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21.
Aamer Saeed 《Monatshefte für Chemie / Chemical Monthly》2003,134(3):457-463
Summary. A short facile synthesis of the fungal metabolite (±)-3,4-dihydro-3,6,8-trihydroxy-3- pentadecylisocoumarin (peniolactol)
has been achieved. Condensation of hexadecanoyl chloride with 3,5-dimethoxyhomophthalic acid afforded 6,8-dimethoxy-3-pentadecylisocoumarin,
which on sequential saponification and demethylation furnished rac-peniolactol in 31% overall yield. The ring-chain tautomerism was studied in solution by 1H NMR and the mass fragmentation pattern. 3-Pentadecyl- isocoumarin was also synthesized and saponified to the corresponding
keto acid as a model compound for comparative studies.
E-mail: aamersaeed@yahoo.com
Received May 23, 2002; accepted May 30, 2002 相似文献
22.
Saeed Yousefinejad Fatemeh Honarasa Samira Akbari Mohsen Nekoeinia 《液相色谱法及相关技术杂志》2020,43(15-16):580-588
AbstractSeparation of amino acids (AAs) and their simple and inexpensive determination/identification is an interesting topic in biological and protein science, different food industries, and drug factories. Also, the presentation of the chromatographic behavior of compounds in a predictive model can be effective to estimate the structural/chemical properties of analyte and mobile phases. In this work for the first time, retardation factor (RF) of 42 AAs in reversed-phase thin layer chromatography (RP-TLC) was modeled. Acetonitrile-sodium azide solution and 1,2 dioxane-sodium azide solution were two mobile phases which have been studied in this work. Results showed that the values of RF are correlated with the structural properties of AAs and these properties had some similarities and differences in two noted mobile phases. For the TLC data in two mobile phases, five parametric linear models were suggested (R2train = 0.93 and 0.97; R2test = 0.93 and 0.99). The models were also evaluated with different statistical approaches. It was shown that increasing the sum of geometrical distances between N and O in AAs causes decreasing their RF in RP-TLC using both mobile phases. Other structural effects of AAs on their separation in the desired RP-TLC system were also discussed. 相似文献
23.
White-Morris RL Stender M Tinti DS Balch AL Rios D Attar S 《Inorganic chemistry》2003,42(10):3237-3244
The preparation and X-ray crystal structures of (CyNC)Au(I)CN, (n-BuNC)Au(I)CN, and (i-PrNC)Au(I)CN.0.5CH(2)Cl(2) are reported and compared with those of (MeNC)Au(I)CN and (t-BuNC)Au(I)CN, which were previously described. These linear molecules are all organized through aurophilic interactions into three structural classes: simple chains ((CyNC)Au(I)CN and (t-BuNC)Au(I)CN), side-by-side chains in which two strands make Au...Au contact with each other ((n-BuNC)Au(I)CN), and nets in which multiple aurophilic interactions produce layers of gold(I) centers ((i-PrNC)Au(I)CN and (MeNC)Au(I)CN). All of these five solids dissolve to produce colorless, nonluminescent solutions with similar UV/vis spectra. However, each of the solids displays a unique luminescence with emission maxima occurring in the range 371-430 nm. 相似文献
24.
Aamer Saeed 《Chemistry of Heterocyclic Compounds》2007,43(8):1072-1075
An efficient, rapid, microwave-accelerated one-step synthesis of some 5-aryl-2-(2-hydroxy-phenyl)-1,3,4-oxadiazoles by reaction
of salicylic hydrazide with carboxylic acids in the presence of thionyl chloride under neat conditions is described.
__________
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 8, pp. 1264–1267, August, 2007. 相似文献
25.
[11C]Carbon monoxide at low concentrations, aryl halides and amines were used in the palladium-mediated synthesis of twenty 11C-amides. In the study several approaches to improve the radiochemical yield were explored. Eight of the selected amides were prepared by in situ activation of the amines using lithium bis(trimethylsilyl)amide and the radiochemical yields of these reactions were improved compared to utilising a previous reported method. In the synthesis of 1-[carbonyl-11C]benzoyl-3-methyl-1H-indole (11) from 3-methyl-1H-indole (25), the corresponding organotin-amine was prepared prior to the acylation reaction. In a typical experiment, N-(4-hydroxyphenyl)[carbonyl-11C]acetamide (5) was prepared in 15% radiochemical yield using 4-aminophenol (20) but the yield increased to 63% when the amine was activated by lithium bis(trimethylsilyl)amide. 相似文献
26.
A simple and environment friendly method was developed for determination of Malathion content of analytical and commercial insecticide samples with no special preparation. Attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectra were characterized and 1000-2000 cm−1 region was selected for quantitative analysis utilizing partial least square (PLS) and two wavelength selection methods: (a) principal component regression (PCR) and (b) genetic algorithm (GA). Relative error of prediction (REP) was calculated in PLS, PCR-PLS and GA-PLS methods and was 3.536, 1.656 and 0.188, respectively. Proposed method is successfully applicable for quantification of Malathion in commercial grade samples and reliable results in comparison with known methods, confirms this idea. 相似文献
27.
M. N. Cheema M. Mufazzal Saeed Akbar Ali Munir Ahmed 《Journal of Radioanalytical and Nuclear Chemistry》1994,178(1):153-163
Extraction of Hg(II), Se(IV), Mn(II) and Co(II) has been carried out with 1-phenyl-3-methyl-4-trifluoroacetyl-2-pyrazolin-5-one (HPMTFP) and triphenylphosphine oxide (TPPO) into chloroform from pH 1–10. Quantitative extraction of Hg(II), Mn(II) and Co(II) at pH 4 with equimolar 0.05M (PMTFP+TPPO) in chloroform was observed. Se(IV) remains unextracted at this pH range. The stoichiometric composition of the extracted complexes M(PMTFP)2·nH2O (M=Mn, Hg), M(PMTFP)2·2TPPO (M=Mn and Co) and Co(PMTFP)2·TPPO·H2O at less than 0.1M TPPO has been established. The formation constantsK
m,0 andK
m,n and stability constants
m,n have been computed. The analytical method developed was applied to the IAEA standard reference material (SRM) potato fluor V-4 for the determination of these elements using NAA technique. 相似文献
28.
Aggregation and dispersion characteristics of calcium oxalate monohydrate: effect of urinary species
Christmas KG Gower LB Khan SR El-Shall H 《Journal of colloid and interface science》2002,256(1):168-174
In this research, screening and central composite experimental designs are used to determine the effect of various factors on the aggregation and dispersion characteristics of previously grown calcium oxalate monohydrate (COM) crystals in artificial urinary environments of controlled variables. The variables examined are pH and calcium, oxalate, pyrophosphate, citrate, and protein concentrations in ultrapure water and artificial urine. Optical density measurements, particle size analysis, optical microscopy, AFM force measurements, and protein adsorption have been used to assess the state of aggregation and dispersion of the COM crystals and to elucidate the mechanisms involved in such a complex system. The data indicate that our model protein, mucin, acts as a dispersant. This is attributed to steric hindrance resulting from the adsorbed mucoprotein. Oxalate, however, promotes aggregation. Interesting interactions between protein and oxalate along with protein and citrate are observed. Such interactions (synergistic or antagonistic) are found to depend on the concentrations of these species. Surface responses for these interactions are presented and discussed in this paper. In summary, solution, surface, and interface chemistries interact in a complex manner in the physiological environment to either inhibit or promote aggregation, and an understanding of such interactions may help determine and control the factors affecting kidney stone formation. 相似文献
29.
Mohammad Ali Karimi Mohammad Mazloum Ardakani Omran Moradlou Reza Behjatmanesh‐Ardakani Fatemeh Banifatemeh 《中国化学会会志》2007,54(1):15-21
Simultaneous kinetic‐spectrophotometric determination of a ternary mixture of hydrazine (HZ) and its derivatives by principal component regression (PCR) and partial least squares (PLS) calibration is described. The methods were based on the difference observed in the reduction rate of iron(III) with HZ, thiosemicarbazide (TSCZ) and phenylhydrazine (PHZ) in the presence of 2,2′‐bipyridine (Bpy). The colored complex of [Fe(Bpy)3]2+ was formed in sodium dodecyl sulfate (SDS) as micellar media, and then monitored at 520 nm. The results showed that simultaneous determination of HZ, TSCZ and PHZ could be performed in their concentration ranges of 1.0–70.0, 0.2–6.0 and 0.1–10.0 μg mL?1, respectively. The root mean squares errors of prediction (RMSEP) of HZ, TSCZ and PHZ were 0.719, 0.164 and 0.105 (for PLS) 0.788, 0.166 and 0.993 (for PCR), respectively. Both methods (PCR and PLS) were validated using a set of synthetic sample mixtures and then applied for simultaneous determination of HZ, TSCZ and PHZ in water samples. 相似文献
30.
The title complexes, the Re(O)L(2)(Solv)(+) complexes (L = hoz, 2-(2'-hydroxyphenyl)-2-oxazoline(-) or thoz, 2-(2'-hydroxyphenyl)-2-thiazoline(-); Solv = H(2)O or CH(3)CN), are effective catalysts for the following fundamental oxo transfer reaction between closed shell molecules: XO + Y --> X + YO. Among suitable oxygen acceptors (Y's) are organic thioethers and phosphines, and among suitable oxo donors (XO's) are pyridine N-oxide (PyO), t-BuOOH, and inorganic oxyanions. One of the remarkable features of these catalysts is their high kinetic competency in effecting perchlorate reduction by pure atom transfer. Oxo transfer to rhenium(V) proceeds cleanly to afford the cationic dioxorhenium(VII) complex Re(O)(2)L(2)(+) in a two-step mechanism, rapid substrate (XO) coordination to give the precursor adduct cis-Re(V)(O)(OX)L(2)(+) followed by oxygen atom transfer (OAT) as the rate determining step. Electronic variations with PyO derivatives demonstrated that electron-withdrawing substituents accelerate the rate of Re(VII)(O)(2)L(2)(+) formation from the precursor adduct cis-Re(V)(O)(OX)L(2)(+). The activation parameters for OAT with picoline N-oxide and chlorate have been measured; the entropic barrier to oxo transfer is essentially zero. The potential energy surface for the reaction of Re(O)(hoz)(2)(OH(2))(+) with PyO was defined, and all pertinent intermediates and transition states along the reaction pathway were located by density functional theory (DFT) calculations (B3LYP/6-31G). In the second half of the catalytic cycle, Re(O)(2)L(2)(+) reacts with oxygen acceptors (Y's) in second-order reactions with associative transition states. The rate of OAT to substrates spans a remarkable range of 0.1-10(6) L mol(-)(1) s(-)(1), and the substrate reactivity order is Ph(3)P > dialkyl sulfides > alkyl aryl sulfides > Ph(2)S approximately DMSO, which demonstrates electrophilic oxo transfer. Competing deactivation and inhibitory pathways as well as their relevant kinetics are also reported. 相似文献