Formaldehyde is a chemical used in many different industrial sectors and is classified as a carcinogen as well as causing allergic reactions. Due to the health effects of formaldehyde, which is widely used in textile dyes and auxiliary chemicals, its analysis in this type of matrices becomes important. In this study, in order to meet these requirements, formaldehyde was converted to oxime derivative by derivatization with o-(2,3,4,5,6-Pentafluorobenzyl)hydroxylamine hydrochloride. This derivative was successfully sampled with the headspace technique and analyzed with a gas chromatography-flame ionization detector (GC-FID). For the developed method, derivatization and salt effect parameters were investigated. For the method, the limit of detection (LOD) was found as 0.05 mg L
−1
and real sample analyzes were made for different types of dyes used in the textile industry, and sodium naphthalene sulfoxylate formaldehyde. In addition, the developed method was validated with sodium naphthalene sulfoxylate formaldehyde against ISO 14184-1 method by applying student t-, F-tests and no difference was found in terms of accuracy and precision. Thus, the applicability of the developed method to dyes and auxiliary chemicals used in the textile industry was successfully demonstrated. This allows all quality control processes to be handled using only one method.