Lim Jeong Sik, Yoon Doohyun, Kim Taewan, Lee Jinbok
Precision Measurement, University of Science and Technology (UST), Gajeong-ro 217, Yuseong-gu, Daejeon 34113, Republic of Korea.
Semiconductor and Display Metrology Group, Korea Research Institute of Standards and Science (KRISS), Gajeong-ro 267, Yuseong-gu, Daejeon 34113, Republic of Korea.
ACS Omega. 2024 Aug 21;9(35):37225-37230. doi: 10.1021/acsomega.4c04563. eCollection 2024 Sep 3.
In this study, an add-on preconcentration device powered by parallelized pretraps (PPTs) was utilized to measure the sub-pmol/mol levels of NF in N. The add-on preconcentrator was coupled to the detachable trap preconcentrator (DTP) with a gas chromatograph-mass spectrometer [ 3342-3349]. The breakthrough volume of the parallel configuration was found to be substantially higher than that of the serial configuration with the same amount of adsorbent (HayeSep D). Liquid oxygen (LO) cooling (-183 °C) exhibited better preconcentration performance for NF in N compared to NF in air (N + O) with liquid nitrogen cooling (-195 °C) and NF in air with LO cooling. The DTP unit was essential to discriminate residual species, such as N, O, CO, and CF, of which the preconcentrated portion in the PPT can be excessive, enabling the overwhelm filtering capability of the quadrupole mass spectrometer. The limit of detection of NF in N of the PPT/DTP/gas chromatograph-mass spectrometer was 0.01 ppt, which is significantly better than that determined without using the add-on preconcentration device (0.21 ppt).
在本研究中,采用了一种由并行预捕集器(PPTs)驱动的附加预浓缩装置来测量氮气中痕量的亚皮摩尔/摩尔水平的NF。该附加预浓缩器与带有气相色谱 - 质谱仪的可拆卸阱预浓缩器(DTP)相连[3342 - 3349]。发现相同吸附剂(HayeSep D)用量下,并联配置的穿透体积显著高于串联配置。与液氮冷却(-195°C)的空气中的NF以及液氧冷却的空气中的NF相比,液氧(LO)冷却(-183°C)对氮气中NF表现出更好的预浓缩性能。DTP单元对于区分残留物种(如N、O、CO和CF)至关重要,其中PPT中预浓缩部分可能过多,这使得四极杆质谱仪具有强大的过滤能力。PPT/DTP/气相色谱 - 质谱仪对氮气中NF的检测限为0.01 ppt,明显优于未使用附加预浓缩装置时测定的检测限(0.21 ppt)。