This article discusses the preparation of environmental samples to be analyzed for chemicals related to the chemical weapons convention (CWC), where analysis takes place on‐site or off‐site by gas chromatography (GC) or liquid chromatography (LC) as an introduction technique to spectrometers or by capillary zone electrophoresis (CZE). The specific sample preparation methods required for analysis by spectroscopic techniques such as Fourier transform infrared (FTIR) and nuclear magnetic resonance (NMR) spectroscopy are dealt with in separate articles. Preparations of analytical samples from air, aqueous liquid (water), soil, active charcoal, wipe, concrete, paint, rubber, and other polymeric samples for off‐site analysis are presented in section 2, and preparations of analytical samples from aqueous liquid (water), soil, and wipe samples for on‐site analysis, are covered in section 3. Preparations for on‐site analysis are as described in the standard operating procedures (SOPs) of the international organization responsible for verifying the Convention (Technical Secretariat of the Organization for the Prohibition of Chemical Weapons) and those for off‐site analysis are as described in the corresponding recommended operating procedures (ROPs). Section 4 examines the question of quality control (QC) in sample preparation and section 5 the important matter of safety in handling samples containing CWC‐related chemicals. Section 6 reports on the use of the methods in international comparison and proficiency tests.