X-ray Diffraction Studies of Echinoderm Plates

X-ray diffraction studies confirm that, with few exceptions, each skeletal element of echtinoderms is a single crystal of magnesium-rich calcite and that a relation exists between the shape of the element and the crystallographic a- and c-axes. The exceptions incluide the teeth of echinoids, and the calcareous ring as well as the anal teeth of holothurians. The tubercles of an echinoid plate begin their growth as parts of the single crystal of the plate; under the mechanical action of the spines that are attached to them, they become partly polycrystalline, as shown by scanning electron microscopy and by x-ray powder diffraction. The interface between inorganic crystalline and organic amorphous matter in the skeletal element appears to be the first example reported in nature of a periodic mninimal suirface.     

X-ray Laue Diffraction from Protein Crystals

In conventional x-ray diffraction experiments on single crystals, essentially monochromatic x-rays are used. If polychromatic x-rays derived from a synchrotron radiation spectrum are used, they generate a Laue diffraction pattern. Laue patterns from single crystals of macromolecules can be obtained in less-than 1 second, and significant radiation damage does not occur over the course of an exposure. Integrated intensities are obtained without rotation of the crystal, and individual structure factors may be extracted for most reflections. The Laue technique thus offers advantages for the recording of diffraction patterns from short-lived structural intermediates; that is, for time-resolved crystallography.     

High Pressure X-ray Diffraction Studies on Barium

Simultaneous x-ray diffraction and electrical resistance measurements on barium establish, with certainty, that Bridgman's 78-kb resistance transition is identical with his 59-kb volumetransition. During this transition, the bodycentered cubic structure changes to hexagonalclose packed. Lattice parameters for the latter structure at 62 kb (volume scale) are: a = 3.90 A, c = 6.15 A, and c/a = 1.58. Compression (AV/Vo) at 62 kb is 0.359 + 0.005 compared to 0.345 previously reported by Bridgman. Below the transition, at 49 kb, compression is 0.300 +/- 0.005 compared to Bridgman's 0.288. Bridgman's 17-kb volume transition was not detected by x-ray diffraction.     

Time-Resolved X-ray Diffraction Study of Solid Combustion Reactions

Real-time synchrotron diffraction has been used to monitor the phase transformations of highly exothermic, fast self-propagating solid combustion reactions on a subsecond time scale down to 100 milliseconds and in some instances to 10 milliseconds. Three systems were investigated: Ti + C --> TiC; Ti + C + xNi --> TiC + Ni-Ti alloy; and Al + Ni --> AlNi. In all three reactions, the first step was the melting of the metal reactants. Formation of TiC in the first two reactions was completed within 400 milliseconds of the melting of the Ti metal, indicating that the formation of TiC took place during the passage of the combustion wave front. In the Al + Ni reaction, however, passage of the wave front was followed by the appearance and disappearance of at least one intermediate in the afterburn region. The final AlNi was formed some 5 seconds later and exhibited a delayed appearance of the (210) reflection, which tends to support a phase transformation from a disordered AlNi phase at high temperature to an ordered CsCl structure some 20 seconds later. This new experimental approach can be used to study the chemical dynamics of high-temperature solid-state phenomena and to provide the needed database to test various models for solid combustion.     

Amorphous Solid Water: An X-ray Diffraction Study

Water vapor that condenses on a metal surface at 10 degrees K forms a noncrystalline phase of estimated density 1.2 grams per cubic centimeter. X-ray diffraction data of high precision and resolution have been analyzed to yield oxygen atom pair correlation functions. The positional correlation in amorphous solid water extends over only a few molecular radii, and the radial distribution of nearneighbor oxygen atoms in amorphous solid water is qualitatively different from that found in the low-pressure ice modifications. Amorphous solid water is a useful material for liquid water models because it can be studied under conditions such that the effects of static disorder and thermal excitation can be separated.     

High-Pressure Polymorph of Thulium: An X-ray Diffraction Study

An x-ray diffractiotn study of thulium at room temperature and high pressure by means of a diamond-anvil press has shown that thulium transforms from a hexagonal close-packed structure to the samarium type, as other rareearth elements (gadolinium, terbium, dysprosium, and holmium) do. Unlike the other rare-earth elements, thulium (hexagonal close-packed) has an axial ratio (c/a) that is independent of pressure within experimental error and the transition is reversible. The transition occurs with increasing pressure in the range of 60 to 116 kilobars. The lattice paralieters of the samarium-type phase of thulium at about 116 kilobars are a = 3.327 +/- 0.005 angstroms and c = 23.48 +/- 0.04 angstroms, and the volume change at the transition is estimated to be - 0.5 percent of the volume of the hexagonal close-packed phase at the transition.     

Lead: X-ray Diffraction Study of a High-Pressure Polymorph

An x-ray diffraction study of lead under pressure has shown that face-centered cubic structure transforms to the hexagonal close-packed structure at room temperature and a pressure of 130+/- 10 kilobars. The volume change for the transformation is -0.18+/- 0.06 cubic centimeter per mole.     

Electron Population Parameters from Least-Squares Refinement of X-ray Diffraction Data

A least-squares refinement of x-ray diffraction data has been developed in which the parameters are the populations of atomic orbital products describing the molecular electron density distribution. The procedure is applied to alpha-oxalic acid dihydrate and cyanuric acid. Complementary structural information obtained by neutron diffraction has been used. In the absence of complementary information, the method allows simultaneous determination of structural and charge-density parameters. There is an indication of a migration of charge from the ppi to the psigma orbitals in both molecules.     

X射线衍射法研究毛竹微纤丝角的变异规律

应用X射线衍射技术对毛竹微纤丝角的变异规律进行了系统的研究。研究结果表明,毛竹微纤丝角在径向的变异幅度很小,并且没有稳定的变化规律。微纤丝角随竹材高度的增大而减小。虽然不同高度之间微纤丝角绝对值的差异小于1°,但方差分析表明,1m处竹材的微纤丝角与3m处之间存在显著差异,而3m和5m处之间的差异则不显著。微纤丝角随竹龄增大有增大的趋势,但绝对值差异也小于1°。同时方差分析表明,2、4、6年生毛竹之间的微纤丝角均存在显著差异,并且2年生与4年生之间的差异程度要大于4年生与6年生之间的差异程度。总体说来,毛竹微纤丝角在各方面的变异程度都比木材小得多,说明微纤丝角可能不是决定毛竹物理力学性能变异的主要因子。     

Synchrotron X-ray Diffraction Measurements of Single-Crystal Hydrogen to 26.5 Gigapascals

The crystal structure and equation of state of solid hydrogen have been determined directly to 26.5 gigapascals at room temperature by new synchrotron x-ray diffraction techniques. Solid hydrogen remains in the hexagonal close-packed structure under these pressure-temperature conditions and exhibits increasing structural anisotropy with pressure. The pressure-volume curve determined from the x-ray data represents the most accurate experimental measurement of the equation of state to date in this pressure range. The results remove the discrepancy between earlier indirect determinations and provide a new experimental constraint on the molecular-to-atomic transition predicted at higher pressures.     

中药材半夏的X射线衍射Fourier指纹图谱分析

[目的]建立中药材半夏的鉴定分析新方法。[方法]采用X射线衍射Fourier指纹图谱法获取中药材半夏的微观衍射图形及相应衍射特征标记峰,分析不同种半夏样品鉴别、炮制品与原药材的差异以及相关组分含量的差异,实现对常用中药材的微观鉴定分析。[结果]对12个半夏药材及其炮制品样品进行试验,获得了半夏的对照X射线衍射Fourier指纹图谱及特征标记峰值,依次将其分为药材半夏、水半夏及其炮制品法半夏、清半夏、姜半夏5个组,将中药材质量标准化从宏观等性状显微定性鉴别推向以图形数据表征的可重复的微观信息。[结论]X射线衍射Fourier指纹图谱法可用于中药材半夏的鉴定。     

利用X-射线衍射法测定竹材纤维素结晶度

应用X-射线衍射法对毛竹发育过程中的纤维素结晶度,以及不同造林方式和不同竹种的纤维素结晶度测定分析,结果表明:毛竹材成熟过程中,随竹龄增加纤维素结晶度的变化没有呈现明显的规律性,介于51%～54%之间。纤维素结晶度的比例是从竹青到竹黄逐渐降低,在竹干高度上的变化规律与竹龄有关。竹龄、竹干高度和竹壁径向位置对纤维素结晶度的影响差异不显著。对比两种造林方式的纤维素的结晶度,各个竹龄竹鞭侧芽育苗的纤维素结晶度均小于实生苗的相应值。6种竹材纤维素结晶度以孝顺竹的最大,毛竹的最小,介于43%～52%之间。     

Synchrotron X-ray Diffraction from a Microscopic Single Crystal Under Pressure

Metallic filaments with submicrometer diametere have been fabricated. Standard diffraction techniques with conventional x-ray sources were unsuccessful in identifying the structure of these materials. However, with the use of synchrotron radiation produced on a wiggler beam line, diffraction data were obtained in measurement periods as short as 10 milliseconds. Two cylindrical single crystals of bismuth were studied, each with a diameter of 0.22 +/- 0.02 micrometer. The volume of sample illuminated for these measurements was 0.38 cubic micrometer, less than 0.5 femtoliter. The crystals are grown in glass capillaries, and, because bismuth expands on solidification, they are under a residual hoop stress. The crystallographic data indicate the presence of a linear compressive strain of about 2 percent, which is assumed to be the result of a residual stress of about 2 gigapascals.     

X-ray Diffraction Studies on Tin at High Pressure and High Temperature

Tin at a pressure of 39 kb and at 314 degrees C has tetragonal symmetry with an atom at each point of a body-centered tetragonal lattice. The unit cell dimensions are a equal to 3.81 A, c equal to 3.48 A, and c/ a = 0.91. The melting curve of tin was observed up to 45 kb and the boundary line between the tin I and tin II phases was observed to 70 kb by x-ray diflraction techniques.     

X-ray Diffraction to 302 Gigapascals: High-Pressure Crystal Structure of Cesium Iodide

X-ray diffraction measurements have been carried out on cesium iodide (CsI) to 302 gigapascals with a platinum pressure standard. The results indicate that above 200 gigapascals CsI at 300 K has a hexagonal close-packed crystal structure with the ideal c/a ratio of 1.63 +/- 0.01. The crystal structure and pressure-volume relations converge at high pressure with those of solid xenon, which is isoelectronic with CsI. The results indicate a significant loss of ionic bonding in the hexagonal close-packed metallic phase of CsI at ultrahigh pressure.     

X射线衍射分析及其在微纤丝角测定中的应用

X射线衍射分析是目前应用十分广泛的一项技术,是利用X射线在晶体、非晶体中的衍射与散射效应进行物相分析、结构类型分析及不完整性分析的有效方法。介绍了X射线衍射分析的原理与方法,同时时X射线在木材微纤丝角测定中的应用技术进行了阐述。     

青海不同产区大黄的X-射线衍射图谱研究

[目的]为区分不同产地大黄药材的质量及鉴别提供依据。[方法]利用x一射线衍射分析法,得到青海不同产区大黄的X-射线衍射图谱,并对其进行相似性分析。[结果]不同产区的大黄中各化学成份的含量有差异,但其衍射图谱及衍射峰值具有一定的指纹特征。[结论]X-射线衍射法是鉴别不同产区的大黄及其他中药材的一种快捷有效的方法。     

Delftia sp.T3-6酰胺水解酶DamH晶体制备及X-射线衍射分析

Dam H是菌株Delftia sp.T3-6产生的具有酯键水解活性的酰胺酶,对其原核表达、纯化、结晶条件及蛋白晶体X-射线衍射条件进行了研究。经过原核表达,采用Ni-NTA亲和层析法和透析法纯化蛋白,成功获得了适合晶体生长的蛋白Dam H。289 K下采用座滴气相扩散法进行晶体筛选和制备,在蛋白浓度为15 mg/m L及含有0.2 mol/L乙酸铵,pH 7.1,21%(W/V)聚乙二醇3350的缓冲液中获得了理想的蛋白晶体。在低温100 K下通过X-射线衍射仪(Rigaku Micro Max-007 HF)收集了晶体衍射数据。晶体衍射分辨率为3.4,空间群为三斜晶系P1,晶胞参数为a=14.1,b=23.9,c=85.7,α=112.6°,β=77.2°,γ=89.1°。结晶条件的优化和晶体制备为Delftia sp.T3-6 Dam H高分辨率晶体制备提供了参考,晶体衍射数据的收集为Dam H三维结构的解析奠定了前期基础,将有助于阐明Dam H的催化机制。     

农业纤维物料压缩研究发展现状

全面分析了国内外关于农业纤维物料压缩研究的现状，指出了存在的问题，即：1）过去的研究多属“闭式”压缩试验研究；2）理论研究与实验脱节；3）对压缩过程中的影响因素考虑得不够全面；4）对压缩过程中被压缩物料的流变学特性研究不够。同时指出今后应加强研究的几个方面：1）以不同喂入量、不同压缩频率压缩时的蠕变和应力松弛问题；2）压缩室内草片和草捆在不同位置时的蠕变和应力松弛问题；3）草捆从压缩室出口释放时的膨胀和张力；4）综合考虑压力、压缩频率、喂入量、压缩室长度和草捆长度等对压缩过程的影响。