当前位置: X-MOL 学术J. Chromatogr. A › 论文详情
Our official English website, www.x-mol.net, welcomes your feedback! (Note: you will need to create a separate account there.)
Preconcentration and partial separation of nitroaromatic vapors using a methyltrimethoxysilane-based sol-gel
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2017-11-04 , DOI: 10.1016/j.chroma.2017.11.006
Michelle M. Cerreta , Kevin J. Johnson , Braden C. Giordano

Typical trace vapor analysis involves sorbent trapping, followed by desorption and chromatographic separation. This communication describes a method for streamlining this process by combining sorbent sampling/preconcentration with partial separation achieved through temperature-programmed thermal desorption. A novel sorbent trap was formulated in which tubular glass liners for a programmable-temperature gas chromatograph inlet were coated with a sol-gel based polymer stationary phase synthesized from methyltrimethoxysilane precursor and installed into the inlet, which was directly connected to a mass-selective detector by a fused silica capillary transfer line. This method is shown to achieve partial separation of two nitroaromatic vapors in a total 3–5 min analysis time, which represents a tenfold improvement in speed in terms of the overall cycle time compared to an analogous conventional vapor analysis method. Both analytes proved to have a high dynamic range and loading capacity, with nitrobenzene achieving both high and low sampling extremes (0.32 ng–4 μg sampling concentration) with only a slight compromise in peak broadening. The multivariate curve resolution by alternating least squares algorithm (MCR-ALS) was shown to successfully resolve the overlapped elution profiles of the two nitroaromatic test vapors examined in this study.



中文翻译:

使用基于甲基三甲氧基硅烷的溶胶-凝胶对硝基芳族蒸气进行预浓缩和部分分离

典型的痕量蒸气分析涉及吸附剂捕集,然后进行解吸和色谱分离。该通讯介绍了一种通过结合吸附剂采样/预浓缩与通过程序升温热脱附实现的部分分离来简化此过程的方法。配制了一种新型的吸附阱,其中用于可编程温度气相色谱仪入口的管状玻璃衬管上涂有由甲基三甲氧基硅烷前体合成的溶胶-凝胶基聚合物固定相,并安装在入口中,该入口直接连接到质量选择检测器通过熔融石英毛细管传输线。结果表明,该方法可在总的3-5分钟分析时间内实现两种硝基芳族气体的部分分离,与类似的常规蒸气分析方法相比,它在总循环时间方面的速度提高了十倍。两种分析物均具有较高的动态范围和负载能力,硝基苯可实现高和低的采样极限值(0.32 ng–4μg采样浓度),并且仅对峰展宽有所影响。通过交替最小二乘算法(MCR-ALS)进行的多变量曲线解析已成功解决了本研究中检测到的两种硝基芳族测试蒸气的重叠洗脱曲线。32 ng–4μg的采样浓度)在峰展宽方面仅稍有妥协。通过交替最小二乘算法(MCR-ALS)进行的多变量曲线解析可成功解决本研究中检测到的两种硝基芳族测试蒸气的重叠洗脱曲线。32 ng–4μg的采样浓度)在峰展宽方面仅稍有妥协。通过交替最小二乘算法(MCR-ALS)进行的多变量曲线解析可成功解决本研究中检测到的两种硝基芳族测试蒸气的重叠洗脱曲线。

更新日期:2017-11-04
down
wechat
bug