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1.
《Electroanalysis》2004,16(9):748-756
A strategy for constructing a global multivariate calibration model that includes calibration samples measured over time on different days is developed and applied in electroanalysis. Both synthetic and real samples (tap, extracted and river water) are analyzed by differential‐pulse anodic stripping voltammetry, showing the suitability of the global model constructed that provides successful results similar to those of the usual multivariate calibration. In addition the capability of discrimination of this model is evaluated in prediction for the mean of three replicates with estimation of probability of false noncompliance, α, and false compliance, β, being found 3.1, 11.2, 6.7 and 64.7 nM for nominal concentrations of zinc, cadmium, lead and copper of 96.0, 40.4, 37.3 and 328.0 nM respectively when α=β=0.05. It has been proven that the use of the global calibration does not imply a loss of multivariate analytical sensitivity, using this parameter as quality index of the analytical procedure. The viability of using calibration maintenance strategies with electroanalytical techniques is shown, providing a way to save time and experimental effort when these techniques are used in routine analysis. 相似文献
2.
P. Davies 《Accreditation and quality assurance》1996,1(6):240-246
Laboratory accreditation is becoming increasingly accepted around the world as a means of identifying technically competent
laboratories. It is also being used as a mechanism for the acceptance of test data both nationally and internationally. The
concept and mechanisms of accreditation have been developed over the past 50 years. The first national laboratory accreditation
system appeared in Australia in 1947. This organisation, known as the National Association of Testing Authorities (NATA),
has since taken a leading role in developing accreditation practices that are now used world-wide in evaluating testing, measurement
and calibration laboratories. This paper examines the development of the world's first and largest laboratory accreditation
system, and looks at the difficulties and triumphs in gaining acceptance and recognition by government and industry of the
benefits of laboratory accreditation.
Received: 24 June 1996 Accepted: 25 June 1996 相似文献
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R. Hoelzl Christian Hoelzl Ludwig Kotz Lazlo Fabry 《Accreditation and quality assurance》1998,3(5):185-188
Inductively coupled plasma mass spectrometry (ICP-MS) and high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS)
are powerful methods of determining metallic impurities in the low- and sub-ppt level in process media such as ultra-pure
water used in semiconductor and wafer manufacturing. By using mass spectrometers for analysis, an isotope dilution analysis
(IDMS) is possible. The reproducibility of an IDMS is unmatched. For concentration levels near the instrument detection limit
a novel method is reported to find the optimal amount of isotopic spike solution. This optimal value can be derived by the
law of propagation of uncertainty combined with the Poisson statistics of the measured number of counts. Generally, an excess
of isotopic spike solution should be used to provide results of lowest possible uncertainty. The results are presented in
a diagram for easy practical use.
Received: 14 October 1997 · Accepted: 13 February 1998 相似文献
6.
Summary The concept of a diffusion-averaged molecular weight, Md is presented, and Md is defined for polydisperse samples. It is shown via oligostyrene mixtures that Md can be determined in 20 minutes with common chromatographic equipment. If Md is measured and Mn or Mw is known, the polydispersity can be obtained. 相似文献
7.
Cuadros-Rodríguez L Almansa-López EM García-Campaña AM González-Casado A Egea-González FJ Garrido-Frenich A Martínez-Vidal JL 《Talanta》2005,66(4):1063-1072
The use of the recovery term has presented some confusion in Analytical Chemistry. Recent IUPAC recommendations propose to distinguish between two terms: recovery or recovery factor, ℜ, and apparent recovery, ℜ*. Apparent recovery includes recovery factor and a new recovery term proposed in this paper, named calibration recovery, ℜC, which depends of the type of systematic error due to the matrix effect (constant and/or proportional) and is related to the applied calibration methodology. This paper highlights the dependence of the calibration recovery on the sample analyte concentration and, for extension, of the apparent recovery, defines the recovery profile, and makes evident the need to determine a “fit for purpose” analyte concentration interval to comply with a regulated recovery requirements. An approach to estimate the calibration recovery and its associated uncertainty in relation to the above-mentioned dependence is presented. The usefulness of the proposed methodology has been shown in the quantification of a pesticide by GC-ECD for assessing dermal exposure. 相似文献
8.
气相渗透法广泛用于测定齐聚物和低分子量聚合物的数均分子量(M_n)。分析文献数据和本文的实验证明,仪器常数K值随溶质的分子量而变化。本文提出了一种新的说明 VPO法 K值依赖于溶质分子量的模式,根据此模式,可清楚地说明这种依赖关系。 相似文献
9.
《Journal of separation science》2003,26(11):1057-1062
The use of glass fiber as a support material for a surface compound serving to generate gaseous standard mixtures of ethene is described. The technique is based on the process of thermal decomposition of the surface compound in a desorber connected on‐line via a multi‐port valve to the calibrated device. The surface compound undergoes thermal decomposition at 245°C, yielding known amounts of ethene. The method enables on‐line preparation of a standard mixture immediately before the calibration step. Consequently, it can be also applied for the generation of standard mixtures containing volatile, malodorous, unstable, and toxic compounds. 相似文献
10.
The application of a new method to the multivariate analysis of incomplete data sets is described. The new method, called maximum likelihood principal component analysis (MLPCA), is analogous to conventional principal component analysis (PCA), but incorporates measurement error variance information in the decomposition of multivariate data. Missing measurements can be handled in a reliable and simple manner by assigning large measurement uncertainties to them. The problem of missing data is pervasive in chemistry, and MLPCA is applied to three sets of experimental data to illustrate its utility. For exploratory data analysis, a data set from the analysis of archeological artifacts is used to show that the principal components extracted by MLPCA retain much of the original information even when a significant number of measurements are missing. Maximum likelihood projections of censored data can often preserve original clusters among the samples and can, through the propagation of error, indicate which samples are likely to be projected erroneously. To demonstrate its utility in modeling applications, MLPCA is also applied in the development of a model for chromatographic retention based on a data set which is only 80% complete. MLPCA can predict missing values and assign error estimates to these points. Finally, the problem of calibration transfer between instruments can be regarded as a missing data problem in which entire spectra are missing on the ‘slave’ instrument. Using NIR spectra obtained from two instruments, it is shown that spectra on the slave instrument can be predicted from a small subset of calibration transfer samples even if a different wavelength range is employed. Concentration prediction errors obtained by this approach were comparable to cross-validation errors obtained for the slave instrument when all spectra were available. 相似文献