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91.
Summary The advantages and disadvantages of high performance precipitation liquid chromatography have been demonstrated for polystyrene
homopolymers. Depending on the mobile phase composition at the dissolution point of the polymeric sample and surface properties
of the stationary phase, elution is governed either by a solution process or by adsorption. A contribution by adsorption was
noticed on silica as well as on reversed phases based on silica with a normal phase gradient of increasing polarity (heptane
to dichloromethane). Elution was solely governed by solubility of the polymers on both types of stationary phase for polystyrenes
with a molecular weight above 35 000 and reversed phase gradient of decreasing polarity (methanol to dichloromethane). Under
these conditions an identical dependence of elution solvent composition on sample size was found as for turbidity titrations.
Due to differences in the velocity of the eluent front and the polymeric sample with porous stationary phases the polymers
can be eluted as colloidal solutions Non-porous stationary phases are superior in this respect because the velocities of eluent
and solutes are identical. 相似文献
92.
建立了同时测定水产品中四溴双酚A(TBBPA)和六溴环十二烷(HBCD)的超高效液相色谱-串联质谱方法。样品前处理采用QuEChERS方法,均质生物样品用水分散后加乙腈提取,经C_(18)分散固相萃取净化。采用CORTECS~?C_(18)色谱柱(4.6 mm×100 mm×2.7μm)分离,以甲醇-水为流动相进行梯度洗脱,流速为0.7 mL/min。采用电喷雾离子源,在负离子模式下以多反应监测(MRM)方式检测。结果表明,TBBPA和3种HBCD单体在0.5~500μg/L范围内线性良好,相关系数(r)大于0.998,检出限(LOD,S/N=3)和定量下限(LOQ,S/N=10)分别为0.04~0.16μg/kg和0.12~0.55μg/kg。在5、20、50μg/kg加标水平下的平均回收率为74.0%~121%,相对标准偏差(RSD)为0.20%~23%。该方法操作简单、快速、重现性好,适用于水产品中TBBPA和HBCD的快速检测。 相似文献
93.
高效液相色谱与原子荧光光谱联用分析汞化合物形态的研究 总被引:15,自引:2,他引:15
建立了高效液相色谱与原子荧光光谱联用测定汞化合物形态的分析方法。实验对淋洗液组分浓度、氧化剂和还原剂浓度、载气流速及紫外消解管长度等操作条件进行了优化,获得了令人满意的分析结果。在优化的分离检测条件下,20μg/L的汞化合物标准溶液平行7次进样分析,甲基汞、无机汞和乙基汞的色谱峰高的相对标准偏差(RSD)分别为2.0%、2.9%和2.4%;3种汞化合物的线性范围为10~1000μg/L,25μL进样检出限分别为3、2和4μg/L。用建立的方法测定了脉红螺样品中甲基汞的含量,甲基汞和乙基汞的加标回收率分别为90%和92%。 相似文献
94.
95.
96.
A rapid and reliable high performance liquid chromatographic (HPLC) method for the simultaneous determination of heterocyclic
compounds, namely nicotinic acid, nicotinamide, and 3-cyanopyridine, in industrial effluent is described. A Φ4.6 mm × 150
mm, 5 μm C-18 reversed phase stationery phase, and a methanol-acetonitrile-water tertiary mobile phase (20:20:60 v/v) were
used for separation. The detection wavelength of a diode array (DAD) was set at 216 nm with a bandwidth of 16 nm. Phenol was
used as an internal standard. The regression equations revealed a linear relationship between the concentration of the analytes
injected and the peak area detected by DAD. The limits of detection (S/N = 3) ranged from 0.70 to 1.18 mg L−1, the recoveries ranged from 87% to 102% and the precision expressed as % RSD intra-day and inter-day varied from 0.9 to 3.9
and 1.2 to 5.6, respectively. This method is rapid, sensitive and suitable for the monitoring of nicotinic acid, nicotinamide,
and 3-cyanopyridine in effluent of related pharmaceutical manufacturing plants. 相似文献
97.
CuO在ZrO2上的分散状态及其对催化性能的影响 总被引:7,自引:3,他引:7
用XRD、TPR和TPD-MS等手段表征了浸渍法制备的CuO/ZrO2催化剂,发现ZrO2上高度分散的氧化铜具有显著的易被还原和再氧化的特性,从而催化剂具有高的CO氧化活性。 相似文献
98.
Wen-Jia Zhou Shu-Juan Bao Yan-Yu Liang Ben-Lin He Hu-Lin Li 《Journal of Solid State Electrochemistry》2006,10(5):277-282
Pure-phase and well-crystallized spinel LiMn2O4 powders were successfully synthesized by a simple rheological phase method. The thermal behavior and structure properties
of the powders prepared by the rheological phase method compared with the solid-state reaction were investigated by thermogravimetry,
powder X-ray diffraction , scanning electron microscopy and transmission electron microscopy. According to the results of
the electrochemical tests, it is obvious that the sample resulting from the rheological phase method shows higher discharge
capacity and better cycling stability than one formed in the solid-state reaction. The cyclic voltammogram and columbic efficiency
curves also confirm that the product by the rheological phase method has a good cycling performance due to its fine cubic
spinel structure and morphology. 相似文献
99.
建立了全自动QuEChERS样品制备系统结合高效液相色谱-串联质谱(HPLC-MS/MS)同时检测植物源性食品中34种农药残留的分析方法。方法利用全自动QuEChERS样品制备系统涡旋振动和离心功能,将手动QuEChERS方法中样品提取和分散固相萃取相结合;优化了操作参数及前处理步骤,在多反应监测(MRM)模式下检测,基质匹配外标法定量。从方法学验证角度对全自动QuEChERS法与手动QuEChERS法进行了比较。结果表明:该方法中大多数农药在一定范围内呈现良好的线性关系,相关系数(R2)均大于0.99,检出限为0.76~3.60 μg/kg,定量限为2.28~10.80 μg/kg,加标回收率为53.0%~125.2%,相对标准偏差(RSD)<15.9%(n=5)。该方法与手动QuEChERS法的方法验证比对结果显示差异不明显,用于植物源性食品中多农药残留检测可有效降低劳动强度和出错概率。 相似文献
100.
Mechanical properties of BPDA-ODA polyimide fibers 总被引:1,自引:0,他引:1
An aromatic polyimide was synthesized via a one-step polycondensation reaction between biphenyltetracarboxylic dianhydride (BPDA) and 4,4′-oxydianiline (ODA) in p-chlorophenol. The polyimide (BPDA-ODA) solution dopes were spun into fibers by means of dry-jet wet spinning. The as-spun fibers were drawn and treated in heating tubes for improving the mechanical properties. The thermal treatment on the fibers resulted in a relatively high tensile strength and modulus. Thermal mechanical analysis (TMA) was employed to study the linear coefficient of thermal expansion (CTE). Thermal gravimetry analysis (TGA) spectra showed that the BPDA-ODA fibers possessed an excellent property of thermo-oxidative degradation resistance. The sonic modulus Es of the polyimide fibers was measured. 相似文献