氯化物的分子吸收光谱法测定

研究用冷分子吸收光谱法测定氯化物的方法．考察各实验参数对测定的影响,Ｃｌ－的检出限为１６．０μｇ／ｍＬ,并测定湖水和自来水中Ｃｌ－的含量     

Synthesis of Highly Sensitive Fluorescent Probe Based on Tetrasubstituted Imidazole and Its Application for Selective Detection of Ag+ Ion in Aqueous Media

A small molecule fluorescent probe, 4-[2-(4-chlorophenyl)-4,5-diphenyl-1H-imidazol-1-yl]aniline(L) for detecting Ag⁺ ion was gently synthesized via one-pot multi-component reaction catalyzed by H₃[PW₁₂O₄₀] under solvent-free microwave irradiation. When the concentration of Ag⁺ ion changed from 0 to 8.0×10⁻⁶ mol/L in the solution of H₂O/CH₃OH(19:1, volume ratio), the fluorescence emission spectrum was blue-shifted and accompanied by a gradual increase in fluorescence intensity with a low detection limit of 3.0×10⁻¹¹ mol/L. Moreover, UV-Vis absorption titration experiment demonstrated a 1:1 stoichiometric ratio and an association constant of (9.95±0.44)×10⁵ L/mol between probe L and Ag⁺ ion, and thus their complexation mechanism was also proposed and verified. More importantly, this fluorescent probe was remarkably specific for Ag⁺ ion under the interference of other metal ions and exhibited a wide pH application range of 4.0-8.0. Additionally, preliminary application of this probe was also carried out and satisfactory results were shown.     

Improved solvent-free microwave extraction of essential oil from dried Cuminum cyminum L. and Zanthoxylum bungeanum Maxim

Solvent-free microwave extraction (SFME) is a recently developed green technique which is performed in atmospheric conditions without adding any solvent or water. SFME has already been applied to extraction of essential oil from fresh plant materials or dried materials prior moistened. The essential oil is evaporated by the in situ water in the plant materials. In this paper, it was observed that an improved SFME, in which a kind of microwave absorption solid medium, such as carbonyl iron powders (CIP), was added and mixed with the sample, can be applied to extraction of essential oil from the dried plant materials without any pretreatment. Because the microwave absorption capacity of CIP is much better than that of water, the extraction time while using the improved SFME is no more than 30 min using a microwave power of 85 W. Compared to the conventional SFME, the advantages of improved SFME were to speed up the extraction rate and need no pretreatment. Improved SFME has been compared with conventional SFME, microwave-assisted hydrodistillation (MAHD) and conventional hydrodistillation (HD) for the extraction of essential oil from dried Cuminum cyminum L. and Zanthoxylum bungeanum Maxim. By using GC-MS system the compositions of essential oil extracted by applying four kinds of extraction methods were identified. There was no obvious difference in the quality of essential oils obtained by the four kinds of extraction methods.     

Enhanced optical immunosensor based on surface plasmon resonance for determination of transferrin

Wavelength modulation surface plasmon resonance biosensors (SPR) using colloidal Au nanoparticles and double-linker sensing membrane enhancement are reported for determination of transferrin. The 2-mercaptoethylamine (MEA) was immobilized on the biosensor surface with traditional amine coupling method. The interaction between colloidal Au nanoparticles and MEA was investigated. The anti-transferrin was immobilized on the biosensor surface prepared with staphylococcal protein A (SPA). The interaction of the antibody and antigen was monitored in real time. The good response was obtained in the concentration range 1-20, 0.1-20 and 0.05-20 μg/mL for directly immune assay, double-linker assay and colloidal Au-amplified assay. The result clearly demonstrates that these methods may obtain significantly enhancement of sensitivity for the wavelength modulation SPR biosensor.     

Extraction and determination of hormones in cosmetics by homogeneous ionic liquid microextraction high-performance liquid chromatography

The homogeneous ionic liquid microextraction was applied to the extraction of hormones from cosmetics and the hormones were determined by high-performance liquid chromatography. 1-Hexyl-3-methylimidazolium tetrafluoroborate was used as extraction solvent. Ammonium hexafluorophosphate as used as ion-pairing agent. Several experimental parameters, including the volume of 1-hexyl-3-methylimidazolium tetrafluoroborate, amount of ammonium hexafluorophosphate and sodium chloride, extraction and centrifuge time, and the pH value, were optimized. The limits of detection and quantification for the analytes ranged from 0.03 to 0.24 ng/mL and from 0.10 to 0.79 ng/mL, respectively. The precision for determining the hormones was lower than 5.2%. The proposed method was successfully developed for the determination of hormones in real cosmetic samples.     

Extraction of the Volatile and Semivolatile Compounds in Seeds of Cuminum cyminum L. Using Hydrodistillation Followed by Headspace-Ionic Liquid-Based Single-Drop Microextraction

Hydrodistillation (HD) coupled with headspace single-drop microextraction by using ionic liquid (IL) as the extraction solvent, followed by gas chromatography analysis technique, was successfully developed to determine the volatile and semivolatile compounds in seeds of Cuminum cyminum L. In the proposed method, a 1.5-??L microdrop of 1-octyl-3-methylimidazolium hexafluorophosphate, working as the extraction solvent was suspended in the headspace of a 50-mL round-bottom sample flask. After extracting for 30?min, both IL and target analytes were injected into the gas chromatographic system by thermal desorption for 5?s under 240?°C. Then, the IL was retracted back to the microsyringe. Thus, the capillary column should not be contaminated and a clean chromatogram was obtained. The parameters affecting extraction performance were investigated and optimized. The extraction efficiency of the proposed method was compared with that of HD, which is a standard extraction method. The contents of constituents in the extract obtained by the proposed method were close to those obtained by HD. It seems to be an environmentally friendly, time-saving, high efficiency and low solvent consumption technique and would be useful, especially for aromatic plants analysis.     

Al-1%Si单晶制备工艺及微观组织分析

在自制的真空熔炼、氩气保护下拉式连续定向凝固设备上成功制取了具有单晶组织的φ8mm Al-1%Si合金棒材,并对其组织演变过程及稳定性进行了研究.分析了定向凝固过程中,硅颗粒在单晶组织中的分布形态,提出了使硅固溶或弥散均匀分布于铝基体中的措施.     

硅砂表面高温改性提高水玻璃砂强度的机理

Ｘ－射线衍射（ＸＲＤ）、扫描电镜（ＳＥＭ）、能谱（ＥＤＳ）等的研究表明,硅砂表面存在吸附膜．高温改性使吸附膜被牢固烧结在砂粒表面,改变了吸附膜和砂粒表面的物理和化学特性,大大改善了湿润性,使粘结桥的断裂形式从附着断裂向内聚断裂转化,提高了水玻璃砂的强度．     

基于KMV-CatBoost增强的企业信用债券违约风险评估模型

针对传统预测模型对于企业信用债券违约预测准确率低、拟合效果差的问题,提出了基于Kaufman-Merton-Voss （KMV）-Categorical Boosting （CatBoost）的企业债券违约预测模型. 首先对原始样本数据进行预处理,降低噪声数据对预测模型的影响;然后,利用KMV模型评估借款公司信用违约概率,计算公司资产市场价值与公司资产市场价值的波动率,获得企业资产价值与违约点之间的差额Distance-to-Default（DD）;最后,利用债务偿还期限、短期无风险收益率、公司股权市场价值、公司债务面值计算出的违约距离,将其加入指标中,利用CatBoost算法预测企业信用债券违约风险,通过基于Ordered Boosting方式的CatBoost算法训练模型,得到无偏梯度估计,以减缓预测偏移,从而增强模型的泛化能力. 实验结果表明：基于KMV-CatBoost增强的模型能够提高企业信用债券违约风险识别的准确率,识别正确率约为95.5%.     

Scalable Network Coding for Heterogeneous Devices over Embedded Fields

In complex network environments, there always exist heterogeneous devices with different computational powers. In this work, we propose a novel scalable random linear network coding (RLNC) framework based on embedded fields, so as to endow heterogeneous receivers with different decoding capabilities. In this framework, the source linearly combines the original packets over embedded fields based on a precoding matrix and then encodes the precoded packets over GF(2) before transmission to the network. After justifying the arithmetic compatibility over different finite fields in the encoding process, we derive a sufficient and necessary condition for decodability over different fields. Moreover, we theoretically study the construction of an optimal precoding matrix in terms of decodability. The numerical analysis in classical wireless broadcast networks illustrates that the proposed scalable RLNC not only guarantees a better decoding compatibility over different fields compared with classical RLNC over a single field, but also outperforms Fulcrum RLNC in terms of a better decoding performance over GF(2). Moreover, we take the sparsity of the received binary coding vector into consideration, and demonstrate that for a large enough batch size, this sparsity does not affect the completion delay performance much in a wireless broadcast network.