{"title":"Non-Destructive Micro X-Ray Fluorescence Quantitative Analysis Of Geological Materials","authors":"Jinhua Li","doi":"10.46770/as.2022.112","DOIUrl":"https://doi.org/10.46770/as.2022.112","url":null,"abstract":": Micro X-ray fluorescence (µXRF) is an atomic spectroscopy for analyzing micro areas of a sample using Xray beams and mapping elemental distribution on the sample by spectrum acquisition at individual pixel positions. We have examined the potential of rapid and non-destructive µXRF analysis to quantitatively determine the chemical composition of geological samples by correcting standardless fundamental parameters (SFP) quantification data. Based on analysis and comparison of a set of certified international standard silicate glass, linear relationships between μXRF SFP quantification data and certified values of Na 2 O, MgO, Al 2 O 3 , SiO 2 , K 2 O, CaO, TiO 2 , MnO, and FeO were developed, and the corresponding calibration equations were calculated. Further tests on flat or uneven homogeneous glass demonstrated that calibrated results of all major elements were similar with certified values, with improved accuracy of ~10%. Analysis of typical geological materials, including pure minerals, heterogeneous basaltic rock, and micro areas, indicated calibrated results were closer to certified/reference values for most elements. This study reveals that µXRF is a promising technique for rapid, non-destructive, and quantitative investigation of chemical composition of specimens at the microscale level. µXRF measurements and calibration equations developed in this study could be used to rapidly characterize geological materials and non-destructively analyze precious extraterrestrial materials.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2022-09-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47086940","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Radiocarbon Sample Preparation Based On The Flam-Sealed Zn/Fe Reduction Method In Accelerator Mass Spectrometry Analysis","authors":"Shenghua Liu","doi":"10.46770/as.2022.121","DOIUrl":"https://doi.org/10.46770/as.2022.121","url":null,"abstract":": An alternative radiocarbon sample preparation with the flame-sealed Zn/Fe reduction method by removing the reagent of TiH 2 was developed, and the specifications and practices are described in detail. The graphitization parameters were optimized with 5 mg Fe powder (-325 mesh; H 2 -reduced spherical particles) as the catalyst, 15 mg Zn dust as the sole reductant and a reduction temperature of 500 °C for 3 h, followed by 550 °C for 4 h. The μm-scale morphology indicated that the spherical Fe particles were coated with a mix of graphite sheets and fuzz carbon. Simultaneously, SEM–EDS, XRD and XPS verified that the graphite-Fe target consisted of mostly graphitizable semidisordered carbon and Zn-Fe crystals, with minimal amounts of ZnO and Fe 3 ZnC crystals, which jointly ensured good performance (high and stable ion current output and good thermal conductivity) during the AMS measurements. The average fraction modern values of the SRM OX-II (consensus value, Fm=1.3407 ± 0.0019) and SRM IAEA-C7 (consensus value, Fm=0.4953 ± 0.0012) samples prepared from 2017 to present were 1.3403 ± 0.0058 (n=73) and 0.4964 ± 0.0031 (n=18), respectively. Thus, the long-term precision of the Zn/Fe sealed tube method was better than 6‰ and good accuracy was achieved over several years. The average background 14 C age of inorganic material was 43392 ± 1489 yr BP (n=44), and the ages of two 14 C-free organic materials were 45285 ± 2016 yr BP (n=15) and 46388 ± 2306 yr BP (n=36), indicating that low and stable carbon contamination levels were maintained throughout the entire chemical preparation process and AMS measurement over the last couple of years. The consistency between measured values and preferential values makes us confident in the preparation of various types of natural samples at normal mass size with our established vacuum line using the flame-sealed Zn/Fe reduction method.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2022-09-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46990272","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Correction Of Self-Absorption Effect In Laser-Induced Breakdown Spectroscopy Analysis For Sea Salt Aerosols Using A Duplicating Mirror","authors":"Lianbo Guo","doi":"10.46770/as.2022.136","DOIUrl":"https://doi.org/10.46770/as.2022.136","url":null,"abstract":": Sea salt aerosols significantly impact marine ecosystems and climate change; however, self-absorption effects unavoidably occur in the detection of sea salt aerosols via laser-induced breakdown spectroscopy (LIBS). This work illustrates the application of a renowned replica plasma method for self-absorption correction in the detection of sea salt aerosols via LIBS. Two sets of spectral data were obtained by adding a duplicating mirror behind the plasma, and the self-absorption correction factor was calculated using a previously described method. Consequently, the experimental results show a marked improvement in the linearity of the calibration curve. The determination coefficients of linear fitting were above 0.99, and the root mean square error of the cross-validation RMSECV was negligible. The duplicating mirror method for self-absorption correction in the detection of sea salt aerosols via LIBS can thus achieve high accuracy and stability within a certain range and therefore can prove useful for sea salt aerosol, aerosol, and gas detection.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2022-09-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47582360","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Non-Destructive Identification And Quantification Of Ilmenite From A Single Particle Of The Chang’E-5 Lunar Soil Sample","authors":"Jinhua Li","doi":"10.46770/as.2022.029","DOIUrl":"https://doi.org/10.46770/as.2022.029","url":null,"abstract":": Ilmenite (FeTiO 3 ) is an early crystallization product of lunar magma and is the most abundant oxide mineral in lunar mare basalts. It is an important lunar resource that is mainly used for He and O 2 production, but also as a source of Fe. Therefore, the identification and quantification of ilmenite from lunar mare basalts is crucial to better understand lunar geological processes and develop lunar resources. Herein, a correlative micro-X-ray fluorescence (µXRF) and three-dimensional X-ray microscopy (3D XRM) approach was applied to non-destructively identify and quantify ilmenite from micro-sized single particles in China’s Chang’E-5 (CE-5) lunar soil samples. Ti-rich particles (P15 and P17) were selected from CE-5 lunar soil samples using scanning µXRF measurements. Scanning electron microscopy (SEM) indicated that both particles contained tiny ilmenite grains, but different major minerals. Ilmenite grains within these two particles were visualized and quantified using 3D XRM analyses. The ilmenite mass fractions estimated using the 3D XRM technique were similar to those obtained via µXRF quantification. Therefore, this study provides a novel nondestructive strategy for rapid ilmenite identification and quantification from single particles in CE-5 soil samples. This protocol can be replicated to characterize ilmenite and other minerals in precious extraterrestrial samples.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2022-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48919258","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"In Situ SIMS Carbon Isotopic Analysis Of Carbon-Bearing Minerals In Nantan And Aletai Iron Meteorites: Implications On Genesis","authors":"Ye Li","doi":"10.46770/as.2022.028","DOIUrl":"https://doi.org/10.46770/as.2022.028","url":null,"abstract":": A better understanding of the fractionation properties of carbon isotope between different carbon-bearing minerals will provide insights into the core-forming process of planets. In this study, we carried out an integrated study of petrography and in situ secondary ion mass spectroscopy (SIMS) carbon isotopic analysis for Nantan and Aletai iron meteorites. Haxonite in Aletai IIIE-an iron meteorite has a δ 13 C value of −14.80 ± 2.31‰, which is different from that of haxonite in Colonia Obrera IIIE iron meteorite. This suggests that the parent body of Aletai has a different initial carbon isotopic composition or experienced different planetary processes ( e.g. , degassing of CO 2 /CH 4 ). A graphite-rich nodule in Nantan IAB iron meteorite, characterized by a core-mantle-rim texture, was systematically studied. Some graphite grains in the nodule mantle (GNM; δ 13 C value as low as −14.65‰) and all graphite grains in the nodule rim (GNR; δ 13 C = −12.65 ± 2.90‰) are more depleted in 13 C than those in the nodule core (GNC; δ 13 C = −7.17 ± 2.42‰). This could be due to the preferential incorporation of 13 C into the early-crystallized GNC. The carbon isotopic fractionation (Δ 13 C = 6.9 ± 2.7 ‰) between coexisting GNR (δ 13 C = −12.65 ± 2.90‰) and cohenite (δ 13 C = −19.60 ± 2.59‰) yielded an equilibrium temperature of ~950–1310 °C, supporting the melt-crystallization genesis for nodule. We concur with previous studies that the early differentiation of Earth could have led to positive carbon isotopic fractionation between graphite/diamond in the mantle and metallic melt sinking to the core.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2022-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43181201","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Microanalysis Techniques Guarantee Long-Term Research On Chang’e-5 Lunar Samples","authors":"Wei Yang, Jinhua Li, Xiong-Yao Li, Yong He","doi":"10.46770/as.2022.025","DOIUrl":"https://doi.org/10.46770/as.2022.025","url":null,"abstract":"Humans have successfully returned samples from the Moon ten times. Sample return missions have two advantages. First, we can carry out high-resolution and high-precision measurements of returned samples using state-of-the-art technologies in the laboratory. Second, the returned samples can support ongoing research for decades or centuries. The same sample can continuously “tell new stories” with the advancement of technology. On July 12, 2021, the allocation of the first batch of Chang'e-5 lunar samples quickly ignited a research bonanza for lunar and planetary sciences in China. State-of-the-art microanalysis techniques have played important roles in both scientific research and the artistic creation of lunar samples. For example, the combination of micro-X-ray fluorescence (μXRF), 3D X-ray microscopy (XRM), and scanning electron microscopy the rapid screening and positioning of Zr-bearing minerals for U-Pb dating. The high spatial resolution U-Pb dating method by secondary ion mass spectrometry it possible to determine the crystallization age of tiny (< tomography; 27 (4) trace element analyses by instrumental neutron activation analysis; 28 (5) high-resolution Cl isotope analyses by NanoSIMS 29 and high-precision C isotope analyses by SIMS; 30 (6) combined separation for high-precision iron, calcium, and magnesium isotope analyses; 31 (7) measurements of thermal-induced alterations by in situ TEM heating; 32 and (8) identification of lunar highland clasts in CE-5 breccias by TIMA-SEM-EPMA.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2022-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46405350","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"First Location And Characterization Of Lunar Highland Clasts In Chang’E-5 Breccias Using TIMA-SEM-EPMA","authors":"Shui‐Jiong Wang","doi":"10.46770/as.2022.030","DOIUrl":"https://doi.org/10.46770/as.2022.030","url":null,"abstract":"In this study, we identify for the first time four lunar highland clasts from the breccias (CE5C0800YJYX132GP) returned by the Chang’E 5 (CE-5) mission by combining Tescan Integrated Mineral Analysis (TIMA), Scanning Electron Microscopy (SEM), and Electron Probe Microanalysis (EPMA) techniques. The chemical compositions of plagioclases (An93.9–97.6) and mafic minerals (Fo71.4–87.9 for olivine and Mg65.1–84.6 for pyroxene) in these clasts are remarkably distinct from the more abundant mare basalts in the CE-5 landing site. They are in noritic anorthositic, troctolitic anorthositic, and troctolitic anorthositic compositions, which represent lunar highland crustal materials. Additionally, the three anorthositic clasts in the CE-5 samples are more magnesian than the Apollo ferroan anorthosites (FANs), but are similar to the magnesian anorthosites (MANs) commonly found in lunar highland meteorites. These newly found MANs in the CE-5 breccia are among the few reported in lunar returned samples, and may represent an important component of the lunar highland crust. Placing MANs in the rock lithologies of lunar feldspathic crust require a more complex crust-mantle process than that predicted by the classic Lunar Magma Ocean (LMO) hypothesis. Therefore, future research and characterization of Mg-suite and magnesian anorthositic rocks in CE-5 samples may help elucidate early lunar crustal evolution and crustmantle interaction.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2022-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47096267","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Determination Of The Multi-Elemental Composition Of Lunar Meteorites Using Instrumental Neutron Activation Analysis","authors":"Caijin Xiao","doi":"10.46770/as.2022.026","DOIUrl":"https://doi.org/10.46770/as.2022.026","url":null,"abstract":": The Moon is a key target for long-term human exploration beyond the Earth. In addition to precious lunar returned samples, lunar meteorites can provide important supplementary information on the composition and evolutionary history of the Moon. Herein, we report the elemental compositions of two lunar meteorites, Northwest Africa (NWA) 4734 and NWA 11111, analyzed using instrumental neutron activation analysis (INAA). Reference materials, including SRM2703 and GWB07105, were used for quality control. The INAA results for most elements in NWA 4734 and NWA 11111 are consistent with the previously reported data obtained by inductively coupled plasma-mass spectrometry analysis within analytical uncertainties. Since the INAA analysis is non-destructive, it can be widely applied to trace element measurements for extraterrestrial samples.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2022-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44188684","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"ICP-MS-Based Methodology In Metallomics: Towards Single Particle Analysis, Single Cell Analysis, And Spatial Metallomics","authors":"Mingli Chen, Meng Wang","doi":"10.46770/as.2022.108","DOIUrl":"https://doi.org/10.46770/as.2022.108","url":null,"abstract":": As an emerging interdisciplinary science, metallomics aims to integrate research fields related to metals and metalloids in biological systems from a systematic perspective. Inductively coupled plasma mass spectrometry (ICP-MS) is considered one of the most versatile tools for metallomics research. This review presents a brief overview of ICP-MS and describes recent advances in ICP-MS instrumentation. Then, ICP-MS-based methods and applications are discussed, focusing on single particle analysis, single cell analysis, and spatial metallomics. With the rapid developments in instrumentation and methodology, ICP-MS-based methodologies will evolve further and play a dominant role in metallomics research.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2022-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45187315","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Iron Isotopic Measurement Using Large-Geometry High-Resolution Multi-Collector Inductively Coupled Plasma Mass Spectrometer","authors":"Ming Li","doi":"10.46770/as.2022.111","DOIUrl":"https://doi.org/10.46770/as.2022.111","url":null,"abstract":": High-precision and accurate Fe isotopic analyses are essential for various geological processes. In this study, Fe isotopic measurements were optimized on a large-geometry, high-resolution Nu Plasma 1700 MC-ICP-MS instrument, which can distinguish Ar-related interferences completely as opposed to other general-sized MC-ICP-MS instruments. Under the conditions of high mass resolution, complete separation of Ar-related interference can be achieved. We evaluated the type and intensity of all Ar-related interferences. The effects of the acid molarity, concentration mismatch, residual HCl, and matrix elements were also evaluated. The results demonstrate that the molarity of the acid, residual HCl, and Cr significantly affected the precision of the Fe isotopic measurements. Fe was purified by one-step column anion-exchange separation using the anion resin AG-MP-1M. The long-term external precisions of δ 56 Fe and δ 57 Fe were greater than ± 0.03‰ (2SD) and ± 0.06‰ (2SD), respectively. The Fe isotopic compositions of the five geological reference materials measured in this study agreed with previously published data, within uncertainties.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2022-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47964798","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}