Journal of Geophysical Research Solid Earth Supporting Information for Experimental constraints on the role of dynamic recrystallization on resetting the Ti-inquartz thermobarometer Nachlas, W.O.1, Hirth, G.2 1 Department 2 Department of Earth Sciences, University of Minnesota, Minneapolis, MN 55455 of Earth, Environmental and Planetary Sciences, Brown University, Providence, RI 02912 Contents of this file Figures S1 to S5 Table S1 Movie S1 Introduction This document contains information that supplements major concepts in the article but is not vital to the body of text and therefore is not necessary to be included as additional figures. This includes further elaboration on analytical methods, additional observations on accessory phase minerals, and processing/refining of analytical results. A supplementary movie shows results of X-ray tomography used to penetrate the solid-salt confining medium to image the deformed sample prior to dissection of the assembly. 1 Figure S1. Secondary electron images show results of analysis of Ti concentration (ppm Ti) from the grain boundary of a single crystal of quartz from the undoped layer of a low strain experiment (W1674), revealing the same concentrations as the population of measurements collected from thin section analysis (see Table 2, Table S1). This observation supports the interpretation that secondary fluorescence is not a major source of contamination for the majority of electron probe measurements. 2 Figure S2. Full CL spectrum collected from doped quartz showing luminosity in the blue region, suggesting that the CL signal is dominated by Ti substitution in quartz (e.g., Gotze et al. [2001]; Muller et al. [2003]). 3 Figure S3. Plane-polarized light micrographs of nodular rutile inclusions present in the doped layer of experimental aggregates from hydrostatic (A-B) and high strain deformed samples (C). 4 Figure S4. Cathodoluminescence intensity halos surrounding rutile needles from hydrostatic (A), low strain (B), intermediate strain (C), and high strain (D) samples. Rutile needles emit highintensity CL enrichment halos, which are interpreted to reflect Ti diffusion from rutile needles into quartz. CL halos are observed to be smoother and wider in high-strain (longer-duration) experiments. 5 Figure S5. Plots showing one representative transect (out of three) of EMP measurements collected across the aggregate layering (points were set with equidistant spacing in all samples except hydrostatic samples, where points were set manually to avoid porosity). Results reveal two compositionally-distinct populations of Ti-in-quartz concentrations in the doped (blue symbols) and undoped (red symbols) layers. Despite changes in the value of concentrations between hydrostatic (A), low strain (B), intermediate strain (C), and high strain (D) samples, the relative difference between quartz in the doped and undoped layer remains consistent: Ti-in-quartz concentrations in the undoped layer are ~50% of the concentrations in the undoped layer, leading us to infer aTiO2 ~ 0.5 for quartz growth in the undoped layer (see Figure 8 and Section 5.1 for further discussion). 6 Sam ple nam e USGS BIR-1 USGS BIR-1 USGS BIR-1 MEAN (atom ic) MEAN (w t% oxide) Recommended values* % error Al 8.332 8.289 8.321 8.314 15.709 Ba Ca 0.001 9.566 0.001 9.460 0.001 9.512 0.001 9.513 0.001 13.310 Fe 8.067 7.978 8.039 8.028 10.328 K 0.013 0.016 0.015 0.015 0.018 Mg 5.871 5.759 5.860 5.830 9.667 Mn 0.139 0.138 0.139 0.139 0.179 Na 1.388 1.381 1.400 1.390 1.873 P 0.010 0.009 0.010 0.009 0.022 Si 22.498 22.569 22.340 22.469 48.068 Sr 0.011 0.011 0.011 0.011 0.013 Ti 0.590 0.589 0.587 0.589 0.982 Zr 0.002 0.002 0.002 0.002 0.002 15.5 -1.3 --- 13.3 -0.1 11.30 8.6 0.030 40.3 9.70 0.3 0.175 -2.2 1.820 -2.9 0.021 -3.1 47.96 -0.2 --- 0.96 -2.3 --- USGS RGM-1 USGS RGM-1 USGS RGM-1 MEAN (atom ic) MEAN (w t% oxide) Recommended values* % error 7.203 7.198 7.212 7.204 13.612 0.082 0.082 0.083 0.082 0.092 0.860 0.885 0.896 0.880 1.232 1.286 1.295 1.291 1.291 1.661 3.631 3.656 3.686 3.658 4.406 0.180 0.205 0.182 0.189 0.313 0.028 0.029 0.029 0.029 0.037 3.038 3.036 3.086 3.053 4.116 0.019 0.018 0.018 0.018 0.042 34.080 34.161 33.712 33.984 72.703 0.011 0.011 0.010 0.011 0.013 0.158 0.158 0.159 0.159 0.264 0.021 0.021 0.021 0.021 0.028 13.7 0.6 --- 1.15 -7.1 1.86 10.7 4.30 -2.5 0.28 -11.9 0.036 -3.5 4.07 -1.1 --- 73.4 0.9 --- 0.27 2.1 --- *as reported by w w w .crustal.usgs.gov Table S1. ICP-OES analysis of USGS geochemical reference materials BIR-1 and RGM-1. 7 doped layer all data unfiltered W1674 mean total n= st.dev 209 n= st.err W1678 mean total n= st.dev 150 n= st.err W1680 mean total n= st.dev 175 n= st.err W1696 mean total n= st.dev 209 n= st.err W1698 mean total n= st.dev 160 n= st.err W1699 mean total n= st.dev 152 n= st.err W1700 mean total n= st.dev 175 n= st.err W1701 mean total n= st.dev 150 n= st.err undoped layer filtered (less than 400 ppm) outliers removed all data unfiltered filtered (less than 300 ppm) outliers removed 523 1356 116 126 230 45 93 5 230 34 88 4 135 22 93 2 135 22 93 2 134 19 88 2 3987 20381 74 2369 127 54 64 7 117 29 61 4 349 2312 76 265 84 38 75 4 76 14 72 2 3807 21560 85 2338 224 61 64 8 211 42 59 6 171 314 90 33 132 32 87 3 130 29 86 3 1541 5316 84 580 138 65 67 8 123 41 62 5 116 223 125 20 85 34 120 3 79 19 114 2 5869 34973 91 3666 161 97 77 11 140 56 72 7 434 1768 69 213 67 24 64 3 63 14 61 2 4208 24546 81 2727 196 39 69 5 191 33 65 4 236 779 71 92 112 38 66 5 106 29 63 4 559 1576 84 172 160 61 69 7 146 36 64 4 145 420 91 44 68 36 87 4 60 23 81 3 766 3391 65 421 163 36 58 5 157 25 55 3 108 197 85 21 87 36 84 4 83 18 74 2 Table S1. Compiled EMP measurements from the doped and undoped layers of the aggregate showing the data processing steps for removing contaminated measurements and outliers. Final values for each sample listed in Table 2. 8 Movie S1. X-ray tomography (XRCT) was used to penetrate the solid-salt confining medium to image the distance between the thermocouple and jacketed sample surface within a deformed sample assembly following a high-strain deformation experiment (W1701). Radiographs from this analysis are included in Figure 2. 9