Center for Environment, Health, and Welfare Research, Korea Institute of Science and Technology (KIST), Seoul, 02792, Republic of Korea.
Lab Chip. 2020 Sep 21;20(18):3435-3444. doi: 10.1039/d0lc00540a. Epub 2020 Aug 13.
In this work, a 3D-printed metal column was developed for micro gas chromatography (GC) applications and its properties and gas separation performances were characterized. By using a Ti6Al4V grade 23 powder, a square spiral one meter-long column (3D-column) was 3D-printed on a planar substrate of 3.4 × 3.3 × 0.2 cm and then perhydropolysilazane (PHPS) was deposited as a pre-treatment agent, followed by a coating of stationary phase (OV-1) onto the inner wall of the micro-channel. The 500 μm-diameter circular channel and two 800 μm-wide ports of the 3D-column were confirmed to be uniform by 3D X-ray microscopy without any distortion. The physical and thermal properties of the 3D-column were found to be very similar to that of the standard Ti6Al4V grade 23 alloy with near zero porosity (∼0.07%). The 3D-column with pre-treatment and stationary coating demonstrated efficient separation performance of gas mixtures containing alkanes, aromatics, alcohols, and ketones compared to a bare or only pretreated 3D-column in terms of the peak shape, broadening, and resolution (R > 1) within 2-3 min. The well-matched thermal responses to the target temperatures were demonstrated at the ramping rates of 10-20 °C min upto 200 °C with uniform heat distribution over the 3D-column. In addition, the column bleed profiles showed that the 3D-column with PHPS had a 71% lower baseline intensity at 350 °C than that without PHPS. The 3D-column was then employed to separate a gas mixture of twelve alkanes (C9-C18, C22, C24) without any significant column bleeding and peak tailing. Therefore, the thermal responses and stability of the 3D-column promise its applicability in high temperature GC applications.
在这项工作中，开发了一种用于微气相色谱（GC）应用的 3D 打印金属柱，并对其性能和气体分离性能进行了表征。使用 Ti6Al4V 2 级粉末，在 3.4×3.3×0.2 cm 的平面基底上 3D 打印了一个一米长的方形螺旋柱（3D 柱），然后用六甲基二硅氮烷（PHPS）作为预处理剂沉积，然后在微通道的内壁上涂覆固定相（OV-1）。通过 3D X 射线显微镜确认，3D 柱的 500μm 直径圆形通道和两个 800μm 宽的端口没有任何变形，均匀一致。发现 3D 柱的物理和热性能与标准 Ti6Al4V 2 级合金非常相似，几乎没有孔隙率（约 0.07%）。与裸柱或仅预处理的 3D 柱相比，经过预处理和固定相涂层处理的 3D 柱在 2-3 分钟内实现了包含烷烃、芳烃、醇和酮的气体混合物的有效分离性能，表现出更好的峰形、展宽和分辨率（R>1）。在 10-20°C/min 至 200°C 的升温速率下，3D 柱表现出与目标温度的良好热响应，在整个 3D 柱上实现了均匀的热分布。此外，柱泄漏轮廓表明，经过 PHPS 处理的 3D 柱在 350°C 时的基线强度比未经 PHPS 处理的 3D 柱低 71%。然后，该 3D 柱用于分离十二烷烃（C9-C18、C22、C24）的混合气，没有明显的柱泄漏和峰拖尾。因此，3D 柱的热响应和稳定性有望使其适用于高温 GC 应用。
