Abstract

AbstractA direct two‐dimensional gas chromatographic method is proposed for simultaneous determination of aqueous formaldehyde and other products present in the reaction sample. Using Deans switch, HCHO‐H2O peak pair eluting from the first dimension column is heart cut into the second column where H2O and HCHO are separated and quantified using thermal conductivity detection. Formaldehyde being a dissolved gas, the influence of the plunger speed on the repeatability was investigated. A reduction in the plunger speed from 300 (default) to 5 μL/min results in a major improvement in repeatability precision from 9.6 to 0.7 (RSD). The method is being used to quantify initial and final amount of HCHO in the range 0.02–0.36 g/g, along with other reaction products. The proposed method is validated by analyzing three commercial aqueous formaldehydes using two different techniques: USP29‐NF24 (by titrimetry) and derivatization method involving HCHO‐2,4‐dinitrophenylhydrazine derivative on a high‐performance liquid chromatography with UV detection system.

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