: In this study, a laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) method is developed for in -situ quantitative imaging of trace impurity elements in Bi 4 Si 3 O 12 (BSO) crystals. This method has unique advantages of low detection limit and high spatial resolution for the analysis of defects in crystal microregions. The regression coefficients of the calibration curves for each element were greater than 0.99, and the detection limits (DLs) were 17, 5, 7, 48, 5, 7, 16, 27, and 7 ng/g for 24 Mg, 45 Sc, 48 Ti, 90 Zr, 139 La, 146 Nd, 172 Yb and 208 Pb, respectively. The LA-ICP-MS measurements were in good agreement with the results obtained using conventional ICP-MS method. Segregation phenomena of elemental impurities in the axial direction of the BSO crystal can exist during crystal growth. Finally, the distribution of the impurity elements in the dendritic crystal defect region of the crystal was visualized. We believe that this work proposes a novel less-invasive analysis method for exploring the composition-defect relationship of crystals.
{"title":"Elemental Quantitative Imaging Analysis Of Bi4Si3O12 Crystals Defects By LA-ICP-MS","authors":"Zheng Wang","doi":"10.46770/as.2023.080","DOIUrl":"https://doi.org/10.46770/as.2023.080","url":null,"abstract":": In this study, a laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) method is developed for in -situ quantitative imaging of trace impurity elements in Bi 4 Si 3 O 12 (BSO) crystals. This method has unique advantages of low detection limit and high spatial resolution for the analysis of defects in crystal microregions. The regression coefficients of the calibration curves for each element were greater than 0.99, and the detection limits (DLs) were 17, 5, 7, 48, 5, 7, 16, 27, and 7 ng/g for 24 Mg, 45 Sc, 48 Ti, 90 Zr, 139 La, 146 Nd, 172 Yb and 208 Pb, respectively. The LA-ICP-MS measurements were in good agreement with the results obtained using conventional ICP-MS method. Segregation phenomena of elemental impurities in the axial direction of the BSO crystal can exist during crystal growth. Finally, the distribution of the impurity elements in the dendritic crystal defect region of the crystal was visualized. We believe that this work proposes a novel less-invasive analysis method for exploring the composition-defect relationship of crystals.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":" ","pages":""},"PeriodicalIF":3.4,"publicationDate":"2023-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44348461","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":"Effect Of Sample Injection Volume On Non-Spectroscopic And Spectroscopic Interferences In Inductively Coupled Plasma Mass Spectrometry","authors":"D. Beauchemin","doi":"10.46770/as.2023.013","DOIUrl":"https://doi.org/10.46770/as.2023.013","url":null,"abstract":"","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":"69 1","pages":""},"PeriodicalIF":3.4,"publicationDate":"2023-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41275226","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":"Preparation Of Five Selenium-Rich Soil Reference Materials, Their Se, Cr, Ni, Zn, Cd, Pb Mass Fraction Certifications And A Study Of Se Geochemical Fractionation","authors":"Zhenan Bao, H. Tian","doi":"10.46770/as.2023.017","DOIUrl":"https://doi.org/10.46770/as.2023.017","url":null,"abstract":"","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":" ","pages":""},"PeriodicalIF":3.4,"publicationDate":"2023-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46434569","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}
: Segregation defects cannot be eliminated from nickel-based superalloy prepared by smelting. Thus, studying the element-content distribution and segregation degree is helpful to guide process improvement and quality control. In this study, the cross section of a cylindrical electro-slag remelting ingot of a wrought superalloy with a diameter of 485 mm was analyzed by micro-beam X-ray fluorescence spectrometry, and continuous point-by-point mode was used to obtain high stability and accuracy. The element-content distribution and quantitative degree of segregation from the edge to the center of the ingot were characterized. The maximum positive segregation, maximum negative segregation, statistic segregation degree, and statistic conformity degree were calculated for each element to quantitatively characterize the degree of segregation from different points of view, and they showed the same trend as the element-content distribution. The results of metallography and scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS) showed that there were differences in the dendritic microstructures and precipitated phases in the interdendrites and dendritic arms from the edge to the center of the ingot, which explain the element-content distribution largely.
{"title":"Characterization Of The Element Distribution And Quantitative Segregation Degree Of Nickel-Based Superalloy Ingot","authors":"Hui Wang","doi":"10.46770/as.2022.235","DOIUrl":"https://doi.org/10.46770/as.2022.235","url":null,"abstract":": Segregation defects cannot be eliminated from nickel-based superalloy prepared by smelting. Thus, studying the element-content distribution and segregation degree is helpful to guide process improvement and quality control. In this study, the cross section of a cylindrical electro-slag remelting ingot of a wrought superalloy with a diameter of 485 mm was analyzed by micro-beam X-ray fluorescence spectrometry, and continuous point-by-point mode was used to obtain high stability and accuracy. The element-content distribution and quantitative degree of segregation from the edge to the center of the ingot were characterized. The maximum positive segregation, maximum negative segregation, statistic segregation degree, and statistic conformity degree were calculated for each element to quantitatively characterize the degree of segregation from different points of view, and they showed the same trend as the element-content distribution. The results of metallography and scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS) showed that there were differences in the dendritic microstructures and precipitated phases in the interdendrites and dendritic arms from the edge to the center of the ingot, which explain the element-content distribution largely.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":" ","pages":""},"PeriodicalIF":3.4,"publicationDate":"2022-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43906799","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}
A new online advanced oxidation process with high efficiency was proposed for the degradation of organic mercury. The oxidation process is based on a high-efficiency photooxidation reactor in which the reaction tube was passed through a low-pressure mercury lamp. The reactor provided efficient irradiation which resulted in the complete degradation of methylmercury and ethylmercury within 4 s and 6 s, respectively. The highlight of this method is the removal of oxidants and high temperature. The oxidation process is extremely high efficiency and therefore is easy to be coupled with flow injection (FI) and high-performance liquid chromatography (HPLC). In FI system, complete oxidations of organic mercury can be accomplished in the plain medium of 0.5% (v/v) HCl, 1% (v/v) HNO3 and H2O, therefore, simple Hg aqueous standard calibration curves can be used to calibrate both inorganic and organic mercury. The detection limits of Hg, CH3Hg and CH3CH2Hg were found to be 0.02 ng mL. In HPLC system, the detection limits were calculated to be 0.55, 0.84, 0.56 ng ml for Hg, CH3Hg and CH3CH2Hg, respectively. In addition, the method provided good repeatability (< 5% RSD) for both systems. The developed method was validated by determination of certified reference material (GBW 10029, tuna fish) and was further applied in speciation of mercury in spiked environmental waters and biological samples.
{"title":"UV Induced Advanced Oxidation Process For The Degradation Of Organic Mercury And Its Application To Mercury Speciation By Atomic Fluorescence Spectrometry","authors":"Zhifu Liu","doi":"10.46770/as.2022.228","DOIUrl":"https://doi.org/10.46770/as.2022.228","url":null,"abstract":"A new online advanced oxidation process with high efficiency was proposed for the degradation of organic mercury. The oxidation process is based on a high-efficiency photooxidation reactor in which the reaction tube was passed through a low-pressure mercury lamp. The reactor provided efficient irradiation which resulted in the complete degradation of methylmercury and ethylmercury within 4 s and 6 s, respectively. The highlight of this method is the removal of oxidants and high temperature. The oxidation process is extremely high efficiency and therefore is easy to be coupled with flow injection (FI) and high-performance liquid chromatography (HPLC). In FI system, complete oxidations of organic mercury can be accomplished in the plain medium of 0.5% (v/v) HCl, 1% (v/v) HNO3 and H2O, therefore, simple Hg aqueous standard calibration curves can be used to calibrate both inorganic and organic mercury. The detection limits of Hg, CH3Hg and CH3CH2Hg were found to be 0.02 ng mL. In HPLC system, the detection limits were calculated to be 0.55, 0.84, 0.56 ng ml for Hg, CH3Hg and CH3CH2Hg, respectively. In addition, the method provided good repeatability (< 5% RSD) for both systems. The developed method was validated by determination of certified reference material (GBW 10029, tuna fish) and was further applied in speciation of mercury in spiked environmental waters and biological samples.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":" ","pages":""},"PeriodicalIF":3.4,"publicationDate":"2022-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49267857","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":"Imaging Of Ce In Cucumber Leaves By Cryogenic Laser Ablation Inductively Coupled Plasma Mass Spectrometry","authors":"Mingli Chen, Jianhua Wang","doi":"10.46770/as.2022.234","DOIUrl":"https://doi.org/10.46770/as.2022.234","url":null,"abstract":",","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":" ","pages":""},"PeriodicalIF":3.4,"publicationDate":"2022-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44906990","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}
: Mothballs are widely used in daily life as an air freshener, but their main components are volatile organic compounds that are harmful to the human body. A system combining laser-induced breakdown spectroscopy (LIBS) with Raman spectroscopy was built for the detection and recognition of volatile substances in mothballs in indoor environments. LIBS is employed for the online in-situ detection of volatile substances in two kinds of mothballs and to find their characteristic spectral lines. A machine learning model is then established to analyze the spectra of air and volatile substance in synthetic mothballs and natural camphor. The model based on principal component analysis and support vector classification achieved a recognition accuracy of 98.33%, indicating that LIBS has significant potential for recognizing volatile substances in mothballs when airborne. By comparing the experimental Raman spectra of mothballs and theoretical Raman spectra of their main components, the spectral fingerprints of mothballs are obtained as a supplement to LIBS detection.
{"title":"Detection And Recognition Of Volatile Substances In Mothballs Using Laser-Induced Breakdown Spectroscopy And Raman Spectroscopy","authors":"Yuzhu Liu","doi":"10.46770/as.2022.231","DOIUrl":"https://doi.org/10.46770/as.2022.231","url":null,"abstract":": Mothballs are widely used in daily life as an air freshener, but their main components are volatile organic compounds that are harmful to the human body. A system combining laser-induced breakdown spectroscopy (LIBS) with Raman spectroscopy was built for the detection and recognition of volatile substances in mothballs in indoor environments. LIBS is employed for the online in-situ detection of volatile substances in two kinds of mothballs and to find their characteristic spectral lines. A machine learning model is then established to analyze the spectra of air and volatile substance in synthetic mothballs and natural camphor. The model based on principal component analysis and support vector classification achieved a recognition accuracy of 98.33%, indicating that LIBS has significant potential for recognizing volatile substances in mothballs when airborne. By comparing the experimental Raman spectra of mothballs and theoretical Raman spectra of their main components, the spectral fingerprints of mothballs are obtained as a supplement to LIBS detection.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":" ","pages":""},"PeriodicalIF":3.4,"publicationDate":"2022-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45622651","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}
: This study presents a method for the ultra-trace determination of several noble metals (Pd, Pt, Au, and Ag) in geological samples through selective preconcentration using a ferrofluid. Specifically, Fe 3 O 4 magnetic nanoparticles (MNPs) coated with silica and titania and functionalized with 3-mercaptopropyltrimethoxysilane and N-(2-aminoethyl)-3-aminopropyltrimethoxysilane were employed for the selective sorption of analytes. After injecting the ferrofluid into an aqueous sample, the functionalized MNPs adsorbed the target analytes within 5 min. The analyte-carrying MNPs were then separated using an external magnet, followed by elution using 10% v/v aqua regia + 3% thiourea. The eluate was analyzed using inductively coupled plasma mass spectrometry. The effects of sample solution pH, eluent composition, elution time, and elution volume on the preconcentration factor were investigated. Under optimized conditions, the detection limits were improved by factors of 8 to 15 for Pt, Pd, Au, and Ag, compared to those obtained without preconcentration. The accuracy of this method was verified by analyzing a certified reference material (CDN-PGMS-29) of ore containing noble metals, and the measured concentrations were consistent with the certified values based on a Student’s t-test at the 95% confidence level.
{"title":"Ferrofluid-Based Preconcentration And Ultra-Trace Determination Of Pt, Pd, Au, And Ag In Complex Matrices Using Inductively Coupled Plasma Mass Spectrometry","authors":"D. Beauchemin","doi":"10.46770/as.2022.229","DOIUrl":"https://doi.org/10.46770/as.2022.229","url":null,"abstract":": This study presents a method for the ultra-trace determination of several noble metals (Pd, Pt, Au, and Ag) in geological samples through selective preconcentration using a ferrofluid. Specifically, Fe 3 O 4 magnetic nanoparticles (MNPs) coated with silica and titania and functionalized with 3-mercaptopropyltrimethoxysilane and N-(2-aminoethyl)-3-aminopropyltrimethoxysilane were employed for the selective sorption of analytes. After injecting the ferrofluid into an aqueous sample, the functionalized MNPs adsorbed the target analytes within 5 min. The analyte-carrying MNPs were then separated using an external magnet, followed by elution using 10% v/v aqua regia + 3% thiourea. The eluate was analyzed using inductively coupled plasma mass spectrometry. The effects of sample solution pH, eluent composition, elution time, and elution volume on the preconcentration factor were investigated. Under optimized conditions, the detection limits were improved by factors of 8 to 15 for Pt, Pd, Au, and Ag, compared to those obtained without preconcentration. The accuracy of this method was verified by analyzing a certified reference material (CDN-PGMS-29) of ore containing noble metals, and the measured concentrations were consistent with the certified values based on a Student’s t-test at the 95% confidence level.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":" ","pages":""},"PeriodicalIF":3.4,"publicationDate":"2022-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47315691","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}
This work involves heating the entire commercially available sample introduction system on a Varian 820MS instrument with off-the-shelf infrared heaters. This heating improves sensitivities by a factor of 2 to 16 times, with high mass elements receiving the greatest improvement. It also improves detection limits by a factor of 1.1 to 3.5 times for most analytes. At the price of doubled oxide formation, the formation of doubly charged species was decreased by a factor of 3. The Be/Li signal ratio, an indicator of plasma robustness, increased from 0.174 to 0.235 with infrared heating. The infrared-heated system enabled the accurate analysis of a drinking water standard reference material (SRM) (for Be, Mg, Al, Cr, Mn, Co, Cu, Zn and As) and of a waste water SRM (for Be, Mg, Cr, Mn, Co, Cu, Zn, Cd, and Pb) by simple external calibration.
{"title":"An Infrared-Heated Sample Introduction System For Inductively Coupled Plasma Mass Spectrometry","authors":"D. Beauchemin","doi":"10.46770/as.2022.233","DOIUrl":"https://doi.org/10.46770/as.2022.233","url":null,"abstract":"This work involves heating the entire commercially available sample introduction system on a Varian 820MS instrument with off-the-shelf infrared heaters. This heating improves sensitivities by a factor of 2 to 16 times, with high mass elements receiving the greatest improvement. It also improves detection limits by a factor of 1.1 to 3.5 times for most analytes. At the price of doubled oxide formation, the formation of doubly charged species was decreased by a factor of 3. The Be/Li signal ratio, an indicator of plasma robustness, increased from 0.174 to 0.235 with infrared heating. The infrared-heated system enabled the accurate analysis of a drinking water standard reference material (SRM) (for Be, Mg, Al, Cr, Mn, Co, Cu, Zn and As) and of a waste water SRM (for Be, Mg, Cr, Mn, Co, Cu, Zn, Cd, and Pb) by simple external calibration.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":" ","pages":""},"PeriodicalIF":3.4,"publicationDate":"2022-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43241364","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}
In geochronology, the isotope dilution (ID) method has been developed as an analytical method that provides accurate and precise element concentration and isotope ratio. For the ideal application of spiked sample, the critical prerequisite is the accurate isotopic composition of spike, which is commonly challenging to determine accurately. In this study, we report the first independent measurement of lutetium (Lu) isotopic composition in a Lu spike by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) using an optimized regression mass bias correction model. The rhenium (Re) reference material (NIST SRM 3143), previously calibrated against the NRC CRM IRIS-1 isotopic iridium (Ir), was selected as the primary calibrant to calibrate the Lu isotope ratio in Lu spike. The obtained ratio of R175/176 Lu was ..19994 .....5. (u, k11), which meets the required precision levels for the Lu-Hf isotopic system application. The accuracy of the Lu Hf isochron age was improved by the application of the precisely calibrated Lu spike, and this Lu spike was successful applied for the determination of Lu concentration in geological reference material. The application of the optimized regression model was further broadened by determining the isotopic composition of the Lu spike.
{"title":"Determination Of The Isotopic Composition Of An Enriched Lutetium Spike By MC-ICP-MS","authors":"K. Zong","doi":"10.46770/as.2022.188","DOIUrl":"https://doi.org/10.46770/as.2022.188","url":null,"abstract":"In geochronology, the isotope dilution (ID) method has been developed as an analytical method that provides accurate and precise element concentration and isotope ratio. For the ideal application of spiked sample, the critical prerequisite is the accurate isotopic composition of spike, which is commonly challenging to determine accurately. In this study, we report the first independent measurement of lutetium (Lu) isotopic composition in a Lu spike by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) using an optimized regression mass bias correction model. The rhenium (Re) reference material (NIST SRM 3143), previously calibrated against the NRC CRM IRIS-1 isotopic iridium (Ir), was selected as the primary calibrant to calibrate the Lu isotope ratio in Lu spike. The obtained ratio of R175/176 Lu was ..19994 .....5. (u, k11), which meets the required precision levels for the Lu-Hf isotopic system application. The accuracy of the Lu Hf isochron age was improved by the application of the precisely calibrated Lu spike, and this Lu spike was successful applied for the determination of Lu concentration in geological reference material. The application of the optimized regression model was further broadened by determining the isotopic composition of the Lu spike.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":" ","pages":""},"PeriodicalIF":3.4,"publicationDate":"2022-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48162052","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}
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