三种扇贝挥发性风味物质指纹图谱分析

为探究海湾扇贝(Argopecten irradians)、栉孔扇贝(Chlamys farreri)、虾夷扇贝(Patinopecten yessoensis)三种扇贝闭壳肌的挥发性风味物质差异,采用气相色谱-离子迁移谱(gas chromatography-ion mobility spectroscopy,GC-IMS)技术,对三种扇贝闭壳肌在新鲜(40℃)和加热(100℃)情况下进行挥发性成分分析。结果表明:在新鲜状态下,海湾扇贝(HWSB-F)、栉孔扇贝(ZKSB-F)、虾夷扇贝(XYSB-F)闭壳肌中,共定性出27种挥发性风味物质,其中醛类8种,醇类5种,酮类5种,酯类3种,以及醚类、苯类、酸类、烯类和噻唑等。在加热情况下,海湾扇贝(HWSB-C)、栉孔扇贝(ZKSB-C)、虾夷扇贝(XYSB-C)闭壳肌中共定性出52种挥发性风味物质,其中醛类20种,酯类5种,酮类7种,醇类8种,烯类4种,酸类2种,醚类2种,还包括吡嗪、胺类、苯类、含氧杂环等物质。对三种扇贝闭壳肌新鲜组和加热组指纹图谱进行分析,发现新鲜扇贝原有的挥发性风味物质加热后减少,且产生了新的其他种类的挥发性风味物质。扇贝闭壳肌加热组的挥发性风味物质种类较多,组成比较复杂,新鲜组的扇贝闭壳肌挥发性风味物质种类较少,组成简单。通过主成分分析,可在新鲜状态和加热状态下,有效区分三种扇贝闭壳肌组织。三种扇贝闭壳肌挥发性风味物质指纹图谱的建立,丰富了不同扇贝呈味物质的组成成分研究内容,证明GC-IMS技术可快速鉴别三种去壳扇贝闭壳肌的种类,为不同种扇贝闭壳肌以次充好提供检测依据。     

国内外钼资源供需形势分析

全面、系统地建立钼矿石、钼矿粉分析方法,对钼元素研究开发和保障钼矿工业发展具有重要意义。目前多采用酸溶或碱熔样品后进行分析,其不足是测定钼含量的范围窄,消耗样品量大,还需使用大量酸碱,且受仪器限制,分析高含量钼时多需对样品溶液进行数次稀释,使分析步骤更加繁琐。发射光谱法则可避免上述问题,但用之准确分析高含量钼矿石钼矿粉尚有测试方法的瓶颈需要突破。本文研究通过内标元素、分析线对、缓冲剂配比、电流程序等环节的实验分析,建立了固体进样-交流电弧发射光谱法测定钼矿石中高含量钼的分析方法：优化样品与光谱缓冲剂质量比至1∶2,优化分析线对,截取曝光时间35s,采用以国家一级合成硅酸盐光谱分析标准物质和国家一级矿石标准物质组成的自研标准系列制作标准曲线,由全谱交直流电弧发射光谱仪自动扣除分析线和内标线背景后以对数坐标二次曲线拟合计算,使测定范围扩展为500～500800μg/g,检出限为27.38μg/g,相对标准偏差（RSD）为3.28%～8.30%,相对误差为-0.43%～0.73%。结果表明,本文方法在实现绿色分析的同时,在检出限相当、精密度合格的条件下,一次性分析高含量钼的上限从5%提高至50%。

     

微量金化学光谱法标准系列配制及活性炭处理的改进

对微量金化学光谱法中活性炭自理及标准系列配制的方法进行了探索,改进了微量金化学光谱法活性炭处理及标准系列配制。将该法配制的标准系列应用于微量金化光谱测定,提高了分析结果的准确度。用标准试样分析及原子吸收（ＡＡＳ）法验证,结果与标准值及ＡＡＳ法相符。     

内蒙古东乌旗沙麦钨矿床成矿机制：来自流体包裹体及稳定同位素的证据

内蒙古东乌旗沙麦钨矿床位于中亚巨型缝合带的最东段,矿床内广泛发育云英岩化,钨矿体主要受NW向断裂构造控制,呈黑钨矿-石英脉状产出在燕山期沙麦岩体（岩性主要为黑云母二长花岗岩）和泥盆系围岩地层（岩性主要为角岩化砂岩、砂砾岩）中。成矿阶段从早到晚分别为：石英-黄玉阶段（Ⅰ）、云英岩-黑钨矿阶段（Ⅱ）和晚期硅化阶段（Ⅲ）。本文对矿床流体包裹体及C-H-O-S同位素进行了研究,结果显示：矿床中普遍发育CO2-H2O包裹体及水溶液气液两相流体包裹体。从成矿早期至成矿晚期,矿床流体中富CO2包裹体逐渐减少,CO2含量逐渐降低。成矿早期可见熔体包裹体与流体包裹体共存的现象,属低盐度、富CO2的岩浆来源流体。矿床成矿作用从早到晚,流体包裹体均一温度分别为279~341℃、196~286℃、103~201℃;流体盐度分别为(1.6~9.1)%NaCleq、(3.0~11.1)%NaCleq、(0.9~4.7)%NaCleq。激光拉曼光谱分析结果显示,流体中的气相主要是CO2,部分含有H2O和CH4。成矿流体从早期中高温、中盐度流体向晚期低温、低盐度流体演化,属NaCl-H2O-CO2±CH4热液体系。矿床稳定同位素研究表明,沙麦钨矿床的成矿流体主要来源于岩浆水,并在成矿晚期混入了大气水。矿床硫的来源与早白垩世岩浆-热液系统或深部幔源岩浆相关,并混入了部分地层硫。综合分析认为,沙麦钨矿为一岩浆期后热液型钨矿床。燕山期侵入体从深部携带成矿物质,经历了岩浆分异和流-熔体相互作用等过程,形成区内岩浆-热液成矿系统。流体的不混溶是导致含钨络合物分解乃至最后沉淀成矿的主要原因。     

Performance of the Nuclear Compton Telescope

On 1 June 2005, the prototype Nuclear Compton Telescope (NCT) flew on a high altitude balloon from Fort Sumner, New Mexico. NCT is a balloon-borne soft γ-ray (0.2–10 MeV) telescope for studying astrophysical sources of nuclear line emission and γ-ray polarization. Our program is designed to develop and test technologies and analysis techniques crucial for the Advanced Compton Telescope; however, our detector design and configuration is also well matched to the focal plane requirements for focusing Laue lenses. The NCT prototype utilizes two, 3D imaging germanium detectors (GeDs) in a novel, ultra-compact design optimized for nuclear line emission in the 0.5–2 MeV range. Our prototype flight provides a critical test of the novel detector technologies, analysis techniques, and background rejection procedures developed for high resolution Compton telescopes.     

Silicates in evolved stars: the lrs-maser chronology revisited

Since the publication of our correlation (1990 Ap.J. 350, L45) suggesting a temporal relationship among: (a) shapes of 10 micron silicates seen in IRAS Low Resolution Spectra (LRS); (b) IRAS broad band colors; (c) light curve asymmetries, and (d) the types of masers associated with various Mira variable stars, the question has arisen whether the implied chronology refelcts the interval between thermal pulses, or the more lengthy ascent of the AGB. There is evidence in favor of the former interpretation. A strong implication of this idea is that variability among pre-silicate spectra should be significant. Several examples of this have been found in the extended LRS database, and are presented. Finally, plans are presented to continue monitoring of selected variables in the 10 micron region, to verify the variability suggested in the limited phase coverage provided in the LRS database. Monitoring will include use of our facilities at the Mt.Evans-Womble Observatory — highest in the world at 4313 meters altitude.     

原位低温拉曼光谱技术在人工合成CaCl_2-H_2O和MgCl_2-H_2O体系流体包裹体分析中的应用Ⅰ:低温拉曼光谱研究

利用原位低温拉曼光谱分析技术,对在设定的实验条件下合成的CaCl2-H2O体系和MgCl2-H2O体系的流体包裹体进行分析研究,结果表明低温下CaCl2水溶液和MgCl2水溶液形成的盐水合物具有各自不同的特征拉曼光谱,通过测定特征光谱,能够简易直接的鉴定这些物质,进而确定盐水体系包裹体的成分.因此,原位低温拉曼光谱技术,能够有效地测定Ca2+和Mg2+这两种盐水体系包裹体流体中常见,但显微测温过程难以观察和判别的二价阳离子.实践表明,原位低温拉曼光谱分析技术是对传统的流体包裹体显微测温技术的一个十分有效的补充,在包裹体研究领域会得到越来越广泛的应用.     

Transport properties of low-sanidine single-crystals, glasses and melts at high temperature

Thermal diffusivity (D) was measured using laser-flash analysis from oriented single-crystal low-sanidine (K_0.92Na_0.08Al_0.99Fe³⁺ _0.005Si_2.95O₈), and three glasses near KAlSi₃O₈. Viscosity measurements of the three supercooled liquids, in the range 10^6.8 to 10^12.3 Pa s, confirm near-Arrhenian behavior, varying subtly with composition. For crystal and glass, D decreases with T, approaching a constant near 1,000 K: D _sat ∼ 0.65 ± 0.3 mm² s⁻¹ for bulk crystal and ∼0.53 ± 0.03 mm² s⁻¹ for the glass. A rapid decrease near 1,400 K is consistent with crossing the glass transition. Melt behavior is approximated by D = 0.475 ± 0.01 mm² s⁻¹. Thermal conductivity (k _lat) of glass, calculated using previous heat capacity (C _P) and new density data, increases with T because C _P strongly increases with T. For melt, k _lat reaches a plateau near 1.45 W m⁻¹ K⁻¹, and is always below k _lat of the crystal. Melting of potassium feldspars impedes heat transport, providing positive thermal feedback that may promote further melting in continental crust.     

Red micas from basal ignimbrites of Mt. Vulture (Italy): interlayer content appraisal by a multi-methodic approach

The crystal chemistry of red phlogopites from Mt. Vulture (Italy) ignimbrites has been studied by electron microprobe, secondary ion mass spectrometry (SIMS), single crystal structural investigation and Fourier transform infrared (FTIR) spectroscopy. The analysed phlogopite has Fe/(Fe + Mg) ∼ 0.35, TiO₂ (wt%): 2.8–5.0 and H₂O (wt%): 1.24–3.37. Infrared spectra revealed the presence of bands due to the NH₄⁺ and H₂O stretching and bending vibrations. The samples belong to the 1M polytype. The bimodal behaviour of several structural parameters allows red micas to be clustered into two distinct groups: K⁺ ↔ NH₄⁺, H₂O and M³⁺-vacancy substitutions dominate in the first group; M^3+,4+-oxy, in the second group. It has to be pointed out that quantitative analysis of hydrogen (via SIMS) together with the characterization of the local environment of the anionic site (via FTIR) are fundamental in assessing the correct structural formula and the substitution mechanisms in micas. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Vibrational states of H<Subscript>2</Subscript>O in beryl: physical aspects

Single-crystal polarized Raman spectra (3,000–4,000 cm⁻¹ at 3 ≤ T ≤ 300 K) were measured for synthetic alkali-free and natural beryl, Be₂Al₃Si₆O₁₈·xH₂O, to determine the behavior of H₂O molecules of both Type I and Type II in the cavities. At low temperature, the H₂O molecules of Type I displace from the center of cavity and give rise to very weak hydrogen bonding with the host lattice. The H₂O Type I translational motion is characterized by substantial anharmonicity and looks like a motion of “a particle in the box” with a frequency of 6.3 cm⁻¹. Water Type II is characterized by a free rotation with respect to the C ₂ molecule axis, and it makes possible the water nuclear isomers (i.e. ortho- and para-) to be observed at low temperature.