Gas Chromatography with In Situ Catalytic Hydrogenolysis and Flame Ionization Detection for the Direct Measurement of Formaldehyde and Acetaldehyde in Challenging Matrices

Abstract

A gas chromatographic strategy to advance the direct detection and quantification of volatile aliphatic aldehydes such as formaldehyde and acetaldehyde in gas phase matrices without the need for sample pretreatment or concentration has been successfully developed. The catalytic hydrogenolysis of aldehydes to alkanes is conducted in situ within the 3D-printed steel jet assembly of the flame ionization detector and without any additional hardware required. Reliable conversion efficiencies of greater than 90% with respectable peak symmetries for the analytes were attained at 400 °C. Quantification of formaldehyde and acetaldehyde at parts-per-million levels over a range of 0.5–300 ppm (v/v) for formaldehyde and 0.2–430 ppm (v/v) for acetaldehyde with a respectable precision of less than 5% RSD (n = 10) was achieved. The total analysis time was less than 10 min. Linearity with a correlation coefficient (R 2) greater than 0.9997 and measured recoveries of >99% for spike tests under the specified conditions were achieved. The 3D-printed steel jet assembly was found to be reliable and resilient to matrices such as air, water, hydrocarbons, and aromatics. An additional benefit realized with this analytical strategy is that the slight restriction induced by the presence of the catalyst in the 3D-printed jet assembly enables backflush via the inlet split vent without the need for additional pressure control or intercolumn-connection devices. The utility of this technique was demonstrated with important aldehyde applications from various segments.

Metal 3D‐printed catalytic jet and flame ionization detection for in situ trace carbon oxides analysis by gas chromatography

“…The reduction in temperatures minimizes chromatographic column stationary phase breakdown due to thermal stress, reduces oven cool‐down time after oven temperature programming is complete and therefore improves sample throughput. The detail of this backflush concept has been described elsewhere .…”

Approaches to Formaldehyde Measurement: From Liquid Biological Samples to Cells and Organisms

“…Further, the catalyst-based method was upgraded and catalytic hydrogenolysis was performed directly in a 3D-printed FID jet consisting of an FID combined with a catalyst support for hydrogenolysis. The sensitivity of this approach reaches ppm level in the range of 0.5–300 ppm [ 63 ]. The main advantages of this method are the absence of the need for preliminary preparation, derivatization, and concentration of the sample.…”

Highly Sensitive and Selective Detection of Formaldehyde via Bio-Electrocatalysis over Aldehyde Dehydrogenase

“…Therefore, a simple detection method with high sensitivity and specificity is desired for quick and accurate assessment of indoor formaldehyde. Analytical methods currently developed for formaldehyde mainly include gas/liquid chromatography, , spectrophotometry, fluorometry, − and sensors. − While these methods served their goals of detecting formaldehyde, a majority of those require long preparation time, unstable chemicals, or expensive equipment and sometimes lack specificity. Electrochemical sensors for formaldehyde detections, owing to their low cost and facile operations properties, have attracted much interest recently.…”