Paull, C.K., Matsumoto, R., Wallace, P.J., and Dillon, W.P. (Eds.), 2000 Proceedings of the Ocean Drilling Program, Scientific Results, Vol. 164 41. DATA REPORT: EFFECTS OF DRYING METHODS AND TEMPERATURES ON WATER CONTENT AND POROSITY OF SEDIMENT FROM THE BLAKE RIDGE1 W.J. Winters2 This study was primarily conducted to determine if a 105°C drying temperature had overestimated the shipboard water content and porosity values of sediment from Holes 991A, 995A, and 996E during Leg 164. Water contents were determined at sea by drying metal beakers filled with sediment in a convection oven at 105°C for 24 to 36 hr (Paull, Matsumoto, Wallace, et al., 1996). Those data, in conjunction with the measurement of mass and volume of the dried sediment, were used to calculate downhole porosity (volume of voids/total sample volume) profiles. The porosity values, in turn, were used in a number of other studies. For example, they set boundaries on the amount of gas hydrate that was present in Pressurized Coring System (PCS) samples (Dickens et al., Chap. 11, this volume). This re-examination of shipboard porosity was undertaken after it was suggested by some investigators that a potential existed for a gross overestimation of water content caused by the oven-drying process. The data presented here, determined from samples dried at different temperatures, can also be used in a comparison with more direct measurements of porosity by other methods (e.g., mercury injection). The effect of drying temperature on water content has been examined previously for a number of soils (Lambe, 1951), but not for modern deep-sea marine sediment. Brown and Ransom (1996) proposed that drying smectite-containing sediment at a high temperature can drive off interlayer water and thereby significantly overestimate water content and porosity. This is increasingly important for deeper sub-bottom sediments where bound water can comprise a majority of the sample’s moisture content. METHODS A 3-cm-thick, whole-round subsample was trimmed from each 10-cm whole-round section initially obtained at sea for consolidation testing. The consolidation sample had been completely sealed in wax and was stored at a temperature of ~4°C. The 3-cm subsample was quartered and used for the following analyses: (1) air drying at 23°C, and then oven drying in 10°C increments from 30° to 120°C; (2) oven drying at 60°C for mineralogy and grain-size analyses; (3) freeze drying; and (4) microwave oven drying. This report focuses on the incrementally dried water content results because the technique used to obtain them was the most similar to the shipboard procedure. Each drying temperature increment lasted at least 24 hr. Grain-size analyses, for estimating hydraulic equivalents, were performed using methods presented in Poppe (1988a). The coarse fraction was determined by use of a settling tube or sieves, and a Coulter Counter measured the amount of fine fraction present. Sample mineralogy was determined by X-ray diffraction (XRD) methods (Poppe, 1988b). Unoriented aggregate mounts were used to estimate the relative mineralogic composition using external stanPaull, C.K., Matsumoto, R., Wallace, P.J., and Dillon, W.P. (Eds.), 2000. Proc. ODP, Sci. Results, 164: College Station, TX (Ocean Drilling Program). 2 U.S. Geological Survey, 384 Woods Hole Rd., Woods Hole, MA 02543, U.S.A. [email protected] 1 dards, whereas oriented clay mineral mounts were created by a technique described by Pollastro (1982). Clay estimates were made using Biscaye’s (1965) method. RESULTS Water content values obtained from incremental oven drying to 60°C compare favorably with those obtained from drying at a constant temperature of 60°C (Fig. 1). This suggests that incremental drying produces results that are similar to those obtained from typical constant temperature drying techniques. Approximately 80% of the water content and porosity values calculated during this study are similar to at-sea determined values (Figs. 2, 3) indicating that most samples did not lose water during storage. The progressive increase in drying temperature continually reduced the amount of water left in the sample, thereby increasing the calculated water content and resultant porosity values. However, each increase in temperature produced a relatively small change in water content. The average poros90 80 70 Water content (%) oven dried at 60°C INTRODUCTION 60 50 40 30 20 10 0 0.00 10.00 20.00 30.00 40.00 50.00 60.00 70.00 80.00 90.00 Water content (%) incrementally dried to 60°C Figure 1. Water contents determined at a constant 60°C drying temperature vs. incrementally dried samples. 431 DATA REPORT A B 0.00 0.00 WC (dry) (%) Ship WC (dry) (%) 23°C 100.00 WC (dry) (%) 60°C 10.00 WC (dry) (%) Ship WC (dry) (%) 120°C WC (dry) (%) 23°C 200.00 WC (dry) (%) 60°C WC (dry) (%) 120°C 20.00 Depth (mbsf) 300.00 400.00 30.00 500.00 40.00 600.00 50.00 700.00 800.00 60.00 0 20 40 60 80 Water content (dry) (%) 100 120 0 20 40 60 80 100 Water content (dry) (%) 120 140 160 995A 991A C 0.00 10.00 WC (dry) (%) Ship WC (dry) (%) 23°C 20.00 WC (dry) (%) 60°C Depth (mbsf) WC (dry) (%) 120°C 30.00 40.00 50.00 60.00 20 30 40 50 60 70 80 Water content (dry) (%) 996E 90 100 110 Figure 2. A. Water content vs. depth for Hole 991A. Shipboard drying was performed at a constant temperature of 105°C. Air drying was at 23°C, whereas other drying temperatures were reached in 10°C increments. B. Water content vs. depth for Hole 995A. Shipboard drying was performed at a constant temperature of 105°C. Air drying was at 23°C, whereas other drying temperatures were reached in 10°C increments. C. Water content vs. depth for Hole 996E. Shipboard drying was performed at a constant temperature of 105°C. Air drying was at 23°C, whereas other drying temperatures were reached in 10°C increments. 432 DATA REPORT A B 0.00 0.00 Porosity (%) Ship Porosity (%) Ship Porosity (%) 23°C Porosity (%) 23°C 100.00 Porosity (%) 60°C Porosity (%) 60°C 10.00 Porosity (%) 120°C Porosity (%) 120°C 200.00 20.00 Depth (mbsf) 300.00 400.00 30.00 500.00 40.00 600.00 50.00 700.00 800.00 60.00 50 55 60 65 Porosity (%) 991A 70 75 30 80 35 40 45 50 55 60 Porosity (%) 995A 65 70 75 80 C 0.00 10.00 Depth (mbsf) 20.00 30.00 Porosity (%) Ship Porosity (%) 23°C Porosity (%) 60°C Porosity (%) 120°C 40.00 50.00 60.00 40 45 50 55 60 Porosity (%) 65 70 75 996E Figure 3. A. Porosity vs. depth for Hole 991A. Results were obtained by air drying samples at 23°C or in 10°C increments. B. Porosity vs. depth for Hole 995A. Results were obtained by air drying samples at 23°C or in 10°C increments. C. Porosity vs. depth for Hole 996E. Results were obtained by air drying samples at 23°C or in 10°C increments. 433 DATA REPORT ity increase with temperature change from air drying at 23°C to oven drying at 10°C increments to 120°C ranged from 0.95 to 3.31 points (1.7% to 7.1%) (Table 1; Figs. 2, 3). All sediment samples graded as clayey silt according to the shorebased technique (Table 1), whereas semiquantitative shipboard analysis typically described the sediment as nannofossil-rich silty clay or predominantly clay sized. The relatively small amount of smectite (8% to 17% of total sample mass; Table 1) occurring in only four of the samples (Hole 995A) may explain why small changes in porosities were observed with large temperature changes. However, the magnitude of porosity change is not directly related to the amount of smectite present. The northern Barbados accretionary wedge sediments studied by Brown and Ransom (1996) possessed considerably more smectite than the samples collected from the Blake Ridge on this Ocean Drilling Program (ODP) leg. SUMMARY Oven drying of sediment samples at 105°C at sea during Leg 164 produced water content and porosity results that are comparable to other methods of drying and do reflect actual in situ conditions in undisturbed cores despite the clay-rich composition of the sediment. Therefore, the original shipboard index values are valid for use in gas hydrate and other models. Because smectite was present in relatively small amounts in Hole 995A sediment, and perhaps at other locations, the drying temperature had little effect on the calculation of porosity and other index properties. However, future ODP legs may want to address the drying temperature issue during an early stage of the cruise. Valentine and Judy Commeau for providing helpful reviews. The author also wishes to thank the captain and crew of the JOIDES Resolution and to thank ODP for providing the sediment samples upon which this study was based. REFERENCES Biscaye, P.E., 1965. Mineralogy and sedimentation of recent deep-sea clays in the Atlantic Ocean and adjacent seas and oceans. Geol. Soc. Am. Bull., 76:803–832. Brown, K.M., and Ransom, B., 1996. Porosity corrections for smectite-rich sediments: impact on studies of compaction, fluid generation, and tectonic history. Geology, 24:43–84. Lambe, T.W., 1951. Soil Testing for Engineers: New York (Wiley). Paull, C.K., Matsumoto, R., Wallace, P.J., et al., 1996. Proc. ODP, Init. Repts., 164: College Station, TX (Ocean Drilling Program). Pollastro, R.M., 1982. A recommended procedure for the preparation of oriented clay-mineral specimens for X-ray diffraction analysis: modification to Drever’s filter-membrane peel technique. Open-File Rep.—U.S. Geol. Surv., 82–71. Poppe, L., 1988a. Texture. In Booth, J.S. (Ed.), Sediment Monitoring at Deep-Ocean Low-Level Radioactive Waste Disposal Sites: Methods Manual. EPA Rep. 520/1-88-002:18–41. ————, 1988b. X-ray diffraction mineralogy. In Booth, J.S. (Ed.), Sediment Monitoring at Deep-Ocean Low-Level Radioactive Waste Disposal Sites: Methods Manual. EPA Rep. 520/1-88-002:42–50. ACKNOWLEDGMENTS The author is grateful to Larry Poppe and Alex Robinson for performing the XRD and grain-size analyses, respectively; and to Page Date of initial receipt: 15 April 1998 Date of acceptance: 25 September 1998 Ms 164SR-240 Table 1. Calculated water content and porosities of samples in this study at different incremental drying temperatures, grain sizes, and smectite quantity. Sample description (cm) 434 Depth (mbsf) Water content, dry 23°C (%) Water content, dry 60°C (%) Water content, dry 120°C (%) Porosity, 23°C (%) Porosity, 60°C (%) Porosity, 120°C (%) Sand (%) Silt (%) Clay (%) 164-991A1H-4, 130 2H-4, 136 3H-4, 130 4H-4, 70 5H-4, 60 6H-5, 100 5.80 14.96 24.40 33.30 42.70 54.10 70.73 63.96 52.05 65.94 59.18 53.16 73.06 66.46 54.50 70.16 62.95 57.88 74.26 67.68 55.59 71.80 64.81 59.57 65.20 62.89 57.96 63.59 61.05 58.48 65.93 63.78 59.08 65.02 62.52 60.53 66.30 64.19 59.56 65.54 63.19 61.21 2.6 2.0 5.8 2.4 1.0 4.0 65.8 56.6 65.5 67.1 66.8 70.5 31.7 41.4 28.7 30.5 32.5 25.5 164-995A2H-1, 139 7H-1, 37 19H-2, 140 31X-1, 110 42X-2, 70 57X-2, 130 66X-4, 125 80X-1, 75 3.09 49.57 148.48 253.40 350.80 467.00 546.11 666.85 66.54 83.48 57.44 48.09 40.02 33.11 45.76 34.85 68.71 86.99 61.60 51.68 43.78 36.60 49.64 38.56 69.56 88.32 62.77 52.67 44.77 37.80 50.83 39.45 63.80 68.86 60.35 56.02 51.46 46.73 54.80 48.00 64.54 69.74 62.01 57.79 53.70 49.23 56.80 50.53 64.82 70.06 62.45 58.25 54.25 50.04 57.39 51.10 5.6 1.5 0.3 0.4 0.2 0.4 1.4 0.2 55.2 51.2 61.1 56.6 53.6 55.8 49.7 52.3 39.2 47.2 38.6 43.0 46.2 43.8 49.0 47.5 164-996E2H-1, 125 2H-5, 107 4H-6, 43 5H-6, 62 6X-5, 140 7H-7, 60 5.35 11.17 29.63 38.72 49.41 58.53 65.93 43.97 63.57 63.33 67.14 50.23 68.52 45.10 65.81 65.78 69.66 52.50 69.68 45.68 66.75 66.67 70.64 53.37 63.59 53.81 62.74 62.65 64.01 57.10 64.48 54.44 63.55 63.54 64.86 58.17 64.86 54.76 63.88 63.85 65.17 58.57 8.0 6.1 4.5 5.3 5.3 6.8 57.6 56.1 67.9 51.9 68.6 62.5 34.4 37.8 27.7 42.9 26.1 30.7 Smectite (%) 8 8 10 17
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