Highly selective adsorption of cadmium ions by water‐dispersible magnetic thioglycolic acid/graphene oxide composites

A new selective and fast procedure based on magnetic dispersive solid‐phase extraction and zeta potential analysis is proposed for the determination of Cd (II) in some food samples. In the developed method, novel magnetic nanoparticles modified with thioglycolic acid were synthesized/characterized and also applied for quantitative determination of trace amounts of Cd (II) in food samples. The prepared nanoparticles were characterized via infrared spectroscopy, electron microscopy and adsorption–desorption experiments. These magnetic nanocomposites carrying Cd (II) could be easily separated from real samples simply by applying an external magnetic field; no filtration or centrifugation was necessary. Several parameters affecting the analytical performance, such as sample pH, amounts of nanocomposite sample, desorption solution volumes and coexisting ions, were investigated in detail. The detection limit of the method was 0.1 μg l^?1 while the relative standard deviation was 1.2% for a Cd (II) concentration of 0.5 mg l^?1. The proposed method was successfully applied to food sample analysis and standard reference material samples with satisfactory results, and excellent recoveries were obtained in the range 95–99% even when the matrix, such as sea water, was complex.     

高光谱技术融合图像信息的牛肉品种识别方法研究

高光谱图像包含了大量的光谱信息和图像信息,采用高光谱成像技术对牛肉品种进行识别。获取可见-近红外(400~1000 nm)光谱范围内的安格斯牛、利木赞牛、秦川牛、西门塔尔牛、荷斯坦奶牛五个品种共252个牛肉样本的高光谱图像。在ENVI软件中对高光谱图像进行阈值分割并构建掩膜图像,获取样本的感兴趣区域(ROI),并结合伪彩色图对牛肉样本的反射率指数进行可视化表达;采用Kennard-Stone(KS)法对样本集进行划分以提高模型的预测性能;对原始光谱采用卷积平滑(SG)、区域归一化(Area normalize)、基线校正(Baseline)、一阶导数(FD)、标准正态变量变换(SNV)及多元散射校正(MSC)等6种方法进行预处理;采用竞争性自适应重加权算法(CARS)提取特征波长。然后利用颜色矩对不同牛肉样本的颜色特征进行提取;对原始光谱图像进行主成分分析,结合灰度共生矩阵(GLCM)算法,提取主要纹理特征。最后结合偏最小二乘判别(PLS-DA)算法建立牛肉样本基于特征波长、颜色特征以及纹理特征的识别模型。KS法将牛肉样本划分为校正集190个,预测集62个;将未经预处理的光谱数据与经过6种不用预处理的光谱数据进行建模分析,结果发现经FD法处理后的光谱数据所建模型的识别率最高;结合CARS法对经FD法预处理后的光谱数据进行特征波长提取,共提取出22个波长;利用颜色矩和GLCM算法分别提取出每个牛肉样本的9个颜色特征、48个纹理特征。将特征波长数据与颜色、纹理特征信息进行融合建模,结果表明,基于特征光谱+纹理特征的模型识别效果最佳,其校正集与预测集识别率分别为98.42%和93.55%,均高于特征光谱数据模型识别率,说明融合纹理特征后使样本分类信息的表达更加全面;融合颜色特征后模型的校正集识别率均有所增加,但预测集识别率稍逊,颜色特征虽携带了部分有效信息,但这些信息与牛肉样本的相关性不大。因此,寻找与牛肉样本相关性更大的颜色特征是提高模型识别率的重要途径之一。该研究结果为牛肉品种的快速无损识别提供了一定的参考。     

First EMC3-EIRENE modelling of JT-60SA edge plasmas with/without resonant magnetic perturbation field

The first EMC3-EIRENE modelling for the JT-60SA edge plasmas with/without the resonant magnetic perturbation field (RMP) was conducted. Both core degradation in the vacuum approximation and strike-point splitting were observed due to the application of the RMP, as in previous studies in other devices. Toroidally averaged divertor heat fluxes with and without the RMP were fitted by using a one-dimensional diffusive model function, showing similar profiles. To extract the modulation components of the divertor heat flux profile, the proper orthogonal decomposition (POD) method was applied. By using the POD outputs, a modulation ratio with respect to the toroidally averaged profile was quantitatively calculated.     

不同加载边界下混凝土巴西劈裂过程及强度的DIC实验分析

平板、垫条、圆弧压模及平台试样等不同加载方式下, 脆性材料巴西劈裂实验结果的差异一直是人们所讨论的问题. 本文设计了混凝土平板直接加载与采用垫条加载实验, 采用理论、高速相机与数字图像相关法(digital image correlation, DIC)相结合的方法, 对试样表面应变场演化、起裂位置及裂纹扩展过程进行分析, 探讨了不同的加载边界对试样应变集中演化及劈裂拉伸强度结果的影响. 结果显示: (1)混凝土拉伸非线性特性导致的应变集中演化对不同加载条件非常敏感, 平板加载时应变集中较早在加载端起始并向中心演化, 即使满足巴西实验"中心起裂"条件, 其强度仍低于垫条加载情况, 两者差别达17.9%; (2)如果软垫条加载接触角合理设计, 与平板直接加载相比, 其应力场更稳定, 有利于保证圆盘试样的应变集中及断裂均从中心起始, 更好满足巴西劈裂实验条件; (3)仅校验巴西实验 "中心起裂"有效性条件是不充分的, 设计时必须谨慎考虑. 研究结果对脆性材料巴西劈裂实验设计、测试分析具有重要参考意义.      

Application of Novel Calix[4]arene Metal-free Sensitizers in Dye-sensitized Photoelectrochemical Cells for Water Splitting

A series of novel calix[4]arene metal-free dyes, featuring macrocyclic structure and unique conical conformation, has been introduced into photoanode-based dye-sensitized electrochemical cell system as photosensitizers. The electrochemical properties of the corresponding sensitized photoanodes were systematically studied in the absence/presence of water oxidation catalyst(WOC). Furthermore, the visible-light-driven overall water-splitting reactions were conducted by fully assembled devices, obtaining a performance trend of Calix-3 > Calix-2 > Calix-1. The corresponding device of Calix-3 exhibited the best photoactivity, giving an initial photocurrent density of ca. 300 μA/cm², an IPEC peak value of ca. 9.0% at 365 nm and a wide photo-respond band up to ca. 620 nm. The best performance of Calix-3 can be attributed to its most effective light-harvesting ability, best ICT transition property, highest oxidation potential and thus best ability of activating WOC. This work offers an inspiration for the application of new-type effective metal-free sensitizers in photocatalytic water-splitting device.     

Development of air‐assisted dispersive micro‐solid‐phase extraction‐based supramolecular solvent‐mediated Fe3O4@Cu–Fe–LDH for the determination of tramadol in biological samples

A simple method, air‐assisted dispersive micro‐solid‐phase extraction‐based supramolecular solvent was developed for the preconcentration of tramadol in biological samples prior to gas chromatography–flame ionization detection. A new type of carrier liquid, supramolecular solvent based on a mixture of 1‐dodecanol and tetrahydrofuran was combined with layered double hydroxide coated on a magnetic nanoparticle (Fe₃O₄@SiO₂@Cu–Fe–LDH). The supramolecular solvent was injected into the solution containing Fe₃O₄@SiO₂@Cu–Fe–LDH in order to provide high stability and dispersion of the sorbent without any stabilizer agent. Air assisted was applied to enhance the dispersion of the sorbent and solvent. A number of analytical techniques such as Fourier transform‐infrared spectrometry, field emission scanning electron microscope, energy‐dispersive X‐ray spectroscopy and X‐ray diffraction measurements were applied to assess the surface chemical characteristics of Fe₃O₄@SiO₂@Cu–Fe–LDH nanoparticles. The effects of important parameters on the extraction recovery were also investigated. Under optimized conditions, the limits of detection and quantification were obtained in the range of 0.9–2.4 and 2.7–7.5 μg L^?1 with preconcentration factors in the range of 450–472 in biological samples. This method was used for the determination of tramadol in biological samples (plasma, urine and saliva samples) with good recoveries.     

Bismuth Gadolinium Oxychloride with a Remarkable Visible-Light-Responsive O2 Evolution Activity Promoted by Iodine Doping

Visible-light-responsive bismuth-based oxyhalide has recently attracted extensive attention, however, the promotion of its charge separation is still challenging. Herein, we introduce iodine into Bi₂GdO₄Cl to synthetize I-doped Bi₂GdO₄Cl (denoted as yI−Bi₂GdO₄Cl, 0≤y≤2). The incorporation of I⁻ ions is found to enhance light absorption and to accelerate charge separation by combining various characterizations such as density functional theory calculation, photoelectrochemical test, electrochemical impedance spectroscopy, photoluminescence spectrum, and open-circuit voltage decay. The O₂-evolving performances of 1I−Bi₂GdO₄Cl with optimized dopant concentration of I⁻ ion and IrO₂ loaded 1I−Bi₂GdO₄Cl are tremendously enhanced by ca. 4 and 45 times compared to pristine Bi₂GdO₄Cl. Notably, The O₂ evolution rate reaches as high as 154.8 μmol ⋅ h⁻¹ with an apparent quantum efficiency of ∼1.1 % at 420 nm. The synthetic iodine-doped photocatalyst remains stable after long-term photoreaction, demonstrating its potential in the field of photocatalysis.     

Analytical methodologies for the determination of nitroimidazole residues in biological and environmental liquid samples: A review

Nitroimidazoles (NDZs) are antiprotozoal drugs that are typically used in veterinary and human medicine. NDZs and their metabolites are believed to possess genotoxic, carcinogenic and mutagenic properties, and this is (one reason) why their use has been banned within the European Union. Hence, the determination of trace residues of these substances in edible animal tissues has been of growing concern over the past few years. Even, though there has been a need to develop sensitive and reliable analytical methods to study the residues of these compounds in different matrices, available methodologies in environmental samples are rather limited. These and other pharmaceutical compounds have become one of the most important new classes of environmental pollutants that have been detected in wastewater-treatment-plant (WWTP) effluents, receiving waters, drinking water and groundwater. A compilation of the most representative analytical methodologies for the determination of NDZ residues during the last decade is presented in this paper. Its scope is the two main areas which require their determination, namely biological and environmental matrices. A detailed explanation of both areas, including sample treatment and detection systems, and future trends is presented, focusing on the difficulties of confirming analytes at low concentration levels.     

超声波破碎-高效液相色谱法定量检测核酸

采用超声波破碎结合高效液相色谱技术,建立了定量检测质粒DNA的方法,测量结果可以溯源至核苷酸标准物质.采用超声波破碎(功率300 W,频率24 kHz)技术将质粒DNA破碎成200～500 bp的小片段DNA,再用蛇毒磷酸二酯酶将其水解为4种核苷酸(dCMP:3.2 min;dTMP:4.7 min; dGMP:5.3...     

QSRR Study on the Components of Styrax Japonicus Sieb Flowers Using Improved Molecular Electronegativity-distance Vector （I-MEDV）

Atoms in most organic molecules are often carbon,oxygen,nitrogen,sulfur,halogens,etc. Based on the three-dimensional structure of a molecule,a molecular structural characterization(MSC) method called improved molecular electronegativity-distance vector(I-MEDV) was developed. It was used to describe the structures of 37 compounds of styrax japonicus sieb flowers. Through multiple linear regression(MLR),a QSRR model was built up. The correlation coefficient(R1) of the model was 0.980. Then,4 vectors were selected to build another model through the method of stepwise multiple regression(SMR) ,and the correlation coefficient(R2) of the model was 0.975. Moreover,all the two models were evaluated by performing the crossvalidation with the leave-one-out(LOO) procedure and the correlation coefficients(Rcv) were 0.948 and 0.968,respectively. The results show that the I-MEDV could successfully describe the structures of organic compounds. The stability and predictability of the models were good.