Multivariate calibration method for mass spectrometry of interfering gases such as mixtures of CO, N₂, and CO₂

Abstract

A multivariate calibration method for mass spectrometry is presented that enables a quantitative analysis of gas mixtures containing interfering gases that contribute to the same mass‐to‐charge ratios at nominal resolution. Multiple calibration gas mixtures with linearly independent compositions are used in order to obtain the calibration constants for the contribution of each gas to each of the mass‐to‐charge ratio peaks. The method was successfully applied to the quantitative detection of CO in a mixture with CO2 and N2, which represents a difficulty commonly encountered in heterogeneous catalysis and electrocatalysis research.

Investigation and Optimisation of Operating Conditions for Low-Temperature CO2Reduction to CO in a Forward-Bias Bipolar-Membrane Electrolyser

“…It allows for signal deconvolution in the MS, which enables the simultaneous detection of CO 2 , CO as well as N 2 . 82 Due to the well-studied selectivity of the employed Ag catalyst, the main products of interest were CO and H 2 , which were measured in addition to the Ar background, residual CO 2 and N 2 . A gas chromatograph (GC) from SRI Instruments® was employed in parallel to measure the produced CO and H 2 at an interval of 30 min, acting as an additional and continuous verification of the MS measurements.…”

An Online Gas Chromatography Cell Setup for Accurate CO2-Electroreduction Product Quantification

“…Thereafter, the working electrode compartment (11) was placed atop the PTFE foil, followed by a second PTFE foil piece (12) and the membrane (Chemours, Nafion XL-13). This was followed by another PTFE foil piece (12), the counter electrode compartment (15) and a fourth PTFE gasket (16). The cell assembly was finalized by placing a 2.5 × 2.5 cm 2 piece of 0.05 mm thick Pt-foil (Alfa Aesar, 99.99%-17) as the counter electrode, and the assembly was closed using the counter electrode current collector piece (18).…”

“…Using the above-described assembly, the contact resistance between the catalyst drop-casted on the glassy carbon or the platinum foil used as working-vs. counter-electrodes and their corresponding, stainless steel current collectors accounted for ≈0.6 Ω. (1), the cathode current collector (2), a piece of graphite foil (3), the glassy carbon plate with the drop-casted working electrode (4), PTFE gaskets (5,12,16), porous glass frits (6), PTFE frit holders (7), input line adapter screws (8), product output lines (9), PTFE plugs (10), the working electrode compartment (11), a piece of Nafion XL membrane (13), a leak-free Ag/AgCl reference electrode (14), the counter electrode compartment (15), the platinum counter electrode (17), the counter electrode current collector (18), and the PEEK inserts (19) and nuts (20) to close the assembly. phosphate (KH 2 PO 4 , Merck, LiChropur, anhydrous, 99.999%) in 50 ml of ultrapure water.…”

Insight into the Activity and Selectivity of Nanostructured Copper Titanates during Electrochemical Conversion of CO2 at Neutral pH via In Situ X-ray Absorption Spectroscopy

“…One of the channels was used to follow the changes in the total pressure, and the other five channels were used to measure the following fragments: m / z = 1, m / z = 15, m / z = 18, m / z = 26, and m / z = 28, corresponding to H 2 , CH 4 , H 2 O, C 2 H 4 , and CO/N 2 , respectively. To determine the quantitative distinction of CO (as a product), CO (as a fragment of CO 2 ), and N 2 during the reduction of CO 2 , the calibration method described by Binninger et al was implemented . The methodology for the NMR characterization of the liquid products is described in the Supporting Information.…”

“…To determine the quantitative distinction of CO (as a product), CO (as a fragment of CO 2 ), and N 2 during the reduction of CO 2 , the calibration method described by Binninger et al was implemented. 33 The methodology for the NMR characterization of the liquid products is described in the Supporting Information.…”