石菖蒲根中微量元素的含量分析

目的：运用火焰原子吸收光谱法测定中药石菖蒲根中的 Fe、 Zn、 Mg、 Ca、 Cu 5种金属元素的含量。方法用浓 HNO3-HClO4消解样品,采用标准曲线法测定其5种金属元素含量。结果所测的样品中含有丰富的人体必需微量元素,尤其是 Fe 含量极高。方法回收率在98．60％～104．60％之间,样品相对偏差小于5％。结论该法简单、准确,结果令人满意。     

火焰原子吸收法测定中草药地胆草中微量元素的含量

目的运用火焰原子吸收光谱法测定中草药地胆草中的Fe、Zn、Mg、Ca、Cu5种微量元素的含量。方法用浓HNO3-HCIO4消解样品,采用标准曲线法测定其五种金属元素含量。结果所测的样品中含有丰富的人体必需微量元素,Ca含量尤其丰富,高达12225μg／g。方法回收率在99．4％～104．0％之间,样品相对偏差小于5％。结论该法快速简便、重复性好、准确度好,适用于同类生物样品中微量元素的测定,结果令人满意。     

火焰原子吸收法测定翼梗五味子中微量元素的含量

目的：运用火焰原子吸收光谱法测定中草药翼梗五味子藤中的 Fe、 Zn、 Mg、 Ca、 Cu 5种微量元素的含量。方法用浓 HNO3-HClO4消解样品,采用标准曲线法测定其5种金属元素含量。结果所测的样品中含有丰富的人体必需微量元素, Ca 含量尤其丰富,高达15827μg/g。方法回收率在99．7％～105．0％之间,样品相对偏差小于5％。结论该法快速简便、重复性好、准确度好,适用于同类生物样品中微量元素的测定,结果令人满意。     

火焰原子吸收法测定中药络石藤茎中六种金属元素的含量

目的：运用火焰原子吸收光谱法测定中药络石藤茎中的Fe、 Zn、 Mg、 Ca、 Cu、 Mn 6种金属元素的含量。方法用浓HNO3-HClO4消解样品,采用标准曲线法测定其6种金属元素含量。结果所测的样品中含有丰富的人体必需微量元素。回收率在99.56％～105.0％之间,样品相对偏差小于5％。结论该法简单、准确,结果令人满意。     

火焰原子吸收法测定中药艾草中四种金属元素的含量

目的运用火焰原子吸收光谱法测定中药艾草中的Fe、Zn、Mg、Ca 4种金属元素的含量。方法用浓HNO3-HClO4消解样品,采用标准曲线法测定其4种金属元素含量。结果所测的样品中含有丰富的人体必需微量元素,尤其是Ca含量极高。方法回收率在96.50%~103.80%之间,样品相对偏差小于5%。结论方法简单、准确,结果令人满意。     

火焰原子吸收法测定中草药海金沙茎中五种金属元素的含量

目的运用火焰原子吸收光谱法测定中草药海金沙茎中的Fe、zn、Mg、Ca、Cu5种微量元素的含量。方法用浓HNO3-HCIO4消解样品,采用标准曲线法测定其5种金属元素含量。结果所测的样品中含有丰富的人体必需微量元素。方法回收率在98.68％～104.4％之间,样品相对偏差小于5％。结论该法快速简便、重复性好、准确度好,适用于同类生物样品中微量元素的测定,结果令人满意。     

火焰原子吸收法测定中药草珊瑚叶中五种金属元素的含量

目的运用火焰原子吸收光谱法测定中药草珊瑚叶中的Fe、Zn、Mg、Ca、Cu 5种金属元素的含量。方法用浓HNO3-HCl O4消解样品,采用标准曲线法测定其5种金属元素含量。结果所测的样品中含有丰富的人体必需微量元素。方法回收率在99.35%-103.30%之间,样品相对偏差小于5%。结论该法简单、准确,结果令人满意。     

原子吸收光谱法测定新生儿脐血中微量金属元素

将样品用硝酸消解预处理后,用原子吸收光谱法测定新生儿脐血中微量金属元素Fe、Zn、Cu、Ca、Mg。对酸介质浓度、共存元素的干扰等进行了探讨,该方法的平均加标回收率为94．9％～101．3%。Fe、Zn、Cu、Ca、Mg测定结果的相对标准偏差分别为0．70％、4．70％、5．26%、3．54％、1.10%。     

微波消解和直接溶解进样法测定板蓝根颗粒剂中六种金属元素的比较研究

目的使用微波消解和热酸溶液直接溶解板蓝根颗粒,运用火焰原子吸收光谱法测定这两种溶液中Fe、Zn、Cu、Mg、Ca和Mn 6种金属元素的含量。方法分别采用浓HNO3湿法微波消解和直接溶解板蓝根颗粒样品,用原子吸收分光光度计测定上述样品中6种金属元素含量。结果所测定的板蓝根颗粒中含有丰富的金属元素,两种前处理方法测定的结果相差很小。采用此法回收率在92.0%~110.0%之间,样品相对偏差小于3%。结论板蓝根颗粒中金属元素可作为人体元素的重要补充。     

火焰原子吸收法测定木槿中微量元素的含量

目的运用火焰原子吸收光谱法对木槿中茎和叶的Fe、Zn、Mg、Ca、Cu 5种金属元素含量进行了测定。方法用浓V(HNO3)+V(HClO4)=4+1消解样品,采用标准曲线法测定。结果所测的样品中含有丰富的人体必需微量元素。回收率在95.10%～105.00%之间,RSD小于2%。结论该法简单、准确,结果令人满意。     

On-line microwave sample pretreatment for the determination of mercury in blood by flow injection cold vapor atomic absorption spectrometry

A method for on-line treatment of whole blood in a microwave oven and determination of mercury by flow injection cold vapor atomic absorption spectrometry was developed. After dilution of the whole blood and addition of oxidant, all further treatment and measurement were performed automatically, on-line. Recoveries of five mercury compounds were complete. Good agreement between measured and recommended values of mercury in whole blood reference materials was obtained. Measured mercury values also agreed with results from other accepted methods. Sample throughput was about 45 measurements/hr. Detection limit (3s) in diluted sample was 0.1 μg/l corresponding to 1μg/l Hg in whole blood. The RSD value at 0.5 μg/l Hg in the diluted sample was 6–7% (11 measurements and 0.5 ml sample volume). Mercury concentrations between 1 and 150 μg/l in whole blood can be measured using this method. For three replicate measurements, 0.5 ml of whole blood is required.     

Simultaneous microdetermination of sulfur and phosphorus in organic compounds

A simple method for the simultaneous determination of sulfur and phosphorus in 3–8 mg organic sample is presented. Following oxidative combustion by the oxygen flask method, sulfate is precipitated by addition of a known amount of Ba(II) and the excess of the latter is measured polarographically. After filtration, the quinoline phosphomolybdate method is used to precipitate phosphate; the unreacted Mo(VI) is determined polarographically. The mean relative error for 13 determinations was 2.99% for S and 4.07% for P; the mean relative standard deviation was 1.43 and 4.19%, respectively.     

氧亚甲基连接的聚氧乙烯电解质

<正> 聚氧乙烯(PEO)和锂盐混合后具有聚合物电解质(Polymer electrolyte)的离子导电性,可用于制作高能量密度薄膜固体电池。存在的问题是因聚氧乙烯导电发生在非晶区,而未经改性的聚氧乙烯在室温下结晶度X_c>70％,必须在熔化时才具有良     

Thermoelectric properties of Ru2Si2 prepared by spark plasma sintering method

Electrical conductivities, Seebeck coefficients and thermal diffusivities were measured for Ru₂Si₃ samples with different densities prepared by spark plasma sintering method and an Rh-doped sample prepared by the floating zone melting and spark plasma sintering methods. Electrical conductivities, Seebeck coefficients and thermal diffusivities increased with sample density for undoped Ru₂Si₃. The thermoelectrical figure of merit also increased with sample density. Electrical conductivity of the 4% Rh-doped sample was larger than that of our previous samples prepared by floating zone melting method. Values of Seebeck coefficients were similar for samples prepared by either method. This revised version was published online in August 2006 with corrections to the Cover Date.     

Automatic determination of insolubles in lubricating oils by flow injection analysis employing an LED-photometer detector

A flow injection system is presented for the determination of the insolubles content in used lubricating oil samples. The system is based on the injection of an aliquot of the sample in a stream of organic solvent where it is dispersed, and measurement of the scattered radiation (measured as apparent absorbance) in the visible range (λ = 640 nm). An LED-based photometer was used for this purpose. The whole system including sample injection and data acquisition was controlled by a personal computer. Calibration curves exhibited good linearity (h = 0.415 ± 0.016C + 0.00 ± 0.03, r² = 0.9995, confidence level of 95%) in the range up to 2.68% (insolubles in pentane). Detection and quantification limits were respectively 0.07% and 0.16% (w/w). The method was validated by analysis of 25 real samples by the proposed method and the FTIR method finding high correlation. Waste generation and reactive consumption is much less than in the official method (ASTM D-893). The proposed method employs 25 mL of kerosene per sample while the official method employs 200 mL of pentane.     

热分析-质谱联用中逸出气体的脉冲热分析定量方法

利用脉冲热分析技术(PulseTA)实现对热分析-质谱(TA-MS)联用系统中逸出气体质谱信号的定量,考察了多种实验参数如不同载气流速、温度以及分析样品量等因素对热分析-质谱联用系统中逸出气体质谱信号定量校正的影响.实验结果表明,利用PulseTA对TA-MS联用系统中逸出气体CO2定量结果与理论计算值的相对误差约2.85%.同时利用TG-DTG-MS联用技术对氮化铟(InN)粉体的热分解行为进行研究,在氩气气氛下InN粉体的热分解过程一步完成,InN粉体在550～750℃得到相应的正离子质谱峰:N2+(m/z=28),所释放的N非常接近InN中N的理论含量.利用PulseTA技术检测到InN粉体受热分解放出氮气质量的实验测量值与理论计算值的相对误差约为1.36%.     

Mercury speciation and total trace element determination of low-biomass biological samples

Current approaches to mercury speciation and total trace element analysis require separate extraction/digestions of the sample. Ecologically important aquatic organisms--notably primary consumers such as zooplankton, polychaetes and amphipods--usually yield very low biomass for analysis, even with significant compositing of multiple organisms. Individual organisms in the lower aquatic food chains (mussels, snails, oysters, silversides, killifish) can also have very low sample mass, and analysis of whole single organisms is important to metal uptake studies. A method for the determination of both methyl Hg and total heavy metal concentrations (Zn, As, Se, Cd, Hg, Pb) in a single, low-mass sample of aquatic organisms was developed. Samples (2 to 50 mg) were spiked with enriched with (201)MeHg and (199)Hg, then leached in 4 M HNO(3) at 55 degrees C for extraction of MeHg. After 16 h, an aliquot (0.05 mL) was removed to determine mercury species (methyl and inorganic Hg) by isotope dilution gas chromatography inductively coupled plasma mass spectrometry (ICP-MS). The leachate was then acidified to 9 M HNO(3) and digested in a microwave at 150 degrees C for 10 min, and total metal concentrations were determined by collision cell ICP-MS. The method was validated by analyzing five biological certified reference materials. Average percent recoveries for Zn, As, Se, Cd, MeHg, Hg(total) and Pb were 99.9%, 103.5%, 100.4%, 103.3%, 101%, 97.7%, and 97.1%, respectively. The correlation between the sum of MeHg and inorganic Hg from the speciation analysis and total Hg by conventional digestion of the sample was determined for a large sample set of aquatic invertebrates (n = 285). Excellent agreement between the two measured values was achieved. This method is advantageous in situations where sample size is limited, and where correlations between Hg species and other metals are required in the same sample. The method also provides further validation of speciation data, by corroborating the sum of the Hg species concentrations with the total Hg concentration.     

碱性溶液微波消解-氢化物发生-原子荧光光谱法测定土壤中锡

土壤样品先在烘箱内于(102±3)℃下干燥2h。称取此样品0.10g置于聚四氟乙烯(PTFE)消解罐中,加入500g·L^-1氢氧化钠溶液2mL,按程序升温模式在微波消解仪中进行消解。消解完成后,加二次去离子水将溶液稀释至25.0mL,样品溶液经载流(1mol·L^-1氢氧化钠溶液)通过三通阀进入仪器,并在线被5%(体积分数)硫酸溶液中和后与由蠕动泵传送的还原剂硼氢化钾反应生成氢化锡,传送进入原子化器迅速原子化,在高性能空心阴极灯的作用下产生荧光,由检测器检测其峰面积。测得锡的标准曲线的线性范围在100μg·L^-1以内。以3倍空白值求得的标准偏差计算其检出限(3s)为0.062μg·g^-1。用此方法测定了7个GBW标准物质,所得结果与认定值之间的相对误差为-1.61%~3.07%,测定值的相对标准偏差(n=7)为1.8%~3.2%。     

Standard signal extraction for analyzing target analytes in real samples with complex matrices

A second‐order method, standard signal extraction was proposed for quantitative analysis of target analytes in the samples with complex matrices by gas chromatography–mass spectrometry. In the method, standard addition was adopted. The data of the pure standard, sample, and spiked sample were used in the calculation. By performing principal component analysis on the data aligned with the measured signals of the sample and standard, the standardized signal that is orthogonal to the signals of interferences in the sample can be extracted. Then, the signal of spiked sample was projected to the standardized signal. The concentration ratio of the target analyte in the sample and spiked sample can be obtained. Finally, the concentration of the target analyte in the sample can be calculated with the added concentration in the spiked sample. Both simulated and experimental data were investigated with the proposed approach, compared with rank annihilation factor analysis. The recoveries of standard addition were found in a range of 99–105%, and the relative standard deviations obtained in three repeated measurements were less than 3%. Results show that the method can accurately estimate the quantitative information of analytes of interest in the presence of interferents and can be applied more widely compared with rank annihilation factor analysis. Copyright © 2015 John Wiley & Sons, Ltd.