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Isotopic signatures of atmospheric methanol and acetaldehyde have the potential to improve our ability to quantitatively assess their importance in atmospheric chemistry. However, isotopic measurements of atmospheric methanol and acetaldehyde and their individual source and sink processes have been limited. In this service, we examined gas chromatography-isotope ratio mass spectrometry combined with headspace solid-phase microextraction to measure the carbon isotope ratios of methanol and acetaldehyde in air samples.