Identification of Thiadiamondoids in Oil Samples from Tazhong Uplift, Tarim Basin
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摘要: 硫代金刚烷被认为是硫酸盐热化学还原反应（TSR）的标志物，在塔里木盆地原油中检出了大量硫代金刚烷.使用银离子柱层析法分离塔里木盆地海相原油中有机含硫化合物（organic sulfur compound，OSC），进一步采用气相色谱质谱联用（GC⁃MS）技术，在OSC组分中检测出了完整的低聚硫代金刚烷和部分高聚硫代金刚烷及金刚烷硫醇系列共76个化合物.其中，大部分油样中C0⁃C2硫代单金刚烷（易挥发硫代金刚烷）占据总硫代金刚烷含量的50%左右，中深1C和中深5井油样比较特殊，易挥发硫代金刚烷仅占据20%左右的相对丰度. 同时，中深1C和中深5井油样中硫代单金刚烷：硫代双金刚烷：硫代三金刚烷含量比值大约为4∶4∶1，而其它样品中该比值为8∶1∶0.硫代金刚烷的丰度可定量反映TSR作用的强度，硫代单金刚烷的高比值与易挥发硫代金刚烷的高相对丰度指示油样发生过运移. 这可有效应用于指示TSR作用强度以及TSR是否为原位反应，TSR作用的产物除了OSC组分还有大量H2S气体. 而原油中该发现为预测硫化氢分布与判识硫化氢成因及深层油气勘探提供理论依据.Abstract: Thiadiamondoids are commonly considered to be typical products of thermochemical sulfate reduction (TSR). Thiadiamondoids have been found in high quantities in crude oil in the Tarim Basin. By using a silver nitrate impregnated silica gel column, organic sulfur compounds (OSC) were separated from the marine oil samples from the Tarim Basin. By using GC⁃MS analysis, 76 compounds were identified in OSC fraction, including all lower thiadiamondoids (1⁃, 2⁃, and 3⁃cage thiadiamondoids), part of higher thiadiamondoids (4⁃, 5⁃, and 6⁃cage thiadiamondoids), and diamondoidthiols. C0⁃C2 thiaadamantanes (high volatile thiadiamondoids) comprise nearly half of the total thiaadamantanes in most of the samples. ZS1C and ZS5 samples are special compared with the rest of the samples, in which high volatile thiadiamondoids occupies only about 20% relative abundance. the ratios of thiaadamantanes: thiadiamantanes: thiatriamantanes of these two samples are approximately 4∶4∶1, while those of the other samples are generally 8∶1∶0. Thiadiamondoids can serve as a quantitative indicator of the strength of TSR. The oil sample has migrated, as evidenced by the high ratio of thiaadamantanes and the high relative abundance of high volatile thiadiamondoids. The content differences of thiadiamondoids can effectively indicate the intensity of TSR and to judge whether TSR is in⁃situ, and the OSC component of the TSR product is also present, along with a significant quantity of H2S gas. It can also provide guidance for the prediction of the distribution and genesis of hydrogen sulfide and petroleum exploration and exploitation decisions in deep strata.
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Key words:
- thiadiamondoid /
- thermochemical sulfate reduction(TSR) /
- diamondoidthiol /
- Tarim Basin /
- petroleum geology /
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图 1 塔里木盆地塔中地区主要断裂分布及油样位置
Fig. 1. Distribution of major faults and sampling locations in the Tazhong area, Tarim Basin
图 2 中深1C井原油分离富集前后TIC对比图
Fig. 2. Comparison of TIC before and after separation and enrichment of crude oil in Well ZS1C
图 3 中深1C井原油硫代金刚烷系列质量色谱
Fig. 3. Quality chromatography of thiadiamondoids Series in crude oil of Well ZS1C
图 7 硫代四金刚烷与四金刚烷硫醇系列质谱
Fig. 7. Mass spectrum of thiatetramantanes and tetranantanethiol series
图 8 不同油样中低聚硫代金刚烷百分含量分布直方图
a. 塔中地区油样中各硫代金刚烷含量分布直方图；b. Mobile湾油样中硫代金刚烷含量分布直方图，数据来自文献；易挥发硫代金刚烷：C0⁃C2硫代单金刚烷
Fig. 8. Percentage distribution histogram of lower thiadiamondoids in oil samples
表 1 研究区油样井号及物理性质表
Table 1. Well number and physical properties of oil samples in the study area
井号 层系 深度（m） 密度（g/cm3） 粘度（mPa·s） 含蜡量（%） 胶质（%） 沥青质（%） 含硫量（%） 含水量（%） 凝固点（℃） 中深1C 寒武系 6 944 0.927 4 2.181 0 0.20 0.45 0.08 2.680 0 8.53 < -30.0 中深5 寒武系 6 671 0.793 2 1.378 0 5.80 0.02 0.03 0.142 0 0.19 < -30.0 塔中83 奥陶系 5 681 0.830 6 3.700 0 12.37 1.70 0.70 0.060 0 3.44 -16 中古8 奥陶系 6 146 0.783 3 0.935 8 6.90 0.10 0.01 0.111 0 - -30 中古5 奥陶系 6 460 0.781 5 0.928 0 5.10 0.66 0.26 - - -12 塔中201C 奥陶系 5 779 0.774 4 0.667 2 6.20 0.38 0.15 0.161 0 - -8 中古172 奥陶系 6 210 0.814 3 1.935 0 7.70 0.62 0.38 0.275 0 - -8 中古22 奥陶系 5 893 0.780 1 0.878 9 5.60 0.31 0.07 0.108 0 - -4 中古113-1 奥陶系 7 370 0.790 0 1.162 0 12.80 0.41 0.13 0.081 4 - 20 中古43-9 奥陶系 5 380 0.800 9 1.317 0 9.60 0.14 0.05 0.200 0 - -8 注：“-”表示数据不存在；油的密度测试温度为20 ℃；粘度为50 ℃动力粘度. 
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表 2 硫代金刚烷及金刚烷硫醇鉴定结果(Wei et al., 2007, 2011)
Table 2. Identification results of thiadiamondoids and diamondoidthiols (Wei et al., 2007, 2011)
峰号 名称 缩写 分子式 分子量 峰号 名称 缩写 分子式 分子量 1 2-硫代单金刚烷 TA C9H14S 154 39 “假”四金刚烷硫醇 "p"TeT C21H26S 310 2 5-甲基-2-硫代单金刚烷 5-MTA C10H16S 168 40 硫代四金刚烷 TTe-1 C21H26S 310 3 1-甲基-2-硫代单金刚烷 1-MTA C10H16S 168 41 硫代四金刚烷 TTe-2 C21H26S 310 4 5, 7-二甲基-2-硫代单金刚烷 5, 7-DMTA C11H18S 182 42 硫代四金刚烷 TTe-3 C21H26S 310 5 1, 5-二甲基-2-硫代单金刚烷 1, 5-DMTA C11H18S 182 43 四金刚烷硫醇 TeT-1 C22H28S 324 6 1, 3-二甲基-2-硫代单金刚烷 1, 3-DMTA C11H18S 182 44 四金刚烷硫醇 TeT-2 C22H28S 324 7 3, 5, 7-三甲基-2-硫代单金刚烷 3, 5, 7-TMTA C12H20S 196 45 甲基硫代四金刚烷 MTTe-1 C22H28S 324 8 1, 5, 7-三甲基-2-硫代单金刚烷 1, 5, 7-TMTA C12H20S 196 46 甲基硫代四金刚烷 MTTe-2 C22H28S 324 9 1, 3, 7-三甲基-2-硫代单金刚烷 1, 3, 7-TMTA C12H20S 196 47 甲基硫代四金刚烷 MTTe-3 C22H28S 324 10 1, 3, 5-三甲基-2-硫代单金刚烷 1, 3, 5-TMTA C12H20S 196 48 甲基硫代四金刚烷 MTTe-4 C22H28S 324 11 1, 3, 5, 7-四甲基-2-硫代单金刚烷 1, 3, 5, 7-TeMTA C13H22S 210 49 甲基硫代四金刚烷 MTTe-5 C22H28S 324 12 四甲基-2-硫代单金刚烷 TeMTA-1 C13H22S 210 50 甲基硫代四金刚烷 MTTe-6 C22H28S 324 13 四甲基-2-硫代单金刚烷 TeMTA-2 C13H22S 210 51 甲基硫代四金刚烷 MTTe-7 C22H28S 324 14 四甲基-2-硫代单金刚烷 TeMTA-3 C13H22S 210 52 甲基硫代四金刚烷 MTTe-8 C22H28S 324 15 四甲基-2-硫代单金刚烷 TeMTA-4 C13H22S 210 53 甲基四金刚烷硫醇 MTeT-1 C23H30S 338 16 四甲基-2-硫代单金刚烷 TeMTA-5 C13H22S 210 54 甲基四金刚烷硫醇 MTeT-2 C23H30S 338 17 五甲基-2-硫代单金刚烷 PMTA-1 C14H24S 224 55 二甲基硫代四金刚烷 DTTe-1 C23H30S 338 18 五甲基-2-硫代单金刚烷 PMTA-2 C14H24S 224 56 二甲基硫代四金刚烷 DTTe-2 C23H30S 338 19 五甲基-2-硫代单金刚烷 PMTA-3 C14H24S 224 57 二甲基硫代四金刚烷 DTTe-3 C23H30S 338 20 五甲基-2-硫代单金刚烷 PMTA-4 C14H24S 224 58 二甲基-硫代四金刚烷 DTTe-4 C23H30S 338 21 2-硫代双金刚烷 TD C13H18S 206 59 二甲基硫代四金刚烷 DTTe-5 C23H30S 338 22 甲基-2-硫代双金刚烷 MTD-1 C14H20S 220 60 二甲基硫代四金刚烷 DTTe-6 C23H30S 338 23 甲基-2-硫代双金刚烷 MTD-2 C14H20S 220 61 二甲基硫代四金刚烷 DTTe-7 C23H30S 338 24 二甲基-2-硫代双金刚烷 DMTD-1 C15H22S 234 62 二甲基硫代四金刚烷 DTTe-8 C23H30S 338 25 二甲基-2-硫代双金刚烷 DMTD-2 C15H22S 234 63 二甲基硫代四金刚烷 DTTe-9 C23H30S 338 26 三甲基-2-硫代双金刚烷 TMTD-1 C16H24S 248 64 “假”五金刚烷硫醇 "p"PT C25H30S 362 27 2-硫代三金刚烷 TT C17H22S 258 65 硫代五金刚烷 TP-1 C25H30S 362 28 甲基-2-硫代三金刚烷 MTT-1 C18H24S 272 66 硫代五金刚烷 TP-2 C25H30S 362 29 甲基-2-硫代三金刚烷 MTT-2 C18H24S 272 67 硫代五金刚烷 TP-3 C25H30S 362 30 甲基-2-硫代三金刚烷 MTT-3 C18H24S 272 68 硫代五金刚烷 TP-4 C25H30S 362 31 甲基-2-硫代三金刚烷 MTT-4 C18H24S 272 69 五金刚烷硫醇 PT-1 C26H32S 376 32 二甲基-2-硫代三金刚烷 DMTT-1 C19H26S 286 70 五金刚烷硫醇 PT-2 C26H32S 376 33 二甲基-2-硫代三金刚烷 DMTT-2 C19H26S 286 71 甲基硫代五金刚烷 MTP-1 C26H32S 376 34 二甲基-2-硫代三金刚烷 DMTT-3 C19H26S 286 72 甲基硫代五金刚烷 MTP-2 C26H32S 376 35 三甲基-2-硫代三金刚烷 TMTT-1 C20H28S 286 73 甲基硫代五金刚烷 MTP-3 C26H32S 376 36 三甲基-2-硫代三金刚烷 TMTT-2 C20H28S 286 74 甲基硫代五金刚烷 MTP-4 C26H32S 376 37 三甲基-2-硫代三金刚烷 TMTT-3 C20H28S 286 75 甲基五金刚烷硫醇 MPT-1 C27H34S 390 38 二甲基-2-硫代三金刚烷 TMTT-4 C20H28S 286 76 甲基五金刚烷硫醇 MPT-2 C27H34S 390
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表 3 原油硫代金刚烷及金刚烷硫醇积分参数表
Table 3. Integral parameter table of thiadiamondoids and diamondoidthiols in crude oil
NO. Ion 化合物 中深1C 中深5 塔中83 中古8 中古5 塔中201C 中古172 中古22 中古113-1 中古43-9 （area） （area） （area） （area） （area） （area） （area） （area） （area） （area） 1 154 2-硫代单金刚烷 243 857 - 16 716 7 066 - 20 648 12 110 16 573 20 169 12 231 2 168 5-甲基-2-硫代单金刚烷 4 514 996 32 213 134 092 104 273 - 143 933 74 038 161 813 378 204 122 711 3 168 1-甲基-2-硫代单金刚烷 4 675 353 27 331 109 518 59 311 - 94 691 49 158 76 426 182 141 60 659 4 182 5, 7-二甲基-2-硫代单金刚烷 10 110 254 35 624 110 170 81 644 - 88 633 41 274 94 565 269 689 85 680 5 182 1, 5-二甲基-2-硫代单金刚烷 35 228 395 125 871 564 240 424 593 - 382 751 215 656 437 565 1 619 451 386 889 6 182 1, 3-二甲基-2-硫代单金刚烷 9 989 832 27 488 86 876 46 883 - 83 051 36 890 58 012 121 968 46 893 7 196 3, 5, 7-三甲基-2-硫代单金刚烷 20 474 110 50 550 197 272 143 109 - 131 075 65 107 159 057 376 595 134 418 8 196 1, 5, 7-三甲基-2-硫代单金刚烷 19 484 271 50 616 243 557 165 941 - 121 916 80 238 152 078 616 166 141 033 9 196 1, 3, 7-三甲基-2-硫代单金刚烷 8 012 258 24 015 92 335 93 204 1 369 100 925 35 256 79 251 266 947 73 562 10 196 1, 3, 5-三甲基-2-硫代单金刚烷 5 827 428 32 106 75 938 71 804 1 647 67 114 30 228 67 190 195 097 63 016 11 210 四甲基-2-硫代单金刚烷 5 135 990 14 904 61 267 41 231 - 29 504 19 077 44 526 92 817 39 352 12 210 四甲基-2-硫代单金刚烷 3 489 581 15 854 36 408 33 656 1 321 28 560 13 078 32 581 80 671 30 029 13 210 四甲基-2-硫代单金刚烷 3 911 511 11 858 25 484 24 848 533.4 25 663 9 911 22 262 66 375 20 805 14 210 四甲基-2-硫代单金刚烷 3 235 356 19 687 48 236 37 186 540.6 30 138 16 761 36 904 94 617 36 236 15 210 四甲基-2-硫代单金刚烷 1 261 136 7 557 15 627 16 118 541.54 14 979 5 428 14 788 39 774 14 584 16 210 四甲基-2-硫代单金刚烷 3 969 194 11 379 31 093 26 174 - 23 922 11 772 23 300 60 211 22 639 17 224 五甲基-2-硫代单金刚烷 714 991 - 12 158 8 704 - 5 992 4 345 7 686 16 610 7 628 18 224 五甲基-2-硫代单金刚烷 913 661 - 7 508 7 336 - 6 079 2 887 6 161 15 394 6 061 19 224 五甲基-2-硫代单金刚烷 2 028 952 - 14 159 11 186 - 9 010 4 436 9 689 19 513 9 416 20 224 五甲基-2-硫代单金刚烷 547 207 - 5 457 4 517 - 4 035 1 637 3 853 9 381 4 137 21 206 2-硫代双金刚烷 49 625 678 197 410 109 590 13 212 - 40 448 19 129 16 869 52 577 25 589 22 220 甲基-2-硫代双金刚烷 39 979 896 114 424 67 191 21 339 - 31 727 17 012 16 864 70 847 26 893 23 220 甲基-2-硫代双金刚烷 26 877 375 101 713 38 197 11 670 - 23 867 9 574 8 180 27 998 11 269 24 234 二甲基-2-硫代双金刚烷 21 462 333 60 336 37 494 15 144 - 27 740 11 903 10 865 40 242 16 288 25 234 二甲基-2-硫代双金刚烷 21 703 493 38 336 30 546 15 739 - 31 631 11 618 10 682 32 527 17 044 26 248 三甲基-2-硫代双金刚烷 7 452 861 10 980 10 387 7 691 - 13 312 5 796 4 054 12 354 6 839 27 258 2-硫代三金刚烷 12 515 209 59 855 26 527 1 612 - 4 881 4 172 2 158 9 948 6 036 28 272 甲基-2-硫代三金刚烷 4 764 763 14 911 4 483 796.01 - 2 056 1 141 - 4 304 2 428 29 272 甲基-2-硫代三金刚烷 5 462 785 20 511 8 998 1 857 - 2 401 1 806 - 8 482 3 054 30 272 甲基-2-硫代三金刚烷 1 945 102 7 892 5 533 1 077 - 1 463 1 009 582.14 2 642 1 565 31 272 甲基-2-硫代三金刚烷 4 534 511 20 374 7 947 1 629 - 2 017 2 164 1 128 6 158 3 677 32 286 二甲基-2-硫代三金刚烷 1 924 090 - 2 760 - - 1 114 861.1 - 1 750 2 856 33 286 二甲基-2-硫代三金刚烷 2 182 561 - 3 713 1 003 - 1 375 998.94 - 6 025 2 431 34 286 二甲基-2-硫代三金刚烷 1 605 675 - 2 338 - - 1 518 909.61 - 2 116 1 288 35 300 二甲基-2-硫代三金刚烷 1 614 194 - - - - - - - - - 36 300 二甲基-2-硫代三金刚烷 880 284 - - - - - - - - - 37 300 二甲基-2-硫代三金刚烷 703 787 - - - - - - - - - Sum 352 065 092 1 133 795 2 243 815 1 501 553.01 5 952.54 1 598 169 817 380.65 1 575 662.14 4 819 760 1 445 236 注：“-”表示数据不存在.
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