ABSTRACT
In order to eliminate boron loss and potential isotopic fractionation during chemical pretreatment of natural samples with complex matrices, a three-column ion-exchange separation/purification procedure has been modified, which ensures more than 98% recovery of boron from each step for a wide range of sample matrices, and is applicable for boron isotope analysis by both TIMS and MC-ICP-MS. The PTIMS-Cs2BO2(+)-static double collection method was developed, ensuring simultaneous collection of (133)Cs2(11)B(16)O2(+)(m/z 309) and (133)Cs2(10)B(16)O2(+) (m/z 308) ions in adjacent H3-H4 Faraday cups with typical zoom optics parameters (Focus Quad: 15 V, Dispersion Quad: -85 V). The external reproducibilities of the measured (11)B/(10)B ratios of the NIST 951 boron standard solutions of 1000 ng, 100 ng and 10 ng of boron by PTIMS method are ±0.06, ±0.16 and ±0.25, respectively, which indicates excellent precision can be achieved for boron isotope measurement at nanogram level boron in natural samples. An on-peak zero blank correction procedure was employed to correct the residual boron signals effect in MC-ICP-MS, which gives consistent δ(11)B values with a mean of 39.66±0.35 for seawater in the whole range of boron content from 5 ppb to 200 ppb, ensuring accurate boron isotope analysis in few ppb boron. With the improved protocol, consistent results between TIMS and MC-ICP-MS data were obtained in typical geological materials within a wide span of δ(11)B values ranging from -25 to +40.
ABSTRACT
The dominant period of Pleistocene glacial cycles changed during the mid-Pleistocene from 40,000 years to 100,000 years, for as yet unknown reasons. Here we present a 2.1-million-year record of sea surface partial pressure of CO2 (Pco2), based on boron isotopes in planktic foraminifer shells, which suggests that the atmospheric partial pressure of CO2 (pco2) was relatively stable before the mid-Pleistocene climate transition. Glacial Pco2 was approximately 31 microatmospheres higher before the transition (more than 1 million years ago), but interglacial Pco2 was similar to that of late Pleistocene interglacial cycles (<450,000 years ago). These estimates are consistent with a close linkage between atmospheric CO2 concentration and global climate, but the lack of a gradual decrease in interglacial Pco2 does not support the suggestion that a long-term drawdown of atmospheric CO2 was the main cause of the climate transition.
ABSTRACT
Elevated Pb levels in humans through environmental exposure are a significant health concern requiring scientific study of the sources of, and physiological response to this toxin. This requires a simple and precise method for measuring radiogenic Pb isotopes and Pb levels in blood. Presented here is a combination of methods for separation and analysis of Pb previously used predominantly for geologic samples. This includes separation of Pb from the complex matrix of blood samples using an Fe co-precipitation method, followed by isotopic analysis by multi-collector inductively coupled plasma mass spectrometry. Evaluation of the efficacy of this procedure shows that the precision of sample preparations as measured by % difference between the (207)Pb/(206)Pb of duplicate analyses averages 0.064% (n = 48). Using the same preparation and analysis techniques to measure Pb concentrations by isotope dilution resulted in a reproducibility of better than 6%. The method was successfully used to measure uptake of ingested soil Pb in a study of the bioavailability of Pb in contaminated soils.
