(1) Background: It is well known that various toxic substances, including carcinogens, are generated at the fire scenes, so it is very important for firefighters to wear comprehensive personal protective equipment. The extent of the type and amount of harmful substances contained in the washing water of fire protection suits (FPS) exposed to fire scenes have not yet been confirmed. The purpose of this study is to evaluate the characteristics of harmful substances contained in wash water extracted from FPSs exposed to fire. (2) Methods: The study design was a simulation-based experimental study. To evaluate the degree of contamination exposure of FPSs, 10 sets of fire suits were classified into four groups as follows: newly supplied, field use, one fire exposure, and two consecutive fire exposures. In the experimental environment, after exposing three to four groups of FPSs to residential fire conditions. they were sealed in a plastic bag in the experimental space. The washing water for FPSs was extracted through manual washing in the order of Groups 1 to 4, and 24 items were analyzed according to the water pollution process test standards. (3) Results: According to the results of the FPS laundry analysis, the concentration of acrylonitrile in laundry was higher when exposed to fire twice than when exposed to fire once. Moreover, there was a dose–response relationship, and the risk of cumulative toxicity was shown. Naphthalene and diethylhexyl phthalate (DEHP) were detected to be high in the washing water of Group 3 FPSs exposed to incomplete combustion fire. Of the 24 items that were analyzed for in the water, four item exceeded the standard for sewage discharge facilities in accordance with the Water Environment Conservation Act. Copper and its compounds exceeded the standards by 3.4 times, antimony 4.8 times, acrylonitrile 26.0 times, and DEHP 4.1 times, respectively. (4) Conclusions: Therefore, when removing FPSs after firefighting activities, care should be taken to avoid contaminating the skin. In addition, facilities that wash FPS that have been exposed to a fire scene must have a sewage treatment and purification facility. However, if emergency decontamination of FPSs is conducted at the fire scene, the concentration of toxic substances contained in laundry can be reduced. In the case of large-scale fire, there is a risk of water pollution near the fire scene, so it is necessary to prepare a national countermeasure. The results of this study can be applied to the revision of regulations related to the building of the fire departments, reduction of water pollution, and water environment policy.
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