X射线荧光光谱法测定金红石中主次组分

采用Li2B4O7和LiBO2的混合熔剂(67∶33)熔融制样,波长色散X射线荧光光谱法测定金红石中TiO2,TFe,P,SiO2,Al2O3,MnO,CaO,Cr2O3,MgO,ZrO2,HfO2等组分。实验中样品和熔剂的质量比为1∶14,以溴化锂(LiBr)作脱模剂,采用高频熔炉在1 150℃熔融90s进行制样,所得熔片均匀、强度高、成型良好。方法用于金红石实际样品的测定,结果同参考值或化学分析方法的结果相吻合,相对标准偏差(RSD,n=10)P为3.8%、Al2O3为2.8%,其它均小于2%,能够满足实际测定工作的需要。     

X-射线荧光光谱法分析硅质耐火材料的主次成分

采用硅石标准样品作为校准样品,建立了熔融制样X-射线荧光光谱法测定硅质耐火材料中SiO2、Al2O3、CaO、MgO、P2O5、Fe2O3、TiO2、K2O、Na2O的方法.采用熔融法为样品片和校准片的制备方法,选择四硼酸锂-偏硼酸锂(质量比为67∶33)为助熔剂,1.00mL LiBr溶液为脱模剂,熔融温度1100℃...     

X射线荧光光谱法分析镁砂中的主次成分

采用镁砂标准样品作为校准样品,建立了熔融制样X射线荧光光谱法测定镁砂中MgO,Al2O3,SiO2,CaO,P2O5,Fe2O3的方法。采用熔融法为样品片和校准片的制备方法,选择四硼酸锂-偏硼酸锂(67+33)为助熔剂,1.00mL LiBr溶液为脱模剂,熔融温度为1 100℃,熔融时间20min。对镁砂样品测定的相对标准偏差(RSD)小于3%,对不同镁砂标准样品进行测定,方法的测定结果与认证值相吻合。     

X射线荧光光谱法分析镁砂的主次成分

采用镁砂标准样品作为校准样品,建立了熔融制样X射线荧光光谱法测定镁砂中MgO,Al2O3,SiO2,CaO,P2O5,Fe2O3的方法。采用熔融法为样品片和校准片的制备方法,选择四硼酸锂-偏硼酸锂（67＋33）为助熔剂,1.00mL LiBr溶液为脱模剂,熔融温度为1 100℃,熔融时间20min。对镁砂样品测定的相对标准偏差（RSD）小于3%,对不同镁砂标准样品进行测定,方法的测定结果与认证值相吻合。     

X射线荧光光谱法测定钠冰晶石的主要化学成分

选用国家标准样品和高纯物质配制实验用标准样品,采用混合熔剂(67%Li2B4O7+33%LiBO2)熔融制样,使用X射线荧光光谱法测定钠冰晶石中SiO2、Fe2O3、MgO、CaO、K2O、TiO2、P2O5、Na、F、Al各组分的含量,实验结果表明,各组分的相对标准偏差(RSD)在0.57%~6.5%,与第三方实验室对比测定结果表明,方法可以满足工厂检测要求。     

熔融制样X射线荧光光谱法测定水泥及水泥熟料中成分

采用波长色散X射线荧光光谱仪测定水泥和水泥熟料中的Na2O、MgO、A12O3、SiO2、P2Os、SO3、K2O、CaO、TiO2、MnO、Fe2O3等成分。采用熔融玻璃片方法制样,采用Li2B4O7为熔剂,较混合熔剂的制样效果好;硫在1050℃熔融制样过程中的挥发较慢,对测定结果无明显影响。方法测定准确度、精密度较好,所得结果与湿法化学分析结果相符。     

X射线荧光光谱法测定硅石中主次量元素组分

以Li_2B_4O_7、LiBO_2和LiF(质量比为45∶10∶5)为混合熔剂,NH_4NO_3为氧化剂,LiBr为脱模剂,熔融制作样片,采用硅质砂岩、石英岩标准样品和配制标准样品作为校准样品,建立了熔融制样-X射线荧光光谱法(XRF)测定硅石中主次量成分(SiO_2、Al_2O_3、TFe_2O_3、MgO、CaO、K_2O、MnO、TiO_2、P_2O_5)的快速分析方法。对样品制备以及分析测试过程中的条件进行了优化,在最优条件下,对标准样品(GBW03112、GBW07835)进行重复测定,相对标准偏差RSD2%。同时对3个混合配制的硅石标准样品进行分析,结果与参考值无显著性差异。     

熔融制样-波长色散X射线荧光光谱法测定铁矿石中12种主次成分

采用熔融制样法对铁矿石进行熔融制样;以三氧化二钴(Co2O3)作为铁的内标,并对熔剂、氧化剂、脱模剂、熔融温度和熔融比例进行了讨论。采用理论α系数法、经验系数法校正基体效应和各元素的谱线重叠干扰。建立了波长色散X射线荧光光谱(WDXRF)测定铁矿石中12种组分的分析方法。本法测定铁矿标准物质(GBW07822-GBW07830)各组分的相对标准偏差(RSD)在0.41%~4.2%之间,测定值与标准值相符,且与电感耦合等离子发射光谱的对比测定结果一致。利用本法对实际铁矿样品的全铁含量进行测定,结果与化学分析法的测定结果基本一致。     

熔融制样-X射线荧光光谱法测定土壤矿质全量元素

针对压片制样-X射线荧光光谱法测定土壤矿质全量元素存在的问题,建立了熔融制样-X射线荧光光谱法(XRF)测定土壤矿质全量元素Si、Mg、Fe、Al、Ca、K、Na、P、Mn、Ti含量的方法。为了防止在熔片过程中出现大量气泡,实验称取土壤样品,选择Li2B4O7-LiBO2-H3BO3(m:m:m =45:10:5)混合熔剂,稀释比为10:1,5滴400 g/L LiBr溶液做脱模剂,升温到1050 ℃熔融9 min,助熔剂中H3BO3促使土壤中CaCO3、MgCO3快速反应,迅速释放出CO2,制备出流动性好、无气泡的玻璃样品。选择土壤成分分析标准物质、岩石成分分析标准物质、水系沉积物成分分析标准物质等进行互配,采用基本参数法校正基体效应后,建立校准曲线。方法的检出限为6.71～257 μg/g,测定结果相对标准偏差(RSD,n=11)0.12%～0.51%。采用实验方法对土壤国家有证标准物质GBW07466、GBW07544、GBW07555进行分析,测定结果与认定值相符。     

预氧化熔融制样-X射线荧光光谱法测定硼铁合金中硼、硅、铝和磷

硼铁合金样品经过预氧化熔融,制得样品的玻璃熔片,采用X射线荧光光谱法测定玻璃熔片中硼、硅、铝和磷等4种元素的含量。优化的试验条件如下:(1)熔剂为焦硫酸钾;(2)熔剂与样品的稀释比为40∶1;(3)氧化剂为碳酸锂和硝酸钠;(4)玻璃熔片的熔融时间为20min。4种元素的质量分数在一定范围内与其对应的荧光强度呈线性关系,测定下限为0.006 8%～0.017 9%。对硼铁标准样品平行测定10次,测定值的相对标准偏差为0.22%～3.9%。方法应用于硼铁合金样品的分析,测定结果与湿法分析的结果相符。     

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。