哌仑西平的单扫描示波极谱法测定

本报道一种测定哌仑西平的单扫描示波极谱法，在０．１ｍｏｌ／ＬＮＨ４Ｃｌ－ＮＨ３．Ｈ２Ｏ（ｐＨ８．０±０．１）缓冲液中，哌仑西平有一极谱还原波，其峰电位为－１．５１Ｖ（ｖｓ．ＳＣＥ），其一阶导数峰高与哌仑西闰浓度在６．６×１０＾－７－４．６×１０＾－６ｍｏｌ／Ｌ（ｒ＝０．９９８１）和６．６×１０＾－６－１．６×１０＾－５ｍｏｌ／Ｌ（ｒ＝０．９９９１）范围内有线性关系，检测限为３．４×１０－７ｍｏｌ     

钼（Ⅵ）—向红菲罗啉络合物的吸附伏安行为

在ＰＨ＝４．０的０．３ｍｏｌ／Ｌ的ＨＡｃ－ＮａＡｃ介质中，钼（Ⅵ）－向红菲罗啉体系在悬汞电极上，于－０．５８Ｖ电位处得到钼（Ⅵ）－向红菲罗啉络合物的吸附还原波，其１．５次微分伏安图的峰峰值ｅｐｐ与Ｍｏ（Ⅵ）在３．０×１０＾－１０－－１．２×１０＾－７ｍｏｌ／Ｌ浓度范围内呈良好的线性关系；检测限可达８×１０＾－１１ｍｏｌ／ＬＭｏ（Ⅵ）。方法用于豆类样品微量钼的测定，结果较邹。     

锑—铜—茜素络合剂体系极谱行为的研究

在１．０ｍｏｌ／Ｌ甲酸－甲酸钠－０．０３ｍｏｌ／Ｌ邻苯二甲酸氢钾混合底液（ｐＨ３．５）中，锑－茜素络合剂（ＡＬＣ）络合物在单扫示波极谱上于一０．５３Ｖ（ｖｓ．ＳＣＥ）产生一极谱波，加入１．６×１０＾－３ｍｏｌ／ＬＣｕ（Ⅱ）后，灵敏度有较大提高，峰电流与锑浓度在２．０×１０＾－８～３．０×１０＾－６ｍｏｌ／Ｌ范围内呈线性关系，检测限达１．０×１０＾－８ｍｏｌ／Ｌ，研究了电极反应机理，方法应用于铜合金     

用亚硝基R盐螯合树脂分离富集催化极谱法测定矿石中的铱

本文研究了利用亚硝基Ｒ盐螯合形成的树脂，分离富集试液中痕量贵金属元素铱的实验条件。并利用ＪＰ－１型示波极谱仪，在１．５０ｍｏｌ／Ｌ盐酸＋５．０×１０＾－５ｍｏｌ／Ｌ硫脲＋０．２ｍｏｌ／Ｌ盐酸＋５．０×１０＾－５ｍｏｌ／Ｌ硫脲＋０．２ｍｏｌ／Ｌ碘化钾＋碲（ρ（Ｂ）＝０．４ｍｇ／Ｌ）的混合底液中，对铱进行极谱催化波测定。在示波极谱仪上峰电位约－０．５５Ｖ（银汞齐为参比电极），可测定试液中５．０×１．０     

大量锆存在下铪镧钼杂多酸—耐尔蓝体系测定给

本文研究了耐尔蓝（ＮＢ）－给镧钼杂多酸（ＨｆＬａＭｏ－聚乙烯醇（ＰＶＡ）体系测定铪的超高灵敏光度法。在ＰＶＡ存在下，铪，镧和钼酸铵形成杂多酸，继而与耐尔蓝形成离子缔合物。其适宜条件为〔ＨＣｌｏ４〕＝１．２ｍｏｌ／Ｌ，〔Ｌａ×３＋〕＝２．９×１０＾－７ｍｏｌ／Ｌ，〔ＭｏＯ４×２－〕＝１．１×１０＾－３ｍｏｌ／Ｌ，〔ＮＢ〕＝２．７×１０＾－６ｍｏｌ／Ｌ，ＰＶＡ０．０８％。离子缔合物的最大吸收波长在５９     

单扫描示波极谱法测定甘草酸

本文报道测定甘草酸的单扫描法波极谱方法，在０．１ｍｏｌ／ＬＮａＡｃ－ＨＡｃ（ｐＨ４．１±０．１）缓冲液中，甘草酸还原波峰电位为－１．３８Ｖ（ｖｓ．ＳＣＥ），峰高与其浓度在２．０×１０＾－６～１．０ ×１０＾－４ｍｏｌ／Ｌ范围内有线性关系，检测限为１．２×１０＾－６ｍｏｌ／Ｌ。甘氨酸，半胱氨酸等不干扰测定。应用本方法测定强力宁注射液中甘草酸含量，结果令人满意。本文还讨论了电极过程机理。     

头孢哌酮钠的伏发行为及其应用研究

头孢哌酮钠在０．０５ｍｏｌ／Ｌ Ｈ２ＳＯ４溶液中,形成一良好的示波极谱导数峰。峰电位为－０．８２Ｖ（ｖｓ．ＳＣＥ）。峰电流与头孢哌酮钠的浓度在１．０×１０＾－７－２．０×１０＾６ｍｏｌ／Ｌ范围内成线性关系。检出限为５．０×１０＾－８ｍｏｌ／Ｌ。回收率在９４．０％－１０２．０％之间。并用于尿样的测定,得到满意的结果。     

铜—腺嘌呤络合物吸附波的研究

了在０．０８ｍｏｌ／ＬＮａＡｃ～０．０２ｍｏｌ／ＬＨＡｃ缓冲溶液铜与腺嘌呤（Ａｄｅ）络合物的极谱行为，结果表明，扫描电压为－０．２Ｖ～－０．７Ｖ时铜－腺嘌呤络合物在单扫示波极谱上有一络合物吸附波，其一阶导数峰电位主－０．４Ｖ（ｖｓ．ＳＣＥ），腺嘌呤浓度在１．０×１０＾－６～１．０×１０＾－５ｍｏｌ／Ｌ范围内与一阶导数波高呈良好的线性关系，检出限为１．０×１０＾－７ｍｏｌ／Ｌ，实验证明，该峰具有吸附     

硅钼杂多阴离子薄膜修饰电极线性扫描伏安法测定黑液中要溶性硅

本报导了以玻碳电极为基体的１∶１２硅钼杂多阴离子薄膜化学修，铈电极的制备及其电化学特性。并应用于导数伏安法测定。在４．０×１０＾－３ｍｏｌ／Ｌ９ＮＨ４）６Ｍｏ７Ｏ２４－６６．８×１０＾－２ｍｏｌ／ＬＮａ３Ｃｉｔ－０．４８ｍｏｌ／Ｌ ＮＨＯ３体系中，硅浓度在８．３×１０＾－７～１．７×１０＾－３ｍｏｌ／Ｌ。对可溶性硅（以ＳｉＯ２计）为２４５．０５ｍｇ／Ｌ的黑液，稀释１０倍后，取２．００ｍＬ平行测定     

丁基罗丹明B—钼酸盐光度法连续测定铈和钪

在聚乙烯醇（ＰＶＡ）存在下，丁基罗丹明Ｂ（ＢＲＢ）分别与铈钼、钪钼杂多酸络阴离子形成离子缔合物，其最大吸收均位于５７０ｎｍ，表面摩尔吸光度分别为εＣｅ＝３．９６×１０＾６Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，εＳｃ＝４．７１×１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，服从比耳定律范围分别为０－２４μｇ／Ｌ Ｃｅ和０－６０μｇ／ＬＳｃ，测定极限为Ｃｅ１．０μｇ／Ｌ（ｎ＝１２）和Ｓｃ１．９μｇ／Ｌ（ｎ＝１０），对     

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。     

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.     

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.     

Acid hydrolysis of carboxymethylcellulose of low degree of substitution

Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position.     

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.     

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。     

Estimation of Kinetic Parameters of Thermal Oxidation of Ilmenite

The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of hematite Fe₂O₃. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the best fitting experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.     

Mechanism of action of base-catalyzed oxygenation of phenol derivatives

Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6.     

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^-。