Water analysis is an excellent interdisciplinary topic for project-based learning. An undergraduate course was designed to engage the senior undergraduate chemistry students in a real-life experience. In this course, students developed methodologies based on published American Society for Testing and Materials (ASTM) methods for the measurement of fluoride, phenols, and metals in real water samples. The procedures were utilized to analyze target analytes in real water samples from various sources, such as seawater, sewage water, swimming pool water, tap water, and drinking water in the eastern province of the Kingdom of Saudi Arabia (KSA). These areas are profoundly affected by urbanization. The students analyzed the samples by employing a portable total dissolved solids (TDS) meter, a pH/ion-selective electrode (ISE) benchtop meter, an inductively coupled plasma–optical emission spectrometry (ICP-OES), and a gas chromatography–flame ionization detector (GC-FID). The ASTM methods allowed the students to gather research-level data and study regional environmental issues. The students prepared and presented their results at the departmental conference. Through the water analysis project, students acquired field and laboratory research skills, performed a quantitative analysis of data sets, developed collaborative interactions, as well as utilized their writing and communication skills. The exposure of students to these research tools provided them with experience in dealing with the limitations of trace level analysis in real samples. The outcome of this study provided the students with an overview of how their theoretical knowledge was connected to the country’s limited water sources and pollution problems.