可X射线显影的新型碘代聚碳酸酯的设计与合成

以丝氨醇、 4-碘苯甲酰氯和氯甲酸乙酯为原料, 通过酰胺化和分子内关环两步反应合成了一种新型的碘代环碳酸酯功能单体——4-碘-N-(2-氧代-1,3-二噁烷-5-基)苯甲酰胺(IBTMC). 以异戊醇为引发剂, 1,5,7-三叠氮双环(4.4.0)癸-5-烯(TBD)为催化剂, 使IBTMC与三亚甲基碳酸酯(TMC)进行开环共聚, 合成了一系列具有X射线不透过性的碘代聚碳酸酯材料, 并采用核磁共振氢谱( ¹H NMR)、 凝胶渗透色谱(GPC)、 差示扫描量热仪(DSC)、 热重分析(TGA)和X射线计算机断层成像系统(Micro-CT)表征了其化学结构与组成、 分子量与分子量分布、 热力学性能及X射线不透过性. 研究结果表明, 本文合成的碘代聚碳酸酯具有较窄的分子量分布、 良好的热稳定性及可调的X射线不透过性. 小鼠体内埋置实验结果表明, 碘代聚碳酸酯具备体内X射线成像的能力.     

多晶X射线衍射技术与应用

正本书系统地介绍了多晶X射线衍射技术的原理、仪器、方法和应用。全书内容循序渐进,在介绍X射线的物理基础、射线强度检测技术及其发展、晶体和晶体衍射的理论知识基础上,着重阐述了X射线衍射仪器和多晶衍射仪的原理,详细论述了如何获得正确的衍射数据、如何评估衍射实验数据的可信度以及仪     

《多晶X射线衍射技术与应用》

本书系统地介绍了多晶X射线衍射技术的原理、仪器、方法和应用。全书内容循序渐进,在介绍X射线的物理基础、射线强度检测技术及其发展、晶体和晶体衍射的理论知识基础上,着重阐述了X射线衍射仪器和多晶衍射仪的原理,详细论述了如何获得正确的衍射数据、如何评估衍射实验数据的可信度以及仪器的工作状态等实验技术问题。之后,又     

波长色散X射线荧光光谱仪和多晶X射线衍射仪联用技术鉴定进口铜矿和含铜物料

首次研究进口可利用含铜物料与进口铜矿属性的不同特性并建立了鉴定方法,采用X射线荧光光谱法和X射线衍射光谱法联用技术建立铜矿和含铜物料属性的鉴别方法。通过X射线荧光光谱法对铜矿和含铜物料中元素进行定性半定量分析,再用X射线衍射光谱法对铜矿和含铜物料的特征谱峰进行扫描,与X射线衍射仪中标准卡片比对分析,能够确定铜矿和含铜物料的物相组成。结果显示,X射线荧光光谱法测定的铜矿和含铜物料的共同特点是铜的含量较高,达到冶炼铜对原料的要求;硅、铁、钠、钙和镁元素都能够检出;差异性在铅和锌元素在含铜物料中较高,在铜矿石中基本未检出;用X射线荧光光谱法检测出的金属元素,通过X射线衍射仪扫描后与标准图片比对,各元素以不同的形式存在于含铜物料中,且有规律可循。     

高通量研磨-X射线荧光光谱法测定不同植源性食品中硒含量北大核心

为了提高食品的样品检验效率,采用高通量研磨制备样品,利用X射线荧光光谱法对食品中硒含量进行检测。重点研究了样品含水率、样品颗粒粒径、研磨条件、检测条件等因素对检测结果的影响。结果表明:样品干基含水量小于20%,样品颗粒粒径小于100μm;高通量研磨条件为装样量3 g,频率30 Hz,研磨3 min;高精度X射线荧光光谱仪检测条件为检装样量0.2 g,PP膜压紧,检测90 s时的情况下,硒的检出限0.01 mg/kg,仪器的精密度小于5%,与粉碎法进行对比,相对偏差在-10.37%~8.05%。说明高通量研磨-X射线荧光光谱法检测食品中硒含量的方法快速、准确,可以满足批量样品现场检测分析需求。     

X射线衍射仪仿真实验教学平台的设计与应用

X射线衍射仪测试实验课受学时和射线装置的限制，学生难以理解仪器的结构、工作原理和工作过程，影响实验教学效果。为了提高实验教学质量，做到学以致用，以Unity3D和Java Web为基础设计开发了X射线衍射仪仿真实验教学平台。学生既可以在该平台在线演示测试过程和学习X射线衍射仪工作原理，又可以通过该平台的在线考试系统了解自己对相关知识的掌握情况。该平台的使用不仅丰富了X射线衍射仪测试实验教学的手段和评价体系，而且还有效提升了学生对科研的兴趣和实验动手能力。     

铌酸盐 Ba3 NaBiNb10 O30的 X射线衍射与光电子能谱分析

在BaO-Na2O-Bi2O3-Nb2O5四元系统中,用固相反应法合成了钨青铜矿型结构铌酸盐Ba3NaBiNb10O30;对样品进行了X射线衍射（XRD）与X射线光电子能谱（XPS）分析,获得了铌酸盐Ba3NaBiNb10O30的特征X射线衍射数据,确定了其中Nb元素的价态与结合能数据。     

同步辐射及相关核分析技术在纳米材料生物效应研究中的应用

伴随纳米技术的发展,纳米材料的生物效应研究成为热点,然而这一新兴的研究领域对传统的研究方法提出了挑战,其深入研究有赖于方法学的发展。同步辐射是具有高亮度、高准直、宽频谱等优异性质的光源,其在元素分析及物质原子或分子尺度的结构表征方面具有独特的优势。本文介绍了同步辐射及相关核分析技术,主要包括同步辐射X荧光分析、同步辐射X射线吸收光谱(扩展X射线吸收精细结构EXAFS,X射线吸收近边结构XANES)、同步辐射圆二色谱、电感耦合等离子体质谱、中子活化分析、同位素示踪技术等在纳米生物效应研究中的应用,结合本实验室以及国内外的研究工作详细阐述了基于同步辐射以及相关核分析方法应用于纳米材料表征及其在生物体内的定量、分布、结构分析等方面的最新进展。     

X射线晶体学在高等教育中的通识性

X射线晶体学是一门研究物质晶体结构的科学,X射线衍射技术已成为当今化学、材料、生命等众多科学领域中对物质结构研究的必要手段与方法。本文从X射线晶体学的诞生、发展和迅速普及的角度,谈谈X射线晶体学的发展历程对人类文明的贡献,以及X射线晶体学在当今高等教育中的重要性,从而阐述在高等学校通识教育中加强与推广X射线晶体学的必要性与可行性。     

X射线成像技术在能源材料研究中的应用

随着人类对可持续能源的需求不断增长,先进的表征方法在能源材料研究等领域变得越来越重要。借助X射线成像技术,我们可以从二维和三维角度实时获取能源材料的形貌、结构和应力变化信息。此外,借助高穿透性X射线和高亮度同步辐射源,设计原位实验,可以获取充放电过程中样品的定性和定量变化信息。本文综述了基于同步加速器的X射线成像技术及其相关应用,讨论了包括X射线投影成像、透射式X射线显微成像、扫描透射X射线显微成像、X射线荧光显微成像以及相干衍射成像等几种主要的X射线成像技术在能源材料研究领域的应用,展望了未来X射线成像的应用前景及发展方向。     

Rapid method of uranium determination in solutions based on X-ray fluorescence and absorption

A method of uranium determination in organic and aqueous solutions has been developed, based on fluorescence L X-ray excitation with a¹⁰⁹Cd source of several mCi activity and counting the excited L_α lines with a proportional counter. To eliminate uranium X-ray absorption by the accompanying elements the intensity of the source radiation (Ag K) transmitted through the analysed solution is measured. The ratio of these two intensities is independent of other elements present in the solution over a very broad range of concentration. The analysis time does not exceed 5 minutes. The precision and accuracy of this method in the range 0.5 to 100 g U/1 are comparable to those of the classical titrimetric method.     

Two-photon fluorescent probe for cadmium imaging in cells

A novel two-photon excited fluorescent probe for cadmium (named as TPCd) was designed and synthesized utilizing a prodan (6-acetyl-2-methoxynaphthalene) derivative as the two-photon fluorophore and an o-phenylenediamine derivative as the Cd(2+) chelator, which possessed favorable photophysical properties and good water-solubility. The probe was designed with a photoinduced electron transfer (PET) mechanism and thus was weakly fluorescent itself. After binding with Cd(2+) which blocked the PET process, the fluorescence intensity of the probe was enhanced by up to 15-fold under one-photon excitation (OPE) and 27-fold under two-photon excitation (TPE), respectively. The two-photon action cross-section (Φδ) of the TPCd-Cd complex at 740 nm reached 109 GM compared to 3.6 GM for free TPCd, indicating the promising prospect of the probe in two-photon application. TPCd chelated Cd(2+) with 1 : 1 stoichiometry, and the apparent dissociation constant (K(d)) was 6.1 × 10(-5) M for the one-photon mode and 7.2 × 10(-5) M for the two-photon mode. The probe responded to Cd(2+) over a wide linear range from 0.1 to 30 μM with a detection limit of 0.04 μM. High selectivity of the probe towards Cd(2+) was acquired in Tris-HCl/sodium phosphate buffer. The probe was pH-independent in the biologically relevant pH range and non-toxic to living cells at reasonable concentration levels, warranting its in vivo applications. Through two-photon microscopy imaging, the probe was successfully applied to detect Cd(2+) uptake in living HepG2 cells.     

Determination of iron and titanium in kaolins by the method of non-dispersive X-ray fluorescence

The possibility of application of the radioactive source excited X-ray fluorescence analysis for titanium and iron determination in kaolins to the routine test of the refinement process has been studied. The iron content can be determined with a simple counting system using a single-channel pulse height analyser, argon filled proportional counter and¹⁰⁹Cd source of 3 mCi for the excitation of K Fe rays. The samples were analysed both as pellets and powders. The iron content ranged from 0.2–2.5% and titanium from 0.1–0.64%. For simultaneous determination of titanium and iron a Si(Li) spectrometer has been used. The²³⁸Pu source has been used for K Fe and K Ti excitation. It is the most convenient source for simultaneous determination of titanium and iron.⁵⁵Fe is the most efficient source for the determination of titanium alone. The best values of precision and determination limit have been achieved for iron with²³⁸Pu and for titanium with⁵⁵Fe.     

A theoretical and experimental investigation of the source-sample-detector geometry for an annular type radioisotope excited XRF spectrometer

In this study, the dependence of the characteristic X-ray intensities on the counting geometry has been investigated for a radioisotope excited XRF spectrometer. The collimation factor for the source-sample-detector geometry, which was prepared for an annular type¹⁰⁹Cd radioisotope source, has been determined both theoretically and experimentally. The discrepancy between the theoretical and experimental results is discussed in terms of possible sources of errors.     

Sorption behavior of hydroxyapatite for 109Cd(II) as a function of environmental conditions

In this work, hydroxyapatite (HAP) was prepared by aqueous precipitation technique and was characterized by using FT-IR to determine its chemical functional groups. A series of batch experiments were carried out to investigate the effect of various environmental factors such as contact time, pH, ionic strength, foreign ions, fulvic acid (FA) and temperature on the sorption behavior of HAP towards radionuclide ¹⁰⁹Cd(II). The results indicated that the sorption of ¹⁰⁹Cd(II) on HAP was strongly dependent on pH and ionic strength. A positive effect of FA on ¹⁰⁹Cd(II) sorption was found at pH <7.0, whereas a negative effect was observed at pH >7.0. The Langmuir, Freundlich and D-R models were used to simulate the sorption isotherms at three different temperatures of 298.15, 323.15 and 343.15 K. The thermodynamic parameters (ΔH⁰, ΔS⁰ and ΔG⁰) calculated from the temperature dependent sorption isotherms indicated that the sorption process of ¹⁰⁹Cd(II) on HAP was spontaneous and endothermic. At low pH, the sorption of ¹⁰⁹Cd(II) was dominated by outer-sphere surface complexation and ion exchange on HAP surfaces, whereas inner-sphere surface complexation was the main sorption mechanism at high pH. From the experimental results, it is possible to conclude that HAP has good potentialities for cost-effective treatments of ¹⁰⁹Cd(II)-contaminated wastewaters.     

Possibilities of ED-XRF with radionuclide sources for analysis of plants

A comparative evaluation of the applicability of different radionuclide sources for the determination of toxic elements in plants by ED-XRF is presented.²³⁸Pu or¹⁰⁹Cd are suggested as most suitable single excitation sources in ED-XRF for monitoring investigations. More elements are determined with a combination of⁵⁵F/¹⁰⁹Cd(²³⁸Pu)/²⁴¹Am. The results obtained by radionuclide ED-XRF analysis of different plants show that the method permits the reliable determination of Br, Ca, Fe, K, Mn, Rb, Sr and Zn in plant bioindicators. For toxic elements like As, Cd, Cu Cr, Hg, Ni, Se and Pb the detection limits of the method are not low enough.     

Separation of the no-carrier-added 109Cd from Ag, Cu and 65Zn by use of a precipitation and AG1-X8 resin

The ¹⁰⁹Cd radionuclide was produced in the cyclotron via ^natAg(p,n)¹⁰⁹Cd reaction. The radiochemical separation of ¹⁰⁹Cd from silver and non-isotopic impurities comprised of two stages. The optimum conditions of the ¹⁰⁹Cd separation methods were: Ag precipitation with 0.015 M HCl and Cu and ⁶⁵Zn by use of 0.015 M HCl on AG1-X8 strong anion-exchange resin. Chemical and radionuclidic purity of ¹⁰⁹Cd were measured by ICP-AES and gamma-ray spectrometry respectively. Recovery yield and radionuclidic purity were obtained 99.7% and 99%, respectively.     

Solvent extraction of Cd(II) with N-cyclohexyl-N-nitrosohydroxylamine and 4-methylpyridine into methyl isobutyl ketone

The distribution equilibria of the complexes cadmium-cnha and cadmium-cnha-4-methylpyridine in the water-methyl isobutyl ketone system have been studied at 25 degrees , by using (109)Cd as a radiotracer to measure the metal distribution ratio. A very sensitive method for detection of (109)Cd, based on the use of a liquid scintillator, has been developed. From the graphical treatment of the equilibrium data, it has been deduced that CdL(2) is the complex extracted in the absence of 4-methylpyridine, and that the adduct CdL(2)B is extracted when the second ligand is present. This model has been checked by treating the data with the program LETAGROP-DISTR and the following equilibrium constants have been obtained: stability constants of CdL(2), log beta(1) = 2.82 +/- 0.14, log beta(2) = 5.981 +/- 0.004; distribution constant of CdL(2), log K(DC) = -0.49 +/- 0.01; adduct formation constant of CdL(2)B, log K(s) = 2.70 +/- 0.07.     

Quantitative Model for the Surface-related Electron Transfer in CdS Quantum Dots

The influence of surface S2- dangling bonds and surface doped ions(Se2-, Cu2+, and Hg2+) on the photo-luminescence of Cd2+-rich CdS QDs was investigated. A quantitative model was proposed to understand the complex transfer processes of excited electrons in CdS QDs. The transfer of excited electrons from either the conduction band or the Cd2+-related trap-state to the surface S2+-related shallow hole trap-state is effective. However, the trap of excited electrons by surface doped ion trap-states from the Cd2+-related trap-state is more effective than that from the conduction band. The efficiency of trapping electrons from both the conduction band and the Cd2+-related trap-state can be quantitatively understood with the help of the proposed model. The results show that the transfer efficiency of excited electrons is dependent on the location of the energy-level of the relevant surface-related trap-state. The trap of excited electrons by the surface trap-state with energy-level closer to that of the conduction band is more effective, especially for the trap of excited electrons from Cd2+-related trap-state.     

Determination of yttrium in xenotime ore by energy dispersive X-ray fluorescence spectrometry

A radioisotope-excited X-ray fluorescence analysis is applied for the determination of yttrium in xenotime ore. An annular¹⁰⁹Cd source is employed for excitation of characteristic K X-rays of yttrium. The dilution method using pure starch as a diluent has been examined. Critical thickness of diluted ore sample has been determined. For the estimation of yttrium concentration in xenotime ore, the scattered radiation technique has been utilized. The validity and precision of the method have also been investigated.