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Evaluation of miniaturized ultrasonic nebulization for high-efficiency sampling in characterization of silver nanoparticles by single particle inductively coupled plasma mass spectrometry† 在利用单颗粒电感耦合等离子体质谱法表征银纳米颗粒时,对用于高效采样的小型化超声雾化技术进行评估†。
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-10-21 DOI: 10.1039/D4JA00320A
Junhang Dong, Zhenli Zhu, Lujie Li, Pengju Xing, Shuyang Li, Lei Ouyang, Xing Liu, Wei Guo, Hongtao Zheng and Rong Qian

Single particle inductively coupled plasma mass spectrometry (spICP-MS) has become a powerful tool for the simultaneous characterization of the size, elemental composition and concentration of nanoparticles (NPs). However, the conventional pneumatic nebulization (PN) sampling system used in spICP-MS suffers from low transport efficiency (1–5%), limiting its effectiveness in analyzing environmentally relevant samples with low NP concentrations. To address this limitation, we evaluated a self-designed high-efficiency miniaturized ultrasonic nebulization (MUN) sampling system for spICP-MS analysis. This novel sampling system achieves an exceptionally high transport efficiency of approximately 80% for silver (Ag) NPs. Remarkably, this high transport efficiency is maintained across a sample uptake rate range of 10–25 μL min−1, outperforming other reported highly efficient nebulizers where TE significantly decreased with the increase in sampling rate. The effectiveness and reliability of the MUN system were further demonstrated by analyzing standard Ag NPs of 60 nm and 100 nm, confirming the accurate characterization of particle size distribution. Overall, our MUN-spICP-MS offers a cost-effective and highly efficient method for characterizing NPs, which is of great significance for the NP characterization in natural environmental samples with low particle sizes and concentrations.

单颗粒电感耦合等离子体质谱法(spICP-MS)已成为同时表征纳米颗粒(NPs)尺寸、元素组成和浓度的有力工具。然而,spICP-MS 使用的传统气动雾化(PN)采样系统的传输效率较低(1-5%),限制了其在分析 NP 浓度较低的环境相关样品时的有效性。为了解决这一局限性,我们评估了一种用于 spICP-MS 分析的自行设计的高效微型超声雾化(MUN)取样系统。这种新型取样系统对银 (Ag) NPs 的传输效率非常高,约为 80%。值得注意的是,在 10-25 μL min-1 的样品吸收率范围内都能保持如此高的传输效率,优于其他已报道的高效雾化器,后者的 TE 会随着采样率的增加而显著降低。通过分析 60 nm 和 100 nm 的标准 Ag NPs,进一步证明了 MUN 系统的有效性和可靠性,证实了粒度分布的准确性。总之,我们的 MUN-spICP-MS 为表征 NPs 提供了一种经济高效的方法,这对于表征低粒度和低浓度自然环境样品中的 NP 具有重要意义。
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引用次数: 0
Atomic spectrometry update: review of advances in the analysis of metals, chemicals and materials 原子光谱分析法最新进展:金属、化学品和材料分析进展回顾
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-10-18 DOI: 10.1039/D4JA90052A
Eduardo Bolea-Fernandez, Robert Clough, Andy Fisher, Bridget Gibson and Ben Russell

This update covers the literature published between approximately June 2023 and April 2024 and is the latest part of a series of annual reviews. It is designed to provide the reader with an overview of the current state of the art with respect to the atomic spectrometric analysis of various metals, chemicals and materials. Data processing appears to be the hottest topic in many of the areas. This is especially true for LIBS and (TOF)-SIMS, where huge amounts of data can be acquired. Methods have been used to decrease the dimensions of the data whilst still retaining the most important information. This can then be input into a machine-learning algorithm so that the provenance of a sample, the sample type, or, in the case of TOF-SIMS data, a clear characterisation of the surface of the sample can be obtained while using less computing power and less processing time. Although these algorithms have been used for some years, their use is expanding into new areas. Another development is the combination of complementary techniques on the same instrument platform. This enables data from the two techniques to be obtained simultaneously and from the same spot on the sample. With regard to the different analytical techniques used, LIBS is continuing to increase in popularity, bolstering its reputation as being the rising superstar of the analytical world.

本次更新涵盖了大约 2023 年 6 月至 2024 年 4 月期间出版的文献,是年度综述系列的最新部分。它旨在为读者提供有关各种金属、化学品和材料的原子光谱分析技术现状的概览。数据处理似乎是许多领域最热门的话题。尤其是在可以获取大量数据的 LIBS 和 (TOF)-SIMS 领域。我们已经采用了一些方法来减少数据的尺寸,同时仍然保留最重要的信息。然后将这些信息输入机器学习算法,这样就可以在使用较少计算能力和处理时间的情况下,获得样品的来源、样品类型,或 TOF-SIMS 数据,样品表面的清晰特征。虽然这些算法已经使用了数年,但其应用正在向新的领域扩展。另一项发展是在同一仪器平台上结合使用互补技术。这样就能同时从样品的同一个点获得两种技术的数据。就所使用的各种分析技术而言,LIBS 的普及率正在不断提高,使其作为分析界冉冉升起的超级明星的声誉更加响亮。
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引用次数: 0
Assessing the performance of handheld LIBS for predicting soil organic carbon and texture in European soils† 评估手持式 LIBS 在预测欧洲土壤有机碳和质地方面的性能†。
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-10-17 DOI: 10.1039/D4JA00292J
Alex Wangeci, Maria Knadel, Olga De Pascale, Mogens H. Greve and Giorgio S. Senesi

Laser-induced breakdown spectroscopy (LIBS) has contributed to the advanced and rapid determination of soil properties including soil organic carbon (SOC) and texture. Recent developments of commercial handheld LIBS (hLIBS) have allowed the use of the technique directly in the field. However, to date, the performance of hLIBS on different types of soils covering wide geographical distributions has not been evaluated. In this study, a total of 305 soil samples covering a continental scale were used to assess the repeatability and reproducibility of LIBS data acquired using a commercially available hLIBS instrument. Furthermore, the performance of the prediction models for SOC and texture was evaluated based on the prediction error. The repeatability and reproducibility of LIBS data were evaluated based on the relative standard deviation (RSD) for measurements performed under similar and different environmental conditions (temperature and humidity). First, the RSD of the signal ratios and the predicted values for soil properties under investigation were calculated. Then, the prediction accuracy of the various soil properties was compared based on the standardized root mean error of prediction (SRMSEP) and the ratio of performance to interquartile distance (RPIQ). The signal ratios assessed using the C, Si, Ca, and K LIBS emission lines achieved a repeatability of 4–9% and a reproducibility of 7–10%, whereas the repeatability and reproducibility for predicting SOC and texture were <25%. The prediction of sand content exhibited the lowest error (SRMSEP = 0.14) followed by clay and silt (SRMSEP = 0.15), and then SOC (SRMSEP = 0.16). The results of this work underscore the promising potential of hLIBS for large-scale SOC and texture determination, with the opportunity to enhance the prediction accuracy by integrating soil mineralogy information for soil classification before applying the modeling process.

激光诱导击穿光谱(LIBS)有助于先进、快速地测定土壤特性,包括土壤有机碳(SOC)和质地。最近开发的商用手持式激光诱导击穿光谱仪(hLIBS)可以直接在野外使用该技术。然而,迄今为止,还没有人对 hLIBS 在不同类型、广泛地理分布的土壤上的性能进行过评估。在本研究中,共使用了 305 个覆盖整个大陆的土壤样本,以评估使用市售 hLIBS 仪器获取的 LIBS 数据的可重复性和再现性。此外,还根据预测误差评估了 SOC 和质地预测模型的性能。根据在相似和不同环境条件(温度和湿度)下进行测量的相对标准偏差(RSD),对 LIBS 数据的重复性和再现性进行了评估。首先,计算信号比的 RSD 和所研究土壤性质的预测值。然后,根据预测的标准化均值误差(SRMSEP)和性能与四分位距之比(RPIQ)比较各种土壤特性的预测精度。使用 C、Si、Ca 和 K LIBS 发射线评估的信号比的重复性为 4-9%,重现性为 7-10%,而预测 SOC 和质地的重复性和重现性为 25%。含沙量的预测误差最小(SRMSEP = 0.14),其次是粘土和粉土(SRMSEP = 0.15),然后是 SOC(SRMSEP = 0.16)。这项工作的结果凸显了 hLIBS 在大规模 SOC 和质地测定方面的巨大潜力,在应用建模过程之前,可通过整合土壤矿物学信息进行土壤分类,从而提高预测精度。
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引用次数: 0
Research on a bimodal fusion detection method for surface defects of metal AM components based on LIBS 基于 LIBS 的金属 AM 组件表面缺陷双模融合检测方法研究
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-10-08 DOI: 10.1039/D4JA00159A
Xiaomei Lin, Jiangfei Yang, Yutao Huang, Jingjun Lin and Changjin Che

Metal Additive Manufacturing (AM) holds significant importance in advancing intelligent manufacturing and sustainable development. However, due to the unique manufacturing process of AM, defect detection in AM components has always been a challenging issue. This study employed Laser-Induced Breakdown Spectroscopy (LIBS) technology to capture spectral information and utilized a high-speed camera to record plasma images, comprehensively extracting pertinent details from each laser event. LIBS spectral scores were obtained via principal component analysis (PCA) and plasma image features were extracted to generate a bimodal fusion descriptor. This descriptor was employed to enhance the detection capability of three common surface defects in metal AM, specifically holes, cracks and bulges. Building on this foundation, a mid-level data fusion technique was employed to integrate the scores of LIBS spectra derived from PCA with seven features extracted from plasma images, resulting in the development of a bimodal fusion approach. Subsequently, the distribution of spectral data, plasma image features and bimodal fusion descriptors was discussed. Finally, three models, namely Random Forest (RF), Support Vector Machine (SVM) and Linear Discriminant Analysis (LDA), were used to evaluate the recognition accuracy of component defects. Additionally, the application scenarios of these three different models in spectral data, plasma image features and bimodal fusion descriptors were compared. The results indicate that the LDA model, utilizing bimodal fusion descriptors, yields the most effective classification. For samples #1–#100, the accuracy increased from 99.08% and 97.94% for spectral data and plasma image features to 99.92% for fusion data. Similarly, for samples #101–#120, the accuracy increases from 97.19% and 96.21% for spectral data and plasma image features to 97.34% for fusion data. This method improves the recognition of different defects of metal AM components. This study represents a first attempt to enhance the capability of LIBS in distinguishing various surface defects of metal AM components by inputting laser plasma image data and spectral information to generate statistical descriptors. The bimodal fusion approach offers an efficient method for detecting surface defects of metal AM components, characterized by low data complexity.

金属增材制造(AM)在推进智能制造和可持续发展方面具有重要意义。然而,由于 AM 制造工艺的特殊性,AM 部件的缺陷检测一直是一个具有挑战性的问题。本研究采用激光诱导击穿光谱(LIBS)技术捕捉光谱信息,并利用高速相机记录等离子体图像,全面提取每个激光事件的相关细节。通过主成分分析 (PCA) 获得 LIBS 光谱分数,并提取等离子体图像特征,生成双峰融合描述符。该描述符用于增强金属 AM 中三种常见表面缺陷的检测能力,特别是孔、裂纹和凸起。在此基础上,采用了中层数据融合技术,将 PCA 得出的 LIBS 光谱得分与等离子图像提取的七个特征进行整合,从而开发出一种双模融合方法。随后,讨论了光谱数据、等离子图像特征和双模融合描述符的分布。最后,使用随机森林(RF)、支持向量机(SVM)和线性判别分析(LDA)这三种模型来评估组件缺陷的识别精度。此外,还比较了这三种不同模型在光谱数据、等离子图像特征和双模融合描述符中的应用场景。结果表明,利用双模融合描述符的 LDA 模型能产生最有效的分类。对于 #1-#100 样品,准确率从光谱数据和等离子图像特征的 99.08% 和 97.94% 提高到融合数据的 99.92%。同样,对于 #101-#120 样品,准确率从光谱数据和等离子图像特征的 97.19% 和 96.21% 提高到融合数据的 97.34%。这种方法提高了对金属 AM 组件不同缺陷的识别率。这项研究是首次尝试通过输入激光等离子图像数据和光谱信息来生成统计描述符,从而增强激光等离子体分析仪在区分金属 AM 组件各种表面缺陷方面的能力。双模态融合方法为检测金属 AM 组件的表面缺陷提供了一种高效方法,其特点是数据复杂度低。
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引用次数: 0
Accurate determination of ultra-trace REEs in seawater using a membrane desolvation Q-ICP-MS coupled with an online automatic separation system† 利用膜脱溶 Q-ICP-MS 和在线自动分离系统精确测定海水中的超痕量 REEs†
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-10-07 DOI: 10.1039/D4JA00240G
Ji-Hao Zhu, Feng-You Chu, Feng Liang, Xian-Ying Luo, Qiang Liu, Quan-Hui Xu, Wei Yu, Yong-Chun Li, Jiang-Gu Lu, Yun-Xiu Li, Yan-Hui Dong, Huai-Ming Li, Jun Zhao and Cai Zhang

The determination of rare earth elements (REEs) in seawater, especially marine sediment porewater and open-ocean seawater, is challenging because of their ultra-trace concentrations (ng L−1 to pg L−1) and the high salinity of the matrix (approximately 35‰ NaCl), which limits their application in marine science. Herein, we developed an online method for accurate analysis of ultra-trace REEs in seawater using a traditional Q-ICP-MS. The key aspects were: (i) high sensitivity detection in standard mode with no collision/reaction cell functioned, (ii) online automated matrix removal and preconcentration using a commercially available seaFAST system, (iii) use of membrane desolvation to enhance the sensitivity and limit the interferences of LREE oxides on HREEs, and (iv) monitoring and correction of variations in REE signal intensities caused by instrument drift using standard–samples–standard bracketing and an indium internal standard for normalization. The detection limits (0.1–8.0 pg L−1) and procedural blank values (<3 pg L−1 except for La, Ce, and Nd) of this method were low enough for accurate determination of REEs in seawater, even for REE concentrations at tens of picograms per liter level. The good accuracy and long-term precision (30 h, average: 3.5%, 1σ RSD, n = 10) were achieved for all the REEs as verified using certified seawater reference standards NASS-7 and CASS-6, and a 10 ng L−1 artificial seawater standard, respectively. Each run required only approximately 8 mL of sample and 12 min for the measurement, which are suitable values for practical application. The developed method was used to analyze various natural seawater samples, which demonstrated its effectiveness for exploring subtle changes in REE concentrations, fractionation patterns and anomalies in different marine environments.

海水,尤其是海洋沉积物孔隙水和公海海水中稀土元素(REEs)的测定极具挑战性,因为稀土元素的超痕量浓度(纳克/升-1 至皮克/升-1)和基质的高盐度(约 35‰ NaCl)限制了其在海洋科学中的应用。在此,我们开发了一种在线方法,利用传统的 Q-ICP-MS 对海水中的超痕量 REEs 进行精确分析。其关键在于(i) 在标准模式下进行高灵敏度检测,不使用碰撞/反应池功能;(ii) 使用市售的 seaFAST 系统进行在线自动基质去除和预浓缩;(iii) 使用膜脱溶来提高灵敏度并限制 LREE 氧化物对 HREEs 的干扰;(iv) 使用标准样品-标准括弧和归一化铟内标来监测和校正仪器漂移引起的 REE 信号强度变化。该方法的检出限(0.1-8.0 pg L-1)和程序空白值(<3 pg L-1,La、Ce 和 Nd 除外)都很低,足以准确测定海水中的 REEs,即使 REEs 浓度达到每升几十皮克的水平。使用经认证的海水标准物质 NASS-7 和 CASS-6 以及 10 ng L-1 人工海水标准物质分别对所有 REEs 进行了验证,结果表明该方法具有良好的准确度和长期精密度(30 h,平均:3.5%,1σ RSD,n = 10)。每次运行仅需约 8 mL 样品和 12 分钟的测量时间,这些值都非常适合实际应用。所开发的方法被用于分析各种天然海水样品,证明了其在探索不同海洋环境中 REE 浓度的微妙变化、分馏模式和异常现象方面的有效性。
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引用次数: 0
A single-column and efficient procedure for separating Fe and Mg from geological materials for isotopic analyses using MC-ICP-MS† 利用 MC-ICP-MS† 从地质材料中分离铁和镁以进行同位素分析的单柱高效程序
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-10-05 DOI: 10.1039/D4JA00272E
Guanhong Zhu, Zhenmin Ge, Le Zhang, Gangjian Wei and Jinlong Ma

Fe and Mg isotopes have increasingly served as combined proxies for geological processes. Fe and Mg isotope determination requires consuming different splits of samples and multi-column chromatographic purification to obtain pure Mg and Fe fractions in conventional chemical procedures, which is time-consuming and not suitable for rare and valuable samples. This study presents a novel and efficient chromatographic procedure to purify both Fe and Mg from geological matrices, using a single column loaded with AGMP-50 resin, followed by precise measurements of Fe and Mg isotopes by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). In our experiment, the Fe fraction was first collected using 7 mL of a mixture of 0.2 M HCl and 0.5 M HF, and then the Mg fraction was collected using 9 mL of 1.3 M HCl. This procedure is suitable for processing different types of rock samples and enabling an Fe recovery of >98% and full recovery of Mg, with effective removal of matrix elements such as Al, Ti, Na, K, Ca, and other trace elements. Using this method, the Fe and Mg isotopic compositions of various geological reference materials were reported. All of the Fe and Mg isotopic analytical results were in agreement with the reported data within analytical uncertainties, verifying that the method established here is robust and reproducible. Thus, this procedure will serve as a great option for obtaining both Fe and Mg isotopic compositions of geological samples and tracing geochemical or astrochemical processes in the future.

铁和镁同位素越来越多地成为地质过程的综合代用指标。在传统化学方法中,铁和镁同位素的测定需要对样品进行不同的分割和多柱色谱纯化,以获得纯净的镁和铁馏分,这不仅耗时,而且不适合稀有珍贵的样品。本研究提出了一种新颖高效的色谱程序,利用装有 AGMP-50 树脂的单柱从地质基质中提纯铁和镁,然后利用多收集器电感耦合等离子体质谱法(MC-ICP-MS)精确测量铁和镁的同位素。在我们的实验中,首先用 7 mL 0.2 M HCl 和 0.5 M HF 的混合物收集铁组分,然后用 9 mL 1.3 M HCl 收集镁组分。这种方法适用于处理不同类型的岩石样本,可使铁的回收率达到 98%,镁的回收率达到 100%,并能有效去除基质元素,如 Al、Ti、Na、K、Ca 和其他微量元素。利用这种方法,报告了各种地质参考材料的铁和镁同位素组成。所有的铁和镁同位素分析结果都在分析不确定性范围内与所报告的数据一致,这验证了本文所建立的方法是可靠和可重复的。因此,该方法将成为未来获取地质样本中铁和镁同位素组成以及追踪地球化学或天体化学过程的一个重要选择。
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引用次数: 0
Mg separation from samples with very high Ca/Mg ratios for Mg isotope analysis 从钙镁比非常高的样品中分离出镁,用于镁同位素分析
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-10-03 DOI: 10.1039/D4JA00266K
Niklas Keller and Michael Tatzel

Samples with very high Ca/Mg ratios present challenges for measuring their Mg isotope ratios. Here, we present an efficient method to separate Mg from samples with high Ca/Mg matrices, which also allows for quantitative separation of Sr, Ca and K. The method comprises a three-step chromatographic separation using DGA and AG50W-X12 (200–400 mesh) cation exchange resin. By utilising the automated sample purification system prepFAST MC™ for two of the three separations, the labour is substantially minimised. This analytical approach results in a quantitative Mg yield and a pure Mg solution, with other cations reduced to below the limit of detection (<53 ng mL−1). We demonstrate the efficacy of this method using a set of geochemical reference materials with Ca/Mg ratios ranging from 1.32 to 1271 mol mol−1. This approach enhances sample throughput and ensures high-quality separations in carbonate samples characterised by high Ca/Mg ratios.

钙镁比非常高的样品给镁同位素比的测量带来了挑战。在此,我们介绍一种从高 Ca/Mg 基质样品中分离镁的高效方法,该方法还可以定量分离 Sr、Ca 和 K。该方法包括使用 DGA 和 AG50W-X12(200-400 目)阳离子交换树脂进行三步色谱分离。通过使用自动样品纯化系统 prepFAST MC™ 进行三步分离中的两步,大大减少了劳动力。这种分析方法可获得定量的镁产量和纯净的镁溶液,其他阳离子的含量降至检测限以下(53 毫微克/毫升-1)。我们使用一组钙/镁比值从 1.32 到 1271 mol mol-1 的地球化学参考材料证明了这种方法的有效性。这种方法提高了样品处理量,并确保了以高 Ca/Mg 比值为特征的碳酸盐样品的高质量分离。
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引用次数: 0
Self-absorption correction of NEXAFS spectra for intermediate sample thicknesses applied to organo-sulfur model compounds† 应用于有机硫模型化合物的中间样品厚度的 NEXAFS 光谱自吸收校正†。
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-10-02 DOI: 10.1039/D4JA00232F
Konstantin Skudler, Michael Walter, Michael Sommer and Matthias Müller

Near-Edge X-ray Absorption Fine Structure (NEXAFS) spectra tend to be damped due to self-absorption effects when measured in fluorescence-yield mode in samples which are neither thin nor dilute. While established self-absorption correction methods are only valid for infinitely thick samples and partly inapplicable if the samples are too concentrated, the novel forward correction presented here is widely applicable, especially for intermediately thick and concentrated samples. Aiming towards quantitative analysis supporting the development of lithium sulfur battery materials, which are intermediately thick and not dilutable, the forward correction is applied to organo-sulfur liquid films as a proof of concept.

近边缘 X 射线吸收精细结构(NEXAFS)光谱在既不薄也不稀释的样品中以荧光-产量模式测量时,往往会由于自吸收效应而产生阻尼。已有的自吸收校正方法仅适用于无限厚的样品,如果样品过于浓缩,则部分方法不适用,而本文介绍的新型正向校正方法则广泛适用,尤其适用于中间厚和浓缩的样品。为了进行定量分析以支持锂硫电池材料的开发(这些材料厚度适中且不可稀释),正向校正法被应用于有机硫液体薄膜,作为概念验证。
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引用次数: 0
Data fusion of spectral and acoustic signals in LIBS to improve the measurement accuracy of carbon emissions at varying gas temperatures 将 LIBS 中的光谱信号和声学信号进行数据融合,以提高不同气体温度下碳排放的测量精度
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-10-02 DOI: 10.1039/D4JA00287C
Shu Chai, Jie Ren, Suming Jiang, Aochen Li, Ziqing Zhao, Haimeng Peng, Qiwen Zhang and Wendong Wu

Laser-induced breakdown spectroscopy (LIBS) is a promising technique to monitor carbon emissions in post-combustion flue gas. However, its measurement accuracy is susceptible to variations in gas temperature. In this work, a mid-level data fusion method integrating spectral and acoustic signals generated by laser-induced plasmas (LIPs) was proposed to improve the measurement accuracy. This method utilizes the high sensitivity of acoustic signals to variations in gas temperature, enabling a correction of temperature effects. The acoustic features were extracted from both the time-domain waveforms and frequency spectra, while the spectral features were selected using a SelectKBest method. These features were fused into a new array, on whose basis multivariate regression models including Partial Least Squares (PLS), Support Vector Machines (SVM), and Random Forest (RF) were trained. Data fusion significantly improved the predictive precision and trueness of SVM and RF models, with the RF model achieving the best performance: a coefficient of determination (R2) of 0.9941, a root-mean-square error (RMSE) of 0.4864, a mean absolute error (MAE) of 0.2587, and a mean absolute deviation (MAD) of 0.0980. Shapley additive explanation (SHAP) analysis revealed that in the RF model, the acoustic features that exhibited higher temperature sensitivity could be more frequently selected in the training process and thus had greater impacts on model outputs, which can better correct for the gas temperature effect. Furthermore, the potential of this method in industrial applications was demonstrated in an unsteady flow.

激光诱导击穿光谱法(LIBS)是一种用于监测燃烧后烟道气中碳排放的前景广阔的技术。然而,其测量精度易受气体温度变化的影响。在这项工作中,提出了一种中级数据融合方法,将激光诱导等离子体(LIPs)产生的光谱信号和声学信号整合在一起,以提高测量精度。该方法利用了声学信号对气体温度变化的高灵敏度,从而能够修正温度效应。声学特征是从时域波形和频谱中提取的,而频谱特征则是通过 SelectKBest 方法选择的。这些特征被融合到一个新的阵列中,并在此基础上训练了多元回归模型,包括偏最小二乘法(PLS)、支持向量机(SVM)和随机森林(RF)。数据融合大大提高了 SVM 和 RF 模型的预测精度和真实性,其中 RF 模型的性能最佳:判定系数 (R2) 为 0.9941,均方根误差 (RMSE) 为 0.4864,平均绝对误差 (MAE) 为 0.2587,平均绝对偏差 (MAD) 为 0.0980。夏普利加法解释(SHAP)分析表明,在射频模型中,温度敏感性较高的声学特征在训练过程中被选择的频率较高,因此对模型输出的影响较大,可以更好地校正气体温度效应。此外,该方法在工业应用中的潜力也在非稳态流中得到了验证。
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引用次数: 0
Efficient preconcentration of ultra-trace rhenium from geological materials via induced adsorption for accurate isotope analysis† 通过诱导吸附从地质材料中高效预富集超痕量铼,以进行精确的同位素分析†。
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-09-30 DOI: 10.1039/D4JA00295D
Yumeng Liu, Tianyu Chen, Tao Li, Weiqiang Li, Qingquan Hong and Jiubin Chen

Rhenium (Re) and its isotopes offer valuable information for understanding various geological processes throughout Earth's history. However, Re isotope analysis remains quite challenging owing to its ultra-trace concentration in geological materials. Previous studies have developed column chemistry and analytical methods for Re isotope analysis, but issues such as tedious pretreatment and incomplete Re recovery still exist. Herein, we present a novel procedure integrating preconcentration and fast column chemistry for Re isotope analysis. Utilizing Na2S solution and activated carbon powder under acidified conditions, we achieved the quantitative recovery of Re from aqueous solutions via filtration while removing most matrices. Standard addition to diverse matrix solutions yielded complete Re recovery (99.6 ± 6.7%, n = 10, 2SD) and precise isotopic compositions (δ187Re = −0.49 ± 0.04‰, n = 10, 2SD), as determined using multi-collector inductively coupled plasma–mass spectrometry. Our method was applied to seawater (7.1 pg g−1 for Re) and solid reference materials (∼0.5–75 ng g−1 for Re), which resulted in stable and high recovery with isotopic results consistent with published data. Our method exhibits efficient matrix removal with stable and essentially quantitative Re recovery, which paves the way for wide applications of Re isotopes in the earth and planetary sciences.

铼(Re)及其同位素为了解地球历史上的各种地质过程提供了宝贵的信息。然而,由于铼在地质材料中的超痕量浓度,铼同位素分析仍然具有相当大的挑战性。以往的研究已开发出用于 Re 同位素分析的柱化学和分析方法,但仍存在预处理繁琐和 Re 回收不完全等问题。在此,我们提出了一种集预浓缩和快速柱化学于一体的用于 Re 同位素分析的新方法。在酸化条件下,利用 Na2S 溶液和活性炭粉末,我们通过过滤实现了从水溶液中定量回收 Re,同时去除大部分基质。使用多收集器电感耦合等离子体质谱法测定,在不同基质溶液中添加标准物质可获得完全的铼回收率(99.6 ± 6.7%,n = 10,2SD)和精确的同位素组成(δ187Re = -0.49 ± 0.04‰,n = 10,2SD)。我们的方法适用于海水(Re 含量为 7.1 pg g-1)和固体参考材料(Re 含量为 ∼0.5-75 ng g-1),结果稳定且回收率高,同位素结果与已发表的数据一致。我们的方法具有高效的基质去除能力,能稳定且基本定量地回收 Re,为 Re 同位素在地球和行星科学中的广泛应用铺平了道路。
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Journal of Analytical Atomic Spectrometry
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