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1.
建立了测定白酒中6种邻苯二甲酸酯类增塑剂的真空离心浓缩/气相色谱-质谱联用(GC-MS)分析方法。样品经真空离心浓缩,正己烷提取,取上层正己烷,4000r/min离心5min,采用GC-MS测定,外标法定量。在0.10~5.00μg/mL范围内,相关系数r20.992,样品在0.10~2.00 mg/kg范围内加标,平均回收率在88.83%~111.67%之间,相对标准偏差(RSD)为4.85%~11.35%,检出限(LOD)在0.02~0.05 mg/kg之间。采用该方法对16个白酒样品进行测定,结果表明该法简便、快速、结果准确可靠、灵敏度高,能够满足白酒中6种邻苯二甲酸酯增塑剂检测需求。  相似文献   
2.
The present research aims to characterize the particle size distribution of sub micron particles suspended in a liquid. The particles milled are an organic poorly water soluble crystalline product. To characterize the size of these particles, different techniques have been tested: imaging techniques (SEM, CryoTEM), static light scattering techniques, dynamic light scattering techniques, centrifugation and flow field flow fractionation. The results indicate that the studied milled particles have a primary particle size close to 180nm and there is strong evidence of larger particles which are very likely aggregates. This is clearly seen from the Cryo TEM results. All the above mentioned techniques should in principle be able to measure samples of dispersion containing particles of ca 180 nm but several are disturbed by the presence of large aggregates. It is difficult to estimate the amount of aggregate present, but most of the time one is interested in what the primary particle size distribution is. It is clear that no single piece of equipment is capable of exactly determining the particle size distribution of our samples, but the static light scattering with low shear on mixing does give a good representation of what is seen with the image analysis by cryo TEM.  相似文献   
3.
建立了高效液相色谱测定直接型与氧化型染发剂中11种氨基苯酚含量的分析方法。样品在亚硫酸氢钠的保护下用甲醇提取,高速冷冻离心净化;采用Agilent Zorbax SB C18色谱柱分离,流动相为5 mmol/L庚烷磺酸钠-40 mmol/L pH 2.8磷酸盐缓冲液和乙腈,梯度洗脱,11种氨基苯酚分别于230、270和400 nm下检测。11种氨基苯酚在0.05~500 mg/L线性范围内相关系数不小于0.9992,4-氨基-3-硝基苯酚、2-氨基-5-硝基苯酚、3-硝基-4-(2-羟乙基)氨基苯酚的方法定量限为5 mg/kg,其他8种氨基苯酚包括对氨基苯酚、对甲氨基苯酚、间氨基苯酚、邻氨基苯酚、5-氨基-2-甲基苯酚、4-氨基-3-甲基苯酚、2-甲基-5-(2-羟乙基)氨基苯酚和2-氨基-4-硝基苯酚定量限为20 mg/kg,方法回收率为88.5%~109.5%,相对标准偏差为2.2%~8.3%。测定了多种市售染发剂,结果表明该方法操作简单、测定结果准确,可用于直接型与氧化型染发剂中11种氨基苯酚的测定。  相似文献   
4.
An analytical method using inductively coupled plasma atomic emission spectrometry (ICP-AES) for rapid simultaneous determination of seven heavy metals (Cd, Co, Cr, Cu, Mn, Ni and Pb) in human blood fractions, like plasma, cells fraction and whole blood, is performed. The optimum wavelength was selected using as criterions the sensitivity, the linearity and recovery of aqueous standard solutions. The pretreatment of the sample, the centrifugal conditions, the necessity of digestion and the dilution of the digests were also studied. For plasma it was possible to avoid digestion of the sample, but for cells fractions and whole blood the digestion is necessary. The samples were acid-digested by HNO3 in closed Teflon tubes under high temperature and pressure conditions and were diluted before injection into ICP-AES. Also, optimization of the inductively coupled plasma conditions like nebulizer argon flow rate, sample flow rate and power of radio frequency was performed for each analyte. Finally, the effect of the type of the employed calibration technique on the total variation of the method was examined. Calibration using the standard addition technique was proved more accurate for the determination in terms of analyte recovery. The sensitivity and recovery (Cd 99%, Co 101%, Cr 100%, Cu 99%, Mn 101%, Ni 100% and Pb 97%) of the developed method are presented for all examined blood fractions. Correspondence: George A. Zachariadis, Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University, Thessaloniki 54124, Greece  相似文献   
5.
Nanocrystalline cellulose (NCC) was prepared by sulfuric acid hydrolysis of microcrystalline cellulose. A differential centrifugation technique was studied to obtain NCC whiskers with a narrow size distribution. It was shown that the volume of NCC in different fractions had an inverse relationship with relative centrifugal force (RCF). The length of NCC whiskers was also fractionized by differential RCF. The aspect ratio of NCC in different fractions had a relatively narrow range. This technique provides an easy way of producing NCC whiskers with a narrow size distribution.  相似文献   
6.
A theoretical analysis is presented of viscous incompressible laminar flow in a pipe which rotates around an axis held at small angle with respect to its symmetry-axis. Analogous to the results of Barua and Benton [1, 2], solutions in closed-form are given for circulatory flows in the cross-sectional plane of the pipe due to Coriolis forces in combination with Hagen-Poiseuille flow through the pipe. The solutions are used to derive analytical expressions for trajectories of solid or liquid particles entrained in the gas and being subject to centrifugation and the said secondary flows. It is shown that despite centrifugation, particles can be locked into circulatory trajectories thus remaining suspended in the gas flowing through the pipe.  相似文献   
7.
The synthesis and the study of DC electrical transport properties (electrical conductivity, σ, and Seebeck coefficient, S) as a function of temperature of some recently synthesized nylon 6/12 copolymers with 0, 5, 10, 20, 30, and 50 wt % laurolactam (LL), respectively, are reported. Nylons were obtained by rotational molding via the anionic activated copolymerization of ε‐caprolactam and LL. As evidenced by XRD analyses, they are semicrystalline. The temperature dependences of σ and S are typical for polycrystalline semiconducting (p‐type) materials. The activation energy of electrical conduction lay in the range 0.79–1.22 eV, while the ratio of charge carrier mobilities ranged between 0.53 and 0.77. © 2007 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 45: 794–799, 2007  相似文献   
8.
建立了液相色谱-串联质谱(HPLC-MS/MS)同时测定人血浆中的亚叶酸和5-甲基四氢叶酸两对非对映异构体的方法。血浆经蛋白质沉淀-超滤离心处理后,以甲氨蝶呤为内标,乙腈-10 mmol/L pH 8.0醋酸铵为流动相,通过手性HSA色谱柱(150 mm×4 mm,5 μm)进行梯度洗脱。亚叶酸非对映异构体在25~5000 μg/L范围内、5-甲基四氢叶酸非对映异构体在12.5~2500 μg/L范围内,线性关系均良好。本方法在灵敏度、精密度、准确度、基质效应、提取回收率、稳定性等方面均得到充分验证,并成功应用于125 mg/m2亚叶酸和62.5 mg/m2左旋亚叶酸的药代动力学研究。结果显示:在125 mg/m2亚叶酸剂量组,左亚叶酸和左旋-5-甲基四氢叶酸的血浆峰浓度(Cmax)为(3137.917±408.837)和(1679.633±244.132)μg/L,从时间点0到最后可定量时间点的药物代谢动力学时间曲线下面积(AUC0-t)为(7504.883±1185.101)和(14001.214±2868.949)μg/L;在62.5 mg/m2左亚叶酸剂量组,左亚叶酸和左旋-5-甲基四氢叶酸的Cmax为(3187.917±387.298)和(1739.204±224.755)μg/L,AUC0-t为(7426.664±854.825)和(14884.331±1843.353)μg/L。两剂量组主要药物代谢动力学参数均无显著差异,特征一致,吸收的速度和程度一致,能够为后期进行左亚叶酸钠生物等效性研究提供技术支持。  相似文献   
9.
Particles ranging from ca. 0.1 to 1.0m in 5 ml of pond water are collected on a 10–20 nm carbon film on a gold or copper specimen grid, placed on a special holder in a 7-ml centrifuge tube, by centrifugation at 10000 r. p. m. for 18 min. The specimens thus prepared are reproducible and preserve the morphology of the particles satisfactorily. The proposed technique is more suitable than filtration, direct drying and spray drying techniques for morphological studies and elemental analysis of individual particles with scanning, transmission and analytical electron microscopes.  相似文献   
10.
经过K2S2O8的稀硫酸溶液氧化处理的粗制单壁碳纳米管样品, 在水、DMF 和乙醇等极性溶剂中具有非常好的溶解性. 通过在DMF介质中多次进行超声波分散和高速离心分离, 成功地获得了高纯度可溶性的单壁碳纳米管. UV-vis-NIR吸收光谱研究表明, 这种高纯度可溶性的单壁碳纳米管呈现出更多的吸收特征和更高的吸收强度. 进一步的研究表明, 单壁碳纳米管的纯度达到了“参比样品”的160%, 其单根分散度达到5%以上.  相似文献   
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