Pub Date : 2024-09-16DOI: 10.1186/s40543-024-00463-z
Lin Zhang, Min Yang, Dong Wang, Kaixin Yu, Zhuoyun Chen, Xue Bing, Peng Zhao, Yiqing Bao, Xuebo Yin
Determination of high sulfur content in sulfide minerals is crucial for various applications, including geochemistry, mining, and environmental monitoring. While inductively coupled plasma optical emission spectrometry (ICP-OES) is the preferred method for sulfur analysis, conventional sample preparation techniques often fall short when dealing with high sulfur concentrations. This study investigated optimized digestion conditions for accurate sulfur determination in sulfide minerals using ICP-OES. We employed anti-corrosion acid digestion bombs, an aqua regia–hydrofluoric acid system, and a digestion temperature of 180 °C, achieving exceptional results. Certified reference material recoveries ranged from 99.9 to 100.5%, with relative standard deviations between 0.42 and 0.84%. These results demonstrate the high accuracy and precision of the method. The optimized digestion protocol presented in this study provides a robust and reliable approach for accurate sulfur analysis in sulfide minerals, particularly for high concentrations.
{"title":"Accurate determination of high sulfur content in sulfide samples: an optimized ICP-OES method","authors":"Lin Zhang, Min Yang, Dong Wang, Kaixin Yu, Zhuoyun Chen, Xue Bing, Peng Zhao, Yiqing Bao, Xuebo Yin","doi":"10.1186/s40543-024-00463-z","DOIUrl":"https://doi.org/10.1186/s40543-024-00463-z","url":null,"abstract":"Determination of high sulfur content in sulfide minerals is crucial for various applications, including geochemistry, mining, and environmental monitoring. While inductively coupled plasma optical emission spectrometry (ICP-OES) is the preferred method for sulfur analysis, conventional sample preparation techniques often fall short when dealing with high sulfur concentrations. This study investigated optimized digestion conditions for accurate sulfur determination in sulfide minerals using ICP-OES. We employed anti-corrosion acid digestion bombs, an aqua regia–hydrofluoric acid system, and a digestion temperature of 180 °C, achieving exceptional results. Certified reference material recoveries ranged from 99.9 to 100.5%, with relative standard deviations between 0.42 and 0.84%. These results demonstrate the high accuracy and precision of the method. The optimized digestion protocol presented in this study provides a robust and reliable approach for accurate sulfur analysis in sulfide minerals, particularly for high concentrations.","PeriodicalId":14967,"journal":{"name":"Journal of Analytical Science and Technology","volume":"8 1","pages":""},"PeriodicalIF":2.4,"publicationDate":"2024-09-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142252713","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-16DOI: 10.1186/s40543-024-00462-0
Stefano Frassati, Elena Barbaro, Claudia Rossetti, Giulio Cozzi, Clara Turetta, Federico Scoto, Marco Roman, Matteo Feltracco, Kitae Kim, Carlo Barbante, Andrea Gambaro, Andrea Spolaor
Iodine and bromine play central roles in polar atmospheric chemistry: iodine influences the atmospheric oxidative capacity and can generate cloud condensation nuclei, while bromine participates in ozone depletion reactions, known as bromine explosions. Here we present a very sensitive analytical method for Br and I speciation by coupling the ion chromatography system (IC) with an inductively coupled plasma sector field mass spectrometer (ICP-SFMS). We achieved sub-picogram-per gram (pg g−1) as limits of detection (LODs) ranging from 0.4 pg g−1 for I−, 0.8 pg g−1 for IO3−, 4 pg g−1 for Br−, and 1 pg g−1 for BrO3−, respectively. These values represent a decrease of up to 30 times compared to the LODs reported in other studies. The method was validated using deep snow samples from the Svalbard Islands, collected at the end of the polar night to quantify various oxidized compounds during their seasonal minimum. In the future, this method could prove useful in the paleoclimatic study of ice cores and snow, as well as in ice chemistry research.
{"title":"Inorganic iodine and bromine speciation in Arctic snow at picogram-per-grams levels by IC-ICP-MS","authors":"Stefano Frassati, Elena Barbaro, Claudia Rossetti, Giulio Cozzi, Clara Turetta, Federico Scoto, Marco Roman, Matteo Feltracco, Kitae Kim, Carlo Barbante, Andrea Gambaro, Andrea Spolaor","doi":"10.1186/s40543-024-00462-0","DOIUrl":"https://doi.org/10.1186/s40543-024-00462-0","url":null,"abstract":"Iodine and bromine play central roles in polar atmospheric chemistry: iodine influences the atmospheric oxidative capacity and can generate cloud condensation nuclei, while bromine participates in ozone depletion reactions, known as bromine explosions. Here we present a very sensitive analytical method for Br and I speciation by coupling the ion chromatography system (IC) with an inductively coupled plasma sector field mass spectrometer (ICP-SFMS). We achieved sub-picogram-per gram (pg g−1) as limits of detection (LODs) ranging from 0.4 pg g−1 for I−, 0.8 pg g−1 for IO3−, 4 pg g−1 for Br−, and 1 pg g−1 for BrO3−, respectively. These values represent a decrease of up to 30 times compared to the LODs reported in other studies. The method was validated using deep snow samples from the Svalbard Islands, collected at the end of the polar night to quantify various oxidized compounds during their seasonal minimum. In the future, this method could prove useful in the paleoclimatic study of ice cores and snow, as well as in ice chemistry research.","PeriodicalId":14967,"journal":{"name":"Journal of Analytical Science and Technology","volume":"20 1","pages":""},"PeriodicalIF":2.4,"publicationDate":"2024-09-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142252712","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-07-08DOI: 10.1186/s40543-024-00455-z
Jangil Moon, Yeongcheol Han, Songyi Kim, Jeonghoon Lee, Soon Do Hur
Accurate measurement of water vapor isotopes (δ18O and δ2H) is fundamental for advancing our understanding of the hydrological cycle and improving hydrological model accuracy. This study introduces an innovative calibration methodology using a controlled evaporation mixer (CEM) for determining stable isotopic ratios in atmospheric water vapor via cavity ring-down spectroscopy. The CEM technique reliably produces a stable water vapor stream, crucial for enhancing the precision and accuracy of isotopic measurements. Its rapid adaptation to changes in water vapor concentration and compatibility with different water standards enhance calibration reliability. Demonstrated reproducibility in generating water vapor across a broad concentration range from 900 to over 25,000 ppmv, coupled with a substantial reduction in memory effects, makes this approach highly effective in both laboratory and field settings. This calibration advancement greatly enhances research capabilities for continuous atmospheric water vapor analysis, providing deeper insights into hydrological processes and atmospheric dynamics.
{"title":"Integrating the controlled evaporation mixer with cavity ring-down spectroscopy for enhanced water vapor isotope calibration","authors":"Jangil Moon, Yeongcheol Han, Songyi Kim, Jeonghoon Lee, Soon Do Hur","doi":"10.1186/s40543-024-00455-z","DOIUrl":"https://doi.org/10.1186/s40543-024-00455-z","url":null,"abstract":"Accurate measurement of water vapor isotopes (δ18O and δ2H) is fundamental for advancing our understanding of the hydrological cycle and improving hydrological model accuracy. This study introduces an innovative calibration methodology using a controlled evaporation mixer (CEM) for determining stable isotopic ratios in atmospheric water vapor via cavity ring-down spectroscopy. The CEM technique reliably produces a stable water vapor stream, crucial for enhancing the precision and accuracy of isotopic measurements. Its rapid adaptation to changes in water vapor concentration and compatibility with different water standards enhance calibration reliability. Demonstrated reproducibility in generating water vapor across a broad concentration range from 900 to over 25,000 ppmv, coupled with a substantial reduction in memory effects, makes this approach highly effective in both laboratory and field settings. This calibration advancement greatly enhances research capabilities for continuous atmospheric water vapor analysis, providing deeper insights into hydrological processes and atmospheric dynamics.","PeriodicalId":14967,"journal":{"name":"Journal of Analytical Science and Technology","volume":"3 1","pages":""},"PeriodicalIF":2.4,"publicationDate":"2024-07-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141569997","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-06-18DOI: 10.1186/s40543-024-00453-1
Hyosuk Yun, Jeong-Eun Seon, Kon-Young Ji, Hye Jung Min, Hyung-Sik Kang, Chul Won Lee
Periostin is a matricellular protein that consists of several structural and functional domains, including EMILIN-like, four internal repeat fasciclin1 (FAS1) domains, and a carboxyl-terminal variable domain. It is known that periostin is associated with various fundamental biological processes and diseases, such as several types of cancer and chronic inflammatory diseases. Despite its important roles, the biological function of each domain is poorly understood. In this study, we expressed the fourth FAS1 (FAS1 IV) domain of human periostin, which was highly soluble and stable enough for structural and functional studies. The three-dimensional structure of FAS1 IV was determined using 3D NMR spectroscopy. The overall structure of FAS1 IV consists of six α-helices, one 310 helix, and eight β-strands. Two triangular α-helical modules formed by three α-helices each are located on one side of the molecule, while the orthogonal β-sheet sandwich module of FAS1 IV is located on the other side. The isolated FAS1 IV domain exhibited cell invasion, migration, and adhesion activities for cancer cell lines comparable to those of the full FAS1 I–IV domain. In conclusion, we propose that the FAS1 IV domain is functionally active in human periostin and provides valuable information for understanding the biological function of periostin.
骨膜蛋白是一种由多个结构域和功能域组成的基质细胞蛋白，包括 EMILIN 样结构域、四个内部重复 fasciclin1（FAS1）结构域和一个羧基末端可变结构域。众所周知，表皮生长因子与多种基本生物过程和疾病（如几种癌症和慢性炎症性疾病）有关。尽管其作用重要，但对每个结构域的生物学功能却知之甚少。在本研究中，我们表达了人骨膜增生蛋白的第四个 FAS1（FAS1 IV）结构域，该结构域可溶性高且足够稳定，可用于结构和功能研究。利用三维核磁共振光谱测定了 FAS1 IV 的三维结构。FAS1 IV的整体结构由六个α螺旋、一个310螺旋和八个β链组成。FAS1 IV 的两个三角形 α 螺旋模块分别由三个 α 螺旋组成，位于分子的一侧，而正交的 β 片状夹层模块则位于分子的另一侧。分离出的 FAS1 IV 结构域在癌细胞株中的细胞侵袭、迁移和粘附活性与完整的 FAS1 I-IV 结构域相当。总之，我们认为 FAS1 IV 结构域在人骨膜增生蛋白中具有功能活性，并为了解骨膜增生蛋白的生物功能提供了有价值的信息。
{"title":"NMR structure and functional studies of the fourth FAS1 domain of human periostin","authors":"Hyosuk Yun, Jeong-Eun Seon, Kon-Young Ji, Hye Jung Min, Hyung-Sik Kang, Chul Won Lee","doi":"10.1186/s40543-024-00453-1","DOIUrl":"https://doi.org/10.1186/s40543-024-00453-1","url":null,"abstract":"Periostin is a matricellular protein that consists of several structural and functional domains, including EMILIN-like, four internal repeat fasciclin1 (FAS1) domains, and a carboxyl-terminal variable domain. It is known that periostin is associated with various fundamental biological processes and diseases, such as several types of cancer and chronic inflammatory diseases. Despite its important roles, the biological function of each domain is poorly understood. In this study, we expressed the fourth FAS1 (FAS1 IV) domain of human periostin, which was highly soluble and stable enough for structural and functional studies. The three-dimensional structure of FAS1 IV was determined using 3D NMR spectroscopy. The overall structure of FAS1 IV consists of six α-helices, one 310 helix, and eight β-strands. Two triangular α-helical modules formed by three α-helices each are located on one side of the molecule, while the orthogonal β-sheet sandwich module of FAS1 IV is located on the other side. The isolated FAS1 IV domain exhibited cell invasion, migration, and adhesion activities for cancer cell lines comparable to those of the full FAS1 I–IV domain. In conclusion, we propose that the FAS1 IV domain is functionally active in human periostin and provides valuable information for understanding the biological function of periostin.","PeriodicalId":14967,"journal":{"name":"Journal of Analytical Science and Technology","volume":"25 1","pages":""},"PeriodicalIF":2.4,"publicationDate":"2024-06-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141529293","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-06-04DOI: 10.1186/s40543-024-00445-1
Hayeon Lee, Yeseul Lee, Jinseok Lee, Hyeongseop Jeong, Dong Keon Yon, Clarissa L. Durie, Bumhan Ryu, Jeong Min Chung
The selection of defocus ranges for small datasets in cryo-electron microscopy (cryo-EM) is under-researched. We present a comprehensive benchmark experiment that aimed to evaluate the relationship between contrast, defocus, and resolution, particularly in the context of limited datasets. We conducted a detailed analysis of beta-galactosidase, apo-ferritin, and connexin-46/50 datasets to optimize pre-screening strategies for cryo-EM. Our approach involved classifying micrographs based on image contrast using an artificial intelligence (AI) model without considering the defocus level. This method allowed us to investigate the optimal defocus range for pre-screening in a limited dataset and its impact on the overall image processing. The micrographs were categorized into good, moderate, and bad contrast groups. Subsequent analysis revealed that, contrary to the prevailing assumption that lower contrast (associated with lower defocus) leads to higher resolution, in scenarios with limited datasets higher contrast images yield superior resolution. This finding was consistent across all three protein samples, underscoring the critical role of contrast in determining the quality of 3D reconstructions in limited datasets. This significant finding challenges conventional cryo-EM methodologies. In conclusion, our study provides new benchmarks for selecting appropriate contrast and defocus levels in cryo-EM, particularly for screening approaches that use limited datasets. This strategy promises to enhance the data quality and efficiency in structural biology research, particularly in resource-constrained scenarios.
{"title":"Assessing the interplay of contrast, defocus, and resolution in cryo-EM: a benchmark experiment for limited dataset screening","authors":"Hayeon Lee, Yeseul Lee, Jinseok Lee, Hyeongseop Jeong, Dong Keon Yon, Clarissa L. Durie, Bumhan Ryu, Jeong Min Chung","doi":"10.1186/s40543-024-00445-1","DOIUrl":"https://doi.org/10.1186/s40543-024-00445-1","url":null,"abstract":"The selection of defocus ranges for small datasets in cryo-electron microscopy (cryo-EM) is under-researched. We present a comprehensive benchmark experiment that aimed to evaluate the relationship between contrast, defocus, and resolution, particularly in the context of limited datasets. We conducted a detailed analysis of beta-galactosidase, apo-ferritin, and connexin-46/50 datasets to optimize pre-screening strategies for cryo-EM. Our approach involved classifying micrographs based on image contrast using an artificial intelligence (AI) model without considering the defocus level. This method allowed us to investigate the optimal defocus range for pre-screening in a limited dataset and its impact on the overall image processing. The micrographs were categorized into good, moderate, and bad contrast groups. Subsequent analysis revealed that, contrary to the prevailing assumption that lower contrast (associated with lower defocus) leads to higher resolution, in scenarios with limited datasets higher contrast images yield superior resolution. This finding was consistent across all three protein samples, underscoring the critical role of contrast in determining the quality of 3D reconstructions in limited datasets. This significant finding challenges conventional cryo-EM methodologies. In conclusion, our study provides new benchmarks for selecting appropriate contrast and defocus levels in cryo-EM, particularly for screening approaches that use limited datasets. This strategy promises to enhance the data quality and efficiency in structural biology research, particularly in resource-constrained scenarios.","PeriodicalId":14967,"journal":{"name":"Journal of Analytical Science and Technology","volume":"70 1","pages":""},"PeriodicalIF":2.4,"publicationDate":"2024-06-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141259926","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-06-04DOI: 10.1186/s40543-024-00448-y
Won-Seok Kang, Sung-Wook Choi, Hyo-Sop Kim, Jae-Ho Kim, Jae-Hyeok Lee
Raman spectroscopy is used to investigate the absorption and dispersion of zearalenone (ZEN) and its derivatives. The C=C stretching vibration modes of ZEN and zearalenol (ZENOL) were appeared at 975–990 cm−1. The C=O vibration mode was present at 1680–1690 cm−1 for ZEN and zearalanone (ZAN), but it was absent for ZENOL and zearalanol (ZANOL) which have –OH group instead of –C=O group in ZEN and ZAN molecular structures. On the basis of this characterization, Raman spectra of specific chemical groups and linkages corresponding to the structural difference of ZEN and its derivatives were identified. These results indicated that Raman spectroscopy can apply for the identification of ZEN and its derivatives and has a potential for the non-destructive rapid detection of these compounds in food.
拉曼光谱用于研究玉米赤霉烯酮（ZEN）及其衍生物的吸收和分散。玉米赤霉烯酮（ZEN）和玉米赤霉烯醇（ZENOL）的 C=C 伸展振动模式出现在 975-990 cm-1 处。ZEN 和玉米赤霉烯酮（ZAN）的 C=O 振动模式出现在 1680-1690 cm-1 处，而 ZENOL 和玉米赤霉醇（ZANOL）则没有，因为 ZEN 和 ZAN 分子结构中的 -C=O 基团是 -OH 基团。在此基础上，确定了与 ZEN 及其衍生物结构差异相对应的特定化学基团和连接的拉曼光谱。这些结果表明，拉曼光谱可用于鉴别 ZEN 及其衍生物，并具有非破坏性地快速检测食品中这些化合物的潜力。
{"title":"Raman spectroscopic comparison of zearalenone and its derivatives for non-destructive rapid detection","authors":"Won-Seok Kang, Sung-Wook Choi, Hyo-Sop Kim, Jae-Ho Kim, Jae-Hyeok Lee","doi":"10.1186/s40543-024-00448-y","DOIUrl":"https://doi.org/10.1186/s40543-024-00448-y","url":null,"abstract":"Raman spectroscopy is used to investigate the absorption and dispersion of zearalenone (ZEN) and its derivatives. The C=C stretching vibration modes of ZEN and zearalenol (ZENOL) were appeared at 975–990 cm−1. The C=O vibration mode was present at 1680–1690 cm−1 for ZEN and zearalanone (ZAN), but it was absent for ZENOL and zearalanol (ZANOL) which have –OH group instead of –C=O group in ZEN and ZAN molecular structures. On the basis of this characterization, Raman spectra of specific chemical groups and linkages corresponding to the structural difference of ZEN and its derivatives were identified. These results indicated that Raman spectroscopy can apply for the identification of ZEN and its derivatives and has a potential for the non-destructive rapid detection of these compounds in food.","PeriodicalId":14967,"journal":{"name":"Journal of Analytical Science and Technology","volume":"14 1","pages":""},"PeriodicalIF":2.4,"publicationDate":"2024-06-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141254524","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-06-04DOI: 10.1186/s40543-024-00446-0
Sheriff A. Balogun, Tesleem O. Abolarinwa, Funmilola A. Adesanya, Collins N. Ateba, Omolola E. Fayemi
This study aimed to compare the spectroscopy, morphological, electrocatalytic properties, and antibacterial activities of cobalt nanoparticles (CoNPs) with nickel nanoparticles (NiNPs). Cobalt nanoparticles and NiNPs were prepared via a chemical reduction approach and characterized utilizing transmission electron microscopy (TEM), energy-dispersive X-ray (EDX), and X-ray diffraction (XRD) techniques. The result from XRD and TEM analysis revealed that the synthesized nanoparticles exhibit face-centered cubic with smooth spherical shape, having average particles size of 12 nm (NiNPs) and 18 nm (CoNPs). The electrochemical properties of the nanoparticles were examined via cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) techniques. The CV results showed that GCE-Ni (35.6 μA) has a higher current response compared to GCE-Co (10.5 μA). The EIS analysis revealed that GCE-Ni (1.39 KΩ) has faster electron transport capability compared to GCE-Co (2.99 KΩ) as indicated in their Rct values. The power density of the synthesized nanoparticles was obtained from their "knee" frequency (f°) values, with GCE-Ni (3.16 Hz) having higher f° values compared to GCE-Co (2.00 Hz). The antibacterial activity of the nanoparticles was evaluated against multidrug-resistant Escherichia coli O157, Escherichia coli O177, Salmonella enterica, Staphylococcus aureus, and Vibrio cholerae. The result from the antibacterial study revealed that at low concentrations both CoNPs and NiNPs have significant antibacterial activities against E. coli O157, E. coli O177, S. enterica, S. aureus, and V. cholerae. NiNPs showed better antibacterial activities at low concentrations of 61.5, 61.5, 125, 61.5, and 125 µg/mL compared to CoNPs with minimum inhibitory concentrations of 125, 125, 250, 61.5, and 125 µg/mL against E. coli O157, E. coli O177, S. enterica, S. aureus, and V. cholerae, respectively. These promising antibacterial activities emphasize the potential of CoNPs and NiNPs as effective antibacterial agents, which could aid in the development of novel antibacterial medicines.
{"title":"Spectroscopic and antibacterial activities of cobalt and nickel nanoparticles: a comparative analysis","authors":"Sheriff A. Balogun, Tesleem O. Abolarinwa, Funmilola A. Adesanya, Collins N. Ateba, Omolola E. Fayemi","doi":"10.1186/s40543-024-00446-0","DOIUrl":"https://doi.org/10.1186/s40543-024-00446-0","url":null,"abstract":"This study aimed to compare the spectroscopy, morphological, electrocatalytic properties, and antibacterial activities of cobalt nanoparticles (CoNPs) with nickel nanoparticles (NiNPs). Cobalt nanoparticles and NiNPs were prepared via a chemical reduction approach and characterized utilizing transmission electron microscopy (TEM), energy-dispersive X-ray (EDX), and X-ray diffraction (XRD) techniques. The result from XRD and TEM analysis revealed that the synthesized nanoparticles exhibit face-centered cubic with smooth spherical shape, having average particles size of 12 nm (NiNPs) and 18 nm (CoNPs). The electrochemical properties of the nanoparticles were examined via cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) techniques. The CV results showed that GCE-Ni (35.6 μA) has a higher current response compared to GCE-Co (10.5 μA). The EIS analysis revealed that GCE-Ni (1.39 KΩ) has faster electron transport capability compared to GCE-Co (2.99 KΩ) as indicated in their Rct values. The power density of the synthesized nanoparticles was obtained from their \"knee\" frequency (f°) values, with GCE-Ni (3.16 Hz) having higher f° values compared to GCE-Co (2.00 Hz). The antibacterial activity of the nanoparticles was evaluated against multidrug-resistant Escherichia coli O157, Escherichia coli O177, Salmonella enterica, Staphylococcus aureus, and Vibrio cholerae. The result from the antibacterial study revealed that at low concentrations both CoNPs and NiNPs have significant antibacterial activities against E. coli O157, E. coli O177, S. enterica, S. aureus, and V. cholerae. NiNPs showed better antibacterial activities at low concentrations of 61.5, 61.5, 125, 61.5, and 125 µg/mL compared to CoNPs with minimum inhibitory concentrations of 125, 125, 250, 61.5, and 125 µg/mL against E. coli O157, E. coli O177, S. enterica, S. aureus, and V. cholerae, respectively. These promising antibacterial activities emphasize the potential of CoNPs and NiNPs as effective antibacterial agents, which could aid in the development of novel antibacterial medicines.","PeriodicalId":14967,"journal":{"name":"Journal of Analytical Science and Technology","volume":"76 1","pages":""},"PeriodicalIF":2.4,"publicationDate":"2024-06-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141259813","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-05-07DOI: 10.1186/s40543-024-00440-6
K. Terada, K. Ninomiya, A. Sato, D. Tomono, Y. Kawashima, M. Inagaki, A. Nambu, T. Kudo, T. Osawa, M. K. Kubo
In Earth and planetary science, Pb isotopic composition is well known to play a key role in deciphering the origin and evolution of materials because they provide unique chronological and/or indigenous regional information as a radiogenic daughter nuclide from U and Th. To determine such an isotopic composition, mass spectrometers have been widely used over several decades, which requires a destructive/consuming treatment such as sputtering, laser ablation and thermal ionization. Here, we first report the non-destructive Pb isotopic measurement of natural galena (PbS) using the energy shift of muon-induced characteristic X-rays. The observed Pb isotopic composition of the natural galena is in good agreement with that obtained by conventional mass spectrometry. Such a muon-based Pb isotopic analysis method is expected to be applied to identify the production area of archaeological artefacts (e.g. bronze products), where non-destructive analysis is highly desirable compared to conventional mass spectrometry.
在地球和行星科学中，众所周知，铅同位素组成在破译物质的起源和演化方面起着关键作用，因为它们作为铀和钍的放射性子核素，提供了独特的年代学和/或本地区域信息。为了测定这种同位素组成，几十年来质谱仪得到了广泛应用，但这需要进行破坏性/消耗性处理，如溅射、激光烧蚀和热电离。在此，我们首次报告了利用μ介子诱导特征 X 射线的能量位移对天然方铅矿（PbS）进行非破坏性铅同位素测量的结果。所观测到的天然方铅矿的铅同位素组成与传统质谱法所获得的结果十分吻合。这种基于μ介子的铅同位素分析方法有望应用于确定考古文物（如青铜制品）的产地，与传统质谱法相比，非破坏性分析是非常理想的。
{"title":"Development of non-destructive isotope measurement of the natural galena (PbS) using negative muon beams","authors":"K. Terada, K. Ninomiya, A. Sato, D. Tomono, Y. Kawashima, M. Inagaki, A. Nambu, T. Kudo, T. Osawa, M. K. Kubo","doi":"10.1186/s40543-024-00440-6","DOIUrl":"https://doi.org/10.1186/s40543-024-00440-6","url":null,"abstract":"In Earth and planetary science, Pb isotopic composition is well known to play a key role in deciphering the origin and evolution of materials because they provide unique chronological and/or indigenous regional information as a radiogenic daughter nuclide from U and Th. To determine such an isotopic composition, mass spectrometers have been widely used over several decades, which requires a destructive/consuming treatment such as sputtering, laser ablation and thermal ionization. Here, we first report the non-destructive Pb isotopic measurement of natural galena (PbS) using the energy shift of muon-induced characteristic X-rays. The observed Pb isotopic composition of the natural galena is in good agreement with that obtained by conventional mass spectrometry. Such a muon-based Pb isotopic analysis method is expected to be applied to identify the production area of archaeological artefacts (e.g. bronze products), where non-destructive analysis is highly desirable compared to conventional mass spectrometry.","PeriodicalId":14967,"journal":{"name":"Journal of Analytical Science and Technology","volume":"29 1","pages":""},"PeriodicalIF":2.4,"publicationDate":"2024-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140884913","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-05-07DOI: 10.1186/s40543-024-00442-4
Filipe M. J. Figueiredo, José M. Carretas, João P. Leal, José M. Sardinha
The measurement of metals in solution is usually performed using inductive coupled plasma hyphenated techniques or atomic absorption. Although very sensitive and accurate, these analytical techniques are quite expensive and do not allow field measurements. The present work takes advantage of energy-dispersive X-ray fluorescence (ED-XRF) ease-of-use features to determine the concentration of rare earth elements (Y, Pr, Nd, Eu) and others (S, Fe, Ni, Cu, Zn) in aqueous solutions, after appropriate sample treatment. The approach turned out to be a reliable and very convenient procedure for field analysis. The simplicity, speed and reliability of the methodology used combined with the possibility of simultaneous analysis and low cost of the method can be advantageous in industrial context. The approach relies on the suspension of the target solutions in a cellulose matrix that is further converted into a pellet for direct analysis. Calibration curves obtained by regression analysis at 5% significance are shown for a variety of elements (S, Fe, Ni, Cu, Zn, Y, Pr, Nd, Eu) with correlation coefficients between 0.9555 and 0.9980. Higher coefficients of variance were obtained for the calibration of S and Pr due to low sensitivity and the overlapping with the L lines of Nd, respectively. The performed calibrations were not affected by the presence of other analytes in the matrix. Results obtained showed that it is possible to use the proposed methodology to accurately quantify d and f block metals in aqueous solutions by ED-XRF after sequestering the chemical content into a cellulose powder matrix and further processing into a pellet.
溶液中金属的测量通常采用电感耦合等离子体联用技术或原子吸收技术。虽然这些分析技术非常灵敏准确，但价格昂贵，而且无法进行实地测量。本研究利用能量色散 X 射线荧光（ED-XRF）易于使用的特点，在对样品进行适当处理后，测定水溶液中稀土元素（Y、Pr、Nd、Eu）和其他元素（S、Fe、Ni、Cu、Zn）的浓度。事实证明，该方法是一种可靠且非常方便的现场分析程序。该方法简单、快速、可靠，可同时进行分析，而且成本低廉，在工业领域具有优势。这种方法是将目标溶液悬浮在纤维素基质中，然后再将其转化为颗粒，直接进行分析。在 5%的显著性下，通过回归分析获得的校准曲线显示了多种元素（S、Fe、Ni、Cu、Zn、Y、Pr、Nd、Eu）的相关系数在 0.9555 和 0.9980 之间。由于 S 和 Pr 的灵敏度较低，且与 Nd 的 L 线重叠，因此校准 S 和 Pr 的方差系数较高。所进行的定标不受基质中存在其他分析物的影响。结果表明，在将化学成分封存到纤维素粉末基质中并进一步加工成颗粒后，可以使用所提出的方法通过电离-XRF 对水溶液中的 d 和 f 块状金属进行精确定量。
{"title":"Fast, accessible and reliable method for elemental analysis of metals in solution by ED-XRF spectroscopy","authors":"Filipe M. J. Figueiredo, José M. Carretas, João P. Leal, José M. Sardinha","doi":"10.1186/s40543-024-00442-4","DOIUrl":"https://doi.org/10.1186/s40543-024-00442-4","url":null,"abstract":"The measurement of metals in solution is usually performed using inductive coupled plasma hyphenated techniques or atomic absorption. Although very sensitive and accurate, these analytical techniques are quite expensive and do not allow field measurements. The present work takes advantage of energy-dispersive X-ray fluorescence (ED-XRF) ease-of-use features to determine the concentration of rare earth elements (Y, Pr, Nd, Eu) and others (S, Fe, Ni, Cu, Zn) in aqueous solutions, after appropriate sample treatment. The approach turned out to be a reliable and very convenient procedure for field analysis. The simplicity, speed and reliability of the methodology used combined with the possibility of simultaneous analysis and low cost of the method can be advantageous in industrial context. The approach relies on the suspension of the target solutions in a cellulose matrix that is further converted into a pellet for direct analysis. Calibration curves obtained by regression analysis at 5% significance are shown for a variety of elements (S, Fe, Ni, Cu, Zn, Y, Pr, Nd, Eu) with correlation coefficients between 0.9555 and 0.9980. Higher coefficients of variance were obtained for the calibration of S and Pr due to low sensitivity and the overlapping with the L lines of Nd, respectively. The performed calibrations were not affected by the presence of other analytes in the matrix. Results obtained showed that it is possible to use the proposed methodology to accurately quantify d and f block metals in aqueous solutions by ED-XRF after sequestering the chemical content into a cellulose powder matrix and further processing into a pellet. ","PeriodicalId":14967,"journal":{"name":"Journal of Analytical Science and Technology","volume":"63 1","pages":""},"PeriodicalIF":2.4,"publicationDate":"2024-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140889618","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-05-01DOI: 10.1186/s40543-024-00439-z
Keewook Yi, Yuri Amelin
We report developing a procedure for measuring concentrations of U, Th and Pb (including all natural Pb isotopes) to establish the distribution of these elements in meteorite minerals and correctly interpret Pb-isotopic ages of meteorites. The concentrations were measured on KBSI SHRIMP IIe by peak jumping using a discrete-dynode secondary electron multiplier. The concentrations were calculated relative to BCR-2G glass and monitored by analysis of the NIST glasses SRM-615 and SRM-617 as secondary reference materials. The detection limits using the spot sizes of ca. 180 μm2, primary O2− beam current of 10.6 nA, and with amplifier dark noise of 0.015 counts per second are ~ 0.2 parts per billion (ppb) for U (500 s integration), ~ 0.6 ppb for Pb (100 s integration for each of the major isotopes), and ~ 1.2 ppb for Th (100 s integration). Analyses of the NIST glasses confirm that the measured concentrations of U and Th are consistent with their certified values, while the Pb concentrations are about four times too low, most likely due to the compositional mismatch between the primary and secondary reference materials. The achieved level of sensitivity and concentration precision (~ 20–30%) is adequate for measuring U, Th and Pb distributions in both rock-forming and accessory minerals in chondrites, achondrites, and their components.
{"title":"SIMS study of fine-scale distribution of U, Th and Pb in meteorites","authors":"Keewook Yi, Yuri Amelin","doi":"10.1186/s40543-024-00439-z","DOIUrl":"https://doi.org/10.1186/s40543-024-00439-z","url":null,"abstract":"We report developing a procedure for measuring concentrations of U, Th and Pb (including all natural Pb isotopes) to establish the distribution of these elements in meteorite minerals and correctly interpret Pb-isotopic ages of meteorites. The concentrations were measured on KBSI SHRIMP IIe by peak jumping using a discrete-dynode secondary electron multiplier. The concentrations were calculated relative to BCR-2G glass and monitored by analysis of the NIST glasses SRM-615 and SRM-617 as secondary reference materials. The detection limits using the spot sizes of ca. 180 μm2, primary O2− beam current of 10.6 nA, and with amplifier dark noise of 0.015 counts per second are ~ 0.2 parts per billion (ppb) for U (500 s integration), ~ 0.6 ppb for Pb (100 s integration for each of the major isotopes), and ~ 1.2 ppb for Th (100 s integration). Analyses of the NIST glasses confirm that the measured concentrations of U and Th are consistent with their certified values, while the Pb concentrations are about four times too low, most likely due to the compositional mismatch between the primary and secondary reference materials. The achieved level of sensitivity and concentration precision (~ 20–30%) is adequate for measuring U, Th and Pb distributions in both rock-forming and accessory minerals in chondrites, achondrites, and their components.","PeriodicalId":14967,"journal":{"name":"Journal of Analytical Science and Technology","volume":"43 1","pages":""},"PeriodicalIF":2.4,"publicationDate":"2024-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140832088","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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