一种直热式快速气相色谱快速升温装置的设计

用大电流脉冲直接加热不锈钢毛细管柱, 将脉冲间隔调整到正好使柱管局部完成热平衡, 用快速PID技术控制脉冲频率和宽度, 设计了一种直热式快速升温装置. 该装置最高升温速率可达到5 ℃/s, 升温范围 40~150 ℃, 程序升温线性相关系数大于0.9996, 最大功耗74 W, 加热平均功耗小于50 W, 在34 s内完成nC8~nC17 10种正构烷烃的分离, 保留时间重复精度误差RSD在0.22%~0.55％之间, 降温和平衡时间仅为30 s. 与常规气相色谱仪相比, 该装置分析挥发性和半挥发性有机物速度可提高20倍以上, 专用于快速气相色谱仪.     

Possibilities and Limitations of Fast Temperature Programming as a Route towards Fast GC

One possible way to speed up a gas chromatographic analysis is the application of fast temperature programming by using resistive heating techniques. With this heating technique programming rates up to 20° per second can be reached. A relative standard deviation of retention times better than 0.2% is obtained. Using fast temperature programming the analysis-times of a mineral oil sample, an industrial oligomer sample, and toxic compounds in diesel fuel have been reduced 5 to 20 times, compared to a standard temperature programmed analysis. In most cases resistive heating cannot be applied to reduce the analysis time of a complex sample. The use of fast temperature programming is preferable to the use of short columns and columns operated at above-optimum carrier gas velocities.     

毛细管气相色谱法测定果蔬中20种有机磷农药残留量

毛细管气相色谱法测定果蔬中２０种有机磷农药残留量庄无忌周昱（中国商检技术研究所北京１０００２５）（厦门商检局厦门３６１０１２）１前言食品中多种有机磷农药残留量的测定国外已有报道￣［１～４］,国内也正在开展此项工作。李聪等￣［５］曾报道了低脂肪样品中１...     

快速毛细管气相色谱分析白酒中的香味成分

本文建立了快速毛细管气相色谱法,在10 min内分离了白酒中的香味成分,并对其中的醇、醛、酸、酯进行定性分析,对主要呈味成分己酸乙酯进行定量分析,方法重复性好,回收率较高。与常规毛细管色谱法相比,快速毛细管气相色谱法有效地缩短了分析时间,提高了白酒的分析效率。     

用毛细管色谱柱分离有机磷农药

本文介绍了用SE-30毛细管柱、高速率程序升温分离13种有机磷农药。其分离效果较好,分析速度较快,有良好的线性关系和重复性。     

Fast Capillary Gas Chromatography: Comparison of Different Approaches

Savings in analysis time in capillary GC have always been an important issue for chromatographers since the introduction of capillary columns by Golay in 1958. In laboratories where gas chromatographic techniques are routinely applied as an analytical technique, every reduction of analysis time, without significant loss of resolution, can be translated into a higher sample throughput and hence reduce the laboratory operating costs. In this contribution, three different approaches for obtaining fast GC separations are investigated. First, a narrow-bore column is used under conventional GC operating conditions. Secondly, the same narrow-bore column is used under typical fast GC conditions. Here, a high oven temperature programming rate is used. The third approach uses a recent new development in GC instrumentation: Flash-2D-GC. Here the column is placed inside a metal tube, which is resistively heated. With this system, a temperature programming rate of 100°/s is possible. The results obtained with each of these three approaches are compared with results obtained on a column with conventional dimensions. This comparison takes retention times as well as plate numbers and resolution into consideration.     

Fast Solvating Gas Chromatography of Environmentally Important Compounds Using Polymer-Encapsulated Silica Particles

Rapid separations of selected environmentally important polar compounds using polymer-encapsulated silica stationary phases and a carbon dioxide mobile phase under solvating gas chromatography (SGC) conditions are reported. Ten underivatized short chain aldehydes and ten nitrogen-containing herbicides were separated within 1 min and 5 min, respectively, using a 30 cm×250 μm i. d. column packed with diol-bonded, polyethylenimine (PEI)-coated, and hexamethyldisilazane (HMDS)-end-capped silica particles (5 μm, 120 Å). Seven organophosphorus pesticides were resolved in less than 5 min using a 30 cm×250 μm i. d. column packed with polymethylhydrosiloxane-deactivated and SE-54 encapsulated silica particles. Separation numbers per unit time increased with pressure and temperature ramps. Both rapid pressure and temperature programming can be used to increase the speed of SGC. The effects of pressure and temperature on apparent retention factors of solutes with various polarities were investigated using diol-PEI-HMDS silica particles in SGC.     

聚硅氧烷离子液体用于快速气相色谱固定相的研究

合成了聚硅氧烷键合离子液体[PSOMIM][NTf2],并将其用作快速气相色谱柱的固定相.初步探索了采用短柱及小内径毛细管柱(3 m×75 μm i.d.)时的分离性能及固定相膜厚对分离性能的影响.与常规柱(8m×0.25 mmi.d.)相比,在不损失分离度的前提下,分离速度可提高1～6倍;当膜厚为0.056 μm时,可以将分离速度提高2～4倍.实验结果表明,聚硅氧烷键合离子液体固定相可以有效弥补由于缩短柱长所导致的分离度减小的问题,在快速气相色谱固定相方面具有较好的应用前景.     

快速气相色谱法测定汽车工业废气中芳烃排放量

采用气体直接进样及快速程序升温气相色谱法,能在８０ｓ内快速,简单地测定废气中芳烃等多种组分的含量。在本方法中,芳烃的最低检出浓度为０．１ｍｇ／ｍ６３,该方法允在两周内测定了汽车喷漆车间４８个排气口的５７６个样品,具有简单,快速,灵敏,实用等优点,特别适合于涂装工业气体稀释溶剂样品的测定。     

气相色谱法同时测定粮食中14种有机磷残留量

建立了气相色谱法同时测定粮食中14种有机磷农药残留的方法。样品经乙腈溶解,高速匀浆,振荡提取,离心浓缩定容,气相色谱外标法定性定量。敌敌畏等14种有机磷农药在DB-1701毛细管柱上得到了很好的分离,在浓度为0.05～2.00mg/L范围内线性关系良好,相关系数r为0.99～1.00,最低检出限为0.01～0.08mg/kg;当添加水平为0.100、0.500、1.000mg/kg 时,回收率为71.2%～113.1% ,相对标准偏差为2.2%～6.9%。方法简单、快速、准确、灵敏,适用于一般检验机构的日常检验需要。     

分散液液微萃取-气相色谱法快速测定水中23种有机磷农药

建立了分散液液微萃取(DLLME)的新型样品前处理方法,并采用气相色谱/火焰光度检测器对饮用水中的治螟磷、甲拌磷、二嗪农、乙拌磷、甲基毒死蜱、甲基对硫磷、皮蝇磷、杀螟松、马拉硫磷、毒死蜱、倍硫磷、对硫磷、溴硫磷、嘧啶磷、甲基异硫磷、稻丰散、杀扑磷、丙溴磷、乙硫磷、三唑磷、三硫磷、哒嗪硫磷、亚胺硫磷23种痕量有机磷农药残...     

网格搜索法优化毛细管气相色谱线性程序升温

 用一种新的计算程序进行毛细管气相色谱线性程序升温的优化。在OV 10 1固定相上对 2 1种Kovats保留指数为 6 0 0～ 10 0 0的组分进行了自动寻优工作 ,并分别在起始温度为 2 5℃和 30℃的线性程序升温条件下取得了较好的结果。这种优化方法不但节省了计算时间 ,而且在对计算程序进行适当修改后 ,可以用于多阶程序升温的优化工作。     

毛细管气相色谱法测定热不稳定有机磷农药辛硫磷

The thermo-labile organophosphorous pesticide Phoxim was determined by capillary gas chromatographywith flame phototnetric detector. When high linear velocity H_2(>200cm/s) was used as carrier gas,the thermo-decomposition of Phoxim was considerably reduced.The most important gas chromatography conditions,injectortempereture and column head pressure,were studied.The thermo-decomposition preducts were identified by gaschromatography-mass spectrometry.     

固相萃取-气相色谱法测定茶叶中多种有机磷农药

建立了固相萃取-气相色谱法同时测定茶叶中16种有机磷农药残留的方法.样品用丙酮超声提取后,经自制的N-丙基乙二胺(PSA)/活性炭固相萃取柱净化,以混合溶剂乙腈/甲苯(V(乙腈)∶V(甲苯)=1∶3)洗脱,采用气相色谱-氮磷检测器(GC-NPD)测定.方法的回收率在62.8%～109.1%之间,相对标准偏差小于14.7%1,6种有机磷农药的检出限在0.01～0.16 mg/kg之间.方法快速简便、经济实用。     

快速气相色谱控制系统的设计与应用

设计了一种用于快速气相色谱(Fast gas chromatography,FGC)的新型控制系统。该控制器主要由色谱柱温度控制系统、自动进样及气路压力控制系统组成。其温度控制范围为30~160℃,升温速度约为3℃/s,温度控制精度为±0.5℃,载气压力控制范围为0~0.5 MPa。将本控制器应用于自制快速色谱,并用色谱对由直链正构烷烃(C1~C8)以及甲苯9种物质组成的标准样品进行测试。结果显示,色谱能在100 s内将此9种物质完全分开。     

超声波辅助萃取-气相色谱法同时测定蔬菜中5种有机磷农药残留

建立超声波辅助萃取-气相色谱法同时分离测定蔬菜中5种有机磷农药残留量的：弓．法。实验结果表明,采用超声波加速提取有机磷农药残留,样品提取效果好,干扰物少,检测快速;在DB-1701色谱柱中,供试的5种有机磷农药分离良好;以FPD为检测器,选择性较好。方法的检出限为0．004-0．01μg／mL,5种农药在2个添加水平下的回收率为78．9％-105．9％,测定结果的相对标准偏差为2．6％-7．6％（n=6）。该方法具有测定有机磷农药种类多、快速等优点,能满足农药多残留分析的要求。     

固相萃取/气相色谱法测定禽蛋中19种农药残留

建立了QuEChERS及固相萃取净化技术结合气相色谱法测定禽蛋中19种农药(联苯菊酯、甲氰菊酯、氯菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯、敌敌畏、甲胺磷、乙酰甲胺磷、二嗪磷、乐果、甲基嘧啶磷、毒死蜱、杀螟硫磷、丙溴磷、氟虫腈、氟甲腈、氟虫腈硫醚及氟虫腈砜)残留的分析方法。蛋液样品经乙腈及QuEChERS提取盐包提取后,采用石墨化碳黑(GCB)吸附剂和十八烷基硅烷键合硅胶(C₁₈)SPE小柱净化,以Agilent DB-1701(30 m×0.32 mm,0.25μm)毛细管色谱柱分离,在气相色谱火焰光度检测器(Flame photometric detector,FPD)及电子捕获检测器(Electron capture detector,ECD)上检测,外标法定量。结果显示,19种农药在各自线性浓度范围内线性关系良好,相关系数(r²)均不小于0.999 3;在低、中、高3个加标水平下的回收率为78.6%～105%,相对标准偏差(n=6)为1.6%～9.3%,检出限(LOD,S/N=3)为0.138～8.33μg/kg,定量下限(LOQ,S/N=...     

气相色谱法分离检定血中八种氨基甲酸酯

采用国产Ｃ＿１８往固相提取血中八种氨基甲酸酯,用乙酸乙酯洗脱,用气相色谱分离检定,用气相色谱／质谱进行确证。此法灵敏度为１～２μｇ／ｍＬ血,最低检出限为２０～４０ｎｇ,回收率在６２～９２％之间。