全文获取类型
收费全文 | 2424篇 |
免费 | 267篇 |
国内免费 | 165篇 |
专业分类
化学 | 1033篇 |
力学 | 188篇 |
综合类 | 20篇 |
数学 | 349篇 |
物理学 | 1266篇 |
出版年
2024年 | 5篇 |
2023年 | 17篇 |
2022年 | 50篇 |
2021年 | 35篇 |
2020年 | 52篇 |
2019年 | 48篇 |
2018年 | 36篇 |
2017年 | 83篇 |
2016年 | 112篇 |
2015年 | 95篇 |
2014年 | 147篇 |
2013年 | 201篇 |
2012年 | 205篇 |
2011年 | 172篇 |
2010年 | 135篇 |
2009年 | 171篇 |
2008年 | 158篇 |
2007年 | 169篇 |
2006年 | 117篇 |
2005年 | 120篇 |
2004年 | 121篇 |
2003年 | 80篇 |
2002年 | 65篇 |
2001年 | 57篇 |
2000年 | 58篇 |
1999年 | 44篇 |
1998年 | 39篇 |
1997年 | 44篇 |
1996年 | 39篇 |
1995年 | 22篇 |
1994年 | 26篇 |
1993年 | 29篇 |
1992年 | 19篇 |
1991年 | 14篇 |
1990年 | 12篇 |
1989年 | 4篇 |
1988年 | 9篇 |
1987年 | 3篇 |
1986年 | 6篇 |
1985年 | 7篇 |
1984年 | 7篇 |
1983年 | 2篇 |
1982年 | 9篇 |
1981年 | 5篇 |
1980年 | 1篇 |
1979年 | 3篇 |
1978年 | 1篇 |
1973年 | 1篇 |
1957年 | 1篇 |
排序方式: 共有2856条查询结果,搜索用时 609 毫秒
51.
B A Finnin M A A O'Neill S Gaisford A E Beezer J Hadgraft P Sears 《Journal of Thermal Analysis and Calorimetry》2006,83(2):331-334
Isothermal
calorimetry is becoming indispensable as a tool for the study of a wide variety
of systems. As with all scientific instruments it is essential that robust
calibration routines be developed in order to validate the data obtained.
Chemical test reactions offer many advantages over (the traditionally used)
joule effect heating methods, not least because they have the potential to
validate instrument performance (i.e. they can be used to assess all aspects
of calorimeter operation). In this work the results of a validation exercise,
conducted by Thermal Hazard Technology as part of an installation routine,
using the base catalysed hydrolysis of methyl paraben are discussed. In the
case described, a systematic misreporting of the reported temperature of a
calorimeter was identified, caused by an upgrade to the calorimeter's
firmware, a discrepancy which may not have been noted using traditional electrical
calibration methods and one which highlights the importance of both manufacturers
and end-users adopting chemical test reactions into their test and validation
routines. 相似文献
52.
A method is proposed for the simultaneous determination of albumin and immunoglobulin G (IgG1) with fluorescence spectroscopy and multivariate calibration with partial least squares regression (PLS). The influence of some instrumental parameters were investigated with two experimental designs comprising 19 and 11 experiments, respectively. The investigated parameters were excitation and emission slit, detection voltage and scan rate. When a suitable instrumental setting had been found, a minor calibration and test set were analysed and evaluated. Thereafter, a larger calibration of albumin and IgG1 was made out of 26 samples (0-42 μg ml−1 albumin and 0-12.7 μg ml−1 IgG1). This calibration was validated with a test set consisting of 14 samples in the same concentration range. The precision of the method was estimated by analysing two test set samples for six times each. The scan modes tested were emission scan and synchronous scan Δ60 nm. The results showed that the method could be used for determination of albumin and IgG1 (albumin, root mean square error of prediction (RMSEP) <2, relative standard error of prediction (RSEP) <6% and IgG1, RMSEP <1, RSEP <8%) in spite of the overlapping fluorescence of the two compounds. The estimated precision was relative standard deviation (R.S.D.) <1.7%. The method was finally applied for the analysis of some sample fractions from an albumin standard used in affinity chromatography. 相似文献
53.
54.
A new approach is developed for estimating the limit of detection in second-order bilinear calibration with the generalized rank annihilation method (GRAM). The proposed estimator is based on recently derived expressions for prediction variance and bias. It follows the latest IUPAC recommendations in the sense that it concisely accounts for the probabilities of committing both types I and II errors, i.e. false positive and false negative declarations, respectively. The estimator has been extensively validated with simulated data, yielding promising results. 相似文献
55.
Y. Ladino-Ospina L. Giraldo-Gutierréz J. C. Moreno-Piraján 《Journal of Thermal Analysis and Calorimetry》2005,81(2):435-440
Summary This work shows the result of the study of the Pb(II) and Cr(VI) ions adsorption by means of a Calvet type calorimeter of heat conduction that can operate at 150şC. The calorimeter was electrically calibrated to establish its sensitivity and reproducibility, obtaining K=12.95±0.05 W V-1 and chemically it was examined with tris-(hydroxymethyl)-aminomethane (THAM)-HCl system, obtaining ΔH= -30.91±0.03 kJ mol-1. The activated carbon sample obtained from coffee husk and the calorimetric results obtained were related to other techniques used to perform this type of studies. 相似文献
56.
A. Gustavo González M. Ángeles Herrador Agustín G. Asuero 《Accreditation and quality assurance》2005,10(7):386-391
The uncertainty evaluation of mass measurements when using “in-house” calibrated analytical balances is revisited according
to the Guide to the expression of Uncertainty Measurement (GUM). The calibration of analytical balances is discussed according
to the guidelines of several bodies such as ASTM, UKAS and DKD/PTB. The remainder components of uncertainty can be estimated
from the balance data sheet specifications. 相似文献
57.
凝胶渗透色谱法测定聚丙烯腈共聚物分子量中宽分布校正法的应用 总被引:4,自引:0,他引:4
应用宽分布校正法对凝胶渗透色谱(GPC)进行了校正,将校正曲线用于聚丙烯腈(PAN)共聚物分子量的计算。对扣除色谱峰扩展效应前后的测试结果与乌氏粘度法测得的数据进行比较。结果表明,应用宽分布校正法时,必须扣除色谱峰扩展效应,才能得到较为准确的测试结果。 相似文献
58.
Interference-free determination of Sudan dyes in chilli foods using second-order calibration algorithms coupled with HPLC-DAD 总被引:1,自引:0,他引:1
This paper presents a new method for the determination of Sudan dyes contained in hot chilli samples. The method employs second-order calibration algorithms to handle the recorded data. The second-order calibration algorithms are based on the popular parallel factor analysis (PARAFAC), alternating trilinear decomposition (ATLD) and self-weighted alternating trilinear decomposition (SWATLD), respectively. These chemometric methodologies have the second-order advantage, which is the ability to get accurate concentration estimates of interested analytes even in the presence of uncalibrated interfering components. The results on a set of spiked chilli test shows that low contents of Sudan I and Sudan II in complex chilli mixtures can be accurately determined using the new method. The sample preparation was based on solvent extraction, and internal standard was not required. Quantification was carried out with simple mobile phase. 相似文献
59.
V. A. Drebushchak 《Journal of Thermal Analysis and Calorimetry》2005,79(1):213-218
One-point (Mettler) and many-point (Netzsch) heat flow calibration of a DSC is discussed. It is shown that the two types of calibration are the alternative extremes between quick but rough procedure and time-consuming but accurate one. One-point calibration compares a typical function k(T) at the melting point of indium with the measured value for particular DSC and multiplies k(T) by a scaling factor. Many-point calibration is based on general mathematical procedure, namely fitting a set of experimental values of sensitivity to a polynomial. The polynomial coefficients are evaluated by the method of least squares. Based on the relationship between the sensitivity of a thermocouple and calibration coefficient of a DSC sensor made from it, two-point heat flow calibration is suggested. This is an optimal calibration procedure, for the relationship contains only two unknown coefficients. An example of how to perform the two-point calibration with Netzsch-Proteus Software is described in the Appendix. 相似文献
60.
Fabrizio Casarini Luigi Marcheselli Andrea Marchetti Lorenzo Tassi Giuseppe Tosi 《Journal of solution chemistry》1993,22(10):895-905
The relative permittivities for the ternary 1,2-ethanediol (component 1) + 2-methoxyethanol (2) + water (3) solvent system have been measured for 66 mixtures covering the whole mole fraction composition 0X1/X2/X3 1 range at –10, –5 and 0 °C. The experimental data were used to test some empirical relations stating the dependence of = (X1, X2, X3). A comparison between the calculated and experimental data show that these equations can be usefully employed to predict values in correspondence of the experimental data gaps. 相似文献