碱式碳酸铜制备实验的改进

以硫酸铜与氨水的反应原理为基础,对碳酸钠和硫酸铜为反应原料制备碱式碳酸铜实验进行了改进,即CuSO4溶液中滴加氨水,且反应一段时间后用酒精灯加热;并进一步探讨了反应物配比对样品的影响,依据TG曲线、XRD图谱对实验结果进行分析。结果表明：Na2CO3与CuSO4物质的量之比为1.0~1.6时可迅速看到绿色样品,样品均为纯相Cu2（OH）2CO3。改进后,实验耗时少,操作简便,现象明显,成功率高。     

正交实验法制备碱式碳酸铜及其组成测定

结合单因素实验,运用正交实验的方法,研究了实验室制备碱式碳酸铜中物料比、温度、时间3个因素对产率与组成的影响,并对产品进行红外表征。实验证明,影响产率的因素是物料比,影响反应速率的因素是温度,影响产品组成的主要因素是反应的时间。综合考虑产品组成、产率和实验课时间的因素,同浓度下硫酸铜和碳酸钠的体积比为1：1.2,反应温度75℃,初产品室温放置24 h,是最佳的制备条件。     

碱式碳酸铜的制备

以CuSO4.5H2O和Na2CO3为反应原料制备碱式碳酸铜。学生通过查阅文献制定实验方案,经指导教师同意后开展实验。通过改变反应物的配比、体系pH、反应温度等条件制备碱式碳酸铜;通过测定产物Cu2+含量、TG/DTG曲线等对产物品质进行初步分析。用反应的产率和反应速率综合判断较优制备条件。     

水杨酸甲酯制备实验的改进

"水杨酸甲酯的制备"是一个经典的有机化学实验，作为考核实验考查学生操作技能，并根据产品的质量和纯度给予学生成绩。教材中提供的实验方案不合理，导致学生制备产品的收率很低。对传统实验方法的不足之处进行分析，提出了先用碳酸钠中和硫酸（去除催化剂），再蒸馏分离甲醇的实验路线。改进的实验方案设计更合理，避免了水杨酸甲酯分解，提高了产品的收率，达到了良好的教学效果。     

大学无机化学实验中碱式碳酸铜制备方法探讨

探讨大学无机化学实验中有关碱式碳酸铜制备的实验方法,并以Cu(NO3)2为原料、NaOH和Na2CO3的混合液为沉淀剂制备碱式碳酸铜。讨论反应物最佳配比、pH、温度等因素对产品的影响,并对所制产品进行XRD分析,提出一种制备碱式碳酸铜的大学无机化学实验方法。     

以情境-实验-问题突破传统——“二氧化硅和信息材料”的教学

针对"二氧化硅和信息材料"这部分内容在传统教学过程中存在缺乏合适的实验探究活动、教学情境素材对学生的吸引力不强、对高纯硅制备的反应原理分析不够深入等问题，通过创设真实而富有价值的问题情境（手机芯片），设计纳米二氧化硅与氢氧化钠溶液反应等实验探究活动，设计帮助学生深度理解高纯硅制备原理的问题等一系列措施进行相应的教学改进，并在此基础上展开教学实践。     

镁铝原电池数字化实验的意外——再探铝与碱性溶液的反应

用电压传感器测得使用铝、镁作电极,氢氧化钠溶液或氨水作电解质的原电池,在放电过程中存在电极极性翻转现象,说明铝片不仅能与强碱反应,也能与氨水反应。该结论和铝片和氨水反应的试管实验的结果一致。换用碳酸钠溶液作电解质的原电池不存在电极极性翻转现象;结合试管实验中铝片与碳酸钠溶液反应的产物分析,发现有难溶于水的碱式碳酸钠铝生成,推测其覆盖在铝片表面,避免了电极极性翻转。     

一种快速生成铜锈的实验方法

本实验运用电化学的方法,将简单易得的材料用于快速制备铜锈,在几十秒到几分钟不等的时间就会迅速产生铜锈。依据XRD图谱对产物进行分析,确定了形成碱式氯化铜(Cu₂Cl-(OH)₃)的最佳电解质溶液配比,并成功制备了碱式碳酸铜(Cu₂(CO₃)(OH)₂)。实验结果可用作中学化学教学演示实验和学生实验,也可用于指导学生探究不同条件对铜锈制备的影响,进行探索性学习练习。此外,相关实验原理可提供试题情境对学生学习质量进行评价。     

温度对铜和浓硫酸反应的影响探究

铜和浓硫酸反应在高中化学教学中是一个演示实验,但在实验中经常会出现黑色物质,导致溶液变浑浊,很难观察到蓝色的硫酸铜溶液。从温度对该反应产物、现象的影响角度进行探究,发现可以通过控制反应温度,使反应出现明显的“溶液变蓝色”现象,并且使黑色固体生成的量明显减少。     

对乙酸乙酯制备实验中饱和碳酸钠溶液作用的定量研究

乙酸乙酯的制备实验,是中学化学教材中的一个比较重要的实验,收集乙酸乙酯时使用了饱和碳酸钠溶液。对于该实验,有几个问题困扰着我们:(1)饱和碳酸钠溶液起何作用?(2)可否用饱和碳酸氢钠溶液     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

Synthesis of phenolic components of Grains of Paradise

Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.     

Acid hydrolysis of carboxymethylcellulose of low degree of substitution

Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position.     

Study of hydration of two cements of different strengths

Main hydration products of two cement pastes, i.e. CSH-gel, portlandite (P) (and specific surface S) were studied by static heating, and by SEM, TEM and XRD, as a function of cement strength (C-33 and C-43) hydration time (th) and subsequent hydration in water vapour.Total change in mass on hydration and air drying, M_o, increased with strength of cement paste and with hydration time. Content of water escaping at 110 to 220°C, defined as water bound with low energy, mainly interlayer and hydrate water, was independent on cement strength but its content increased with (th). Content of chemically bound (zeolitic) water in CSH-gel, escaping at 220-400°C, was slightly dependent on strength and increased with (th). It was possibly derived from the dehydroxylation of CSH-gel and AFm phase. Portlandite water, escaping at 400-500°C, was independent on cement strength and was higher on longer hydration. Large P crystals were formed in the weaker cement paste C-33. Smaller crystals were formed in C-43 but they increased with (th). Carbonate formated on contact with air (calcite, vaterite and aragonite), decomposed in cement at 600-700^oC. It was high in pastes C-33(1 month) and C-43(1 month), i.e. 5.7 and 3.3%, respectively; it was less than 1% after 6 hydration months (low sensitivity to carbonation) in agreement with the XRD study showing carbonates in the air dry paste (1month), and its absence on prolonged hydration (6 months) and on acetone treatment. Water vapour treatment of (6 months) pastes or wetting-drying increased this sensitivity.Nanosized P-crystals, detected by TEM, could contribute to the cement strength; carbonate was observed on the rims of gel clusters.This revised version was published online in November 2005 with corrections to the Cover Date.     

Estimation of Kinetic Parameters of Thermal Oxidation of Ilmenite

The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of hematite Fe₂O₃. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the best fitting experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.     

Mechanism of action of base-catalyzed oxygenation of phenol derivatives

Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6.     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。     

化学计量中不确定度评定研究进展

测量不确定度是表征合理地赋予被测量之值的分散性的参数。本文针对化学计量不确定度评定基础模型仅适用于线性模型、概率分布为正态分布或缩放位移t分布等局限,介绍了近年来不确定度评定的研究热点:蒙特卡罗方法(Monte Carlo Method,MCM),不确定度评定的来源、评定概念、评估方法及其发展过程,扩大了测量不确定度评定与表示的适用范围。