端视ICP-AES中用铟内标校正钠基体干扰的研究

端视电感耦合等离子体原子发射光谱中易电离元素引起的非光谱干扰,常使分析结果产生偏差。本文就不同浓度钠基体对分析谱线产生的干扰进行了试验和研究,并用铟作为内标元素来补偿钠基体的干扰。得出选择用几个内标元素和多条内标谱线时可以校正钠基体的干扰。     

ICP-AES法测定不锈钢中高含量镍和铬的光谱干扰和校正

使用HNO3,HF,HCl O4溶解不锈钢样品,以Ni 231.6 nm,Cr 267.7 nm作为分析谱线,以干扰系数法校正Fe对Ni和Cr的光谱干扰,建立了ICP-AES法测定不锈钢中高含量Ni和Cr的方法。通过测定不同铁基体浓度下Ni和Cr的发射强度,考察铁基体对Ni和Cr的光谱干扰。实验结果表明:铁基体对Ni和Cr均存在光谱干扰,将实验方法用于不锈钢标准样品中Ni和Cr的测定,经光谱干扰校正后,结果与参考值吻合,测定结果的绝对误差在0.35%~0.63%间,相对标准偏差(RSD,n=6)在0.68%~1.1%间。     

海底沉积物的ICP-AES分析

海底沉积物用硝酸-高氯酸-氢氟酸消解,然后用ICP-AES法同时测定常量和微量元素。研究了样品中基体元素对微量元素测定的光谱干扰,并采用干扰曲线斜率法进行干扰校正,分析批量海底沉积物样品获得满意结果。     

ICP－AES半智能直接测定稀土氧化物

本文报道了一种用ＩＣＰ－ＡＥＳ直接测定稀土氧化物的半智能方法，稀土基体对某一稀土分析谱线的光谱干扰被预先扫描并存于谱图集中。在实际测定中，相应的干扰谱图被调用，参加扣除干扰谱线影响的校正计算。结果表明该法令人满意。     

电感耦合等离子体原子发射光谱法测定铁基合金中铅量——联合应用FACT技术及标准加入法消除干扰

联合应用随同仪器提供的快速自动曲线拟合技术(FACT)校正软件和标准加入法同时消除了在电感耦合等离子体原子发射光谱法(ICP-AES)测定铁基材料中铅含量时的基体干扰和光谱干扰。试验按1常规方法,2标准加入法和3联合应用FACT校正法和标准加入法校正后,用ICP-AES分别测定混合标准溶液中的铅。选用的分析谱线为182,217,220nm。结果表明:按1测得的铅量,由于基体负干扰而偏低;按2所得结果接近已知值,这是由于仪器附带的软件有"Fitted"校正功能,当发生光谱干扰时能自动进行校正;按3所得结果准确性最好。将上述成果应用于铁钉样品分析,测得结果的准确度和精密度均较好,基体干扰和光谱干扰都得到了消除。     

ICP-AES中元素间干扰的逐步逼近校正方法

本文基于干扰系数校正法,提出一种新的校正元素间相互干扰的方法——逐步逼近校正法,以及相应的计算机软件系统。对复杂体系中元素间相互光谱干扰和元素“自身”非光谱干扰进行校正,获得了良好的结果。     

高纯氧化钬的电感耦合等离子体原子发射光谱分析及光谱干扰的校正

本文提出了以PGS-2型平面光栅摄谱仪与Plasma Therm ICP-5000D射频发生器联用,乙醇溶液预去溶进样方法,直接同时测定高纯氧化钬中5个稀土杂质元素的方法,并讨论了基体浓度对分析方法检出限的影响和光谱干扰及其校正。当样品溶液中稀土总浓度为5mg/ml时,测定下限分别为铽0.003％,镝、铒和铥0.002％,钇0.0003％。其相对标准偏差为2.8％～7.4％。     

小麦粉的ICP-AES多元素同时测定

本文报告了ICP-AES法同时测量小麦粉中Ca、Mg、Al、Fe、Cu、Zn、Mn、Ba、Y、Ni的含量。采用元素间干扰系数法校正主要基体元素对微量元素测定的光谱干扰。本法应用于湖南省粮食中重金属含量调查与评价,获得了令人满意的结果。     

ICP—AES半智能直接测定稀土氧化物

本文报道了一种用ＩＣＰ－ＡＥＳ直接测定稀土氧化物的半智能方法，稀土基体对某一稀土分析谱线的光谱干扰补预先扫描并存于谱图集中，在实际测定中，相应的干扰谱图被调用，参加扣除干扰谱线影响的校正计算。结果表明该法令人满意。     

电感耦合等离子体发射光谱法测定地质样品中钨时对锌的光谱干扰校正

采用硝酸-氢氟酸-高氯酸消解样品,电感耦合等离子体发射光谱法测定地质样品中的钨.讨论了Zn 207.908对W 207.911的光谱干扰,并应用光谱干扰系数校正法(IEC)校正干扰.结果表明:Zn对W的光谱干扰可以用IEC进行有效的消除,进行光谱校正后的结果明显优于未加校正的试验结果.     

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。