Centro de Investigaciones en Catálisis (CICAT), Escuela de Ingeniería Química, Universidad Industrial de Santander, Parque Tecnológico de Guatiguará, Km 2 vía El Refugio, Piedecuesta, Santander 681011, Colombia.
Laboratorio de Ciencia de Superficies (SurfLab), Universidad Industrial de Santander, Parque Tecnológico de Guatiguará, Km 2 vía El Refugio, Piedecuesta, Santander 681011, Colombia.
J Am Soc Mass Spectrom. 2021 Aug 4;32(8):2135-2143. doi: 10.1021/jasms.1c00090. Epub 2021 Jun 28.
The accuracy of the online quantification of gaseous effluents from catalytic reactors by mass spectrometry (MS) is rarely addressed by researchers despite the extensive use of the technique. MS results are strongly sensitive to both the operation conditions of the reactor and to the state of the instrument. Therefore, most studies use them as qualitative descriptors of the performance of catalytic reaction systems. The purpose of this work was to develop an accurate method for the quantification of gaseous effluents from catalytic reactors. For this purpose, the mathematical expressions from the so-called external and internal standard calibration methods for MS were coupled to the typical metrics used for studying catalytic reactions, namely, conversion, selectivity, and carbon mass balances. The catalytic combustion of methane was selected as a model reaction to test the developed approach. The accuracy of the developed method was validated by comparison with results obtained in a separate reaction system coupled online to a gas chromatograph. The closure of the carbon mass balance was used as control metrics allowing for the assessment of the physical meaning of the method. In general, the internal standard method of calibration was found to be best for the accurate quantification of gaseous streams by online mass spectrometry. In general, the results of this investigation may be of use to researchers in the field of catalysis as well as to research workers using mass spectrometry for various purposes.
尽管质谱（MS）技术被广泛应用，但研究人员很少关注在线定量催化反应器中气态排放物的准确性。MS 结果对反应器的操作条件和仪器的状态都非常敏感。因此，大多数研究将其用作催化反应系统性能的定性描述符。本工作旨在开发一种用于定量催化反应器中气态排放物的准确方法。为此，将所谓的外部和内部标准校准方法的数学表达式与用于研究催化反应的典型指标（转化率、选择性和碳质量平衡）相结合。选择甲烷的催化燃烧作为模型反应来测试所开发的方法。通过与在线耦合到气相色谱仪的单独反应系统获得的结果进行比较，验证了所开发方法的准确性。碳质量平衡的闭合用作控制指标，允许评估方法的物理意义。一般来说，发现内部标准校准方法最适合通过在线质谱法对气态流进行准确定量。总的来说，这项研究的结果可能对催化领域的研究人员以及使用质谱进行各种目的的研究人员有用。
