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11.
12.
A chemometric study on the prediction of the main nutritional aspects of milk has been carried out by using fourier transform infrared spectroscopy (FTIR) attenuated total reflectance (ATR) measurements of commercially available milk samples of different types. Whole, semi and skimmed milks, enriched or not with calcium, vitamins or modified by alteration of lipid or sugar composition were considered. After evaluating different strategies for data acquisition and ATR cleaning between samples, hierarchical cluster analysis (HCA) was carried out for classification of samples in order to choose the calibration set. The prediction capabilities of partial least squares (PLS) data treatment were evaluated in order to obtain information about total fat, total protein, total carbohydrates (CH), calories and calcium. On using the mean square error of cross-validation and prediction as control variables, a critical evaluation were made about the calibration set to be used, the spectral range to be considered and the data treatment (PLS-1 or PLS-2) to be performed. By selecting a calibration set of 33 samples the properties of 48 samples were predicted with relative precision of triplicates of 0.062, 0.040 and 0.039% w/v for total fat, protein and carbohydrates, and 0.66 kcal/100 ml for calories, and 2.1 mg of Ca/100 ml. The mean difference (dx−y) between predicted and actual values and standard deviation of mean differences (sx−y), were of 0.06 (0.38), 0.03 (0.18) and −0.15 (0.41), being sx−y values between brackets, for total fat, proteins and carbohydrates, 0.06 (3.8) kcal/100 ml for calories and −4.5 (9) mg/100 ml for calcium.The sensitivity and selectivity of the methodology developed were evaluated on terms of the net analyte signal. Selectivity factors ranging from 2 to 7.6% have been calculated for the five parameters considered. 相似文献
13.
Summary In this study, a rapid and efficient semi-micro extraction procedure is presented for the extraction of some higher n-alkanes
from water and soil samples. In the case of water samples n-hexane was used as the organic phase in a phase volume ratio (volume
of aqueous phase/volume of organic phase) higher than 285, while in the case of soil samples, extraction with n-hexane was
carried out in the presence of an excess of 2 M NaCl solution. The extraction rate from soil samples is very high and is better
than Soxhlet extraction, comparable with supercritical fluid extraction. High preconcentration factor in water samples allows
the limits of detection to be in the ng.mL−1 level with the use of gas chromatographic analysis. Flame ionization detector was used for monitoring the analytes. The obtained
recoveries of all studied compounds from both water and soil samples are higher than 90%. This method was successfully used
to determine some n-alkanes in municipal wastewater and contaminated soil. 相似文献
14.
A method is described for the gas-chromatographic determination of the diastereomers of vitamin K1 (phylloquinone) in the form of their dihydro dimethyl ethers. The reported method of derivatization and chromatographic analysis in conjunction with optical rotation measurements are useful approaches for characterization of vitamin K1 samples with respect to their origin. 相似文献
15.
A novel method for the determination of trace amounts of Al(III) based on resonance Rayleigh scattering (RRS) has been developed. In the presence of some surfactants, Al(III) can react with morin and form an Al(III)-morin-surfactant complex, which results in the enhancement of RRS intensity and the appearance of the corresponding RRS spectral characteristics. Their maximum scatter peaks are at 476 nm for the cetyltrimethylammonium bromide (CTAB) system, 489 nm for the cetylpyridinium chloride (CPC) system, 474 nm for the Triton X-100 system, and 473 nm for the Tween-20 system. The enhanced RRS intensity is directly proportional to the concentration of Al(III). The detection limits are in the range of (0.50-1.2)×10−7 mol l−1 depending on the surfactant. The characteristics of RRS spectra of the complexes, the optimum conditions of these reactions and the influencing factors have been investigated. The method has high selectivity, and was successfully applied to the determination of Al(III) in natural and biological samples. Furthermore, according to different complexation capacity of Al(III)-morin-CTAB system under two pH conditions, speciation analysis of Al(III) in natural waters was explored. The labile monomeric Al fraction (mainly inorganic Al, Ali) is determined at acidic pH and the total monomeric Al fraction (Ala) is determined at alkaline pH. The results are in agreement with those obtained by Driscoll’s 8-hydroxyquinoline extraction-ion exchange method. 相似文献
16.
An ion-exchange procedure is proposed for determination of Pt and Pd in environmental samples, using a Dowex 1-X10 anion-exchange resin. Pt and Pd were separated from the matrix elements in the sample by selective retention on the column as anionic chloro complexes and subsequent elution by circulated thiourea at 60 °C. The eluent, containing Pt and Pd was analyzed by inductively coupled plasma (ICP) atomic emission spectrometry (AES). Average recoveries of 98% and detection limit of 15 ng/g for both metals were achieved. Analysis of Pt and Pd concentrations in road dust, sampled from several sites in Germany was performed. The comparison of the obtained data with the concentrations of Pt and Pd in the same samples, determined by ICP-MS showed a very good agreement. 相似文献
17.
K. H. Kim J. H. Lee M. Y. Ko K. S. Shin J. S. Kang W. C. Mar J. R. Youm 《Chromatographia》2002,55(1-2):81-85
Summary A method for the assay of R-(+)- and S-(−)- metoprolol in human urine has been developed using gas chromatography-mass spectrometry.
The method involved purification by liquid-liquid extraction and derivatization with N-methyl-N-(trimethylsilyl)trifluoroacetamide
to form an O-silyl ether, followed by subsequent chiral derivatization with (−)-α-methoxy-α-(trifluoromethyl)phenylacetyl
chloride to form diastereomeric amide. The reaction was rapid and the diastereomeric derivatives were well resolved. Quantitation
was performed by selected-ion monitoring of fragment ions of the diastereomers in electron impact ionization mode. No racemization
was found during the reaction. The detection limit was 0.5 ng·mL−1. The intra-day variation ranged between 0.38 and 7.86% in relation to the measured concentration and inter-day variation
was 2.26–8.06%. The method has been applied to the determination of R-(+)-and S-(−)- metoprolol in human urine from healthy
volunteers dosed with racemic metoprolol tartrate. 相似文献
18.
An analytical scheme is proposed which combines three speciation techniques for determination of particular Al species in soil extracts and percolating waters. A cation-exchange fast protein liquid chromatography — inductively coupled plasma atomic emission spectrometry (FPLC-ICP-AES) procedure, a microcolumn chelating ion-exchange chromatography- atomic absorption spectrometry (MCC-ETAAS) technique and the 8-hydroxyquinoline spectrophotometric method (8HQ-spectrophotometry) were employed. The FPLC-ICP-AES procedure offers determination of Al3+ (retention time 4.5 min) and Al(OH)2+ species (retention time 4.0 min) which are separated from Al(OH)+
2 (retention time 1.5min). AlF2+ coelutes with Al(OH)2+ species, while Al(SO4)+, AlF+
2 and negatively charged Al organic complexes coelute with Al(OH)+
2 species. The MCC-ETAAS technique enables determination of the sum of positively charged monomeric aqua- and hydroxy-Al species plus sulphate- and fluoro-Al complexes. Employing the 8HQ-spectrophotometry the sum of positively charged monomeric aqua- and hydroxy-Al species plus sulphato- and most of the labile organic Al species are determined. The sensitivities of these selected techniques were adequate for speciation of Al in the samples analyzed. On the basis of the specific selectivity of a particular technique various groups of Al species may be determined. Thus, the comparison of analytical data from complementary procedures provides more comprehensive information on Al species present in soil extracts and percolating waters. 相似文献
19.
For the major, minor and trace element analysis of the inorganic compounds of a Ruhr-Saar coal different preparation techniques are investigated with X-ray fluorescence analysis, electron microprobe and classical wet chemical methods minimizing sample weight at standard preparation times and analytical accuracies. Considering accuracy as well as preparation efforts, determinations by electron microprobe on small sample amounts (<50 mg) proved to be superior to the other methods.Abbreviations AAS
atomic absorbtion spectrometry
- EMA
electron microprobe analysis
- IC
ion chromatography
- ISE
ion sensitive electrode
- PHOT
photometry
- WCA
wet chemical analysis
- XRF
X-ray fluorescence analysis
- LTA
low temperature plasma ashing
- HTA
high temperature ashing
- l.o.i.
loss on ignition 相似文献
20.
Flow-injection spectrofluorometric determination of trace amounts of formaldehyde in water after derivatization with acetoacetanilide 总被引:1,自引:0,他引:1
A novel fluorophotometric method for formaldehyde determination in environmental waters was developed: the method does not require any enrichment procedures. A flow-injection analysis method for the spectrofluorometric determination of formaldehyde in waters, which is based on the reaction of formaldehyde with acetoacetanilide and ammonia, is proposed. The proposed method shows a good linearity from 0.50 to 40 × 10−7 M, and the limit of detection (LOD) of 3 × 10−9 M (0.09 ppb) is achievable. The sample throughput is 15 h−1. One of the main advantages in the proposed method is that the reaction can be carried out at room temperature without any heating system. The effect of various interferences possibly present in the real water samples was investigated. Most cations and anions, as well as organic compounds, do not interfere with the determination of formaldehyde in environmental water samples. The proposed method is very simple, rapid, less expensive, and highly sensitive, and can be applied to the environmental water samples, such as rain, tap water and river water, at low concentration levels without any enrichment procedure. 相似文献