热脱附管实验及应用

前言

我们希望采用热脱附的方法进行气体中微量化合物的富集，从而在GC系统中进行气体中物质组分分析。
 

定义

热脱附通常对由不锈钢管、吸附材料、两端的黄铜盖和聚四氟乙烯套圈等部分组成的不锈钢吸附管进行操作。不锈钢管的内部结构，以及吸附材料以怎样的方式附着在不锈钢管内，还有待通过论文探索。

直接脱附通常采用玻璃管，因为更容易定位样品，并在分析前后监测其状态。直接脱附是一种从含有较高浓度挥发物的均匀材料中采集挥发性有机物的有效方式。
 

作用

吸附管的作用是为了预富集微量化合物，这些物质称为 痕量物质。痕量物质一般指试样中含量少于0.01%的物质，如果它的含量低于分析方法的测定下限，就必须采用预富集的办法，从大量母体物质中搜集欲测定的痕量元素至一较小的体积，从而提高其含量至测定下限以上，这种分析方法称为痕量富集。

吸附管的采样方式有两种：主动（泵）采样，被动（扩散）采样。
 

文献实验

《Evaluation of a standardized collection device for exhaled breathsampling onto thermal desorption tubes》
doi:10.1088/1752-7163/ab7e3b

Exhaled breath was concentrated simultaneously on stainless steel reconditioned Tenax TA (35/65 mesh, PN: C1-AXXX-5003) and Tenax/Carbograph 5TD (5TD, PN: C2-AXXX-5149), thermal desorption (TD) tubes (Markes International, South Wales, UK). The Tenax TA adsorbent tubes were selected due to their frequent use among exhaled breath researchers [14–36]. Tenax/Carbograph 5TD tubes were selected based on the recommendation of Owlstone Medical, the ReCIVA manufacturer. To minimize TD tube batch variability, the same forty tubes, twenty of each adsorbent material, were used randomly for all exhaled breath collections. Control and background samples were collected on each TD tube adsorbent type, Tenax TA or 5TD, using serial numbers independent of those used for exhaled breath collections. Reconditioning, following each use, was performed at 320 ◦C for 1 h with 85 ml min−1 of 99.999% nitrogen backflush on a Markes International TC-20. All thermal desorption tubes were stored at ambient temperature with brass caps and polytetrafluoroethylene ferrules affixed to each end until experimental use.

《Stability of Propofol (2,6-Diisopropylphenol) in Thermal Desorption Tubes during Air Transport》
doi.org/10.1155/2019/3987417

We dissolved propofol (97%, Sigma Aldrich,Munich, Germany) in HPLCgrade water (VWR, Darmstadt, Germany) to a 50 𝜇g/mL propofol stock solution. The stock solution was gravimetrically diluted in 50 mL flasks to 5, 10, 20, and 50 𝜇g/mL samples. For sample preparation and application into the GC-MS, we used Tenax sorbent tubes (Tenax GR, Gerstel, M¨uhlheim, Germany).

《Recovery and reactivity of polycyclic aromatic hydrocarbons collectedon selected sorbent tubes and analyzed by thermal desorption-gaschromatography/mass spectrometryM.》
doi.org/10.1016/j.chroma.2019.05.030

A 2000 ng/uL Restek Corporation (Bellefonte, PA, USA) PAH standard (catalog no. 31011, lot no. A099403) with 16 compoundswas diluted in HPLC grade methanol (Fisher Scientific, Hamp-ton, NH, USA) to prepare 1.0 and 2.0 ng/uL PAH standards. PAH standards were loaded onto sorbent tubes in 1 or 2 uL volumes. The sorbent tubes utilized for experimental analysis of PAHsare listed in Table 1, and were supplied by Markes International(Gold River, CA, USA) or PerkinElmer Life & Analytical Sciences(Shelton, CT, USA).

 

实际应用

 

填料选型

Markes公司的热脱附管填料参考手册（非完整版）如下：