膨润土有机改性的FTIR和XRD研究

研究内容是制备有机膨润土以提高膨润土与有机相的相容性,同时观察膨润土的层状结构在有机化前后的变化情况。以钠基膨润土为原料,并用十八胺试剂作为有机插层剂取代膨润土层间的Na+,制得有机膨润土,且对其结构进行表征。FTIR和DTA-TG都证明有机插层剂已进入膨润土的层间;XRD表明膨润土的层间距由1.4增大到4.3 nm;从实验结果可知,钠化膨润土在各种指标上都比原钙基膨润土有显著的改善,如吸蓝量、膨胀容、胶质价、阳离子交换容量等。改性后的膨润土使其晶片层间的亲水环境改变为疏水环境以及增大晶片层间距离,从而有利于制备综合性能较好的复合材料。     

XRD和FTIR对沸石合成机制的光谱学解析

以粉煤灰为原料,采用优化的水热晶化一步法合成沸石。比较晶化反应过程沸石产物CEC值及化学成分的变化,推断固液体系中物质转换及元素迁移方式和途径。借助XRD,SEM,FTIR等表征反应过程沸石的晶型变化及成核特性,提出可能存在的沸石生成机制。合成产物主要为NaP1型沸石,反应24h后CEC值最大为135mmol/100g。12h后,产物中初步发现NaP1沸石相特征峰和亚晶结构,48h后出现羟基方钠石的特征弱峰。沸石生成过程涉及到固液体系间的物质流动:碱熔融作用将粉煤灰组分侵蚀进入液相体系,为沸石形成提供了原料组分,而固相体系为沸石生长提供骨架结构,液相体系和固相体系分别为晶化反应的"源"和"汇",这是液相转化机制和固相转化机制的客观反映。     

苯甲酰胺对高岭石插层的FTIR和XRD研究

苯甲酰胺在熔融状态下取代前驱体中的DMSO分子插层高岭石,产物经丙酮洗涤,得到纯净的高岭石/苯甲酰胺插层复合物。XRD结果显示高岭石层间距从0.717 nm膨胀到1.437 nm。插层作用使高岭石内表面羟基红外伸缩振动峰由3 696和3 657 cm-1移动至3 701和3 651 cm-1处;苯甲酰胺3 368和3 172 cm-1处NH₂基伸缩振动峰红移至3 474和3 184 cm-1处,1 659 cm-1处羰基峰移至1 640 cm-1处,这些表明原高岭石层间氢键的损失及与苯甲酰胺分子之间氢键的形成。插层反应于30 min迅速达到平衡,插层率随反应温度的增加先增加后减小,180 ℃时有最大插层率;以丙酮作为洗涤剂可以消除表面吸附和残余的苯甲酰胺晶体而不影响复合物的结构。     

交联淀粉微球酶降解过程的FTIR和XRD分析

以可溶性淀粉为原料,N,N′-亚甲基双丙烯酰胺为交联剂,采用反相悬浮聚合得到了一种交联淀粉微球(CSM)。为了深入了解交联淀粉微球(CSM)的降解过程,利用傅里叶变换红外光谱(FTIR)和X射线粉末衍射(XRD) 等光谱分析手段,对可溶性淀粉、CSM及其CSM在模拟肠液中不同时间的降解产物进行了分析。FTIR和SEM的研究结果表明, CSM在消化液中3 h内可稳定维持其交联结构,降解后3和12 h之间1 090 cm-1处的C—O—C弯曲振动峰减弱,酰胺的Ⅰ带吸收峰和Ⅱ带吸收峰强度的减弱说明了淀粉分子链被降解, 交联结构开始解聚,12 h后酰胺的Ⅰ带吸收峰和Ⅱ带吸收峰完全消失,说明交联结构已完全被除去;XRD结果表明,CSM在消化液中降解12 h后的情况与可溶性淀粉的降解情况相似,非结晶性部分被分解,结晶度随降解过程的进行而提高,但是仍然小于可溶性淀粉的结晶度。     

FTIR和XRD在断层构造煤结构分析中的应用

为探究断层构造作用对煤化学结构特征和微晶结构特征的影响,采用傅里叶变换红外光谱(FTIR)和X射线衍射(XRD)分析,对红庆梁矿和段王矿的原生煤及断层构造煤进行分析。结果表明,受断层构造作用影响,红庆梁、段王断层构造煤中苯环二取代、苯环四取代的含量明显大于原生煤,苯环三取代和苯环五取代的含量低于原生煤,断层构造煤中C—O—C伸缩振动、—CH₂反对称弯曲振动、—CH₃、—CH₂和芳环—OH含量均多于原生煤,断层构造煤中醚C—O振动、芳烃CC、—CH和OH—π含量低于原生煤。红庆梁、段王断层构造煤的芳碳率f_a是原生煤的1.01和1.03倍,芳环缩合度DOC是原生煤的1.01倍和3.7倍,CH₂/CH₃值是原生煤样的0.933倍和0.94倍,芳香度I分别是原生煤样的1.01倍和1.34倍。说明断层构造作用促使官能团和脂肪链脱落,增加煤的缩聚程度,降低煤中脂肪侧链的长度,增大芳香结构含量。XRD测试结果表明,原生煤和断层构造煤具有相近的矿物组分,断层构造作用未对煤...     

掺稀土元素Dy和Mn,P,Cu的MgSO4的热释发光光谱

实验测定了MgSO4:Dy,Mn和MgSO4:Dy,P以及MgSO4:Dy,P,Cu等的热释光磷光体的三维发光谱.结果表明,掺入Dy的MgSO4磷光体的热释发光谱线的波长与Dy3+离子的能级跃迁相关,Dy3+为热释光主要发光中心.MgSO4中只掺入Mn时,温度在140℃和190℃附近呈现波长为660nm宽范围的连续发光带,这是Mn形成的发光中心的光谱.当MgSO4中同时掺入Dy和Mn时,660nm的Mn发光带和低于300℃的Dy3+离子的发光谱强度均受到抑制,出现了波长为480nm和580nm峰温在380℃的主发光峰.这表明原MgSO4:Dy的360℃发光峰向高温方向移动了约20℃,Dy3+仍为热释光主要的发光中心,Mn则主要起能量转移的作用.MgSO4:Dy,P热释光三维发光谱可看出,P掺入使MgSO4:Dy的260℃发光峰移至283℃,并且强度大大增加,原360℃发光峰的峰温基本不变.当MgSO4:Dy,P中同时掺入Cu时,主要发光峰的峰温仍在283℃,但360℃发光峰的强度被抑制,480nm和580nm的发光峰的相对强度发生了变化.因此,Dy3+仍是热释光主要的发光中心,P和Cu参与形成新的俘获中心.     

龙岩高岭土的苯乙烯原位聚合插层的FTIR和XRD研究

以福建龙岩高岭土为主要原料,用沉降的方法得到平均粒径为1.75μm的沉降高岭土。用DMSO插层高岭土,后用苯乙烯单体取代前驱体中的DMSO分子,产物经四氯化碳洗涤后,在马弗炉中270℃本体聚合2h得到高岭土/聚苯乙烯复合物。红外在1 453,1 499和1 606cm-1的吸收振动峰证明了聚苯乙烯的存在。XRD结果显示高岭土层间距0.712nm,苯乙烯聚合后片状结构已经被剥离。热重显示聚苯乙烯占复合物质量的40%,还有约5%的未除去DMSO和4.8%的羟基,估算出高岭土∶聚苯乙烯=1.375∶1(质量比)。扫描电镜也验证了这种剥离。     

基于FTIR和XRD的降低连铸保护渣红外辐射传热研究

根据常用工业保护渣的成分范围配制出含有TiO2的连铸结晶器保护渣,通过实验检测并分析了渣样FTIR光谱及X射线衍射图谱,探讨了熔渣辐射传热特性随TiO2变化的规律.FTIR分析结果表明,在1～6 μm波段范围内,TiO2具有明显降低渣膜红外透过率的作用.X射线衍射结果表明渣中枪晶石的含量减少,析出CaTiO3等晶体,枪晶石的大量减少有利于铸坯的润滑.通过辐射传热模型计算得到铸坯与结晶器之间的辐射热流密度.TiO2的加入使渣样热流密度大为降低,并随其含量增加而降低,最高达30%.由于试样表面及晶界强烈的折射和散射,结晶态试样对辐射传热的降低作用比玻璃态试样更明显.     

掺稀土元素Dy和Mn,P,Cu的MgSO4的热释发光光谱

实验测定了MgSO₄:Dy,Mn和MgSO₄:Dy,P以及MgSO₄:Dy,P ,Cu等的热释光磷光体的三维发光谱.结果表明,掺入Dy的MgSO₄磷光体的热释发 光谱线的波长与Dy³⁺离子的能级跃迁相关,Dy³⁺为热释光主要发光 中心.MgSO₄中只掺入Mn时,温度在140℃和190℃附近呈现波长为660nm宽范围的 连续发光带,这是Mn形成的发光中心的 关键词： 热释发光光谱 稀土元素镝 硫酸镁     

FTIR和XRD研究甲酰胺在高岭石插层复合体系中的形态及其复合物的微观结构

插层复合体系中,有机插层剂在插层的同时也可能吸附在复合物的表面或以自由态存在,对插层分子的表征将会产生较大的影响。以丙酮作淋洗剂,用FTIR及XRD技术对淋洗前后的插层复合体系监控,插层剂分子在复合体系中的可能存在形式,探讨水的作用及复合物微观结构的变化。结果显示：甲酰胺有插层、游离和吸附在复合物表面三种存在形态。3 355和3 462 cm-1处的红外振动峰归属于表面吸附的插层剂分子,3 626 cm-1的峰归属于插层的H₂O分子,在干燥后均消失。H₂O作为填充空间的分子参预了插层过程,且插入到层间,并在干燥后脱嵌。3 534 cm-1处的振动峰在淋洗前后一直存在,是由于插层的甲酰胺分子与高岭石层间形成氢键作用的结果。以丙酮作为淋洗剂,可以选择性的消除表面吸附的甲酰胺而不影响复合物的结构。插层的甲酰胺分子以C—N键垂直于层片呈单分子层排列,并通过氨基与高岭石铝氧八面体层的内表面羟基和硅氧四面体层的氧形成了两种氢键作用。     

EDXRF,FTIR, and XRD characterization of low calcium oxalate urinary stones collected from arid area

Low calcium oxalate urinary stones from the kidney, bladder, and ureter have been collected from the arid area (Taif, Saudi Arabia). After careful washing and drying of the collected stones, the samples were converted into a contamination-free homogenous fine powder with a particles' size smaller than 50 μm. The processed urinary stone powders were studied using attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR), laboratory setup and synchrotron radiation X-ray diffraction (XRD), and energy-dispersive X-ray fluorescence (EDXRF). The activated function groups, quantitative phase analysis, and the semi-quantitative elemental analysis of the present urinary stones were identified. Seventeen elements were measured in most of the urinary stone samples. The significant elements are Ca, P, S, Cl, Zn, K, Fe, and Cu, whereas other elements were found alternatively in a few number of urinary stone samples. It was recognized that Ca exists with low concentration, which indicates the presence of different calcium phases even with low percentages. In 33% of the urinary stones, the phosphorus (P) was not measured, but there were high concentrations of sulfur (S) and low concentrations of Ca up to 2.15 ± 0.05%. The ATR-FTIR results indicate that the most compounds of the present urinary stones were urea and cystine combined with low ratios of calcium oxalate and calcium phosphate compounds. The quantitative phase analysis of the XRD of selected samples proves the presence of the cystine, urea, and calcium oxalate phases with different weight percent.     

A study of thermoluminescence emission spectra and optical stimulation spectra of quartz from different provenances

The present study examines (1) variability in the thermoluminescence (TL) emission spectrum and optical stimulation (OSL) spectrum of quartz from different provenances and, (2) possible correlations between spectral features and the nature of the complex growth curves (ranging from saturating exponential to those described by a cubic polynomial function), so as to determine the validity of the currently used experimental protocols. The results suggest that commonly used UV emission for dating constitutes only a minor component of the total quartz emission and in view of this a dose-dependent contribution from blue/blue–green emission peak to the UV detection is likely. The OSL stimulation spectrum shows a definite change in stimulation response between 500–520 nm, hence implying that stimulation in this window may contribute as an additional source of scatter in multi-grain samples.     

N-乙酰化壳聚糖的FTIR和XRD研究

壳聚糖分子的脱乙酰度(DD)是影响壳聚糖性质的主要因素之一。文章通过壳聚糖的N-乙酰化反应制备了不同脱乙酰度的壳聚糖。采用傅里叶变换红外光谱(FTIR)和X射线衍射(XRD)分别研究了由N-乙酰化反应得到的不同脱乙酰度的壳聚糖的红外光谱特性和晶体结构,并由此分别计算确定了样品的脱乙酰度和结晶度,探讨了N-乙酰化程度对壳聚糖脱乙酰度以及结晶度的影响。 由FTIR可知,随N-乙酰程度的增加,壳聚糖分子中剩余氨基的反应速度变慢。另外XRD也表明,伴随N-乙酰反应,壳聚糖分子的结晶区被破坏,规整度下降,并逐渐形成新的结晶区。     

Thermoluminescence and thermoluminescence spectra of synthetic fluorapatite

On account of their fairly long life, alkaline earth halophosphate phosphors are still the mainstay of the fluorescent lamp industry. For higher efficiency and an increased selection of spectral distribution, with minor variation in composition and dopants, halophosphates are synthesised nowadays. It is not surprising, therefore, that these synthesised apatite phosphors are still attracting the attention of the research workers too. In this paper the results of TL and TL spectra of X-irradiated synthetic fluorapatite are reported with a view to understand the nature of the recombination processes in the system, vis-à-vis the defects created by irradiation. Such studies are ultimately aimed at unravelling the causes for the fatigue and quantum efficiency changes that are occuring at present in such phosphors.     

不同地理居群大蒜FTIR图谱比较研究

为了比较不同地理居群大蒜的理化性质差异,以25份不同地理居群的大蒜为研究对象,采用傅里叶变换红外光谱仪获取各样品的FTIR图谱,利用光谱仪随机软件中的"快速比较"功能进行了不同地理居群大蒜的相似度比较.结果发现,不同地理居群大蒜的FTIR图谱存在差异,快速比较显示其相似度为76.3%～99.8%,呈现出较为明显的多样性...     

Dose response of thermoluminescence emission spectra of LiF:Mg,Ti with different Mg, Ti impurity concentrations

The dose response of the TL emission spectra of an LiF:Mg,Ti (TLD-100) sample and three LiF:Mg,Ti samples with different impurity concentrations (0–6 ppm Ti and 80–100 ppm Mg) have been measured. At a dose less than 22 Gy the emission spectrum of the TLD-100 sample comprises one emission band at 420 nm. The sample without Ti shows also one emission band but now at 620 nm. The spectra of the other two samples comprises two emission bands at 420 nm and 620 nm of which the intensity of the 420 nm band increases with increasing Ti concentration. The dose response of the glow peaks is different for peaks at different temperatures and emission bands. From these observations it can be concluded than in LiF:Mg,Ti at least some of the traps and luminescent centers are coupled.     

UV excitation spectra of thermoluminescence in quartz

Thermoluminescence was excited at 300 K in natural quartz crystals by monochromatic ultraviolet radiation. The excitation spectra of the main glow peaks were measured in the spectral region 1150–2000 Å. A strong excitation maximum appeared for all measured glow peaks in the region of high absorbance on the long wavelength tail of a sharp reflectance peak at 1275 Å. Some glow peaks showed excitation maxima also at photon energies smaller than the absorption edge of the material. The dependence of the TL intensities on the dose of the exciting radiation was investigated for various glow peaks and excitation wavelengths. A sublinear dependence was recorded for some peaks by excitation at 1275 Å, while the same peaks showed a strictly linear dependence up to relatively high radiation doses, when excited at 1600 Å.     

溶胶-凝胶法制备钼铁催化剂及其XRD、FTIR光谱分析

利用溶胶-凝胶法合成了Mo-Fe催化剂,用对二甲苯的选择性氧化作为探针反应,对其进行了催化剂的活性评价,结果表明：金属原子数的最佳配比为n(Mo)∶n(Fe)∶n(Co)=2.4∶1∶0.02,这时的催化剂活性最高;Mo-Fe系催化剂的活性组分为Fe₂(MoO₄)₃与少量的MoO₃,它们在催化氧化过程中,存在着协同作用,FTIR和XRD均得到了证实。该研究为工业装置的技术改造提供了较好的实验依据。