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Olenitic tourmaline with high amounts of tetrahedral B (up to 2.53  [4] B pfu) has been synthesized in a piston-cylinder press at 4.0 GPa, 700 °C, and a run duration of 9 days. Crystals are large enough (up to 30 × 150 μm) to allow for reliable and spatially resolved quantification of B by electron microprobe analysis (EMPA), single-crystal X-ray diffraction, and polarized single-crystal Raman spectroscopy. Tourmalines with radial acicular habit are zoned in  [4] B-concentration [core: 2.53(25)  [4] B pfu; rim: 1.43(15)  [4] B pfu], whereas columnar crystals are chemically homogeneous [1.18(15)  [4] B pfu]. An amount of 1.4(1)  [4] B pfu was found in the columnar tourmaline by single-crystal structure refinement (SREF) ( R  = 1.94%). The EMPA identify  [T] Si −1  [V,W] O −1  [T] B 1  [V,W] (OH) 1  as the main and [X]⃞ -1  [T] Si –1  [X] Na 1  [T] B 1  as minor exchange vectors for  [4] B-incorporation, which is supported by the SREF. Due to the restricted and well-defined variations in chemistry, Raman bands in the OH-stretching region (3000–3800 cm −1 ) are unambiguously assigned to a specific cation arrangement. We found the sum of the relative integrated intensity ( I  rel ) of two low-frequency bands at 3284–3301 cm −1  (ν1) and 3367–3390 cm −1  (ν2) to positively correlate with the  [4] B concentrations:  [4] B [pfu] = 0.03(1) × [ I  rel  (ν1) +  I  rel  (ν2)]. Hence, those bands correspond to configurations with mixed Si/B occupancy at the T site. Our semi-quantitative correlation also holds for well-characterized natural  [4] B-bearing tourmaline from the Koralpe, Austria. This work shows the potential for Raman spectroscopy as a non-destructive method for the chemical classification of (precious) natural tourmaline, and as a tool to rapidly characterize chemical zonation of tourmalines in thin section.

Tetrahedral boron in natural and synthetic HP/UHP tourmaline: Evidence from Raman spectroscopy, EMPA, and single-crystal XRD