Evaluation of split/splitless operation and rapid heating of a multi-bed sorption trap used for gas chromatography analysis of large-volume air samples.
Evaluation of split/splitless operation and rapid heating of a multi-bed sorption trap used for gas chromatography analysis of large-volume air samples.
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对用于大体积空气样品气相色谱分析的多床吸附阱的分流/不分流操作和快速加热进行评估。
DOI：
10.1002/jssc.200500276
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发表时间：
2006
影响因子：
3.1
通讯作者：
Sacks,RichardD
中科院分区：
文献类型：
--
作者：
Whiting,JoshuaJ;Sacks,RichardD
评估了分流操作和快速阱加热对来自电加热的微型多床吸附阱的注入塞宽度的影响。吸附阱的设计目的是定量收集大体积蒸气样品中的挥发性有机化合物，并将其注入气相色谱仪。以前的捕集器设计导致进样塞宽度通常为1秒或更长，这显著降低了色谱分离度，特别是对于早期洗脱的样品组分和高速分离。进样塞的宽度取决于样品解吸过程中捕集器的加热速率和载气通过捕集器的体积流速。研究了捕集器的加热速率和通过捕集器的载气速度对戊烷、辛烷和十一烷的注入塞宽度的影响。通过将来自捕集器的流在柱和排气口之间分流来增加通过捕集器的载气速度。这减少了从捕集器到色谱柱的传输时间，从而减少了注射塞宽度。通过增加4 V至30 V范围内的施加电压来增加捕集器的加热速率。增加加热速率可以减少从吸附剂床中解吸分析物所需的时间，从而减少注射塞宽度。在分流模式下，对于正戊烷、正辛烷和正十一烷，分别以非常快的加热速率获得了小至89、210和520 ms的注入塞宽度。还评价了分流比对分离度、峰高和峰宽的影响。
The effects of split‐flow operation and rapid trap heating on injection‐plug widths from an electrically heated, microscale, multibed sorption trap were evaluated. The sorption trap has been designed to quantitatively collect volatile organic compounds from large‐volume vapor samples and inject them into a gas chromatograph. Previous trap designs resulted in injection‐plug widths of typically a second or more, and this significantly degraded chromatographic resolution, particularly for early‐eluting sample components and for high‐speed separations. Injection‐plug widths are determined by the heating rate of the trap during sample desorption and the volumetric flow rate of carrier gas through the trap. The effects of the heating rate of the trap and carrier gas velocity through the trap on the injection‐plug widths of pentane, octane, and undecane were studied. Carrier gas velocity through the trap was increased by splitting the flow coming from the trap between the column and a vent. This decreases transport time from the trap to the column, and thus decreases injection‐plug widths. The heating rate for the trap was increased by increasing the applied voltage in the range from 4 to 30 V. Increasing the heating rate decreases the time required to desorb the analytes from the sorbent bed, thus decreasing injection‐plug width. Injection‐plug widths as small as 89, 210, and 520 ms were obtained in the split mode with very fast heating rates forn‐pentane,n‐octane, andn‐undecane, respectively. The effect of split ratio on resolving power, peak height, and peak width was also evaluated.
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DOI：
10.1007/s002160050014
发表时间：
2000-01-01
期刊：
FRESENIUS JOURNAL OF ANALYTICAL CHEMISTRY
影响因子：
--
作者：
Dettmer, K;Knobloch, T;Engewald, W
通讯作者：
Engewald, W
影响因子：
3.1
作者：
Sanchez, JM;Sacks, RD
通讯作者：
Sacks, RD
影响因子：
7.4
作者：
Calogirou, A;Larsen, BR;Kotzias, D
通讯作者：
Kotzias, D
影响因子：
7.4
作者：
Lu, CJ;Whiting, J;Zellers, ET
通讯作者：
Zellers, ET
影响因子：
6.1
作者：
Lu, CJ;Steinecker, WH;Zellers, ET
通讯作者：
Zellers, ET