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报道了农药杀菌剂三环唑有效体的脉冲极谱测定新方法。三环唑硝化产物的极谱波在磷酸缓冲溶液中 (Na3 PO4 H3 BO3 NaOH) ,其峰电位Ep =-0 .5 5V (Ag/AgCl电极 ) ,其浓度和峰高在 :1× 10 - 5mol/L~ 3.4×10 - 5mol/L时线性关系良好 ,利用该法测定了粉剂中的三环唑 ,其结果与GLC法吻合。另外 ,对极谱电极反应机理进行了较详细的论证 ,实验结果与理论推导一致性很好。 相似文献
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研究了以碳酸铷(Rb2CO3)和乙酰丙酮锂(LiAcac)为催化剂,异山梨醇(IS)和碳酸二甲酯(DMC)为原料合成聚碳酸酯(PC)的工艺过程。优化了酯交换反应催化剂用量、原料配比、缩聚反应催化剂用量、缩聚反应温度以及缩聚反应停留时间,并对酯交换产物和聚碳酸酯产品进行了红外光谱、核磁氢谱、核磁碳谱和热重分析,得到较优工艺条件为:Rb2CO3用量1×10-3mol/molIS、原料配比n(DMC)/n(IS)=14、LiAcac用量2×10-3mol/molIS、缩聚温度225℃、缩聚停留时间4h,所得的PC产品特性黏数可达36.55mL/g,数均分子量(Mn)为30659,重均分子量(Mw)为42551,Mw/Mn为1.39,色差为6.92,玻璃化转变温度(Tg)为155.6℃。 相似文献
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通过高温固相法合成了Ca3La1.96(BO3)4:0.04Pr3+荧光粉。通过X射线衍射(XRD)确定了样品的晶体结构,通过激发光谱和发射光谱对样品发光性能进行了研究。X射线衍射测试结果表明,样品已经成相。光谱测试结果表明,在449 nm、473 nm和485 nm光的激发下,样品的发射谱峰位于607 nm附近,这归因于Pr3+的1D2→3H4跃迁。监测607 nm时,样品的激发谱由位于320~400 nm的宽激发带和分别位于449 nm、473 nm和485 nm处的窄激发峰组成。位于449 nm、473 nm和485 nm处的激发峰分别归因于Pr3+的3H4→3P2、3H4→3P1... 相似文献
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聚乙烯醇(PVA)产品醇解度是影响产品品质和下游应用的一项重要指标,通常采用化学滴定法测定,但耗时耗力。目前文献报道的核磁共振波谱测定醇解度的方法虽然大大简化了实验流程,提高了测定速度,但大多存在谱峰指认不清导致测定结果误差较大的问题。本文优化了样品制备和测试条件,如溶剂、温度等,在此基础上通过一系列二维核磁实验对不同谱峰进行了准确的归属,并通过定量核磁实验进行了定性、定量分析。结果表明,3种1H谱计算方法和13C谱计算方法结果高度一致,并与滴定结果十分吻合。与定量13C谱相比,定量1H谱实验方法在10 min以内即可得到结果,是一种快速准确的聚乙烯醇产品醇解度测定方法。 相似文献
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合成了配合物[La(Glu-sal)(H2O)2Cl].2H2O,并通过化学分析、红外光谱、紫外光谱、摩尔电导和TG-DTA等对其进行了表征,运用Achar法和Coats-Redfern法,研究了配合物第3步、第4步热分解的动力学过程,第3步非等温动力学方程为dα/dt=Ae-E/RT3/2(1-α)2/3[1-(1-α)1/3]-1,其表观活化能E=216.4 kJ/mol,指前因子lnA=45.2 s-1;而第4步动力学方程为dα/dt=Ae-E/RT(1-α)2,其表观活化能E=289.8 kJ/mol,指前因子lnA=50.9 s-1。 相似文献
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Y3Al5O12:Ce3+(YAG:Ce3+)发射谱中红光成分的不足导致了白光LED色温偏高且显色性较差,一种解决方案是引入能发射红光的激活离子与Ce3+共掺杂以使YAG:Ce3+发射谱红移。本工作报道了Ce3+–Eu3+共掺Y3Al5O12(YAG:Ce3+/Eu3+)透明陶瓷的制备、结构和荧光性能。该材料体系在Eu含量高达25%时仍保持纯石榴石相结构,且Eu3+的荧光猝灭浓度高达9%左右,比Pr3+和Sm3+等离子更适合用作YAG的红光发射激活剂。YAG:Ce3+/Eu3+透明陶瓷在蓝光(如442和466 nm)激发下的Ce3+荧光发射随着Eu含量的... 相似文献
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采用密度泛函理论的DFT/B3LYP/6-311+G(d,p)方法和基组,对甲基苯丙胺的UV-Vis光谱,IR光谱,1HNMR光谱和荧光光谱进行了理论模拟和指认。自然电荷计算表明,胺基N和H原子很可能是其发挥药理活性的亲电和亲核反应中心。 相似文献
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以三氯化铝为催化剂、过渡金属氯化物MCl3(VCl3、CrCl3和TiCl3)为促进剂,催化1-癸烯齐聚制备了具有高黏度指数的聚α-烯烃(PAO)合成油,系统研究了促进剂的作用机制和齐聚反应条件对齐聚反应活性和PAO性能和结构的影响。结果表明:VCl3和CrCl3的加入能明显增加1-癸烯齐聚反应收率和齐聚物的黏度指数。过渡金属氯化物通过双氯桥结构与三氯化铝形成双金属化合物,通过双金属间的协同效应,改变三氯化铝的吸电子能力来增加其催化活性。通过核磁氢谱(1H NMR)和核磁碳谱(13C NMR)分析,确定了AlCl3/MCl3催化1-癸烯齐聚遵循阳离子聚合机制,1-癸烯齐聚物中主要的不饱和双键为三取代和双取代内烯烃。过渡金属氯化物促进剂可以调整优势反应途径从而改变齐聚产物的分布。 相似文献
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K.M. McNamara K.K. Gleason D.J. Vestyck J.E. Butler 《Diamond and Related Materials》1992,1(12):1145-1155
The quality of chemically vapor deposited diamond films was assessed in terms of sp2/sp3 content as determined by solid-state nuclear magnetic resonance (NMR) and Raman spectroscopy. While the results of the two techniques are in qualitative agreement, only the NMR spectra yield quantitative values for the sp2/sp3 ratio. Only sp3 carbon was observed in the NMR spectra of very high quality hot-filament, microwave plasma, and d.c. arc-jet chemically vapor deposited films. As expected, Raman spectroscopy is extremely sensitive to sp2 bonded carbon, identifying small amounts below the detection limit of the NMR spectrometer. Comparison of the two techniques, however, indicates that Raman spectroscopy may be so sensitive to sp2 bonded carbon that sp3 bonded carbon in films containing as much as 90% sp3 bonded material may remain undetected. NMR linewidths indicate that the sp3 carbon in such material shows more disorder than that found in high-quality polycrystalline films. 相似文献
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The effects of the hydrolysis and condensation processes on the molecular structure of γ-glycidoxypropyltrimethoxysilane (γ-GPS) in aqueous solutions were investigated using Fourier-transform nuclear magnetic resonance (FT-NMR) spectroscopy and FT-Raman spectroscopy. Hydrolysis was characterized by monitoring the production of methanol and the decrease in concentration of SiOCH3 groups in 1% solutions of deuterium oxide using proton NMR. The production of methanol and loss of methoxy groups in 25% solutions of γ-GPS in water was characterized using Raman spectroscopy. Hydrolysis was found to be a very rapid process, whose rate could be increased or decreased by altering the pH of the solution. NMR spectroscopy showed that hydrolysis was complete in a 1% γ-GPS solution in deuterium oxide after 34 minutes. Raman spectroscopy also showed hydrolysis to be rapid and complete in a 25% solution of γ-GPS in water after 1 hour. Condensation, on the other hand, took a relatively long time to occur. In the NMR spectra, condensation was observed by the broadening of peaks due to the protons on the carbon atom adjacent to the silicon atom. In the Raman spectra, condensation was characterized by the disappearance of the SiOH band near 725 cm-1 and the development of an SiOSi band near 600 cm-1. In addition to the proton NMR, Si-29 NMR was used to characterize the silane in 10% solutions of γ-GPS in water. The Si-29 NMR showed oligomer growth with respect to time. The oligomer growth was correlated with mechanical test results. 相似文献
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Electrochemical oxidation of 3,5-di-tert-butylcatechol (1) has been studied in ethanol/water mixtures by means of cyclic voltammetry and controlled-potential coulometry. The results revealed that 3,5-di-tert-butyl-1,2-benenzoquinone (2) derived from oxidation of 3,5-di-tert-butylcatechol participate in noncovalently linked interactions with 1 converted to an ortho-benzoquinhydrone (3). The structure of 3 was characterized by MS, IR, 1H NMR and 13C NMR. The 1H NMR studies reveal that the benzoquinhydrone complex 3 is stabilized by one H-bonding interaction. In this work we derived a novel ortho-bezoquinhydrone type complex (3) based on electrochemical oxidation of 3,5-di-tert-butylcatechol at carbon electrode in an undivided cell. 相似文献
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采用13C NMR及FTIR对霍林河褐煤的化学结构特性进行深入分析,通过13C NMR计算得到霍林河褐煤包含34.32%的脂肪族碳、61.25%的芳香族碳以及4.43%的羰基碳。平均每个芳环团簇包含1~2个芳香环,每个芳香环中平均碳原子取代数为3~4。平均亚甲基碳链数为1.4,烷链支化度为25.47%,说明脂肪族多以短链分支形式存在。通过对霍林河褐煤红外光谱进行分峰拟合,计算得到煤的FTIR结构参数(平均亚甲基碳链数、芳香环取代度、烷链支化度)与13C NMR计算结果相吻合。虽然芳碳率(far-F=55.37%)与13C NMR计算结果存在一定的偏差,但是FTIR很大程度上仍然可以反映煤的碳骨架结构特性。 相似文献
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由香茅醛与盐酸羟胺在碳酸钠作用下反应制得香茅醛肟(2),再由香茅醛肟与溴代烷、氢氧化钠在四丁基溴化铵的作用下反应合成了4种香茅醛肟烷基醚,分别为香茅醛肟乙基醚(3a)和香茅醛肟正丙基醚(3b)、香茅醛肟正丁基醚(3c)和香茅醛肟正戊基醚(3d)。5个化合物经红外光谱(FT-IR)、核磁共振(1H NMR、13C NMR)、气质联用(GC-MS)分析表征了结构,并用菌丝生长速率法对11种植物病原真菌的抑制作用进行了测试。结构分析数据表明所用方法能合成得到5种目标化合物。在药液质量浓度为500 mg/L时,5种化合物对所用植物病原真菌均有一定的抑制作用,化合物2对水稻纹枯病菌的抑制率与百菌清一样高达100%,对辣椒菌核病菌、辣椒疫霉病菌、猕猴桃果实拟茎点霉菌、梨链格孢菌和毛竹枯梢病菌的抑制率高达100%,对油茶炭疽病菌、层出镰刀菌的抑制率也很高(≥95%),明显优于百菌清对这些病菌的抑制效果,3a对莴苣菌核病菌的抑制率高达100%,3b对葡萄炭疽病菌的抑制率为100%,3c对毛竹枯梢病菌的抑制率为87.7%,3d对莴苣菌核病菌的抑制率为96.2%,均高于同等质量浓度下百菌清对这些植物病原真菌的抑制率。 相似文献