An in situ facile growth procedure was developed in this paper, for the first time for preparing a hierarchical threedimensional composite containing graphene layers with layered double hydroxide (LDH) nanosheet groups. The production procedure includes covering TiOOH colloids over the graphene surfaces and the following in situ evolution of layered NiTi-LDH nanosheet groups on the graphene sheets surfaces within a hydrothermal procedure. It was understood that by growing the NiTi-LDH nanosheet groups uniformly and perpendicularly over graphene sheets’ both sides, a hierarchical three-dimensional nanocomposite is constructed. The volatile Lavandula angustifolia compounds were collected and detected through headspace solid-phase microextraction utilizing GO/Ni–Ti-LDH fiber along with capillary GC–MS as a controlling method. The laboratory parameters included sample weight, humidity effect, extraction time, extraction temperature, desorption temperature, and desorption time, which were tested and enhanced. HS-SPME was used after GC–MS to separate and identify thirty-two compounds.
