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A novel method for extracting potassium (K) from K-poor and sodium-rich samples for high-precision stable K isotope analysis 从贫钾和富钠样品中提取钾(K)用于高精度稳定钾同位素分析的新方法
IF 3.4 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-07-15 DOI: 10.1039/d4ja00168k
Xin-Yuan Zheng
Reconstruction of stable potassium isotope composition (41K/39K) in ancient seawater has significant implications for our understanding of the fundamental controls on the long-term stability of Earth’s climate and ocean chemistry, but the relevant research is hampered by scarce preservation of seawater K in geological records. Marine halite (NaCl) samples are potentially valuable archives of seawater K isotope signatures because they often contain abundant fluid inclusions directly sourced from evaporated ancient seawater. However, the extremely high Na matrix relative to low K concentrations in halite presents a formidable challenge for K isotope analysis. This study reports a novel and efficient K extraction method that can separate K from a high Na matrix by precipitating K as a sparsely soluble salt using sodium tetraphenylborate (TPB). Development of this method was based on an in-depth understanding of the TPB precipitation reaction and solubility equilibrium of relevant TPB salts. Key parameters, including reaction time, precipitate recovery and rinse, and further K purification for isotope analysis, have been optimized through extensive laboratory experiments. It is demonstrated that this new method can extract small quantities of K down to 20 μg from a large quantity of NaCl matrix up to 1 gram. In addition, preliminary results show that this new extraction method can be also applied to prepare carbonate samples, which represent another important type of samples pertinent to K isotope research but notoriously difficult to analyze due to their low K concentrations and high Ca matrices. For the first time, this study demonstrates the utility of TPB chemistry in preparing challenging K-poor, matrix-rich samples for high-precision stable K isotope analysis.
重建古海水中稳定的钾同位素组成(41K/39K)对我们了解地球气候和海洋化学长期稳定性的基本控制具有重要意义,但由于地质记录中保存的海水钾元素很少,相关研究受到了阻碍。海洋海绿石(NaCl)样本可能是海水 K 同位素特征的宝贵档案,因为它们通常含有大量直接来自蒸发的古海水的流体包裹体。然而,相对于低 K 浓度而言,海泡石中的 Na 基质含量极高,这给 K 同位素分析带来了巨大挑战。本研究报告了一种新颖高效的钾萃取方法,该方法通过使用四苯基硼酸钠(TPB)将钾沉淀为稀溶盐,从而将钾从高Na基质中分离出来。该方法的开发基于对 TPB 沉淀反应和相关 TPB 盐类溶解平衡的深入理解。通过大量的实验室实验,对包括反应时间、沉淀回收和冲洗以及用于同位素分析的进一步 K 纯化在内的关键参数进行了优化。实验结果表明,这种新方法可以从多达 1 克的大量氯化钠基质中提取低至 20 微克的少量钾。此外,初步结果表明,这种新的萃取方法还可用于制备碳酸盐样品。碳酸盐样品是与钾同位素研究相关的另一种重要样品类型,但由于其钾浓度低、钙基质含量高而难以分析。这项研究首次证明了 TPB 化学在制备具有挑战性的贫钾、富含基质的样品以进行高精度稳定钾同位素分析方面的实用性。
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引用次数: 0
Cadmium isotopes analysis of environmental samples with high organic matter by dry ashing method under wet plasma conditions 在湿等离子体条件下采用干灰化法对有机物含量高的环境样品进行镉同位素分析
IF 3.4 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-07-14 DOI: 10.1039/d4ja00083h
Xian Wu, Zeyu Wang, Guangyi Sun, Yu Lin, Xuewu Fu, Yang Tang, Xinbin Feng
Isotope data of key pollutants are needed for source apportionment analysis in natural ecosystems. Isotope data for cadmium (Cd), a rare and dispersed but toxic element, are very limited mainly due to its low contents in the natural environment. In this study, for samples with low Cd content but high organic matter content, a dry ashing pre-treatment method was proposed to effectively enrich Cd to meet the requirements of its isotope analysis (Cd content > 20 ng). This method was applied to soils, sediments, biological tissues, and coal, with a maximum digestion weight of 1.67 g or more. With the assistance of quartz microfiber filter membranes during dry ashing, good Cd recovery (91.6–108.0%) and significant removal of organic matter were achieved. Mass bias was corrected by combining the silver external standard (Ag-doping) method with the sample-standard-bracketing (SSB) method, and Cd isotope measurements were performed under wet plasma conditions (with an accuracy of 0.060‰). Cd isotopic compositions obtained by the dry ashing method were compared with those obtained by the high-pressure bomb digestion method, and the differences ranged from −0.056 to 0.076‰, indicating that the dry ashing with wrapped membranes method did not cause any fractionation of Cd during the sample pre-treatment process. Meanwhile, the tolerance of tin (Sn) and zinc (Zn) elements provided a significant advantage under wet plasma conditions over dry plasma conditions without reducing the tolerance of molybdenum (Mo) and zirconium (Zr). The method developed in this study should enhance the application of Cd isotopes in investigating Cd cycling in primary ecosystems and organisms.
自然生态系统中的污染源分配分析需要主要污染物的同位素数据。镉(Cd)是一种稀有、分散但有毒的元素,其同位素数据非常有限,这主要是由于镉在自然环境中的含量较低。本研究针对镉含量低但有机质含量高的样本,提出了一种干灰化预处理方法,以有效富集镉,满足其同位素分析的要求(镉含量为 20 毫微克)。该方法适用于最大消化重量为 1.67 克或以上的土壤、沉积物、生物组织和煤炭。在干灰化过程中,在石英微纤维滤膜的辅助下,实现了良好的镉回收率(91.6-108.0%)和有机物的显著去除。质量偏差通过银外标法(Ag-doping)和样品-标准-配准法(SSB)进行校正,镉同位素测量在湿等离子条件下进行(精度为 0.060‰)。将干灰化法得到的镉同位素组成与高压炸弹消解法得到的镉同位素组成进行比较,两者的差异在-0.056 至 0.076‰之间,表明包裹膜干灰化法在样品预处理过程中没有引起镉的分馏。同时,在湿等离子体条件下,锡(Sn)和锌(Zn)元素的耐受性比干等离子体条件下有明显优势,而钼(Mo)和锆(Zr)的耐受性并没有降低。本研究中开发的方法可提高镉同位素在研究原生生态系统和生物体内镉循环中的应用。
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引用次数: 0
Outstanding Reviewers for Journal of Analytical Atomic Spectrometry in 2023 分析原子光谱学报》2023 年杰出审稿人
IF 3.4 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-07-12 DOI: 10.1039/d4ja90033b
We would like to take this opportunity to thank all of Journal of Analytical Atomic Spectrometryreviewers for helping to preserve quality and integrity in the chemical science literature. We would also like to highlight our Outstanding Reviewers for Journal of Analytical Atomic Spectrometry in 2023.
我们想借此机会感谢《分析原子光谱学报》的所有审稿人,感谢他们帮助维护化学科学文献的质量和完整性。此外,我们还要特别介绍《分析原子光谱学报》2023 年的杰出审稿人。
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引用次数: 0
Label free, machine learning informed plasma-based elemental biomarkers of Alzheimer's disease 无标签、基于机器学习的阿尔茨海默病血浆元素生物标志物
IF 3.4 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-07-12 DOI: 10.1039/d4ja00090k
Ali Safi, Noureddine Melikechi, Kemal Efe Eseller, Richard M. Gaschnig, Weiming Xia
Using inductively coupled plasma mass spectrometry (ICP-MS), we have measured the elemental concentrations of Na, Fe, Cu, P, Mg, Zn, K in plasma samples of 25 Alzheimer's disease (AD) patients and 34 healthy individuals. Given the multidimensional nature of the ICP-MS data, we used support vector machines and logistic regression to illustrate the elemental distribution of each donor and seek key features that may differentiate plasma samples of AD patients from those of healthy individuals. We found that ratios of the elemental concentrations of Na over K, Fe over Na, and P over Zn yield specificity, sensitivity, and accuracy of 79%, 84% and 81% respectively. This information was then used to seek from the mass spectrometric data a differentiation of the plasma samples from AD and healthy donors. Plotted as a function of the Na/K, Fe/Na, and P/Zn, the ICP-MS data reveals a linear delineation between the two groups of samples yielding to the correct classification 21 of 25 AD and 28 of 34 HC plasma samples. These findings highlight the importance of elemental ratios present in plasma and suggest that the ratios of the elemental concentrations of blood metals may be considered as biomarkers that can distinguish plasma samples of AD patients from healthy subjects.
我们使用电感耦合等离子体质谱法(ICP-MS)测量了 25 名阿尔茨海默病(AD)患者和 34 名健康人血浆样本中的钠、铁、铜、磷、镁、锌、钾元素浓度。鉴于 ICP-MS 数据的多维性,我们使用支持向量机和逻辑回归来说明每个供体的元素分布情况,并寻找可能区分 AD 患者和健康人血浆样本的关键特征。我们发现,Na 相对于 K、Fe 相对于 Na 和 P 相对于 Zn 的元素浓度比值的特异性、灵敏度和准确度分别为 79%、84% 和 81%。然后,我们利用这些信息从质谱数据中寻求区分注意力缺失症和健康捐献者血浆样本的方法。通过绘制 Na/K、Fe/Na 和 P/Zn 的函数图,ICP-MS 数据揭示了两组样本之间的线性界限,在 25 个 AD 和 34 个 HC 血浆样本中,分别有 21 个和 28 个样本被正确分类。这些发现凸显了血浆中元素比率的重要性,并表明血液中金属元素浓度的比率可被视为生物标志物,可将注意力缺失症患者的血浆样本与健康人的血浆样本区分开来。
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引用次数: 0
A potential natural chalcopyrite reference material for in situ copper, iron, and sulfur isotope measurements 用于原位测量铜、铁和硫同位素的潜在天然黄铜矿参考材料
IF 3.4 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-07-12 DOI: 10.1039/d4ja00147h
Lie-Wen Xie, Hong-Rui Fan, Hui-Min Yu, Chao Huang, Lei Xu, Yue-Heng Yang, Shi-Tou Wu, Hao Wang
Chalcopyrite has been extensively utilized for tracing geological processes through its Cu, Fe and S isotopic compositions. However, the matrix-matched reference materials for micro-analysis are lacking. This study focused on assessing the feasibility of a natural chalcopyrite specimen (IGGCcp-1) as a matrix-matched reference material for in situ micro-analysis of Cu, Fe, and S isotopes. Electron probe microanalysis validated the uniform distribution of major elements within chalcopyrite grains, with no evidence of growth zoning. Random spot isotopic measurements using LA-MC-ICP-MS demonstrated remarkable consistency in δ65Cu, δ56Fe and δ34S. These results indicated that the IGGCcp-1 specimen exhibited its suitability as a reference material. Using SN-MC-ICP-MS technique, the δ65Cu value was accurately determined to be 0.43 ± 0.05 ‰ (2S, N = 30). Furthermore, the δ56FeIRMM-014 and δ57FeIRMM-014 values were recorded as -0.24 ± 0.04 ‰ (2S, N = 18) and -0.36 ± 0.09 ‰ (2S, N = 18), respectively. Additionally, the δ34SVCDT measurement, performed with EA-IRMS, yield a value of -0.28 ± 0.60 ‰ (2S, N = 10). These precisely measured isotope ratios established the recommended reference values for the IGGCcp-1 sample in future applications of Cu, Fe, and S isotope micro-analysis.
黄铜矿的铜、铁和硫同位素组成被广泛用于追踪地质过程。然而,用于显微分析的基质匹配参考材料却十分缺乏。本研究的重点是评估将天然黄铜矿标本(IGGCcp-1)作为基质匹配参考材料进行铜、铁和硒同位素原位显微分析的可行性。电子探针显微分析验证了黄铜矿晶粒内主要元素的均匀分布,没有生长分带的迹象。使用 LA-MC-ICP-MS 进行的随机点同位素测量表明,δ65Cu、δ56Fe 和 δ34S 具有显著的一致性。这些结果表明,IGGCcp-1 试样适合作为参考材料。利用 SN-MC-ICP-MS 技术,δ65Cu 值被准确测定为 0.43 ± 0.05 ‰(2S,N = 30)。此外,δ56FeIRMM-014 和 δ57FeIRMM-014 值分别为 -0.24 ± 0.04 ‰(2S,N = 18)和 -0.36 ± 0.09 ‰(2S,N = 18)。此外,使用 EA-IRMS 进行的 δ34SVCDT 测量得出的值为 -0.28 ± 0.60 ‰(2S,N = 10)。这些精确测量的同位素比值为 IGGCcp-1 样品在未来铜、铁和 S 同位素微分析应用中确立了推荐参考值。
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引用次数: 0
Ultra-sensitive determination of mercury in flue gas by atmospheric pressure glow discharge atomic emission spectrometry coupled with gold amalgam enrichment 利用常压辉光放电原子发射光谱法和金汞合金富集法超灵敏测定烟气中的汞含量
IF 3.4 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-07-10 DOI: 10.1039/d4ja00165f
Meng Gao, Rong Rong, Zhaoqing Cai, Zheng Wang
In this work, a highly sensitive procedure for the determination of mercury in flue gas was developed, based on direct-current atmospheric pressure glow discharge in hydrogen and helium (H2-He) atomic emission spectroscopy (APGD-AES) coupled with gold amalgam enrichment (GA). Calibration mercury vapor generated by the cold vapor generation (CVG) system was sent to GA system for enrichment. Subsequently, mercury was thermally resolved and transmitted to APGD for excitation, at the same time the signal at 253.6 nm was recorded by a micro-spectrometer. The parameters of GA and APGD systems were optimized, including the type and flow rate of carrier gas, discharge current and discharge gap. Under the optimum operating conditions, when the sampling volume of flue gas was 10 L the detection limit (DL) of Hg was 0.1 μg m−3, which met the actual measurement needs and the relative standard deviation (RSD) was 2% (n=11), the linear correlation coefficient was better than 0.999. The accuracy and practicality of GA-APGD-AES were verified by the analysis of flue gas. The results were consistent with those of a direct mercury analysis (DMA) system (n=3, relative deviation was less than 3 %).
在这项工作中,基于氢和氦气(H2-He)中的直流大气压辉光放电原子发射光谱(APGD-AES)与金汞合金富集(GA)相结合,开发了一种用于测定烟气中汞含量的高灵敏度程序。冷蒸汽发生(CVG)系统产生的校准汞蒸汽被送入 GA 系统进行富集。随后,汞被热解析并传送到 APGD 进行激发,同时用微型光谱仪记录 253.6 纳米波长的信号。对 GA 和 APGD 系统的参数进行了优化,包括载气类型和流量、放电电流和放电间隙。在最佳操作条件下,当烟气采样量为 10 L 时,汞的检出限(DL)为 0.1 μg m-3,满足实际测量需要,相对标准偏差(RSD)为 2%(n=11),线性相关系数优于 0.999。烟气分析验证了 GA-APGD-AES 的准确性和实用性。结果与直接汞分析(DMA)系统的结果一致(n=3,相对偏差小于 3%)。
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引用次数: 0
Multi-Channel Dilution Analysis 多通道稀释分析
IF 3.4 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-07-09 DOI: 10.1039/d4ja00112e
Willis B. Jones, Robbie M. Huff, Adam L. Richardson, Taylor Dessoffy, Sophie M. Lewis, Alexandria Eddy, Abigail J. Crossman, Bradley T. Jones
Multi-channel dilution analysis (MCDA) is a new calibration method that performs multiple dilutions of a standard solution as it makes its way from an autosampler to an analytical instrument. MCDA is based on the standard dilution analysis (SDA) method that combines the traditional standard additions and internal standardization calibration methods, correcting for both matrix interferences and fluctuations in signal levels associated with variations in the sample environment. Analysts operate the instrument in the normal manner, as all dilutions are performed automatically by splitting the sample stream entering the instrument into multiple channels of different tubing diameters and lengths. This setup results in a signal “stairstep” as portions of solution are measured at different points in time. A calibration curve is prepared from the plateau regions of the signal stairstep. MCDA has been exhibited using inductively coupled plasma optical emission spectrometry, which is a workhorse for the determination of trace metals in solution. However, MCDA is applicable for any analyte of interest in any sample type, as long as the selected measurement technique accepts samples as a flowing liquid stream. MCDA is applied to the analysis of three certified reference materials by inductively coupled plasma optical emission spectrometry (ICP-OES). Percent recoveries for a suite of analytes range from 87-106%, with relative standard deviations on the order of 1%. MCDA simplifies the analysis process, increasing sample throughput by significantly decreasing the time required for solution preparation.
多通道稀释分析(MCDA)是一种新的校准方法,在标准溶液从自动进样器进入分析仪器的过程中对其进行多次稀释。MCDA 以标准稀释分析 (SDA) 方法为基础,结合了传统的标准添加和内部标准化校准方法,可校正基质干扰和与样品环境变化相关的信号水平波动。分析人员以正常方式操作仪器,因为所有稀释都是通过将进入仪器的样品流分成不同管径和长度的多个通道自动进行的。这种设置会导致信号 "步进",因为在不同的时间点测量溶液的不同部分。根据信号 "台阶 "的高原区绘制校准曲线。MCDA 已通过电感耦合等离子体光发射光谱法进行了展示,这是测定溶液中痕量金属的主要方法。不过,MCDA 也适用于任何样品类型中的任何分析物,只要所选的测量技术能接受流动液流样品即可。MCDA 适用于通过电感耦合等离子体光发射光谱法 (ICP-OES) 分析三种经认证的标准物质。一系列分析物的回收率为 87-106%,相对标准偏差在 1%左右。MCDA 简化了分析过程,大大减少了溶液制备所需的时间,从而提高了样品处理量。
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引用次数: 0
Potential of external (in air) particle induced gamma-ray emission method for the preparation of isotopic composition of boron in-house reference standard in boron carbide matrix for quality control work 外部(空气中)粒子诱导伽马射线发射法在碳化硼基质中制备硼内部参考标准同位素组成的潜力,用于质量控制工作
IF 3.4 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-07-08 DOI: 10.1039/d4ja00156g
Sk Wasim Raja, R. Acharya, Arati D. Sonawane, T. S. R. C. Murthy, S. Majumdar
The quality control (QC) of an analytical method for any analytical data measurement depends directly on the matrix matching standard and certified reference material (CRM). In many cases, obtaining a matrix match standard and an RM or CRM as a control sample in sufficient amounts for QC analysis is difficult. It is also not advised to use a CRM as a standard for routine analysis owing to its high cost and availability in lower quantities. In view of this, in-house reference standards/materials for isotopic compositions of boron (IC, 10B/11B atom ratio) in natural and enriched boron carbide matrix were prepared in the present work. These in-house reference standards/materials will be helpful for method validation, quality control and quality assurance in the IC determination of boron carbide samples using particle induced gamma-ray emission (PIGE) method. A total of five different isotopic compositions, namely natural (19.8 atom% of 10B) and 30, 40, 50 and 67 atom% of 10B-enriched B4C, were prepared in sufficient quantities (0.8 kg each). Homogeneity and stability tests were performed for the prepared materials with respect to their isotopic composition by analysing direct powder samples using the external PIGE method, and they were found sufficiently homogeneous and stable for the property value for use as in-house reference standards. Assigned values of isotopic compositions were determined through external PIGE using both powder and pellet samples. The obtained values of the isotopic compositions are 0.247(1), 0.427(2), 0.662(3), 0.991(4), and 2.028(7) for the natural and 30, 40, 50 and 67 atom% of 10B-enriched boron carbide, respectively.
任何分析数据测试方法的质量控制 (QC) 都直接取决于基质匹配标准和有证标准物质 (CRM)。在许多情况下,很难获得足够数量的基质匹配标准和 RM 或有证标准物质作为质控分析的对照样品。此外,由于有证标准物质成本高、数量少,也不建议将其作为常规分析的标准。有鉴于此,本研究制备了天然和富集碳化硼基质中硼同位素组成(IC,10B/11B 原子比)的内部参考标准/材料。这些内部参考标准/材料将有助于利用粒子诱导伽马射线发射(PIGE)法测定碳化硼样品中硼同位素组成的方法验证、质量控制和质量保证。共制备了五种不同的同位素成分,即天然(10B 含量为 19.8 原子%)和 30、40、50 和 67 原子%的 10B 富集 B4C,每种成分的制备量均为 0.8 千克。通过使用外部 PIGE 方法分析直接粉末样品,对所制备材料的同位素组成进行了均匀性和稳定性测试。通过使用粉末和颗粒样品的外部 PIGE 方法确定了同位素组成的指定值。天然碳化硼和 30、40、50 和 67 原子%的 10B 富集碳化硼的同位素组成值分别为 0.247(1)、0.427(2)、0.662(3)、0.991(4) 和 2.028(7)。
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引用次数: 0
Towards the best total consumption infrared-heated sample introduction system for nanoparticle measurement using single particle inductively coupled plasma mass spectrometry 为使用单颗粒电感耦合等离子体质谱仪测量纳米颗粒开发最佳总消耗量红外加热样品导入系统
IF 3.4 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-07-04 DOI: 10.1039/d4ja00075g
Zichao Zhou, Mirah J. Burgener, John Burgener, Diane Beauchemin
Nanoparticles (NPs) are ubiquitous because they find applications in nanomedicine, materials science, and consumer products to name a few, and eventually end up in the environment. The various techniques available to analyze NPs each have strengths and limitations. This study focuses on improving the single particle inductively coupled plasma mass spectrometry (spICPMS) technique to address the limitations of existing methods and improve the size detection limit for Pt and Au NPs. Infrared heating of the spray chamber and connection to the torch is used to pre-evaporate the aerosol and improve the transport efficiency. Eight modified cyclonic spray chambers with a volume ranging from 25 to 125 mL, where an IR emitter is inserted in a modified baffle and the gap between the top of the baffle and the top service of the spray chamber was varied, are tested for the characterization of NPs to see their effect on sensitivity, detection limit, and transport efficiency. The results indicate that the 50 mL modified spray chamber with a 2 mm gap between the top of the baffle and the top service of the spray chamber offers the best detection limit for Pt. It enhances sensitivity and precision and allows accurate characterization of Au and Pt NPs without any measurement of the transport efficiency. Furthermore, this sample introduction system provided similar improvements in sensitivity and detection limit when used with the same nebulizer on two different spICPMS instruments.
纳米粒子(NPs)无处不在,因为它们被应用于纳米医学、材料科学和消费品等领域,并最终进入环境。用于分析 NPs 的各种技术各有优势和局限性。本研究的重点是改进单颗粒电感耦合等离子体质谱(spICPMS)技术,以解决现有方法的局限性,并提高铂和金 NPs 的尺寸检测限。喷雾室的红外加热和与火炬的连接用于预蒸发气溶胶和提高传输效率。为表征 NPs,测试了 8 个容积从 25 到 125 mL 不等的改良旋风式喷雾室,在这些喷雾室中,红外发射器插入改良挡板,挡板顶部与喷雾室顶部服务之间的间隙各不相同,以观察它们对灵敏度、检测限和传输效率的影响。结果表明,50 mL 改良喷雾室的挡板顶部与喷雾室顶部服务之间的间隙为 2 mm,可提供最佳的铂检测限,提高了灵敏度和精度,无需测量传输效率即可准确表征金和铂 NPs。此外,在两台不同的 spICPMS 仪器上使用相同的雾化器时,该样品导入系统在灵敏度和检测限方面也有类似的改进。
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引用次数: 0
Reference value of the JNdi-1 isotopic material without normalization 未经归一化处理的 JNdi-1 同位素材料参考值
IF 3.4 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-07-03 DOI: 10.1039/d4ja00140k
Alexandre Quemet, Guillaume Lasnier, Sébastien Mialle, Hélène Isnard, Maud Boyet, Marion Garçon, Delphine Auclair
The most used international reference material for neodymium isotope ratio is the JNdi-1 standard. The literature reference values were evaluated by Thermal Ionization Mass Spectrometry (TIMS) and using a conventional internal normalization. In nuclear field, such normalization is not possible for samples after irradiation, as there is no known and stable isotope ratio that can be considered as a reference ratio. To offer reference values without normalization, 61 measurements of the JNdi-1 material were obtained in three different laboratories on four thermal ionization mass spectrometers using the total evaporation method. Acquired measurements were compared to the exponential mass fractionation law demonstrating that the dominant bias comes from isotope fractionation which can be minimized using the total evaporation method. The suggested reference values and its associated uncertainties with a coverage factor of 2 were calculated using the DerSimonian-Laird procedure (n=3): 142Nd/144Nd = 1.13966(23), 143Nd/144Nd = 0.511613(50), 145Nd/144Nd = 0.348729(33), 146Nd/144Nd = 0.72329(15), 148Nd/144Nd = 0.242505(95) and 150Nd/144Nd = 0.23780(14). All these ratios are significantly different from those obtained after normalization using 146Nd/144Nd=0.7219. The acquired values can be used in nuclear laboratories where Nd isotope ratios differ from natural isotopic compositions. The Nd isotopic analysis is essential for calculating the burnup of a reactor.
国际上最常用的钕同位素比值参考材料是 JNdi-1 标准。文献参考值是通过热电离质谱法(TIMS)和传统的内部归一化方法评估的。在核领域,辐照后的样品不可能进行这种归一化,因为没有已知和稳定的同位素比值可作为参考比值。为了提供无需归一化的参考值,我们在三个不同的实验室使用四台热电离质谱仪,采用全蒸发法对 JNdi-1 材料进行了 61 次测量。获得的测量结果与指数质量分馏定律进行了比较,结果表明,主要偏差来自同位素分馏,而使用全蒸发方法可以将这种偏差降至最低。使用 DerSimonian-Laird 程序(n=3)计算了建议的参考值及其相关的不确定性(覆盖因子为 2):142Nd/144Nd = 1.13966(23),143Nd/144Nd = 0.511613(50),145Nd/144Nd = 0.348729(33),146Nd/144Nd = 0.72329(15),148Nd/144Nd = 0.242505(95),150Nd/144Nd = 0.23780(14)。所有这些比率都与使用 146Nd/144Nd=0.7219 进行归一化后得到的比率有明显差异。获得的数值可用于钕同位素比值与天然同位素组成不同的核实验室。钕同位素分析对于计算反应堆的燃烧率至关重要。
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引用次数: 0
期刊
Journal of Analytical Atomic Spectrometry
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