胺菊酯·高效氯氰菊酯气雾剂的气相色谱分析

介绍了 0 .2 8 %胺菊酯·高效氯氰菊酯气雾剂的气相色谱分析方法。选用 5 %SE - 30 ChromsorbWAW -DMCS(15 0～ 180um)色谱柱 ,以邻苯二甲酸二正辛酯为内标物进行定量分析测定 ,该方法简单、快速、准确、适用。结果表明胺菊酯和高效氯氰菊酯的标准偏差分别为 0 .2 4 %和 0 .11% ;变异系数分别为 0 .94 %和 1.74 % ;平均回收率分别为 99.6 4 %和 99.95 % ;线性回归系数分别为 0 .9999和 0 .9998。     

Kinetics of microwave‐assisted polymerization of ϵ‐caprolactone

The kinetics of polymerization of ?‐caprolactone (CL) in bulk was studied by irradiating with microwave of 350 W and frequency of 2.45 GHz with different cycle‐heating periods (30–50 s). The molecular weight distributions were determined as a function of reaction time by gel permeation chromatography. Because the temperature of the system continuously varied with reaction time, a model based on continuous distribution kinetics with time/temperature‐dependent rate coefficients was proposed. To quantify the effect of microwave on polymerization, experiments were conducted under thermal heating. The polymerization was also investigated with thermal and microwave heating in the presence of zinc catalyst. The activation energies determined from temperature‐dependent rate coefficients for pure thermal heating, thermally aided catalytic polymerization, and microwave‐aided catalytic polymerization were 24.3, 13.4, and 5.7 kcal/mol, respectively. This indicates that microwaves increase the polymerization rate by lowering the activation energy. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 91: 1450–1456, 2004     

纤维素衍生化手性固定相的制备和对噻吗洛尔拆分

用超声方法合成了三(3,5-二硝基苯甲酰基)纤维素(CTNB)、三(4-溴苯甲酰基)纤维素(CTBB)、三(苯甲酰基)纤维素(CTB)、三(4-甲基苯甲酰基)纤维素(CTMB)、三(4-硝基苯甲酰基)纤维素(CTPB).将此类衍生化纤维素作为薄层色谱的手性固定相,结合展开剂的优化,对噻吗洛尔对映体进行拆分研究,并对衍生化取代基对拆分效果的影响以及对映体在手性固定相上的拆分机理进行了详细的探讨.     

离子色谱法测定配煤、焦炭和焦油中的氯含量

研究了用带电导检测器的离子色谱对配煤、焦炭和焦油中的Cl- 进行测定的方法。在YSA型8126A-4# 阴离子分离柱上用3.5mmol/LNa2CO3、5.3mmol/LNaHCO3做淋洗液对Cl-进行测定,方法简便快速。Cl-的检出限为2×10-6。该法也适用于F-、NO2-、NO3-、SO42-等的测定。     

Identification of some volatile compounds in the odor of fecal pellets of the rabbit,Oryctolagus cuniculus

A study has been made of the volatile constituents in the vapors collected from fecal pellets of wild rabbits,Oryctolagus cuniculus. Measurements of changes in the heart rates of adult male rabbits exposed to the effluent of a gas chromatographic capillary column were used to indicate the presence of compounds which may be of behavioral significance. Combined with the use of high-resolution columns in gas chromatography and gas chromatography-mass spectrometry, this approach has implicated several classes of compounds, including volatile fatty acids and phenols, which in certain absolute or relative concentrations may be involved in the formation of signals of territorial importance.     

丙二醇单甲醚丙酸酯合成体系的气相色谱分析

自行研制了氰乙基(25%,质量分数)甲基硅橡胶(XE-60)石英毛细管色谱柱。建立了对含游离酸的丙二醇单甲醚丙酸酯的色谱分析方法。该法具有分离效果好,分析速度快的优点。     

8─羟基喹啉─5─磺酸柱前衍生反相HPLC分离测定痕量Al（Ⅲ）、Co（Ⅲ）、Fe（Ⅲ）和Pd（Ⅱ）

本文采用８－羟基喹啉－５－磺酸（ＨＱＳ）为柱前衍生试剂，用含有１０ｍｍｏｌ·Ｌ－１的四丁基溴化铵（ＴＢＡ＋Ｂｒ－）、７．５×１０－５ｍｏｌ·Ｌ－１的ＥＤＴＡ和２０ｍｍｏｌ·Ｌ－１的ｐＨ５．６乙酸－乙酸钠缓冲溶液的甲醇－水（４５：５５，Ｖ／Ｖ）溶液为流动相，以Ｃ１８硅烷化载体为固定相，１６ｍｉｎ内分离测定了Ｃｏ（Ⅲ）、Ｆｅ（Ⅲ）、Ａｌ（Ⅲ）和Ｐｄ（Ⅱ）的ＨＱＳ的配合物、信噪比为３时，检出限分别为：Ｃｏ（Ⅲ）０．９ｐｐｂ、Ｆｅ（Ⅲ）１．５ｐｐｂ和Ｐｄ（Ⅱ）５．４ｐｐｂ，方法灵敏度高，干扰少，用于测定试剂级盐酸，硝酸和中国红茶样品中的这些离子，结果良好。     

15%田草灵高效液相色谱分析

采用Ｎｏｖａ－Ｐａｋ Ｃ１８不锈钢色谱柱进行反相液相色谱分析，以甲醇：水＝６５：３５（Ｖ／Ｖ）为注动相，以邻苯二甲醇二乙酯为内标物，用内标法测定田草灵除草剂中苄嘧黄隆和异丙甲草胺的含量，结果表明，各有效成分与内标物色谱峰分离完全，杂质无干扰，测定结果，苄嘧黄隆和异丙甲草胺的变异系数分别为０．７４％和１．０７％，回收率分别为９９．４％￣１００．８％和９９．１％￣１０１．３％。     

气相色谱法测定1,1-二氯-1-氟乙烷

研究了HCFC - 14 1b的气相色谱分析 ,色谱柱为HP - 1柱 ,氢火焰检测 ,相对误差在 5 %以内 ,该定量分析快速、简便、准确     

毛细管气相色谱法分析双丙酮丙烯酰胺的含量

用毛细管气相色谱，FID检测器，内标法定量，分离测定了双丙酮丙烯酰胺及其主要杂质丙烯酰胺的含量，其相对标准偏差分别为0．19和0．014；变异系数分别为0．19％和4．71％。