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171.
建立了测定尿液中3种羟基多环芳烃的氮化碳复合材料磁性固相萃取结合高效液相色谱-荧光检测法。所构筑的磁性氮化碳材料,经扫描电子显微镜、X射线衍射仪、振动样品磁强计和比表面积分析仪表征后,用于尿液中3种羟基多环芳烃的富集净化。考察了吸附剂用量、吸附时间、洗脱溶液和洗脱体积(单次洗脱体积×洗脱次数)对萃取效率的影响。结合高效液相色谱-荧光分析,在0.25~250 μg/L范围内线性关系良好(相关系数r=0.999),3种羟基多环芳烃的检出限和定量限分别为0.08和0.25 μg/L,回收率为90.1%~102%,日内和日间精密度分别为1.5%~7.7%和2.2%~8.7%。该本方法简单、快速、高效,可用于尿液中羟基多环芳烃的分析。 相似文献
172.
Andrzej Czopnik Nataly Shitsevalova Alexander Krivchikov Vasyl Pluzhnikov Yuriy Paderno 《Journal of solid state chemistry》2004,177(2):507-514
We have measured heat capacity and thermal expansion of rare earth dodecaborides REB12 (RE=Y, Tb-Tm, Lu). YB12 and LuB12 are diamagnetics whereas the other dodecaborides are ordered antiferromagnetically. The amplitude of the heat capacity discontinuity at the Néel temperature and the shape of the heat capacity variation in the critical region for all these antiferromagnetics are characteristics for amplitude-modulated magnetic structures. In the ordered state TbB12 reveals two first-order phase transitions, most likely due to magnetic structure changes. The heat capacity of ErB12 just below the Néel point shows an anomaly of unclear origin. From the Schottky contribution to the heat capacity we have determined crystal field parameters. They are completely different than that is estimated from Point Charge Model. 相似文献
173.
174.
K. Grob 《Journal of separation science》1980,3(6):286-290
The sensitivity of an FID may change when the carrier gas flow rate changes during a chromatographic run. Sample parts which are eluted at reduced FID sensitivity produce a reduced peak area, hence are discriminated as compared to other components. Sensitivity changes were studied for hydrogen as carrier gas. For the detector tested, differences in the carrier gas flow rates of 1 ml/min shifted the FID sensitivity by 1 to 5% (depending on the fuel gas supply). Thus the stability of the sensitivity is no longer ensured as soon as the carrier gas flow rate is changed manually or by an automatic programmer during an analysis. Sensitivity drifts may also occur during temperature programmed runs with a pressure regulated carrier gas supply since the gas flow through the capillary drops with increasing temperature. Such shifts in the response became noticeable as soon as relatively high carrier gas flow rates combined with long range temperature programmes were used. The typical patterns of such discriminations are shown, closing with a discussion on the possibilities for minimizing such undesired effects. 相似文献
175.
一种低磁矩、大功率复合稀土石榴石铁氧体的工艺和性能研究 总被引:4,自引:0,他引:4
为满足低场区几百兆赫的超大功率器件的性能要求,以钇铁石榴石铁氧体为基础,制备了一种低磁矩复合稀土石榴石铁氧体YGd CaVInIG,研究了少量Mn3+替代Fe3+和预烧温度、烧结温度对铁氧体性能和结构的影响。实验表明,以少量Mn3+替代Fe3+可以提高铁氧体电阻率,降低磁损耗和介电损耗。Mn3+掺入量以x为0.04~0.06比较合适,铁氧体最佳予烧温度为1050℃,最佳烧结温度1350~1380℃,保温5h,氧气中烧结,其性能为:4πMs=500±10%kA·m-1,ΔH=5.25~5.55kA·m-1,TC>180℃,tgδe≤0.5×10-5,这种材料适合微波低频段器件性能要求。X射线衍射分析指出,掺Mn3+的YGdCaVInIG铁氧体相变完全,呈单相复合石榴石铁氧体,空间群为I230,点阵常数1.25057~1.25101nm,单胞分子数n为7.75~7.80。 相似文献
176.
Pt3Co核-Pt壳型纳米粒子的制备及磁性 总被引:1,自引:1,他引:1
Pt3Co alloy nanoparticles were prepared by the reduction of H2PtCl6 and Co(OOCCH3)2 using NaBH4 as a reducing agent. The Pt3Co core-Pt shell nanoparticles (Pt3Co@Pt) were synthesized using hydrogen absorption reduction and characterized by plasma-atomic emission spectrometry (ICP), transmission electron microscopy (TEM), X-ray diffraction (XRD) and SQUID magnetometer. The results show that average size of Pt3Co@Pt nanoparticles is 3.6 nm with a standard deviation of 0.9 nm. Heating Pt3Co nanoparticles in air at 700 ℃ for 1 h, Co in Pt3Co nanoparticles was oxidized to Co3O4 and CoO; while no oxidation tendency was detected for Pt3Co@Pt nanoparticles. The crystallize structure of Pt3Co@Pt changed from the face centered cube (fcc) to the face centered tetragonal (fct) after the heating treatment. The coercivity of the heated Pt3Co@Pt reached to 276 Oe at room temperature. 相似文献
177.
活性酚醛树脂中羟甲基含量的测定 总被引:12,自引:0,他引:12
本文提出一种酚醛树脂中羟甲基含量的化学分析法,分别以^13CNMR和化学分析法测定酚醛树脂的羟甲基含量。将两种测试结果与已知的投料量进行比较,证明所建立的化学分析法可行。 相似文献
178.
The synthesis and characterisation of five newβ-aminodiketones is reported: (a) 3,3,5,8,10,10-hexamethyl-5,8-diazadodecane-2,11-dione; (b) 3,3,11,11-tetramethyl-5,8-diazatridecane-2,12-dione;
(c) 3,3,12,12-tetramethyl-5,10-diazatetradecane-2,13-dione; (d) 3,3,10,10-tetramethyl-5,8-diphenyl-5,8-diazadodecane-2,11,dione
and (e) 6,7-benzo-3,3,10,10-tetramethyl-5,8-diazadodecane-2,11-dione. These compounds are discussed as potential precursors
in the synthesis of tetra-aza macrocyclic complexes. 相似文献
179.
180.
Zanolari B Wolfender JL Guilet D Marston A Queiroz EF Paulo MQ Hostettmann K 《Journal of chromatography. A》2003,1020(1):75-89
The bark of catuaba (Erythroxylum vacciniifolium Martius, Erythroxylaceae), a tree native to the northern part of Brazil, was investigated for its alkaloid content. With the aim of obtaining preliminary structure information on-line, the alkaloid extract was analysed by high-performance liquid chromatography coupled to diode array UV detection, to mass spectrometry and to nuclear magnetic resonance. Interpretation of on-line spectroscopic data obtained from this extract led to structural elucidation of six new alkaloids and partial identification of 18 potentially original alkaloids bearing the same tropane skeleton esterified in positions 3 and 6 by 1-methyl-1H-pyrrol-2-carboxylic acid and/or 4-hydroxy-3,5-dimethoxybenzoic acid. 相似文献