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31.
Removal of humic matter interference in the determination of Cr(VI) in soil extracts by the diphenylcarbazide method 总被引:1,自引:0,他引:1
Alkaline digestion of soil samples, which is recommended for minimizing Cr(III)–Cr(VI) interconversions during the extraction of Cr(VI), may also solubilize humic matter (HM). The latter is responsible for both positive and negative interference in the analysis of Cr(VI) in the extract by the diphenylcarbazide (DPC) method. Humic compounds indeed absorb light at 540 nm as the Cr-DPC product and are also able to rapidly reduce Cr(VI) under the pH conditions of the standard DPC method. To prevent any risk of interference and make the DPC method applicable to soil extracts, a new protocol is proposed. This consists of three successive steps: (1) extraction of Cr(VI) by the U.S.EPA method 3060A in the presence of Mg2+; (2) batch removal of solubilised HM by the XAD-7 sorbent at pH 3.0 ± 0.1 with 3–5 min contact time; (3) analysis of Cr(VI) with the DPC method at pH 3.0 ± 0.1. The application of this new protocol to the soil product SQC-012 Lot 4 certified by R.T. Corporation (RTC, USA) gave significantly lower Cr(VI) concentrations and smaller variability compared to certified values (46.5 ± 2.3 instead of 153 ± 32.6 mg/kg). The new protocol was validated by Cr(VI) and Cr(III) spikes either to the soil/extractant suspension or to the exctract. Cr(VI) results in the wide range of acceptance limits (104–202 mg/kg) reported by RTC were only obtained when the U.S.EPA method 3060A without the addition of Mg2+ and DPC analysis at pH 1.0 were applied. The latter procedure appears questionable since it leads to largely variable results which reflect the complex role played by humic matter in the determination of Cr(VI) and the instability of Cr(III) during the extraction. 相似文献
32.
Extracting organotin compounds (OTC) from soils is difficult due to the high cation exchange and complexation capacity of soils, and little information about OTC in soils is available. In this study, a new extraction method, combining 1 M CaCl2, 0.1% tropolone, and glacial acetic acid was developed. Recoveries of mono-substituted OTC from spiked plant litter, and soil samples were improved substantially to 40% compared to classical glacial acetic acid extraction commonly used in sedimentology, yielding <10% recovery in C-rich soil samples. Simultaneously, the recovery of other OTC, trimethyllead and monomethylmercury was satisfactory. The recoveries of most species from the spiked litter, upland and wetland soils exceeded 70%. The new method extracted much more organometallics from unspiked organic soils and litter than microwave- and ultrasound-assisted extraction and accelerated solvent extraction, most likely due to exchange of organometallics from the solid phase by Ca2+. The method is simple, highly efficient and with low contamination. Together with GC-ICP-mass spectrometry, the method allows the detection of these organometallics in the pg g−1 range and it is particularly suitable for soil and plant materials with low organometallics contents. 相似文献
33.
MITIC Snezana ZIVANOVIC Valentina OBRADOVIC Mirjana TOSIC Snezana PAVLOVIC Aleksandra 《中国化学》2007,25(4):531-534
The kinetic method for the determination of phosphate microamounts was described. The developed method is based on catalytic effect of phosphate on sodium pyrogallol-5-sulphonate (PS) by dissolved oxygen. The reaction was followed spectrophotometrically by measuring the rate of change in the values of the absorbance of the oxidation product at 437 nm. The optimum reaction conditions are PS (0.44×10^-3 mol·L^-1) and HClO4 (3.6×10^-6 mol·L^-1) at 25 ℃. Following this procedure, phosphate can be determined with a linear calibration graph up to 0.23 μg·mL^-1. The interference effect of several species was also investigated and it was found that the most common cations and anions did not interfere with the determination. The developed procedure was successfully applied to the determination of phosphate in natural waters and soil. 相似文献
34.
Digrazia Philip M. Blackburn James W. Bienkowski Paul R. Hilton Barry Reed Gregory D. King J. M. Henry Sayler Gary S. 《Applied biochemistry and biotechnology》1990,(1):237-252
An experimental and mathematical method is developed for the microbial systems analysis of polyaromatic hydrocarbon (PAH)-degrading
mixed cultures in PAH-contaminated “town gas” soil systems. Frequency response is the primary experimental and data analysis
tool used to probe the structure of these complicated systems. The objective is to provide a fundamental protocol for evaluating
the performance of specific mixed microbial cultures on specific soil systems by elucidating the salient system variables
and their interactions. Two well-described reactor systems, a constant volume stirred tank reactor (CSTR) and a plug flow
differential volume reactor, are used in order to remove performance effects that are related to reactor type as opposed to
system structure. These two reactor systems are well-defined systems that can be described mathematically and represent the
two extremes of one potentially important system variable, macroscopic mass transfer. The experimental and mathematical structure
of the protocol is described, experimental data is presented, and data analysis is demonstrated for the stripping, sorption,
and biodegradation of napththalene. 相似文献
35.
Three non-specific methods for the extraction of total petroleum hydrocarbons (TPH) from soil into organic solvent were compared.
The techniques used for sample preparation were Soxhlet extraction, closed-vessel microwave-assisted extraction, and CEN shake
extraction. The total concentrations of extracted compounds in the boiling point range of C10–C40 were determined by gas chromatography
with flame ionization detection. The best recovery (99%) and repeatability (±3%) from standard oil mixtures were obtained
with microwave-assisted extraction. However, the different extraction methods exhibited different behaviour when spiked soil
samples were extracted. The best repeatability was obtained with CEN shake extraction (±6%) but the repeatability values for
Soxhlet and microwave-assisted methods were quite high (>20%). However, the larger uncertainties of the latter extraction
methods does not necessarily limit the applicability of these methods to the determination of petroleum hydrocarbons in soil,
as in the assessment of soil contamination the expanded uncertainty of the result is usually not limited by analytical uncertainty,
but rather by the uncertainty of the primary sampling stage. However, distinctive variation found in the chromatographic profiles
illustrates that discretion should be obeyed when chromatograms obtained after application of different extraction methods
on petroleum contaminated samples are to be used in the fingerprinting or age dating studies. Otherwise, misleading conclusions
concerning the age of spillage could be drawn. 相似文献
36.
痕量砷流动注射在线还原氢化物发生原子吸收测定 总被引:5,自引:0,他引:5
方法采用流动注射停流技术使水及土壤浸出液中As(V)在线还原为As(Ⅲ),不经手工还原,用氢化物发生原子吸收光谱法直接测定砷的含量。含4mol/L HCl的样品溶液与30%碘化钾溶液在编结式反应器中混合,并在采样环中停流40s,达完全还原后注入到载流中与硼氢化钠反应,采样速度55次/h,检出限(3δ)0.1μg/L,对自来水和土壤浸出液的加标回收结果满意。 相似文献
37.
Peter Schramel 《Mikrochimica acta》1989,99(3-6):355-364
The most sensitive emission lines for the elements B, Be, Co and Mo are strongly influenced by disturbing emission lines of Fe using normal optical resolution. The advantages of high resolution, applying the new ICP-spectrometer JY 38 Plus (Jobin-Yvon, France) with the 2400 lines/mm grating measuring in the 1st and 2nd order will be discussed. Beside the concentrations in soils, sediments and sludges, applying aqua regia and HF decomposition methods, the detection limits in these matrices will be given. The possibilities of ICP-spectrometry for the determination of the above-mentioned elements are shown at the examples of SRMs (standard reference materials). The materials used here were three soils and three sludges from the BCR (Community Bureau of Reference, European Communities) and one sediment from NBS (National Bureau of Standards, USA). For example, the most sensitive and normally used line for the determination of boron at 249.7733 nm cannot be used in case of this type of matrix due to normally high Fe-concentrations and due to a strong Fe-interference. Therefore, it is necessary to use the line at 249.6778 nm, where an interference-free measurement can be achieved in case of high optical resolution. The measured B-contents in these samples are in the range of 20 to 60 g/g, for Co in the 10 g/g region, for Be well below 1 g/g, for Sn between 3 and 400 g/g. Mo was only detectable in the sludge samples (limit of determination 0.5 g/g).Presented in part at the 1989 European Winter Conference on Plasma Spectrochemistry, Reutte, Austria 相似文献
38.
An alternative to traditional hydrocarbon bioremediation is to pump air through unsaturated soils to create aerobic conditions
and induce biodegradation. This study examines the effects of moisture and nutrient augmentation on biodegradation of petroleum
hydrocarbons in aerated soils. Findings indicate that forced aeration, coupled with additions of nutrients and moisture, stimulate
hydrocarbon-degrading microorganisms and present a feasible approach to bioremediation management. 相似文献
39.
Arelí Durón-Castellanos Vanesa Zazueta-Novoa Hortencia Silva-Jiménez Yolanda Alvarado-Caudillo Eduardo Peña Cabrera Roberto Zazueta-Sandoval 《Applied biochemistry and biotechnology》2005,121(1-3):279-288
Different soluble NAD+-dependent alcohol dehydrogenase (ADH) isozymes were detected in cell-free homogenates from aerobically grown mycelia of YR-1
strain of Mucor circinelloides isolated from petroleumcontaminated soil samples. Depending on the carbon source present in the growth media, multiple NAD+-dependent ADHs were detected when hexadecane or decane was used as the sole carbon source in the culture media. ADH activities
from aerobically or anaerobically grown mycelium or yeast cells, respectively, were detected when growth medium with glucose
added was the sole carbon source; the enzyme activity exhibited optimum pH for the oxidation of different alcohols (methanol,
ethanol, and hexadecanol) similar to that of the corresponding aldehyde (≈7.0). Zymogram analysis conducted with partially
purified fractions of extracts from aerobic mycelium or anaerobic yeast cells of the YR-1 strain grown in glucose as the sole
carbon source indicated the presence of a single NAD+-dependent ADH enzyme in each case, and the activity level was higher in the yeast cells. ADH enzyme from mycelium grown in
different carbon sources showed high activity using ethanol as substrate, although higher activity was displayed when the
cells were grown in hexadecane as the sole carbon source. Zymogram analysis with these extracts showed that this particular
strain of M. circinelloides has four different isozymes with ADH activity and, interestingly, one of them, ADH4, was identified also as phenanthrene-diol-dehydrogenase,
an enzyme that possibly participates in the aromatic hydrocarbon biodegradation pathway. 相似文献
40.
红树林湿地土壤矿物的分析 总被引:2,自引:0,他引:2
以湛江湾南海堤典型红树林湿地土壤为研究对象,采用X射线衍射(XRD)和傅立叶变换红外光谱(FTIR)快速批量鉴定土壤中矿物成分,利用扫描电子显微镜(SEM)观察土壤颗粒形貌特征并获得化学成分组成信息;同时采集附近光滩土壤样品进行对比研究,以揭示红树林湿地土壤特殊的生态环境特征。结果表明,红树林湿地土壤矿物主要由高岭石、石英、白云母、埃洛石、地开石和蛇纹石等组成;与光滩土壤相比,红树林湿地土壤矿物类型多样,而光滩土壤矿物相对单一,主要为石英和高岭石;红树林湿地土壤颗粒以片状聚合体为主,主要元素组成为C、O、S、Al、Si、Mg、Fe等,常见含有Cu、Zn、Mo等重金属元素。同时发现红树林湿地土壤颗粒含有较丰富的硫化物;而光滩土壤未发现上述特征,表明红树林湿地处于一个特殊的生态环境,土壤沉积物中富含有机质、Fe、S等,比一般潮滩更易于富集硫化物或重金属。 相似文献