<table><caption>Table T4 (continued). (Continued on next page.)</caption><thead><tr><th>Diatom zonation<br>(Scherer et al., 2007)</th><th></th><th>Diatom bioevent</th><th>GTS2012<br>age (Ma)</th><th>Age reference</th></tr></thead><tbody><tr><td rowspan="14">Cestodiscus peplum</td><td rowspan="10">B</td><td>B Actinocyclus ellipticus var. spiralis</td><td>14.03</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>T Coscinodiscus blysmos</td><td>14.33</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>B Thalassiosira tappanae</td><td>14.40</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>T Actinopychus splendens</td><td>14.52</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Goniothecium decoratum</td><td>14.52</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Cavitatus miocenicus</td><td>14.63</td><td>Lazarus et al., 2014; Cody et al., 2008</td></tr><tr><td>T Crucidentica paranicobarica</td><td>14.79</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>B Thalassiosira perispinosa</td><td>14.89</td><td>Lazarus et al., 2014; Tanimura, 1996</td></tr><tr><td>T1 Anellinus californicus</td><td>14.90</td><td>Burckle, 1978</td></tr><tr><td>B Crucidentica nicobarica</td><td>15.10</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>T Cavitatus lanceolatus</td><td>15.20</td><td>Lazarus et al., 2014; Yanagisawa and Akiba, 1998</td></tr><tr><td>T Cymatogonia amblyoceras</td><td>15.20</td><td>Lazarus et al., 2014; Barron et al, 2013</td></tr><tr><td>T Azpeitia praenodulifera</td><td>15.40</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>T Goniothecium odontella</td><td>15.50</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>B Azpeitia endoi</td><td>15.50</td><td>Lazarus et al., 2014; Barron, 1976</td></tr><tr><td>T Cavitatus rectus</td><td>~15.50</td><td>Lazarus et al., 2014; Fenner, 1985</td></tr><tr><td rowspan="10">A</td><td>B Cavitatus lanceolatus</td><td>15.60</td><td>Lazarus et al., 2014; Yanagisawa and Akiba, 1998</td></tr><tr><td>T Coscinodiscus lewisianus var. similis</td><td>15.70</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>B Crucidentica paranicobarica</td><td>16.00</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>T Crucidentica sawamurae</td><td>16.20</td><td>Lazarus et al., 2014; Yanagisawa and Akiba, 1990</td></tr><tr><td>T Thalassiosira fraga</td><td>16.30</td><td>Lazarus et al., 2014; Barron, 1985</td></tr><tr><td>B Cestodiscus peplum</td><td>16.40</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>T Cestodiscus kugleri</td><td>16.50</td><td>Lazarus et al., 2014; Barron, 2005</td></tr><tr><td>T Cestodiscus ovalis</td><td>16.50</td><td>Lazarus et al., 2014; Barron, 2005</td></tr><tr><td>T Cestodiscus pulchellus</td><td>16.50</td><td>Lazarus et al., 2014; Barron, 2005</td></tr><tr><td>T Crucidentica kanayae</td><td>16.50</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>T Raphidodiscus (Rhaphidodiscus)<br>marylandicus (marylandica)</td><td>16.50</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td rowspan="14">Crucidentica nicobarica</td><td rowspan="10">B</td><td>B Azpeitia vetustissima</td><td>16.50</td><td>Lazarus et al., 2014; Baldauf and Barron, 1982</td></tr><tr><td>B Azpeitia vetustissima var. voluta</td><td>16.50</td><td>Lazarus et al., 2014; Baldauf and Barron, 1982</td></tr><tr><td>B Crucidentica kanayae</td><td>16.90</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>T Cestodiscus rapax</td><td>17.10</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Coscinodiscus lewisianus var. similis</td><td>17.10</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>T Coscinodiscus lewisianus var. robustus</td><td>17.30</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Coscinodiscus rhombicus</td><td>17.30</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Coscinodiscus blysmos</td><td>17.30</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Azpeitia bukryi</td><td>17.40</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Crucidentica ikebei</td><td>17.40</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Azpeitia salisburyana</td><td>17.40</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Triceratium pileus</td><td>17.60</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td rowspan="10">A</td><td>B Anellinus californicus</td><td>17.60</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Craspedodiscus coscinodiscus</td><td>17.60</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Crucidentica ikebei</td><td>17.70</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Bogorovia puncticulata</td><td>18.10</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>B Crucidentica sawamurae</td><td>18.20</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>B Cestodiscus kugleri</td><td>18.40</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Thalassiosira praefraga</td><td>18.60</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Actinocyclus barronii</td><td>18.70</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Actinocyclus jouseae</td><td>18.70</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Actinocyclus radionovae</td><td>18.70</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td rowspan="10">Triceratium pileus</td><td>B Cestodiscus pulchellus var. maculata</td><td>18.70</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>B Cestodiscus rapax</td><td>18.90</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Triceratium pileus</td><td>18.90</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Craspedodiscus barronii</td><td>19.10</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Craspedodiscus elegans</td><td>19.10</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Dimeregramma (Dimerogramma) fossile</td><td>19.20</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>B Cestodiscus ovalis</td><td>19.20</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Actinocyclus barronii</td><td>19.40</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Azpeitia gombosii</td><td>19.50</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Coscinodiscus lewisianus var. robustus</td><td>19.50</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Actinocyclus praellipticus</td><td>19.60</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td rowspan="10">Craspedodiscus elegans</td><td>T Cestodiscus japonicus</td><td>19.60</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Distephanosira architecturalis</td><td>19.60</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Actinocyclus jouseae</td><td>19.60</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Actinocyclus hajosiae</td><td>19.80</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Rossiella fennerae</td><td>19.90</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Bogorovia veniamini</td><td>20.00</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Thalassiosira fraga</td><td>20.40</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Azpeitia oligocenica</td><td>20.50</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>Rossiella paleacea</td><td>C</td><td></td><td></td><td></td></tr></tbody></table>
<table><caption>Table T4 (continued). (Continued on next page.)</caption><thead><tr><th>Diatom zonation<br>(Scherer et al., 2007)</th><th></th><th>Diatom bioevent</th><th>GTS2012<br>age (Ma)</th><th>Age reference</th></tr></thead><tbody><tr><td rowspan="20">Rossiella paleacea</td><td rowspan="10">B</td><td>B Rhizosolenia alata</td><td>20.50</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Actinocyclus mutabilis</td><td>20.60</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Craspedodiscus barronii</td><td>20.60</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Craspedodiscus elegans</td><td>20.60</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Cestodiscus trochus</td><td>20.80</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Bogorovia puncticulata</td><td>20.80</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>B Actinocyclus praellipticus</td><td>20.90</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Cestodiscus pulchellus</td><td>20.90</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Rossiella paleacea</td><td>20.90</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>T Pseudopyxilla russica (rossica)</td><td>21.10</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>B Cymatogonia amblyoceras</td><td>21.10</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>B Dimeregramma (Dimerogramma) fossile</td><td>21.10</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Bogorovia barronii</td><td>21.20</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Actinocyclus radionovae</td><td>21.20</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Rossiella symmetrica</td><td>21.40</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Actinocyclus hajosiae</td><td>21.40</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Thalassiosira primalabiata</td><td>21.40</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td rowspan="10">A</td><td>B Actinocyclus mutabilis</td><td>21.40</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Actinocyclus nigriniae</td><td>21.50</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Stephanopyxis marginata</td><td>21.60</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Cestodiscus umbonatus</td><td>21.70</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Rossiella fourtanierae</td><td>21.70</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Cestodiscus japonicus</td><td>21.70</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Azpeitia praenodulifera</td><td>21.80</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>T Bogorovia gombosii</td><td>21.90</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Actinocyclus nigriniae</td><td>21.90</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Thalassiosira praefraga</td><td>21.90</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Bogorovia barronii</td><td>22.20</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td rowspan="10">B</td><td>B Rossiella symmetrica</td><td>22.31</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Thalassiosira leptopus</td><td>22.31</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>B Rossiella fourtanierae</td><td>23.00</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Bogorovia gombosii</td><td>23.26</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Coscinodiscus lewisianus var. rhomboides</td><td>23.32</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Rocella schraderi</td><td>23.32</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Rocella gelida</td><td>23.42</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Azpeitia tabularis</td><td>23.42</td><td>Lazarus et al., 2014; Barron, 2003</td></tr><tr><td>B Azpeitia gombosii</td><td>23.52</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>T Cestodiscus stokesianus</td><td>23.62</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>B Raphidodiscus (Rhaphidodiscus)<br>marylandicus (marylandica)</td><td>23.82</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td rowspan="10">Rocella gelida</td><td>T Rocella vigilans</td><td>23.92</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Rocella princeps</td><td>24.00</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Cestodiscus umbonatus</td><td>24.24</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Rocella schraderi</td><td>24.24</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Thalassiosira primalabiata</td><td>24.87</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Cestodiscus parmula</td><td>25.05</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>B Coscinodiscus lewisianus var. rhomboides</td><td>25.11</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Rocella gelida</td><td>25.31</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Rocella princeps</td><td>25.42</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Rossiella fennerae</td><td>25.73</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Coscinodiscus lewisianus</td><td>26.59</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Coscinodiscus lewisianus var. levis</td><td>26.68</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td rowspan="10">Bogorovia veniamini</td><td>T Kozloviella minor</td><td>27.23</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Goniothecium decoratum</td><td>27.53</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Kozloviella pacifica</td><td>27.76</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Rocella vigilans var. 1</td><td>27.76</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Bogorovia veniamini</td><td>27.76</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Coscinodiscus lewisianus var. levis</td><td>27.76</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Baxteriopsis brunii</td><td>27.91</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Kozloviella pacifica</td><td>28.04</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Cavitatus rectus</td><td>28.12</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Coscinodiscus rhombicus</td><td>28.20</td><td>Lazarus et al., 2014; Barron, 2006</td></tr><tr><td>B Cavitatus jouseana</td><td>28.27</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td rowspan="10">Rocella vigilans</td><td>B Kozloviella minor</td><td>28.27</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Rocella vigilans var. 1</td><td>28.51</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Hemiaulus lyriformis</td><td>28.63</td><td>Barron, pers. comm., 2017</td></tr><tr><td>T Rocella semigelida</td><td>28.63</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Rocella semigelida</td><td>28.75</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Hemiaulus polycistinorum var. mesolepta</td><td>29.44</td><td>Lazarus et al., 2014; Scherer et al., 2000</td></tr><tr><td>B Rocella vigilans</td><td>29.58</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr></tbody></table>
<table><caption>Table T4 (continued).</caption><thead><tr><th>Diatom zonation<br>(Scherer et al., 2007)</th><th>Diatom bioevent</th><th>GTS2012<br>age (Ma)</th><th>Age reference</th></tr></thead><tbody><tr><td rowspan="24">Cestodiscus reticulatus</td><td>T Hemiaulus subacutus</td><td>29.83</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Hemiaulus exiguus</td><td>29.95</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Cestodiscus demergitus</td><td>30.55</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Rocella praenitida</td><td>30.55</td><td>Lazarus et al., 2014; Scherer and Koç, 1996</td></tr><tr><td>B Azpeitia bukryi</td><td>30.75</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Cestodiscus robustus</td><td>30.84</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Pyxilla reticulata</td><td>30.84</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Hemiaulus barbadensis</td><td>30.93</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Skeletonemopsis barbadense</td><td>30.93</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Hemiaulus altar</td><td>31.02</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Cestodiscus convexus</td><td>31.12</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Coscinodiscus excavatus</td><td>31.12</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Rouxia hannae</td><td>31.12</td><td>Barron, pers. comm., 2017</td></tr><tr><td>B Cavitatus miocenicus</td><td>31.12</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Thalassionema nitzschioides</td><td>31.12</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Coscinodiscus excavatus var. semilunaris</td><td>31.71</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Asterolampra insignis</td><td>32.01</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Coscinodiscus bulliens</td><td>32.10</td><td>Lazarus et al., 2014; Gombos, 1982</td></tr><tr><td>T Pterotheca aculeifera (aculifera)</td><td>32.10</td><td>Lazarus et al., 2014; Hajos, 1976</td></tr><tr><td>B Rouxia hannae</td><td>32.10</td><td>Barron, pers. comm., 2017</td></tr><tr><td>T Trinacria subcapitata</td><td>32.30</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Cestodiscus reticulatus</td><td>32.40</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Coscinodiscus hajosiae</td><td>32.40</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Hemiaulus hostilis</td><td>32.40</td><td>Lazarus et al., 2014; Fenner, 1994</td></tr><tr><td>B Coscinodiscus excavatus var. semilunaris</td><td>32.40</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Riedelia claviger</td><td>32.70</td><td>Lazarus et al., 2014; Barron et al., 2014</td></tr><tr><td>B Thalassiothrix longissima</td><td>32.70</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Cestodiscus sp. 2</td><td>32.99</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Hemiaulus dubius</td><td>33.09</td><td>Barron, pers. comm., 2017</td></tr><tr><td>B Cestodiscus reticulatus</td><td>33.31</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Rhizosolenia styliformis</td><td>33.31</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>B Cestodiscus parmula</td><td>33.55</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>B Goniothecium odontella</td><td>33.55</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Coscinodiscus decrescens</td><td>33.66</td><td>Lazarus et al., 2014; Fenner, 1978</td></tr><tr><td>B Cestodiscus robustus</td><td>33.78</td><td>Lazarus et al., 2014; Barron et al., 2014</td></tr><tr><td>B Coscinodiscus excavatus</td><td>33.78</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>T Hemiaulus gracilis</td><td>33.91</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>B Cestodiscus sp. 2</td><td>33.91</td><td>Lazarus et al., 2014; Barron et al., 2014</td></tr><tr><td>B Hemiaulus barbadensis</td><td>33.91</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Cestodiscus fennerae</td><td>34.09</td><td>Lazarus et al., 2014; Barron et al., 2014</td></tr><tr><td>B Cestodiscus trochus</td><td>34.15</td><td>Lazarus et al., 2014; Barron et al., 2014</td></tr><tr><td>T Kozloviella subrotunda</td><td>34.28</td><td>Lazarus et al., 2014; Scherer et al., 2007</td></tr><tr><td>B Rocella praenitida</td><td>34.28</td><td>Lazarus et al., 2014; Scherer and Koç, 1996</td></tr><tr><td>B Azpeitia oligocenica</td><td>34.53</td><td>Lazarus et al., 2014; Barron et al., 2014</td></tr><tr><td>B Cestodiscus convexus</td><td>34.53</td><td>Lazarus et al., 2014; Barron et al., 2014</td></tr><tr><td>B Cestodiscus demergitus</td><td>34.53</td><td>Lazarus et al., 2014; Barron et al., 2014</td></tr><tr><td>B Hemiaulus gracilis</td><td>34.53</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>B Trinacria subcapitata</td><td>34.53</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>B Baxteriopsis brunii</td><td>34.65</td><td>Lazarus et al., 2014; Scherer et al., 2007</td></tr><tr><td>T Cestodiscus pulchellus var. novazealandica</td><td>34.90</td><td>Lazarus et al., 2014; Barron et al., 2014</td></tr><tr><td>B Cestodiscus stokesianus</td><td>35.13</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>T Azpeitia tuberculata</td><td>35.70</td><td>Lazarus et al., 2014; Barron et al., 2014</td></tr><tr><td>B Actinocyclus octonarius</td><td>>36.39</td><td>Lazarus et al., 2014; Hajós, 1976</td></tr><tr><td>B Triceratium acutangulum</td><td>>36.39</td><td>Lazarus et al., 2014; Edwards, 1991</td></tr><tr><td>B Triceratium condecorum</td><td>>36.39</td><td>Lazarus et al., 2014; Edwards, 1991</td></tr><tr><td>T Hemiaulus grassus</td><td>36.39</td><td>Lazarus et al., 2014; Scherer et al., 2007</td></tr><tr><td>B Cestodiscus fennerae</td><td>36.84</td><td>Lazarus et al., 2014; Barron et al., 2014</td></tr><tr><td>T Hemiaulus gondolaformis</td><td>37.28</td><td>Lazarus et al., 2014; Scherer et al., 2007</td></tr><tr><td>B Hemiaulus altar</td><td>37.39</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>B Macrora stella (Azpeitia)</td><td>37.39</td><td>Lazarus et al., 2014; Cervato and Burckle, 2003</td></tr><tr><td>B Skeletonemopsis barbadense</td><td>37.39</td><td>Lazarus et al., 2014; Barron et al., 2004</td></tr><tr><td>B Cestodiscus pulchellus var. novazealandica</td><td>>38.36</td><td>Lazarus et al., 2014; Barron et al., 2014</td></tr><tr><td>T Triceratium kanayae</td><td><40.08</td><td>Lazarus et al., 2014; Scherer et al., 2007</td></tr><tr><td>B Asterolampra marylandica</td><td>40.08</td><td>Lazarus et al., 2014; Scherer et al., 2007</td></tr></tbody></table>

<caption>Table T5. Taxonomic list of relevant diatom species, Expeditions 367 and 368. Download table in CSV format.</caption>
# Paleomagnetism

Shipboard paleomagnetic investigations were conducted on both the archive and working halves of cores recovered during Expeditions 367 and 368. The primary objectives were to determine directions of natural remanent magnetization (NRM) components, including magnetic polarity, and downhole variation of magnetic properties.

Shipboard paleomagnetic investigations combined three complementary approaches: (1) measurement and in-line alternating field (AF) demagnetization of archive-half sections on the pass-through 2G Enterprises (model 760R-4K) superconducting rock magnetometer (SRM), (2) measurement and thermal demagnetization of oriented discrete samples on the SRM, and (3) measurement and AF demagnetization of oriented discrete samples on the spin-ner magnetometer (AGICO model JR6). Additionally, the anisotropy of magnetic susceptibility (AMS) was measured on discrete samples with the AGICO KLY 4 Kappabridge.

Discrete cube samples were collected from the central part of working-half sections to reduce the effect of drilling disturbance. The discrete sampling strategy was modified depending upon lithology (sediments versus basement), type of drilling used (e.g., soft sediments can be disturbed by RCB coring to the point of not being usable for magnetic inclination), and recovery rate. For basement rocks, at least one cube was collected per major lithologic unit (as defined by petrologists) to characterize the magnetic response of major units, different grain-size distributions, and deformation. These data were to be used by shipboard paleomagnetists to construct the magnetostratigraphy and by structural geologists to orient cores. Due to the low recovery in basement (<20%), samples were shared with the petrophysics team to measure porosity and moisture during Expedition 367 and until Hole U1501D of Expedition 368. The sample sharing significantly slowed down data acquisition for both teams (old protocol in Table T6). Furthermore, heating samples to 105°C in a magnetically unshielded oven imparts an undesirable artificial magnetization on samples. The only way to remove this artificial magnetization is to thermally demagnetize the sample to 250°/350°C, which results in the loss of all demagnetization steps between 95° and 350°C. Considering that a cube is not necessary to perform a density and porosity measurement, a new protocol was suggested that includes the use of residuals (Table T6). Moreover, for shared samples (cubes of hard rock) we proposed to use the magnetically shielded oven (ASC Scientific model TD-48SC), which can accommodate up to 48 samples at a time. Both teams agreed to follow this protocol and to apply it for the rest of Expedition 368.

Previous paleomagnetic studies documented a coring-induced, isothermal remanent magnetization (IRM) imparted on the core (e.g., Pinto and McWilliams, 1990; Fuller et al., 1998; de Wall and Worm, 2001).

Both section-half and discrete data, collected on the pass-through SRM and spinner magnetometer, respectively, were uploaded to the LIMS database. We then analyzed the stepwise demagnetization data of the discrete samples by principal component analysis (PCA) to define the characteristic remanent magnetization (ChRM) (Kirschvink, 1980). Data visualization (Zijderveld demagnetization plots and equal area projections) and PCA were conducted using the PuffinPlot software (version 1.03, 23 April 2015) (Lurcock and Wilson, 2012).

## Magnetic measurements on archive-half sections

The remanent magnetization of archive-half sections was measured using a pass-through SRM equipped with direct-current superconducting quantum interference devices (SQUIDs) and an in-line, automated three-axis AF demagnetizer capable of reaching a peak field of 80 mT.

Measurement of archive halves was conducted using the SRM software (IMS-SRM version 9.2) assuming a sample area of 17.5 cm² for conversion to volume-normalized magnetization units (A/m). The interval between NRM measurement points was typically at 2.5 to 5 cm spacing for sedimentary material (depending on the expected sedimentation rate) and 2.0 cm for igneous rocks at the speed of 10 cm/s. The response functions of the pick-up coils of the SQUID sensors have a full width of 7.25–8.8 cm at half height. Therefore, data collected within ~4 cm of piece boundaries (or voids) can be significantly affected by edge effects and have to be treated with caution.

We performed successive AF demagnetizations using the SRM in-line AF demagnetizer on all split-core archive sections. The in-line AF demagnetizer applies a field to the x-, y-, and z-axes of the SRM in this fixed order (Figure F23A, F23D). Previous reports suggest that higher AF demagnetization fields have produced significant anhysteretic remanent magnetization (ARM) along the z-axis of the SRM (e.g., Harris et al., 2013b). Considering this limitation, we only used demagnetization steps up to 25 mT to demagnetize the sections. Depending on time constraints imposed by the rate of core recovery, for most of the sediment sections we performed 3–6 steps from NRM up to 15 or 25 mT. For basement rocks during Expedition 367, we adopted a set of narrower AF steps of 2 mT from NRM to 10 mT and steps of 5 mT from 10 to 25 mT. For Hole U1505C (starting from Section 3H-2) and for Holes U1504A, U1504B, and U1505C, only NRM was measured. This decision was

<table><caption>Table T6. Sampling protocols, Expeditions 367 and 368. Download table in CSV format.</caption><thead><tr><th>Sample type</th><th>Team</th><th>Treatment</th><th>Time</th></tr></thead><tbody><tr><td colspan="4">Old protocol</td></tr><tr><td>CUBE</td><td>Petrophysics</td><td>P-wave velocity on dry sample</td><td>10 min</td></tr><tr><td>CUBE</td><td>Paleomagnetism</td><td>NRM and AMS at room temperature and after heating at 95°C</td><td>3 h</td></tr><tr><td>CUBE</td><td>Petrophysics</td><td>Moisturized to prepare for density and porosity measured</td><td>24–48 h or more</td></tr><tr><td>CUBE</td><td>Petrophysics</td><td>Measure P-wave velocity on wet sample</td><td>10 min</td></tr><tr><td>CUBE</td><td>Petrophysics</td><td>Heated at 105°C</td><td>24 h</td></tr><tr><td>CUBE</td><td>Petrophysics</td><td>Measured for density and porosity</td><td>30 min/sample</td></tr><tr><td>CUBE</td><td>Paleomagnetism</td><td>Complete thermal demagnetization process</td><td>48 h</td></tr><tr><td colspan="4">New protocol</td></tr><tr><td>CUBE</td><td>Petrophysics</td><td>P-wave velocity on dry/wet sample</td><td>24 h</td></tr><tr><td>CUBE</td><td>Paleomagnetism</td><td>Complete thermal demagnetization process</td><td>48 h</td></tr><tr><td>Residuals</td><td>Petrophysics</td><td>Complete density and porosity treatment</td><td>48–52 h or more</td></tr></tbody></table>
<figure><img src="image_67.png" /><figcaption>Figure F23. A. IODP coordinates of paleomagnetic samples (after Richter et al., 2007). B. Natsuhara-Giken sampling cubes (7 cm³ volume) with sample coordinate system. Red hatched arrow is parallel to up arrow on sample cube and points in -z-direction. C. Measurement positions in JR-6A spinner magnetometer. D. Coordinate system used for the SRM on board the JOIDES Resolution.</figcaption></figure>

made after a comparison of magnetization intensities between discrete samples and sections led us to suspect that the SRM was not properly calibrated (geometrically) for core sections. AF demagnetization results were plotted individually as vector plots (Zijderveld, 1967) and as downhole variations with depth. We inspected the plots visually to evaluate whether the remanence after demagnetization at the highest AF step reflects the ChRM and geomagnetic polarity sequence.

Low-field magnetic susceptibility (κ), measured on whole-round core sections using the WRMSL and archive-half core sections using the SHMSL (see Physical properties), was used to assess the concentration of magnetic minerals and to determine the downhole relative paleointensity (NRM/κ). These whole-round records of magnetic susceptibility were compared to visual features in the split cores to flag possible artifacts.

## Magnetic measurements on discrete samples

Discrete samples were initially measured on both the SRM and a spinner magnetometer. These samples were subjected to AF demagnetization treatments using both the 2G in-line AF demagnetizer (as described above) and the DTECH (model D-2000) AF demagnetizer. But the resultant demagnetization behavior of the discrete samples becomes noisy at higher AF treatments, and thus measurement on the SRM is not recommended for discrete samples. This recommendation is also confirmed by shipboard tests of the reliability of discrete measurements on the 2G SRM. The routine AF demagnetization treatment was performed using the DTECH (model D-2000) AF demagnetizer. In addition, to avoid contamination by the ambient magnetic field during shipboard measurements, two cylindrical mu-metal shields provided a suitable low-field environment for temporary sample storage.

Oriented discrete samples were taken preferentially in fine-grained intervals where drilling deformation was minimal. In soft sediment, discrete samples were taken in plastic "Japanese" Natsuhara-Giken sampling cubes (7 cm³ sample volume; Figure F23B). Cubes were pushed into the working half of the core with the "up" arrow on the cube pointing upsection in the core. In lithified sedi-

ments and hard rocks, 2 cm cubes (8 cm³ sample volume) were cut with the parallel saw.

Incremental AF demagnetization of discrete samples was performed with the DTECH AF demagnetizer (model D-2000) at fields up to 45 or 50 mT for lower coercivity samples and 120 or 200 mT for high-coercivity samples. We also applied progressive thermal demagnetization using a thermal specimen demagnetizer (ASC Scientific model TD-48SC) up to 700°C at steps of 25° to 50°C depending on the magnetic minerals present in the sample. During Expedition 367, a combination of stepwise AF and thermal demagnetization was applied.

AMS was measured on an AGICO KLY 4S Kappabridge instrument at a field of 300 A/m using the AMSSpin LabVIEW program designed by Gee et al. (2008) or the SUFAR (AGICO) program. The KLY 4S Kappabridge measures AMS by rotating the sample along three axes, stacking the data, and calculating the best-fit second-order tensor. It also measures the volume-normalized calibrated bulk susceptibility (χ).

## Coordinates

All magnetic data are reported relative to the IODP orientation conventions: +x is into the face of the working half, +y points toward the left side of the face of the working half, and +z points downsection. The relationship of the SRM coordinates (X-, Y-, and Z-axes) to the data coordinates (x-, y-, and z-directions) is as follows: for archive halves, x-direction = X-axis, y-direction = -Y-axis, and z-direction = Z-axis; for working halves, x-direction = -X-axis, y-direction = Y-axis, and z-direction = Z-axis (Figure F23). The coordinate systems for the spinner magnetometer and Natsuhara-Giken sampling cubes are also shown in Figure F23.

## Core orientation

Paleomagnetic study of marine sediment cores is greatly enhanced if the angle between magnetic north and the double line marked on the core liner can be determined. Core orientation of APC cores was achieved with the orientation tool (Icefield MI-5 core orientation tool) mounted on the core barrel. The Icefield MI-5
core orientation tool consists of triaxial magnetometers and accelerometers. These sensors provide an azimuthal correction for the core barrel that, combined with the local magnetic declinations, allows the measured NRM declinations to be transformed into true geographic coordinates. In the orientation deployment, the tool is connected to the core barrel with the double lines on the core liner at a fixed and known angle relative to its sensors. Previous expeditions have reported that in general these orientation tools have an accuracy of 20°–30°. Unlike earlier expeditions that reported reversed directions (i.e., 180° instead of 0°) during a period of normal polarity, the declinations (above ~160 m from the APC cores) corrected based on the Icefield data are consistent with the inclinations.

The ChRMs can also provide a reference frame to orient cores (see Structural geology). Provided that the reference magnetic pole is known, the orientation of the paleomagnetic vector is then used to restore the azimuth of the +x core axis (e.g., Fuller, 1969).

## Magnetostratigraphy reference scale and interpretations

The magnetostratigraphy at each site was constructed by correlating observed polarity sequences with a reference GPTS in combination with biostratigraphic biohorizons. The GPTS used for Expeditions 367 and 368 (Table T7) is the GPTS2016 synthesis of astronomical tuning of Cenozoic through latest Cretaceous polarity zones updated in Ogg et al. (2016). The Cenozoic portion of GPTS2016, together with microfossil and nannofossil biozones, is plotted in Figure F24.

For azimuthally unoriented samples from sedimentary rocks that formed at low latitudes, such as those at the Expedition 367 and 368 drill sites, determining the polarity of sedimentary units can be difficult. The polarity ambiguity arises when the samples are azi-

muthally unoriented and the inclination is very shallow near the Equator (the angular distance between reversed and normal polarity inclinations is small). Because paleomagnetic inclinations from any samples will have some degree of dispersion about their mean inclination, it is likely that when the mean inclination is shallow (near zero), the sign of the inclination will not be indicative of the polarity (e.g., McFadden and Reid, 1982; Cox and Gordon, 1984). The sign of the inclination of these samples should be used carefully as a definitive estimate of magnetic polarity.

We applied the following methods to establish magnetozones:

* Observing near-180° shift in declinations and significant changes in inclinations from pass-through measurements on long coherent core sections after AF demagnetization. The observed magnetozones are then checked with the ChRM directions of the discrete samples from the corresponding intervals.

* Comparison of inclination trends with predicted paleolatitudes of the drill sites according to the absolute plate motion of the South China plate on global plate circuit reconstructions (e.g., Scotese, 2014a, 2014b). However, the reconstructed position of the drill holes through the Cenozoic has negligible displacement in paleolatitude because that plate and the adjoining main Asian landmass underwent clockwise rotation.

Whenever possible, we provide an interpretation of the magnetic polarity, with the naming convention following that of comparative chron and anomaly numbers prefaced by the letter C (e.g., Ogg et al., 2016). Normal polarity subchrons are referred to by adding suffixes (n1, n2, etc.) that increase with age. For the younger part of the timescale (Pliocene–Pleistocene), we use the traditional names to refer to the various chrons and subchrons (e.g., Brunhes, Jaramillo, Olduvai, etc.). In general, polarity reversals occurring at the end of core sections have been treated with extreme caution.

<table><caption>Table T7. Geomagnetic polarity timescale used during Expeditions 367 and 368. Cenozoic and latest Cretaceous magnetic polarity chron nomenclature and age model based on astronomical tuning as used in Ogg et al. (2016). GSSP = Global Boundary Stratotype Section and Points. (Continued on next three pages.)
Download table in CSV format.</caption><thead><tr><th>Period</th><th>Epoch</th><th>Age (stage)</th><th>Base age (Ma)</th><th>Chron</th><th>Polarity chron</th><th>Age at base of chron (Ma)</th><th>Duration (My)</th><th>Remarks</th></tr></thead><tbody><tr><td rowspan="10">Quaternary</td><td rowspan="10">Pleistocene</td><td rowspan="3">late (Tarantian)</td><td>11.8 ka</td><td rowspan="3">C1</td><td>Present</td><td>0</td><td></td><td></td></tr><tr><td>0.126</td><td>C1n (Brunhes)</td><td>0.773</td><td>0.773</td><td>Base of middle Pleistocene (Ionian) is base of Brunhes Chron.</td></tr><tr><td>middle (Ionian)</td><td>0.773</td><td>C1r.1r (youngest chron within Matuyama)</td><td>1.008</td><td>0.235</td><td></td></tr><tr><td rowspan="2">early (Calabrian)</td><td rowspan="2">1.806</td><td>C1r.1n (Jaramillo)</td><td>1.076</td><td>0.068</td><td></td></tr><tr><td>C1r.2r</td><td>1.189</td><td>0.113</td><td></td></tr><tr><td rowspan="4">early (Gelasian)</td><td rowspan="4">2.588</td><td>C1r.2n (Cobb Mountain)</td><td>1.221</td><td>0.032</td><td>Cobb Mountain is within early part of Matuyama (C1r).</td></tr><tr><td>C1r.3r</td><td>1.775</td><td>0.554</td><td></td></tr><tr><td>C2n (Olduvai)</td><td>1.934</td><td>0.159</td><td>Base of Calabrian is in lower part of Olduvai.</td></tr><tr><td>C2r.1r</td><td>2.12</td><td>0.186</td><td></td></tr><tr><td rowspan="2">early (Gelasian)</td><td rowspan="2">3.6</td><td>C2r.1n (Feni)</td><td>2.155</td><td>0.035</td><td></td></tr><tr><td>C2r.2r (oldest chron within Matuyama)</td><td>2.61</td><td>0.455</td><td>Base of Pleistocene is near base of Matuyama.</td></tr><tr><td rowspan="5">Neogene</td><td rowspan="5">Pliocene</td><td rowspan="3">late (Piacenzian)</td><td rowspan="3">3.6</td><td rowspan="5">C2A</td><td>C2An.1n (youngest chron within Gauss)</td><td>3.032</td><td>0.422</td><td>"Gauss Normal Chron" (C2An) contains two reversed intervals; Kaena (2An.1r) and Mammoth (2An.2r).</td></tr><tr><td>C2An.1r (Keana)</td><td>3.116</td><td>0.084</td><td></td></tr><tr><td>C2An.2n (Gauss)</td><td>3.207</td><td>0.091</td><td></td></tr><tr><td rowspan="2">early (Zanclean)</td><td rowspan="2">5.333</td><td>C2An.2r (Mammoth)</td><td>3.33</td><td>0.123</td><td></td></tr><tr><td>C2An.3n (oldest chron within Gauss)</td><td>3.596</td><td>0.266</td><td>Base of Piacenzian is base of C2An.3n.</td></tr><tr><td></td><td></td><td></td><td></td><td></td><td>C2Ar (youngest chron within Gilbert)</td><td>4.187</td><td>0.591</td><td>"Gilbert Reversed Chron" spans C2Ar through C3r.</td></tr></tbody></table>
<table><caption>Table T7 (continued). (Continued on next page.)</caption><thead><tr><th>Period</th><th>Epoch</th><th>Age (stage)</th><th>Base age (Ma)</th><th>Chron</th><th>Polarity chron</th><th>Age at base of chron (Ma)</th><th>Duration (My)</th><th>Remarks</th></tr></thead><tbody><tr><td rowspan="14">Neogene</td><td rowspan="10">Pliocene</td><td rowspan="5">early (Zanclean)</td><td rowspan="5">5.333</td><td rowspan="5">C3</td><td>C3n.1n (Cochiti)</td><td>4.3</td><td>0.113</td><td></td></tr><tr><td>C3n.1r</td><td>4.493</td><td>0.193</td><td></td></tr><tr><td>C3n.2n (Nunivak)</td><td>4.631</td><td>0.138</td><td></td></tr><tr><td>C3n.2r</td><td>4.799</td><td>0.168</td><td></td></tr><tr><td>C3n.3n (Sidufjall)</td><td>4.896</td><td>0.097</td><td></td></tr><tr><td rowspan="2">late (Messinian)</td><td rowspan="2">7.246</td><td rowspan="2">C3A</td><td>C3n.3r</td><td>4.997</td><td>0.101</td><td></td></tr><tr><td>C3n.4n (Thvera)</td><td>5.235</td><td>0.238</td><td>Base of Pliocene is in uppermost C3r.</td></tr><tr><td rowspan="10">late (Tortonian)</td><td rowspan="10">late (Tortonian)</td><td rowspan="10">7.246</td><td rowspan="10">C3A</td><td>C3r (oldest chron within Gilbert)</td><td>6.033</td><td>0.798</td><td></td></tr><tr><td>C3An.1n</td><td>6.252</td><td>0.219</td><td></td></tr><tr><td>C3An.1r</td><td>6.436</td><td>0.184</td><td></td></tr><tr><td>C3An.2n</td><td>6.733</td><td>0.297</td><td></td></tr><tr><td>C3Ar</td><td>7.14</td><td>0.407</td><td></td></tr><tr><td>C3Bn</td><td>7.212</td><td>0.072</td><td></td></tr><tr><td>C3Br.1r</td><td>7.251</td><td>0.039</td><td>Base of Messinian is in lowermost C3Br.1r.</td></tr><tr><td>C3Br.1n</td><td>7.285</td><td>0.034</td><td></td></tr><tr><td>C3Br.2r</td><td>7.454</td><td>0.169</td><td></td></tr><tr><td>C3Br.2n</td><td>7.489</td><td>0.035</td><td></td></tr><tr><td rowspan="10">late (Tortonian)</td><td rowspan="10">late (Tortonian)</td><td rowspan="10">7.246</td><td rowspan="10">C3B</td><td>C3Br.3r</td><td>7.528</td><td>0.039</td><td></td></tr><tr><td>C4n.1n</td><td>7.642</td><td>0.114</td><td></td></tr><tr><td>C4n.1r</td><td>7.695</td><td>0.053</td><td></td></tr><tr><td>C4n.2n</td><td>8.108</td><td>0.413</td><td></td></tr><tr><td>C4r.1r</td><td>8.254</td><td>0.146</td><td></td></tr><tr><td>C4r.1n</td><td>8.3</td><td>0.046</td><td></td></tr><tr><td>C4r.2r</td><td>8.771</td><td>0.471</td><td>C4r.2r-1 is within C4r.2r (8.661–8.699 Ma).</td></tr><tr><td>C4An</td><td>9.105</td><td>0.334</td><td></td></tr><tr><td>C4Ar.1r</td><td>9.311</td><td>0.206</td><td></td></tr><tr><td>C4Ar.1n</td><td>9.426</td><td>0.115</td><td></td></tr><tr><td rowspan="10">late (Tortonian)</td><td rowspan="10">late (Tortonian)</td><td rowspan="10">7.246</td><td rowspan="10">C4A</td><td>C4Ar.2r</td><td>9.647</td><td>0.221</td><td></td></tr><tr><td>C4Ar.2n</td><td>9.721</td><td>0.074</td><td></td></tr><tr><td>C4Ar.3r</td><td>9.786</td><td>0.065</td><td></td></tr><tr><td>C5n.1n</td><td>9.937</td><td>0.151</td><td></td></tr><tr><td>C5n.1r</td><td>9.984</td><td>0.047</td><td></td></tr><tr><td>C5n.2n</td><td>11.056</td><td>1.072</td><td>C5n.2n-1 through 3</td></tr><tr><td>C5r.1r</td><td>11.146</td><td>0.09</td><td></td></tr><tr><td>C5r.1n</td><td>11.188</td><td>0.042</td><td></td></tr><tr><td>C5r.2r</td><td>11.592</td><td>0.404</td><td>C5r.2r-1 is within C5r.2r (11.263-11.308 Ma).</td></tr><tr><td rowspan="10">Miocene</td><td rowspan="10">Miocene</td><td rowspan="10">11.625</td><td rowspan="10">C5</td><td>C5r.2n</td><td>11.657</td><td>0.065</td><td>Base of Tortonian is near base of C5r.2n.</td></tr><tr><td>C5r.3r</td><td>12.049</td><td>0.392</td><td></td></tr><tr><td>C5An.1n</td><td>12.174</td><td>0.125</td><td></td></tr><tr><td>C5An.1r</td><td>12.272</td><td>0.098</td><td></td></tr><tr><td>C5An.2n</td><td>12.474</td><td>0.202</td><td></td></tr><tr><td>C5Ar.1r</td><td>12.735</td><td>0.261</td><td></td></tr><tr><td>C5Ar.1n</td><td>12.77</td><td>0.035</td><td></td></tr><tr><td>C5Ar.2r</td><td>12.829</td><td>0.059</td><td></td></tr><tr><td>C5Ar.2n</td><td>12.887</td><td>0.058</td><td></td></tr><tr><td>C5Ar.3r</td><td>13.032</td><td>0.145</td><td></td></tr><tr><td rowspan="6">middle (Serravalian)</td><td rowspan="6">middle (Serravalian)</td><td rowspan="6">11.625</td><td rowspan="6">C5A</td><td>C5AAn</td><td>13.183</td><td>0.151</td><td></td></tr><tr><td>C5AAr</td><td>13.363</td><td>0.18</td><td></td></tr><tr><td>C5ABn</td><td>13.608</td><td>0.245</td><td></td></tr><tr><td>C5ABr</td><td>13.739</td><td>0.131</td><td></td></tr><tr><td>C5ACn</td><td>14.07</td><td>0.331</td><td>Base of Serravalian is upper C5ACn.</td></tr><tr><td>C5ACr</td><td>14.163</td><td>0.093</td><td></td></tr><tr><td rowspan="6">middle (Langhian)</td><td rowspan="6">middle (Langhian)</td><td rowspan="6">13.82</td><td rowspan="6">C5A</td><td>C5ADn</td><td>14.609</td><td>0.446</td><td></td></tr><tr><td>C5ADr</td><td>14.775</td><td>0.166</td><td></td></tr><tr><td>C5Bn.1n</td><td>14.87</td><td>0.095</td><td></td></tr><tr><td>C5Bn.1r</td><td>15.032</td><td>0.162</td><td></td></tr><tr><td>C5Bn.2n</td><td>15.16</td><td>0.128</td><td></td></tr><tr><td>C5Br</td><td>15.974</td><td>0.814</td><td>Base of Langhian is base of C5Br.</td></tr><tr><td rowspan="10">early (Burdigalian)</td><td rowspan="10">early (Burdigalian)</td><td rowspan="10">20.44</td><td rowspan="10">C5C</td><td>C5Cn.1n</td><td>16.268</td><td>0.294</td><td></td></tr><tr><td>C5Cn.1r</td><td>16.303</td><td>0.035</td><td></td></tr><tr><td>C5Cn.2n</td><td>16.472</td><td>0.169</td><td></td></tr><tr><td>C5Cn.2r</td><td>16.543</td><td>0.071</td><td></td></tr><tr><td>C5Cn.3n</td><td>16.721</td><td>0.178</td><td></td></tr><tr><td>C5Cr</td><td>17.235</td><td>0.514</td><td></td></tr><tr><td>C5Dn</td><td>17.533</td><td>0.298</td><td></td></tr><tr><td>C5Dr.1r</td><td>17.717</td><td>0.184</td><td></td></tr><tr><td>C5Dr.1n</td><td>17.74</td><td>0.023</td><td>Cryptochron in C5Dr</td></tr><tr><td>C5Dr.2r</td><td>18.056</td><td>0.316</td><td></td></tr></tbody></table>
<table><caption>Table T7 (continued). (Continued on next page.)</caption><thead><tr><th>Period</th><th>Epoch</th><th>Age (stage)</th><th>Base age (Ma)</th><th>Chron</th><th>Polarity chron</th><th>Age at base of chron (Ma)</th><th>Duration (My)</th><th>Remarks</th></tr></thead><tbody><tr><td rowspan="20">Neogene</td><td rowspan="10">Miocene</td><td rowspan="5">early (Burdigalian)</td><td rowspan="5">20.44</td><td>C5E</td><td>C5En</td><td>18.524</td><td>0.468</td><td></td></tr><tr><td rowspan="3">C6</td><td>C5Er</td><td>18.748</td><td>0.224</td><td></td></tr><tr><td>C6n</td><td>19.722</td><td>0.974</td><td></td></tr><tr><td>C6r</td><td>20.04</td><td>0.318</td><td>Cryptochron C6r-1</td></tr><tr><td rowspan="2">C6A</td><td>C6An.1n</td><td>20.213</td><td>0.173</td><td></td></tr><tr><td>C6An.1r</td><td>20.439</td><td>0.226</td><td>Base of Burdigalian (working version) is approximate base of C6An.1r (used here) or of C6An.1n.</td></tr><tr><td rowspan="5">early (Aquitanian)</td><td rowspan="5">23.03</td><td>C6A</td><td>C6An.2n</td><td>20.709</td><td>0.27</td><td></td></tr><tr><td rowspan="4">C6AA</td><td>C6Ar</td><td>21.083</td><td>0.374</td><td></td></tr><tr><td>C6AAn</td><td>21.159</td><td>0.076</td><td></td></tr><tr><td>C6AAr.1r</td><td>21.403</td><td>0.244</td><td></td></tr><tr><td>C6AAr.1n</td><td>21.483</td><td>0.08</td><td></td></tr><tr><td rowspan="5">C6B</td><td>C6AAr.2r</td><td>21.659</td><td>0.176</td><td></td></tr><tr><td>C6AAr.2n</td><td>21.688</td><td>0.029</td><td></td></tr><tr><td>C6AAr.3r</td><td>21.767</td><td>0.079</td><td></td></tr><tr><td>C6Bn.1n</td><td>21.936</td><td>0.169</td><td></td></tr><tr><td>C6Bn.1r</td><td>21.992</td><td>0.056</td><td></td></tr><tr><td rowspan="5">C6C</td><td>C6Bn.2n</td><td>22.268</td><td>0.276</td><td></td></tr><tr><td>C6Br</td><td>22.564</td><td>0.296</td><td></td></tr><tr><td>C6Cn.1n</td><td>22.754</td><td>0.19</td><td></td></tr><tr><td>C6Cn.1r</td><td>22.902</td><td>0.148</td><td></td></tr><tr><td>C6Cn.2n</td><td>23.03</td><td>0.128</td><td>Base of Miocene is base of C6Cn.2n.</td></tr><tr><td rowspan="10">Oligocene</td><td rowspan="5">late (Chattian)</td><td rowspan="5">28.09</td><td>C7</td><td>C6Cn.2r</td><td>23.233</td><td>0.203</td><td></td></tr><tr><td rowspan="3">C7A</td><td>C6Cn.3n</td><td>23.295</td><td>0.062</td><td></td></tr><tr><td>C6Cr</td><td>23.962</td><td>0.667</td><td></td></tr><tr><td>C7n.1n</td><td>24</td><td>0.038</td><td></td></tr><tr><td rowspan="2">C8</td><td>C7n.1r</td><td>24.109</td><td>0.109</td><td></td></tr><tr><td>C7n.2n</td><td>24.474</td><td>0.365</td><td>Cryptochron C7r-1</td></tr><tr><td rowspan="5">C9</td><td>C7r</td><td>24.761</td><td>0.287</td><td></td></tr><tr><td>C7An</td><td>24.984</td><td>0.223</td><td></td></tr><tr><td>C7Ar</td><td>25.099</td><td>0.115</td><td></td></tr><tr><td>C8n.1n</td><td>25.264</td><td>0.165</td><td></td></tr><tr><td>C8n.1r</td><td>25.304</td><td>0.04</td><td></td></tr><tr><td rowspan="10">Paleogene</td><td rowspan="5">early (Rupelian)</td><td rowspan="5">33.89</td><td>C10</td><td>C8n.2n</td><td>25.987</td><td>0.683</td><td>Cryptochron C8n.2n-1</td></tr><tr><td rowspan="4">C11</td><td>C8r</td><td>26.42</td><td>0.433</td><td></td></tr><tr><td>C9n</td><td>27.439</td><td>1.019</td><td>Cryptochrons C9n-1; C9n-2</td></tr><tr><td>C9r</td><td>27.859</td><td>0.42</td><td>Cryptochron C9r-1</td></tr><tr><td>C10n.1n</td><td>28.087</td><td>0.228</td><td>Base of Chattian (working version) is base of C10n.1n. Note: base is potentially at ~70% up in "undifferentiated Chron C10n" in candidate GSSP in Italy (Coccioni et al.; 2008); which would project as equivalent to C10n.1n.4.</td></tr><tr><td rowspan="10">Eocene</td><td rowspan="5">late (Priabonian)</td><td rowspan="5">37.99</td><td>C10n.1r</td><td>C10n.1n</td><td>28.141</td><td>0.054</td><td></td></tr><tr><td>C10n.2n</td><td>C10n.2n</td><td>28.278</td><td>0.137</td><td></td></tr><tr><td>C10r</td><td>C10n.1n</td><td>29.183</td><td>0.905</td><td>Cryptochrons C10r-1; C10r-2</td></tr><tr><td>C11n.1n</td><td>C11n.1n</td><td>29.477</td><td>0.294</td><td></td></tr><tr><td>C11n.1r</td><td>C11n.1r</td><td>29.527</td><td>0.05</td><td></td></tr><tr><td rowspan="4">C12</td><td>C11n.2n</td><td>29.97</td><td>0.443</td><td></td></tr><tr><td>C11r</td><td>30.591</td><td>0.621</td><td>Cryptochron C11r-1</td></tr><tr><td>C12n</td><td>31.034</td><td>0.443</td><td></td></tr><tr><td>C12r</td><td>33.157</td><td>2.123</td><td>Cryptochrons C12r-1 through C12r-8</td></tr><tr><td rowspan="5">middle (Bartonian)</td><td rowspan="5">41.03</td><td>C13</td><td>C13n</td><td>33.705</td><td>0.548</td><td>Cryptochron C13n-1</td></tr><tr><td>C13r</td><td>35.102</td><td>1.397</td><td>Base of Rupellian is at C13r.86. Cryptochrons C13r-1 through C13r-4</td></tr><tr><td>C15</td><td>C15n</td><td>35.336</td><td>0.234</td><td>"C14" does not exist.</td></tr><tr><td rowspan="4">C16</td><td>C15r</td><td>35.58</td><td>0.244</td><td></td></tr><tr><td>C16n.1n</td><td>35.718</td><td>0.138</td><td></td></tr><tr><td>C16n.1r</td><td>35.774</td><td>0.056</td><td></td></tr><tr><td>C16n.2n</td><td>36.351</td><td>0.577</td><td></td></tr><tr><td rowspan="5">C17</td><td rowspan="5">41.03</td><td>C16r</td><td>C17n.1n</td><td>37.385</td><td>0.812</td><td>Base of Priabonian (working version) assigned as base of C17n.1n.</td></tr><tr><td>C17n.1r</td><td>C17n.1n</td><td>37.53</td><td>0.145</td><td></td></tr><tr><td>C17n.2n</td><td>C17n.2n</td><td>37.781</td><td>0.251</td><td></td></tr><tr><td>C17n.2r</td><td>C17n.2r</td><td>37.858</td><td>0.077</td><td></td></tr><tr><td>C17n.3n</td><td>C17n.3n</td><td>38.081</td><td>0.223</td><td></td></tr><tr><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td></tr></tbody></table>
<table><caption>Table T7 (continued).</caption><thead><tr><th>Period</th><th>Epoch</th><th>Age (stage)</th><th>Base age (Ma)</th><th>Chron</th><th>Polarity chron</th><th>Age at base of chron (Ma)</th><th>Duration (My)</th><th>Remarks</th></tr></thead><tbody><tr><td rowspan="22">Paleogene</td><td rowspan="10">Eocene</td><td rowspan="4">middle (Bartonian)</td><td rowspan="4">41.03</td><td>C18</td><td>C18n.1n</td><td>39.582</td><td>1.184</td><td>Cryptochron C18n.1n-1</td></tr><tr><td rowspan="4">middle (Lutetian)</td><td rowspan="4">47.84</td><td>C19</td><td>C18n.1r</td><td>39.666</td><td>0.084</td><td></td></tr><tr><td rowspan="4">middle (Lutetian)</td><td rowspan="4">47.84</td><td>C20</td><td>C18n.2n</td><td>40.073</td><td>0.407</td><td></td></tr><tr><td rowspan="4">middle (Lutetian)</td><td rowspan="4">47.84</td><td>C21</td><td>C18r</td><td>41.03</td><td>0.957</td><td>Base of Bartonian (working version) assigned as base of C18r.</td></tr><tr><td rowspan="4">early (Ypresian)</td><td rowspan="4">55.96</td><td>C19</td><td>C19n</td><td>41.18</td><td>0.15</td><td></td></tr><tr><td rowspan="4">early (Ypresian)</td><td rowspan="4">55.96</td><td>C20</td><td>C19r</td><td>42.124</td><td>0.944</td><td></td></tr><tr><td rowspan="4">early (Ypresian)</td><td rowspan="4">55.96</td><td>C21</td><td>C20n</td><td>43.426</td><td>1.302</td><td></td></tr><tr><td rowspan="4">early (Ypresian)</td><td rowspan="4">55.96</td><td>C22</td><td>C20r</td><td>45.724</td><td>2.298</td><td></td></tr><tr><td rowspan="4">early (Ypresian)</td><td rowspan="4">55.96</td><td>C23</td><td>C21n</td><td>47.349</td><td>1.625</td><td></td></tr><tr><td rowspan="4">early (Ypresian)</td><td rowspan="4">55.96</td><td>C24</td><td>C21r</td><td>48.566</td><td>1.217</td><td>Base of Lutetian (GSSP ratified Feb 2011) is base of nannofossil <i>Blackites inflatus</i> at Gorrondatxe section in Spain.</td></tr><tr><td rowspan="4">late (Thanetian)</td><td rowspan="4">59.24</td><td>C22</td><td>C22n</td><td>49.344</td><td>0.778</td><td></td></tr><tr><td rowspan="4">late (Thanetian)</td><td rowspan="4">59.24</td><td>C23</td><td>C22r</td><td>50.628</td><td>1.284</td><td></td></tr><tr><td rowspan="4">late (Thanetian)</td><td rowspan="4">59.24</td><td>C24</td><td>C23n.1n</td><td>50.835</td><td>0.207</td><td></td></tr><tr><td rowspan="4">late (Thanetian)</td><td rowspan="4">59.24</td><td>C25</td><td>C23n.1r</td><td>50.961</td><td>0.126</td><td></td></tr><tr><td rowspan="4">late (Thanetian)</td><td rowspan="4">59.24</td><td>C26</td><td>C23n.2n</td><td>51.833</td><td>0.872</td><td></td></tr><tr><td rowspan="4">late (Thanetian)</td><td rowspan="4">59.24</td><td>C27</td><td>C23r</td><td>52.62</td><td>0.787</td><td></td></tr><tr><td rowspan="4">late (Thanetian)</td><td rowspan="4">59.24</td><td>C28</td><td>C24n.1n</td><td>53.074</td><td>0.454</td><td></td></tr><tr><td rowspan="4">late (Thanetian)</td><td rowspan="4">59.24</td><td>C29</td><td>C24n.1r</td><td>53.199</td><td>0.125</td><td></td></tr><tr><td rowspan="4">late (Thanetian)</td><td rowspan="4">59.24</td><td>C30</td><td>C24n.2n</td><td>53.274</td><td>0.075</td><td></td></tr><tr><td rowspan="4">late (Thanetian)</td><td rowspan="4">59.24</td><td>C31</td><td>C24n.2r</td><td>53.416</td><td>0.142</td><td></td></tr><tr><td rowspan="4">late (Thanetian)</td><td rowspan="4">59.24</td><td>C32</td><td>C24n.3n</td><td>53.983</td><td>0.567</td><td>This is NOT tied proportionally within C24r, but some indicate it as C24r.36 (e.g., used in Agnini et al., 2007, for calibrating nannofossil datums near boundary). Age used here is from U-Pb ≥ 0.05 My lower. Base of Eocene is 0.94 My (0.98 in another table) above top C25n according to cycle stratigraphy.</td></tr><tr><td rowspan="4">middle (Selandian)</td><td rowspan="4">61.61</td><td>C24</td><td>C24r</td><td>57.101</td><td>3.118</td><td></td></tr><tr><td rowspan="4">middle (Selandian)</td><td rowspan="4">61.61</td><td>C25</td><td>C25n</td><td>57.656</td><td>0.555</td><td></td></tr><tr><td rowspan="4">middle (Selandian)</td><td rowspan="4">61.61</td><td>C26</td><td>C25r</td><td>58.959</td><td>1.303</td><td></td></tr><tr><td rowspan="4">middle (Selandian)</td><td rowspan="4">61.61</td><td>C27</td><td>C26n</td><td>59.237</td><td>0.278</td><td>Base of C26n = same as temporary assignment in GTS2004 (GSSP in Zumaya, Spain), as in Berggren et al., 1995.</td></tr><tr><td rowspan="4">early (Danian)</td><td rowspan="4">66.04</td><td>C27</td><td>C26r</td><td>62.221</td><td>2.984</td><td>Onset of a carbon isotope shift and sea level drop (Exxon/Hardenbol sequence boundary "Sel1"); near diversification of the Fasciculith group of calcareous nannoplankton, preceding the lowest <i>Fasciculithus tympaniformis</i> (base of nannoplankton Zone NP5).</td></tr><tr><td rowspan="4">early (Danian)</td><td rowspan="4">66.04</td><td>C28</td><td>C27n</td><td>62.517</td><td>0.296</td><td></td></tr><tr><td rowspan="4">early (Danian)</td><td rowspan="4">66.04</td><td>C29</td><td>C27r</td><td>63.494</td><td>0.977</td><td></td></tr><tr><td rowspan="4">early (Danian)</td><td rowspan="4">66.04</td><td>C30</td><td>C28n</td><td>64.667</td><td>1.173</td><td></td></tr><tr><td rowspan="4">early (Danian)</td><td rowspan="4">66.04</td><td>C31</td><td>C28r</td><td>64.958</td><td>0.291</td><td></td></tr><tr><td rowspan="4">early (Danian)</td><td rowspan="4">66.04</td><td>C32</td><td>C29n</td><td>65.688</td><td>0.73</td><td></td></tr><tr><td rowspan="4">early (Danian)</td><td rowspan="4">66.04</td><td>C33</td><td>C29r</td><td>66.398</td><td>0.71</td><td>Mesozoic/Cenozoic boundary event is ~C29r.5 in total C29r span of ~710 ky, according to cycles; Husson et al., 2012.</td></tr><tr><td rowspan="4">Cretaceous</td><td rowspan="4">Late</td><td rowspan="4">Masstrichtian</td><td rowspan="4">66.04</td><td>C30</td><td>C30n</td><td>68.196</td><td></td><td></td></tr></tbody></table>
Figure F24. Selected Cenozoic marine and terrestrial biostratigraphic zonations. Age is the time equivalent of the rock-record stage. Subepoch groupings of these ages into "late" or "early" are informal common usage. Magnetic polarity zones are scaled to astronomical cycles (e.g., Hilgen et al., 2012; Vandenberghe et al., 2012; Westerhold et al., 2015). Planktonic foraminifer zones and main markers are from GPTS2012 (Hilgen et al., 2012; Anthonissen and Ogg, 2012) with Paleogene modified from Wade et al. (2011), but late Pliocene details for Zones PL4–PL5 between Atlantic (Atl.) and Pacific (Pac.) basins are omitted. Placement of proposed base Chattian marker of last common occurrence (LCO) of *Chiloguembelina cubensis* is relative to Oligocene magnetic polarity chrons; hence, the assigned age to the Rupelian/Chattian boundary is uncertain. Calcareous nannofossil (CN) zones and markers from Backman et al. (2012) and Agnini et al. (2014) are shown with commonly used NN and NP zonations of Martini (1971). Major sea level sequence boundaries and highstands are from Hardenbol et al. (1998). Additional zonations, biostratigraphic markers, geochemical trends, sea level curves, and details on calibrations are compiled in Hilgen et al. (2012) and Vandenberghe et al. (2012) and in internal data sets within the TimeScale Creator visualization system (free at https://engineering.purdue.edu/Stratigra phy/tscreator/index/index.php). Modified from Ogg et al. (2016). LGM = last glacial maximum. Megacycles: T = transgression, R = regression. (Continued on next two pages.)

<table><caption>Neogene and Quaternary timescale</caption><thead><tr><th>Age (Ma)</th><th>Epoch/Age (Ma) (Stage)</th><th>Polarity Chron</th><th>Planktonic foraminifers</th><th>Calcareous nannoplankton</th><th>Megacycles</th></tr></thead><tbody><tr><td>1</td><td>Holo-<br>e.</td><td>m. 0.77 m. Pleist.</td><td rowspan="3">Pt1</td><td rowspan="3">Globorotalia tosaensis<br>Globorotalia truncatinoides</td><td rowspan="3">Emiliania huxleyi<br>Gephyrocapsa spp. &gt;4 µm reentrance</td><td rowspan="3">LGM</td></tr><tr><td>2</td><td>Pleistocene</td><td>Calabrian 1.81</td></tr><tr><td>3</td><td>e.</td><td>Gelasian 2.59</td></tr><tr><td>4</td><td>Pliocene</td><td>I. Piacenzian 3.6</td><td rowspan="2">C2A</td><td rowspan="2">Globorotalia miocenica (Atl.)<br>Sphaeroidinellopsis seminulina</td><td rowspan="2">Gephyrocapsa spp. &gt;4 µm<br>Discoaster brouweri<br>Discoaster pentaradiatus</td><td rowspan="2">G. spp. &gt;5.5 µm, G. spp. &gt;4 µm</td></tr><tr><td>5</td><td>e.</td><td>Zanclean 5.33</td></tr><tr><td>6</td><td></td><td>Messinian 7.25</td><td rowspan="2">C3</td><td rowspan="2">Globorotalia tumida (Pac.)<br>Globorotalia nepenthes</td><td rowspan="2">Discoaster asymmetricus (common)<br>Ceratolithus rugosus<br>Ceratolithus acutus<br>Nicklithus amplificus</td><td rowspan="2">Discoaster tamalis<br>Reticulofenestra pseudoumbilicus<br>Amauroolithus tricorniculatus</td></tr><tr><td>7</td><td></td><td></td></tr><tr><td>8</td><td></td><td>Tortonian 11.63</td><td rowspan="2">C4A</td><td rowspan="2">Globorotalia lenguensis (Pac.)<br>Globorotalia plesiotumida<br>Neogloboquadrina acostaensis (subtropical)</td><td rowspan="2">Discoaster quinqueramus<br>Discoaster berggrenii<br>Reticulofenestra pseudoumbilicus (absence)</td><td rowspan="2">Discoaster hamatus</td></tr><tr><td>9</td><td></td><td></td></tr><tr><td>10</td><td></td><td>Tortonian 13.82</td><td rowspan="2">C4</td><td rowspan="2">Neogloboquadrina acostaensis (temperate)<br>Paragloborotalia mayeri (subtropical)</td><td rowspan="2">Discoaster hamatus<br>Catinaster coalitus<br>Discoaster kugleri (common)</td><td rowspan="2">Discoaster kugleri (common)</td></tr><tr><td>11</td><td></td><td></td></tr><tr><td>12</td><td>Miocene</td><td>e.</td><td rowspan="2">C5</td><td rowspan="2">Globoturbورotalita nepenthes<br>Fohsella robusta<br>Fohsella fohsi</td><td rowspan="2">Discoaster quinqueramus<br>Discoaster berggrenii<br>Reticulofenestra pseudoumbilicus (absence)</td><td rowspan="2">Discoaster hamatus</td></tr><tr><td>13</td><td></td><td></td></tr><tr><td>14</td><td></td><td>Serravallian 15.97</td><td rowspan="2">C5A</td><td rowspan="2">Fohsella "praefohsi"<br>Fohsella peripheroacuta<br>Orbulina suturalis</td><td rowspan="2">Discoaster hamatus<br>Catinaster coalitus<br>Discoaster kugleri (common)</td><td rowspan="2">Discoaster kugleri (common)</td></tr><tr><td>15</td><td></td><td></td></tr><tr><td>16</td><td></td><td>Langhian 15.97</td><td rowspan="2">C5B</td><td rowspan="2">Praeorbulina glomerosa s.str.<br>Praeorbulina sicana<br>Globigerinatella insueta s.str.</td><td rowspan="2">Discoaster hamatus<br>Catinaster coalitus<br>Discoaster kugleri (common)</td><td rowspan="2">Discoaster kugleri (common)</td></tr><tr><td>17</td><td></td><td></td></tr><tr><td>18</td><td></td><td>Burdigalian 20.44</td><td rowspan="2">C5D</td><td rowspan="2">Globigerinatella sp.<br>Paragloborotalia dehiscens<br>"Paragloborotalia" kugleri</td><td rowspan="2">Discoaster hamatus<br>Catinaster coalitus<br>Discoaster kugleri (common)</td><td rowspan="2">Discoaster kugleri (common)</td></tr><tr><td>19</td><td></td><td></td></tr><tr><td>20</td><td></td><td>Aquitanian 23.03</td><td rowspan="2">C6</td><td rowspan="2">Globoquadrina dehiscens<br>"Paragloborotalia" kugleri</td><td rowspan="2">Helicosphaera euphratis → H. carteri dominance<br>Triquetrorhabdulus carinatus (common)</td><td rowspan="2">Helicosphaera ampliaperta</td></tr><tr><td>21</td><td></td><td></td></tr><tr><td>22</td><td></td><td>Aquitanian 23.03</td><td rowspan="2">C6A</td><td rowspan="2">Globoquadrina dehiscens<br>"Paragloborotalia" kugleri</td><td rowspan="2">Sphenolithus heteromorphus<br>Sphenolithus belemnos</td><td rowspan="2">Sphenolithus heteromorphus<br>Sphenolithus belemnos</td></tr><tr><td>23</td><td></td><td></td></tr><tr><td></td><td>Paleogene</td><td></td><td>C6B</td><td>M1</td><td>Globigerinatella sp.</td><td>Sphenolithus heteromorphus<br>Sphenolithus belemnos</td><td>Sphenolithus belemnos</td></tr><tr><td></td><td></td><td></td><td>C6C</td><td>O7</td><td></td><td>Helicosphaera euphratis → H. carteri dominance<br>Triquetrorhabdulus carinatus (common)</td><td>Helicosphaera ampliaperta</td></tr><tr><td></td><td></td><td></td><td></td><td></td><td></td><td>Sphenolithus disbelemnos<br>Discoaster druggi (s.s.)</td><td>Sphenolithus delphix<br>Reticulofenestra bisecta (&gt;10 µm)</td></tr><tr><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td></tr></tbody></table>
# Geochemistry

The shipboard geochemistry program for Expeditions 367 and 368 included the following measurements:

* Headspace gas content;

* Interstitial water composition;

* Sedimentary geochemistry, including total inorganic carbon, total carbon, total nitrogen, and major and minor element content; and

* Igneous and metamorphic rock geochemistry (major and minor element content).

Our analytical procedures follow those described by Integrated Ocean Drilling Program Expedition 345 and IODP Expeditions 349, and 352 (Gillis et al., 2014; Li et al., 2015; Reagan et al., 2015). Our analyses were conducted to satisfy routine shipboard safety and pollution prevention requirements; characterize interstitial water, sediment, and rock geochemistry for shipboard interpretation; and provide a basis for sampling for subsequent shore-based research.

## Headspace gas analysis

For headspace gas analysis, 5 cm³ samples were collected immediately after core retrieval on deck, placed in a 20 cm³ glass vial, sealed with a septum, and crimped with a metal cap. When consolidated or lithified samples were encountered, chips of material were placed in the vial and sealed and soft-sediment samples were collected with a sawn-off syringe or with a scoop. If an interstitial water sample was obtained, the headspace sample was taken from the top of the section immediately next to the interstitial water sample whenever possible. Otherwise, the headspace sample was taken from the top of the third section. The vial was labeled with the core, section, and interval from which the sample was taken and then placed in an oven at 70°C for 30 min. A 5 cm³ aliquot of gas was extracted through the septum with a gas-tight glass syringe and then injected into a gas chromatograph (GC).

An Agilent 6890 GC equipped with a flame ionization detector (FID) was used to measure the concentrations of methane ($C_1$), ethane ($C_2$), ethylene ($C_2$), propane ($C_3$), and propylene ($C_3$). A 2.4 m × 2.0 mm stainless steel column packed with 80/100 mesh HayeSep “R” was installed in the GC oven. The injector consists of a 1/16 inch Valco union with a 7 µm screen connected to a Valco-to-Luer lock syringe adapter. This injector connects to a 10-port Valco valve that is switched pneumatically by a digital valve interface. The injector temperature was set at 120°C throughout each run. Samples were introduced into the GC through a 0.25 cm³ sample loop connected to the Valco valve. The valve can be switched automatically to backflush the column. The oven temperature was programmed to start at 80°C for 8.25 min and then increase to 150°C at a rate of 40°C/min and hold for 5 min. Helium was used as the carrier gas. Initial helium flow in the column was 30 mL/min. Flow was then ramped up to 60 mL/min after 8.25 min to accelerate elution of $C_3$ and $C_3^-$: The run time was 15 min. The GC was also equipped with an electronic pressure control module to control the overall gas flow. The FID was set at 250°C. Data were collected and evaluated with an Agilent Chemstation data handling program. Chromatographic response was calibrated against known standards provided by Scott Specialty Gases.

No accurate measurement of the sediment mass was carried out. As such, measured concentrations are semiquantitative (likely carrying a ±25% relative uncertainty, mainly reflecting variations in the sediment mass around the target mass) and are only indicative

for safety monitoring. However, gas ratios (e.g., $C_1/C_2$) are not affected by the uncertainty on the sediment mass.

## Interstitial water chemistry

### Interstitial water collection

Routine interstitial water samples were obtained by squeezing whole-round sections cut from cores. Standard whole-round samples were 5 cm long, but as water content decreased downhole, the size of the whole-round samples was increased to 15 cm to enable extraction of ~30 mL of water needed for shipboard and shore-based analyses. Interstitial water collection stopped when it was no longer possible to obtain ~10 mL for shipboard analyses by squeezing 15–20 cm long whole-round sediments. Whole-round samples were cut and capped as quickly as possible after the core arrived on deck and immediately moved to the chemistry laboratory for squeezing. Whole-round samples were typically collected at a frequency of ~3 samples per core in the first 5 cores, 2 samples per core for cores 5–10, and subsequently 1 sample per core. Samples of basement were not collected for squeezing interstitial water.

The exterior of the whole-round sample was carefully scraped with a spatula to remove potential contamination from drilling fluid and sediment smearing in the borehole. In APC cores, ~0.5 cm of material from outside of the whole round was removed, whereas in XCB and RCB cores, where borehole contamination is higher, as much as two-thirds of the sediment was removed from each whole round. The cleaned sediment was placed into a 9 cm diameter titania squeezer that was then placed in a Carver hydraulic press (Manheim and Sayles, 1974) and squeezed at pressures no higher than 30,000 lb (~20.3 MPa) to extract interstitial water. The squeezed interstitial water was collected in precleaned high-density polyethylene syringes attached to the squeezing assembly. Subsequently, the interstitial water was filtered through a 0.45 µm polyethersulfone membrane disc filter into various sample containers, except for aliquots taken for dissolved organic carbon (DOC) analysis, which were filtered through a 0.2 µm polyethersulfone membrane disc filter.

Sample allocation was determined based on the pore fluid volume obtained and analytical priorities based on the objectives of the expedition. Aliquots for major and minor elements by ICP-AES were acidified by adding ~10 µL of trace metal–grade concentrated $HNO_3$ and placed in 2 mL cryovials. Aliquots for chloride and alkalinity titration, ammonium and phosphate spectrophotometry analyses, and ion chromatography analyses were put in 8 mL glass vials. Aliquots for isotopic analyses of oxygen and hydrogen were placed in zero-headspace 2 mL septum screw-lid glass vials. Aliquots for Sr, B, and Li isotopes were acidified by adding ~10 µL of trace metal–grade concentrated $HNO_3$ and placed in two 5 mL cryovials. Aliquots for dissolved inorganic carbon (DIC) and DOC and their $\delta^{13}C$ were treated with 10 µL of a saturated $HgCl_2$ solution and placed in zero-headspace 2 mL and 5 mL septum screw-lid glass vials, respectively. Aliquots for $TH_2S$ were placed in 2 mL septum screw-lid glass vials with 0.5 mL of ~50 mM zinc acetate solution. The samples were stored at 4°C after collection.

Alkalinity, pH, and salinity were analyzed immediately after interstitial water was obtained. Other shipboard analyses were carried out in batches. Dissolved sodium, calcium, magnesium, chloride, bromide, and sulfate were analyzed by ion chromatography. Ammonium and phosphate were analyzed by UV-VIS spectrophotometry. Minor element concentrations were analyzed by ICP-AES.

After interstitial water extraction was complete, sediment squeeze cakes were divided and sealed in plastic bags for shipboard
and shore-based analyses. Squeeze cake samples for shore-based organic analysis were stored at -20°C. All other squeeze cake samples were refrigerated at 4°C.

## Shipboard interstitial water analysis

Interstitial water samples were analyzed on board following the protocols in Gieskes et al. (1991), Murray et al. (2000), and the Integrated Ocean Drilling Program user manual for shipboard instrumentation, which was updated during Expedition 344 (Harris et al., 2013).

### Salinity, alkalinity, and pH

Salinity, alkalinity, and pH were measured immediately after squeezing, following the procedures in Gieskes et al. (1991). Salinity was measured using a Fisher temperature-compensated handheld refractometer. The pH was measured with a combined glass electrode, and alkalinity was determined by Gran titration with an auto-titrator (Metrohm 794 basic Titrino). Three milliliters of interstitial water sample was titrated against 0.1 M HCl at 25°C. International Association for the Physical Sciences of the Oceans (IAPSO) standard seawater was used for calibration and was analyzed at the beginning and end of a set of samples for each site and also every 5–10 samples. Both the analytical precision and accuracy of alkalinity titrations were better than 3% based on repeated analysis of IAPSO standard seawater.

### Chloride by titration

High-precision chloride concentrations were acquired using a Metrohm 785 DMP autotitrator and silver nitrate ($AgNO_3$) solution calibrated against repeated titrations of IAPSO standard. A 0.5 mL aliquot of sample was diluted with 30 mL of 0.32 M $HNO_3$ solution and titrated with 0.1 M $AgNO_3$. Repeated analyses of an IAPSO standard yielded a precision better than 0.06%; however, the chloride concentrations yielded by titration includes not only dissolved chloride but also all of the other halide elements and bisulfide. The *JOIDES Resolution* is equipped with a Metrohm 850 Professional ion chromatograph that can analyze anions and cations simultaneously. The chloride concentration was analyzed by both titration and ion chromatography for Holes U1499A, U1501C, U1501D, U1502A, U1504A, and U1505C. Chloride concentrations analyzed by ion chromatography were not greater than those by titration, indicating that ion chromatography can provide mostly reliable chloride data. As a result, chloride concentration was analyzed by both titration and ion chromatography only for the upper 50 m section for all sites during Expeditions 367 and 368.

### Sulfate, chloride, bromide, calcium, magnesium, potassium, and sodium

Sulfate, chloride, bromide, calcium, magnesium, and sodium concentrations were analyzed by ion chromatography (Metrohm 850 Professional IC) using aliquots of 100 µL that were diluted 1:100 with deionized water (18 MΩ/cm). At the beginning and end of each run, different dilutions (1:80 to 1:500) of IAPSO standard seawater were analyzed to create a six point calibration curve. The r² for the calibration curve was always >0.99, and relative standard deviation varied from 0.8% to 3.4%. The 1:100 diluted IAPSO standard seawater was also analyzed every ~10 samples for quality control and to determine accuracy and precision. A new calibration curve was run if measured concentrations deviated from the expected values (28.9 mM for $SO_4^{2-}$ and 0.865 mM for $Br^-$). Based on measurements of IAPSO standard seawater, analytical precision (2σ) was

within 1% for chloride, 5% for bromide, 2% for sulfate, 5% for calcium, 3% for magnesium, and 1% for sodium.

### Ammonium and phosphate

Ammonium and phosphate concentrations were determined using an Agilent Technologies Cary Series SPS3 spectrophotometer with a sipper sample introduction system following the protocol in Gieskes et al. (1991). For ammonium concentration analysis, a 0.2 mL sample aliquot was diluted with 2 mL reagent water to which 1 mL phenol ethanol, 1 mL sodium nitroprusside, and 2 mL oxidizing solution of sodium hypochlorite were added in a 15 mL capped plastic tube (Gieskes et al., 1991). The solution was kept at room temperature for ~6.5 h to develop color. Ammonium concentrations were determined at an absorbance of 640 nm. Precision and accuracy of the ammonium analyses of a standard were within 4% and 10%, respectively.

For phosphate analysis, a 0.6 mL sample was diluted with 2 mL deionized water (18 MΩ/cm) and 4 mL mixed reagent solution of ammonium molybdate, sulfuric acid, ascorbic acid, and antimony potassium tartrate in a 15 mL plastic tube. Then 2 mL of mixed reagent (ammonium molybdate, sulfuric acid, ascorbic acid, and potassium antimonyl tartrate) was added to the vial (Gieskes et al., 1991), which was capped and kept at room temperature for at least several minutes to develop color. The phosphate concentration was determined at an absorbance of 885 nm ~30 min after adding the mixed reagent solution. At beginning of each run, different concentrations (0–300 µM) of phosphorus standards were analyzed to create an 11-point calibration curve. Based on the measurements of 100 µM phosphorus standard during the expedition, precision (1σ) and accuracy of the phosphate analyses were better than 2% and 0.3%, respectively.

### Minor elements

Dissolved minor elements were determined by Teledyne Lee-man Prodigy ICP-AES. The general method for shipboard ICP-AES analysis of samples is described in Murray et al. (2000) and the user manuals for shipboard instrumentation.

For minor element (B, $Ba^{2+}$, $Fe^{2+}$, $Mn^{2+}$, $Li^+$, Si, and $Sr^{2+}$) analyses, interstitial water samples were diluted 1:20 (v/v) using 2% $HNO_3$ solution with 10 ppm Y (the interstitial water matrix solution) as an internal standard. Because the high concentration of salt in interstitial water samples at the 1:20 dilution demands matrix matching of standards and samples, standards were prepared with an acidified synthetic seawater of 35‰ NaCl with 2% $HNO_3$ to have an ionic strength similar to seawater. A stock multielement synthetic standard solution was gravimetrically prepared from ultrapure primary standards (SPC Science PlasmaCAL) diluted in the acidified synthetic seawater. An eight-point calibration curve was created through diluting the stock multielement standard in the acidified synthetic seawater at various degrees. Drift correction was made using the factor from a drift monitor solution of 100% stock standard solution, which was analyzed every 8–10 samples. The ICP-AES autosampler and analysis chamber were rinsed with a 3% (by volume) $HNO_3$ solution between samples. Multiple wavelengths were measured for each element, and the best were selected for reporting element concentrations. Wavelengths were selected based on possible interferences, the linearity of calibration curves, and the precision and accuracy of measurements of several standards. The selected wavelengths were Ba = 493.409 nm, B = 249.772 nm, Li = 670.784 nm, Fe = 259.940 nm, Si = 288.158 nm, Mn = 257.610 nm, and Sr = 460.733 nm.
# Sediment geochemistry

## Sediment nitrogen and inorganic and organic carbon content

Samples (~50 mg) for carbon, sulfur and nitrogen analyses were collected from squeeze cakes from interstitial water analyses and taken from intervals of distinct lithologic importance for expedition aims. Samples were freeze-dried for ~24 h, crushed using an agate pestle and mortar, and then analyzed for total carbon (TC), total inorganic carbon (TIC), total sulfur (TS) and total nitrogen (TN).

TC, TS, and TN of the bulk sediment samples were determined with a ThermoElectron Corporation Flash EA 1112 CHNS elemental analyzer equipped with a ThermoElectron packed column CHNS/NCS GC and a thermal conductivity detector (TCD). Approximately 12–13 mg of dry sediment was weighed into a tin cup, and 5–10 mg of vanadium pentoxide was added. Samples were then combusted at 950°C in a stream of oxygen. The reaction gases were passed through a reduction chamber to reduce nitrogen oxides to N₂, and then the evolved N₂, CO₂, and SO₂ were separated by the GC column before detection by the TCD. All measurements were calibrated to a set of reference standards covering the range in expected TC, TS, and TN values (Soil Reference Material: Buffalo River Sediments PWDR7837591) that was run every 9 samples. Peak areas from the TCD were calculated to determine the TC, TS, and TN of the samples. Blank levels were determined by analyzing empty tin cups and were subtracted from each measurement. Blank contributions for C is on the order of 1 µg. Given the typical sample mass used (12.5 mg on average) and using a signal/blank threshold of 10, this translates into a detection limit of ~0.04 wt%. For N, blanks were also estimated from the intercept of the calibration curve, which gave results similar to direct blank determination (i.e., empty tin cup blank). Blank contribution for N is on the order of 12 µg, unsurprisingly high considering the use of a sampler open to the atmosphere. This translates into a detection limit of ~0.06 wt%. Accuracy of TC determination was estimated using repeated measurements of reference material and was found to be better than 5% of the TC value (i.e., <0.05 wt% for the vast majority of samples analyzed). Precision of TC determination was estimated from limited duplicate measurements and was systematically within estimated accuracy. TS determination was less accurate than for nitrogen or carbon, and based on the analysis of both blank cups and minimum detection limits obtained from calibration curves, this equates to a TS of 0.1 wt%.

Sulfur analyses were only carried out for Expedition 368. TIC was determined using a Coulometrics 5015 CO₂ coulometer. Approximately 13 mg (10 mg for lithologies dominated by carbonates) of sediment was weighed into a glass vial and acidified with 2 M HCl. The liberated CO₂ was titrated, and the corresponding change in light transmittance in the coulometric cell was monitored using a photodetection cell. The weight percent of calcium carbonate was calculated from the inorganic carbon content using the following equation:

$$CaCO_3 (wt\%) = TIC (wt\%) \times 100/12.$$

Blank levels were determined by analyzing empty reactors, were found to vary between 3 and 7 µg C, and were subtracted from each measurement. Repeated measurements of pure CaCO₃ (several times at the beginning and every 10 samples) were used to estimate accuracy, which was <2% of the TIC. TOC content was calculated by subtraction of TIC from TC.

## Surface-enhanced Raman spectroscopy of solvent extractable sedimentary organic matter

Samples for surface-enhanced Raman spectroscopy (SERS) of solvent extractable organic matter were only collected during Expedition 368. They were obtained from freeze-dried residues used for TC analysis or collected from locations of lithologic interest to expedition goals. Powdered samples were placed in 10 mL extraction vials and sonicated for 15 min in 3:1 DCM/MeOH (dichloromethane/methanol) to obtain a solvent extract. The extract was decanted into a separate vial; more DCM was added to the sediment-residue before sonication was repeated for another 15 min. The solvent was again decanted, and the process was repeated to produce three extraction stages. The combined extract was reduced to dryness.

The extract was dissolved in DCM, and 4 µL of it was introduced in small increments to the sample wells of a gold-coated SERS-substrate. Introducing samples as small increments allowed the solvent to evaporate under ambient conditions until the entire volume had been loaded. When the solvent had evaporated, 4 µL of dilute nitric acid (1 M concentration) was dispensed into the pit and allowed to stand for ~2–3 min. The aqueous phase remaining within the pit was then removed to aid focusing of the microscope on the base of the pit. Raman spectroscopic measurements were performed using a BW Tek i-Raman Pro fitted with a 532 nm light source and mounted on 20x video-microscope. Spectra were collected by accumulating 20 spectra over 20 s; spectral acquisition was in the range 200–2000 per centimeter. Laser spot size was approximately 1–2 µm, and laser power was 50% (<13 mW delivered to the sample). Identification of key bands was made with reference spectra presented in Alabi et al., 2015.

## Elemental analysis of bulk sediment/sedimentary rock by ICP-AES

Elemental composition of bulk sediment was determined using a Leeman ICP-AES. Our analytical approach followed the general procedure outlined by Murray et al. (2000) and the constraints indicated by Quintin et al. (2002). Analytical blanks were prepared using 400 mg of lithium metaborate (LiBO₂) flux to ensure matrix matching. Samples analyzed by ICP-AES were ignited before dissolution by heating 5 g of oven-dried (600°C for 12 h) ground sediment at 1025°C for 5 h to determine weight loss on ignition (LOI), release volatile phases (H₂O, CO₂, and S), and fully oxidize all iron to ferric iron.

Aliquots of 100 mg of ignited sediment and standards were mixed with 400 mg of LiBO₂ flux. Subsequently, 10 µL of a wetting agent, 0.172 mM lithium bromide (LiBr), was added to the samples, standards, and blanks. This mixture was fused at 1050°C for 5 min in a Bead Sampler NT-4100 prior to dissolution in 50 mL of 10% HNO₃. For complete dissolution, 1 h of shaking with a Burrell wrist-action shaker was required. Aliquots of 5 mL of the resulting solutions were filtered (0.45 µm) and diluted with 35 mL of 10% HNO₃, resulting in a 4000× dilution of the original sediment.

A range of standards was selected to cover the entire range of expected sediment compositions, with their suitability monitored during the expedition. These standards were: STSD1, STSD2, STSD4, SO-1, SO-2, SO-3, SO-4, NBS-1c, JR-2, and BCR-2. BHVO-2 was also selected as both the drift and consistency standard. A range of major and trace elements was analyzed. Major elements included Al, Ca, Fe, K, Mg, Mn, Na, Si, and Ti, and trace elements included Ba, Co, Cr, Cu, Sc, Sr, V, Zn, and Zr. Major elements were expressed as weight percent oxide, and trace elements were expressed as parts per million. LOI values were determined routinely.
Samples were analyzed in duplicate. The procedures used to pro-
cess the data are outlined in **Data reduction**, below.

The elemental compositions of sediment/sedimentary rock
were only determined during Expedition 368 because the bead
maker for the ICP did not work during Expedition 367.

Igneous and metamorphic rock geochemistry

**Sample preparation**

Representative samples of igneous and metamorphic rocks were
analyzed for major and trace element concentrations during Expe-
ditions 367 and 368 using the Leeman ICP-AES.

Samples ranging in size from ~2 to ~8 cm³ were cut from the
core with a diamond saw blade. A thin section billet was taken from
the same or adjacent interval for petrographic analysis and alter-
ation determination (see **Igneous and metamorphic petrology** and
**Alteration**). All outer surfaces were ground on a diamond-impreg-
nated disk to remove altered rinds and surface contamination de-
rived from the drill or saw. Each sample was then placed in a beaker
containing acetone and washed ultrasonically for 15 min. The ace-
tone was decanted, and the samples were sonicated in deionized
water (18 MΩ/cm) twice for 10 min. The cleaned pieces were dried
for 10–12 h at 110°C.

The cleaned, dried samples were crushed to <1 cm chips be-
tween two disks of Delrin plastic in a hydraulic press. The rock
chips were then ground to a fine powder in tungsten carbide in a
SPEX 8515 Shatterbox. After grinding, a 5.0 ± 0.5 g aliquot of the
sample powder was weighed on a Mettler Toledo balance and ig-
nited at 1025°C for 4 h to determine LOI.

Murray et al. (2000) describes in detail the shipboard procedure for digestion of rocks and ICP-AES analysis of samples. The following protocol is an abbreviated form of this procedure with minor modifications. After determination of LOI, 100.0 ± 0.2 mg splits of the ignited whole-rock powders were weighed and mixed with 400.0 ± 0.5 mg of LiBO₂ flux that had been preweighed on shore. Standard rock powders and full procedural blanks were included with unknowns in each ICP-AES run (note that among the elements analyzed, contamination from the tungsten carbide mills is negligible; Shipboard Scientific Party, 2003). All samples and standards were weighed on a microbalance with weighing errors estimated to be ±0.05 mg under relatively smooth sea-surface conditions.

To prevent the cooled bead from sticking to the crucible, 10 mL of 0.172 mM aqueous LiBr solution was added to the mixture of flux and rock powder as a nonwetting agent. Samples were then fused individually in Pt-Au (95:5) crucibles for ~12 min at a maximum temperature of 1050°C in an internally rotating induction furnace (Bead Sampler NT-4100).

After cooling, beads were transferred to high-density polypro-
pylene bottles and dissolved in 50 mL of 10% (by volume) HNO₃,
aided by shaking with a Burrell wrist-action bottle shaker for 1 h.
Following digestion of the bead, the solution was passed through a
0.45 µm filter into a clean 60 mL wide-mouth high-density polypro-
pylene bottle. Next, 1.25 mL of this solution was transferred to a
plastic vial and diluted with 10% HNO₃ to a total volume of 10 mL.
The final solution-to-sample dilution factor was ~4000x.

**Analyses of igneous and metamorphic rocks**

Major (Al, Ca, Fe, K, Mg, Mn, Na, Si, and Ti) and trace (Ba, Co,
Cr, Cu, Sc, Sr, V, Zn, and Zr) element concentrations of standards
and samples were determined with a Leeman ICP-AES instrument.
The plasma was ignited at least 30 min before each run of samples
to allow the instrument to warm up and stabilize.

The ICP-AES data presented in the Geochemistry section of each site chapter were acquired using the Gaussian mode of the Prodigy software. This mode fits a curve to points across a peak and integrates the area under the curve for each element measured. Each sample was analyzed four times from the same dilute solution (i.e., in quadruplicate) within a given sample run. For elements measured at more than one wavelength, we either used the wavelength giving the best calibration line in a given run or, if the calibration lines for more than one wavelength were of similar quality, used the data from all wavelengths and reported the average concentration.

The ICP-AES run included the following:

* Certified rock standards, analyzed twice during each run, cho-
sen to cover a wide range of compositions in order to calibrate
the analyses (peridotite: JP-1; basalt: BIR-1, BHVO-2, and BCR-
2; gabbro: MRG-1; andesite: AGV-1; and granodiorite: JG-1A);

* Samples (unknowns) analyzed in quadruplicate;

* A drift-correcting standard (BHVO-2) analyzed in every eighth sample position and at the beginning and end of each run;

* A blank solution analyzed near the beginning;

* Two or three “check” standards run as unknowns, each also analyzed in quadruplicate; check standards were chosen for their compositions similar to that of the analyzed material (ultra-mafic: DTS-1, basalt: JB-1a, JB-2, felsic rocks: JG-2, JG-3, etc.); and

* A 10% HNO₃ wash solution run for 60 s between each analysis.

**Data reduction**

Following each run of the instrument, the measured raw inten-
sity values were transferred to a data file, corrected for instrument
drift, and then corrected for the procedural blank. Drift correction
was applied to each element by linear interpolation between the
drift-monitoring solutions run in every eighth sample position.

After drift correction and blank subtraction, a calibration line
for each element was calculated using the results for the certified
rock standards. Element concentrations in the samples were then
calculated from the relevant calibration lines.

Individual analyses of both standards and samples produced to-
tal volatile-free major element weight percentages that vary from
100 wt% by as much as several percent. Possible causes include
some combination of errors in weighing the sample (particularly in
rougher seas) and/or flux powders (although even when weighed on
land, weighing errors are possible), variability in the dilutions
(which were done volumetrically), and the duration and relatively
low temperature of ignition. To facilitate comparison of Expedition
367 and 368 results with each other and with data from the litera-
ture, the measured major element values were normalized to 100
wt% totals.

Estimates of accuracy and precision of major and trace element
analyses were based on replicate analyses of check standards com-
pared to values published in Govindaraju (1994) and the GeoReM
database (http://georem.mpch-mainz.gwdg.de) for international
rock standards and to values published in Puchelt et al. (1996). Re-
sults are presented in Table T1. During Expeditions 367 and 368,
run-to-run relative standard deviation by ICP-AES was generally
±1% for major elements except for MgO (±5%) and ±10% for trace
elements. Accuracy was better than 2% for major elements and bet-
ter than 5% for most trace elements, with the exception of low-con-
centration data for Cr and Zr.
# Physical properties

High-resolution physical property measurements were made during Expeditions 367 and 368 mainly to aid lithostratigraphic characterization and to tie core descriptions to borehole data and seismic profiles. In particular, physical property data play a major role in hole-to-hole and site-to-site stratigraphic correlation, detection of discontinuities and inhomogeneities, collection of information about differences in the composition and texture of sediment, identification of major seismic reflectors, and construction of synthetic seismic profiles. A variety of techniques and methods were used to characterize Expedition 367 and 368 cores on whole-round, split section-half, and discrete samples. Core sections are generally 1.5 m in length, so a typical coring length (stroke) of 9.5 m yields six sections plus a shorter seventh section. Procedures for measuring sediment or hard rock cores differed slightly.

## Sedimentary cores

Recovered whole-round sections were first allowed to equilibrate to ambient room temperature (~20°C) and pressure for ~4 h. After thermally equilibrating, core sections were run through the WRMSL for measurement of density by GRA, magnetic susceptibility, and compressional wave velocity on the PWL. Cores recovered with the XCB or the RCB coring systems are slightly smaller in diameter than those cored with the APC system. As a result, sections cored with the XCB or RCB systems typically have gaps between the liner and the core, so P-wave velocity was not measured with the WRMSL. Sections were then measured with the NGRL. Thermal conductivity was measured on one whole-round section per sediment core (typically Section 3) by a needle probe inserted into the section through a small hole drilled through the plastic core liner close to the middle of the section. When the sediment cores were too hard to insert the needle probe, a contact probe was used instead to measure the thermal conductivity later on the section half after core splitting. Cores were split longitudinally, with one half designated as archive and one as working half for sampling and analysis. The archive half of the core was passed through the SHMSL for measurement of point magnetic susceptibility and color reflectance. P-wave velocity measurements on split cores were made on the working halves at least for every section that had been sampled for MAD, or on other sections according to the lithology, employing the transducers oriented in x- and z-axis directions (see directions defined in Figure F23). Discrete samples were collected from the working halves (every other section) to measure wet bulk density, dry bulk density, water content, porosity, and grain density with MAD procedures.

## Hard rock cores

Recovered hard rock sections were shaken onto sterile liners in the core splitting room for examination by a petrologist and/or a structural geologist, who decided where the pieces should be split between working and archive halves. The pieces were then put back into liners and run through the WRMSL and NGRL. P-wave velocity was not measured because the spaces between the liner and the rock core pieces make these measurements meaningless. After physical property measurements on whole-round cores, the core sections were split into working and archive halves and all rock pieces were labeled. The archive half of the core was passed through the SHMSL for measurement of point magnetic susceptibility and color reflectance. Thermal conductivity was measured once per core using a contact probe on a piece of section half in a bath of seawater for igneous rock pieces. Samples were taken from the working

half of the core at a sampling interval of ~1 m depending on lithologic variability. Samples from igneous basement were shared for both paleomagnetic and MAD measurements. P-wave velocity measurements were made on these discrete samples.

A full discussion of all methodologies and calculations used aboard the *JOIDES Resolution* in the Physical Properties Laboratory is available in Blum (1997). Details and procedures for each physical property measurement are described below.

## Whole-Round Multisensor Logger measurements

GRA-derived bulk density, P-wave velocity, and magnetic susceptibility were measured nondestructively with the WRMSL (Figure F25). To optimize the measurement process, sampling intervals and measurement integration times were set to be uniform for all sensors. Sampling intervals were set at 2 cm with an integration time of 5 s for each measurement. These sampling intervals are common denominators of the distances between the sensors installed on the WRMSL (30–50 cm), which allows sequential and simultaneous measurements. After every core, quality assurance/quality control (QA/QC) was monitored by passing a single core liner filled with deionized water through the WRMSL; if deviations from expected values were observed, recalibrations could be conducted if needed.

### GRA bulk density

Bulk density can be used to estimate the pore volume in sediment and evaluate the consolidation state of sediment. GRA density is an estimate of bulk density based on the attenuation of a gamma ray beam. The beam is produced by a ¹³⁷Cs gamma ray source at a radiation level of 370 MBq within a lead shield with a 5 mm collimator that is directed through the whole-round core. The gamma ray detector on the opposite side of the core from the source includes a scintillation detector and an integral photomultiplier tube to record the gamma radiation that passes through the core. The attenuation of gamma rays occurs primarily by Compton scattering, in which gamma rays are scattered by electrons in the formation; the degree of scattering is related to the material bulk density. Therefore, for a known thickness of sample, the density (ρ) is related to the intensity of the attenuated gamma rays and can be expressed as follows:

Figure F25. WRMSL (measures GRA bulk density, magnetic susceptibility, and P-wave velocity), Expeditions 367 and 368. Water standard is measured at end of each core to control measurement quality.

<figure><img src="image_68.png" /></figure>
$$ \rho = \ln(I_0/I)/(\mu d), $$

where

I = the measured intensity of gamma rays passing through the sample,

I₀ = gamma ray source intensity,

μ = Compton attenuation coefficient, and

d = sample diameter.

The μ and I₀ are treated as constants, such that ρ can be calculated from I. Note that this equation differs from the equation (5) in Blum (1997) in order to correct a typo.

In general, WRMSL measurements are most accurate when taken on a completely filled core liner with minimal drilling disturbance; otherwise, measurements tend to underestimate true values. By default, the instrument reports measurements using the internal diameter of the core liner (66 mm) as the assumed sample diameter. This assumption is suitable for most sediment cores obtained by the APC system; however, for sediment and/or hard rock cored by the XCB or RCB systems, core diameter is usually about 58 mm or less. Following Jarrard and Kerneklian (2007), the density measurements of cores obtained by XCB or RCB may be corrected by multiplying the density values by 66/58 = 1.138 to account for this bias. We chose not to correct the raw values but to mention the offset in the description of the measurements. The spatial resolution of the GRA densitometer is less than ±1 cm. The gamma ray detector is calibrated with sealed calibration cores (one standard core liner filled with distilled water and aluminum cylinders of various diameters). To establish the calibration curves, gamma ray counts were taken through each aluminum cylinder for 60 s. Each aluminum cylinder has a density of 2.7 g/cm³, and d is 1, 2, 3, 4, 5, or 6 cm. The relationship between I and μd is

$$ \ln(I) = A(\mu d)^2 + B(\mu d) + C, $$

where A, B, and C are coefficients determined from the calibration.

Recalibration was performed as needed when the deionized water QA/QC standard density deviated significantly (more than a few percent) from 1 g/cm³.

## Magnetic susceptibility

Magnetic susceptibility (χ) is a dimensionless measure of the degree to which a material can be magnetized by an external magnetic field:

$$ \chi = M/H, $$

where M is the magnetization induced in the material by an external field of strength H. Magnetic susceptibility is primarily sensitive to the concentration of ferrimagnetic minerals (e.g., magnetite and maghemite). It is also sensitive to magnetic mineralogy and can be related to the origin of the materials in the core and their subsequent diagenesis. Igneous materials typically have magnetic susceptibility a couple of orders of magnitude greater than their alteration products, such as clay.

The measurements were made using a Bartington MS2C loop sensor with a 9 cm diameter. An oscillator circuit in the sensor, which operates at a frequency of 0.565 kHz and an AF of ~140 A/m, produces a low-intensity, nonsaturating alternating magnetic field. Sediment or hard rock core sections passing through the influence of this field cause a change in oscillator frequency. Frequency information

returned in pulse form to the susceptibility meter is converted into magnetic susceptibility. The loop sensor has a spatial resolution of 23–27 mm, and it is accurate to within 2%.

## P-wave velocity

P-wave velocity data can be used to evaluate small-strain moduli, correlate downhole logging and core data, and evaluate porosity and cementation. P-wave (compressional) velocity (Vp) is defined by the time required for a compressional wave to travel a specific distance:

$$ V_p = d/t_{core}, $$

where d is the path length of the wave across the core and tcore is the traveltime through the core.

The PWL measures the traveltime of 500 kHz ultrasonic waves horizontally across the core at 2 cm intervals while it remains in the core liner. Waves are transmitted to the core by plastic transducer contacts connected to linear actuators. Pressure is applied to the actuators to ensure coupling between the transducers and the core liner. P-wave velocity transducers measure total traveltime of the compressional wave between transducers. The wave travels horizontally across the whole core and core liner. The total observed traveltime, tcore, is composed of

tdelay = time delay related to transducer faces and electronic circuitry,

tpulse = delay related to the peak detection procedure,

tliner = transit time through the core liner, and

tcore = traveltime through the sediment.

The system is calibrated using a core liner filled with distilled water, which provides control for tdelay, tpulse, and tliner. From these calibrations, Vp can be calculated for the whole-round specimens in core liners as

$$ V_p = (d_{cl} - 2d_{liner})/(t_o - t_{pulse} - t_{delay} - 2t_{liner}), $$

where

dcl = measured diameter of core and liner,

dliner = liner wall thickness, and

to = measured total traveltime.

The above equation assumes that the core completely fills the core liner. The PWL of the WRMSL was turned off for cores recovered with the XCB and RCB systems, which often do not fill the core liner.

## Natural Gamma Radiation Logger measurements

Gamma radiation is emitted from the decay of mineral-hosted ²³⁸U, ²³²Th, and ⁴⁰K. The NGRL measures this natural emission on whole-round cores using a system designed and built at the Integrated Ocean Drilling Program US Implementing Organization (USIO) (Texas A&M University) (Vasiliev et al., 2011; Dunlea et al., 2013) (Figure F26). When ²³⁸U, ²³²Th, and ⁴⁰K radioisotopes decay, they and their daughter products emit gamma radiation at specific energy levels unique to each isotope. NGR spectroscopy measures a wide energy spectrum that can be used to estimate the abundance of each isotope based on the strength of the signal at characteristic energies (Blum, 1997; Gilmore, 2008). Spectral data were collected and can be used for postcruise processing for U, Th, and K abundance. We estimated concentrations of K, U, and Th using NGR and
Figure F26. NGRL for whole-round cores (conducts 8 measurements at a time in 2 positions, resulting in 16 measurements per core), Expedition 367 and 368. During Expedition 367, scintillation Detector 7 was deficient, so only 14 measurements per core were performed.

<figure><img src="image_69.png" /></figure>

bulk density measurements (see Figure F26), based on a study and Matlab scripts from De Vleeschouwer et al. (2017). High total counts usually identify fine-grained deposits containing K-rich clay minerals and their absorbed U and Th isotopes. NGR data thus reveal stratigraphic details that aid in core-to-core correlations. The system was initially installed on the renovated *JOIDES Resolution* in 2009 and has been used during every Integrated Ocean Drilling Program USIO and IODP *JOIDES Resolution* Science Operator (JRSO) expedition starting with Expedition 320. The main NGR detector unit consists of 8 sodium iodide (NaI) detectors arranged along the core measurement axis at 20 cm intervals surrounding the lower half of the section (Figure F27). During Expedition 367, scintillation Detector 7 was deficient, which led to a small gap in the measurements. Before Expedition 368, the deficient scintillation detector was fixed by the IODP technicians, and all detectors performed well during Expedition 368. The detector array has passive (layers of lead) and active (plastic scintillometers) shielding to reduce the background environmental and cosmic radiation. The overlying plastic scintillometers detect incoming high-energy gamma and muon cosmic radiation and cancel this signal from the total counted by the NaI detectors.

A measurement run consisted of two sample positions, 10 cm apart, for a total of 16 (14 during Expedition 367) measurements per 150 cm section. During Expedition 367, measurements at distances of 20 and 30 cm in each section have no measured values because of the scintillation detector failure. The quality of the energy spectrum measured in a core depends on the concentration of radionuclides in the sample but also on the counting time, with higher times yielding better spectra. Counting times were chosen as 5 min per position, or ~10 min per core, yielding statistically significant energy spectra (Vasiliev et al., 2011).

## Thermal conductivity measurements

After NGR measurements were completed, thermal conductivity was measured with the TK-04 (Teka Bolin) system using a needle-probe method in full-space configuration for whole-round sediment cores (Von Herzen and Maxwell, 1959) or a contact-probe method in half-space configuration on split cores for hard rock. The probes contain a heater wire and calibrated thermistor.

Figure F27. NGRL detectors (from Vasiliev et al., 2011), Expeditions 367 and 368. The main NGR scintillation detector unit consists of 8 sodium iodide (NaI) scintillometers arranged along core measurement axis at 20 cm intervals surrounding the lower half of the core section.

<figure><img src="image_70.png" /></figure>

For soft sediment, the needle probe was inserted into a 2 mm diameter hole drilled through the liner along one of the lines that later guided core splitting. To avoid interference from air flow in the laboratory, the core was placed into an enclosed box outfitted with foam.

For hard rock cores, samples were selected from the working half and returned unaltered to the core liner upon completion of the measurements. The contact probe embedded in the surface of an epoxy block with a low thermal conductivity (Vacquier, 1985) was maintained in contact with the sample. For igneous rock pieces, both rock and probe were equilibrated together in a bath of seawater at room temperature in a cooler insulated with extruded polystyrene foam. The calibrated heat source of the probe was then turned on, and the increase in temperature was recorded over 80 s. A heating power of 1.5 to 1.8 W/m was typically used in soft sediment and for indurated material. In cases when this heating power did not lead to reliable measurements, we used a higher value, up to 2.0 W/m. The solution to the heat conduction equation with a line source of heat was then fit to the temperature measurements to obtain the thermal conductivity. Because the probe is much more conductive than sediment or hard rock, the probe is assumed to be a perfect conductor. Under this assumption, the temperature of the superconductive probe has a linear relationship with the natural logarithm of the time after the initiation of the heat:

$$T(t) = (q/4\pi k) \times \ln(t) + C,$$

where

$T$ = temperature (K),

$q$ = heat input per unit length per unit time (J/m/s),

$k$ = thermal conductivity (W/[m·K]),

$t$ = time after the initiation of the heat (s), and

$C$ = instrumental constant.

Three measuring cycles were automatically performed to calculate average conductivity. A self-test, which included a drift study, was conducted at the beginning of each measurement cycle. Once the probe temperature stabilized, the heater circuit was closed and the temperature rise in the probe was recorded. Thermal conductivity was calculated from the rate of temperature rise while the heater current was flowing. Temperatures measured during the first 80 s of
the heating cycle were fitted to an approximate solution of a con-
stantly heated line source (for details, see Kristiansen, 1982; Blum,
1997). Measurement errors were 5%–10%. Thermal conductivity
measurements were routinely taken in one section per core (usually
the third section of each core). Some cores retrieved by the XCB
system did not yield results for thermal conductivity because cracks
in the hard sediment caused bad coupling of the probe to the sedi-
ment.

## Section Half Multisensor Logger measurements

We measured color reflectance and magnetic susceptibility on
archive section halves using the SHMSL. The archive half of the
split core was placed on the core holder, above which an electronic
platform moves along a track, recording the height of the split-core
surface with a laser sensor. The laser establishes the location of the
bottom of the section, and then the platform reverses the direction
of movement, moving from bottom to top making measurements of
point magnetic susceptibility and color reflectance. All foam inserts
were removed from the section-half cores before measurement, so
the measured range of values represents that of the core material
only. During Expeditions 367 and 368, point magnetic susceptibility
and color reflectance data were collected at constant intervals for
each core but varied between 0.5 and 2.0 cm for different cores, de-
pending on the available time for processing and the type of rock
recovered. These measurements have a sufficient resolution for
comparing with the results obtained from the magnetic susceptibil-
ity loop of the WRMSL.

## Color reflectance spectrometry

The color reflectance spectrometer uses an Ocean Optics 30
mm integrating sphere and both halogen and LED light sources,
which cover wavelengths from ultraviolet through visible to near in-
frared. The measurements were taken from 380 to 900 nm wave-
lengths at 2 nm intervals. The approximate 3 s data acquisition
offset was applied for the entire scan of the archive section half. The
data are reported using the L*a*b* color system, in which L* is light-
ness, a* is redness (positive) versus greenness (negative), and b* is
yellowness (positive) versus blueness (negative) of the rock. The
color reflectance spectrometer calibrates on two spectra, pure white
(reference) and pure black (dark). Color calibration was conducted
automatically approximately once every 6 h (twice per shift).

## Point magnetic susceptibility

Point magnetic susceptibility was measured with a Bartington
MS2 meter and an MS2K contact probe with a flat 15 mm diameter
round sensor with a field of influence of 25 mm and an operation
frequency of 930 Hz. The instrument averages three measurements
from the sensor for each offset, leading to an accuracy of ~5%. The
spatial resolution of the point magnetic susceptibility instrument is
~3.8 mm, higher than that of the whole-round magnetic susceptibil-
ity (23–27 mm), making it especially useful for sections containing
broken pieces <4 cm in length. As with whole-round measure-
ments, the output displayed by the point magnetic susceptibility
sensor must be converted to dimensionless SI units by multiplying
by 10⁻⁵. The probe is zeroed in air before each measurement loca-
tion to avoid influence from the metal track. The point magnetic
susceptibility meter was calibrated by the manufacturer before in-
stallation on the ship and is quality checked every ~6 h at the same
time as color reflectance sensor calibration.

<figure><img src="image_71.png" /><figcaption>Figure F28. SHMG showing x-axis caliper and y- and z-axis bayonets used to measure P-wave velocity on split core sections of soft sediments or discrete samples of indurated sediment or hard rock, Expeditions 367 and 368. Insert shows measurement of P-wave velocity on a hard rock discrete sample using x-axis caliper.</figcaption></figure>

## Section Half Measurement Gantry measurements

For soft-sediment cores, *P*-wave velocity measurements were
performed on the working half of split cores before any samples
were taken. *P*-wave velocity measurements used the *x*-axis caliper
and *z*-axis bayonet contact probe transducers on the Section Half
Measurement Gantry (SHMG) (Figure F28) with one analysis com-
pleted every other section. Measurements were usually taken at ~75
cm in the section; however, if this interval lacked good sedi-
ment/transducer coupling (e.g., caused by high amounts of sand or
cracks), different positions were chosen to generate viable data.
Cores drilled with the XCB sometimes did not provide usable data
because of bad sediment/liner contact and disturbed sediment. For
hard rock cores, *P*-wave velocity was measured on the discrete sam-
ples chosen for both physical property and paleomagnetic measure-
ments.

### P-wave velocity

The *P*-wave velocity system uses Panametrics-NDT Microscan
delay line transducers, which transmit at 0.5 MHz. The signal re-
ceived through the section half or the discrete sample was recorded
by the computer attached to the system, with the peak (*P*-wave ar-
rival) usually chosen by autopicking software. In case of a weak sig-
nal, the first arrival was manually picked. The distance between
transducers was measured with a built-in linear voltage displace-
ment transformer. Calibration was performed with a series of
acrylic cylinders of differing thicknesses and a known *P*-wave veloc-
ity of 2750 ± 20 m/s. The determined system time delay from cali-
bration was subtracted from the picked arrival time to give a
traveltime of the *P*-wave through the sample. The thickness of the
sample (calculated by the linear voltage displacement transformer,
in meters) was divided by the traveltime (in seconds) to calculate *P*-
wave velocity in meters per second.

## Discrete sample MAD measurements

Discrete samples were collected from the working halves to de-
termine wet and dry bulk density, grain density, water content, and
porosity. In soft sediment, samples of ~10 cm³ volume were collected with a plastic syringe, the diameter of which fits that of the glass vials. We sampled every other section of core (usually Sections 1, 3, and 5). In indurated sediment and hard rock, minicores or pieces were extracted from the working halves for physical property measurements. Samples from igneous basement were shared for paleomagnetic measurements.

## Sample preparation

Soft-sediment samples were placed in numbered, preweighed ~16 mL Wheaton glass vials for wet and dry sediment weighing, drying, and dry volume measurements. Determination of an accurate wet mass of the minicore samples of indurated sediment and hard rock first required that the pore space of the samples be completely saturated with seawater. To do this, we placed the samples in individual plastic vials filled with seawater and used a vacuum chamber. A vacuum pump removed the air from the chamber to a pressure of ~40–50 kPa below the atmospheric pressure, forcing seawater into the samples. The samples were kept under saturation for at least 24 h, with the vacuum maintained in the chamber by turning the pump on for 30 min every 5 h. After removal from the saturator, the minicores were patted dry with a paper towel, and wet mass was immediately determined using the dual balance system. P-wave velocities were then measured on the wet samples. Following the velocity measurements, the samples were dried in a convection oven for at least 24 h at 105° ± 5°C. Dried samples were then cooled in a desiccator for at least 4 h before the dry mass and the volume were measured.

## Dual balance mass measurement

The weights of wet and dry sample masses were determined to a precision of 0.005 g using two Mettler Toledo electronic balances, with one acting as a reference. A standard weight of similar value to the sample was placed upon the reference balance to increase accuracy. A computer averaging system was used to compensate for the ship’s motion. The default setting of the balances is 300 measurements (taking ~1.5 min).

## Pycnometer volume measurement

Dry sample volume was determined using a hexapycnometer system of a six-celled, custom-configured Micrometrics AccuPyc 1330TC helium-displacement pycnometer (Figure F29). The precision of each cell is 1% of the full-scale volume. Volume measurement was preceded by three purges of the sample chamber with helium warmed to ~28°C. Three measurement cycles were run for each sample. A reference volume (a set of two calibration spheres) was placed sequentially in one of the chambers to check for instrument drift and systematic error. The volumes occupied by the numbered Wheaton vials were calculated before the cruise by multiplying each vial’s weight against the average density of the vial glass. The procedures for the determination of these physical properties comply with the American Society for Testing and Materials (ASTM) designation (D) 2216 (ASTM International, 1990). The fundamental relation and assumptions for the calculations of all physical property parameters are discussed by Blum (1997) and summarized below.

## Mass and volume calculation

We measured wet mass ($M_{wet}$), dry mass ($M_{dry}$), and dry volume ($V_{dry}$). The ratio of mass (rm) is a computational constant of 0.965 (i.e., 0.965 g of freshwater per 1 g of seawater). Salt precipitated in

<figure><img src="image_72.png" /><figcaption>Figure F29. Pycnometer used to measure volume of dry samples, either in small vials for soft sediments or as discrete samples, Expeditions 367 and 368.</figcaption></figure>

sediment pores during the drying process is included in the $M_{dry}$ and $V_{dry}$ values. The mass of the evaporated water ($M_{water}$) and salt ($M_{salt}$) in the sample are given by

$$M_{water} = M_{wet} - M_{dry} \text{ and}$$

$$M_{salt} = M_{water}[s/(1 - s)],$$

where s is the assumed saltwater salinity (0.035%) corresponding to a pore water density ($\rho_{pw}$) of 1.024 g/cm³ and a salt density ($\rho_{salt}$) of 2.22 g/cm³. The corrected mass of pore water ($M_{pw}$), volume of pore water ($V_{pw}$), mass of solids excluding salt ($M_{solid}$), volume of salt ($V_{salt}$), volume of solids excluding salt ($V_{solid}$), and wet volume ($V_{wet}$) are

$$M_{pw} = (M_{wet} - M_{dry})/rm,$$

$$V_{pw} = M_{pw}/\rho_{pw},$$

$$M_{solid} = M_{wet} - M_{pw},$$

$$M_{salt} = M_{pw} - (M_{wet} - M_{dry}),$$

$$V_{salt} = M_{salt}/\rho_{salt},$$

$$V_{wet} = V_{dry} - V_{salt} + V_{pw}, \text{ and}$$

$$V_{solid} = V_{wet} - V_{pw}.$$

## Calculation of bulk properties

For all sediment samples, water content (w) is expressed as the ratio of mass of pore water to wet sediment (total) mass:

$$w = M_{pw}/M_{wet}.$$

Wet bulk density ($\rho_{wet}$), dry bulk density ($\rho_{dry}$), sediment grain density ($\rho_{solid}$), porosity ($\phi$), and void ratio ($VR$) are calculated as follows:
$$\rho_{\text{wet}} = M_{\text{wet}}/V_{\text{wet}},$$

$$\rho_{\text{dry}} = M_{\text{solid}}/V_{\text{solid}},$$

$$\rho_{\text{solid}} = M_{\text{solid}}/V_{\text{solid}},$$

$$\phi = V_{\text{pw}}/V_{\text{wet}}, \text{ and}$$

$$VR = V_{\text{pw}}/V_{\text{solid}}.$$

MAD properties reported and plotted in the Physical properties sections of all site chapters were calculated with the MADMax shipboard program set with the “method C” calculation process.

## Downhole measurements

Downhole logs are used to determine physical, chemical, and structural properties of the formation penetrated by a borehole. The data are rapidly collected, continuous with depth, and measured in situ; they can be interpreted in terms of the stratigraphy, lithology, mineralogy, magnetic characteristics, and geochemical composition of the penetrated formation. Where core recovery is incomplete or disturbed, log data may provide the only way to characterize the borehole section. Where core recovery is good, log and core data complement one another and may be interpreted jointly.

Downhole logs measure formation properties on a scale that is intermediate between those obtained from laboratory measurements on core samples and those from geophysical surveys. They are useful in calibrating the interpretation of geophysical survey data (e.g., through the use of synthetic seismograms) and provide a necessary link for the integrated understanding of physical and chemical properties on different scales.

During Expeditions 367 and 368, downhole wireline log data was collected at Sites U1499–U1501, and U1503. In addition, a total of 14 downhole temperature measurements were acquired using the APCT-3 in Holes U1499A (6), U1501C (4), and U1505C (4).

## Wireline logging

During wireline logging operations, logs were recorded with Schlumberger logging tools combined into several tool strings that were lowered into the hole after completion of coring operations. Three standard IODP tool string configurations were used during Expeditions 367 and 368 (Figure F30; Table T8). The first was a variant of the triple combo tool string, which measures borehole fluid temperature, NGR, porosity, density, electrical resistivity, and magnetic susceptibility. The second was the FMS-sonic tool string, which measures NGR, sonic velocity, and FMS resistivity images of the borehole wall. The third was the Versatile Seismic Imager (VSI) tool string, which measures a vertical seismic profile in order to integrate well and seismic data. Each tool string also contains an Enhanced Digital Telemetry Cartridge (EDTC) for communicating through the wireline to the Schlumberger data acquisition system (i.e., multitasking acquisition and imaging system [MAXIS]) on the drillship. See the site chapters for detailed lists of which tools were run in which combinations in each hole.

In preparation for logging, the boreholes were reamed in their lower sections, flushed of debris by circulating drilling fluid, and filled with seawater-based logging gel (i.e., sepiolite mud mixed with seawater and weighted with barite; approximate density = 10.5 lb/gal) to help stabilize the borehole walls in sections where instability would be expected based on drilling and coring results. The

BHA was pulled up to a logging depth determined by the borehole conditions. Although log data can be collected while lowering the tool string to the bottom of the hole, the primary data set is collected while raising the tool strings upward at a constant speed, typically ~300 m/h for the triple combo and 600 m/h for the FMS-sonic.

Each tool string deployment is termed a logging “run.” During each run, tool strings can be lowered and pulled up in the hole several times to check repeatability and increase coverage of the FMS borehole images. Each lowering or hauling-up of the tool string while collecting data constitutes a “pass.” Incoming data were recorded and monitored in real time on the Schlumberger Minimum Configuration MAXIS logging computer. A wireline heave compensator (WHC) was typically used to minimize the effect of ship’s heave on the tool position in the borehole (see below).

## Logged sediment properties and tool measurement principles

The logged properties and the principles used with the tools that measure them are briefly described below. The main tools are listed in Tables T8 and T9. More detailed information on individual tools and their geological applications may be found in Serra (1984, 1986, 1989), Schlumberger (1989, 1994), Rider (1996), Goldberg (1997), Lovell et al. (1998), and Ellis and Singer (2007). A complete list of acronyms for the Schlumberger tools and measurement curves is available at http://www.apps.slb.com/cmd. The complete list of downhole logging tools used during Integrated Ocean Drilling Program and IODP expeditions and additional information about tool physics are available at http://iodp.ldeo.columbia.edu/TOOLS_LABS/tools.html and http://iodp.tamu.edu/tools/logging/index.html.

## Natural gamma radiation

The Hostile Environment Natural Gamma Ray Sonde (HNGS) was used on both the triple combo and FMS-sonic tool strings to measure NGR in the formation. The HNGS uses two bismuth germanate scintillation detectors and five-window spectroscopy to determine concentrations of potassium (in weight percent), thorium (in parts per million), and uranium (in parts per million) from the characteristic gamma ray energies of isotopes in the $^{40}$K, $^{232}$Th, and $^{238}$U radioactive decay series, which dominate the natural radiation spectrum. The computation of the elemental abundances uses a least-squares method of extracting U, Th, and K elemental concentrations from the spectral measurements. The HNGS filters out gamma ray energies below 500 keV, eliminating sensitivity to bentonite or KCl in the drilling mud and improving measurement accuracy. The HNGS also provides a measure of the total spectral gamma ray (HSGR) and computed gamma ray (HCGR) that are measured in American Petroleum Institute gamma radiation units (gAPI). The HNGS response is influenced by the borehole diameter; therefore, the HNGS data are corrected for borehole diameter variations during acquisition.

An additional NGR sensor was housed in the EDTC to communicate data to the surface. The sensor includes a sodium iodide scintillation detector that also measures the total NGR emission of the formation. It is not a spectral tool (i.e., it does not provide U, Th, and K concentrations), but it provides total gamma radiation for each pass.

The inclusion of the HNGS in every tool string allows use of the gamma ray data for precise depth match processing between logging strings and passes and for core-log integration.
Figure F30. Wireline tool strings, Expeditions 367 and 368. Triple combo tool string takes downhole measurements of hole diameter, NGR, bulk density, electrical resistivity, and magnetic susceptibility of the borehole. FMS-sonic tool string measures borehole resistivity images, NGR, and P- and S-wave velocities. VSI tool string acquires seismic waveform data in a check shot experiment. LEH-MT = logging equipment head-mud temperature, EDTC = Enhanced Digital Telemetry Cartridge, HNGS = Hostile Environment Natural Gamma Ray Sonde, APS = Accelerator Porosity Sonde, HLDS = Hostile Environment Litho-Density Sonde, HRLA = High-Resolution Laterolog Array, MSS = magnetic susceptibility sonde, DSI = Dipole Sonic Imager, GPIT = General Purpose Inclinometry Tool. Except for MSS, all acronyms are trademarks of Schlumberger. Also see Tables T8 and T9.

<figure><img src="image_73.png" /></figure>

## Density and photoelectric factor

Formation density was measured with the Hostile Environment Litho-Density Sonde (HLDS). The sonde contains a radioactive cesium (¹³⁷Cs) gamma ray source (622 keV) and far and near gamma ray detectors mounted on a shielded skid that is pressed against the borehole wall by a hydraulically activated decentralizing arm. Gamma radiation emitted by the source undergoes Compton scattering, in which gamma rays are scattered by electrons in the formation. The number of scattered gamma rays that reach the detectors is proportional to the density of electrons in the formation, which is

in turn related to bulk density. Porosity may also be derived from this bulk density if the matrix (grain) density is known.

The HLDS also measures the photoelectric effect factor (PEF), a measure of the photoelectric absorption of low-energy gamma radiation. Photoelectric absorption occurs when the energy of the gamma rays falls below 150 keV as a result of being repeatedly scattered by electrons in the formation. PEF is determined by comparing the counts from the far detector in the high-energy region, where only Compton scattering occurs, to those in the low-energy region, where count rates depend on both reactions. Because PEF
<table><caption>Table T8. Downhole measurements made by wireline tool strings, Expeditions 367 and 368. For definitions of tool acronyms, see Table T9. All tool and tool string names except the MSS are trademarks of Schlumberger. **Download table in CSV format.**</caption><thead><tr><th>Tool string</th><th>Tool</th><th>Measurement</th><th>Sampling interval (cm)</th><th>Approximate vertical resolution (cm)</th></tr></thead><tbody><tr><td rowspan="6">Triple combo</td><td>EDTC</td><td>Total gamma ray</td><td>5 and 15</td><td>30</td></tr><tr><td>HNGS</td><td>Spectral gamma ray</td><td>15</td><td>20–30</td></tr><tr><td>APS</td><td>Porosity</td><td>15</td><td>38</td></tr><tr><td>HLDS</td><td>Bulk density and caliper</td><td>2.5 and 15</td><td>38</td></tr><tr><td>HRLA</td><td>Resistivity</td><td>15</td><td>30</td></tr><tr><td>MSS</td><td>Magnetic susceptibility</td><td>4</td><td>12–36</td></tr><tr><td rowspan="4">FMS-sonic</td><td>EDTC</td><td>Total gamma ray</td><td>5 and 15</td><td>30</td></tr><tr><td>GPIT</td><td>Tool orientation and acceleration</td><td>3.8</td><td>15</td></tr><tr><td>DSI</td><td>Acoustic velocity</td><td>15</td><td>107</td></tr><tr><td>FMS</td><td>Microresistivity and caliper</td><td>0.25</td><td>1</td></tr></tbody></table>

<table><caption>Table T9. Acronyms and units used for downhole wireline tools and measurements, Expeditions 367 and 368. For the complete list of acronyms used in IODP and for additional information about tool physics, consult IODP-USIO Science Services, LDEO, at http://iodp.ldeo.columbia.edu/TOOLS_LABS/tools.html. **Download table in CSV format.**</caption><thead><tr><th>Tool</th><th>Output</th><th>Description</th><th>Unit</th></tr></thead><tbody><tr><td>EDTC</td><td></td><td>Enhanced Digital Telemetry Cartridge</td><td></td></tr><tr><td></td><td>GR</td><td>Total gamma ray</td><td>gAPI</td></tr><tr><td></td><td>ECGR</td><td>Environmentally-corrected gamma ray</td><td>gAPI</td></tr><tr><td></td><td>EHGR</td><td>High-resolution environmentally corrected gamma ray</td><td>gAPI</td></tr><tr><td>HNGS</td><td></td><td>Hostile Environment Gamma Ray Sonde</td><td></td></tr><tr><td></td><td>HSGR</td><td>Standard (total) gamma ray</td><td>gAPI</td></tr><tr><td></td><td>HCGR</td><td>Computed gamma ray (HSGR minus uranium contribution)</td><td>gAPI</td></tr><tr><td></td><td>HFK</td><td>Potassium</td><td>wt%</td></tr><tr><td></td><td>HTHO</td><td>Thorium</td><td>PPM</td></tr><tr><td></td><td>HURA</td><td>Uranium</td><td>PPM</td></tr><tr><td>APS</td><td></td><td>Accelerator Porosity Sonde</td><td></td></tr><tr><td></td><td>APLC</td><td>Near/array limestone corrected porosity</td><td>Dec. fraction</td></tr><tr><td></td><td>STOF</td><td>Computed standoff</td><td>Inches</td></tr><tr><td></td><td>SIGF</td><td>Formation capture cross section</td><td>Capture units</td></tr><tr><td>HLDS</td><td></td><td>Hostile Environment Litho-Density Sonde</td><td></td></tr><tr><td></td><td>RHOM</td><td>Bulk density</td><td>g/cm³</td></tr><tr><td></td><td>PEFL</td><td>Photoelectric effect</td><td>barn/e⁻</td></tr><tr><td></td><td>LCAL</td><td>Caliper (measure of borehole diameter)</td><td>Inches</td></tr><tr><td></td><td>DRH</td><td>Bulk density correction</td><td>g/cm³</td></tr><tr><td>HRLA</td><td></td><td>High Resolution Laterolog Array Tool</td><td></td></tr><tr><td></td><td>RLA1-5</td><td>Apparent Resistivity from Computed Focusing Mode 1-5</td><td>Ωm</td></tr><tr><td></td><td>RT</td><td>True resistivity</td><td>Ωm</td></tr><tr><td></td><td>MRES</td><td>Borehole fluid resistivity</td><td>Ωm</td></tr><tr><td>MSS</td><td></td><td>Magnetic susceptibility sonde</td><td></td></tr><tr><td></td><td>LSUS</td><td>Magnetic susceptibility, deep reading</td><td>Uncalibrated units</td></tr><tr><td>FMS</td><td></td><td>Formation MicroScanner</td><td></td></tr><tr><td></td><td>C1, C2</td><td>Orthogonal hole diameters</td><td>Inches</td></tr><tr><td></td><td>P1AZ</td><td>Pad 1 azimuth</td><td>°</td></tr><tr><td></td><td></td><td>Spatially oriented resistivity images of borehole wall</td><td></td></tr><tr><td>GPIT</td><td></td><td>General-purpose inclinometer tool</td><td></td></tr><tr><td></td><td>DEVI</td><td>Hole deviation</td><td>°</td></tr><tr><td></td><td>HAZI</td><td>Hole azimuth</td><td>°</td></tr><tr><td></td><td>Fₓ, Fᵧ, F_z</td><td>Earth's magnetic field (three orthogonal components)</td><td>°</td></tr><tr><td></td><td>Aₓ, Aᵧ, A_z</td><td>Acceleration (three orthogonal components)</td><td>m/s²</td></tr><tr><td>DSI</td><td></td><td>Dipole Sonic Imager</td><td></td></tr><tr><td></td><td>DTCO</td><td>Compressional wave slowness</td><td>µs/ft</td></tr><tr><td></td><td>DTSM</td><td>Shear wave slowness</td><td>µs/ft</td></tr><tr><td></td><td>DT1</td><td>Shear wave slowness, lower dipole</td><td>µs/ft</td></tr><tr><td></td><td>DT2</td><td>Shear wave slowness, upper dipole</td><td>µs/ft</td></tr></tbody></table>

depends on the atomic number of the elements in the formation (heavier elements have higher PEF), it also varies according to the chemical composition of the minerals present and can be used for the identification of the overall mineral makeup of the formation. For example, the PEF of calcite is 5.08 barn/e⁻, illite is 3.03 barn/e⁻,

quartz is 1.81 barn/e⁻, and hematite is 21 barn/e⁻. Good contact between the tool and the borehole wall is essential for good HLDS logs; poor contact results in underestimation of density values. Both the density correction and caliper measurement of the hole are used to check the contact quality. In the deeper parts of the hole, the PEF
log should be used with caution, especially in washouts, because barium in the logging mud swamps the signal despite correction for mud effect.

## Electrical resistivity

The High-Resolution Laterolog Array (HRLA) provides six resistivity measurements with different depths of investigation (including the borehole or mud resistivity and five measurements of formation resistivity with increasing penetration into the formation). The tool sends a focused current into the formation and measures the intensity necessary to maintain a constant drop in voltage across a fixed interval, providing direct resistivity measurements. The array has one central (source) electrode and six electrodes above and below it, which serve alternatively as focusing and returning current electrodes. By rapidly changing the role of these electrodes, a simultaneous resistivity measurement at six penetration depths is achieved. The tool is designed to ensure that all signals are measured at exactly the same time and tool position and to reduce the sensitivity to “shoulder bed” effects when crossing sharp beds thinner than the electrode spacing. The design of the HRLA, which eliminates the need for a surface reference electrode, improves formation resistivity evaluation compared to traditional dual induction and allows the full range of resistivity to be measured from low (e.g., in high-porosity sediments) to high (e.g., in basalt). The HRLA needs to be run centralized in the borehole for optimal results, so knuckle joints were used to centralize the HRLA while allowing the density and porosity tools to maintain good contact with the borehole wall (Figure F30).

Calcite, silica, and hydrocarbons are electrical insulators, whereas ionic solutions like interstitial water are conductors. Electrical resistivity, therefore, can be used to evaluate porosity for a given salinity and resistivity of the interstitial water. Clay surface conduction also contributes to the resistivity values, but at high porosities, this effect is relatively minor.

## Acoustic velocity

The Dipole Shear Sonic Imager (DSI) measures the transit times between sonic transmitters and an array of eight receivers. It combines replicate measurements, thus providing a direct measurement of sound velocity through formations that is relatively free from the effects of formation damage and an enlarged borehole (Schlumberger, 1989). Along with the monopole transmitters found on most sonic tools, it also has two crossed-dipole transmitters that allow the measurement of shear wave velocity in addition to compressional wave velocity. Dipole measurements are necessary to measure shear velocities in slow formations with shear velocity less than the velocity of sound in the borehole fluid. Such slow formations are typically encountered in deep-ocean drilling.

## Formation MicroScanner

The FMS provides high-resolution electrical resistivity-based images of borehole walls. The tool has four orthogonal arms and pads, each containing 16 button electrodes that are pressed against the borehole wall during logging (Figure F30). The electrodes are arranged in two diagonally offset rows of 8 electrodes each. A focused current is emitted from the button electrodes into the formation, with a return electrode near the top of the tool. Resistivity of the formation at the button electrodes is derived from the intensity of current passing through the button electrodes.

Processing transforms the resistivity measurements into oriented high-resolution images that reveal geologic structures of the

borehole wall. Features such as bedding, stratification, fracturing, slump folding, and bioturbation can be resolved (Luthi, 1990; Salimullah and Stow, 1992; Lovell et al., 1998). Because the images are oriented to magnetic north, further analysis can provide measurement of the dip and direction (azimuth) of planar features in the formation. In addition, when the corresponding planar features can be identified in the recovered core samples, individual core pieces can be reoriented with respect to true north.

Approximately 30% of a borehole with a diameter of 25 cm (9% inches) is imaged during a single pass. Standard procedure is to make two full upward passes with the FMS to maximize the chance of getting full borehole coverage with the pads. The maximum extension of the caliper arms is 40.6 cm (16 inches). In holes with a diameter greater than this maximum, the pad contact at the end of the caliper arms is inconsistent, and the FMS images may appear out of focus and too conductive. Irregular (rough) borehole walls will also adversely affect the images if contact with the wall is poor.

## Magnetic susceptibility

The magnetic susceptibility sonde (MSS) is a nonstandard wireline tool designed by the Lamont-Doherty Earth Observatory (LDEO). It measures the ease with which formations are magnetized when subjected to a magnetic field. The ease of magnetization is ultimately related to the concentration and composition (size, shape, and mineralogy) of magnetic minerals (principally magnetite) in the formation. These measurements provide one of the best methods for investigating stratigraphic changes in mineralogy and lithology because the measurement is quick, repeatable, and nondestructive and because different lithologies often have strongly contrasting susceptibilities.

The MSS dual-coil sensor provides ~40 cm resolution measurements, with ~20 cm depth of horizontal investigation. The MSS was run as the lowermost tool in the triple combo tool string using a specially developed data translation cartridge to enable the MSS to be run in combination with the Schlumberger tools. The MSS also has an optional single-coil sensor to provide high-resolution measurements (~10 cm), but this sensor was not used during Expeditions 367 and 368 because it has a large bowspring that requires the MSS to be run higher up in the tool string and because it is very sensitive to separation from the borehole wall.

Magnetic susceptibility data from both the high-resolution and deep-reading sensors are plotted as uncalibrated units. The MSS reading responses are affected by temperature and borehole size (higher temperatures lead to higher susceptibility measurements). Preliminary processing was performed offshore to remove the temperature drift by calculating a least-squares polynomial fit to the data and subtracting the calculated trend from the data set. When the magnetic susceptibility signal in sediment is very low, the detection limits of the tool may be reached. For quality control and environmental correction, the MSS also measures internal tool temperature, z-axis acceleration, and low-resolution borehole conductivity.

## Acceleration and inclinometry

The General Purpose Inclinometry Tool (GPIT) was included in the FMS-sonic tool string to calculate tool acceleration and orientation during logging. Tool orientation is defined by three parameters: tool deviation, tool azimuth, and relative bearing. The GPIT utilizes a three-axis inclinometer and a three-axis fluxgate magnetometer to record the orientation of the FMS as the magnetometer records the magnetic field components (Fx, Fy, and Fz). Thus, the FMS im-
ages can be corrected for irregular tool motion, and the dip and di-
rection (azimuth) of features in the FMS image can be determined.

Versatile Seismic Imager

Borehole seismic tools are used in wells to detect the acoustic
signal generated at the surface. The VSI is used to determine the
time-depth relation and to produce a zero-offset vertical seismic
profile and/or check shots in the borehole. The VSI (Figure F30)
uses three-axis single sensor seismic hardware and software and ad-
vanced wireline telemetry for efficient data delivery from the bore-
hole to the surface. Each sensor package delivers high-fidelity wave
fields through the use of a three-axis geophone accelerometer that is
acoustically isolated from the main body of the tool (Figure F30).
The geophone accelerometer detects particle motion and provides a
linear and flat response from 3 to 200 Hz. The VSI maximal opera-
tional temperature is 177°C, or 350°F.

During Expeditions 367 and 368, the VSI was anchored against
the borehole wall or the casing at ~50 m intervals, and 5–10 record-
ings were typically taken at each station. The recorded waveforms
were stacked, and a one-way traveltime was determined from the
first breaks for each station. The seismic source was a Sercel G-gun
parallel cluster composed of two 250 inch³ air guns separated by 1
m. It was positioned by one of the ship cranes off the port side of the
ship at a total horizontal offset of ~30 m from the top of the well-
head and was maintained at a fixed water depth (typically between 2
and 7 m; see Figure F50 in the Site U1500 chapter [Stock et al.,
2018]).

Log data quality

The main influence on log data quality is the condition of the
borehole wall. Where the borehole diameter varies over short inter-
vals because of washouts of softer material or ledges of harder mate-
rial, the logs from tools that require good contact with the borehole
wall (i.e., FMS, density, and porosity) may be degraded. Deep inves-
tigation measurements such as gamma radiation, resistivity, and
sonic velocity, which do not require contact with the borehole wall,
are generally less sensitive to borehole conditions. "Bridged" sec-
tions, where borehole diameter is much below the bit size, also
cause irregular log results. The quality of the borehole is improved
by minimizing the circulation of drilling fluid while drilling, flush-
ing the borehole to remove debris, and logging as soon as possible
after drilling and conditioning are completed. During Expeditions
367 and 368, the necessity of flushing loose material from sandy for-
mations up and out of the borehole required heavy circulation.

The quality of the wireline depth determination depends on sev-
eral factors. The depth of the logging measurements is determined
from the length of the cable payed out from the winch on the ship.
The seafloor is identified on the NGR log by the abrupt reduction in
gamma ray count at the water/sediment interface (mudline). Dis-
crepancies between the drilling depth and the wireline log depth
may occur. In the case of drilling depth, discrepancies are due to
core expansion, incomplete core recovery, or incomplete heave
compensation. In the case of log depth, discrepancies between suc-
cessive runs occur because of incomplete heave compensation, in-
complete correction for cable stretch, and cable slip. Tidal changes
in sea level affect both drilling and logging depths, although these
were <1 m in the South China Sea.

Wireline heave compensator

During wireline logging operations, the up-and-down motion of
the ship (heave) causes a similar motion of the downhole logging

tools. If the amplitude of this motion is large, depth discrepancies
can be introduced into the logging data. The risk of damaging
downhole instruments is also increased. A WHC system was thus
designed to compensate for the vertical motion of the ship and
maintain a steady motion of the logging tools to ensure high-quality
logging data acquisition (Liu et al., 2013; Iturrino et al., 2013). The
WHC uses a vertical accelerometer (motion reference unit [MRU])
positioned under the rig floor near the ship's center of gravity to cal-
culate the vertical motion of the ship with respect to the seafloor. It
then adjusts the length of the wireline by varying the distance be-
tween two sets of pulleys through which the cable passes in order to
minimize downhole tool motion. Real-time measurements of up-
hole (surface) and downhole acceleration are made simultaneously
by the MRU and the EDTC, respectively. An LDEO-developed soft-
ware package allows these data to be analyzed and compared in real
time, displaying the actual motion of the logging tool string and en-
abling monitoring of the efficiency of the compensator.

Logging data flow and log depth scales

Data for each wireline logging run were monitored in real time
and recorded using the Schlumberger MAXIS 500 system. Initial
logging data were referenced to the rig floor (wireline depth below
rig floor [WRF]). After logging was completed, the data were shifted
to a seafloor reference (WSF) that is based on the step in gamma
radiation at the sediment/water interface.

Data were transferred onshore to LDEO, where standardized
data processing takes place. The main part of the processing is
depth matching to remove depth offsets between logs from differ-
ent logging runs, which results in a new depth scale: wireline log
matched depth below seafloor (WMSF). Also, corrections are made
to certain tools and logs (e.g., FMS imagery is corrected for tool ac-
celeration, including "stick and slip"), documentation for the logs
(with an assessment of log quality) is prepared, and the data are con-
verted to ASCII for the conventional logs and GIF for the FMS im-
ages. The Schlumberger Geo-Quest GeoFrame software package is
used for most of the processing of the collected wireline logging
data. The data were transferred back to the ship within a few days
after logging, and this processed data set was made available to the
science party (in ASCII and DLIS formats) through the shipboard
IODP logging database and shipboard servers.

In situ temperature measurements and
heat flow calculation

During Expeditions 367 and 368, in situ temperature measure-
ments were made with the APCT-3 (Figure F31) at each site when
the APC was deployed. The APCT-3 fits directly into the coring
shoe of the APC and consists of a battery pack, data logger, and plat-
inum resistance-temperature device calibrated over a temperature
range from 0° to 30°C. Before entering the borehole, the tool is first
stopped at the mudline for 5 min to thermally equilibrate with bot-
tom water. However, the lowest temperature recorded during the
run is occasionally used instead of the average temperature at the
mudline as an estimate of the bottom water temperature because
(1) it is more repeatable and (2) the bottom water is expected to
have the lowest temperature in the profile. When the APC is
plunged into the formation, there is an instantaneous temperature
rise from frictional heating. This heat gradually dissipates into the
surrounding sediment as the temperature at the APCT-3 equili-
brates toward the temperature of the sediment. After the APC pen-
etrates the sediment, it is held in place for 5 min while the APCT-3
records the temperature of the cutting shoe every second.
<figure><img src="image_74.png" /><figcaption>Figure F31. APCT-3 for in situ temperature measurements, Expeditions 367 and 368.</figcaption></figure>

The equilibrium temperature of the sediment is estimated by applying a mathematical heat-conduction model to the temperature decay record (Horai and Von Herzen, 1985). The synthetic thermal decay curve for the APCT-3 is a function of the geometry and thermal properties of the probe and the sediment (Bullard, 1954; Horai and Von Herzen, 1985). Equilibrium temperature is estimated by applying a fitting procedure (Pribnow et al., 2000). However, where the APC does not achieve a full stroke or where ship heave pulls the APC up from full penetration, the temperature equilibration curve is disturbed and temperature determination is less accurate. The nominal accuracy of the APCT-3 temperature measurements is ±0.05°C.

APCT-3 temperature data is combined with thermal conductivity measurements obtained from whole-round core sections to retrieve heat flow values. Heat flow and geothermal gradient are calculated according to the Bullard (1939) method to be consistent with the synthesis of ODP heat flow data by Pribnow et al. (2000). This method assumes a linear relation between temperature T and thermal resistance of the sediments:

$$T(z) = T_0 + Q \times \Omega(z),$$

where

$T$ = temperature,

$z$ = depth,

$T_0$ = surface temperature ($z = 0$),

$Q$ = is heat flow, and

$\Omega(z)$ = thermal resistance, expressed as

$$\Omega(z) = \int_{0}^{z} \{dz/[\lambda(z)]\} \approx \sum_{i=1}^{l} [(z_i - z_{i-1})/\lambda_i],$$

with $z_i$ and $z_{i-1}$ as bottom and top depths, respectively, of a horizontal layer with thermal conductivity $\lambda_i$. I is the number of layers between the surface and depth $z$.

Plotting $\Omega(z)$ as a function of $T(z)$, the Bullard plot allows estimation of the surface temperature ($T_0$) from the intercept with $z = 0$ and of the heat flow ($Q$) from the slope. The conditions for the linearity of the plot are affected by conductive conditions, steady state, and absence of internal heat source.

To obtain the thermal conductivity at the depth of the temperature measurements, we estimated a continuous profile of $\lambda(z)$, assuming that there is a linear variation of thermal conductivity with depth (Pribnow et al., 2000):

$$\lambda_{\text{LIN}}(z) = \lambda_0 + \Gamma \times z.$$

The linear trend was confirmed at each site. The thermal resistance $\Omega_{\text{LIN},j}$ for the depth $z_{\text{T},j}$ of the jth temperature value $T_j$ was calculated using the results of the linear regression, $\lambda_0$ and $\Gamma$ (slope) with

$$\Omega_{\text{LIN},j} = [\ln(\lambda_0 + \Gamma \times z_{\text{T},j}) - \ln(\lambda_0)]/\Gamma,$$

which allows the calculation of the heat flow.

## Correlation to seismic data

The Chinese National Offshore Oil and Gas Company (CNOOC) holds an extensive database of 2-D and 3-D reflection seismic data covering the northern South China Sea margin. Interpretations of these data by CNOOC allow a suite of regional seismic unconformities to be identified. These are named by CNOOC with the capital letter T followed by a number (e.g., T30, T50, etc.). The ages of these seismic stratigraphic unconformities are constrained by industry wells located significantly landward of our study area.

During this expedition, we tried to extend the regional seismic unconformities mapped by CNOOC within the northern SCS continental slope (e.g., Dai et al., 2015) into our more southerly located study area of the slope and deep SCS basin. We applied the principle of seismic stratigraphy established by Vail et al. (1977) in the mapping of these horizons. That is, each unconformity and its relative conformity are determined by recognizing systematic reflection terminations (including onlap, downlap, truncation, etc.). We expect there to be ten horizons tied to the CNOOC scheme in our area (Table T10), although at some of our sites one or more of these could not be identified due to lack of age control and/or disruption by faulting. Following the seismic stratigraphic principle, these can all be considered time markers, but only where they have a true conformal relationship to strata above and below will they represent a specific age. In all other settings, they represent a hiatus of a shorter or longer time interval.

We follow the convention established by CNOOC to name the base of the Cenozoic sedimentary succession Reflector Tg. This horizon is also often referred to as the “acoustic basement.” By this we mean a strong reflector that to a large but variable degree masks the underlying reflectors and does not allow any regional seismic stratigraphic mapping below it. Importantly, Tg is not a seismic stratigraphically defined horizon, nor does it represent any particular age or lithology. In our study area, it can represent the top of anything from volcanic basement of Neogene age to Mesozoic sediments or continental crystalline crust.
<table><caption>Table T10. Chinese National Offshore Oil and Gas Company (Shenzhen Branch) scheme for correlation between the regional seismic stratigraphic unconformities and the chrono- and lithostratigraphy in the Pearl River Mouth Basin, northern South China Sea margin (Shi et al., 2014; Dai et al., 2015). Modified with regard to Reflector Tg. Download table in CSV format.</caption><thead><tr><th>Seismic horizon</th><th>Age (Ma)</th><th>Corresponding lithostratigraphic boundaries</th></tr></thead><tbody><tr><td>T20</td><td>2.6</td><td>Base of Quaternary</td></tr><tr><td>T30</td><td>5.3</td><td>Base of Pliocene Wanshan Formation</td></tr><tr><td>T32</td><td>10</td><td>Base of upper Miocene Yuehai Formation</td></tr><tr><td>T40</td><td>16</td><td>Base of middle Miocene Hanjiang Formation</td></tr><tr><td>T50</td><td>19.1</td><td>Upper/lower Zhujiang Formation</td></tr><tr><td>T60</td><td>23</td><td>Base of lower Miocene Zhujiang Formation</td></tr><tr><td>T70</td><td>33.9</td><td>Base of Oligocene Zhuhai Formation</td></tr><tr><td>T80</td><td>38</td><td>Base of upper Eocene Enping Formation, underlain by lower Eocene Wenchang Formation</td></tr><tr><td>T83</td><td>Unknown</td><td></td></tr><tr><td>Tg</td><td>No specific age</td><td>Acoustic basement</td></tr></tbody></table>

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