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The mining industry carried out without an adequate planning and control, can cause serius damages to the environment, especially to the courses of water as rivers, whether during the works of extraction and processing of the minerals like also in the phase of abandonment of the activity. The effluents with high contents in metals, originating in mines abandoned, they represent one of the greater environmental problems of the metallic mining industry, above all because its persistence in the environment can be extended during decades. This is the case of various existing mining districts in the world and particularly in Peru, as the Mining District of Hualgayoc, located close to the Bambamarca district, in the province of Hualgayoc, department of Cajamarca, Peru. Generally, for the knowledge of level of contamination of a river or a river bed, is used to take samples of water and its corresponding chemical analysis. This is, without doubt, basic and important information, but it gives us information very limited to carry out a deeper study of the contamination found. The present investigation adds to the water quality studies, the study of sediments taken in the river bed Hualgayoc and the subsequent application of not only techniques of classical chemical analysis, but also techniques of mineralogical analysis, like the microscopy and reflection techniques. Additionally, the processing of the results of chemical analysis of water and sediments is carried out by means of statistical techniques, including the multivariate. The joint of techniques used constitutes a useful tool to establish affinities and correlation among the samples of water and sediments and for the clarification of the possible sources or causes of the contamination of the river beds..