Relative precision in the determination of some structurally-similar O-pentafluorophenylsulfonylphenols by ultratrace gas chromatography.
Relative precision in the determination of some structurally-similar O-pentafluorophenylsulfonylphenols by ultratrace gas chromatography.
复制标题
超痕量气相色谱法测定一些结构相似的邻五氟苯磺酰基酚的相对精度。
DOI：
10.1016/0021-9673(85)80046-7
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发表时间：
1985
期刊：
影响因子：
--
通讯作者：
Giese,RW
中科院分区：
文献类型：
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作者：
Sentissi,A;O'Connell,K;Giese,RW
注391来自Fisher Scientific （Medford， MA， USA）。甲苯，在玻璃中蒸馏，是从伯迪克和杰克逊实验室获得的。（美国密歇根州马斯基根）。氯仿（试剂级）、环己烷（高效液相色谱级）、盐酸（试剂级）和碳酸氢钠（试剂级）购自JT Baker （Phillipsburg， NJ， USA）。硅胶60,230400目（E. Merck）购自VWR Scientific （Boston， MA， USA）。GHLF硅胶薄层色谱（TLC）荧光指示剂单片购自Analtech （Newark， DE， USA）。制备级高效液相色谱（HPLC）分离在25 cm × 10 mm ID柱上进行，柱上填充Davisil Cs（粘接并在室内填充），流动相为70%（v/v）乙腈。分析分离采用15 cm x 4.5 mm ID的Supelcosil LC-8色谱柱（Supelco, Bellefonte， PA， USA），乙腈（50-90%,v/v）梯度在水中进行。水经去离子、蒸馏、过滤（0.6~ pm聚氯乙烯膜，Millipore, Bedford， MA， USA），真空脱气；乙腈过滤（0.5 pm氟孔，Millipore），真空脱气。采用瓦里安3700型气相色谱仪，配备瓦里安1095柱上毛细管进样器和实验用350~ 1瓦里安63Ni电子捕获检测器。采用10 mx 0.25 mm ID DB5熔融硅胶毛细管柱（J&W Scientific, Ranch0 Cordova， CA， USA）。超高纯度氦气和氮气（Matheson, Gloucester， MA， USA）分别以5 ml mm1和25 ml min- 1的流速作为载体和补充气体，在室温和未校正的情况下测量。用5 ~ 1柱上注射器（Scientific Glass, Austin， TX， USA）注射甲苯中的溶质。色谱记录和峰面积集成与光谱物理SP 4270积分器。当色谱运行开始时，在180℃min- 1的设置下，将进样器温度设定为30 ~ 150℃；柱箱温度在70℃下保持1分钟，然后在50℃min- 1的设置下编程到150℃。探测器温度为340℃。
NOTES 391 chased from Fisher Scientific (Medford, MA, USA). Toluene, distilled in glass, was acquired from Burdick & Jackson Labs.(Muskegan, MI, USA). Chloroform (reagent grade), cyclohexane (HPLC grade), hydrochloric acid (reagent grade) and sodium bicarbonate (reagent grade) were purchased from JT Baker (Phillipsburg, NJ, USA). Silica gel 60, 230400 mesh (E. Merck) was obtained from VWR Scientific (Boston, MA, USA). GHLF silica gel Uniplates with fluorescence indicator for thin-layer chromatography (TLC) were purchased from Analtech (Newark, DE, USA).Preparative scale high-performance liquid chromatographic (HPLC) separations were done on a 25 cm x 10 mm ID column packed with Davisil Cs (bonded and packed in house) with a mobile phase of 70%(v/v) acetontrile in water. Analytical separations were performed on a 15 cm x 4.5 mm ID Supelcosil LC-8 column (Supelco, Bellefonte, PA, USA) with an acetonitrile (50-90%, v/v) gradient in water. The water was deionized, distilled, filtered (0.6~ pm polyvinylchloride membrane, Millipore, Bedford, MA, USA) and degassed under vacuum; the acetonitrile was filtered (0.5-pm fluoropore, Millipore) and degassed under vacuum. A Varian Model 3700 gas chromatograph, equipped with a Varian 1095 oncolumn capillary injector and an experimental, 350~ 1 Varian 63Ni electron capture detectors was employed. A 10 mx 0.25 mm ID DB5 fused-silica-capillary column (J&W Scientific, Ranch0 Cordova, CA, USA) was used. Ultra high purity helium and nitrogen (Matheson, Gloucester, MA, USA) were used as carrier and makeup gases at flow-rates of 5 ml mm1 and 25 ml min-l, respectively, measured at room temperature and uncorrected. Injections of the solutes in toluene were made with a 5-~ 1 on-column syringe (Scientific Glass, Austin, TX, USA). Chromatograms were recorded and peak areas integrated with a Spectra-Physics SP 4270 integrator. When the chromatographic run was initiated, the injector temperature was programmed from 30 to 150 C at a setting of 180 C min-l; the column oven temperature was held at 70 C for 1 min and then programmed to 150 C at a setting of 50 C min-l. The detector temperature was 340 C.