罗丹明B共振光散射法测定阴离子表面活性剂

在B-R缓冲溶液中,基于罗丹明B与阴离子表面活性剂(ASF)产生强烈共振光散射增强效应,建立了一种测定阴离子表面活性剂(SDS和SDBS)的方法。试验发现对于SDS和SDBS,最大共振光散射峰位于518和373 nm处。方法具有高的灵敏度,检出限分别为0.023 mg.L-1(SDS)和0.038 mg.L-1(SDBS),用于合成样和环境水样中阴离子表面活性剂含量的测定,回收率为94.0%~105.0%之间,并与亚甲蓝光度法相比,结果满意,可用于环境水样中阴离子表面活性剂的测定。     

非离子表面活性剂和无机阴离子对Be-CAS-CTMAB体系增敏作用的研究

本文研究了非离子表面活性剂及无机阴离子对Be-CAS-CTMAB、Al-CAS-CTMAB体系显色反应的影响,并探讨了非离子表面活性剂、无机阴离子的作用机理及规律。实验表明,两者的加入均起列进一步提高反应的灵敏度,增加配合物的稳定性,改善反应条件,展宽反应适宜pH范围等作用,实验了多种物质对测定铍的影响,建立了合金及水样中微量铍的测定方法。     

原子吸收光谱法测定水中微量PEO非离子型表面活性剂的研究

叙述了原子吸收光谱法间接测定水中微量非离子型表面活性剂的分析原理、条件和方法。该法主要是根据聚氧乙烯（ＰＥＯ）型表面活性剂能与钡盐和磷钼酸铵定量生成络盐沉淀，且络盐中Ｍｏ与ＰＥＯ有较大的摩尔比，因而在试样的萃取液中沉淀表面活性剂，然后通过原子吸收光谱法测定沉淀中Ｍｏ的含量，能间接测定表面活性剂含量。回收实验表明，该法灵敏度、选择性和重现性均较好，适宜测定水中微量非离子型表面活性剂。     

流动注射在线萃取荧光法测定痕量阴离子表面活性剂

报道了痕量阴离子表面活性剂的流动注射在线萃取荧光分析方法．该方法测定的线性范围为 ０．０１～０． ２０ ｍｇ／Ｌ；进样频率为 ２０样／ｈ．应用本法测定了水样中痕量阴离子表面活性剂，得到了满意的结果．     

阳离子表面活性剂的间接原子吸收分光光度法测定

在HAc-NaAc的缓冲溶液中，银离子与过量的溴离子反应生成的配阴离子能与阳离子表面活性剂十六烷基三甲基溴化铵(CTMAB)反应，生成白色的离子缔合物沉淀，该沉淀经离心分离后，用氨水溶解，以火焰原子吸收分光光度计测定溶液中银的吸收值，从而可间接求得阳离子表面活性剂CTMAB的含量；该法的线性范围为8．0～120．0mg/L，方法可应用于合成水样和护发素样品中CTMAB含量的分析，加入回收试验的回收率在95％～106％。     

两性表面活性剂胶束增溶显色反应的应用及机理的研究 Ⅰ.DDMAA-CAS高灵敏度分光光度法测定微量铝

将阳离子表面活性剂、非离子表面活性剂和阴阳离子表面活性剂应用于铝(Al)-铬天青S(CAS)体系以测定微量铝,已有不少报导,对提高反应的灵敏度,改善反应条件取得了良好的效果,有的体系已用于钢铁中微量铝的测定。我们曾把两性表面活性剂用于稀士元素的分析,表现出灵敏度高,选择性强,水溶性、稳定性好等优点。本文试图把两性表面活性剂应用于Al-CAS体系,研究其分光光度性质和反应机理,并寻求一个高灵敏度测定微量铝的新方法。试验证明,两性表面活性剂:N-十二烷基二甲基铵基乙酸(DDMAA),N-十二烷基二聚氧乙烯铵基乙酸(DDPAA)均能与铝、铬天青S形成三元胶束络合物,并表现出突出     

表面活性剂增敏阻抑动力学光度法测定痕量草酸

在稀盐酸介质中，微量草酸对H2O2氧化靛红的褪色反应有显著的阻抑作用，非离子表面活性剂Triton X-100对此体系有强烈的增敏作用，据此建立了表面活性剂增敏阻抑动力学光度分析测定微量草酸的新方法。方法的线性范围是0．005-0．50mg/L，检出限为0．005mg/L。方法简便，快速，灵敏度高，用于菠菜和尿样中草酸含量的测定，结果满意。     

催化动力学光度法测定阴离子表面活性剂

基于在H2SO4介质中,阴离子表面活性剂对高碘酸钠氧化罗丹明B褪色的反应具有较强的催化作用,建立了测定阴离子表面活性剂的催化动力学光度法.本文以十二烷基硫酸钠为标准品进行实验,线性范围为0.08～0.20 mg/L,检出限为0.0193 mg/L.用于水样中阴离子表面活性剂总量的测定,测定结果的相对标准偏差为1.3%～1.4%,回收率为104%～106%.     

4,5—二溴苯基荧光酮和十二烷基硫酸钠吸光光度法测定锗

用取代苯基荧光酮作为显色列的胶束增敏吸光光度法测定锗已有不少报道.形成的多元体系中,各种类型表面活性剂都有应用,但以阳离于表面活性剂为主,而阴离子及两性表面活性剂则极少报道.笔者通过试验发现,使用阴离子表面活性剂十二烷基硫酸钠(SDS)参与锗与4,5-二溴苯基荧光酮(DBPF)的显色反应.不仅具有较高灵敏度,而且具有很好选择性.低价金属离子及非金属离子均不干扰锗的测定.易产生干扰的高价金属离子的允许存在量均达数百微克以上,优于已有的光度法测定锗的所有体系.直接测定了煤样中微量锗,方法简便快速,获满意结果.     

1-(5-萘酚-7-磺酸)-3-[4-(苯基偶氮)苯基]-三氮烯-溴化十六烷基三甲胺-阴离子表面活性剂的显色反应

1-(5-萘酚-7-磺酸)-3-[4-(苯基偶氮)苯基]-三氮烯(NSPAPT),在三乙醇铵介质和溴化十六烷基三甲胺(CTMAB)存在下,与阴离子表面活性剂(AS),十二烷基苯磺酸钠(DBOSO3Na)、十二烷基磺酸钠(DOSO3Na)、十二烷基硫酸钠(DSO4Na)分别形成1∶2紫红色配合物,配合物最大吸收峰位于598 nm,此方法应用于水样中微量阴离子表面活性剂的分析,所得结果的RSD均小于2%,且与亚甲基蓝光度法的测定结果相符。     

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。