TEOS hybrids on a molecular level can be obtained provided that the PEG. content in the hybrids is less than 30% by weight. (C) 1998 John Wiley & Sons, Inc.

MICROSTRUCTURE ANALYSIS OF 3 SEGMENTED COPOLYMERS CONTAINING POLYDIMETHYLSILOXANE BY SOLID-STATE HIGH-RESOLUTION NMR

The microstructure of two bicomponent and one tricomponent segmented copolymers, based on polydimethylsiloxane, poly(p-hydroxystyrene) or/and polysulfone, were investigated using an extended Goldman-Shen pulse sequence, proton spin-spin relaxation measurements, and C-13 and Si-29 NMR spectra. The results indicate that there exist four phases with different sizes, components and morphological structure in the segmented copolymers studied in this work, i. e., a rigid-chain phase of very slow motion, a rigid-chain-rich phase of slow motion, a flexible-chain-rich phase of fast motion and a flexible-chain phase of faster motion. The sizes of different domains, calculated from the spin diffusion rates, are about 50-100 angstrom for the flexible-chain-rich phase of fast motion and 200-300 angstrom for the flexible-chain phase of faster motion. The relative quantities of polydimethylsiloxane in the flexible-chain phase of fast motion are slightly different in different kinds of segmented copolymers.

A HIGH-RESOLUTION SOLID-STATE NMR AND DSC STUDY OF MISCIBILITY AND CRYSTALLIZATION BEHAVIOR OF POLY(VINYL ALCOHOL)/POLY(N-VINYL-2-PYRROLIDONE) BLENDS

Blends of crystallizable poly(vinyl alcohol) (PVA) with poly(N-vinyl-2-pyrrolidone) (PVPy) were studied by C-13 cross-polarization/magic angle spinning (CP/MAS) n.m.r. and d.s.c. The C-13 CP/MAS spectra show that the blends were miscible on a molecular level over the whole composition range studied, and that the intramolecular hydrogen bonds of PVA were broken and intermolecular hydrogen bonds between PVA and PVPy formed when the two polymers were mixed. The results of a spin-lattice relaxation study indicate that blending of the two polymers reduced the average intermolecular distance and molecular motion of each component, even in the miscible amorphous phase, and that addition of PVPy into PVA has a definite effect on the crystallinity of PVA in the blends over the whole composition range, yet there is still detectable crystallinity even when the PVPy content is as high as 80 wt%. These results are consistent with those obtained from d.s.c. studies.

ON THE SIGNIFICANCE OF WAVELENGTH POSITIONING ACCURACY IN MULTICOMPONENT ANALYSIS TECHNIQUES FOR THE CORRECTION OF LINE INTERFERENCES IN INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION-SPECTROMETRY

The present paper reports some definite evidence for the significance of wavelength positioning accuracy in multicomponent analysis techniques for the correction of line interferences in inductively coupled plasma atomic emission spectrometry (ICP-AES). Using scanning spectrometers commercially available today, a large relative error, DELTA(A) may occur in the estimated analyte concentration, owing to wavelength positioning errors, unless a procedure for data processing can eliminate the problem of optical instability. The emphasis is on the effect of the positioning error (deltalambda) in a model scan, which is evaluated theoretically and determined experimentally. A quantitative relation between DELTA(A) and deltalambda, the peak distance, and the effective widths of the analysis and interfering lines is established under the assumption of Gaussian line profiles. The agreement between calculated and experimental DELTA(A) is also illustrated. The DELTA(A) originating from deltalambda is independent of the net analyte/interferent signal ratio; this contrasts with the situation for the positioning error (dlambda) in a sample scan, where DELTA(A) decreases with an increase in the ratio. Compared with dlambda, the effect of deltalambda is generally less significant.

A HIGH-RESOLUTION SOLID-STATE NMR-STUDY OF THE MISCIBILITY, MORPHOLOGY, AND TOUGHENING MECHANISM OF POLYSTYRENE WITH POLY(2,6-DIMETHYL-1,4-PHENYLENE OXIDE) BLENDS

An extended Goldman-Shen pulse sequence was used to observe indirectly the proton spin diffusion in the blends of polystyrene (PS) with poly(2,6-dimethyl-1,4-phenylene oxides) (PPO). The results indicate that the average distance between PS and PPO is less than 5 angstrom in the intimately mixed phase, but there are heterogeneous domains on a 100-angstrom scale. The data of spin relaxation of carbons, T1(C), for homopolymers and their blends suggest that there is a strong pi-pi electron conjugation interaction between the aromatic rings of PS and those of PPO, while the aromatic rings of PPO drive the aromatic rings of PS to move cooperatively. It is the cooperative motion that markedly improves the impact strength of PS.

评价水产动物生长性能的生理生化指标和分子生物学指标

以奥利亚罗非鱼(Oreochromis aureus)为实验对象，设计了3种不同的摄食类型，分别是鲜活饵料组、饥饿3周后饱食投喂组和人工饲料组。鲜活饵料组投喂冰冻赤子爱胜蚓，利用蚯蚓体内丰富的营养成分和活性物质，以期获得奥利亚罗非鱼良好的生长状况；饥饿后饱食组是指饥饿3周后，以人工饲料饱食投喂2周，用于研究饥饿与补偿生长获得快速生长时血液理化指标的变化情况；人工饲料组作为对照组。纯淡水条件下养殖，水温25±2℃。测定了奥利亚罗非鱼在3种摄食类型饲喂下某些血液生理生化指标变化的情况，并将指标变化情况与增重率做相关性分析，试图找出能够反映奥利亚罗非鱼生长性能的血液生理生化指标。 研究结果表明，奥利亚罗非鱼在饥饿3周后获得了补偿生长，补偿生长时的增重率和特定生长率显著高于人工饲料组(P<0.05)，高于鲜活饵料组，但差别不显著；相关性分析研究表明血清总蛋白、胆固醇、四碘甲状腺原氨酸（T4）与增重率极显著相关(P<0.01)，血红蛋白显著相关(P<0.05)，红细胞、白细胞、碱性磷酸酶高度相关(相关系数为0.580、0.551和0.557)，因此，建议血清总蛋白、胆固醇和血红蛋白可作为能够反映罗非鱼生长性能的新指标。 根据序列设计引物，PCR反应条件：变性温度：95 ℃，3 min；退火温度：57℃，20 sec；延伸温度：72℃，5 min，共36个循环，从牙鲆、黑鲪和鲈鱼中克隆出胰岛素样生长因子（IGF-Ⅰ）部分序列，首次证实了IGF-Ⅰ在3种海水鱼中的存在。 利用蛋氨酸与ZnSO4•7H2O，在pH 5.5、80℃下，反应1小时，采用蛋氨酸与硫酸锌2：1的配料比，合成出了产物蛋氨酸螯合锌，蛋氨酸螯合锌外观白色，粉状，室温下微溶于水，不溶于乙醇，并用原子吸收光谱法测定其含锌量为15%，螯合率为88.2%。

Determination of trace arsenic and selenium in jellyfish by microwave digestion-hydride generation-atomic fluorescence spectrometry

A method of hydride generation-atomic fluorescence spectrometry was proposed in the present paper for the determination of trace arsenic and selenium in jellyfish. The samples were treated by the combination of microwave digestion and lyophilization. The optimal conditions for treating and analyzing samples were established. The problem of the effect of the superfluous acid in the digesting solution on the results was solved, and the influence of coexisting foreign ions on the determination of arsenic and selenium was investigated. The accuracy of the method was confirmed by the method of standard additions. This method proved to be simple, rapid and repeatable, and is suitable for the analysis of biologic samples containing water.

Effects of hypoxia on contents of essential elements in pika and rat heart

The effects of hypoxia on the levels of essential macroelements and trace elements (K, Na, Ca, Mg, Cu, Zn, Fe, and Mn) in the heart muscles of Wistar rats and plateau pikas (Ochotona curzoniae) were studied by atomic absorption spectrometry. Unlike the rat, the plateau pika is tolerant to hypoxia. The levels of K, Na, and the trace element Mn were not significantly changed in rat or pika hearts after exposure to hypoxia for 1, 10, or 25 d at simulated altitudes of 5000 and 7000 m. Other minerals (Ca, Mg, Cu, Zn, and Fe) were significantly affected by hypoxia and the levels followed different time-courses under different hypoxic regimes in these two animals. There were marked differences between the rat and pika in myocardial accumulation of essential elements such as Ca, which was increased to high levels in the rat but not affected in the pika. The results suggest that hypoxia affects animal physiological mechanisms by regulating the levels of essential elements.

A high-resolution solid-state NMR study on nano-structured HZSM-5 zeolite

Variations in the structure and acidity properties of HZSM-5 zeolites with reduction in crystal sizes down to nanoscale (less than 100 nm) have been investigated by XRD, TEM and solid-state NMR with a system capable of in situ sample pretreatment. As evidenced by a combination of Al-27 MAS NMR, Si-29 MAS, CP/MAS NMR and H-1 MAS NMR techniques, the downsize of the zeolite crystal leads to an obvious line broadening of the Al-27, Si-29 MAS NMR spectrum, an increasing of the silanol concentration on the external surface, and a pronounced alteration of the acidity distribution between the external and internal surfaces of the zeolite. In a HZSM-5 zeolite with an average size at about 70 nm, the nonacidic hydroxyl groups (silanols) are about 14% with respect to the total amount of Si, while only 4% of such hydroxyl groups exist in the same kind of zeolite at 1000 nm crystal size. The result of H-1 MAS NMR obtained using Fluorinert(R) FC-43 (perfluorotributyl amine) as a probe molecule demonstrates that most of the silanols are located on the external surface of the zeolite. Moreover, the concentration of Bronsted acid sites on the external surface of the nano-structured zeolite appears to be distinctly higher than that of the microsized zeolite.

The stability of nanosized HZSM-5 zeolite: a high-resolution solid-state NMR study

The thermal and hydrothermal stabilities of HZSM-5 zeolites with crystal sizes less than 100 nm have been studied by multinuclear solid-state NMR, combined with BET and XRD. As evidenced by Al-27 and Si-29 MAS as well as their corresponding cross-polarization/MAS NMR investigations, the thermal stability of nanosized HZSM-5 is not so good as that of microsized HZSM-5. This is due to two processes concerning dealumination and desilicification involved in the calcination of nanosized HZSM-5, while only the dealumination process is conducted in microsized HZSM-5 under the similar calcination process. The hydrothermal stability of nanosized HZSM-5 is, contrary to what was expected, not so bad as that of the microsized HZSM-5 in the course of steam treatment. The actual resistance of the hydrothermal stability to the crystal size of HZSM-5 can be ascribed to an active reconstruction of zeolitic framework through an effective filling of amorphous Si species into nanosized HZSM-5 during hydrothermal treatment. (C) 2001 Published by Elsevier Science B.V.