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641.
642.
Determination of carbonation profiles in non-hydraulic lime mortars using thermogravimetric analysis
The carbonation profile of material taken at various depths in a lime mortar specimen has been determined at different times from manufacture using a novel, high-speed thermogravimetric analysis (TGA) method. While conventional phenolphthalein staining suggests a sharp boundary between carbonated and non-carbonated regions, the new TGA technique shows that up to 15% (w/w) of portlandite remains uncarbonated at the exterior of the mortar and that the extent of carbonation declines linearly over up to 15 mm into the interior. The technique demonstrates the possibility of identifying the presence of Liesegang patterns by measuring variations in the concentration of Ca(OH)2 through the depth profile. 相似文献
643.
Summary A simple method is described for the collection of volatile compounds from a biological matrix and for their subsequent GC-MS
analysis. (E)-2-decenal and (E)-2-decenyl acetate odorous compounds from bugs of theNezara viridula species were detected together with n-dodecane and n-tridecane hydrocarbons as carriers. The chemical composition of the
secretions of the bugs collected in the Veneto region corresponds to one obtained from the same American pentatomidae. 相似文献
644.
以0.50mol.L^-1盐酸为底液,预镀汞膜的玻碳电极为工作电极,用微分电位溶出法对车间空气中镉进行测定,用标准加入法定量,在选定的条件下,线性关系良好,精密度CV为1.256%-2.23%,平均回收率为96%-107%,本法与原子吸收法对比,测定结果显著性差异,结果令人满意。 相似文献
645.
为了减少室内有毒氢化物的排放,同时保证测试结果的准确可靠,本文利用原子荧光光度计以As为例在实验的基础上,适当缩短了仪器烟道距上端与抽风机抽风口的距离(h)。该调节对砷测定的影响表现在,h〈10cm时,砷(As)荧光值显著降低,10.00μg/L(As)荧光值由1200左右降低到500~1100,同时,系列标准的浓度-荧光值线性变差,相关系数(r^2)一般〈0.999,特别是其积分曲线不平滑;只有h≥10cm,测试As标准系列时荧光值正常、积分曲线平滑,并且浓度-荧光值相关系数(r^2)〉0.999。将仪器烟道距抽风口的距离h设定为10cm,在这一优化条件下,利用HNO3和HClO4体系(V(HNO3):V(HClO4)=6:1)中温消解的方法,测试了5个土壤国家标准样品和2个生物国家标准样品中As和Hg量,结果均落在参考值范围内。 相似文献
646.
The direct and near-real-time determination of lead, manganese and mercury in laboratory air by electrostatic precipitation-atomic absorption spectrometry is reported. Background levels in the low-to-sub ng m?3 range were found, which increased by up to two orders of magnitude if the air was disturbed. Detection limits were sub-ng m?3 and a linear relationship between sampling time and atomic absorption signal was obtained if the laboratory air sampled was undisturbed or homogeneous. 相似文献
647.
648.
649.
A highly sensitive gas chromatographic-mass spectrometric (GC-MS) analytical method for the determination of the opioid narcotics fentanyl, alfentanil, and sufentanil in industrial hygiene personal air samples and surface contamination wipes was developed and comprehensively validated. Sample preparation involved a single step extraction of the samples with methanol, fortified with a fixed amount of the penta-deuterated analogues of the opioid narcotics as internal standard. The GC-MS analytical procedure using selected ion monitoring (SIM) was shown to be highly selective. Linearity was shown for levels of extracted wipe and air samples corresponding to at least 0.1-2 times their surface contamination limit (SCL) and accordingly to 0.1-2 times their time weighted average occupational exposure limit (OEL-TWA) based on a full shift 9601 air sample. Extraction recoveries were determined for spiked air samples and surface wipes and were found to be quantitative for both sampling media in the entire range studied. The air sampling method's limit of detection (LOD) was determined to be 0.4 ng per sample for fentanyl and sufentanil and 1.6 ng per sample for alfentanil, corresponding to less than 1% of their individual OEL for a full shift air sample (9601). The limit of quantification (LOQ) was found to be 1.4, 1.2, and 5.0 ng per filter for fentanyl, sufentanil, and alfentanil, respectively. The wipe sampling method had LODs of 4 ng per wipe for fentanyl and sufentanil and 16 ng per wipe for alfentanil and LOQs of respectively, 14, 12, and 50 ng per wipe. The analytical intra-assay precision of the air sampling and wipe sampling method, defined as the coefficient of variation on the analytical result of six replicate spiked media was below 10 and 5%, respectively, for all opioids at all spike levels. Accuracy expressed as relative error was determined to be below 10%, except for alfentanil at the lowest spike level (-13.1%). The stability of the opioids during simulated air sampling was investigated. For fentanyl and sufentanil a quantitative recovery was observed at all spike levels, while for alfentanil recoveries ranged from 60.3 to 85.4%. When spiked air samples were stored at ambient temperature and at -15 degrees C quantitative recovery was found for fentanyl and sufentanil after 7 and 14 days. For alfentanil a slight loss seemed to occur upon storage during 7 days, being more explicit after 14 days. Ambient storage of spiked wipes seemed to lead to significant losses of all opioids studied, yielding recoveries of 37.7-88.3%. Upon storage of similar wipes at -15 degrees C a significantly higher recovery was found ranging from 77.3 to 88.3%. The developed analytical and sampling procedures have been recently applied in an explorative field study of which the results of surface contamination wipe sampling are presented in this paper. To our knowledge, this is the first study addressing the development and validation of analytical procedures for the assessment of external occupational exposure to potent opioid narcotics. 相似文献
650.
The assumption of an instrument response that is linear with carbon number is frequently used to quantify atmospheric non-methane hydrocarbons (NMHCs) when using gas chromatography (GC) and detection by flame ionisation detector (FID). In order to assess the validity of this widely used method the results of intercomparison measurements by 14 laboratories across Europe were evaluated. The intercomparison measurements were made on synthetic, gravimetrically-prepared, gas mixtures containing 30 hydrocarbons (C2-C9) in the low ppbv range, using various different GC-FID systems. The response per carbon atom of GC-FID systems to individual NMHCs, relative to that of butane, were found to differ by more than 25% across different systems. The differences were mostly caused by analytical errors within particular GC-FID systems and to a more minor degree by systematic deviations related to the molecular structure. (Correction factors due to the molecular structure would lessen the differences, e.g. by about 5% for olefin compounds.) The differences were larger than 10% even after elimination of obvious outliers. Thus, calibration of GC-FID systems with multicomponent NMHC mixtures is found to be essential whenever the accuracy of NMHC measurements is required to be better than about 10%. If calibration by multicomponent gas mixtures is not possible and effective carbon atom response factors are used to quantify the individual NMHC compounds then the particular analytical system should be carefully characterised and its responses to individual compounds be verified. 相似文献