全文获取类型
收费全文 | 1253篇 |
免费 | 20篇 |
国内免费 | 11篇 |
专业分类
化学 | 1123篇 |
力学 | 8篇 |
综合类 | 11篇 |
数学 | 5篇 |
物理学 | 137篇 |
出版年
2024年 | 5篇 |
2023年 | 25篇 |
2022年 | 34篇 |
2021年 | 49篇 |
2020年 | 37篇 |
2019年 | 21篇 |
2018年 | 15篇 |
2017年 | 32篇 |
2016年 | 47篇 |
2015年 | 41篇 |
2014年 | 45篇 |
2013年 | 51篇 |
2012年 | 87篇 |
2011年 | 94篇 |
2010年 | 72篇 |
2009年 | 89篇 |
2008年 | 60篇 |
2007年 | 86篇 |
2006年 | 63篇 |
2005年 | 73篇 |
2004年 | 53篇 |
2003年 | 50篇 |
2002年 | 28篇 |
2001年 | 21篇 |
2000年 | 20篇 |
1999年 | 12篇 |
1998年 | 7篇 |
1997年 | 7篇 |
1996年 | 15篇 |
1995年 | 9篇 |
1994年 | 2篇 |
1993年 | 6篇 |
1992年 | 8篇 |
1991年 | 6篇 |
1990年 | 6篇 |
1989年 | 3篇 |
1988年 | 2篇 |
1985年 | 1篇 |
1984年 | 2篇 |
排序方式: 共有1284条查询结果,搜索用时 31 毫秒
41.
42.
采用微波制样技术,用石墨炉原子吸收光谱法测定水产品中痕量铍。方法的线性范围为0-10μg·L-1,检出限为0.076 ng·g-1,相对标准偏差为2.7%,回收率为97.0%。方法准确、快速、简便,并与常压消解法的结果比较,基本一致,已用于水产品中痕量铍的测定。 相似文献
43.
A microwave-assisted digestion procedure using HNO3, HF, and H2O2 has been developed for analysis of elements in ambient particulate matter (PM). The samples are collected on cellulose filters and analyzed by inductively coupled plasma mass spectrometry (ICP-MS). The ICP-MS is calibrated with external standards, and recovery of analytes is tested with NIST SRM 1648 Urban Dust. This method has been used to quantify the airborne concentrations of a large number of elements, including Ag, As, Ba, Be, Ca, Cd, Ce, Co, Cr, Cs, Cu, Fe, Ga, K, Li, Mg, Mn, Mo, Ni, Pb, Rb, Se, Sb, Sr, Ti, Tl, V, and Zn. For the majority of these elements, recovery of the NIST SRM is within 15% of the certified values. 相似文献
44.
The microwave acid digestion method was applied to the decomposition of rock samples and optimum conditions were investigated. Samples of 10–100 mg were decomposed by changing the amount and composition of acid, heating time and number of reheating steps and then the concentrations of Si, Fe, Mn, Na, K and Mg in these samples were measured. The concentrations agreed with reported values when 10 mg of sample were decomposed by heating for 60 s with 0.3 ml of concentrated HNO3 and 0.1 ml of concentrated HF. Similarly, 100 mg of sample were also decomposed successfully by heating for 45–110 s with 0.3–1.0 ml of concentrated HNO3 and 0.4–0.7 ml of concentrated HF. It is concluded that the microwave acid digestion method decomposes rock samples with a very short heating time and with small amount of reagents compared with methods using conventional sealed PTFE vessels, which require several hours for the heating step and several millilitres of reagents. 相似文献
45.
The High Pressure Asher (HPA-S) was adapted with a Teflon liner for pressurized wet digestion in open vessels. The autoclave was partly filled with water containing 5% (vol/vol) hydrogen peroxide. The digestion vessels dipped partly into the water or were arranged on top of the water by means of a special rack made of titanium or PTFE-coated stainless steel. The HPA-S was closed and pressurized with nitrogen up to 100 bars. The maximum digestion temperature was 250 °C for PFA vessels and 270 °C for quartz vessels. Digestion vessels made of quartz or PFA-Teflon with volumes between 1.5 mL (auto sampler cups) and 50 mL were tested. The maximum sample amount for quartz vessels was 0.5–1.5 g and for PFA vessels 0.2–0.5 g, depending on the material. Higher sample intake may lead to fast reactions with losses of digestion solution. The samples were digested with 5 mL HNO3 or with 2 mL HNO3+6 mL H2O+2 mL H2O2. The total digestion time was 90–120 min and 30 min for cooling down to room temperature. Auto sampler cups made of PFA were used as digestion vessels for GFAAS. Sample material (50 mg) was digested with 0.2 mL HNO3+0.5 mL H2O+0.2 mL H2O2. The analytical data of nine certified reference materials are also within the confidential intervals for volatile elements like mercury, selenium and arsenic. No cross contamination between the digestion vessels could be observed. Due to the high gas pressure, the diffusion rate of volatile species is low and losses of elements by volatilisation could be observed only with diluted nitric acid and vessels with large cross section. In addition, cocoa, walnuts, nicotinic acid, pumpkin seeds, lubrication oil, straw, polyethylene and coal were digested and the TOC values measured. The residual carbon content came to 0.2–10% depending on the sample matrix and amount. 相似文献
46.
Renata Wietecha Paweł Kościelniak Teresa Lech Tomasz Kielar 《Mikrochimica acta》2005,149(1-2):137-144
This study describes a simple, rapid and reliable method for simultaneous determination of selenium and arsenic in human hair by means of atomic fluorescence spectrometry combined with a hydride generation technique (HG-AFS). The procedure developed encompasses microwave digestion of a sample in the nitric acid environment only. The interferences caused by nitrous oxides are eliminated by removing a gas from above the digested solution with a stream of argon. The sample is then chemically treated in a flow-through hydride generation system and exposed to measurements in a double-channel atomic fluorescence spectrometer. The method permits determining both analytes in the linear range of 0.5–100µgL–1 with a detection limit equal to 0.2µgL–1, as well as with very good repeatability not exceeding 1% for Se and 2% for As. No mutual interferences from either of the analytes in the concentrations ranges matching the hair composition were found. The method was verified in terms of accuracy with the use of a reference material and then applied to the analysis of the natural samples of human hair. 相似文献
47.
Samuel Melaku Ilse Gelaude Frank Vanhaecke Luc Moens Richard Dams 《Mikrochimica acta》2003,142(1-2):7-12
Microwave digestion reduction-aeration and pyrolysis combined with cold vapour atomic absorption and cold vapour atomic fluorescence
are compared for the determination of total mercury in several biological and environmental matrices. The biological samples
were digested in a mixture of HNO3/H2O2, the environmental samples in a mixture of HNO3/HClO4. After reduction with SnCl2, the mercury was collected by two-stage gold amalgamation. After microwave digestion reduction-aeration, detection limits
of 1.4 ng g−1 and 0.6 ng g−1 were obtained for cold vapour atomic absorption spectrometry (CVAAS) and cold vapour atomic fluorescence spectrometry (CVAFS),
respectively, for 250 mg of environmental samples. For biological samples (500 mg) the detection limits were 0.7 ng g−1 (CVAAS) and 0.4 ng g−1 (CVAFS). After pyrolysis, detection limits of 3.5 ng g−1 and 1.6 ng g−1 for CVAAS and CVAFS, respectively, were obtained for a 10 mg sample. Pyrolysis can only be applied when the organic content
of the sample is not too high. Accurate results were obtained for 8 certified reference materials of both environmental and
biological origin. In addition, a real sludge sample was analysed.
Author for correspondence. E-mail: richard.dams@rug.ac.be
Received September 18, 2002; accepted December 3, 2002
Published online May 5, 2003 相似文献
48.
Simplified method for the Re-Os dating of molybdenite using acid digestion and isotope dilution ICP-MS 总被引:1,自引:0,他引:1
An analytical method was developed for Os-Re dating of molybdenite. The method is based on determination of Os and Re concentrations in molybdenite by isotope dilution inductively-coupled plasma mass spectrometry (ID-ICP-MS). Sample digestion and sample/spike equilibration were achieved by a two-stage autoclave-based procedure using a mixture of nitric and sulphuric acids. Os was separated from the sample digest by modified single-stage distillation of osmium tetraoxide (OsO4) using elevated temperature and on-line addition of hydrogen peroxide. OsO4(g) was trapped in a mixture of 0.05% thiourea in 0.05 M sodium hydroxide. An anion-exchange column was used to separate Re from excess Mo in the solution remaining after distillation. Os and Re isotope ratio measurements were performed by single-collector, double focusing inductively-coupled plasma mass spectrometry (ICP-MS) with on-line mass-bias correction. Typical instrumental precision was in the range 0.02-0.2% relative standard deviation (R.S.D.) depending on the analyte concentrations. Notorious Os memory effects in the ICP-MS introduction system were eliminated using 5% ammonia solution, both as matrix for final dilution of the trap mixture as well as for washing between the samples. The reproducibility of the entire analytical procedure was accessed by replicate dating of two molybdenite standards and three molybdenite separates, and was found to be in the range 0.87-1.52% R.S.D. Though accuracy of the method is limited by difficulties in evaluating exact concentration of Os in spike solution, ages obtained in the course of these work agrees well with previously published data. 相似文献
49.
The pretreatment of waste-activated sludge (WAS) by electron beam irradiation was studied in order to improve anaerobic sludge
digestion. The irradiation dose of the electron beam was varied from 0.5 to 10 kGy. Batch and continuous-flow stirred tank
reactors (CFSTRs) were operated to evaluate the effect of the electron beam pretreatment on anaerobic sludge digestion. Approximately
30–52% of the total chemical oxygen demand (COD) content of the WAS was solubilized within 24 h after electron beam irradiation.
A large quantity of soluble COD, protein, and carbohydrates leached out from cell ruptures caused by the electron beam irradiation.
Volatile fatty acids production from the irradiated sludge was approx 90% higher than that of the unirradiated sludge. The
degradation of irradiated sewage sludge was described by two distinct first-order decay rates (k
1 and k
2). Most initial decay reaction accelerated within 10 d, with an average k
1 of 0.06/d for sewage sludge irradiated at all dosages. The mean values for the long-term batch first-order decay coefficient
(k
2) were 0.025/d for irradiated sewage sludge and 0.007/d for unirradiated sludge. Volatile solids removal efficiency of the
control reactor fed with unirradiated sewage sludge at a hydraulic retention time (HRT) of 20 d was almost the same as that
of the CFSTRs fed with irradiated sludge at an HRT of 10 d. Therefore, disintegration of sewage sludge cells using electron
beam pretreatment could reduce the reactor solid retention time by half. 相似文献
50.
Efforts were made to assess the efficiency of an anaerobic filter packed with porous floating ceramic media and to identify
the optimum operational condition of anaerobic filter as a pretreatment of swine wastewater for the subsequent biological
removal of nitrogen and phosphorus. A stepwise decrease in hydraulic retention time (HRT) and an increase in organic loading
rate (OLR) were utilized in an anaerobic filter reactor at mesophilic temperature (35°C). The optimum operating condition
of the anaerobic filter was found to be at an HRT of 1 d. A soluble chemical oxygen demand (COD) removal efficiency of 62%
and a total suspended solids removal efficiency of 39% at an HRT of 1 d were achieved with an OLR of 16.0 kg total COD/(m3·d), respectively. The maximum methane production rate approached 1.70 vol of biogas produced per volume of reactor per day
at an HRT of 1 d. It was likely that the effluent COD/total Kjeldahl nitrogen ratio, of 22, the COD/total phosphorous ratio
of 47, and the high effluent alkalinity >2500 mg/L as CaCO3 of the anaerobic filter operated at an HRT of 1 d was adequate for the subsequent biological removal of nitrogen and phosphorus. 相似文献