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341.
This study demonstrates the application of laser‐induced breakdown spectroscopy (LIBS) and hyperspectral imaging to the investigation of coprolite and fossil samples. Solid samples from the Permian (seven coprolites and one fossil), Cretaceous (one coprolite) and Oligo‐Miocene (two coprolites) periods were directly analysed, and emission spectra from 186 to 1042 nm were obtained in several areas covering coprolite/fossil and rock material. Initial exploratory analyses were performed using principal component analysis with the data set normalised by the norm (Euclidean norm = 1). After identification and selection of emission lines of eleven elements (Al, Ca, Cr, Fe, K, Mg, Mn, Na, Ni, P and Si), the signals were normalised again by the relative intensity of the selected element. Phosphorus was identified mainly in the coprolites, while K and Na were primarily found in the rock material. In several cases, there was a positive correlation between Ca and P. A sample from the Oligo‐Miocene series was also analysed using inductively coupled plasma‐optical emission spectrometry (ICP‐OES) (rock and coprolites were analysed separately). Based on the quantitative results from ICP‐OES, it was confirmed that the tendency was the same as that observed with the results obtained from LIBS directly in the solid sample.  相似文献   
342.
A measurement procedure for determining of Ru, Pd, Ir, Pt and Au mass fractions in ferromanganese deposits by inductively coupled plasma‐mass spectrometry after acid digestion and anion exchange preconcentration is presented. To eliminate incomplete recovery after sorption preconcentration of the platinum‐group elements (PGE) and Au, a standard addition method was used. Detection limits ranged from 0.02 ng (Pd, Ir) to 0.19 ng (Ru). The measurement results for ferromanganese nodule reference material NOD‐A‐1 and NOD‐P‐1 agree with earlier reported values. Intermediate precision of PGE concentration data for nodule reference materials in this work was 5–24% (1s) and could reflect sample heterogeneity.  相似文献   
343.
Experimental determination of the pressure and temperature controls on Ti solubility in quartz provides a calibration of the Ti‐in‐quartz (TitaniQ) geothermometer applicable to geological conditions up to ~ 20 kbar. We present a new method for determining 48Ti mass fractions in quartz by LA‐ICP‐MS at the 1 μg g?1 level, relevant to quartz in HP‐LT terranes. We suggest that natural quartz such as the low‐CL rims of the Bishop Tuff quartz (determined by EPMA; 41 ± 2 μg g?1 Ti, 2s) is more suitable than NIST reference glasses as a reference material for low Ti mass fractions because matrix effects are limited, Ca isobaric interferences are avoided, and polyatomic interferences at mass 48 are insignificant, thus allowing for the use of 48Ti as a normalising mass. Average titanium mass fraction from thirty‐three analyses of low temperature quartz from the Czech Erzgebirge is 0.9 ± 0.2 μg g?1 (2s) using 48Ti as a normalising mass and Bishop Tuff quartz rims as a reference material. The 2s average analytical uncertainty for individual analyses of 48Ti is 8% for 50 μm spots and 7% for 100 μm spots, which offers much greater accuracy than the 21–41% uncertainty (2s) incurred from using 49Ti as an analyte.  相似文献   
344.
This study uses MC‐ICP‐MS for the precise analysis of the stable tin isotopic composition in ore minerals of tin (cassiterite, stannite), tin metal and tin bronze. The ultimate goal is to determine the provenance of tin in ancient metal objects. We document the isotope compositions of reference materials and compare the precision of different isotope ratios and the accuracy of different procedures of mass fractionation correction. These data represent a base with which isotopic data of future studies can be directly compared. The isotopic composition of cassiterite and stannite can be determined after reduction to tin metal and bronze, respectively. Both metals readily dissolve in HCl, but while the solutions of tin metal can be directly measured, the bronze solutions must be purified with an anion exchanger. The correction of the mass bias is best performed with an internal Sb standard and an empirical regression method. A series of Sn isotope determinations on commercially available mono‐element Sn solutions as well as reference bronze materials and tin minerals show fractionations ranging from about ?0.09‰ to 0.05‰/amu. The combined analytical uncertainty (2s) was determined by replicate dissolutions of reference materials of bronze (BAM 211, IARM‐91D) and averages at about 0.005‰/amu.  相似文献   
345.
Microanalysis of native gold specimens has been hampered by the lack of a suitable reference material (RM) known to be sufficiently homogeneous at the scale of microanalytical sampling. The suitability of gold reference material AuRM2 for microanalysis was assessed. This RM was created for bulk analysis of refined gold and was only certified for homogeneity at the bulk scale. However, it contains trace elements in appropriate mass fraction ranges for analysis of native gold. This study was not intended to provide alternative mass fractions from the original certified values, only to assess its suitability for microanalytical methods. Micro‐scale (~ 3.4 μg sample mass) heterogeneity was calculated from measurement repeatability of LA‐ICP‐MS analyses of AuRM2 by factoring in signal (represented by counting statistics) and instrument set‐up‐specific variability (determined using measurement variability of a reference material known to be homogeneous). Elements determined to be homogeneous or to have minor heterogeneity (< 10% calculated heterogeneity RSD) are Mg, Al, Ti, Fe, Ni, Cu, Zn, Se, Rh, Sn, Sb, Pt and Pb. Elements with moderate heterogeneity (10–20% heterogeneity RSD) are: Mn, As, Pd, Te and Bi. Correlation of element mass fractions indicates that micro‐scale inclusions of chalcophile‐rich phases along grain boundaries may be responsible for some of the chemical heterogeneity. However, the level of heterogeneity is statistically negligible compared with the ranges of chemical signatures observed in sample populations of native gold. Therefore, AuRM2 is shown to be sufficiently homogenous at a micro‐scale for use as a RM for microanalysis of native gold.  相似文献   
346.
感耦等离子体发射光谱法测定原油中痕量铁镍铜钒   总被引:3,自引:0,他引:3  
系统地试验了用感耦等离子体发射光谱同时测定原油中痕量元素Fe、Ni、Cu和V的多种前处理方法,制定出H2SO4、HNO3分步炭化,500℃灰化,HCl+HNO3(VHCl∶VHNO3=1∶1)溶解灰分的最佳分解方案。该方法的检出限为1.0~6.0μg/L,精密度好,RSD(n=4)<4.6%,加标回收率为96.2%~111%。方法已应用于大庆、苏北、惠州等原油样品的分析。  相似文献   
347.
针对地铁隧道点云数据特征点少、在大视角点云数据间配准拼接时出现精度差、效率低等问题,本文以提高配准效率及精度作为出发点,以目前主流的ICP算法为基础,首先将激光点云按中心投影方式生成反射强度图像并以此作为配准源,采用规则格网分割提取匹配,建立均匀分布的同名点;然后利用反射强度图像上的同名点与点云之间的一一对应关系,完成视角点云间的初配准;最后在初次配准的基础上,采用KD树改进算法进行点云数据的精细配准。试验结果表明,本文在实现点云数据自动配准的同时,提高了地铁隧道点云数据的配准效率及精度。  相似文献   
348.
基于特征点法向量的点云配准算法   总被引:2,自引:0,他引:2  
在传统的迭代最近点算法(ICP)中,需要两片点云具有良好的初始位置,否则在配准时容易陷入局部最优。针对该问题,本文提出了一种基于特征点提取与配对的粗配准方法,以调整两片点云重叠部分的初始位置。首先,利用SIFT算法提取两片点云公共部分的特征点;其次,根据特征点法向量之间的欧氏距离将两片点云的特征点两两配对;然后,利用法向量的夹角对特征点对进行提纯;最后,通过单位四元数法,求解出旋转及平移矩阵,完成粗配准。试验表明,本文基于特征点法向量的粗配准方法可为精配准提供良好的初始位置,在一定程度上避免配准时陷入局部最优的现象。  相似文献   
349.
针对ICP迭代点云配准算法,利用MATLAB中封装的三角剖分函数,迅速搜索迭代过程中的最近点,简化ICP配准算法的实现,并设计一种模拟实验的方法验证算法的有效性。实验表明,利用基于三角剖分的ICP迭代算法可以达到较好的配准精度。  相似文献   
350.
在维修和改造8410型电感耦合等离子体直读光谱仪过程中,经常需要对ICP高频发生器中的开关电源进行维修和调整。简述开关电源基本原理,介绍-145V开关电源稳压过程及故障维修。  相似文献   
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