工业废水中苯并[a]芘的高效液相色谱法测定

工业废水中苯并［ａ］芘的高效液相色谱法测定汤加云高恩革（攀枝花钢铁（集团）公司劳动卫生防护研究所攀枝花６１７０２３）关键词工业废水苯并（ａ）芘高效液相色谱法萃取中图分类号Ｏ６５７．７２苯并［ａ］芘简称Ｂａｐ，又名３，４－苯并芘，是一种由五个苯环构成的...     

4,4‘二氯二苯砜部分水解制取4—氯—4’羟基二苯砜

用高效液相色谱法对４，４＇－二氯二苯砜（双氯），４，４＇－二羟基二苯砜（双酚）及４－氯－４＇－羟基二苯砜（单酚）进行了完全的分离，研究双氯部分水解制单酚发现，ＮａＯＨ用量越大，反应温度越高，水解速度越快，极值产率却越低；副产物双酚的含量随着反应时间增加，超过极值单酚产率的，由于副产物的增加，产率相对降低，最佳水解条件为水解温度１３５－１４０℃，ＮａＯＨ／双氯（摩尔比）为３．２５：１水解时间２．５－     

牙本质中天冬氨酸消旋化程度的测定——手性毛细管气相色谱法与高效液相色谱法的比较

 应用手性毛细管气相色谱法（酸性异丙醇、三氟乙酸酐为衍生试剂）、高效液相色谱法（邻苯二甲醛－Ｎ－乙酰－Ｌ－半胱氨酸为手性衍生试剂）同时测定人类第一磨牙牙本质中天冬氨酸的消旋化程度，结果表明，两者均可有效地用于天冬氨酸对映体的分离测定，但气相色谱检测限（０．２ｐｍｏｌ）低于高效液相色谱（１．０ｐｍｏｌ），而变异系数（７％）、总分析时间（１００ｍｉｎ）均高于高效液相色谱（分别对应为４％，３１ｍｉｎ）。     

牙本质中天冬氨酸消旋化程度的测定——手性毛细管气相色谱法与高效液相色谱法的比较

应用手性毛细管气相色谱法（酸性异丙醇、三氟乙酸酐为衍生试剂）、高效液相色谱法（邻苯二甲醛－Ｎ－乙酰－Ｌ－半胱氨酸为手性衍生试剂）同时测定人类第一磨牙牙本质中天冬氨酸的消旋化程度，结果表明，两者均可有效地用于天冬氨酸对映体的分离测定，但气相色谱检测限（０．２ｐｍｏｌ）低于高效液相色谱（１．０ｐｍｏｌ），而变异系数（７％）、总分析时间（１００ｍｉｎ）均高于高效液相色谱（分别对应为４％，３１ｍｉｎ）。     

4，4＇－二氯二苯砜部分水解制取4－氯－4＇－羟基二苯砜

用高效液相色谱法（ＨＰＬＣ）对４，４＇－二氯二苯砜（双氯），４，４＇二羟基二苯砜（双酚）及４－氯－４＇－羧基二苯砜（单酚）进行了完全的分离，研究双氯部分水解制单酚发现，ＮａＯＨ用量越大、反应温度越高，水解速度越快，极值产率却越低；副产物双酚的含量随着反应时间增加，超过极值单酚产率后，由于副产物的增加，产率相对降低。最佳水解条件为水解温度１３５～１４０℃，ＮａＯＨ／双氯（摩尔比）为３．２５∶１，水解时间２．５～３小时，产率９０％以上。另外，还对水解过程中的缩聚现象及产物的纯化条件进行了讨论。     

用反相高效液相色谱法纯化白细胞介素－2条件初探

用反相高效液相色谱法纯化白细胞介素－２条件初探胡明（沈阳军区军事医学研究所沈阳１１００３１）关键词反相高效液相色谱法，白细胞介素－２１前言高效液相色谱法（ＨＰＬＣ）是一项分辨率很高的液相色谱技术，具有速度快，灵敏度高、样品可回收等优点。除被广泛地应用...     

反相高效液相色谱法拆分α-氯代丙酰替苯胺光学异构体

采用反相高效液相色谱法在手性柱上分离芳氧基丙酸类除草剂中间体α－氯代丙酰替苯胺的光学异构体。实验结果表明,在三苯甲酸纤维素酯（CTB）手性柱上,以无水乙醇为流动相时,能在较大程度上拆分－α－氯代丙酰替苯胺的光学异构体,其分离因子为1．52,分离度Rh为0．60。     

氯吡苯脲标准物质的研制

采用半制备液相色谱法制备了氯吡苯脲标准物质。以UV,IR,MS和NMR方法对氯吡苯脲标准物质进行定性分析,高效液相色谱方法进行了均匀性检验和稳定性检验,经F检验表明,在置信区间为95%的范围内测定结果稳定性良好。利用国内8家资质合格的实验室进行联合定值,计算出不确定度。氯吡苯脲标准物质的定值结果为99.92%,在置信区间为95%的扩展不确定度为0.06%(k=2)。该氯吡苯脲标准物质可用于有关农药残留检测方法的校正。     

α－取代苯甲醇类化合物对映体的高效液相色谱法分离

 采用高效液相色谱法，用ＯＤ手性色谱柱直接分离α－取代苯甲醇类化合物的对映异构体。研究了流动相组成比例的改变对化合物对映体的分离色谱保留行为的影响，并将已知标准旋光的手性化合物采用高效液相色谱法拆分数据计算出的对映体过量百分值（ｅ．ｅ．％）与旋光仪测得的过量百分值（Ｏ．Ｐ％）进行了比较。     

α－取代苯甲醇类化合物对映体的高效液相色谱法分离

采用高效液相色谱法，用ＯＤ手性色谱柱直接分离α－取代苯甲醇类化合物的对映异构体。研究了流动相组成比例的改变对化合物对映体的分离色谱保留行为的影响，并将已知标准旋光的手性化合物采用高效液相色谱法拆分数据计算出的对映体过量百分值（ｅ．ｅ．％）与旋光仪测得的过量百分值（Ｏ．Ｐ％）进行了比较。     

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.     

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。     

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.

     

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.     

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.     

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.     

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^-。     

Thermodynamics of the formation of oxosulfides of rare-earth elements

The enthalpies of solution of several oxosulfides of rare-earth elements and the high-temperature enthalpies of oxosulfides and oxosulfates of lanthanum and yttrium were measured using solution calorimetry and high-temperature microcalorimetry techniques. Standard enthalpies of formation and some thermodynamic properties of oxosulfides and oxosulfates were calculated. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2 pp. 294–297, February, 1997.     

探究“铁的锈蚀条件”实验创新设计

设计了铁的锈蚀实验,说明了铁钉的处理方法,增加了温度、酸、碱的影响条件,实现了铁跟蒸馏水及空气中氧气快速反应而生锈,使实验在5 min左右就能够得到准确的结果。