The article introduces a novel technique called triboelectric spectroscopy (TES) for in situ chemical analysis of liquids. TES combines triboelectrification and charge transfer on the surface of electrical insulators to detect ions and small organic molecules in liquid samples. The method is nondestructive, ultrafast (<1 s), and can identify over 30 types of common salts, acids, bases, and organic molecules with a qualitative and quantitative accuracy of about 93%. The detection limit is as low as ppb levels. The TES profile is unique and can be automated for identification, making it a portable and low-cost tool for chemical analysis. The mechanism behind TES involves the competition of cation adsorption on the charged insulator surface and the interfacial concentration distribution of H3O+. The technique is applicable to a wide range of chemicals and can be integrated with microchip technology for miniaturized, portable, and in situ detection, potentially finding applications in chemistry, biology, environmental sciences, and health monitoring.The article introduces a novel technique called triboelectric spectroscopy (TES) for in situ chemical analysis of liquids. TES combines triboelectrification and charge transfer on the surface of electrical insulators to detect ions and small organic molecules in liquid samples. The method is nondestructive, ultrafast (<1 s), and can identify over 30 types of common salts, acids, bases, and organic molecules with a qualitative and quantitative accuracy of about 93%. The detection limit is as low as ppb levels. The TES profile is unique and can be automated for identification, making it a portable and low-cost tool for chemical analysis. The mechanism behind TES involves the competition of cation adsorption on the charged insulator surface and the interfacial concentration distribution of H3O+. The technique is applicable to a wide range of chemicals and can be integrated with microchip technology for miniaturized, portable, and in situ detection, potentially finding applications in chemistry, biology, environmental sciences, and health monitoring.