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Boron Isotope Analysis of Silicate Glass with Very Low Boron Concentrations by Secondary Ion Mass Spectrometry
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We present an improved method for the determination of the boron isotopic composition of volcanic glasses with boron concentrations of as low as 0.4–2.5 μg g?1, as is typical for mid‐ocean ridge basalt glasses. The analyses were completed by secondary ion mass spectrometry using a Cameca 1280 large‐radius ion microprobe. Transmission and stability of the instrument and analytical protocol were optimised, which led to an improvement of precision and reduction in surface contamination and analysis time compared with earlier studies. Accuracy, reproducibility (0.4–2.3‰, 2 RSD), measurement repeatability (2 RSE = 2.5–4.0‰ for a single spot with [B] = 1 μg g?1), matrix effects (? 0.5‰ among komatiitic, dacitic and rhyolitic glass), machine drift (no internal drift; long‐term drift: ~ 0.1‰ hr?1), contamination (~ 3–8 ng g?1) and machine background (0.093 s?1) were quantified and their influence on samples with low B concentrations was determined. The newly developed set‐up was capable of determining the B isotopic composition of basaltic glass with 1 μg g?1 B with a precision and accuracy of ± 1.5‰ (2 RSE) by completing 4–5 consecutive spot analyses with a spatial resolution of 30 μm × 30 μm. Samples with slightly higher concentrations (≥ 2.5 μg g?1) could be analysed with a precision of better than ± 2‰ (internal 2 RSE) with a single spot analysis, which took 32 min. 相似文献
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A Rapid Method for Determining Boron Concentration (ID‐ICP‐MS) and δ11B (MC‐ICP‐MS) in Vegetation Samples after Microwave Digestion and Cation Exchange Chemical Purification
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Philippe Roux Damien Lemarchand Harold J. Hughes Marie‐Pierre Turpault 《Geostandards and Geoanalytical Research》2015,39(4):453-466
We present in this article a rapid method for B extraction, purification and accurate B concentration and δ11B measurements by ID‐ICP‐MS and MC‐ICP‐MS, respectively, in different vegetation samples (bark, wood and tree leaves). We developed a rapid three‐step procedure including (1) microwave digestion, (2) cation exchange chromatography and (3) microsublimation. The entire procedure can be performed in a single working day and has shown to allow full B recovery yield and a measurement repeatability as low as 0.36‰ (± 2s) for isotope ratios. Uncertainties mostly originate from the cation exchange step but are independent of the nature of the vegetation sample. For δ11B determination by MC‐ICP‐MS, the effect of chemical impurities in the loading sample solution has shown to be critical if the dissolved load exceeds 5 μg g?1 of total salts or 25 μg g?1 of DOC. Our results also demonstrate that the acid concentration in the sample loading solution can also induce critical isotopic bias by MC‐ICP‐MS if chemistry of the rinsing‐, bracketing calibrator‐ and sample solutions is not thoroughly adjusted. We applied this method to provide a series of δ11B values of vegetal reference materials (NIST SRM 1570a = 25.74 ± 0.21‰; NIST 1547 = 40.12 ± 0.21‰; B2273 = 4.56 ± 0.15‰; BCR 060 = ?8.72 ± 0.16‰; NCS DC73349 = 16.43 ± 0.12‰). 相似文献
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为更合理选取涌潮河口的底摩擦系数,基于无结构三角网格和有限体积法,建立了适用于反演潮汐涌潮河口底摩擦系数随空间和涨、落潮变化的伴随资料同化模型。一系列"孪生"实验均较精确地反演出了给定底摩擦系数。孪生实验表明底摩擦系数的空间分布会影响反演的精度,也表明充足的观测数据资料能够提高反演的准确性。利用实测数据进行了钱塘江河口伴随同化实验,得到涨、落潮底摩擦系数分别为0.000149和0.001520(相当于曼宁系数为0.012206和0.038987),利用该值模拟出了潮波变形和涌潮形成等现象,验证了前人在钱塘江河口数值模拟时关于底摩擦系数选取经验的合理性,反映了钱塘江河口底摩擦"涨小落大"的实质。 相似文献
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Isotopic reference materials are essential to enable reliable and comparable isotope data. In the case of boron only a very limited number of such materials is available, thus preventing adequate quality control of measurement results and validation of analytical procedures. To address this situation a unique set of two boron isotope reference materials (ERM‐AE102a and ‐AE104a) and three offset δ11B reference materials (ERM‐AE120, ‐AE121 and ‐AE122) were produced and certified. The present article describes the production and certification procedure in detail. The isotopic composition of all the materials was adjusted by mixing boron parent solutions enriched in 10B or 11B with a boron parent solution having a natural isotopic composition under full gravimetric control. All parent solutions were analysed for their boron concentration as well as their boron isotopic composition by thermal ionisation mass spectrometry (TIMS) using isotope dilution as the calibration technique. For all five reference materials the isotopic composition obtained on the basis of the gravimetric data agreed very well with the isotopic composition obtained from different TIMS techniques. Stability and homogeneity studies that were performed showed no significant influence on the isotopic composition or on the related uncertainties. The three reference materials ERM‐AE120, ERM‐AE121 and ERM‐AE122 are the first reference materials with natural δ11B values not equal to 0‰. The certified δ11B values are ?20.2‰ for ERM‐AE120, 19.9‰ for ERM‐AE121 and 39.7‰ for ERM‐AE122, each with an expanded uncertainty (k = 2) of 0.6‰. These materials were produced to cover about three‐quarters of the known natural boron isotope variation. The 10B enriched isotope reference materials ERM‐AE102a and ERM‐AE104a were produced for industrial applications utilising 10B for neutron shielding purposes. The certified 10B isotope abundances are 0.29995 for ERM‐AE102a and 0.31488 for ERM‐AE104a with expanded uncertainties (k = 2) of 0.00027 and 0.00028, respectively. Together with the formerly certified ERM‐AE101 and ERM‐AE103 a unique set of four isotope reference materials and three offset δ11B reference materials for boron isotope determination are now available from European Reference Materials. 相似文献
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TJ-Ⅱ型钻孔体应变仪数字化观测资料分析 总被引:13,自引:6,他引:7
对位于山东省不同地理、构造条件的4个TJ-Ⅱ型钻孔体应变仪数字化观测资料进行了分析,结果表明:4个台的体应变资料不同程度地受降雨、地下水位、气压、温度的影响,其完整性、稳定性和可靠性不同,记录地震波的能力也存在差异。 相似文献
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就上海软土地区大直径(设计直径≥800mm)钻孔灌注桩承载力普遍低于按规范计算的极限承载力的原因进行了分析,认为大直径尺寸效应、编制规范时引用的资料存在一定的局限性以及成桩工艺时间长短等对大直径钻孔灌注桩承载力充分发挥都有不同程度的影响。建议在设计取值时,以取f_i和f_p的低限值为宜;同时,施工队伍应加强管理,缩短成桩时间;并应视具体情况适当增大泥浆比重。 相似文献