Vo(acac)_2在Y-型分子筛上固载化的变温ESR波谱研究

固载在Y-型分子筛上VO~(2+)的多种变温ESR波谱已被报道。在较低的温度下,ESR谱由各向异性谱和各向同性谱组成,随着温度的增加,各向同性谱渐渐转变为各向异性谱,这被解释为主要是结构(Ⅰ)转变为结构(Ⅱ)。并计算了结构(Ⅱ)的△E。     

水平管泡状流压力信号的功率谱特性比较

为比较Welch功率谱、AR功率谱和EV功率谱对气液二相水平管泡状流压力信号的功率谱分析效果,对泡状流压力波动信号进行了分析.将提取的泡状流压力波动信号经小波去噪后,分别进行Welch功率谱、AR功率谱和EV功率谱估计,并分析比较所得3种功率谱密度图.分析表明:Welch、AR和EV功率谱均能正确反映泡状流压力波动信号...     

异山梨醇化学结构确证

对采用一次高真空蒸馏 ,粉状活性炭吸附得到的异山梨醇成品 ,进行了紫外光谱、红外光谱、质谱、核磁共振氢谱和碳谱测定。经波谱解析确证了异山梨醇的化学结构为 1,4;3 ,6 二脱水 D 山梨醇     

4种二硫代羧酸酯的合成与表征

以乙酰乙酸乙酯为原料,经烷基反应、亲核加成反应,得到4种新的二硫代羧酸酯化合物,并用红外光谱、核磁共振氢谱、核磁共振碳谱和质谱进行了表征.     

Vo（acac）2在Y—型分子筛上固地载化变温ESR波谱研究

固载在Y－型分子筛上VO^2＋的多种变温ESR波谱已被报道。在较低的温度下ESR谱由各向异性谱和各向同性谱组成，随着温度的增加，各向同性谱渐渐转变为各向异性谱，这被解释为主要是结构（I）转变为结构（Ⅱ）。并计算了结构（Ⅱ）的△E。     

抗流感药物奥司他韦的结构确证

抗流感药物磷酸奥司他韦是流感早期治疗的有效药物,采用多种波谱仪器对该合成药物结构进行了确证,详细讨论了合成药物的核磁氢谱和碳谱的特征,应用二维核磁谱提供的碳氢键合相关信息对碳谱和氢谱信号进行了归属,为合成新药及生产过程质量控制提供了重要的参考信息。     

核磁共振技术及其应用进展

核磁共振技术是有机物结构测定的有力手段,不破坏样品,是一种无损检测技术.从连续波核磁共振波谱发展为脉冲傅立叶变换波谱,从传统一维谱到多维谱,技术不断发展,应用领域也越广泛.核磁共振技术在有机分子结构测定中扮演了非常重要的角色,核磁共振谱与紫外光谱、红外光谱和质谱一起被有机化学家们称为"四大名谱".     

偕胺肟基化合物的合成及表征

以盐酸羟胺和氰基化合物为原料,设计、合成了标题化合物.利用红外光谱、核磁共振(H谱、C谱)、元素分析、质谱等方法确定了标题化合物的结构,优化了标题化合物的合成条件.     

ICP-OES测量金属眼镜架镍析出量的波长选择

现行国家标准中并未规定电感耦合等离子体发射光谱法测量金属眼镜架镍析出量时所用的谱线。选取镍元素波长为231.604 nm和352.454 nm的两条特征光谱谱线测试金属眼镜架的镍析出量,并建立了分析方法。测试结果表明：两条谱线的测试结果准确,灵敏度高,可作为镍元素的测试谱线。在标准曲线线性范围内,两条谱线的光谱强度和镍元素浓度呈现良好的线性关系,曲线相关系数均大于0.999 9,检出限分别为0.000 8μg/mL和0.003 5μg/mL,结果的相对标准偏差(n=11)均小于1.0%,加标回收率为96.4%～105.6%。因此,镍元素的231.604 nm和352.454 nm谱线适合作为测试金属眼镜架镍析出量的分析谱线。     

铝硅酸盐矿物的Raman振动特征解析

分别测定了蓝晶石、红柱石和夕线石3种铝硅酸盐天然矿物晶体的Raman光谱,并利用Materials Studio3.0软件计算3种矿物的Raman振动频率,分析其简正振动模式,确定了三种矿物特征谱峰的归属,解析了铝对铝硅酸盐Raman光谱振动特征的影响.结果表明:随着四配位铝的增加(从蓝晶石、红柱石到夕线石),800～1 200 cm-1波数区间内谱峰频率降低,该区间的谱峰归属于Si-Onb间非桥氧对称伸缩振动;700～800 cm-1区间内出现的谱峰归属于Al-Onb间非桥氧的对称伸缩振动.当铝全部为六配位时,会引起800～1 200 cm-1区间内的谱峰向高频方向迁移.这为进一步利用Raman光谱来研究硅酸盐玻璃和熔体结构中铝的作用提供了重要依据.     

诺卜醇的合成研究

多聚甲醛和过量 β-蒎烯反应合成了诺卜醇 ,平均产率达 71 .3%。并通过红外光谱、核磁共振、质谱对产物结构进行了确证。     

罗丹明B的三维荧光光谱研究

本文利用三维荧光激发-发射光谱研究了罗丹明B的荧光光谱特性。考察了罗丹明B浓度、pH值大小等因素对罗丹明B的荧光光谱影响,给出了其三维荧光光谱图。结果显示,罗丹明B的三维荧光光谱图较二维荧光光谱图能更详细地描述被测组分的性质,为综合考查罗丹明B的结构特征提供了参考。     

Derivative ultraviolet and visible spectrophotometry: Applications to polymer analysis

First- to fourth-derivative spectra of humic acids, polystyrene, and mixtures of several prepolymers were measured and the advantage of derivative spectrophotometry such as resolution enhancement and background correction was discussed. Although the vis-absorption spectra for humic acids in pH solutions from pH 2.0 to 10.0 could be hardly discriminated, humic acids in solutions above pH 7.0 could be clearly distinguished from those in solutions below pH 6.0 by first-derivative spectrophotometry. Similarly, the first-derivative spectra of the copper-humic acid complex were different from those of free humic acids, though both absorption spectra resembled each other. UV absorption spectrum of a mixture of phenol-novolac resin and methylated methylol-melamine resin was similar to and the second-derivative spectrum was different from that of phenol-novolac resin. The difference of derivative spectra of a mixture of polycarbonate and epoxy resin was also discussed. Shoulder and unresolved peaks were clearly revealed by differentiation of absorption spectra and peak assignments from the fourth-derivative spectra were more accurate than those from the absorption spectra. This advantage was discussed by using polystyrene as an example.     

染料掺杂有机改性硅酸盐的制备与光谱特性

１９８８年Ｐａｖｌｏｐｏｕｌｏｓ等人发现１,３,５,７四甲基吡咯亚甲基ＢＦ２化合物是一个性能优良的激光染料［１］．它的荧光量子效率高,激光效率比香豆素５４０Ａ高１０％,并具有低的三重态吸收和高的光化学稳定性．因此,在染料激光、生物荧光探针、光动力疗法等方面都有潜在的应用背景［２～４］．溶胶凝胶法是目前研究最多,应用最广低温制备玻璃的方法．广泛地运用于制备各种光学材料、陶瓷、薄膜等功能材料．但运用传统的溶胶凝胶法制备的样品易在热处理过程中脆裂,力学性能和柔韧性均很差,不能直接抛光达到所需的光…     

不对称酰胺基卟啉的合成及表征

通过5-（4-氨基）苯基-10,152,0-三苯基卟啉（MATPP）与3-氰基苯甲酸在CH2Cl2中直接反应得到一种新型不对称酰胺基卟啉配体5-（4-3-氰基苯甲酸酰亚胺基）苯基-101,5,20-三苯基卟啉配体（CBTPPH2）,利用紫外-可见光谱、红外光谱、核磁共振氢谱、质谱、元素分析等测试方法对化合物的结构加以确认。     

N,N-二甲基胺基丙基-甲基丙烯酰胺的合成及其NMR表征

以甲基丙烯酸甲酯与N,N-二甲基丙二胺进行酯交换反应合成N,N-二甲基胺基丙基-甲基丙烯酰胺(DMAPMA),收率可达70.3%。用~1H-NMR、~(13)C-NMR、和DEPT等表征了DMAPMA的结构。     

Determination of the Molecular Structure of Interphases Between Epoxy/4,4'-Diaminodiphenylsulfone Adhesives and Silver Substrates Using SERS and XPS

The molecular structure of interphases formed by curing an epoxy/4,4'-diaminodiphenylsulfone (DADPS) adhesive against rough silver substrates was determined using surface-enhanced Raman scattering (SERS) and x-ray photoelectron spectroscopy (XPS). SERS spectra obtained from the adhesive deposited onto silver island films were very similar to SERS spectra obtained from the DADPS curing agent spun onto silver island films, indicating that DADPS in the adhesive system segregated to the interphase and was preferentially adsorbed onto the silver substrate. Differences in the relative intensity of several bands in the normal Raman and SERS spectra of DADPS were observed. For example, the band near 1603 cm^-1 was stronger in SERS spectra of DADPS than in normal Raman spectra. The band near 1150 cm^-1 was weaker in SERS spectra of DADPS than in normal Raman spectra. These results implied that DADPS was adsorbed through one of the NH groups with an end-on conformation. Consistent results were also obtained from XPS spectra. C(ls) spectra of the adhesive and silver fracture surfaces of specimens prepared by curing the adhesive against silver substrates were more similar to the C(ls) spectra of DADPS than to those of the bulk adhesive. These results confirmed the preferential adsorption of DADPS onto the silver substrate from the adhesive system. The similarity of the C(ls) spectra obtained from adhesive and silver fracture surfaces indicated that a thin DADPS-rich interphase was formed between the bulk adhesive and the silver substrate and that the locus of failure was partially within this layer. However, less nitrogen and sulfur were detected on the silver fracture surface than on the adhesive fracture surface. A large amount of silver was observed on the substrate fracture surface and a trace was found on the adhesive fracture surface. These results indicated that failure of the adhesive joints was within the interphase but near the silver substrate. No evidence of chemisorption of DADPS onto the substrate was observed.     

一种新型液晶化合物的合成及表征

以CH2C12为溶剂,通过5-（4-氨基）苯基-10,15,20-三苯基卟啉（MATPP）与十二酸直接反应得到一种新型不对称酰胺基卟啉配体5-（4-十二酸酰亚胺基）苯基．10,15,20．三苯基卟啉配体（PDTPPH2）,利用紫外-可见光谱、红外光谱、核磁共振氢谱、元素分析等测试方法对化合物的结构加以确认。     

分子蒸馏和固相微萃取法分析树苔浸膏的化学成分

采用分子蒸馏法和固相微萃取法与气相色谱/质谱仪联用对树苔浸膏的化学成分进行了分析;结合谱库检索技术、质谱图解析及保留指数对化合物进行了鉴定,并采用峰面积归一化法进行了半定量研究.结果表明,采用固相微萃取法鉴定出63种化学成分,分子蒸馏法三级馏分共鉴定出61种成分,可见两种不同前处理方式鉴定出的化合物种类差异不大.采用分子蒸馏技术能够将浸膏中的轻质和重质组分有效分离、纯化,降低干扰,适合于组分复杂的浸膏类香料的分析.利用谱库检索及图谱解析技术,结合保留指数对树苔浸膏化学成分进行定性,能够显著提高定性结果的准确性和可靠性.     

含吡嗪、喹啉荧光探针的合成及其对金属离子的识别研究

设计合成了3个含有吡嗪基团的荧光探针分子和喹啉基团的荧光探针分子,其结构通过红外(FT-IR)、质谱(MS)、核磁共振氢谱(1HNMR)进行表征,通过吸收光谱和荧光光谱研究了不同金属离子对目标探针分子的影响。结果表明:Cd2+使401 nm处荧光蓝移了20 nm;Co2+、Hg2+、Pb2+、Zn2+使357 nm处荧光分别红移了20、50、1401、40 nm;Cd2+、Hg2+使349 nm处荧光分别红移了707、5 nm。