高效液相色谱法测定柴油族组成

在银型磺酸键合硅胶柱上以含苯或环己烯的正己烷为流动相,实现了饱和烃、烯烃的基线分离,以改进的迁移丝式氢火焰离子化检测器（ＭＷ－ＦＩＤ）进行定量检测,同时考察了Ａｇ－ＳＣＸ柱的使用性能及改进的ＭＷ－ＦＩＤ的定量准确性。在此基础上建立了高效液相色谱体系分离柴油族组成（饱和烃、烯烃、芳烃及胶质）。     

高效液相色谱—荧光检测法测定蒽和荧蒽

采用高效液相色谱－荧光检测法测定多环芳烃化合物蒽和荧蒽。在Ｓｈｉｍ－ｐａｃｋ ＣＬＣ－ｐｌｅｎｙｌ柱上，以５０％的乙腈水溶液作流动相，１２ｍｉｎ内实现了两组分的同时分离测定。线性范围为０－８０μｇ／ｍＬ，检测限低于５０ｎｇ／ｍＬ，相对标准偏差小于１％。     

高效液相色谱－荧光检测法测定蒽和荧蒽

采用高效液相色谱－荧光检测法测定多环芳烃化合物蒽和荧蒽。在Ｓｈｉｍ－ｐａｃｋＣＬＣ－ｐｈｅｎｙｌ柱上，以５０％的乙腈水溶液作流动相，１２ｍｉｎ内实现了两组分的同时分离测定。线性范围为０～８０μｇ／ｍＬ，检测限低于５０ｎｇ／ｍＬ，相对标准偏差小于１％。     

多环芳烃的超临界流体色谱分离研究

烃中多环芳烃（晕苯和卵苯）的分离是极其困难的。研究了在不同极性毛细管填充ＳＦＣ柱上多环芳烃的分离条件。选用国产１５０ｍｍＣＮ填充柱,ＣＯ＿２为流动相,线性升压,ＦＩＤ检测,可在２６ｍｉｎ内将烃中三到十环多环芳烃分离,定量重复性良好。     

聚丙烯酰胺存在下Mohr法直接滴定碘、银等离子和硫氰酸根

1引言　　　　经典莫尔法对于　０．０１　ｍｏｌ／Ｌ的Ｃｌ－滴定误差达十０．６％需要进行指示剂的空白校正．且因　Ａｇｌ、ＡｇＳＣＮ沉淀强烈吸附Ｉ－和ＳＣＮ－、Ａｇ２ＣｒＯ４。沉淀凝聚后再转化成ＡｇＣｌ极慢，故不适于直接滴定Ｉ－、ＳＣＮ－、Ａｇ－。作者以聚丙烯酰胺（ＰＡＭ）化学修饰ＡｇＸ（ｘ－＝Ｉ－、ＳＣＮ－、Ｂｒ－、Ｃｌ－）及Ａｇ２ＣｒＯ４沉淀的结构，减小Ａｇｘ对Ｘ－的吸附与促进Ａｇ２ＣｒＯ４的转化，用莫尔法直接测定Ｉ－、ＳＣＮ－、Ａｇ＋及不需空白校正能准确滴定　０．０１　ｍｏｌ／ＬＣｌ－未见报道…     

使用C18固要萃取膜—色质联用定量分析饮用水中痕量多环芳烃的初步 …

参照美国ＥＰＡ５２５．１方法,Ｃ１８－固相萃取膜萃取饮用水中的有机物,利用ＧＣ／ＭＳ法鉴定多环芳烃（ＰＡＨＳ）,使用１６种多环芳烃混合标准样绘制标准曲线,以内标法对ＰＡＨＳ进行定量分析。采用本方法某水厂经过深度处理后的出厂水中的７种多环芳烃的含量,ＰＡＨＳ的平均回收率为９４．０－９７．７％。检测限为０．００１μｇ／Ｌ。     

活性碳纤维ZnO—SACF氧化还原机理的研究

本文借助于ＩＲ，ＴＧ和ＸＰＳ，研究了ＺｎＯ－ＳＡＣＦ制备过程中及其吸附Ａｇ＾＋和Ａｕ＾３＋前后的化学结构变化。实验结果表明：从ＳＡＣＦ到ＺｎＯ－ＳＡＣＦ，纤维表面上的Ｏ／Ｃ原子比和含氧基团如Ｃ＝Ｏ和ＣＯＯ都有所减少；ＺｎＯ－ＳＡＣＦ上还原性功能基团主要是－Ｃ－ＯＨ，当ＺｎＯ－ＳＡＣＦ吸附Ａｇ＾＋后，－Ｃ－ＯＨ被氧化为－Ｃ＝Ｏ，而当其吸附Ａｕ＾３＋后，－Ｃ－ＰＨ被氧化为－Ｃ＝Ｏ和－（Ｏ＝Ｃ）－ＯＨ，     

二—（2,4,4—三甲基戊基）膦酸浸渍树脂分离Tb^3＋,Dy^3＋,Ho^3＋,Er^3＋的研究

研究了大孔风状树脂ＸＡＤ－Ｒ,ＸＡＤ－７,ＸＡＤ－１１８０对二－（２,４,４－三甲基戊基）膦酸浸渍树脂的吸附及制备方法,并对Ｃｙａｎｅｘ５７１浸渍树脂分离稀土的性能进行了研究,发现在盐酸介质中Ｃｙａｎｅｘ５７１／ＸＡＤ－７具有最强的萃取能力,树脂中的萃取剂含量在０．３５－０．４５ｇ．ｇ＾－１时,其萃取性能最好,将上述浸渍树装入色层柱对稀土元素进行了分离,且降低负载量和流速分离效果量好。     

单柱离子色谱法测定过热器管垢和锅炉垢中铁、镁和钙的含量

首先用碱熔融法分解试样,然后加抗坏血酸将试液中的Ｆｅ３＋还原为Ｆｅ２＋,再用离子色谱法测定试液中的Ｆｅ２＋,Ｍｇ２＋和Ｃａ２＋。采用Ｓｈｉｍ－ｐａｃｋＩＣ－Ｃｌ阳离子交换柱分离样品离子,以０．２５ｍｍｏｌ／Ｌ乙二胺－０．５０ｍｍｏｌ／Ｌ柠檬酸（ｐＨ４．５０）为流动相,以ＣＤＤ－６Ａ电导检测器检测,使被测组分得到满意的分离和检测。Ｆｅ,Ｍｇ和Ｃａ的加标回收率均在９０％以上。测定结果与原子吸收光谱法测定结果相近。     

C_(60)键合硅胶液相色谱固定相的合成及其性能评价

 以γ－（乙二胺基）丙基三乙氧基硅烷为偶联剂合成了Ｃ６０键合硅胶固定相；用元素分析法测定得到该固定相的Ｃ６０键合量为５７．５７μｍｏｌ／ｇ。考察了多环芳烃和杯芳烃在Ｃ６０键合硅胶固定相上的分离，多环芳烃在该固定相上的洗脱顺序与ＯＤＳ固定相相似；杯芳烃的洗脱顺序为杯［８］、杯［４］和杯［６］芳烃。     

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.     

恶臭嗅辨实验室建设探讨

针对恶臭测试的环境影响问题,提出了解决的实例方案,并对方案的要点及优缺点进行讨论,此方案在实际操作中具有较好的效果。     

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.

     

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。     

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.     

解决能源问题的新途径——光解水制氢的研究

面对日益枯竭的能源危机,氢能是一种洁净、最有前景的替代能源。目前在各种制氢的方法中光催化分解水制氢的研究最多,光解水过程中催化剂最关键,本文对利用太阳能光解水的途径、提高光催化反应效率以及光催化剂的开发研究进行了综述。     

黄酮化合物的合成研究进展

黄酮化合物是一类具有多种生物活性的天然产物,其经典的合成方法主要为查耳酮路线和β-丙二酮路线.近年来出现了许多新技术、新方法.本文介绍了2'-羟基查尔酮的氧化关环法、黄烷酮氧化法、改进的Baker-Venkataraman法及其他合成黄酮化合物的方法.     

Summary of development of the theory of stability of colloids and thin films

In this review, the research of the author in the field of colloidal systems is summarized. The factors influencing colloidal stability are systematized and analyzed. Examples are presented to illustrate the practical utilization of the theory of stability of colloids and thin films.This review was prepared on the basis of the works of the author, which were awarded the State Premium for 1991 in the field of science and technology, chemistry section.Institute of Physical Chemistry, Russian Academy of Sciences, 117915 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 8, pp. 1708–1717, August, 1992.     

NiY分子筛表面酸性影响其选择性吸附脱硫性能的机理研究

采用原位红外光谱技术,以噻吩、环己烯和苯为模型探针分子,分别考察单一烃分子在NiY分子筛上的吸附与反应行为以及噻吩与烯烃、芳烃间的竞争吸附和催化反应行为。单一探针分子吸附研究发现,NiY分子筛中与Ni物种相关的Lewis(L)酸位是噻吩的选择性吸附活性位;噻吩和环己烯在NiY分子筛中Brnsted(B)酸位上发生的质子化和低聚反应明显弱于HY分子筛。双探针分子竞争吸附研究发现,环己烯二聚体在NiY中强B酸位上的强化学吸附与噻吩存在显著的竞争吸附行为。另外,苯和噻吩在NiY上的竞争吸附现象在373K时明显减弱。由此,在选择性吸附脱硫过程中,减少吸附剂表面B酸中心可降低烯烃对噻吩的竞争吸附,另外适当提高吸附体系的温度可以有效避免芳烃对噻吩的竞争吸附。     

化学单元教学设计的探索

论述了单元教学是落实化学新课程三维目标的基本教学过程,同时对教学单元的含义、教学单元的选择与建构、化学单元教学设计及其意义进行了阐述。