Naturally occurring heavy metals are commonly adsorbed onto substances with a large active surface, such as clays and iron oxyhydroxides. Different heavy metals could show different adsorbing preference to clays or iron oxyhydroxides, whereas a deep clay pit sediment sample with frequent subsampling gives the results that are more reliable. This study aimed to reveal differences in behavior of heavy metals and their relationships to total and amorphous iron in the deep clay pit core sample. In this research, 110 samples of the 33.0 m deep clay pit core sample were studied. Nine heavy metals from the clay open pit mine were investigated: total Fe (Fe t ) and amorphous (e.g., limonite) or poorly crystalline (e.g., ferrihydrite) (Fe am ), Mn, Co, Cr, Cu, Ni, Pb, V, and Zn. Total amounts of metals (M t ) were extracted by means of concentrated HNO 3 and HF. Amorphous amounts of iron (Fe am ) were extracted using the ammonium oxalate method. Concentrations of heavy metals were measured with an ICP-OES instrument. For statistical evaluation purposes, the following descriptive statistics tools were used: maximum, minimum, average, and median value. Behavior of heavy metals was investigated through standard deviation (SD), coefficient of variance (CV), skewness (SK), Z score (Z), PCA analysis, correlations, and correlations after Al normalization. The results of the SD and CV indicate that the clay pit sample is very heterogeneous. Heavy metals are mostly highly correlated with total and amorphous Fe. High correlation was found between the pH-related parameters, Fe t −Fe am , Fe−Mn, Fe−Ni, Fe−Co, Co−Ni, Co−Mn, and Pb−Cr (negative). Multivariate statistical analysis distinguished three subgroups: (1) Fe t , Fe am , Ni, Co, and Mn; (2) Pb, Zn, and Cr; and (3) Cu and V, suggesting a possible common source and similar behavior. Although clays are much more present in the samples, heavy metals are mostly connected to iron oxyhydroxides.