自动电位滴定法测定铬铁中铬含量的不确定度评定

建立了自动电位滴定法测定铬铁中铬含量的数学模型,对数学模型中各个参数进行不确定度来源分析,分别对A类不确定度及B类不确定度进行评定,对各不确定度分量进行合成,得到铬质量分数的不确定度。当铬铁中铬含量为68.31%时,扩展不确定度为0.52%(k=2)。结果表明玻璃器具的精度、自动电位滴定仪自带体积管的误差、自动电位滴定仪终点识别的误差是测量不确定度的主要来源。     

石墨炉原子吸收法测定酱卤肉中铬的不确定度评定

对石墨炉原子吸收光谱法测定酱卤肉中铬的不确定度进行评定。参照GB 5009.123–2014,采用微波消解–石墨炉原子吸收法测定酱卤肉制品中铬含量,分析不确定度来源,包括测量重复性、标准工作溶液浓度、定容体积、称样质量、样品处理等,对各类不确定度分量进行评定,最终合成得到标准不确定度和扩展不确定度。当酱卤肉制品中铬含量为0.23 mg/kg时,测定结果在95%置信水平时的扩展不确定度为0.017 mg/kg(k=2)。石墨炉原子吸收光谱法测定酱卤肉中铬的不确定度主要来源于测量重复性、铬标准溶液浓度和样品消解处理过程。评定结果可为提高原子吸收法测定肉制品中铬含量的准确性提供参考。     

火焰原子吸收光谱法测定空气中铬含量的不确定度评定

用火焰原子吸收光谱法测定空气中铬含量,评定了测定过程的不确定度,把不确定度分解为标准溶液及配制引入的不确定度、标准曲线拟合引入的不确定度和样品重复测定引入的不确定度等七个因素,系统分析并计算各不确定度分量和扩展不确定度.结果表明,其中采集样品引入的不确定度是主要影响因素,空气中铬含量为3.88 μg/m3时,扩展不确定度为0.12 μg/m3.     

钢铁及其合金中铬含量测定结果的不确定度评定

对用GB／T223、11—1991《过硫酸铵氧化容量法测定铬量》的方法测定钢铁及合金中铬含量测量结果的不确定度进行了评定。对样品测量过程中的不确定度分量进行了分析和量化,求得铬含量测定结果的标准不确定度和扩展不确定度分别为0．06％和0．12％。     

火焰光度法测定烤烟烟叶中钾的不确定度评定

根据JJF 1059.1–2012 《测量不确定度评定与表示》建立了数学模型,对火焰光度法测定烤烟上、中、下部烟叶中钾含量的标准不确定度分量进行评定和合成。不确定度主要来源于标准曲线拟合、标准溶液配制、加标回收率和测定重复性。当烤烟上部烟叶钾含量为1.817 1%时,其扩展不确定度为0.068 3% (k=2);当中部烟叶钾含量为2.154 8%时,其扩展不确定度为0.073 3%(k=2);当下部烟叶钾含量为2.420 7%时,其扩展不确定度为0.071 2%(k=2)。该方法确定了影响火焰光度法测定烤烟烟叶中钾的关键因素,提高了检测准确性和可靠性。     

铬铁矿中三氧化二铬测定结果不确定度的评定

讨论了影响铬铁矿中三氧化二铬测定结果不确定度的各种因素,并评定了地质样品中三氧化二铬测定结果的不确定度.结果表明,采用硫酸亚铁铵溶液滴定方法,当样品三氧化二铬的含量为43.78％时,其扩展不确定度U=0.32％.     

气相色谱法测定中、长链脂肪乳注射液中大豆油和中链甘油三酸酯含量的不确定度评定

建立气相色谱法测定中、长链脂肪乳注射液中大豆油和中链甘油三酸酯含量的不确定度评定方法。建立数学模型，分析气相色谱法测定中、长链脂肪乳注射液中大豆油和中链甘油三酸酯含量的不确定度来源及影响因素，对各不确定度分量进行评价，计算合成标准不确定度及扩展不确定度。当大豆油质量分数为9.63%时，其扩展不确定度为0.10%(k=2)。当中链甘油三酸酯质量分数为10.00%时，其扩展不确定度为0.11%(k=2)。气相色谱法测定中、长链脂肪乳注射液中大豆油和中链甘油三酸酯含量的不确定度主要来源于对照品和样品溶液制备过程。该不确定度评定为实验过程的控制和测定结果的评估提供了参考，有利于保证该类药品的质量控制水平和检验结果的准确性。     

分子吸收分光光度法测定辉钼矿中钼的不确定度评定

对分子吸收分光光度法测定辉钼矿中钼元素的不确定度进行了评定,分析了不确定度的来源,包括工作曲线拟合、标准溶液配制、样品重复测定、分析仪器、样品称量、样品溶液定容等引入的不确定度。计算了钼含量测定结果的合成标准不确定度和扩展不确定度。当辉钼矿中钼含量为0.108 1%时,扩展不确定度为0.002 1%(k=2)。     

火焰原子吸收分光光度法测定土壤样品中铜、锌、铅、镍、铬的不确定度评定

评定火焰原子吸收分光光度法测定土壤样品中的铜、锌、铅、镍、铬结果的不确定度。从样品称量、定容、标准物质、标准曲线拟合、测量重复性等方面分析和计算不确定度分量，对不确定度分量进行合成和扩展，最终给出不确定度评定报告。土壤样品中铜、锌、铅、镍、铬的测定结果分别表示为（31.6±1.2）、（86.5±2.4）、（25.8±1.8）、（37.7±1.3）、（75.2±2.3）mg/kg,k=2。结果显示：土壤中各元素含量的不确定度主要来源于标准溶液配制过程和标准曲线拟合过程。     

电感耦合等离子体原子发射光谱法测定塑胶中镉、铅、汞、铬含量的不确定度

对电感耦合等离子体发射光谱法测定塑胶中镉、铅、汞、铬含量的不确定度进行了评定.分析了测定过程中不确定度的主要来源,对各不确定度分量进行了量化.镉、铅、汞、铬的合成标准不确定度分别为0.146、2.27、1.71、1.06 mg/kg.     

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.     

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.     

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。     

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.     

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.