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Ti separation was achieved by ion-exchange chromatography using Bio-Rad AG 1-X8 anion-exchange and DGA resins. For high-Fe/Ti and high-Mg/Ti igneous samples, a three-column procedure was required, whereas a two-column procedure was used for low-Fe/Ti and low-Mg/Ti igneous samples. The Ti isotopes were analysed by MC-ICP-MS, and instrumental mass bias was corrected using a 47Ti-49Ti double-spike technique. The 47Ti-49Ti double-spike and SRM 3162a were calibrated using SRM 979-Cr, certificated value 53Cr/52Crtrue = 0.11339. Isobaric interference was evaluated by analysing Alfa-Ti doped with Na, Mg, Ca, and Mo, and results indicate that high concentrations of Na and Mg have no significant effect on Ti isotope analyses; however, Ca and Mo interferences lead to erroneous δ49/47Ti values when Ca/Ti and Mo/Ti ratios exceed 0.01 and 0.1, respectively. Titanium isotopic compositions were determined for 12 igneous reference materials, BCR-2, BHVO-2, GBW07105, AGV-1, AGV-2, W-2, GBW07123, GBW07126, GBW07127, GBW07101, JP-1, and DTS-2b. Samples yield δ49/47Ti (‰) of ?0.035 ± 0.022, ?0.038 ± 0.031, 0.031 ± 0.022, 0.059 ± 0.038, 0.044 ± 0.037, 0.000 ± 0.015, 0.154 ± 0.044, ?0.044 ± 0.018, 0.010 ± 0.022, 0.064 ± 0.043, 0.169 ± 0.034, and ?0.047 ± 0.025 (relative to OL-Ti, ±2SD), respectively; of which isotopic compositions of DTS-2b, JP-1, GBW07101, GBW07105, GBW07123, GBW07126, and GBW07127 are reported for the first time. Standard Alfa-Ti was analysed repeatedly over a ten-month period, indicating a reproducibility of ±0.047 (2SD) for δ49/47Ti, similar to the precisions obtained for geochemical reference materials.  相似文献   
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For studies of mass-dependent fractionation of calcium isotopes in natural materials, the 48Ca/42Ca ratio is a superior choice to the conventionally measured 44Ca/40Ca ratio for two important reasons. These are (1) mass-dependent fractionation can be determined free from the effects of inherited or ingrown radiogenic 40Ca and (2) this ratio increases the spread of measured isotopic masses by 50%, resulting in statistically better resolution of fractionation, assuming similar precision. A third, though strictly technical, advantage is the inherent ability of a mass spectrometer to measure ratios close to unity (48Ca/42Ca) more precisely than very small or large ratios (44Ca/40Ca). However, because of the very low natural abundance of both 48Ca and 42Ca, their ratio has been very difficult to measure, the only attempt so far being on a high mass resolution MC-ICP-MS with a precision of 0.33%. We report here determination of the 48Ca/42Ca ratio by the more commonly available and user-friendly multi-collector TIMS using a 43Ca-46Ca double-spike, with a significantly better precision of 0.18% (2s). The 48Ca/40Ca or 44Ca/40Ca ratio can also be measured in the same mass spectrometer run to provide complementary information on any radiogenic component.  相似文献   
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本研究建立了适用于玄武岩、纯橄岩和页岩样品的阳离子树脂铬元素化学分离方法, 并采用双稀释剂校正化学分离和质谱仪测量过程中的质量分馏。在化学分离过程中铬有3个淋洗峰, 反映了盐酸体系中铬至少具有3种络合物。页岩样品中Al、Ti含量较高, 在淋洗过程中会有过载现象。采用了SRM 979对50Cr-54Cr双稀释剂进行了标定, 双稀释剂的铬同位素组成为50Cr/52Cr=41.66, 54Cr/52Cr=22.28。铬元素标准NIST 3112a相对于SRM 979的δ53Cr= –0.063±0.05‰(2SD, N=22)。玄武岩、纯橄岩等标准物质的结果与已发表数据在误差范围内一致, 精度达到国际同类实验室平均水平。  相似文献   
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