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81.
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Mahendra P. Verma 《Geostandards and Geoanalytical Research》2004,28(3):391-409
A statistical evaluation of the results of HCO3‐ determinations in geothermal waters during the interlaboratory comparison programmes of the International Association of Geochemistry and Cosmochemistry (IAGC) and International Atomic Energy Agency (IAEA) indicated that the analytical uncertainty increases with decreasing concentration of HCO3‐ and was ? 25% for 50 μg ml‐1 and ? 60% for 25 μg ml‐1 of HCO3‐. The analytical method (Method 1) used by chemists and hydrologists works well for waters containing carbonic alkalinity, whereas Method 2 used by geochemists is conceptually incorrect. A stepwise comparison between the theoretical and experimental titration results for a given concentration Na2CO3 (0.0988 mol l‐1) solution was performed to understand the limitations of the titration method for geothermal water analysis. Backward titration from the carbonic acid equivalence point (H2CO3EP) to the original pH after CO2 removal, as had been practised earlier in the geothermal industry, in order to estimate the contribution of silicic and boric alkalinities to the total alkalinity, is incorrect because the amount of standard base (NaOH) added is equivalent to silicic and boric alkalinities plus some OH‐ alkalinity. In a Na2CO3 solution, the added NaOH is equivalent to OH‐ alkalinity only. Backward titration is only needed from the forward titration end point to the H2CO3EP in order to correct the total alkalinity for the excess of standard acid (HCl) added during the forward titration. In the case of a Na2CO3 solution, the H2CO3EP, after removal of CO2 during the forward titration, is at pH = 7, not at pH = 4.5 (3.8) as has been considered in literature. Similarly, the liberation of CO2 during titration occurs well before the point expected theoretically and it is less for shorter titration time. The revised procedure for the determination of carbonic species concentration is presented and illustrated for a water sample from Alchichica Lake, Puebla, Mexico. 相似文献
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An Improved Procedure for the Determination of Ferrous Iron Mass Fraction in Silicate Rocks Using a Schlenk Line‐Based Digestion Apparatus to Exclude Oxygen 下载免费PDF全文
Dingshuai Xue Hongyue Wang Yanhong Liu Liewen Xie Ping Shen 《Geostandards and Geoanalytical Research》2017,41(3):411-425
Precise and accurate determination of ferrous iron mass fraction in silicate rocks and geological reference materials is still a significant challenge due to the labile nature of the analyte. Here, we report a modified and improved procedure for the determination of ferrous iron mass fraction, capable of yielding moderately accurate and highly precise results in a relatively shorter time than before. This modified technique requires a more convenient operational procedure than the classical method. A sample digestion apparatus was designed that included a Schlenk line to expel air in order to prevent oxidation. The advantages of this procedure over the classical procedure are shorter process flow, higher efficiency and absence of an additional redox indicator. The composition of the acid matrix used to dissolve the samples as well as the incubation temperature and time was investigated. Comparative data for twenty‐one reference materials are reported, with five of them reported for the first time by the Schlenk line procedure. A series of experiments were carried out to identify and minimise the main source of error. In addition, the possibility of eliminating the reducing substances before digestion, by pretreatment of the sample by cold 10% methanolic bromine, was also studied. 相似文献
85.
对2-(5-氯-2-吡啶偶氨)-5-二乙基氨基酚(5-Cl-DEPAP)作锌的络合滴定指示剂进行了实验。在pH5.5的HAc—NaAc介质中,以5-Cl-DEPAP作指示剂,EDTA标准溶液滴定锌,溶液颜色由紫红色变为亮黄色,终点变化敏锐,易于观察,锌量在0-25mg与EDTA消耗量成正比。方法用于化学试剂和铝合金中锌的测定,5次测定的RSD小于0.1%。结果表明,5-Cl-DEPAP符合络合滴定对指示剂的基本要求,扩大了该试剂的应用范围。 相似文献
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通过调节pH值,加入氟化氢铵消除铁的干扰,用硫代硫酸钠滴定碘,淀粉溶液做指示剂等方法。探讨了快速滴碘法在金属矿中铜含量分析的应用,方法快速易掌握,结果准确。适用于金属矿中铜的测定。 相似文献