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同位素稀释法定量分析中,当待测样品中某一目标同位素的丰度被示踪剂影响而不能保持天然丰度时,需要测量样品中各同位素的丰度比。在待测样品量或测量时间有限时,常规同位素稀释法的应用受到局限。为了降低样品消耗量、简化测量步骤、减小记忆效应影响、提高测量效率,本研究建立了一种可省略待测样品丰度比测量环节的快速同位素稀释定量方法。基于物质的量守恒原理,通过关联的运算,得到待测样品后,只需进行一次添加同位素稀释剂后混合样品的丰度比测量即可完成目标同位素的定量分析。以天然丰度Xe标准气体作为模拟样品,6次测量值与标称值的相对偏差均小于1%,相对标准偏差(RSD)为0.4%,与使用常规同位素稀释法得到的测量结果完全相符。此外,以128Xe作为示踪同位素,得到的示踪同位素扩散曲线符合气体在封闭空间的扩散规律。本方法适用于有3种或更多稳定同位素的元素,既保证了测量结果的准确性,又可缩短分析时间,减少样品消耗量。 相似文献
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基于三氧化钼易升华的特性,建立了一种纯化浓缩钼同位素试剂的新方法.采用天然丰度掺杂样品Synthetic-Mo对纯化过程中的氧化时间、样品加入量及真空蒸发温度等条件进行了优化.用高分辨等离子体质谱分析了样品中杂质的含量,计算得到纯化后95Mo和98Mo浓缩同位素试剂的纯度分别为99.992%和99.990%.通过多接收器等离子体质谱测定纯化前后样品中钼同位素的组成,δX/95Mo(X=92,94,96,97,98,100)值均在仪器测量精度(0.3‰)范围之内,未观察到明显的质量分馏现象.该方法能够满足校正质谱法对浓缩同位素试剂的要求,对建立高准确度的钼同位素丰度比测量方法具有重要意义. 相似文献
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碰撞池-多接收电感耦合等离子体质谱测定硒同位素的质量偏移效应 总被引:1,自引:0,他引:1
通过改变雾化气流量、RF射频发生器功率、矩管位置和碰撞气流量等仪器参数,研究了碰撞池-多接收电感耦合等离子体质谱(Collision Cell-MC-ICP-MS)中的质量偏移效应。实验结果表明,雾化气流量、RF发生器功率和矩管位置等是质量偏移效应的主要来源,而碰撞气流量的影响很小。在此基础上,建立了MC-ICP-MS分析硒同位素丰度的最优化测量条件,同位素比R82/76的测量精度达到0.0043%。采用化学计量方法配制了两个系列硒同位素丰度校正样品,通过不同的同位素丰度比的质量偏移校正因子β和与其对应的同位素对的质量平均值成线性的关系,分析了样品GBW(E)080215和SRM3149中硒的同位素丰度组成。与样品SRM3149中82Se/76Se的比值相比,样品GBW(E)080215中的硒同位素分馏系数δ82/76为-4.78‰。 相似文献
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通过优化和组合不同脱铝补硅方法,依次经氟硅酸铵处理、600oC水热处理、硅溶胶+草酸处理和800oC水热处理过程,成功实现了200nm超细NaY分子筛的深度脱铝,最终产品骨架硅铝比高达27.3,比表面积为581.9m2/g,分子筛结晶度保持在65%以上.结果表明,对于超细NaY分子筛脱铝,第一步采用氟硅酸铵进行部分缺陷修补尤为重要.根据分子筛晶粒尺寸不同,需严格控制氟硅酸铵用量和处理次数.当晶粒为200nm时,氟硅酸铵与分子筛骨架铝的摩尔比为0.16,处理一次较为适宜.在连续脱铝过程中及时补修脱铝产生的缺陷是保障超细NaY分子筛成功脱铝的关键,而采用氟硅酸铵、硅溶胶、800oC高温水热处理,可有效实施这种骨架修正作用. 相似文献
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Patrick J. A. Hill Neil R. Banerjee Arshad Ali Iffat Jabeen Gordon R. Osinski Fred J. Longstaffe 《Journal of mass spectrometry : JMS》2019,54(8):667-675
We present a procedure for the determination of the isotopic ratios of silicon and oxygen from the same aliquot of anhydrous silicate material. The sample is placed in a bromine pentafluoride atmosphere as it is heated with a CO2 laser system releasing silicon tetrafluoride and oxygen gasses. The oxygen gas is then purified to remove other reaction by‐products through several liquid nitrogen traps before being captured onto a molecular sieve and transferred to an isotope ratio mass spectrometer. The silicon tetrafluoride gas is then purified using a supplementary line by repeatedly freezing to ?196°C with liquid nitrogen and then thawing with an ethanol slurry at ?110°C through a series of metal and Pyrex traps. The purified gas is then condensed into a Pyrex sample tube before it is transferred to an isotope ratio mass spectrometer for silicon isotope ratio measurements. This system has silicon yields of greater than 90% for pure quartz, olivine, and garnet standards and has a reproducibility of ±0.1‰ (2σ) for pure quartz for both oxygen and silicon isotope measurements. Meteoritic samples were also successfully analyzed to demonstrate this system's ability to measure the isotopic ratio composition of bulk powders with precision. This unique technique allows for the fluorination of planetary material without the need for wet chemistry. Though designed to analyze small aliquots of meteoritic material (1.5 to 3 mg), this approach can also be used to investigate refractory terrestrial samples where traditional fluorination is not suitable. 相似文献
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采用浊度法和静态抑垢法,研究了抑制剂2-膦酸基-1,2,4-三羧酸丁烷(PBTCA)与水解聚马来酸酐(HPMA)对氟硅酸钠(钾)结晶的影响。 运用经典结晶成核理论解释了抑制机理,利用扫描电子显微镜和X射线衍射技术表征了氟硅酸钠(钾)的晶体形貌和晶型。 结果表明,PBTCA与HPMA通过提高氟硅酸钠(钾)结晶时的表面自由能而抑制氟硅酸钠(钾)的析出。 PBTCA与HPMA之间存在明显的协同作用,PBTCA与HPMA共同作用使Na2SiF6的结晶表面自由能从108 mJ/m2升高至126 mJ/m2,溶液中Na+的阻垢率从6.2%上升至70.3%;使K2SiF6的结晶表面自由能从199 mJ/m2升高至230 mJ/m2,溶液中K+的阻垢率从10.2%升高至45.3%。 PBTCA与HPMA的加入使氟硅酸钠(钾)的粒径变小,颗粒分散;空白溶液中晶体主要为NaKSiF6,PBTCA与HPMA混合体系中结晶产物主要为Na2SiF6和K2SiF6。 相似文献
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Masahisa Kakiuchi 《Journal of solution chemistry》1994,23(10):1073-1087
The D/H ratios of hydrogen gas in equilibrium with aqueous sodium chloride solutions of 2, 4 and 6 molalities were determined within the range 10 to 95°C, using a hydrophobic platinum catalyst. With each of the different sodium chloride concentrations, the hydrogen isotope effect between the solution and pure water changes linearly with the square of the reciprocal temperature. On the basis of the results for hydrogen isotope fractionation observed in this study, and those of hydrogen isotope fractionation between pure water and vapor, it is concluded that the structure of the aqueous sodium chloride solution does not change significantly with temperature. The hydrogen isotope effect is evidently different from the results of vapor pressure isotope effects (VPIE) on sodium chloride solutions measured on separated isotopes. The difference between the present work and the VPIE studies is probably due to a non-ideal behavior in a mixture of isotopic water molecules and/or to a H2O-D2O disproportionation reaction in sodium chloride solutions. The distinction between the latter two mechanisms can not be differentiated at present. 相似文献
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Tyler M. Wilson Brett J. Murphy Adrian Abad Chris Packer Ariel Poulson Richard E. Carlson 《Molecules (Basel, Switzerland)》2022,27(9)
Ocimum campechianum Mill. (Peruvian basil) is an essential oil-bearing plant of the Lamiaceae family. Volatile oil produced through steam distillation of Peruvian basil was examined to establish the aromatic and stable isotope profiles of samples (n = 9) from three different cultivated plots in Peru. The resulting essential oils were analyzed by GC/FID, GC/MS, and GC/IRMS. In accordance with findings from other researchers, multiple chemotypes, defined by the most abundant aromatic compounds, exist within these populations. Overall, 55% of samples are the eugenol chemotype (values ranging 15.4–30.2%), 33% are the methyl eugenol chemotype (values ranging 68.1–68.7%), and a single sample is a mixture of both chemotypes, containing high levels of both eugenol (38.1%) and methyl eugenol (8.6%). Stable isotope ratios, δ2H and δ13C, performed on prominent compounds provide supporting data for distinguishing chemotypes. Complete aromatic profiles, stable isotope ratios, and essential oil yield are established for each sample. This study confirms the existence of multiple chemotypes and, for the first time, to the author’s best knowledge, establishes stable isotope ratios for O. campechianum essential oil, which proves a useful tool in further investigating plant metabolism and determining essential oil authenticity. 相似文献
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Davydova E. I. Virovets A. V. Peresypkina E. V. Timoshkin A. Yu. 《Russian Journal of General Chemistry》2021,91(10):1964-1968
Russian Journal of General Chemistry - The crystal structure of the silicon tetrafluoride molecular complex with 4-phenylpyridine SiF4·2ppy has been determined by X-ray diffraction analysis.... 相似文献
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提出了一种(NH4)2SiF6处理提高SBA-15介孔材料水热稳定性的改良方法.采用SBA-15介孔材料中预引入Al3+离子,再进行1%SiO2计量的(NH4)2SiF6处理,最后用强酸洗脱预引入的Al3+.结果显示,由此处理的SBA-15材料,其水热稳定性明显优于相同条件下未预引入Al3+时(NH4)2SiF6处理的样品.两者在800°C、100%水蒸气处理12 h后,虽然均能很好保持其介观有序度、形貌及六方孔道结构,但前者的比表面积可高达271 m2/g,而后者仅为224 m2/g.表明Al3+离子介入能大幅度提升(NH4)2SiF6处理对SBA-15介孔材料的稳定化作用.这主要得益于预引入的骨架Al3+在保障(NH4)2SiF6处理修复SBA-15材料表面缺陷和进行表面疏水化、提升其水热稳定性的同时,能减缓(NH4)2SiF6释放的多余F-离子对SBA-15材料骨架的刻蚀破坏作用. Al3+离子介入的这种提升作用与其引入方式和SBA-15材料所经受的温度密切相关. 相似文献
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Annemie Adriaens Luc Van't dack Freddy Adams Renaat Gijbels 《Mikrochimica acta》1995,120(1-4):139-147
Secondary ion mass spectrometry has been used to measure the silicon isotope ratio as a function of depth in feldspars after their interaction with dilute acid solutions. The reaction of feldspars with aqueous solutions implies the formation of relatively thick K, Na and Al depleted surface layers, especially when the dissolution experiments are conducted in the presence of silica powder. The latter is used to lower the silicon concentration gradient at the solid-solution interface. This generates an uncertainty in the interpretation of the results: the depleted surface layer may have been formed by leaching of the above-mentioned elements from the solid, or by precipitation of silica from the solution. Measurements using isotopically enriched silica powder (30SiO2) were therefore performed in the hope that they would solve the uncertainty. The measured silicon isotope ratio at the surface of the mineral appears to be different from its normal terrestrial value and from the enriched powder value, having a value somewhere in between which decreases towards its normal value as a function of depth. In addition the silicon isotope ratio of the solution, which was measured using thermal ionization mass spectrometry, shows an altered value compared with the enriched silica powder. The results of both analyses therefore indicate an exchange in silicon between solid and solution and suggest the combination of two or more mechanisms during dissolution. 相似文献