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61.
Hai Pham Tuan Hans-Gerd Janssen Ellen M. Kuiper-van Loo Harm Vlap 《Journal of separation science》1995,18(9):525-534
Determination of trace concentrations of sulfur components in natural gas is a true analytical challenge. Only analytical procedures based on gas chromatography can meet the sensitivity and accuracy requirements dictated by environmental regulation institutions and modern chemical industry. In the present contribution the sample pretreatment and chromatographic separation steps have been evaluated and optimized based on the use of a flamebased sulfur chemiluminescence detector (SCD) for target compound detection. The proposed instrument consists of a programmed temperature vaporizing (PTV) injector employing a liner packed with Chromosorb 104, a 4 μm thick film apolar column and a flame-based SCD. Using a 13 mL sample loop the detection limit achievable with the new method is 3 μg S/m3. The precision of replicate measure. ments is generally in the range of 5–15% relative standard deviation. Lower detection limits can be achieved by preconcentrating larger sample volumes, e.g. 100 mL. 相似文献
62.
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Irina V. Ledenyova Vitaly V. Didenko Alexander S. Shestakov Khidmet S. Shikhaliev 《Journal of heterocyclic chemistry》2013,50(3):573-578
Diazotization of 3‐methyl‐4‐phenyl‐1H‐pyrazol‐5‐amine 1 in hydrochloric acid has been reported to afford the corresponding diazonium salt 2 . The latter underwent azocoupling with a variety of active methylene compounds (barbituric 3a and thiobarbituric 3b acid, 2‐hetarylpyrimidine‐4,6‐dione 6a , 6b , 4‐hydroxy‐6‐methylpyridin‐2(1H)‐one 10a , 4‐hydroxy‐6‐methyl‐2H‐pyran‐2‐one 10b , 4‐hydroxy‐1‐p‐tolyl‐1H‐pyrazole‐3‐carboxylic acid ethyl ester 14 , 1,3‐thiazolidine‐2,4‐dione 16a , 2‐thioxo‐1,3‐thiazolidin‐4‐one 16b ) to yield new pyrazolylazo derivatives. Fused pyrazolo[5,1‐c][1,2,4]triazines 5 , 9a , 9b , 12 , 13 were obtained by heterocyclization reactions. Copyright © 2013 HeteroCorporation 相似文献
64.
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Li Q Zhao C Li Y Chang Y Wu Z Pang T Lu X Wu Y Xu G 《Journal of separation science》2011,34(2):119-126
An approach was developed for extracting and analyzing the chemical components of tobacco leaves based on solvent extraction and rapid & resolution liquid chromatography/quadrupole time-of-flight mass spectrometry analysis. Two solvents with different polarities were used to extract hydrophilic components and hydrophobic components, respectively, the combined analytical data can provide a "global" view of metabolites. Based on the evaluation of parallel samples, it was found that this approach provided good repeatability, accurate and reliable profiling data, and is suitable for the metabolomics study of tobacco leaves. In order to find the chemical component differences of tobacco leaves, 56 samples from Zimbabwe and China were analyzed using the developed method. The metabolite data were processed by multivariate statistic technique; an obvious group classification between Zimbabwe and China was observed, 14 significantly changed compounds were found, and 9 of them were identified. 相似文献
66.
A technique has been developed for performing headspace GC-MS analysis of volatile components of food, in which the carrier gas flow is reversed during sampling in order to overcome problems caused by the diffusion of substances not retained by the cold trap. Chromatographic profiles of volatile compounds from cheeses, obtained at room temperature, provide confirmation of the validity of the reversed flow technique, and the versatility of the system is evidenced by its successful application to both solid and liquid matrixes: the absence of any discrimination against the various components reveals its efficacy for compounds with a wide range of volatility. Addition of internal standards to the sample enables the use of the technique for quantitative analysis. 相似文献
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68.
G. Stringari Ivo Pancheri Frank Möller Osvaldo Failla 《Accreditation and quality assurance》1998,3(3):122-126
Chemical analyses of trace elements are affected by relatively high analytical errors due to the different steps of the laboratory
procedures: samples grinding, mineralisation and instrumental measurements. In the present communication, the influence of
the grinding phase on the global uncertainty of Pb, Cd, Ni and Cr determinations in plant samples by the classical method
of atomic absorption spectrometry/electrothermal atomisation (AAS-ETA) after dry ashing is quantified. Two grinding machines,
a planetary mill with balls and jars of agate versus a stainless steel grinder were compared by analysing leaf samples of
cucumber, strawberry, kiwivines, apple trees and grapevines from agricultural experimental plots under controlled conditions.
Variance components due to the difference between grinding methods and experimental plots were estimated. Further, the simultaneous
effects of the grinding methods on all considered metals have been evaluated by analysis of variance. With the stainless steel
grinder, on average, higher levels of the considered heavy metals were obtained (up to 67% of the mean values). On average,
the increments were similar for metals contained in steel (Ni and Cr) and those not contained (Pb and Cd). The true causes
of these differences need further investigation to determine whether the higher metal detection is due to possible contamination,
to a different grinding quality or to other reasons. Finally, the grinding methods did not seem to affect the combined uncertainty
of the analyses.
Received: 3 November 1997 · Accepted: 29 November 1997 相似文献
69.
Summary The method of iterative target transformation factor analysis (ITTFA) used in conjunction with second derivative peak finding
has shown to be a practical method for the peak deconvolution and reconstruction of HPLC chromatograms and spectra. The second
derivative method of peak finding is acceptable for resolutions above 0.5 for peaks of similar heights. Above 0.5 resolution
the labelling gives correct results where the spectra are substantially different and also when reasonably similar. Below
this value the peak labelling was still accurate where the spectra were different. Solvent effects on the spectra of the compounds
studied are small and do not hinder the peak labelling process. Thus small “local” libraries are feasible.
Presented at the 17th International Symposium on Chromatography, September 25–30, 1988. Vienna, Austria. 相似文献
70.