@ Pll $0146-6380(97)00102-2 (Org. Geochem. Vol. 8, No. 1/2, pp. 27-41, 1998 {© 1998 Published by Elsevier Science Lid. All righs reserved Printed in Great Brain 01466380/98 $19.00 + 000 Geochemical characteristics of terrigenous- and marine-sourced oils in Hokkaido, Japan AMANE WASEDA! and HIDEKI NISHITA' APEX Research Center, Japan Petroleum Exploration Co. Ltd, 1-2-1 Hamada, Mihama, Chiba 261 Japan (Received 13 June 1997; rewurned t0 author for revision 27 July 1997; accepted 1S September 1997) Abstract—Crude oils in Hokkaido, Japan, ate divided into two genetic groups based on bulk proper- ties, carbon-isotope compositions and biomarker distributions. One group is characterized by high car- bon-isotope canonical variables (Sofer, 1984), high wax and low sulfur content, high Pr/Ph ratios, low *Cyp) sterane ratios, relatively low Ts(Ts + Tm) ratios, and the absence of tricyclic terpanes homohopanes. These characteristics suggest that the oils were generated mainly from terrige- ous ofganic matter in source rocks deposited under highly oxic conditions. The other group is charac- terized by low canonical variables, low wax and high sulfur content, low Pr/Ph ratios, high Cry! (Cay Co) sterane ratios, relitively high Ts/(Ts + Tm) ratios, and the presence of tricyclic terpanes and Css homohopanes, properties that suggest that they were generated from marine shales. Based on the biomazker distributions, the terrigenous oils correlate to Paleogene coals and coaly shales, whereas the marine oils correlate to Miocene marine shales. The atomic H/C ratios of the coals indicate that they have oil-generating potential. The geographic distribution of the terrigenous and marine source rocks, and their thermal maturity control the distribution of the oils in Hokkaido. The geographic dis: Uuibution of the Paleogene coal-bearing formations corresponds to the distribution of the terrigenous oils in central Hokkaido. The marine oils are restricted either to areas of high heat ow related to vol ‘aie activity, of to the area wits thick Neogene and Quaternary sediments, where the Miocene source rocks are buried deep enough for oil generation. (> 1998 Published by Elsevier Science Ltd. All rights reserved Key words—Japan, Hokkaido, terrigenous oi, marine oil, biomarker, carbon isotope, oilsource rock correlation, eoal INTRODUCTION In Hokkaido, Japan (Fig. 1), the Ishikari oil field ‘was first discovered in 1903, and by 1960 fourteen oil and gas fields had been discovered. All oil fields were depleted and closed by 1970, but three gas fields are still operating. The largest field was the Ishikari field, which produced a total of 150,000 kl crude oil (Editorial Committee of Hokkaido, 1990). In 1988, the Yufutsu gas field was discovered, and the production of oil and gas started in 1996, Since geological provinces in Hokkaido generally extend north-south, it is divided into western, cen- tral, and eastern areas (Fig. 1). All oil fields are located in a north-south trending belt, west of the Hidaka Range in the central area. Oil seeps are common in Hokkaido, including the western and astern areas, In the central area, oils seeped from ccoal measures in some Paleogene coal fields. In the western and eastern areas small amounts of oil are associated with hot springs. ‘We investigated the geochemical characteristics of ‘two genetic groups of crude oils in Hokkaido. Oil- to-source rock correlation studies were performed using biomarker distributions. Relationships 2 between the geographic distribution of the oils and the distribution of mature source rocks were also examined. SAMPLES. Crude oils Twenty-two samples, taken from the locations shown in Fig. 1, were used in this study. Eighteen samples were collected in the central area, and two samples were taken from each of the western and eastern areas. In the central area, reservoir ages range from Cretaceous to Neogene, In the western and eastern areas, all oil samples are from Neogene formations. Twelve of the samples were collected from oil and gas wells, four were oil seeps collected from coal fields, two were oil seeps collected from surface outcrops, and four were collected from hot- spring wells (Table 1). None of the samples selected in this study show any indication of biodegradation of isoprenoid, sterane, or triterpane compounds. The general sequence of increasing resistance to biodegradation of biomarkers is: n-paraffins, isoprenoids, steranes,8 A. Waseda and H, Nishita Fig. 1. Map showing sampling localities of oil samples used in this study. hopanes/diasteranes, aromatic steroids, porphyrins (Seifert et al, 1984; Moldowan et al, 1992). In three of the four samples from hot-spring wells, some of the n-alkanes are degraded, but the isopre- roids, steranes and triterpanzs are intact. Source rocks ‘Twenty-three coals or cosly shales and 28 shales were collected for the oil-tource rock correlation study (Table 2). Thirty-seven of these samples were collected from surface outcrops. Fourteen are cores taken from petroleum exploration wells. The shales were taken from Miocene marine formations near the oil samples. Fourteen of the shale samples were collected in the central area, three from the western area, and eleven from the eastern area. All coals and coaly shales were collected form Paleogene coal-bearing formations in the central area. Five additional coal samples were collected form. the Paleogene coal-bearing formations for determi- nation of carbon, hydrogen and oxygen elemental compositions. METHODS Oils were analyzed for API gravity, wax content, sulfur content, and stable carbon-isotope compo- sitions of the whole oil, saturated, and aromatic hy- rocarbon fractions. Rock samples were analyzed for total organic carbon content, Rock-Eval pyrol- ysis, and vitrinite reflectance, Cys alkane, sterane and triterpane compounds in the saturated hydro- carbon fractions of oils and rock extracts were ana- lyzed in oils as well as rock extracts. Elemental analyses (C, H and O) were performed on selected coal samples. Stable carbon isotopes Stable carbon-isotope compositions of the whole oil, saturated and aromatic hydrocarbon fractions were determined using a VG Isotech SIRA Series II isotope ratio mass spectrometer. The whole oil and fractions were placed in quartz tubes with cupric oxide and silver granules. The tubes were evacuated and sealed while connected to a high-vacuum line. The samples were converted to carbon dioxide for isotope analysis by combustion at 900°C. Results were reported in the standard delta notation (6"°C; %) relative to the PDB standard. NBS-22 oil was used for calibrations, measuring —29.81%» against PDB (Schoell et al, 1983). Gas chromatography-mass spectrometry (GC-MS) Cis-talkane, sterane and triterpane compounds in the saturate fractions were analyzed using a Hewlett Packard 890A gas chromatograph with @ 25m Hewlett Packard Ultra 1 capillary column (02mm id.), coupled to a 5970B mass spec- trometer. Saturated hydrocarbon fractions were injected at 300°C. After injection, volatile com- pounds were concentrated at 50°C for I min. The ‘oven temperature was increased at 15°C min” to 200°C, then increased at 2°C min”! to 300°C, where it was held for 10 min. The mass spectrometer was operated at 70 eV electron energy in the scan mode for Cie +alkanes, and in the selected ion monitoring rode for the sterane and triterpane biomarker com- poundsnd 9-16) soundo4 HE = x9 yoo} fuRdOY-EL |: 25) = sundoy) 941, {oH0e +S oc¥soePues-eLt G22 + 169,866 — — (1QEUEA [ENUOTED)AD eure = aun u8}0 Geochemical characteristics of Japanese crude oils a of ra ” ze tf ot fl ut a st st a e FT rs " a ‘euor + sac) © 05 o “ a Ea ra 5 a + : a = Cara0e wr t t aye 8 we we ies st eee we woe oF se we ee st see wo S10 ovo soo 300 #0 0 wo w0 900 zo 500 £00 300 a0 wo Gaim) Aine anidond ad BEE Ez Zz PERE ERE E RRR EE aKL adues dnoup mz 1m « 6 ul o #1 © a 6 8 L 5 s , t t oN, pa 8 1 sj YO OpIEOH 205 FFP OHEHEOAD T AAR 0 2412-8,A, Waseda and H. Nishita » sco oO mm EO ow a woo domino ‘00611 oo om hr oo SOORSHN, 10 90 wm 6 m0 TW0eSHIN iro & ot & Go = a no ose, iro Or 6 O50 sr} 86 ico srieetn eo x OF se ocr 60 corr zo m St 950 ope er for tan so @ 6 oe sO wm OS 0s. a0 esweH aro x OW so et ‘sr 50 wien are yes) sys 82041) 00 o oF et or we 9K0s6HN 100 ie ul sc oat SROSGHN 300 is or ita we TeoseHN oro » sr oe we zo SeOS6HN zo ws a se Os6HIN * ww 98 a (SSH o% = wz GoOSGHN as oor 950 OcOEGHN zo ‘8 or TeOSHN too se o doing, 6ce8HN too a fer domino, VLZHN oo a uy domino, aNTESHN too o wo dosing, E6HN too ra uo SIzeHN “00 3 to RIGsHN, S00 a a0 a0 a se soo rt) feo 500 8 zo io 8 irs 00 i 06 zo a 0 ‘aco6RHN, Tedoq auedoy svedou (UL 4 4D) (woe +500) a ©) Guy Rw) — ay — RW) IBM) Coy) aKy UN xd Fun} doyey au, aL soe mu = +10 a 5 ts lg 90k dus Sandon ey Sstenkd eA PO ‘pms sy uF sues p04 D4n0s 1) EP POH AWELGeochemical characteristics of Japanese crude oils 3 RESULTS ‘The analytical data for the oils in this study are listed in Table 1. The sample numbers in this table correspond to those in Figs 1-7 and Figs 10-13. The Cis+saturate gas chromatograms, m/z 217 sterane mass chromatograms, and m/z 191 triter- pane mass chromatograms of two representative oil samples are shown with other geochemical data in Fig. 2. Carbon-isotope compositions of saturated and aro- matic hydrocarbon fractions Sofer (1984) evaluated the statistical difference between the carbon-isotope compositions of satu- rated and aromatic hydrocarbons for 339 oils. He 023 026 023 028 on 042 040 035 om O31 om 032 038 on 032 04 bas as 888 22989588385 defined the canonical variable (CV = ~2.53 8!’ Cysturates + 2.22 5'°Cycomaties— 11.65) as an isotopic relationship between the saturate and aromatic hy- eeumnnnen drocarbon fractions capable of distinguishing oils RASRR ARK RARARARKARS derived from waxy (terrigenous) sources and non- mnaee ree anseaunsnae waxy (marine) sources, The waxy oils have higher ee ® # values of the canonical variable (CV>0.47) than Sngan Rak aaanazzgagas|E —— nonwaxy oils (CV < 047), E The relationships between the carbon isotope z 85/2 compositions of saturated and aromatic hydro- = carbon fractions are shown in Fig. 3. The carbon- 2 isotope compositions of 15 of the 18 oils in the cen- g 8 2 tral area (oils nos 1-15) show small variations and 2i8ssge iigiageegle plot near the correlation line of the waxy (terrige- t i = nous) organic sources defined by Sofer (1984) with é 3 high canonical variables (-0.2 to +3.5). The other nence oo esensesesel three oils (oils nos 16-18) in the central area show BEASS SOE SESSESEIEES|~ heavier carbon-isotope compositions. Since these three samples are geographically distinct from the 2 other samples, the central area can be subdivided HERR A into two areas, which are designated in this paper 2 as the central A (cls nos 1-15) and central B (oils anges tos 16-18) areas, as shown in Fig. 1. Although the 98382 {ils in the western, eastern, and central B areas show wide variations in the carbon-isotope compo- sitions of the saturated and aromatic hydrocarbon fractions, all the samples plot near the correlation st os 22 03s 0.86 {ine of the marine organic sources with low canoni- 3 cal variables (-2.2 to -0.6). The isotope results eee HE —Sggest that the oils in the central A area were de- eedes rived from source rocks dominated by terrigenous £ organic matter and the other oils in the western, Z eastern, and central B areas are derived form source ESSSE SEL SGEFSESSSES|F — rocks “dominated by marine organic matter. However, these results do not necessary mean that the source rocks for the terrigenous oils deposited in nonmarine environments. They indicate import- ant higher-plant input to the source rocks but do not exclude marine depositional settings. Core Core Core Core Core Pristane over phytane ratios Didyk er al. (1978) first proposed the pristane/ phytane (Pr/Ph) ratio as an indicator of redox po- {ential of source sediments and suggested that low vyB21500.97 TYR 10028 TYK200261 NH92087 NHO2088 Ni92089 NH92005, TYK-60122 A. Waseda and H. Nishita ‘Sample No.=17 Marine ‘Area: Central B Apt= 20" i la le 23.2% Fiesieeee) SORrSO8Ds, 886 lromatcay a0, Reservoir: Miocene BannosawaF, = “wmu= 0" C15 Saturates —— Steranes fr meni ‘Sample No.=10 Central A Yututsu rvoir: Paleogene {shikarl G. vest .C15+ Saturates ‘Steranes: meee baba Waretaa% 3186 ‘Sulfur = 6.00% Terrigenous| 3S feat te 261% Fig, 2. Gas chromatograms and anes, and triterpanes together with 17 and 191 mass chromatograms showing C,s-+ saturates, ster- her geochemical data for representative oils from the two oil Broups. Pr/Ph ratios (<1) indicate anoxic conditions, whereas higher Pr/Ph ratios (> 1) indicate oxic con. ditions. Powell (1988) noted that the high Pr/Ph ratios (>3.0) suggest terrigenous organic matter deposited under oxic conditions. The Pr/Ph ratios of all samples in this study are shown in Fig. 4(a), together with the carbon-isotope 26 19C (uaturates) (4) Fig, 3, Relationships between carbon-isotope compositions of saturated and aromatic hydrocarbon fractions of the oils, Diagonal lines (from Sofee, 1984) refer to the average isotope compositions of waxy (oonmarine) and nonwaxy (marine) oils. CV = canonical variable defined by Sofer (0984)= — 2.53 I! Carnes + 2.22 3! Comin 11S, canonical variables, The oils in the central A area have high Pr/Ph ratios (>2), whereas the oils in the western, eastern, and central B areas have lower Pr; Ph ratios (<2). These data suggest that the oils in the central A area were derived from source rocks deposited under more oxic conditions than the other oils, and support the hypothesis that the oils in the central A area are of mainly terrigenous ori- ‘ain, while the other oils are derived mainly from marine organic matter, The two oil groups are clearly separated from each other in Fig. 4(a) Bulk properties Specific gravities of the oils range from 16.8 to 48.7” API (Table 1), They are classified as medium to light oils except for one heavy oil (oil 12), based on the classification of Martinez er al. (1983). The APL gravities show no distinct relationship with the other geochemical parameters in this study Average sulfur content of world crude oils, based con 9347 samples, is 0.65 wt% (Tissot and Welte, 1984). High sulfur oils are generally associated with marine carbonates or siliceous shales, while oils de- rived from marine clastic shales show moderate or variable sulfur content and terrigenous oils showGeochemical characteristies of Japanese crude oils 3 Canonical variable Sterane steranes. For the source rock bitumens, Cy steranes are pre dominant in the Paleogene coals and coaly shales, SY Cos {Shae Ronse * Miocene marine shale © Paleogene coal and coal shale Fig. 10. Ternary diagram showing the relative abundance of Cay, Coyr, and Coy- regular steranes (Sa, 14a, 17a, 20R) for the bitumens from the Miocene marine shales, ‘and Paleogene coals and coaly shales (a). and for the oils (b). whereas the marine shales contain much more Coy steranes. Consequently, the steranes in the terrige- nous oils in the central A area generally correlate with the Paleogene coals and couly shales, whereas the marine oils correlate well with the Miocene marine shales. The triterpane distributions in the oils and source rock extracts support these correlation results. The Ts/(Ts + Tm) ratios are low in the Paleogene coals and coaly shales, whereas the marine shales have high values, Considering the maturity: differences between the oils and source rocks, the terrigenous ils in the central A correlate with the Paleogene coals and coaly shales, whereas the mar- ine oils in the other areas correlate with the Miocene marine shales in a diagram of Ts (Ts + Tm) and Cry sterane 20$;(20S + 20R) ratios (Fig. 11). C3y + Cay trieyelic terpanes are not detected in any samples of the Paleogene coals and coaly shales (Table 2), similar to the terrigenous oils in the central A area, whereas the marine shales contain significant amounts of those terpanes, simi- lar (0 the marine oils in the western, eastern, and central B areas. Three terrigenous oils (oils nos. 2, § and 5) in the central A area show sterane compositions inter- mediate between those of the Miocene marine shales and those of the Paleogene coals and coaly shales (Fig. 10). Oil no. 2 (from the Yuchi field) in particular plots closer to the marine shales than to the coals and coaly shales. This result suggests that these three oils might have contributions from both marine and terrigenous sources (Waseda er al., 1996). However, the other parameters do not necessarily support this idea of mixing, but rather consistently suggest a terrigenous origin, Contamination of steranes from marine sediments along the migration path is another possibility Biomarkers such as steranes are “trace” com- ponents measured in parts per million (ppm) in 0. ‘Source rocks cere maine shal * Patagre oa nd oath o.| "eyo op * +t lis (oneal A Scena “eso ; oN C29 Sterane 208 / (208+20R) Fig, 11. Ts(Ts + Tm) ratio versus 208)(208 + 20R) ratio of Cry steranes for the bitumens from the Mioeene marine shales, and Paleogene coals and coaly shales, and for the oils38 A, Waseda and H. Nishita most oils, whereas bitumens in immature organic rich sediments generally contain much higher quan- tities of biomarkers. Therefore, if terrigenous oils poor in steranes migrate through marine sediments and extract the bitumens rich in steranes of marine origin, the sterane composition of the oils could be strongly affected by those of bitumen. This process is particularly plausible for oil no. 2, since the reser- voir rocks are the Neogene marine sediments, which also include siliceous organic-rich shales. Mattavelli and Novelli (1990) suggesteé pick up of traces of oleanane from Upper Cre-aceous and Tertiary rocks during migration as « possible explanation for the presence of oleanane in Sicilian oils thought to be generated from Lower Jurassic carbor Distribution of the Paleogene formations The geographic distribution of the Paleogene source rocks coincides with that of the terrigenous oils in the central area (Fig. 12). The Paleogene for- mations, including coal-bearing formations, mainly occur in the central Hokkaido coal basin, where most of the coal fields in Hokkaido are located. Furthermore, in central Hokkaido they occur in the central A area, but not in the central B area. Therefore, the coincidence of the geographic distri: ution of the oils and the Paleogene coal-bearing formations supports the conclusion from the oil- source rock correlation by the biomarker distri- butions that the Paleogene is the source for the ter~ rigenous oils in the central A area, “The Paleogene formations also occur in the east ern area (Fig. 12), However, the coal-bearing for- mations and coal fields are limited in the southern part and coastal area necr the Pacific Ocean, Moreover, they are generally of lower maturity Fig, 12. Geographic distributios of the Paleogene source rock formations [modified after Editorial Committee of Hokkaido (1990)), and of the occurrences of terrigenous ‘and marine oils from this study Fig. 13. Trends in geothermal gradient in Hokkaido (after Wakahama ef al, 1995), together with locations of terrige hows and marine-sourced oils from this study than the coab-bearing formations in the central area (Aihara, 1979). Distribution of the geothermal gradient Miocene marine shales are widely distributed throughout Hokkaido, but their maturity is gener- ally not high enough for oil generation due to shal- low burial. The Paleogene coal-bearing formations, in contrast, are generally mature in the central area. Figure 13 is a geothermal gradient map of Hokkaido, which shows the present thermal struc- ture shallower than about 2000m (Wakahama er al., 1995), Aihara (1979) suggested that regional or- ganic maturity, based on vitrinite reflectance data, has a close relationship to the present geothermal structure for the upper Cretaceous and Tertiary sys tems in Hokkaido. There are many hot springs and geothermal regions in the western and eastern areas, All four oils in the western and eastern areas were collected from hot-spring wells, which are located in geothermal regions. This evidence indi- cates that those oils were generated from Miocene marine source rocks affected by local high geother- ‘mal heat in the western and eastern areas. The central B area is not located in a geothermal region (Fig. 13). However, the Neogene and Quaternary sediments are thicker there than in the other areas, and the marine source rocks should be deep enough for oil generation, Omokawa et al (1990) suggested that the oils from the Barato field (represented by oil no. 17 in this study) in the cen- tral B area correlate to Miocene marine source rocks based on similarities in carbon-isotope com- position between the oils and kerogens. In summary, maturity is a critical problem for petroleum generation in the younger Miocene mar- ine source rocks, The distribution of marine-sourced oils is restricted cither to areas of high heat flowGeochemical characteristics of Japanese crude oils » ‘Table 3. Summary of geochemical characteristics forthe two groupe of ols in Hokkaido Tevnigenour 15 Marine ‘Geochemical Characters anton iotpe ‘Conon variable High (-02- + 35) Low (22-06) sult properics, We High (14-21.7%) Low (015-14 Slur Tow (002-0364) Higher (209-051%) teoprenit isan tae Higk 2) Low (<2) Eco + Coto Low (<045) High (045) Teverpane “Tscte + Tm Lower ister “Theele erpane Ant Present hs Homotopane ‘bent Present Occurence “age Paleogene, Neogene and Cretaceous Neogene Disribution Cconsident withthe dstibution of cosl- Limited in asus of gh geothermal gradient Tearing formations inthe cna area ‘or deep burial ofthe Neogene source rocks Source rook ms ° i ‘Ree Patopsne Miocene Facies Coal or coal shale Marie shale Depontional conditions Hiziy oxe es one caused by volcanic activity in some part of the east- ern and western areas, or to te area with thick Neogene and Quaternary sediments, where the Miocene sediments are buried deep enough for oil generation, CONCLUSIONS ‘The geochemical characteristics of the oils in this study are summarized in Table 3. Twenty-two oil samples are classified into two oil groups Fifteen oils have high carbon-isotope canonical variables, high wax contents, low sulfur contents, high Pr/Ph ratios, low C>y/(Coy+ Cay) sterane ratios, relatively low Tsi(Ts + Tm) ratios, and lack tri- cyclic terpanes and Cys homohopanes. These characteristics suggest that the oils were generated from terrigenous source rocks deposited under highly oxic conditions. Their reservoir ages range from Cretaceous to Neogene. Their distribution is limited to central Hokkaido, and coincides with the distribution of Paleogene coal-bearing formations Based on the biomarker distributions, the terrige- nous oils correlate with the Paleogene coals and coaly shales. Thus, the coals and zoaly shales in the Paleogene coal-bearing formatioas should be the major source rocks for the terrigenous oils in oen- tral Hokkaido, The other seven oils have lew carbon-isotope canonical variables, low wax contents, higher sulfur contents, low PriPh ratios, high Czy/(Cay + Cz) ster- ane ratios, relatively high Ts/(Ts + Tm) ratios, and contain tricyclic terpanes and C35 homohopanes, ‘These characteristics suggest that the oils were gen- erated from marine shales deposited under less-onic conditions. They are only found in Neogene reset- voirs, and only in areas of high geothermal gradient or deep burial of the Miocene marine source rocks. Based on the biomarker distributions, the marine oils are well correlated to the Miocene marine shales. Consequently the marine shales in the Miocene formations should be the major source rocks for the marine oils in both western and east- ern Hokkaido. ‘Among the bulk, isotope and biomarker par- ameters used in this study, the carbon-isotope cino- nical variables, the Pr/Ph ratios, and the Czy (Ca + Cap) sterane ratios show no overlap between the two oil groups, showing that these three par- ameters are most useful to distinguish marine and terrigenous oils in Hokkaido. Associate Editor-—K. E. Peter Acknowledgements —We ate grateful to Japan Petroleum Exploration Co., Lid (APEX) for authorizing the publi- cation of this paper. Analytical assistance by Keietsu Kato, Yoshiteru Kajiwara, Hirotsugu Iwano, Kumiko Yuki, Emiko Takamiya and Atsuko Tadokoro is greatly acknowledged, Helpful review of the manuscript was pro- vided by Fumio Akiba, We acknowledge Mamoru Omokawa, Nobuyori Takeda, and other geologists and seachemists of JAPEX for giving us helpful discussions ‘This work also benefitted from reviews by Kenneth E Peters and Louis W. Elrod REFERENCES Aihara, A. (1979) Organic metamorphism and petroleum generation in upper Cretaceous and Tertiary Systems of Hokkaido, Japan. (in Japanese with English abstract). Journal of the Japanese Association for Petroleum Technology 44, 128-133. Aquino Neto, F. R., Trendel, J. M., Restle, A.. Connan, J. and Albrecht, P. A. (1983) Occurrence and formation fof tricyclic and tetracyelic terpanes in sediments and petroleums. In Advances in Organic Geochemistry 1981, ed. M, Bjoroy et al, pp. 659-667. John Wiley & Sons, New York. Aquino Neto, FR. Triguis, J. Azevedo. D. A. 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