韭菜花挥发性成分的气相色谱-质谱分析

1　实验部分1.1　仪器　　ＨＰ5890气相色谱 ＨＰ5970Ｂ质量检测器;ＳＥ 54弹性石英毛细管柱(30ｍ×0 25ｍｍｉ.ｄ.,0 25μｍ);蒸馏 萃取器(海门玻璃仪器厂产品[1])。1.2　气相色谱 质谱(ＧＣ ＭＳ)条件　　柱温:初始40℃,保持2ｍｉｎ,以4℃/ｍｉｎ升至160℃,以8℃/ｍｉｎ升至250℃,保持31 25ｍｉｎ;进样口温度250℃;转移线温度280℃;载气高纯氦气;柱压45ｋＰａ;ＥＩ源,全扫描方式,扫描范围30～500ｕ,电子倍增器电压1800Ｖ。1.3　样品来源　　由市场购买两种不同花期的韭菜花,一种为全部开花期的韭菜花(样品Ａ),另一种为部分已结种子的韭菜…     

猪油挥发油成分的气相色谱/质谱法分析

1　引　　言油脂是人类的主要食品之一 ,其主要成分是脂肪酸甘油三酯 ,它参与人体正常生理代谢。油脂香气成分是其微量成分 ,含量一般在油脂总量的 1%以下 ,却构成其各自特征香气。奶油、玉米油、牛油等均有较详细的报道。本文以ＧＣ ＭＳ分析猪油香气成分 ,70种成分被确定。2　实验部分2 .1　主要仪器　ＨＰ5 973气质联用仪 (ＧＣ ＭＳ) ,ＨＰＩＮＮＯＷＡＸ 30ｍ× 0 .2 5ｍｍ× 0 .2 5 μｍ毛细管柱 ,ＮＩＳＴ98谱库。2 .2　ＧＣ ＭＳ条件　进样口温度 2 5 0℃ ,检测器温度 2 80℃ ,柱温 6 0℃ (2ｍｉｎ) 2℃ ｍｉｎ12 0℃ (1ｍｉｎ) 10…     

气相色谱/质谱法分析研究蜂胶中化学成分

1　引　　言用ＧＣ/ＭＳ分析方法分离鉴定蜂胶中的化学成分。试样经提取、酯化、浓缩后 ,采用ＨＰ 5( 30ｍ× 0 .2 5ｍｍ× 0 2 5ｍｍ)弹性石英毛细管柱进行测定。分离鉴定了黄酮类、脂肪酸、芳香酸、醇类等 77个化合物。用峰面积归一法通过Ｇ1 70 1ＢＡ化学工作站数据处理系统得出各化学成分在蜂胶中的百分含量为 97 1 2 %。2　实验部分2 1　仪器与试剂　ＨＰ6890 / 5973ＧＣ/ＭＣ联用仪 (美国惠普公司 ) ,三球ＫＤ旋转蒸发浓缩仪 (上海玻璃仪器公司 ) ,色谱柱为ＨＰ 5( 30ｍ× 0 .2 5ｍｍ×0 .2 5μｍ)弹性石英毛细管柱 (美国惠普公司 )…     

高效毛细管电泳检测克莱保健烟贴中的尼古丁

1　引　　言尼古丁是一种生物碱。尼古丁的检测方法有薄层色谱法、容量法、电导滴定法等。本文研究了用毛细管电泳技术分离测定克莱保健烟贴中的尼古丁 ,获得了比较满意的结果。2　实验部分2 1　仪器与试剂　 12 2 9型高效毛细管电泳仪 (北京新技术应用研究所 ) ,固定波长紫外检测器 ,ＡＣＳ2 0 0 0高压电源 ,ＡＣＳ2 0 0 0色谱工作站 (中国科学院研究生院应用化学研究所 ) ,石英毛细管 5 0 μｍ(ｉｄ)× 6 0ｃｍ ,有效长度约 4 4 5ｃｍ(河北永年光导纤维厂 ) ,ｐＨ ＨＪ90Ｂ型酸度计 (上海雷磁仪器厂 )。尼古丁 (ｎｉｃｏｔｉｎｅ)标样 (…     

GDX短柱快速GC分析空气中苯、甲苯和二甲苯

空气中苯、甲苯和二甲苯 (简称三苯 )测定 ,通常采用的气 液色谱及长柱[1～ 3 ] ,保留时间长。本法采用ＧＤＸ10 2担体和 0 .4 5ｍ短柱 ,只需 1ｍｉｎ即可完全分离 ,且具有简便快速 ,线性良好的特点。测定苯、甲苯和二甲苯的精密度分别为 1.84 % ,1.78%和 0 .6 3% ,检出限分别为 0 .8,1.0和 1.8ｍｇ·ｍ-3 。1　试验部分1.1　仪器与试剂ＳＰ2 30 5Ｅ气相色谱仪 ,ＦＩＤ检测器 ,附六通阀及1ｍｌ定量管 (北京分析仪器厂 )。三苯标准液 :苯、甲苯、二甲苯以 1.0 + 1.5 + 3 0混合。1.2　色谱条件色谱柱 :用 0 .4 5ｍ× 3.5ｍｍ玻璃管加工成Ｕ…     

5-Br-PADAP光度法测定锰矿中微量钴

5 Ｂｒ ＰＡＤＡＰ作为显色剂 ,已被广泛用于测定许多金属元素。本文将其用于锰矿中微量钴的测定 ,获得满意结果。1　试验方法取 0～ 10 μｇ钴标准于 5 0ｍｌ容量瓶 ,加入0 0 5ｍｏｌ·Ｌ-1氨三乙酸 5ｍｌ,10 0ｇ·Ｌ-1ＮＨ4 Ｆ溶液 2ｍｌ,以水稀至约 30ｍｌ ,加入 7.5× 10 -4 ｍｏｌ·Ｌ-15 Ｂｒ ＰＡＤＡＰ溶液 4ｍｌ ,摇匀 ,放置 2 0ｍｉｎ ,在摇动下加入硫酸 (1+2 ) 10ｍｌ,以水稀释至刻度 ,用 2ｃｍ比收稿日期 :2 0 0 1 0 4 2 9色皿 ,5 80ｎｍ波长处 ,在 72 1Ａ分光光度计上测其吸光度。2　样品分析称取样品 0 .2 0 0 0ｇ于 2 0 0…     

气相色谱法同柱测定莠去津·二甲戊灵复配制剂

1　引　　言莠去津 (化学名 :2 氯 4 乙氨基 6 异丙氨基 1 ,3 ,5 三嗪 )·二甲戊灵〔化学名 :Ｎ (乙基丙基 ) 3 ,4 二甲基 2 ,6 二硝基苯胺〕复合除草剂为新型的芽前除草剂 ,防除谱广 ,对旱地常见的禾本科杂草及阔叶杂草的防除效果较好 ,对作物安全。本文提出该复配制剂的检测方法 ,对保证产品的有效成分含量、稳定产品质量有着积极的作用。2　实验部分2 1　仪器、试剂与分析条件　ＳＰ 680 0Ａ气相色谱仪 (鲁南分析仪器厂 ) ;ＨＰ 3 3 94色谱数据处理机。色谱柱为 5 %ＯＶ 1 0 1涂布于 1 5 0～ 1 80 μｍｃｈｒｏｍｏｓｏｒｂＡＷＤＭ…     

气相色谱法测定污水中对硫磷的农残量

1　引言对硫磷 ,是一种具有触杀和胃毒作用的硫代磷酸酯类有机磷杀虫剂。对棉花、蔬菜、水稻等的害虫 ,有很好的防治效果 ,但有机磷农药对人畜的毒性较大 ,所以必然会造成对生态环境的污染。关于有机磷农药的检测 ,虽有报道 ,但很少 ,特别是水样中微量对硫磷的测定 ,目前未见报道 ,本文用 30 0～ 40 0 μｍ的活性炭作吸附剂 ,富集污水中的对硫磷 ,收到满意的效果。2　实验部分2 1　仪器和试剂ＳＰ—50 2气相色谱仪 ,火焰光度检测器 ,ＣＤＭＣ— 2Ａ色谱处理仪 ,玻璃层析柱 ( 7.0× 1 .4ｃｍｉ.ｄ)玻璃柱。Ｂ70— 30型真空抽气泵。对硫磷 :…     

凝胶渗透色谱法测定木素磺酸盐相对分子质量分布

1　引　　言用凝胶渗透色谱 (ＧＰＣ)测定木素磺酸盐相对分子质量和相对分子质量分布 ,国外早在 6 0年代起就有文献报道 ,但国内在这方面文献报道较少。本文使用示差折光和紫外检测器 ,分别获得木素磺酸钠和木素磺酸钙的色谱图 ,用激光光散射检测器和标定线两种方法计算样品的平均相对分子质量及相对分子质量分布 ,并探讨了影响结果的因素。2　实验部分2 .1　仪器与试剂　Ｓｐｅｃｔｒａ公司凝胶渗透色谱仪 ,配Ｐ10 0泵 ,ＴＳＫ ＧＥＬ柱 ,接ＤａｗｎＷｙａｔｔ公司ＤＳＰ多角度激光检测器(ＭＡＬＬＳ)和ＲＩ 15 0检测器 ;Ｗａｔｅｒｓ公司…     

新试剂1-(2,6-二溴-4-硝基苯)-3-(4-硝基苯)-三氮烯与汞的显色反应及应用

三氮烯试剂与第ＩＢ、ＩＩＢ族金属元素有高灵敏的显色反应 1 [1] ,可用来测定样品中微量的Ｃｄ2 + 、Ｈｇ2 + 、Ｚｎ2 + 、Ｎｉ2 + 。随着表面活性剂引入该显色体系 ,使该试剂与金属离子显色反应的灵敏度有了很大的提高。目前报道的三氮烯显色剂与Ｈｇ2 + 显色反应的灵敏度一般在ε =1 .0× 1 0 5Ｌ·ｍｏｌ-1·ｃｍ-1左右 ,但也有部分试剂的灵敏度较高 ,如ＯＣ Ｃａｄｉｏｎ[2 ] 的ε =1 .77× 1 0 5Ｌ·ｍｏｌ-1·ｃｍ-1,ＤＮＡＡＢ[3 ] ε=1 .74× 1 0 5Ｌ·ｍｏｌ-1·ｃｍ-1,ＭＤＡＡ[4]的ε=1 .8× 1 0 5Ｌ·ｍｏｌ-1·ｃｍ-1,ＡＰＤ…     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

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.     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

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.

     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

Calculation of enthalpies of hydrogenation of hydrocarbons

Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.     

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。