Facile galvanic replacement deposition of nickel on copper substrate in deep eutectic solvent and its activation ability for electroless Ni–P plating

Journal of Solid State Electrochemistry - Electroless nickel-phosphorus plating is an important surface treatment method for copper due to its good corrosion resistance and nonmagnetic properties....     

n-In0.35Ga0.65N/p-Si异质结的制备及其电学性能研究

采用双光路双靶材脉冲激光沉积(PLD)系统在p-Si衬底上外延生长InGaN薄膜,研究了InGaN薄膜的显微组织结构和n-InGaN/p-Si异质结的电学性能。研究表明,InGaN薄膜为单晶结构,沿[0001]方向择优生长,薄膜表面光滑致密,In的原子含量为35%。霍尔(Hall)效应测试表明In_0.35Ga_0.65N薄膜呈n型半导体特性,具有高的载流子浓度和迁移率及低的电阻率。I-V曲线分析表明In_0.35Ga_0.65N/p-Si异质结具有良好的整流特性,在±4 V时的整流比为25,开路电压为1.32 V。In_0.35Ga_0.65N/p-Si异质结中存在热辅助载流子隧穿和复合隧穿两种电流传输机制。经拟合,得到异质结的反向饱和电流为1.05×10^-8 A,势垒高度为0.86 eV,理想因子为6.87。     

偏硼酸锂-四硼酸锂熔融-电感耦合等离子体原子发射光谱(ICP-AES)法测定石膏中多组分含量

石膏在我国储量丰富,应用广泛,快速准确分析其成分含量对石膏资源的综合利用具有重要意义。针对酸溶法无法测定SiO2,碱熔法无法测定K2O、Na2O的问题,本文建立一种偏硼酸锂-四硼酸锂熔融-电感耦合等离子体发射光谱法同时测定石膏中CaO、SO3、Al2O3、Fe2O3、MgO、TiO2、K2O、Na2O、SiO2含量。实验优化了熔剂用量、熔融温度,结果表明采用试样与偏硼酸锂-四硼酸锂混合熔剂质量比例1：5,在铂金坩埚中1000 ℃熔融10 min,在超声条件下,于50 mL 10 %盐酸中浸取熔融物,能够有效分解试样而浸取待测组分。向标准溶液系列中加入偏硼酸锂-四硼酸锂-盐酸基体溶液以消除基体对测试结果的影响。各待测组分的校准曲线的相关性系数均大于0.9990,方法检出限在3~292 μg/g范围内;采用实验方法分别对国家一级标准物质GBW03109a、GBW03110和实际样品进行测定,标准物质的5次平行测试的相对标准偏差在0.14 %~8.86 %之间,测定结果的相对误差在0.03~8.75 %之间,测试结果与标准值无显著性差异;实际样品中各成分测定值的RSD（n=5）为0.24~8.80 %。该方法操作简单、准确度高、精密度好、检出限低,可以同时测定石膏中的多组分含量,能够为石膏资源综合利用调查评价提供一定的技术支撑 。     

Preparation of D-histidine modified zeolitic imidazolate framework-90 coated capillary column and its application in open-tube capillary electrochromatography enantioseparation

Metal-organic framework materials are a class of novel crystalline porous materials with regular pore structures formed by covalent bonding between metal centers and organic functional groups. Metal-organic framework materials have attracted great interest in analytical chemistry due to their unique properties such as good stability and permanent porosity. In this work, D-histidine was used to carry out chiral modification of zeolitic imidazolate framework-90 under mild conditions, and the D-histidine modified zeolitic imidazolate framework-90 coated capillary column was prepared. This chiral capillary column was used to separate epinephrine, norepinephrine, terbutaline, and tryptophan enantiomers. Under optimum conditions, baseline separations were achieved. The intra-day, inter-day, and inter-column relative standard deviations (n = 3) of the four pairs of enantiomeric migration times were 0.15%–0.56%, 0.74%–2.40%, and 1.93%–3.18%, respectively. Moreover, the D-histidine modified zeolitic imidazolate framework-90 coated capillary could be reused for at least 150 runs without significant changes in the separation efficiency and migration time.     

HPLC柱效对检测水中磺胺二甲基嘧啶色谱条件的影响

研究色谱柱的柱效降低后对高效液相色谱测定水中磺胺二甲基嘧啶色谱条件的影响。比较了新旧色谱柱的分离效果、色谱峰的对称性和峰面积,结果表明,旧色谱柱的柱效降低,对目标物的分离效果变差,目标物的吸收峰面积变小,峰形不对称。对色谱条件进行了优化试验,结果表明,对流动相水相添加0.125%的冰乙酸调节p H值为4.5后色谱峰的峰形对称性和分离效果得到改善。     

Screening anti‐tumor compounds from Ligusticum wallichii using cell membrane chromatography combined with high‐performance liquid chromatography and mass spectrometry

Tyrosine 367 Cysteine‐fibroblast growth factor receptor 4 cell membrane chromatography combined with high‐performance liquid chromatography and mass spectrometry was developed. Tyrosine 367 Cysteine‐HEK293 cells were used as the cell membrane stationary phase. The specificity and reproducibility of the cell membrane chromatography was evaluated using 1‐tert‐butyl‐3‐{2‐[4‐(diethylamino)butylamino]‐6‐(3,5‐dimethoxyphenyl)pyrido[2,3‐d]pyrimidin‐7‐yl}urea, nimodipine and dexamethasone acetate. Then, anti‐tumor components acting on Tyrosine 367 Cysteine‐fibroblast growth factor receptor 4 were screened and identified from extracts of Ligusticum wallichii. Components from the extract were retained on the cell membrane chromatographic column. The retained fraction was directly eluted into high‐performance liquid chromatography with mass spectrometry system for separation and identification. Finally, Levistolide A was identified as an active component from Ligusticum wallichii extracts. The 3‐(4,5‐dimethylthiazol‐2‐yl)‐2,5‐diphenyl‐tetrazolium bromide‐formazan colorimetric assay revealed that Levistolide A inhibits proliferation of overexpressing the mutated receptor cells with dose‐dependent manner. Phosphorylation of fibroblast growth factor receptor 4 was also decrease under Levistolide A treatment. Flex dock simulation verified that Levistolide A could bind with the tyrosine kinase domain of fibroblast growth factor receptor 4. Therefore, Levistolide A screened by the cell membrane chromatography combined with high‐performance liquid chromatography and mass spectrometry can arrest cell growth. In conclusion, the two‐dimensional high‐performance liquid chromatography method can screen and identify potential anti‐tumor ingredients that specifically act on the tyrosine kinase domain of the mutated fibroblast growth factor receptor 4.     

金作保护剂铅试金分离富集石墨炉原子吸收光谱法测定矿石中痕量铑

铑矿石是获取铑的重要来源,但矿石中的铑含量极低,且分布不均匀,准确测定其含量一直是分析测试中的难题。本研究建立了一种可高效富集矿石中铑元素的铅试金——石墨炉原子吸收光谱分析方法。采用金作保护剂,铅试金分离富集矿石中的铑,形成的金-铑合金用王水溶解,石墨炉原子吸收光谱法进行测定。实验结果表明：熔剂配比m（硼砂）：m（纯碱）：m（黄丹粉）：m（淀粉）=5:5:10:1,加入15mg金做为保护剂,灰吹温度900℃,可完全富集50 μg铑。用石墨炉原子吸收光谱仪进行检测,方法的相对标准偏差RSD（n=11）为6.97%～11.23%,线性范围为0.17～50 μg?L-1,加标回收率为99.36%～100.94%,10倍于铑的其他共存贵金属对测定无干扰。方法准确、可靠、简便,可用于矿石样品中铑的日常分析。本研究对铑资源勘探开采及铑矿物的综合利用研究具有重要意义。     

Photometric determination of free cholesterol via cholesterol oxidase and carbon nanotube supported Prussian blue as a peroxidase mimic

Microchimica Acta - The authors describe a photometric method for the determination of free cholesterol based on the oxidation of cholesterol by the catalytic action of the enzyme...     

Copper-catalyzed regioselective allylic oxidation of olefins via C–H activation

A regioselective oxidation of allylic C–H bond to C–O bond catalyzed by copper (I) was developed with diacyl peroxides as oxidants. The oxidation of allylic C–H bond was accomplished with good yield and regioselectivity under mild reaction conditions. This method has a broad substrate scope including cyclic olefins, terminal and internal acyclic olefins and allyl benzene compounds. The reaction proceeds by a radical mechanism as suggested by spin trapping experiments.     

二氧化碳间接转化制化学品的研究进展

二氧化碳直接利用较为困难, 因此先将其转化为环碳酸酯等二氧化碳衍生物, 进而间接转化为其它化学品是实现二氧化碳资源化利用的重要手段之一, 具有良好的应用前景. 本文综合评述了二氧化碳转化为环碳酸酯继而间接利用的近期研究进展, 重点介绍了环碳酸酯的加氢反应、 醇解反应和氨解反应中的均相和多相催化体系, 对反应机理进行了阐述, 并展望了该领域仍待解决的问题和发展前景.