电感耦合等离子体原子发射光谱法测定硅锰合金中磷

建立了电感耦合等离子体-原子发射光谱法(ICP-AES)测定硅锰合金中磷的方法.进行了样品分解试验,并考察了基体、共存元素对磷测定的影响,选择P214.914 nm为分析谱线.方法的检出限为0.003％,R2=0.9998,RSD小于2％,回收率为96.9％％～101.6％％.方法用于国际能力验证样品分析,结果满意,与...     

电感耦合等离子体原子发射光谱（ICP-AES）法测定铁矿石中磷

采用盐酸-硝酸-高氯酸-氢氟酸前处理样品,电感耦合等离子体原子发射光谱法测定铁矿石中的磷。对磷元素的分析谱线、样品称样量等工作条件进行了优化,解决了非金属元素磷的分析谱线难选择、样品称样量影响测定准确度的技术难点;采用内标法,降低了样品基体效应及仪器波动产生的影响,提高了分析结果的精密度和准确度。利用所建立的方法快速分析了铁矿石中磷的含量,方法检出限为0.0036 mg/L,测定范围为0.012%~2%,测定结果与标准值和化学法测定结果相符,相对标准偏差(RSD,n=9)小于2%。拟定的方法和分光光度法进行比对实验,技术优势明显。     

电感耦合等离子体原子发射光谱(ICP-AES)法测定铁矿石中磷

采用盐酸-硝酸-高氯酸-氢氟酸前处理样品,电感耦合等离子体原子发射光谱法测定铁矿石中的磷。对磷元素的分析谱线、样品称样量等工作条件进行了优化,解决了非金属元素磷的分析谱线难选择、样品称样量影响测定准确度的技术难点;采用内标法,降低了样品基体效应及仪器波动产生的影响,提高了分析结果的精密度和准确度。利用所建立的方法快速分析了铁矿石中磷的含量,方法检出限为0.003 6mg/L,测定范围为0.012%～2%,测定结果与标准值和化学法测定结果相符,相对标准偏差(RSD,n=9)小于2%。拟定的方法和分光光度法进行比对实验,技术优势明显。     

电感耦合等离子体原子发射光谱法测定铝锰铁中硅和磷

采用电感耦合等离子体原子发射光谱法测定铝锰铁中硅、磷的含量。选择178.242nm和251.611nm作为磷、硅的分析谱线,可消除谱线的重叠干扰。使用与分析样品基体相接近的标准样品和相同的测定条件,可克服物理干扰,并比较了酸、碱熔样方式对待测元素的影响。本法已应用于铝锰铁样品中硅、磷的测定,对照试验测定结果的相对标准偏差(n=6)不大于7.0%。     

电感耦合等离子体发射光谱法测定植物油中的磷

用电感耦合等离子体发射光谱法(ICP-AES)测定了植物油中的磷.采用多谱线拟合技术(MSF)校正了铜对P213.617 nm和P214.914 nm光谱干扰.比较了活性炭炭化灰化法和微波消解法两种样品前处理方法对分析结果的影响.结果表明这两种前处理方法所得结果都能与国标磷钼蓝分光光度法的分析结果吻合,其中活性炭炭化灰化法的方法检出限(0.053 mg/kg)较微波消解法的方法检出限(0.42 mg/kg)更低,所以对低含量的磷的检测结果其相对误差及精密度更好.该法应用于植物油中磷的测定.     

王水溶解-电感耦合等离子体发射光谱法测定铁矿石中的微量磷

样品经王水分解后,在电感耦合等离子体发射光谱仪上测定了样品溶液中磷的含量。通过实验确定了基体元素的干扰、酸度、样品提升量、雾化气流速、功率、观测高度、分析谱线等分析条件。通过铁的干扰实验结果表明,样品中的基体元素铁不影响磷含量的测定。在用Ｐ178.222 nm分析线测定时,方法的检出限为P 0.0006％（相对于0.1ｇ样品,定容至100 mL）,相对标准偏差在3.14%～6.04％（ｎ＝11）,样品加标回收率在92%～110%。方法测定样品中磷含量的结果同光度法测定结果对比数据相符。     

电感耦合等离子体发射光谱法测定钢铁中的磷

探讨电感耦合等离子体发射光谱法测定钢铁中磷的方法。试验确定了微波消解器处理样品的条件、仪器最佳工作参数,研究了共存元素谱线的干扰情况。该法能够准确、快速地测定钢铁样品中0.010％～0.20％范围内的磷,测定结果的相对标准偏差RSD<5％,回收率为98％～104％。     

高分辨连续光源原子吸收光谱法对土壤中磷的测定

磷元素在适宜的空气-乙炔火焰中可形成PO双原子分子,PO分子的部分吸收谱线具有原子谱线的轮廓和强度.该文主要研究了利用连续光源原子吸收光谱法,在空气-乙炔火焰条件下测定PO分子的吸光度值,从而测定土壤样品中的磷元素.实验研究了测定过程中可能存在的光谱干扰和化学干扰、乙炔/空气流速比、燃烧器高度对PO双原子分子吸光度的影响,以及不同消解方式对测定结果的影响.在优化的实验条件下,PO 246.40 nm的检出限为20 mg/L.通过对土壤标准物质中磷元素含量的测定比对证明,连续光源原子吸收光谱法是一种测定土壤中磷元素含量的简单、快速的方法.     

电感耦合等离子体光谱法测定镍基高温合金中的硅、锰、磷

建立了电感耦合等离子体光谱测定镍基高温合金中硅、锰、磷元素的方法,优化了试样前处理方法,对前处理所用酸的酸度进行不同比例试验,确定了仪器测量条件及分析谱线.在一定浓度范围内,各元素的浓度与谱线强度呈线性关系,相关系数大于0.9999.加标回收率为93.3%～106.7%,测定结果的相对标准偏差小于3.0%(n=10)....     

Microwave Digestion-ICP- OES Determination of Common or Micro Impurities in Titanium Slag

钛渣样品采取高压密闭微波加热方式以HF、HNO3进行消解,采用电感耦合等离子体原子发射光谱法(ICP- OES)直接同时测定常量、微量杂质铁、铅、砷、铬、铜、磷、锰、钒、镁、钙.考察了消解条件、基体钛以及共存元素之间的干扰影响、等离子体参数等测定条件,通过优选元素分析谱线、以及采用基体匹配与同步背景校正相结合的方式消除光谱干扰和基体效应.测定50、60、70、80、90等不同品位钛渣中杂质元素的结果表明:方法检测范围涵盖了0.005％～10.0％的钙、镁、铁,以及0.005％ ～2.0％的铅、砷、铬、铜、磷、锰、钒,校准曲线相关系数大于0.9992;背景等效浓度0.002％ ～0.0015％,检测限0.0009～0.0038％;含量不小于1.0％的RSD低于0.677％,在0.010％～0.10％含量范围内RSD低于3.85％;回收率为90.0％～108.0％.以本法对70、80、90 3个高钛渣标准样品的定值分析结果与传统化学方法对照一致.     

有机金配合物催化羰化胺制甲酰胺

Au(PPh3)2Cl,[Au(PPh3)]2S等有机金配合物催化羰化脂肪族二胺制相应二酰胺显示出非常好的活性,与同一类的有机钯催化剂相比,具有更好的催化转化能力和选择性。实验结果还表明适量分子氧的引入对反应有明显的促进作用。     

Structure of amorphous poly-(ethylmethacrylate): a wide-angle x-ray scattering study

The local, temperature dependent structure of poly-(ethylmethacrylate) was studied with wide-angle x-ray scattering. The results were set into context to recent wide-angle neutron scattering results as well as to the results from a multitude of studies of the dynamics of this polymer. The temperature dependence of the wide angle x-ray results point to the development of local order which is backed by the neutron scattering results and which is connected to characteristic temperatures of the relaxation dynamic T(g) and T(c). The poly-(ethylmethacrylate) was studied in its predominantly syndiotactic as well as predominantly isotactic state displaying vastly different local structures as manifested in the x-ray results.     

Synthesis of mesoporous nano-TiO<Subscript>2</Subscript> doped with Sn by auto-assembly method and photo-catalytic property

Frank and Bard firstly reported that suspending TiO2 powder could photo-catalyze the solution con-taining CN?. Research on photo-degradation of delete-rious pollutants with nano-semiconductor material has become one of the most popular topics. Owing to it…     

铅离子印迹固相萃取原子吸收光谱分析

以Pb2+为模板,丙烯酸为功能单体,乙二醇二甲基丙烯酸酯为交联剂,采用本体聚合技术,制备了对Pb2+具有特异性识别作用的离子印迹材料。通过红外光谱,吸附容量,干扰实验等讨论了该离子印迹材料的相关性质。结果表明,该离子印迹材料对Pb2+的结合能力明显强于非印迹材料,能够很好的排除其他金属离子的干扰。通过制备该离子印迹材料,能够富集水体中的痕量铅,结合原子吸收光谱法对其进行定量分析,为测定复杂环境样品中痕量铅离子提供一个高选择性,高预富集效率的固相萃取材料和分析方法。     

Cure Kinetics of DGEBA with Hyperbranched Poly （3-hydroxyphenyl） Phosphate as Curing Agent Studied by Non-isothermal DSC

IntroductionEpoxy resins are widely used in the fields of coa-tings,adhesives,insulating materials,etc..Diglycidylether of bisphenol A(DGEBA)is the most importantepoxy resin in industry because of its fluidity,physicaland mechanical properties after cure,…     

Vibrational relaxation in hydrogen bonded systems: II. Experimental results

Experimental results are presented, supporting the theory presented earlier. These results, obtained by studying the shape of the as. OCO stretching band of acetate ions in CH₃OH and deuterated analogs, show vibrational relaxation by near-resonant vibrational energy transfer to the solvent. The essential role of the H-bond in this process, as derived theoretically, is borne out by the results.     

离子色谱法测定酸雨中的阳离子

用离子色谱法测定酸雨中的Na^ 、NH4^ 、K^ 、Mg^2 、Ca^2 等阳离子，并同时用原子吸收分光光度法进行了对比实验。结果表明，利用离子色谱法测定阳离子，方法简便、快捷，能一次同时测定多种离子，测定结果和原子吸收法相符。     

Metal hydroxides as catalysts for the Baeyer-Villiger oxidation of cyclohexanone with hydrogen peroxide

This paper reports the results obtained in the Baeyer-Villiger oxidation of cyclohexanone with a hydrogen peroxide/benzonitrile mixture as oxidant in the presence of synthetic metal hydroxides or their calcined products as catalysts. The metal hydroxides were obtained by coprecipitation. The best ε-caprolactone conversion results were provided by magnesium hydroxide.     

基于氦离子化气相色谱法测定微量氧、氮的影响因素

探讨氦离子化气相色谱法测定样品中微量氧、氮含量的影响因素。采用控制变量法,对色谱柱温度、进样流量、进样管道环境及极化电压等因素对微量氧、氮测定结果的影响进行讨论和分析。结果表明,当色谱柱温度为25~45℃时,色谱柱对氧、氮吸附量最小;当进样流量不小于70 mL/min时,微量氧、氮测定结果受外界干扰最小;当极化电压为80~160 V时,氧、氮具有最佳的响应值;初次测定样品中微量氧、氮含量时,需使进样管道表面吸附的氧、氮处于饱和状态,以便获得理想的测定结果。讨论的结果可为氦离子化气相色谱法测定相关样品中微量氧、氮含量时提供技术参考。     

Isopiestic Determination of Water Activity on the System LiNO<Subscript>3</Subscript>+KNO<Subscript>3</Subscript>+H<Subscript>2</Subscript>O at 273.1 and 298.1 K

Water activities in the ternary LiNO₃+KNO₃+H₂O system and its sub-binary systems have been measured by the isopiestic method at 273.1 and 298.1 K. The measured results were treated by a Pitzer-Simonson-Clegg thermodynamic model, from which the predicted solubility isotherms were compared with the experimental results. Based on this comparison, the reliability of the measured results was discussed. The measured results help in predicting the phase diagram of the ternary system, as well as other multi-component systems based on the ternary system.