水玻璃模数的快速测定

水玻璃是含水的多硅酸钠 ,为粘稠状液体。在建筑上常用作接合剂或胶粘剂 ,也是生产耐酸水泥的重要原料之一。其主要成分为氧化钠、二氧化硅和水分。水玻璃模数是指水玻璃试样中二氧化硅与氧化钠的含量之比。通常的做法是分别测出两者的质量分数然后算出。但是在实际应用中 ,用户往往并不需要知道二氧化硅和氧化钠的实际含量 ,而只需了解两者含量的比例即水玻璃的模数即可。为此本法提出水玻璃模数的快速测定法 ,并进行了理论推导。1　理论推导水玻璃中的硅酸钠水解后生成硅酸和氢氧化钠 ,由于硅酸为弱酸 ,所以水玻璃溶液显碱性。可用盐酸标…     

水玻璃模数快速测定法

模数,是衡量水玻璃产品质量好坏的一个重要指标。它是指水玻璃产品中二氧化硅物质的量与氧化钠物质的量之比,以n表示。因此,模数的大小,间接地反映了二氧化硅与氧化钠含量的高低。     

读者园地

问:GB/T 4209-1996,工业硅酸钠[S],JB/T 8835-1999,铸造用水玻璃[S]等将模数定义为二氧化硅摩尔数与氧化钠摩尔数之比(这个定义与传统意义上的模数也相一致),所以模数为wwNSiaO22O×1.032,如果同一份试样用同一盐酸标准溶液滴定,那么模数的计算式应是0.5×VV12。为什么相同的滴定数据,就可产生不同的测定结果?武汉读者———李传启答:(1)关于模数的定义早期文献与之后制定的标准中有差别,以往常称为“含二氧化硅与氧化钠的比率”,“二氧化硅与氧化钠含量之比”及“二氧化硅与氧化钠质量之比”等。由于分析者理解上的不同常引起一些议…     

容量法测碱度时指示剂的改进

在水质分析中用容量法测定甲基橙碱度时常用0.1％甲基瞪作指示剂,由于甲基瞪终点不够灵敏,红黄界限不明,误差较大。曾有人改用甲基红-亚甲基蓝混合指示剂,这种指示剂灵敏度较高,终点界限也很清楚,但是由于混合指示剂是用96％的酒精溶液配制,久置后由于甲基红     

甲基橙作指示剂误差究竟有多大——关于强酸强碱滴定时指示剂的选择

现行高中化学教材第二册(人教版),酸碱中和滴定的指示剂仅选择了酚酞,有些人认为不选甲基橙的原因是使用甲基橙时的误差太大。对于强酸、强碱之间的中和滴定,使用甲基橙和酚酞的误差到底有多大呢?我们不妨以0·1 mol/L的NaOH和0·1 mol/L HCl之间的滴定为例,通过计算来说明一下     

甲基橙在酸性溶液中的变色机理

早在18世纪80年代,甲基橙就作为指示剂而用于酸碱滴定,现在已成为酸碱滴定中最常应用的三种指示剂(酚酞、甲基橙、甲基红)之一。甲基橙是对氨基偶氮苯的衍生物,其结构式为:     

NiO亚微米球的制备及其光催化性质

在混合溶剂体系中,通过简单的二步方法成功合成了NiO亚微米球。第一步,以Ni(CH3COO)2和精氨酸为主要反应物,160℃溶剂热反应8 h制备出前驱体;第二步,煅烧前驱体成功合成了NiO产物。利用X射线粉末衍射(XRD),扫描电子显微镜(SEM),透射电子显微镜(TEM),热重分析(TGA)等手段对产物进行了表征。在紫外光照射下,研究不同光催化剂对甲基橙溶液降解效果。结果表明,NiO亚微米球在紫外光照射条件下对甲基橙溶液有光降解作用。     

光度法测定甲基橙和二甲基黄在甲醇—水混合溶剂中的离解常数

利用光度法测定了酸碱指示剂甲基橙（ＭＯ）和二甲基黄（ＤＹ）在０％～９０％（Ｖ／Ｖ）和３５％～８４％（Ｖ／Ｖ）甲醇－水混合溶剂中的离散常数ｐＫａ（２５℃，离子强度Ｉ＝０．１ｍｏｌ／ＬＫＣｌ）实验结果表明，随着混合溶剂中甲醇含量的增加，两种指示剂的ｐＫａ均不断减小，当混合溶液中甲醇含量小于７５％时，ｐＫａ同甲醇的摩尔分数Ｘ２之间存在着良好的线性关系。甲醇的加入，指示剂在可见光区的吸收光谱有较明显的改变     

对二甲基氨基偶氮苯染料共振瑞利散射法测定红霉素

在pH 4的HCl介质中,对二甲基氨基偶氮苯染料在50℃下可与红霉素作用形成稳定的离子缔合物。冷却至室温后在荧光分光光度计上同步扫描得到各溶液的共振瑞利散射光谱,发现单一的红霉素溶液的最大响应波长在334 nm附近,波峰和坡度变化均不明显;而与对二甲基氨基偶氮苯染料反应后最大响应波长增加到368 nm(甲基橙体系)和356 nm(甲基红体系)附近,在597 nm附近还有一肩峰,波峰、波谷分明;散射强度I也明显增强,且强度与红霉素质量浓度成正比,分别在0~50 mg/L或0~80 mg/L范围内符合Beer定律,线性回归方程为:IRRS=7.745×104ρ-15.17,r=0.9855(对甲基橙体系),IRRS=1.139×105ρ-36.91,r=0.9913(对甲基红体系)。据此,建立了测定红霉素的共振瑞利散射新方法,检出限可达0.15μg/mL。方法应用于红霉素肠溶片中红霉素的质量分析,加标回收率在97.6%~103.9%之间。     

聚苯胺/凹凸棒石负载纳米铁降解水溶液中甲基橙

以聚苯胺/凹凸棒石(PANI/ATP)为载体,采用液相还原法合成了负载型纳米零价铁(nZVI),用扫描电子显微镜(SEM)、透射电子显微镜(TEM)及X射线光电子能谱分析仪(XPS)等技术手段对纳米复合材料进行表征,考察了反应时间和pH值对甲基橙降解性能的影响,对降解过程进行了动力学分析,探讨了nZVI/PANI/ATP复合材料对甲基橙的降解机理。 结果表明,nZVI/PANI/ATP复合材料在较大pH值范围内能有效降解水中甲基橙并具有降解长效性,当催化剂用量1.0 g/L,降解体积50 mL,甲基橙的浓度20 mg/L,降解时间30 min时,复合材料对甲基橙的降解率达到95.8%以上,对甲基橙的降解过程符合准二级动力学模型。     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

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.     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

Calculation of enthalpies of hydrogenation of hydrocarbons

Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.     

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。