2,4-二羟基苯乙酮苯腙荧光猝灭法测定铜

1 引 言胺类试剂是一类理想的荧光分析试剂,用其测定Al3+、Ga3+、Zn3+已显示出其灵敏度高、选择性好的优点。现虽有腙试剂荧光法测铜的报道,但这些方法检出限多数都在1μg/L以上,尚未见2,4-二羟基苯乙酮苯腙在荧光分析中的应用报道。本文首次合成了2,4-二羟基苯乙酮苯腙,研究了该试剂与铜荧光猝灭反应的最佳条件,建立的分析方法的检出限为0.22μg/L。方法用于矿泉水中铜的测定,结果满意。     

苯偶氮水杨醛异烟酰腙与镉的高灵敏度荧光反应及其应用

1引言镉是一种剧毒重金属。长期接触镉,能引起多种癌症。人们急需各种改进的方法来检测各种环境样品、工业废水以及生物组织里的Cd2 含量。本研究合成了新荧光试剂苯偶氮水杨醛异烟酰腙(BSIH),实验了试剂与镉的荧光反应新体系的最适宜条件。建立了一个新的测定痕量镉的荧光分析方法,方法的线性范围为0.6~120.0μg/L;检出限为0.32μg/L,方法成功地应用于自来水、河水和废水中镉的测定。2实验部分2.1仪器与试剂RF-5000型荧光光度计(日本岛津公司);PHS-2C型pH计(上海雷磁仪器厂);Cd2 标准溶液1 g/L;标准工作液:1μg/L;1×10-4mol/L苯偶…     

交联聚合β-环糊精-邻香草醛苯甲酰腙的合成及其应用

合成了交联聚合β-环糊精-邻香草醛苯甲酰腙(β-CDP-OVBH)的新型主体试剂,并进行了IR及NMR结构分析.研究了该主体试剂与铝离子的识别荧光反应,确定了反应的最佳条件,在pH=4.80的HOAc-NH₄OAc缓冲溶液和3.00 mL二甲基甲酰胺(DMF)介质中,主体试剂与客体铝离子配位生成摩尔比β-CDP-OVBH:Al³⁺为1:1的强荧光包合物,建立了测定Al³⁺荧光分析新方法.该方法线性范围为0.67～150 μg/L,检测限0.20 μg/L;通过对27种常见离子干扰实验的研究,显示出该主体试剂对客体铝离子有很高的选择性.该方法能够快速、简便地用于注射液、饮料中痕量铝的测定,结果令人满意.     

铝-水杨醛苯甲酰腙荧光反应的研究及应用

本文研究了Al~(3+)-水杨醛苯甲酰腙高灵敏度荧光体系,络合物的荧光激发波长=375nm,发射波长=450nm。铝量在0～1.4μg/10ml范围内,荧光强度与其含量成正比,灵敏度为0.4ppb。方法可用于试剂中微量铝的检测,结果令人满意。     

抑制动力学流动注射分光光度法测定甲醛的研究

实验中发现，在pH=8.0的磷酸缓冲溶液介质中，SO3^2-能迅速还原孔雀绿褪色，甲醛对该褪色反应具有强的抑制作用，氯化十六烷基吡啶对该体系有明显的增敏效应，同时还能进一步增强甲醛的抑制作用。研究了最佳条件，考察了共存物质的影响，建立了抑制动力学流动注射分光光度测定甲醛的新方法。方法的线性范围为0．055－3．00μg/mL，检出限为0．018μg/mL，不需要特殊的试剂，用于饮料中甲醛的测定，结果满意。     

流动注射催化光度法测定微量钒

采用流动注射与催化动力学光度法相结合,研究了在H3PO4介质中微量钒(Ⅴ)催化溴酸钾氧化吡啶偶氮变色酸试剂-2-(5-硝基-2-吡啶偶氮)-1,8-二羟基萘-3,6二磺酸(简称5-NO2-PACA)褪色反应,建立了测定微量钒的新方法。该方法线性范围为0.02~0.20μg/mL,线性回归方程为:ΔA=-0.004 2.63ρ(μg/mL),相关系数r=0.9988,检出限为:4.1×10-6g/L。方法已用于水样中微量钒的测定。     

酰腙类Schiff碱汞(Ⅱ)配合物的合成及晶体结构

合成了Schiff碱配体3-乙酰吡啶缩邻氨基苯甲酰腙(L1)及4-乙酰吡啶缩邻氨基苯甲酰腙(L2),并分别与Hg Cl2进行了配位反应,得到2个配位聚合物{[Hg(L1)Cl2]·CH3OH}n(1)和[Hg(L2)Cl2]n(2),采用1H NMR、FTIR和元素分析等手段对化合物进行了表征,并对配合物的热稳定性进行了考察。通过X射线单晶体衍射技术测定了2个配合物的单晶结构,结构解析表明,配合物1属于三斜晶系,P1空间群,配合物2属于单斜晶系,P21/n空间群。     

新型主体试剂交联聚合β-环糊精-邻香草醛苯甲酰腙的合成及荧光法识别锌

合成了新型主体试剂交联聚合 β 环糊精 邻香草醛苯甲酰腙 (β CDP OVBH) ,探讨了与Zn2 + 的荧光识别反应。在pH =8.30的NH3·H2 O NH4 Ac ,5 .0 0mLDMF中 ,β CDP OVBH与Zn2 + 络合生成 1∶1的包合物 ;线性范围 2 .5 0～ 5 0 0 μg L ;检测限 0 .6 0 8μg L ;2 8种常见离子干扰实验的研究 ,显示出该主体试剂对客体Zn2 + 有较高的选择识别效果。方法简便、快速地用于茶叶、人发中痕量锌的测定 ,结果满意。     

流动注射分光光度法测定皮革制品中的甲醛

研究了流动注射变色酸分光光度法测定皮革制品中的甲醛。与传统的变色酸光度法相比,该方法具有灵敏度更高,干扰更少的特点。在0.4 mol/L硫酸介质中,甲醛与变色酸在85℃左右形成络合物,该络合物在390 nm有最大吸收峰,且能稳定存在至少96 h。详细考察了各种测试条件如萃取剂、萃取时间、显色时间、反应温度、反应时间等对甲醛测定结果的影响,优化了反应的化学因素和流动注射系统反应条件。该方法的检出限和线性范围分别为0.1μg/L(3σ)和50~1000μg/L,相对标准偏差为0.56%(连续注射500μg/L甲醛标液11次)。该方法成功用于皮革制品或者皮质材料中的甲醛的测定。     

吖啶红动力学荧光法测定痕量甲醛

在H2SO4介质中，以KCIO3-吖啶红为指示反应，建立了测定甲醛的动力学荧光分析法。方法的线性范围为40～600μg／L，检出限为27μg／L。方法用于树脂整理特殊织物和动物标本室内空气中甲醛的测定，与标准方法乙酰丙酮分光光度法进行对照，所测结果经t-检验无显著性差异。     

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.     

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。