Samples and experimental procedures

lain by Phanerozoic sedimentary rocks, and are locally intruded by Cretaceous granitic rocks in the southern part of the area. The Wonnam group, the oldest unit in the study area, is mainly composed of mica schists, garnet-mica schists, biotite gneisses, quartzite, and aplitic gneisses to- gether with subordinate calcsilicates and amphi- bolites. The Pyeonghae gneiss comprises mainly well-foliated biotite gneisses and aplitic gneisses, showing augen and banded structures. In the fel- sic interlayer, K-feldspar porphyroblasts about 2 cm in length are commonly observed. Kim et al. 1991 suggested an upper amphibolite facies metamorphic condition for the Pyeonghae gneiss, but quantitative estimates of temperature and pressure are not available yet. No geochronologi- cal data have been reported for the Precambrian rocks in the Pyeonghae area.

3. Samples and experimental procedures

Pb and Nd whole rock isotopic compositions were measured for selected samples of the Won- nam group and the Pyeonghae gneiss. The loca- tions of analyzed samples are shown in Fig. 1C. The rock chosen for the PbSL garnet dating PH13 is a fresh specimen of garnet-biotite schist collected from the central part of the Wonnam group Fig. 1C. The garnet ranges from 1 to 4 mm in diameter. The garnets are predomin- antly almandine-pyrope solid solutions with minor spessartine and grossular components Alm 66 – 71 Pyr 17 – 25 Spe 1.7 – 2.7 Gro 4.4 – 9.1 . Pure garnet separates were hand-picked under a binocular mi- croscope from rock fragments ranging from 20 to 60 mesh in size. Garnet separates were repeatedly rinsed with acetone and Millipore ® water in an ultrasonic cleaner for 30 min. All the analyses including chemical separation and mass spectrometry were performed at the Korea Basic Science Institute. About 100 mg of rock powder was mixed with a 150 Nd – 149 Sm mixed spike and then dissolved with a mixed acid HF: HClO 4 : HNO 3 = 4:1:1 in Teflon vessels. REE rare earth element fractions were collected by the conventional cation column chemistry. Sm and Nd fractions were separated from each other by the second step cation column chemistry using 0.2 M HIBA alpha-hydroxy-iso butyric acid Makishima et al., 1993. Three 120°C leaching steps were performed on the garnet separate. The first step was treatment with a mixed acid of 12:1 1N HBr + 2N HCl for 30 min. The second and third steps were per- formed with 4.5N HBr for 3 h and 9N HBr for 18 h, respectively. 30 ml Savillex ® screw-top beakers were used in the leaching experiment. The residue was rinsed three times with purified water and dried between steps. Sm, Nd, Th, and U concen- trations of the leachates were measured using a VG PQ III ® inductively coupled plasma mass spectrometer ICP-MS. For Pb isotope analysis, whole rock powders and PH 13 garnet were di- gested using the same method as above but with- out spikes. The Pb of the PbSL leachates, unleached garnet, and whole rock samples was separated by the anion exchange column chem- istry using an HBr medium. Isotopic ratios were measured on a VG 54-30 ® thermal ionization mass spectrometer TIMS equipped with nine Faraday buckets. The Nd and Pb isotopic compositions were measured with dynamic and static modes, respectively. The 143 Nd 144 Nd ratios were normalized to 146 Nd 144 Nd = 0.7219, and further corrected for Nd contribution from added spikes. Replicate analyses of La Jolla Nd gave 143 Nd 144 Nd = 0.511833 9 0.000005 2s m , N = 13. The Pb iso- tope ratios were corrected for instrumental fractionation using average measured values of the NBS 981 standard. The measured isotopic ratios of the NBS 981 showed mass fractionation of around 0.1 per atomic mass unit relative to the recommended value. Total blank levels were about 10 pg for Sm and 50 pg for Nd. Pb blanks were about 0.3 ng for the PbSL and below 1 ng for the whole rock experiment. Isochron parame- ters were calculated using the computer program of Ludwig 1994. In the isochron calculation, we assumed 2s error of 0.1 = external reproduci- bility of NBS981 data, N = 13 for most of 207 Pb 204 Pb and 206 Pb 204 Pb data because internal errors for individual data were smaller than 0.1. Only for the third leaching step data, internal errors of Table 1 Pb isotope data for Precambrian basement rocks from the Pyeonghae area, northeastern Yeongnam massif, South Korea 206 Pb 204 Pb 9 2s a 207 Pb 204 Pb 9 2s a Rock types 208 Pb 204 Pb Sample 9 2s a Wonnam group 30.303 17.215 Amphibolite YH01 40.009 16.770 15.638 PH03 Amphibolite 35.673 16.833 15.599 Biotite gneiss b YH03 36.265 22.995 YH04 Biotite gneiss b 16.347 42.951 17.782 15.703 Garnet-mica schist PH13 40.955 17.177 15.563 PH14 Garnet-mica schist 39.488 20.565 16.056 Garnet-mica schist PH25-1 41.777 Garnet-mica schist PH26 20.066 15.842 39.821 Pyeonghae gneiss PH04 Augen gneiss 20.674 16.129 41.915 22.383 16.319 42.566 PH09 Augen gneiss 19.345 15.950 Porphyroblastic gneiss PH11 42.969 19.585 15.970 PH15 Porphyroblastic gneiss 42.316 17.038 15.640 Augen gneiss PH19 37.303 23.945 16.545 PH20 49.406 Augen gneiss PbSL for garnet in PH13 17.758 0.06 15.687 Leaching step[1] 0.06 40.946 0.06 20.636 0.07 15.979 0.07 Leaching step[2] 49.740 0.06 Leaching step[3] 79.447 0.25 22.617 0.24 236.273 0.24 26.094 0.09 16.582 0.09 50.851 0.09 Unleached garnet bulk a Internal errors SD, N = 60. For whole rock data, within run errors are sufficiently smaller than 0.1. b Gneissic part of schist-gneiss-quartzite interlayer. ca. 0.25 were given. The residue after the PbSL gave a very poor signal during the mass spectro- metric run, probably indicating little Pb remained after the leaching. So no Pb isotopic data are reported for the residue. Errors of calculated ages were reported at the 95 confidence level.

4. Results and discussion