This paper reports on an unknown yellowish mineral compound found in an archaeological context from Chorrillos cemetery (Calama, Chile) dating to the Early Formative period (800 - 200 B.C.). We used optic microscopy, SEM, EDX, ¹H-RMN, 13C-RMN, and infrared (IR) and Raman spectroscopy to tease out the chemical and molecular composition of the sample. The microscopic images show amorphous yellowish granulates with heterogeneous chemical surfaces. ¹H-RMN and 13C-RMN negative results show that the sample is free of organic matter. The SEM and EDX indicate the presence of arsenic and sulfur in the sample. The IR and Raman analyses suggest the presence of orpiment which is a toxic yellow arsenic sulfide mineral.