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A sample of Sb-rich segnitite from the Black Pine mine, Montana, U.S.A., has been studied by microprobe analyses, single-crystal X-ray diffraction, and μ-EXAFS and XANES spectroscopy. Linear combination fitting of the spectroscopic data provided Sb 5+ :Sb 3+  = 85(2):15(2), where Sb 5+  is in octahedral coordination substituting for Fe 3+  and Sb 3+  is in tetrahedral coordination substituting for As5+. Based upon this Sb 5+ :Sb 3+  ratio, the microprobe analyses yielded the empirical formula Pb 1.02  H 1.02 (Fe 3+  2.36 Sb 5+  0.41 Cu 2+  0.27 ) Σ3.04 (As 5+  1.78 Sb 3+  0.07 S 6+  0.02 ) Σ1.88 O 8 (OH) 6.00 . The crystal structure refinement and bond valence analysis are consistent with these cation site assignments. The formation of Sb-rich segnitite opens new possibilities for Sb sinks within the supergene zone. Segnitite may, in fact, be an ideal host for the sequestering of several toxic elements for pH &lt; 2. At higher pH values, As is more likely to be incorporated into schwertmannite and ferrihydrite.

Sb 5+ and Sb 3+ substitution in segnitite: A new sink for As and Sb in the environment and implications for acid mine drainage