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21.
Žydrė Šaltienė Natalija Jatulienė Mudis Šalkauskas Daiva Brukštienė Asta Ruzgytė Aušra Tarasevičiūtė Julius Kalibatas 《Accreditation and quality assurance》2005,10(8):444-451
The estimation scheme of uncertainty of determination of 1-hydroxypyrene (1-OHP) in urine was developed analysing the main
stages of the analytical procedure: (1) preparation of 1-OHP standards, (2) creation of the calibration curve for the high
performance liquid chromatography (HPLC) analysis method with the evaluation of recovery, (3) measuring procedure of aliquot
of urine, (4) adjusting the pH of aliquot and hydrolysis with enzyme, (5) solid phase extraction, (6) concentration of the
extract, (7) injection of the extract to chromatograph and analysing by the HPLC method, (8) calculation of 1-OHP mass from
the calibration curve, (9) calculation of 1-OHP concentration in urine. The evaluation of the uncertainty is based on quantification
of individual components. Combined uncertainty was calculated using the law of propagation of uncertainties according to the
EURACHEM/CITAC guidelines. Level dependence of the uncertainty arises from the calibration curve.
The limits of detection and quantification were found to be equal to 0.03 and 0.1 ng/mL, respectively. The calculated expanded
level-dependent uncertainty covers 47–27–25% within the concentration range 0.03–0.1–0.4 ng/mL with the materials and equipment
used. These parameters could easily be recalculated according to the proposed scheme if there are some changes in the analysis
procedure. 相似文献
22.
I. Kuselman 《Accreditation and quality assurance》1998,3(3):131-133
It is argued that results of uncertainty calculations in chemical analysis should be taken into consideration with some caution
owing to their limited generality. The issue of the uncertainty in uncertainty estimation is discussed in two aspects. The
first is due to the differences between procedure-oriented and result-oriented uncertainty assessments, and the second is
due to the differences between the theoretical calculation of uncertainty and its quantication using the validation (experimental)
data. It is shown that the uncertainty calculation for instrumental analytical methods using a regression calibration curve
is result-oriented and meaningful only until the next calibration. A scheme for evaluation of the uncertainty in uncertainty
calculation by statistical analysis of experimental data is given and illustrated with examples from the author's practice.
Some recommendations for the design of corresponding experiments are formulated. 相似文献
23.
Reliable, traceable and comparable measurements provide the rational basis for evaluation of the quality of a result and
the starting point for recognized laboratory accreditation in any national area. Modern medical diagnostics and treatment
involve rapidly rising numbers and types of clinical laboratory measurements, that are reliable. Therefore, the basic principles
to be followed to assure the traceability of clinical measurements as required by the Romanian Laws of Metrology are reviewed.
Main sources affecting the quality of the unbroken chain of calibrations that relate the measurements back to appropriate
measurement standards are discussed. Examples of how to achieve traceable measurements in clinical laboratories are presented.
Details of specific uses of reference materials, measuring instruments and standard measurement methods are also discussed.
Received: 8 January 1998 · Accepted: 21 April 1998 相似文献
24.
S. Küppers 《Accreditation and quality assurance》1997,2(1):30-35
Any analytical data is used to provide information about a sample. The "possible error" of the measurement can be of extreme
importance in order to have complete information. The measurement uncertainty concept is a way to achieve quantitative information
about this "possible error" using an estimation procedure. On the basis of the analytical result, the chemist makes a decision
on the next step of the development process. If the uncertainty is unknown, the information is not complete; therefore this
decision might be impossible. The major problem for the in-process control (IPC) procedure is that not only the repeatability
but also the intermediate precision (which expresses the variations within laboratories related to different days, different
analysts, different equipment, etc.) has to be good enough to make a decision. Unfortunately, the statistical information
achieved from one single analytical run only gives information about the repeatability. This paper shows that the estimation
of the measurement uncertainty for IPC is a way to solve the problem and gives the necessary information about the quality
of the procedure. An example demonstrates that an estimate of uncertainty based on the standard deviations of an analytical
method gives a value similar to one based on the standard deviations obtained from a control chart. Therefore, the estimation
is both a very useful and also a very cost-effective tool. Though measurement uncertainty cannot replace validation in general,
it is a viable alternative to validation for all methods that will never be used routinely.
Received: 24 May 1996 Accepted: 10 August 1996 相似文献
25.
采用重量-容量法制备丙酮中除虫脲溶液标准物质。准确称量国家二级标准物质除虫脲溶解到色谱纯丙酮中,通过A级容量瓶定容至500 mL,摇匀后分装到2 mL安瓿瓶内共460瓶,每瓶为1 mL,保持低温迅速封口,配制过程中室温保持在(20±2)℃。采用液相色谱法进行均匀性、稳定性检验和定值结果验证。从样品中随机抽取16瓶进行均匀性检验,经F检验表明,在95%的置信区间范围内该标准物质均匀性良好;采用t检验对标准物质稳定性进行检验,标准物质在12月内稳定性良好。对该标准物质的不确定度进行了评定,研制的丙酮中除虫脲溶液标准物质定值结果为100μg/mL,相对扩展不确定度为2%(k=2)。结果表明,该标准物质均匀性与稳定性良好,量值准确,可用于日常分析检测中的方法评价和仪器校准。 相似文献
26.
A procedure for estimation of measurement uncertainty of routine pH measurement (pH meter with two-point calibration, with
or without automatic temperature compensation, combination glass electrode) based on the ISO method is presented. It is based
on a mathematical model of pH measurement that involves nine input parameters. Altogether 14 components of uncertainty are
identified and quantified. No single uncertainty estimate can be ascribed to a pH measurement procedure: the uncertainty of
pH strongly depends on changes in experimental details and on the pH value itself. The uncertainty is the lowest near the
isopotential point and in the center of the calibration line and can increase by a factor of 2 (depending on the details of
the measurement procedure) when moving from around pH 7 to around pH 2 or 11. Therefore it is necessary to estimate the uncertainty
separately for each measurement. For routine pH measurement the uncertainty cannot be significantly reduced by using more
accurate standard solutions than ±0.02 pH units – the uncertainty improvement is small. A major problem in estimating the
uncertainty of pH is the residual junction potential, which is almost impossible to take rigorously into account in the framework
of a routine pH measurement.1
Received: 11 August 2001 Accepted: 22 February 2002 相似文献
27.
不确定金融是不确定理论在现代金融领域的一种应用,在解决金融问题中发挥着越来越重要的作用。而利率是一个重要的经济指标,经常受到一些不确定因素的影响,在研究期权定价时,有必要考虑浮动利率。本文提出了一种新的不确定指数Ornstein-Uhlenbeck过程模型,假设利率服从不确定均值回复过程,研究了期权定价问题,运用α-轨道方法,分别推导了亚式看涨期权和看跌期权定价公式。最后,设计了计算期权价格的数值算法,并给出数值算例。 相似文献
28.
Stephen L. R. Ellison 《Accreditation and quality assurance》2005,10(7):338-343
A spreadsheet method allowing rapid calculation of combined standard uncertainties is described. The model used allows explicitly
for correlation effects, and requires a user to enter only the parameters, the calculation used to obtain the final result
(including relevant influence factors), the individual standard uncertainties for the parameters, and estimates of correlation
coefficients where necessary. The estimation of correlation coefficients in common cases is discussed, and it is shown that
correlation is likely to be practically significant only when the correlated contribution to individual standard uncertainties
is significantly over about 30% of the relevant standard uncertainty, leading to correlation coefficients |r| greater than 0.1. The implementation includes a more robust differentiation algorithm than previously reported for spreadsheet
use, and initial preparation of the spreadsheets has been automated. The principle is illustrated with a simple example.
Electronic Supplementary Material Supplementary material is available in the online version of this article at and is accessible for authorized users.
相似文献
Stephen L. R. EllisonEmail: |
29.
This work deals with uncertainty analysis of the thermal conductivity measurement using the transient hot wire method. The characterization is made from a sample of low-density, polyethylene BRALEN SA 200-22. The utilized experimental data are obtained from the test measurements performed on the air at room temperature. The sources of measurement errors are analyzed and the uncertainty of the measured value of the thermal conductivity is evaluated. The analysis shows that in the present case the uncertainty of the thermal conductivity measurement is about ±3.3% for 68% confidence level.This revised version was published online in November 2005 with corrections to the Cover Date. 相似文献
30.
讨论了铀同位素标准物质(UIRM)研制中的一些技术问题,如IRM中同位素丰度的定值,IRM不确定度的影响因素等,并介绍了国内外UIRM研制情况。 相似文献