Open File Report OF-AR-35 New Mexico Bureau of Geology and Mineral Resources A division of New Mexico Institute of Mining and Technology 40 Ar/39Ar Geochronology Results from a Navajo Canyon Dike in Mesa Verde National Park Prepared By: Lisa Peters New Mexico Bureau of Geology, Socorro, NM 87801 Prepared For: Paul Carrara Us Geological Survey, Denver, CO Initially prepared as: Data Repository for: NM Geochronology Research Laboratory Internal Report NM Bureau of Geology and Mineral Resources NMGRL-IR 578 March 16, 2007 SOCORRO 2011 Introduction A sample from a minette dike in Navajo Canyon, Mesa Verde National Park was submitted by Paul Carrara of the USGS. Several of these dikes are found in the park and have been assumed to be related to the Shiprock complex (~30 Ma). Biotite was separated from the submitted dike sample (6126) and analyzed by the 40Ar/39Ar method. 40 Ar/39Ar Analytical Methods and Results The minette was crushed, sieved and cleaned with distilled water and the biotite was removed by hand-picking under a binocular microscope. The sample was loaded into an aluminum disc and irradiated for 15 hours at the GSTR TRIGA nuclear reactor at the US Geological Survey in Denver, Colorado. The biotite mineral separate was analyzed with the furnace incremental heating age spectrum method. Abbreviated analytical methods for the dated sample are given in Table 1, and details of the overall operation of the New Mexico Geochronology Research Laboratory is provided in the Appendix. The age results are summarized in Table 1 and the argon isotopic data are given in Table 2. 6126 Weighted Mean Age=25.65±0.08 Ma n/ntotal =5/11 MSWD=0.75 Sample 6126 yielded a slightly disturbed age spectrum with increasing apparent ages (10.51 to 25.89 Ma) over the initial 33.4% of the 39Ar released (Figure 1a). Increasing radiogenic yields (4 to 94%) and K/Ca values (0.43 to 69) are correlated with these increasing apparent ages. A small drop in apparent age from 25.89 Ma to 25.66 Ma is revealed between heating steps E and F. The age’s radiogenic yields remain fairly constant over the next 65.3% of the age spectrum from which a plateau age of 25.65±0.08 Ma is calculated. The K/Ca values reveal a steady decline from 69.9 to 10.9 for the plateau steps. The final heating step reveals a rise in apparent age to 28.00 Ma and a drop in both radiogenic yield (58.9%) and K/Ca (7.4). Inverse isochron analysis (Figure 1b) of -1- steps C-J reveals an atmospheric 40Ar/36Ar intercept (294.2±19.0) and an isochron age of 25.71±0.18 Ma that agrees within error to the weighted mean age. The isochron MSWD of 4.2 suggests scatter that is not solely explained by analytical uncertainty. Discussion We assign the weighted mean age (25.65±0.08 Ma) calculated from steps F-J as the intrusion age of this minette dike. Overall the age spectrum exhibits only minor complexity which suggests to us that the assigned plateau age is an accurate intrusion age. Further support for this interpretation is afforded by the agreement of the total gas and plateau ages. -2- References Cited Renne, P.R., Owens, T.L., DePaolo, D.J., Swisher, C.C., Deino, A.L., and Darner, D.B., 1998. Intercalibration of standards, absolute ages and uncertainties in 40Ar/39Ar dating, Chem. Geol., 145, 117-152. Steiger, R.H., and Jäger, E., 1977. Subcommission on geochronology: Convention on the use of decay constants in geo- and cosmochronology. Earth and Planet. Sci. Lett., 36, 359-362. Taylor, J.R., 1982. An Introduction to Error Analysis: The Study of Uncertainties in Physical Measurements,. Univ. Sci. Books, Mill Valley, Calif., 270 p. -3- Table 1. Summary of 40Ar/39Ar results and analytical methods Sample 6126 Lab # Irradiation 56142 NM-194 mineral biotite age analysis furnace step-heat steps 5 Age 25.65 ±2σ 0.08 MSWD 0.75 Sample preparation and irradiation: Biotite separated with hand-picking techniques. Sample was loaded into a machined Al disc and irradiated for 15 hours at the GSTR TRIGA nuclear reactor, US Geological Survey Denver, Colorado. Neutron flux monitor Fish Canyon Tuff sanidine (FC-2). Assigned age = 28.02 Ma (Renne et al., 1998). Instrumentation: Mass Analyzer Products 215-50 mass spectrometer on line with automated all-metal extraction system. Flux monitor fused by a 50 watt Synrad CO2 laser. Reactive gases removed during a 2 minute reaction with 2 SAES GP-50 getters, 1 operated at ~450°C and 1 at 20°C. Gas also exposed to a W filament operated at ~2000°C and a cold finger operated at -140°C. Biotite step-heated for 8 minutes, using a Mo double-vacuum resistance furnace. Reactive gases removed during furnace analysis by reaction with 3 SAES GP-50 getters, 2 operated at ~450°C and 1 at 20°C. Gas also exposed to a W filiment operated at ~2000°C. Analytical parameters: Electron multiplier sensitivity averaged 2.88 x 10-16 moles/pA. Total system blank and background for laser analyses averaged 2680, 11.6, 2.11, 39.3, 14.2 x 10-18 moles at masses 40, 39, 38, 37 and 36, respectively. J-factors determined to a precision of ± 0.11% by CO2 laser-fusion of 10 single crystals from each of 10 radial positions around the irradiation tray. Correction factors for interfering nuclear reactions were determined using K-glass and CaF2 and are as follows: (40Ar/39Ar)K = 0.01±0.002; (36Ar/37Ar)Ca = 0.000276±0.000001; and (39Ar/37Ar)Ca = 0.000676±0.000005. Table 2. 40Ar/39Ar analytical data. ID Temp 40 Ar/39Ar 37 Ar/39Ar 36 Ar/39Ar -3 (°C) (x 10 ) 39 (x 10 ArK -15 K/Ca 6126, Biotite, 5.35 mg, J=0.0036236±0.11%, D=1.002±0.001, NM-194E, Lab#=56142-01 A 650 40.27 1.175 131.1 2.37 0.43 B 750 8.665 11.77 20.43 6.38 0.043 C 850 5.420 0.1240 5.069 32.5 4.1 D 920 4.556 0.0145 1.952 100.9 35.2 E 1000 4.248 0.0074 0.8447 276.9 68.6 F 1075 4.158 0.0073 0.6653 336.2 69.9 G 1110 4.210 0.0078 0.8432 135.3 65.5 H 1180 4.103 0.0090 0.4616 282.5 56.9 I 1210 4.084 0.0200 0.4822 57.7 25.5 J 1250 4.378 0.0467 1.441 7.54 10.9 Xi K 1680 7.336 0.0686 10.20 16.8 7.4 Integrated age ± 2σ n=11 1255.1 6.8 Plateau ± 2σ steps F-J n=5 MSWD=0.75 Isochron±2σ steps C-J n=8 MSWD=4.16 819.1 Ar* (%) mol) Xi Xi X X X 40 4.0 41.5 72.5 87.3 94.1 95.3 94.1 96.7 96.5 90.3 58.9 39 Ar (%) 0.2 0.7 3.3 11.3 33.4 60.2 71.0 93.5 98.1 98.7 100.0 K2O=24.87% 61.0 ±52.2 65.3 40 Ar/36Ar=294.2±19.0 Age (Ma) ±1σ (Ma) 10.51 23.52 25.46 25.77 25.89 25.66 25.65 25.69 25.53 25.62 28.00 25.70 2.90 0.71 0.15 0.07 0.05 0.04 0.06 0.04 0.08 0.38 0.31 0.10 25.65 0.08 25.71 0.09 Notes: Isotopic ratios corrected for blank, radioactive decay, and mass discrimination, not corrected for interfering reactions. Errors quoted for individual analyses include analytical error only, without interfering reaction or J uncertainties. Integrated age calculated by summing isotopic measurements of all steps. Integrated age error calculated by quadratically combining errors of isotopic measurements of all steps. Plateau age is inverse-variance-weighted mean of selected steps. Plateau age error is inverse-variance-weighted mean error (Taylor, 1982) times root MSWD where MSWD>1. Plateau error is weighted error of Taylor (1982). Decay constants and isotopic abundances after Steiger and Jäger (1977). X symbol preceding sample ID denotes analyses excluded from plateau age calculations. i symbol preceding sample ID denotes analyses excluded from isochron age calculations. Weight percent K2O calculated from 39Ar signal, sample weight, and instrument sensitivity. Ages calculated relative to FC-2 Fish Canyon Tuff sanidine interlaboratory standard at 28.02 Ma Decay Constant (LambdaK (total)) = 5.543e-10/a Correction factors: (39Ar/37Ar)Ca = 0.00067 ± 3e-05 (36Ar/37Ar)Ca = 0.00028 ± 1e-05 (38Ar/39Ar)K = 0.01077 (40Ar/39Ar)K = 0.01 ± 0.002 % Radiogenic 6126 Biotite 1a. 100 50 0 20 0 27.0 25.65 ± 0.08 Ma* (MSWD = 0.75) Apparent Age Ma 26.5 26.0 25.5 25.0 1000 E 920 D 750 850 C 1075 F 1180 H 1110 G 1210 I 1250 J 24.5 24.0 23.5 Integrated Age = 25.70 ± 0.10 Ma 23.0 0 10 20 30 40 50 60 70 80 90 100 Cumulative %39Ar Released 1b. 0.0040 0.0035 A 0.0030 36Ar/40Ar 0.0025 0.0020 B 0.0015 K 0.0010 C Steps C-J Isochron age = 25.71 ± 0.18 Ma 40Ar/36Ar Intercept = 294.2 ± 19.0 0.0005 D J EG FH I MSWD = 4.2, n = 8 0 0 0.04 0.06 0.10 0.14 0.18 0.22 0.26 39Ar/40Ar Figure 1. Age spectrum, K/Ca and radiogenic yield diagrams (1a) and isochron (1b) for 6126 biotite. All errors quoted at two sigma. K/Ca 80 60 40