X射线荧光光谱法对钒氧化物中不同价态钒的定量分析

讨论用普通的X射线荧光光谱仪 ,采用谱峰分解法和谱峰合成法对钒氧化物的混合物中氧化态V2 O3、V2 O4、V2 O5 的定量分析。谱峰分解法系以每种钒氧化态的标准谱形函数为基础 ,用最小二乘法求解。而谱峰合成法则是以每种纯氧化态的测量谱线为基础 ,用定标技术求解。用上述方法测定钒氧化物产品 ,其结果与化学法、电化学法的结果一致 ,最大相对误差为7 7%。

New Oxorhenium（V） Complex with an Aminothiazole Ligand, and Radiochemical Behavior of Its Oxotechenetium（V） Complex Analog

A [ReO（Amino）2OH] complex was successfully synthesized by the ligand exchange method using oxorhenuim gluconate and an aminothiazole ligand. The complex was characterized elemental analysis and IR, UV-Vis, NMR and mass spectroscopes. The technetium tracer 99mTcO-complex has also been synthesized by two methods using Ligand exchange method and direct reduction method. The radiochemical purity of the complex was over 95% as measured by thin layer chromatography. In vitro studies showed that the complex possessed good stability under physiological conditions. The partition coefficient indicated that the complex hydrophilic and the electrophoresis results showed that the complex neutral. Normal biodistributions of the 99mTC complex exhibit high lung, liver and spleen uptake of 27%, I 1%, and 12%, respectively. Blood and lungs clearance was quite, while liver activity remained high for a longer period with 12% injection dose present at 1 h post-inj ection. The radioactivity from the novel technetium complex was excreted mainly through the hepatobiliary system, which passed 35% of the complex at 1 h post-injection, and partially through the kidneys.

Study on the basic nitrogen compounds from coal-derived oil

The distillation range analysis and elemental analysis of fractioned direct liquefied oil were conducted. Each fraction of liquefied oil contains some nitrogen compounds. Using the acid extraction method and gas chromatography/mass spectrometry （GC-MS）, the basic nitrogen compounds have been separated and identified. Compared with the nitrogen content of the liquefied oil before and after separation, the basic nitrogen compounds account for more than half of all nitrogen compounds. The basic nitrogen compounds in the light liquefied oil are easily separated, and contain more types of basic nitrogen compounds. The results also show that there are many basic nitrogen compounds in liquefied oil, such as pyrrole, aniline, pyridine, quinoline and so on. However, there are fewer other types of basic nitrogen compounds.

Biodiesel synthesis via metal oxides and metal chlorides catalysis from marine alga Melanothamnus afaqhusainii

This research article demonstrates the most comprehensive comparative catalytic study of different metal oxides and metal chlorides towards the methanolysis of triglycerides of marine red macroalga Melanothamnus alhqhusainii. CaO was found to be the most reactive metal oxide that yielded 80% biodiesel while ZnCI2 was the most reactive metal chloride that produced 60% biodiesel by mechanical stirring for 6 h at 100-110 ℃. The overall reactivity order of the catalysts was found to be CaO 〉 MgO 〉 Pb02 〉 ZnC12 〉 TIC14 〉 PbO 〉 HgC12 〉 ZnO 〉 AIC13 〉 SnCI2 〉 TiO2 whereas, CaCI2, MgCI2, A1203, HgO, PbCI2, MnO2, MnC12, Fe203 and FeCI3 were found to be non-reactive for transesterification of triglycerides. In addition, a detailed study of the screening of mobile phases and spraying reagents was conducted which showed that petroleum ether ： chloroform ： toluene （7：2：1 ） is the best mobile phase, whereas iodine crystals/silica gel is the best visualizing agent for the thin layer chroma- tography （TLC） examination ofbiodiesel. Biodiesel production was confirmed by comparative TLC examination. It was further supported by the determination of fuel properties of biodiesel, which were found to be similar to the standard limits of American Society for Testing and Materials （ASTM）,

Synthesis and Characterization of LDHs （Layered Double Hydroxides） Intercalated with EDTA （Ethylenediaminetetracetic Acid） or EDDS （N, N＇-1, 2-Ethanediylbis-l-Aspartic Acid）

The hydrotalcite-like compound [Zn2Al·（OH）6] NO3·nH2O and [Mg2Al·（OH）6] NO3·nH2O （shorted as ZnA1-NO3 and MgAl-NO3） was intercalated with the chelating agent EDTA （Ethylenediaminetetraacetic Acid） and EDDS （N, N＇-1, 2-Ethanediylbis-1-Aspartic Acid） by anion exchange. The materials synthesized in this work were characterized by chemical analysis, FT-IR （Fourier Transform Infrared Spectroscopy）, SEM （Scanning Electron Microscopy） and XRD （Powder X-ray Diffraction） to confirm their properties. In order to discuss the adsorption capacity of LDHs （Layered Double Hydroxides）, the adsorption experiment was investigated under the optimum condition （10 mg, 25℃ and 100 μg·L-1）. The amount of metallic ions adsorbed by LDHs intercalated with EDTA and precursor LDHs were determined by ICP-AES （Inductively Coupled Plasma-Atomic Emission Spectrometry） and AAS （Atomic Absorption Spectrometry）. The intercalation of EDTA leads to improve the adsorption capacity of LDHs. LDHs intercalated with chelating agents have generally high affinity for removing metallic ions, and they can be efficient adsorbents for metallic ions.

Analyses on Phenolic Composition and Content of Pomegranate

In order to reveal difference of phenolic substances and the content in the different varieties of pomegranate fruit and different mature period. The article uses 3 different fruit color phenotype （white, red, green） pomegranate cultivars as materials, the peel were determined by high performance liquid chromatography respectively （composition and content of phenolic compounds in the seeds and juice）. Results shows that the varieties of pomegranate peel and seeds were detected in 13 kinds of phenols, juice was detected in 12 type, and which did not detect epicatechin. At the same time, there was a significant difference in different parts of different varieties of pomegranate phenolic content.

湍流入口条件下建筑非定常风场的大涡模拟

考虑湍流入口条件对绕德州理工大学标准模型的三维非定常风场进行了数值模拟;比较了稳态入口边界条件下时均风速剖面形状对建筑表面压力分布的影响;分别采用旋涡法、谱合成法和预前模拟法生成湍流入口风速脉动;并将相应的大涡模拟结果与实测数据和风洞试验数据进行了对比分析。结果表明:时均风速剖面形状对时均流场的影响几乎可以忽略,但对瞬态流场的计算有很大影响,工程应用中建议根据当地实测数据修正风速剖面公式;采用由预前模拟法生成的湍流作为入口边界条件进行大涡模拟得到的建筑表面风压非定常特性与实际情况最为吻合;通过高精度插值算法,预生成的入口湍流时程数据能在位于相同地貌下不同建筑绕流的大涡模拟中反复使用,在一定程度上弥补了预前模拟耗时的缺陷。

Structure characterization,magnetic and photoluminescence properties of Mn doped ZnS nanocrystalline

Wurzite ZnS:Mn nanorods are synthesized via a solvothermal method by using ethylenediamine and water as mixed solvent.The diameters of the nanorods increase and the lengths decrease with the Mn concentration.High resolution transmission electron microscopic images illustrate that a few cubic ZnS:Mn nanoparticles arise along with hexagonal nanorods on high Mn concentration.The samples set off yellow-orange emission at 590 nm,characteristic of 4 T→ 6 A 1 transition of Mn 2+ at T d symmetry in ZnS.Electron spin resonance spectrum of the nanorods shows that high Mn concentrations produce a broad envelope,whereas six-line hyperfine appears for lower Mn concentrations.These results together with the magnetization curves indicate that all the ZnS:Mn samples are paramagnetic even down to 4 K,which suggests that the ZnS:Mn is not suitable for dilute magnetic semiconductor.

Kinetically controlled, high-yield, direct synthesis of [Au_(25)(SePh)_(18)]^-TOA^+

In this article, we present a facile, direct, synthetic approach of preparing monodisperse [Au2s（SePh）ls]- nanoclusters in high yield. In this synthetic approach, two-phase Brust-Schiffrin method is used. Both PhSeH and NaBH4 should be added drop-wise to the solution of Au （III） at the same time. The formula and molecular purity of [Au25（SePh）ls] TOA＋ clusters are characterized by MALDI-TOF mass spectrometry, NMR and TGA analysis. Furthermore, some critical parameters to obtain pure [Au25（SePh）18]-TOA＋ are identified, including the NaBH4-to-Au ratio, the selenolate-to-Au ratio and the temperature. The facile, direct, high yield synthetic method can be widely applied in the theoretical research of Au clusters protected by selenol.