99 resultados para X-RAYS: INDIVIDUALS: 1RXS J141256.0 792204
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用磁控溅射法制备了周期厚度和周期数均相同的Mo/Si多层膜,用原子力显微镜和小角X射线衍射分别研究了Mo靶溅射功率不相同时,Mo/Si多层膜表面形貌和晶相的变化。随后在国家同步辐射实验室测量了Mo/Si多层膜的软X射线反射率。研究发现,随着Mo靶溅射功率的增大,Mo/Si多层膜的表面粗糙度增加,Mo的特征X射线衍射峰也增强,Mo/Si多层膜的软X射线峰值反射率先增大后减小。
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中国东北样带(NorthEast China Transect, NECT)是位于中纬度温带以降水量作为主要驱动因素的陆地样带。本文的工作以此作为研究平台,利用生态信息系统(Ecological Information System, EIS)以及Microsoft Excel 7.0软件包建立了样带的地理数据库和植物多样性数据库,包括气候数据库、植被数据库、遥感数据库和内蒙内C_4植物数据库以及样带内生态系统特征数据库。在此基础上,主要研究了以下四个方面的内容: 1. 利用Holdridge的生命地带方法对NECT内的生物群区进行了划分。 主要是确定了生物群区间过渡带的位置与宽度,并预测了在全球变化三种模式下NECT内生物群区,尤其是过渡带的变化图景。湿度升高2 ℃后,过渡带的面积都呈扩大化的趋势。森林区对于降水量的变化反应很敏感。荒漠灌丛(即荒漠草原类型)由于其水热条件处于样带内较极端类型,因而对于全球气候变化反应也比较敏感。 2. 研究了NECT内的α、β多样性以及包括生活型、水分生态型、区系地理成分等在内的植物群落特征多样性的梯度变化规律。 研究了样带内的多样性梯度,提出了在样带内存在的α多样性测度问题以及β多样性沿样带的变化规律:样带内由东到西,β多样性逐渐升高,群落内物种被替代的速率变慢;两种植被类型边界上的两个样地之间的相似程度由东到西呈上升趋势;同一类型群落之间的物种周转率比不同类型群落间的物种周转率相对要低。同时将各个环境因子与α、β多样性作了回归分析,找出样带内决定α、β多样性的主要环境因子指标。 样带内沿43.5°N一线附近植物群落的生活型共有17类,水分生态型8类,区系地理成分包括17类,以此为基础分析了群落特征沿样带的变化规律。并探讨了生活型分布的历史地理原因。 3. 对样带气候-NDVI间的关系以及植被-NDVI的关系进行了探讨。 利用来自气象卫星的遥感数据一归一化植被指数(NDVI),和数值化后的样带1:100万植被图进行叠加,找到NECT内每种植被类型对应的NDVI值。样带内共有植被类型147种,反映在NDVI变化上的植被类型有106类。其中,自然植被101种。 影响年均NDVI分布的因子主要有经度、辐射日照百分率及7月温度,与经度呈正相关,与辐射日照时数及7月温度呈负相关。回归方程如下: NDVI = -220.426 + 3.273Lon - 80.338Ratio - 1.962T_7 (R~2 = 0.9714, F = 521.52, p < 0.001) 4. 研究了NECT内的光合功能型。 主要包括内蒙古地区的C_4植物及其生态地理特性。揭标C_4植物的分类群特性、生活型、水分生态型与区系地理成分等生态学特性。C_4植物分布的科属极其集中。C_4光合型为维管植物某些分类群(科、属、种)的特性,为它们固有的遗传特性。推断C_4起源于草本的某些科属。C_4植物为喜热、耐旱的类群。世界种、泛热带种、泛地中海种C_4植物较集中。 样带内的C_3、C_4功能型及其与环境因子的相关性。样带内C_4和C_3光合型植物组成比例由东到西表现出两高两低的趋势。分布主要与年均温和降水量呈显著相关。 提出了一种新的C_3、C_4鉴别方法。即根据野外测定的光合数据建立了C_3、C_4的判别模型: f_1(x) = -1.5493 + 0.1427Pn + 0.1035Tr + 0.3768ΔT + 0.1000Gs f_2(x) = -15.6142 + 1.0542Pn - 0.2503Tr - 0.2957ΔT + 0.6491Gs 最后,综合7个GCMs模型(GFDL,GISS,LLNL,MPI,OSU,UKMOH,UKMOL)的输出结果,利用此结果和本文建立的回归模型,模拟了样带内生物多样性的窨分布格局,并预测了末来全球变化下归一化植被指数NDVI的空间分布格局的变化。
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记述了中国产红索藻属ThoreaBoryemend Necchi的 2种 2变种 ,即棘刺红索藻T hispida (Thorea)Desvauxemend Sheath ,VisetCole ,棘刺红索藻小孢变种T hispidavar microsporaS L XieetZ X Shi,蓝色红索藻T vio laceaBoryemend Sheath ,VisetCole和蓝色红索藻长毛变种T violaceavar longipilosaS L XieetZ X Shi.其中 ,蓝色红索藻T vi
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To investigate the occupational exposure levels to polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs), polybrominated diphenyl ethers (PBDEs), and polychlorinated biphenyls (PCBs), indoor dust (n = 3) in workshops and hair samples from male workers (n = 64) were collected at two electrical and electronic equipment waste (E-waste) dismantling factories located in the LQ area in east China in July 11-13, 2006. Pre- and postworkshift urines (64 of each) were also collected from the workers to study oxidative damage to DNA using 8-hydroxy-2'-deoxyguanosine (8-OHdG) as a biomarker. The concentrations of PCDD/Fs, PCDD/F-WHO-TEQs, PBDEs, PCBs and PCB-WHO-TEQs were (50.0 +/- 8.1) x 10(3), 724.1 +/- 249.6, (27.5 +/- 5.8) x 10(6), (1.6 +/- 0.4) x 10(9), (26.2 +/- 3.0) x 10(3) pg/g dry weight (dw) in dust, and (2.6 +/- 0.6) x 10(3), 42.4 +/- 9.3, (870.8 +/- 205.4) x 10(3), (1.6 +/- 0.2) x 10(6), 41.5 +/- 5.5 pg/g dw in hair, respectively. The homologue and congener profiles in the samples demonstrated that high concentrations of PCDD/Fs, PBDEs, and PCBs were originated from open burning of E-waste. The 8-OHdG levels were detected at 6.40 +/- 1.64 mu mol/mol creatinine in preworkshift urines. However, the levels significantly increased to 24.55 +/- 5.96 mu mol/mol creatinine in postworkshift urines (p < 0.05). Then, it is concluded that there is a high cancer risk originated from oxidative stress indicated by the elevated 8-OHdG levels in the E-waste dismantling workers exposed to high concentrations of PCDD/Fs, PBDEs, and PCBs.
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Anadromous Coilia ectenes was sampled from the Yangtze estuary at Chongming and two of the primary upstream spawning grounds at Jingjiang and Anqing in April, May, June and August 2006. Gonad development was analyzed for females. In April, fish were collected in the estuary and at Jingjiang, but not at Anqing. No female was mature (gonad at stages IV or V) at either location. In May, 45% of the females were mature in the estuary, 9% at Jingjiang and 5% at Anqing. In June, 86% were mature in the estuary, 83% at Jingjiang and 7% at Anqing. In August, C. ectenes was absent at Jingjiang. No female was mature in the estuary, and all females were mature at Anqing. Absolute fecundity (AF) increased significantly with standard length (SL) by a power function AF = 2.27 x 10(-6) x SL2.67 (r(2) = 0.57, n = 48, P < 0.05). Mature females in the estuary were smaller than those at Jingjiang and Anqing. Conservation of spawners in the upstream spawning grounds is important because they have a size-related fecundity advantage over the smaller spawners in the estuary.
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Successful applications of expanded bed adsorption (EBA) technology have been widely reported in the literature for protein purification. Little has been reported on the recovery of natural products and active components of Chinese herbal preparations using EBA technology. In this study, the hydrodynamic behavior in an expanded bed of cation resin, 001 x 7 Styrene-DVB, was investigated. Ephedrine hydrochloride (EH) was used as a model natural product to test the dynamic binding capacity (DBC) in the expanded bed. EBA of EH directly from a feedstock containing powdered herbs has also been investigated. These particles are different from commercially available expanded bed adsorbents by virtue of their large size (20S to 1030 gm). When the adsorbent bed is expanded to approximately 1.3 to 1.5 times its settled bed height, the axial liquid-phase dispersion coefficient was found to be of the order 10(-5) m(2) s(-1), which falls into the range 1.0 x 10(-6) to 1.0 X 10(-5) m(2) s(-1) observed previously in protein purification. Because of the favorable column efficiency (low axial dispersion coefficient), the recovery yield and purification factor values of EH directly from a feedstock reached 86.5% and 18, respectively. The results suggest that EBA technology holds promise for the recovery of natural products and active components of Chinese herbal preparations.
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The spatial distribution and morphological diversity of virioplankton were determined in Lake Donghu which contains three trophic regions: hypertrophic, eutrophic and mesotrophic region. Virioplankton abundance measured by transmission electron microscope (TEM) ranged from 7.7 x 10(8) to 3.0 x 109 ml(-1), being among the highest observed in any natural aquatic system examined so far. The spatial distribution of virioplankton was correlated significantly with chlorophyll a concentration (r = 0.847; P < 0.01) at the sampling sites in Lake Donghu. 76 morphotypes were observed. Most morphotypes have tails, belonging to Siphoviridae, Myoviridae and Podoviridae. The majority of tailed phages in the lake were Myoviridae. Morphotypes which were rarely reported, such as prolate-headed virus-like particles, lemon-shaped virus-like particle, and viruses resembling Tectiviridae and Corticoviridae were all observed in the lake. It is concluded that the high viral abundance might be associated with high density of phytoplankton including algae and cyanobacteria. There was high viral diversity in this eutrophic shallow lake. In addition, cyanophage represented an important fraction of the virioplankton community in Lake Donghu. (c) 2006 Elsevier SAS. All rights reserved.
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AlGaN/GaN high electron mobility transistor (HEMT) hetero-structures were grown on the 2-in Si (1 1 1) substrate using metal-organic chemical vapor deposition (MOCVD). Low-temperature (LT) AlN layers were inserted to relieve the tension stress during the growth of GaN epilayers. The grown AlGaN/GaN HEMT samples exhibited a maximum crack-free area of 8 mm x 5 mm, XRD GaN (0 0 0 2) full-width at half-maximum (FWHM) of 661 arcsec and surface roughness of 0.377 nm. The device with a gate length of 1.4 mu m and a gate width of 60 mu m demonstrated maximum drain current density of 304 mA/mm, transconductance of 124 mS/mm and reverse gate leakage current of 0.76 mu A/mm at the gate voltage of -10 V. (C) 2008 Published by Elsevier Ltd.
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This paper studies the development of a real-time stereovision system to track multiple infrared markers attached to a surgical instrument. Multiple stages of pipeline in field-programmable gate array (FPGA) are developed to recognize the targets in both left and right image planes and to give each target a unique label. The pipeline architecture includes a smoothing filter, an adaptive threshold module, a connected component labeling operation, and a centroid extraction process. A parallel distortion correction method is proposed and implemented in a dual-core DSP. A suitable kinematic model is established for the moving targets, and a novel set of parallel and interactive computation mechanisms is proposed to position and track the targets, which are carried out by a cross-computation method in a dual-core DSP. The proposed tracking system can track the 3-D coordinate, velocity, and acceleration of four infrared markers with a delay of 9.18 ms. Furthermore, it is capable of tracking a maximum of 110 infrared markers without frame dropping at a frame rate of 60 f/s. The accuracy of the proposed system can reach the scale of 0.37 mm RMS along the x- and y-directions and 0.45 mm RMS along the depth direction (the depth is from 0.8 to 0.45 m). The performance of the proposed system can meet the requirements of applications such as surgical navigation, which needs high real time and accuracy capability.
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This paper studies the development of a real-time stereovision system to track multiple infrared markers attached to a surgical instrument. Multiple stages of pipeline in field-programmable gate array (FPGA) are developed to recognize the targets in both left and right image planes and to give each target a unique label. The pipeline architecture includes a smoothing filter, an adaptive threshold module, a connected component labeling operation, and a centroid extraction process. A parallel distortion correction method is proposed and implemented in a dual-core DSP. A suitable kinematic model is established for the moving targets, and a novel set of parallel and interactive computation mechanisms is proposed to position and track the targets, which are carried out by a cross-computation method in a dual-core DSP. The proposed tracking system can track the 3-D coordinate, velocity, and acceleration of four infrared markers with a delay of 9.18 ms. Furthermore, it is capable of tracking a maximum of 110 infrared markers without frame dropping at a frame rate of 60 f/s. The accuracy of the proposed system can reach the scale of 0.37 mm RMS along the x- and y-directions and 0.45 mm RMS along the depth direction (the depth is from 0.8 to 0.45 m). The performance of the proposed system can meet the requirements of applications such as surgical navigation, which needs high real time and accuracy capability.
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事务监控器是开发、部署、监控和管理分布式事务性应用的基础平台.随着Internet和企业应用集成的发展,许多应用要求能通过广域网访问部署于事务监控器上的服务,同时能与其它分布式系统互操作,但传统的事务监控器作为一种封闭的结构,对此支持不足.Web服务是一种新的分布式组件标准,可方便地部署于广域网上并灵活地进行企业应用集成,本文提出了事务监控器支持Web服务的一个可移植的设计框架TP-WS,可以在符合X/Open DTP模型的事务监控器中支持Web服务.本文设计现已应用到事务监控器ISTX2.0中.
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本工作采用DSC方法、红外光谱方法、光学显微镜方法、小角激光光散射方法及X射线衍射和散射方法研究了聚(ε-已内酯)(PCL)/苯乙烯-丙烯腈共聚物(SAN)共混物的相容性、熔融行为、结晶过程及结晶形态。观察到PCL/SAN共混物在0~30%wt PCL组成范围内,表现出单一的玻璃化转变,这个转变界于两个纯组合的玻璃化转变之间。在红外光谱上观察到PCL的羰基峰随着SAN的混入移向低频率。说明PCL分子与SAN分子之间存在着特殊的相互作用。从熔点下降计算的相互作用参数结果表明,PCL/SAN共混物在热力学上是相容的。共混物中PCL的熔点下降表明SAN分子对于PCL熔融行为是有影响的,同时不同的退火条件对于PCL/SAN共混物的PCL熔点也是有影响的,退火温度越高相应的PCL熔点越高。在PPCL/SAN共混物体中,PCL的球晶生长速率类似于均聚物,并且随着SAN含量的增加球晶生长速率下降,说明SAN分子阻碍了PCL分子链段的迁移,并且可以从理论上模拟共物混物中PCL的线性生长速率。在结晶性的PCL/SAN共混物中,PCL是以球晶形式存在的,在不同的结晶条件下,产生不同的球晶形态。在慢速降温结晶条件,SAN的加入促使PCL片晶发生扭曲形成环状球晶,通过光学显微镜方法和光散射方法计算出扭曲周期,结果表明扭曲周期随着SAN含量的增加而减少,同时也表明球晶半径随着SAN含量的增加而减小。在等温结晶条件下,SAN的加入,使得PCL的球晶半径减小。X射线衍射结果表明SAN分子并不存在PCL晶体中,而小角X射线散射结果表明在共混物中,随着SAN含量的增加,PCL片晶中心之间距离(长周期)逐渐增加,而且片晶与无定形片层的界面是分明的。指出无定形相是存在在PCL的片晶之间。
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利用溶胶-凝胶法合成了一系列稀土离子掺杂的发光薄膜,包括三元氧磷灰石稀土硅酸盐Ca2RS(SiO4)6O2(R=YGd)体系,YVO4体系,LaPO4体系以及钒磷酸盐形成的固熔体体系1并研究了稀土离子Eu3+,Tb3+,Dy3+,Sm3+,Er3+和类汞离子Pb2+在这些薄膜中的发光性质和能量传递性质。同时利用软石印法结合毛细管微模板技术实现了发光薄膜的图案化。SEM以及AFM结果表明,利用溶胶一凝胶法制备的发光薄膜表面致密均匀,无开裂。通过增加镀膜溶液的粘度、镀膜的次数可以有效的控制薄膜的厚度,使其达到理想的范围。由此可见溶胶一凝胶法是一种比较理想的制备发光薄膜的方法。在三元氧磷灰石稀土硅酸盐Ca2R8(SiO4)6O2(R=YGd)体系中,稀土离子Eu3+,Tb3+在Ca2Y8(SiO4)6O2基质中占据低刘·称性格位6h(Cs)和4f(C3),并以其特征的红光发射(5Do-7F2)和绿光发射(5D4-7F5)为主。Eu3+,Tb3+发光的最佳浓度分别为Y3+的10mol%和6mol%,Ca2Y8(51O4)6O2:Eu3+薄膜样品的发光强度和寿命随着烧结温度的升高而增加,Ca2Y8(SiO4)6O2:Tb3+薄膜样品的发光强度和寿命在800℃时最大,随后又随烧结温度的升高有所下降,Pb2+可以敏化Ca2Gd8(SiO4 )6O2中Gd3+的基质晶格,通过Pb2+→Gd3十→(Gd3+)n→A3+形式传递和转移能量。在YVO4体系中,利用Pechini溶胶一凝胶法以无机盐为主要原料,柠檬酸为络合剂,利用聚乙二醇调节镀膜溶液的粘度,制备了YvO4:A(A=Eu3+ Dy3+,Sm3+,Er3+)纳米发光薄膜。结合软石印法,通过简单工艺实现了发光薄膜图案化烧结过程中图案化薄膜有一定程度的收缩,存在一定的缺陷。得到的条纹在紫外灯下发出明亮的红光。掺杂的稀土离子在YVO4薄膜中显示它们特征发射,同时VO43-和稀土离子之间存在能量传递。Dy3+,Sm3+,Er3十发光的最佳浓度皆为Y3+的2mol%,这三者的发光淬灭是由交叉驰豫引起的。在LaPO4发光薄膜中,Etl3+以591nm的5Do-7Fl跃迁发射为主,呈现红橙光;Tb3+以543nm的5D4-7F5发射为主,属于绿光发射。Ce3+则由其特有的5d-4f双峰发射组成。Tb3+和Eu3+掺杂的样品发光强度和荧光寿命随烧结温度的升局而增加。Tb3+和Eu3+的寿命曲线符合指数衰减,但Tb3十在LaPO4:Ce,Tb薄膜中,所得的寿命曲线不符合单指数衰减。Ce3+和Tb3+之间存在吸收能量传递。通过计算得到能量传递效率可以达到95%以上。XRD结果表明,从x=0到x=1 YVxP1-xO4:Eu3+薄膜形成了一系列具有错石结构的固熔体。在YVxP1-xO4:Eu3+(0≤x≤1)系列薄膜中,随着x值的增加,Eu3+的发光强度和红橙比逐渐增大。除x=0,其它的Eu3+的红橙比都大于1,说明在发射光谱中,以Eu3+禁戒5Do一7F2电偶极跃迁为主,Etls十在基质中处于低对称性格位。当x=0时,即Y0.98Eu0.l2PO4薄膜中,Eu3+,仍处于D2d低对称性格位,但5D0一7FI橙光发射却比SD0一7F2红光发射强。x对Y0.98Eu0.02VxP1-xO4(0≤x≤l)薄膜寿命曲线有很大的影响,当0≤x≤0.5时,Eu3+5 D0-7F2发射呈单指数衰减;当x≥0.6时,Eu3+5D0-7F2发射的衰减曲线比较复杂,不能用单指数拟合。YVxP1-xO4:A3+(0≤x≤1,A=Er,Sm)薄膜中,由于存在VO43-A3+,以及VO43-(VO43-)n-A3+(n≥1)形式的能量传递,同时由于浓度淬灭,VO43-的蓝光发射在0.1≤x≤1范围内,随x的增加而减弱,当x=1时,VO43-的蓝光发射被完全淬灭,而A3+发光强度随x的增加而增加。在RVO4:A3+(R=Y,La,Gd,A=Eu,Sm,Er)纳米发光薄膜中,R对稀土离子发光性质的影响主要是由于基质晶体结构的不同。A3+在YVO4和GdVO4中属于D2d对称性,在YVO4和GdVO4薄膜中A3+的光谱性质基本相同,而LaVO4属于单斜晶系,具有独居石结构。A3+在LaVO4中属于C1对称性。C1对称性比D2d对称性低,A3+的发光光谱中谱线的位置以及谱线的劈裂数目都略有不同。由于Gd3+和发光离子之间的能量传递,A3+在GdVO4基质中的发光最强。
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采伐迹地上运走大径级的原木所剩下的枝桠物质是生态系统养分能量的来源;是动力,植物和微生物物栖息地。在本世纪五十年代就有人(A. A. Loman)对择伐和皆伐迹地上的枝桠进行了研究,用以比较它们树皮存留率的差异,但详细深入的研究是在八十年代以后,以R. L. Edmonds, C. E. Pertson为代表研究不同层次,不同径级研究枝桠的分解速率,我国在此领域的研究尚属空白。本文以长白山阔叶红松林带的四个树种:红松,白桦,落叶松,色木为对象探讨了它们枝桠的生物量,分解速率,分解过程中的养分动态以及枝桠堆对更新和火灾的影响。采伐后0-14后间,迹地上枝桠干重为31.96-9.60T/ha,通过对7个年代采伐迹地上枝桠堆面积估算后得知,枝桠堆平均占地为11.53%,以1CM直径累计值对应的枝桠堆的高度(Y:CM)为因变量,分解时间(X, yr)为自变量,则枝桠堆高度随时间变化的过程可以描述为:Y = 1.288 - 0.000889 X~2 r = -0.9896。本文以密度(Y: g/CM~3)随分解年令(X: yr)的变化来表示分解速率。四十年代样品用排水法求出来的密度与用园柱法求出的密度有如下相关关系:Y排 = 0.0129 +2.316 Y园,r = 0.94 Y表示密度(g/CM~3)。我们用单项指数模型描述分解速率:落叶松:Y = 0.4701 * exp (-0.01783 X) r = -0.927 色木: Y = 0.6742 * exp (-0.07824 X) r = -0.988 红松:Y = 0.5349 * exp (-0.03421 X) r = -0.927 桦树:Y = 0.5316 * exp (-0.1139 X) r = -0.992 红松树皮的分解模型近似于直线:Y = 0.5258 - 0.01133 X r = -0.984 落叶松,红松,色木,桦树的分解常数分别为:0.01783, 0.0.41, 0.0782, 0.1139。依此预测分解原密度的95%所需要的时间分别为:168年,87.6年,38.3年,26年。可以看出这四个树种分解从难到易的顺序为:落叶松 > 红松 > 色木 > 桦树。对枝桠密度的差民显著性检验可以说明:红松样品层次对分解的影响显著而径级对分解的影响仅在下层显著。随着分解的进行,样品的重量损失,我们也探讨了密度的降低与失重百分率之间的关系。桦树样品下层失重比上层快,说明淋溶作用对桦树样品失重的贡献不大。温湿度是影响分解的最主要的生态因子。枝桠堆上下层的湿度差异特别明显。分解时间越长,径级对含水量的影响越显著。水分含量(Y:%)随年代(X: yr)变化的趋势为:Y = 36.18 - 0.004337 X~2 (4-7cm径级)Y = 33.64 - 0.01097 X~2 (1-4cm径级) 温,湿度影响土壤动物及微生物种群分布及数量,进而影响到枝桠的分解速率,分解过程中元素动态变化是:C基本上恒定,全N含量趋于增高。径级对红松N的累积有影响。下层4-6cm径极累积最快,其次是上层4-6cm。层次的影响仅限于红松,除72年以外上层 > 下层。其它元素如P, Mg++, Ca++总的趋势是随分解过程而增加。土壤中的C元素含量受立地条件的影响,但是枝桠堆下面土壤C值高于对照。枝桠堆对森林更新和火灾均有影响。枝桠是林火的燃料,枝桠堆面积占采伐迹地的11.53%,这样减少更新面积。
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本学位论文分为四个部分,第一部分报道了用串联质谱快速分析合成药物中的微量杂质成分以及分析中药材中的化学成分。第二部分报道了通过质谱和串联质谱发现并合成新型的PdPincer 催化剂,同时对其活性进行测试。第三部分为串联质谱自动解析软件的设计及应用。第四部分概述了应用在质谱中的各种碎裂方式。 第一部分首先总结了5-溴粉防己碱及其类似物的裂解规律,并以此为根据推测出2 个微量杂质的结构。随后针对无患子(Sapindus mukurossi Gatren.)中的皂苷成分,由ESI-QTOF 得到各个皂苷成份的高分辨质量数据进而得到其分子式,然后利用ESI-IT 电喷雾串联质谱对无患子总皂苷中各皂苷成分的结构进行进一步的鉴定。进而以同样的方式,先通过ESI-QTOF 得到黄山药(Dioscoreapanthaica)总皂苷中各个组分化合物的分子式,然后对已有的薯蓣皂苷标准品做串联质谱分析,以得到该类化合物的裂解规律并给出解析该类化合物的流程图。在此利用计算化学的方法讨论了离子的丰度与裂解活化能之间的关系。然后应用APCI-MS/MS 方法探讨了四对同分异构体和几个已知的化合物,并最后用液质联用对其进行确认,同时还给出了4 个未知化合物的可能结构。 第二部分报道通过质谱和串联质谱发现并合成新型的PdPincer 催化剂,同时对其活性进行测试。钯催化的交联反应是有机合成中C-C 键形成的最有效的方法,且硫脲是一类对空气和水都稳定的化合物,因此我们设计并合成了一系列的硫脲钯催化剂并得到了很好的催化活性。我们在对其中一类环状双硫脲化合物进行质谱实验的时候,在正离子模式下发现了反常的[M.H]+,通过串联质谱进一步确定了它是一种新型的PdPincer 结构。我们将其合成出来并通过X-ray 衍射实验确定了它的结构。同时测定其催化活性并与未形成pincer 的类似物进行比较发现该类化合物具有较宽的底物适用性。 第三部分为串联质谱自动解析软件的设计及应用。通过前面两部分的启示,独立设计开发了AuMass(1.0)。其算法是:先通过查找特殊的碎片离子,中性丢失或碎片离子质量差来确定某类化合物的骨架结构,然后利用该类化合物的自动解析流程来对其周边取代基进行确认。通过它快速地对白芍中的化学成分进行解析,并对未知的化合物进行了推测。为了增加它的解析能力,我又对其它类型的化合物裂解规律进行总结,并给出了自动解析流程。实践证明该软件具有相当好的应用价值。 第四部分综述了应用在质谱上的各类母离子的碎裂技术。这里包括了碰撞诱导裂解(CID)、光诱导碎裂(LID)、电子捕获裂解/电子转移裂解(ECD/ETD)、红外多光子解离(IRMPD)、黑体辐射解离(BIRD)和PQD 裂解技术。 This dissertation consists of four chapters. The first chapter reports the rapidanalysis of trace impurities from synthetical medicine and analysis of the chemicalconstitutents from Chinese herb medicines. The second chapter elaborates the studieson the discorvery and synthesis of new type of Pd Pincer catalyst by using MS andtandem MS together with the testing of its catalyst activity. The third chapter dwellson the designation and development of automatic tandem mass spectrometry analysissoftware. The last chapter presents a review on the dissociation technique of massspectrometry. The first chapter reports the rapid analysis of trace impurities from synthesismedicine and analysis of the chemical constitutents from Chinese herb medicines. The fission mechanism of 5-bromotetrandrine was obtained by analysis of the dissociationpathways of major product, by using which the possible structure of the two traceimpurties was assumed. There are lots of saponins in Sapindus mukurossi. Except forthe good spumescence and decontamination,it possesses the bioactivity of antigenand antitch. First of all, the high resolution mass information was obtained by ESI-QTOF. Hence the possible molecular formulars were acquired too. Then weconducted the further detection of the structures of its saponins by using ESI-ITtechnology. In the same manner, first the molecular formulars of every constituentfrom Dioscorea panthaica in total saponins were obtained by ESI-QTOF, and thenacquired the fission mechanism of this type of compounds by tandem massexperiment on a series of known and available saponins. In the same time, theanalysis flowchart was concluded. Here the relationship between the ion intensity andthe corresponding dissiociation activation energy was studied by computer chemistry.Then the four pairs of isomers were differentiated by APCI-MS/MS, as well as thecharacterization of known and unknown compounds. The assumption was confirmed by HPLC-MS/MS. Among them the possible structures of four unknown saponinswas presented. The second part was discovery and synthesis of a new type of Pd pincer catalystby MS and tandem MS. The coupling reaction catalyzed by Pd is the most effectivemethod in C-C formation in organic synthesis. Apart from that, thiourea is type ofcompounds that are stable to atmosphere and moisture. Hence we designed a series ofPd thiourea catalysts. Some of them show the excellent catalyst activity. The abnormalparent ion [M.H]+ was founded in positive ESI mode when we conduct some massspectrometry experiments on the bicyclical thiourea Pd complex. The structure wasproposed by mass and tandem mass spectrometry. Because it was a new type of pincer,we want to test its catalyst activity. So the Pd pincer was synthesized and the detailstructure was obtained by x-ray experiment. It shows the more fitness in catalysis ofSuzuki reaction by comparison with the analogue. The third chapter dwells on the design and development of automatic tandemmass spectrometry analysis software. Inspired by the former two chapters, theAuMass (version 1.0) was developed. Its algorithm is: first check the diagnostic ion,diagnostic neutral loss or diagnostic ions mass intervals in database to find out whatthe analyst’s skeleton belongs to, then identify the peripheral functional group by thecorresponding analysis flowchart. The chemical constituents of Paeonia lactiflorawere identified rapidly by using AuMass. To increase the analysis ability, the othertypes of compounds from Chinese herbs was concluded. Actually, the software isproven to have the much valuable application. The last chapter presented the review on the some kinds of fission technique ofmass spectrometry. It involves the collision induced dissociation (CID), laser induceddissociation (LID), electron capture dissociation/electron transfer dissociation(ECD/ETD), infrared multiple photons dissiociation, black body irraditiondissociation and PQD fission technique from Finnigan.