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Regents and solvents All the chemicals were purchased from Aldrich Chemical Co. Other solvents and reagents were analytical grade and used as received, unless otherwise stated. Tetrahydrofuran (THF) was distilled over metallic sodium and dimethyl formamide (DMF) over calcium hydride before use. 1H and 13C NMR spectra were recorded on a Bruker-AC500 (500 MHz) spectrometer with CDCl3 as solvent and tetramethylsilane (TMS) as the internal standard. Elemental analysis was performed on a Perkin-Elmer 2400. UV-vis absorption and diffuse reflectance absorption spectra were recorded on a Hitachi U- 4100 spectrophotometer. Fluorescence measurements were carried out with a Hitachi F-4600 spectrophotometer. The peak wavelength of the lowest energy absorption band was used as the excitation wavelength for the PL measurement. The fluorescence quantum yield (F) was determined at room temperature by the dilution method using fluorescein in water (pH ¼ 11) as the reference. Powder wide-angle X-ray diffraction (PXD) experiments were performed on a powder X-ray diffractometer (INCA Energy, Oxford Instruments) operating at 3 kW. Differential scanning calorimetry (DSC) curves were determined on a Netzsch DSC 204F1 at a heating rate of 10 C min1. |
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【答案】应助回帖
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yhc0316: 金币+50, 翻译EPI+1 2014-10-19 14:13:02
yhc0316: 金币+50, 翻译EPI+1 2014-10-19 14:13:02
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试剂和溶剂 所有的化学品均购自Aldrich化学公司。除非另有说明,其它溶剂和试剂均为分析级并且原样使用。使用前,用金属钠对四氢呋喃(THF)重蒸馏,用氢化钙对二甲基甲酰胺(DMF)重蒸馏。 以CDCl3为溶剂、四甲基硅烷(TMS)为内标,用Bruker-AC500(500 MHz)光谱仪记录1H和13C的NMR光谱。用Perkin-Elmer 2400进行元素分析。用日立U-4100分光光度计记录紫外-可见光吸收光谱和弥散反射吸收光谱。用Hitachi F-4600分光光度计进行荧光测量。用最低能量的吸收带的峰值波长作为激发波长测定PL。用稀释法在室温下测定荧光量子产率(F),以荧光素水溶液(pH=11)作参照。粉末广角X射线衍射(PXD)实验是在粉末X射线衍射仪(INCA能源,牛津仪器)用3千瓦功率进行。差示扫描量热法(DSC)曲线用Netzsch DSC204F1测定,所用升温速率为10度/分钟。 |
3楼2014-10-19 10:31:37
【答案】应助回帖
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(实验)试剂与溶剂 (reagent 是试剂,你复制错了) (实验)所用样品均来自阿拉丁试剂厂。其他试剂及溶剂均为分析纯,且为新到样品(收到即使用),其他纯度的样品除外。使用前先将金属钠用四氢呋喃(THF)进行蒸馏,氢化钙用二甲基甲酰胺(DMF)进行蒸馏。 以CDCl3为溶剂、四甲基硅烷(TMS)为内标物,用Bruker-AC500 (500 MHz)测得1H 和 13C 的NMR光谱。利用 Perkin-Elmer 2400进行基础分析。用Hitachi U- 4100分光光度计记录了紫外可见吸收光谱 和漫反射吸收光谱。以能量最低的吸收谱带的波长的峰值作为激发波长,来进行PL测量。荧光量子的含量在室温下通过稀释法进行了测定,以荧光素水溶液作为其参照。宽角度PXD测试实验在XRD(INCA 能源, 牛津仪器设备生产)上于3KW的功率下进行。扫描差热(DSC)曲线由Netzsch DSC 204F1测试仪以10度每分钟的升温速率进行了描绘。 ![]() |
2楼2014-10-18 21:14:28













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