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用于微气相色谱的 3D 打印金属柱。

A 3D-printed metal column for micro gas chromatography.

机构信息

Center for Environment, Health, and Welfare Research, Korea Institute of Science and Technology (KIST), Seoul, 02792, Republic of Korea.

出版信息

Lab Chip. 2020 Sep 21;20(18):3435-3444. doi: 10.1039/d0lc00540a. Epub 2020 Aug 13.

Abstract

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.

摘要

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。

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