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排序方式: 共有219条查询结果,搜索用时 15 毫秒
1.
Sylwia Studzińska Sandra Mounicou Joanna Szpunar Ryszard Łobiński Bogusław Buszewski 《Analytica chimica acta》2015
This text presents a novel method for the separation and detection of phosphorothioate oligonucleotides with the use of ion pair ultra high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry The research showed that hexafluoroisopropanol/triethylamine based mobile phases may be successfully used when liquid chromatography is coupled with such elemental detection. However, the concentration of both HFIP and TEA influences the final result. The lower concentration of HFIP, the lower the background in ICP-MS and the greater the sensitivity. The method applied for the analysis of serum samples was based on high resolution inductively coupled plasma mass spectrometry. Utilization of this method allows determination of fifty times lower quantity of phosphorothioate oligonucleotides than in the case of quadrupole mass analyzer. Monitoring of 31P may be used to quantify these compounds at the level of 80 μg L−1, while simultaneous determination of sulfur is very useful for qualitative analysis. Moreover, the results presented in this paper demonstrate the practical applicability of coupling LC with ICP-MS in determining phosphorothioate oligonucleotides and their metabolites in serum within 7 min with a very good sensitivity. The method was linear in the concentration range between 0.2 and 3 mg L−1. The limit of detection was in the range of 0.07 and 0.13 mg L−1. Accuracy varied with concentration, but was in the range of 3%. 相似文献
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Bogusław Fugiel 《哲学杂志》2019,99(11):1327-1334
It has been shown that a side electrode perpendicular to the measurement ones can significantly enhance the transverse electric current in TGS. Such a current, measured in a zero external electric field, resembles the classic longitudinal one. However, the amplitude of the transverse current oscillation, observed while cooling and heating the sample, rises much more slowly with the time of the transverse electric field preliminary application. Such exposure to the transverse field is required prior to the measurements for the transverse current to be observed, in a similar way to a longitudinal field that is applied in order to achieve a single domain state before longitudinal pyroelectric current measurements. A huge difference in the time of reaction to the electric fields preliminarily applied in order to achieve the maximum amplitude of the current oscillations in both cases is the evidence that the transverse current cannot be considered to be originated just for geometrical reasons. 相似文献
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Ionics - A new DP AdSV method was developed for the determination of the pesticide clothianidin (Clo) based on its nitro group reduction at the in situ renovated bismuth bulk annular band working... 相似文献
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Andrzej Temeriusz Magdalena Rowińska Bogusława Piekarska‐Bartoszewicz Romana Anulewicz‐Ostrowska Michał K. Cyrański 《Journal of carbohydrate chemistry》2013,32(7):697-704
The title compound was synthesized starting from methyl 3,4,6‐tri‐O‐acetyl‐2‐acetamido‐2‐deoxy‐β‐D‐glucopyranoside, oxalyl chloride, and methyl 3,4,6‐tri‐O‐acetyl‐2‐amino‐2‐deoxy‐β‐D‐glucopyranoside. The crystal and molecular structure of the obtained imidazolidine‐4,5‐dione have been determined by X‐ray analysis as well as 1H and 13C NMR spectroscopy. 相似文献
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An efficient and stereoselective synthesis of pyrrolidine-, piperidine-, and azepane-type N-heterocycles is described by the intramolecular Pd(0)-catalysed cyclisation of amino allylic carbonates. The use of chiral ligands gave the corresponding heterocyclic derivatives having er values that were from moderate to good. 相似文献
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Determination of ascorbic acid and its degradation products by high‐performance liquid chromatography‐triple quadrupole mass spectrometry 下载免费PDF全文
Małgorzata Szultka Magdalena Buszewska‐Forajta Roman Kaliszan Bogusław Buszewski 《Electrophoresis》2014,35(4):585-592
This study describes application of liquid chromatography coupled with triple quadrupole mass spectrometry (LC‐MS) for evaluation of vitamin C stability, the objective being prediction of the degradation products. Detection was performed with an UV detector (UV‐Vis) in sequence with a triple‐quad mass spectrometer in the multiple reaction mode. The negative ion mode of ESI and MS‐MRM transitions of m/z 175→115 (quantifier) and 175→89 (qualifier) for ascorbic acid was used. All the validation parameters were within the range of acceptance proposed by the Food and Drug Administration. The method was fully validated in terms of linearity, LOD, LOQ, accuracy, and interday precision. Validation experiments revealed good linearity with R2 = 0.999 within the established concentration range, and excellent repeatability (9.3%). The LOD of the method was 0.1524 ng/mL whereas the LOQ was 0.4679 ng/mL. LC‐MS methodology proves to be an improved, simple, and fast approach to determining the content of vitamin C and its degradation products with high sensitivity, selectivity, and resolving power within 6 minutes of analysis. 相似文献
10.
Robert Piech Bogusław Baś 《International journal of environmental analytical chemistry》2013,93(5):410-420
Simple cyclic renewable silver amalgam film electrode (Hg(Ag)FE), applied for the determination of gallium(III) using differential pulse anodic stripping voltammetry (DP ASV), is presented. The effects of various factors such as: preconcentration potential and time, pulse height, step potential and supporting electrolyte composition are optimised. The calibration graph is linear from 5?nM (0.35?µg?L?1) to 80?nM (5.6?µg?L?1) for a preconcentration time of 60?s, with correlation coefficient of 0.995. For a Hg(Ag)FE with a surface area of 9.9?mm2 the detection limit for a preconcentration time of 120?s is as low as 0.1?µg?L?1. The repeatability of the method at a concentration level of the analyte as low as 3.5?µg?L?1, expressed as RSD is 3.2% (n?=?5). The proposed method was successfully applied by studying the synthetic samples and simultaneously recovery of Ga(III) from spiked aluminium samples. 相似文献