: Fe-Ni@ACC nanocomposite was synthesized by hydrothermal method and characterized using scanning electron microscope (SEM) and Fourier-transform infrared spectroscopy (FT-IR). Fe-Ni@ACC was used as adsorbent for magnetic dispersive micro solid-phase extraction (M-D-μSPE) procedure for separation and preconcentration of trace level of copper at trace levels before its determination by microsampling flame atomic absorption spectrometry (FAAS). The effects of various parameters such as pH, amount of adsorbent, eluent type and eluent volume, and sample volume on the recoveries of copper on Fe-Ni@ACC were optimized. The presented method is accurate, inexpensive and environmentally friendly and due to magnetic properties of the adsorbent, the separation process is very simple and fast. The method presents limit of detection (LOD)(3s/m) of 0.69 μg L −1 , limit of quantification (LOQ)(10s/m) of 2.29 μg L −1 , preconcentration factor of 40 and relative standard deviation (RSD %) (s/x) 1.18%. The accuracy of the method was confirmed by the analysis of TMDA-53.3 fortified water and TMDA-64.2 fortified water certified reference materials and addition-recovery tests to real samples. The present M-D-μSPE method was successfully applied to determination of copper level of tap water, cigarette, human hairs and black teas samples.
{"title":"Fe-Ni@ACC Nanocomposite For Magnetic Dispersive Micro Solid-Phase Extraction Of Cu (II) From Food And Hair Samples","authors":"M. Soylak","doi":"10.46770/as.2023.086","DOIUrl":"https://doi.org/10.46770/as.2023.086","url":null,"abstract":": Fe-Ni@ACC nanocomposite was synthesized by hydrothermal method and characterized using scanning electron microscope (SEM) and Fourier-transform infrared spectroscopy (FT-IR). Fe-Ni@ACC was used as adsorbent for magnetic dispersive micro solid-phase extraction (M-D-μSPE) procedure for separation and preconcentration of trace level of copper at trace levels before its determination by microsampling flame atomic absorption spectrometry (FAAS). The effects of various parameters such as pH, amount of adsorbent, eluent type and eluent volume, and sample volume on the recoveries of copper on Fe-Ni@ACC were optimized. The presented method is accurate, inexpensive and environmentally friendly and due to magnetic properties of the adsorbent, the separation process is very simple and fast. The method presents limit of detection (LOD)(3s/m) of 0.69 μg L −1 , limit of quantification (LOQ)(10s/m) of 2.29 μg L −1 , preconcentration factor of 40 and relative standard deviation (RSD %) (s/x) 1.18%. The accuracy of the method was confirmed by the analysis of TMDA-53.3 fortified water and TMDA-64.2 fortified water certified reference materials and addition-recovery tests to real samples. The present M-D-μSPE method was successfully applied to determination of copper level of tap water, cigarette, human hairs and black teas samples.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2023-06-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44597617","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}
: The miscellaneous materials, including gangue, plastic, and wood commonly present in coal. These miscellaneous materials affect the reliability of coal analysis using laser-induced breakdown spectroscopy in power plants, but have significantly distinct spectral characteristics from coal. Hence, this paper proposes a step-by-step classification method to screening the false spectra of miscellaneous materials. The first step aims to identify the plastic and wood spectra by determining the existence of specific characteristic spectral lines using the standard deviation (SD) values. The spectral lines Si Ι 288.16 nm with the SD value of more than 850 counts and Li Ι 670.78nm with SD value of more than 1750 counts were used as the distinguishing markers. The classification accuracy of first step was 100%. Due to the high similarity between gangue and coal, the second step utilized the random forest (RF) classification model to identify the gangue spectra. The number of trees and random variables in the RF model was optimized. The accuracy of classification model without and with the proposed step-by-step method was 98.30 and 99.96%, respectively. To assess the necessity of spectra classification, a set of calorific value analysis was performed by adding false spectra of different proportions, which were compared with analysis after removing the false spectra. The root mean square error of prediction ( 𝑅𝑀𝑆𝐸𝑃 ) was 0.42 MJ kg -1 (after removing), compared with 0.50 MJ kg -1 (mixing with 10% gangue spectra), 0.56 MJ kg -1 (mixing with 20% gangue spectra) and 0.57 MJ kg -1 (mixing with 30% gangue spectra). The results demonstrated that the proposed step-by-step classification method could effectively identify the spectra of coal and miscellaneous materials and improve the accuracy of coal analysis.
煤中常见的各种物质，包括脉石、塑料和木材。这些杂项物质影响了电厂用激光诱导击穿光谱分析煤的可靠性，但与煤具有明显不同的光谱特性。因此，本文提出了一种分步分类的方法来筛选杂类材料的假光谱。第一步旨在通过使用标准偏差(SD)值确定特定特征谱线的存在来识别塑料和木材光谱。分别以Si Ι 288.16 nm和Li Ι 670.78nm两种光谱线作为鉴别标记，其SD值均大于850次。第一步的分类准确率为100%。由于脉石与煤具有较高的相似性，第二步采用随机森林(RF)分类模型对脉石光谱进行识别。对模型中的树数和随机变量数进行了优化。采用分步法和不采用分步法的分类模型的准确率分别为98.30%和99.96%。为了评估光谱分类的必要性，通过添加不同比例的假光谱进行了一组热值分析，并与去除假光谱后的分析结果进行了比较。预测结果的均方根误差(𝑅𝑀𝑆值)为0.42 MJ kg -1(去除后)，而混合10%矸石光谱的预测误差为0.50 MJ kg -1，混合20%矸石光谱的预测误差为0.56 MJ kg -1，混合30%矸石光谱的预测误差为0.57 MJ kg -1。结果表明，所提出的分步分类方法能够有效地识别煤和杂物的光谱，提高了煤的分析精度。
{"title":"A Step-By-Step Classification Method Of Coal And Miscellaneous Materials By Laser-Induced Breakdown Spectroscopy","authors":"Shunchun Yao","doi":"10.46770/as.2023.102","DOIUrl":"https://doi.org/10.46770/as.2023.102","url":null,"abstract":": The miscellaneous materials, including gangue, plastic, and wood commonly present in coal. These miscellaneous materials affect the reliability of coal analysis using laser-induced breakdown spectroscopy in power plants, but have significantly distinct spectral characteristics from coal. Hence, this paper proposes a step-by-step classification method to screening the false spectra of miscellaneous materials. The first step aims to identify the plastic and wood spectra by determining the existence of specific characteristic spectral lines using the standard deviation (SD) values. The spectral lines Si Ι 288.16 nm with the SD value of more than 850 counts and Li Ι 670.78nm with SD value of more than 1750 counts were used as the distinguishing markers. The classification accuracy of first step was 100%. Due to the high similarity between gangue and coal, the second step utilized the random forest (RF) classification model to identify the gangue spectra. The number of trees and random variables in the RF model was optimized. The accuracy of classification model without and with the proposed step-by-step method was 98.30 and 99.96%, respectively. To assess the necessity of spectra classification, a set of calorific value analysis was performed by adding false spectra of different proportions, which were compared with analysis after removing the false spectra. The root mean square error of prediction ( 𝑅𝑀𝑆𝐸𝑃 ) was 0.42 MJ kg -1 (after removing), compared with 0.50 MJ kg -1 (mixing with 10% gangue spectra), 0.56 MJ kg -1 (mixing with 20% gangue spectra) and 0.57 MJ kg -1 (mixing with 30% gangue spectra). The results demonstrated that the proposed step-by-step classification method could effectively identify the spectra of coal and miscellaneous materials and improve the accuracy of coal analysis.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2023-06-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45817828","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}
: Lead-tin solder is a useful piece of evidence from a crime scene and may be examined for information related to the construction or source of an improvised explosive device (IED). A technique based on electrothermal vaporization into inductively coupled plasma optical emission spectrometry was improved for the direct quantification of trace and major elements in solder (Ag, As, Bi, Cr, Fe, Sb, Sn). NIST 1728, a tin-alloy certified reference material, was used for external calibration and achieve a direct, fully solid-sampling procedure using only 0.5–3.0 mg of sample. Point-by-point internal standardization with Ar 404.442 nm was performed to compensate for sample loading effects on the plasma, and a background correction technique was introduced to improve the overall efficiency of analysis. As solder was observed to change composition during some mock scenarios of IED preparation, which limits how solder can be examined in forensics, different soldering conditions (temperature, solder size, cleaning of the soldering tip or not between subsequent samples) were studied using an Fe-tip soldering device. Statistical analyses including Student’s t-tests and a one-way analysis of variance revealed that none of these conditions resulted in contamination of the melted solder sample, hence confirming the viability of the mock procedure used to replicate IED soldering in research. A new qualitative discrimination method is introduced and demonstrated in a blind trial for matching and discriminating lead-tin solders. This method represents an improvement from past research and has potential for use in evaluating other forensic evidence involving ferrous-alloys
{"title":"Advances In The Multi-Elemental Analysis Of Solder By ETV-ICPOES For The Discrimination Of Forensic Evidence","authors":"D. Beauchemin","doi":"10.46770/as.2023.113","DOIUrl":"https://doi.org/10.46770/as.2023.113","url":null,"abstract":": Lead-tin solder is a useful piece of evidence from a crime scene and may be examined for information related to the construction or source of an improvised explosive device (IED). A technique based on electrothermal vaporization into inductively coupled plasma optical emission spectrometry was improved for the direct quantification of trace and major elements in solder (Ag, As, Bi, Cr, Fe, Sb, Sn). NIST 1728, a tin-alloy certified reference material, was used for external calibration and achieve a direct, fully solid-sampling procedure using only 0.5–3.0 mg of sample. Point-by-point internal standardization with Ar 404.442 nm was performed to compensate for sample loading effects on the plasma, and a background correction technique was introduced to improve the overall efficiency of analysis. As solder was observed to change composition during some mock scenarios of IED preparation, which limits how solder can be examined in forensics, different soldering conditions (temperature, solder size, cleaning of the soldering tip or not between subsequent samples) were studied using an Fe-tip soldering device. Statistical analyses including Student’s t-tests and a one-way analysis of variance revealed that none of these conditions resulted in contamination of the melted solder sample, hence confirming the viability of the mock procedure used to replicate IED soldering in research. A new qualitative discrimination method is introduced and demonstrated in a blind trial for matching and discriminating lead-tin solders. This method represents an improvement from past research and has potential for use in evaluating other forensic evidence involving ferrous-alloys","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2023-06-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41968101","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}
: Mass-independent chromium (Cr) isotope ratios measurements have been widely used in dating early solar system events and tracing the genetic relationships between different solar system, as well as terrestrial materials. Current analytical techniques need relatively large sample sizes, and this limits the application of Cr isotopes on precious mission return samples and some Cr-poor samples ( e.g. , BCR-2 with Cr contents of ~15 ppm). This paper reports a novel analytical method for mass-independent Cr isotopic ratios measurements using a Thermal Ionization Mass Spectrometer (TIMS) operated in total evaporation (TE) mode. A three-step cation column (AG 50W-X12 resin, 200 ~ 400 mesh) chemistry is used to purify Cr in various samples, including chondrites, basalts and peridotites, and the Cr yield is better than 92%. Residual organics from column resins is detrimental to Cr ionization on filaments, we demonstrate that this can be effectively removed by treating samples with H 2 O 2 at 40 O C on hotplate. Single Cr measurements on rhenium filaments consume 15 to 20 ng of Cr and sustain 52 Cr of ~10V for 10 to 20 minutes. Generally, for one sample of 200 ng Cr, 10-15 ng repeated measurements can be made and 2-standard error precisions of ~ 0.05 and ~ 0.10 for ε 53 Cr and ε 54 Cr*, respectively can be achieved. The reproducibility (the 2-standard deviation) for ε 53 Cr and ε 54 Cr is 0.05 and 0.07, respectively, tested by multiple measurements for DTS-2b (USGS dunite) and NWA 7734 (ordinary chondrite). Concentration and doping test (mainly for Fe) have also been conducted. These tests show that the Fe/Cr must be < 5 % and the measured 56 Fe/ 52 Cr < 1 ‰ in order to achieve accurate ε 54 Cr. Finally, the ε 53 Cr and ε 54 Cr values measured by normal method on TIMS are systematically higher than those measured by total evaporation method on TIMS, which is potentially caused by non-kinetic mass-dependent fractionation during Cr evaporation and ionization on TIMS. The TE method could reduce this effect that may cause inaccurate mass-independent Cr isotope data on TIMS.
{"title":"Precise And Accurate Mass-Independent Chromium Isotope Measurement By Total Evaporation Mode On Thermal Ionization Mass Spectrometry (TE-TIMS) At 200 Ng Level","authors":"K. Zhu","doi":"10.46770/as.2023.079","DOIUrl":"https://doi.org/10.46770/as.2023.079","url":null,"abstract":": Mass-independent chromium (Cr) isotope ratios measurements have been widely used in dating early solar system events and tracing the genetic relationships between different solar system, as well as terrestrial materials. Current analytical techniques need relatively large sample sizes, and this limits the application of Cr isotopes on precious mission return samples and some Cr-poor samples ( e.g. , BCR-2 with Cr contents of ~15 ppm). This paper reports a novel analytical method for mass-independent Cr isotopic ratios measurements using a Thermal Ionization Mass Spectrometer (TIMS) operated in total evaporation (TE) mode. A three-step cation column (AG 50W-X12 resin, 200 ~ 400 mesh) chemistry is used to purify Cr in various samples, including chondrites, basalts and peridotites, and the Cr yield is better than 92%. Residual organics from column resins is detrimental to Cr ionization on filaments, we demonstrate that this can be effectively removed by treating samples with H 2 O 2 at 40 O C on hotplate. Single Cr measurements on rhenium filaments consume 15 to 20 ng of Cr and sustain 52 Cr of ~10V for 10 to 20 minutes. Generally, for one sample of 200 ng Cr, 10-15 ng repeated measurements can be made and 2-standard error precisions of ~ 0.05 and ~ 0.10 for ε 53 Cr and ε 54 Cr*, respectively can be achieved. The reproducibility (the 2-standard deviation) for ε 53 Cr and ε 54 Cr is 0.05 and 0.07, respectively, tested by multiple measurements for DTS-2b (USGS dunite) and NWA 7734 (ordinary chondrite). Concentration and doping test (mainly for Fe) have also been conducted. These tests show that the Fe/Cr must be < 5 % and the measured 56 Fe/ 52 Cr < 1 ‰ in order to achieve accurate ε 54 Cr. Finally, the ε 53 Cr and ε 54 Cr values measured by normal method on TIMS are systematically higher than those measured by total evaporation method on TIMS, which is potentially caused by non-kinetic mass-dependent fractionation during Cr evaporation and ionization on TIMS. The TE method could reduce this effect that may cause inaccurate mass-independent Cr isotope data on TIMS.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2023-06-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45085664","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 this study, a small platinized tungsten coil (TC) with a composite structure was utilized for the first time in a liquid sampling electrothermal vaporizer (ETV) setup. A novel direct sampling mercury (Hg) analyzer coupled with a dielectric barrier discharge (DBD) and a miniature fiber optic spectrometer (FOS) as an optical emission spectrometer was fabricated for the sensitive determination of Hg in environmental water. This ETV setup displayed a maximum sample volume of 100 μL and fulfilled the task of sequestering Hg during the dehydration and ashing processes under high temperature due to the formation of a platinum (Pt) and Hg amalgam. Under optimized conditions, the limit of detection (LOD) of Hg was 0.1 μg L -1 for a 100 μL liquid sample and the relative standard deviation (RSD) of 11 repeated measurements of Hg standard solution was 3.2%; the linearity ( R 2 ) was > 0.999 in the range of 0.4-100 μg L -1 . The results for the GBW08063 sample (9.89 μg L -1 ) agreed with the certified values of certified reference materials (CRMs) (10 μg L -1 ), and the spiked recoveries were 94-100%, which proved favorable analytical accuracy and precision. The total analysis time was observed to be less than 3 min, and this small-sized ETV-DBD-OES system consumes only ~100 W of power while weighting less than 12 kg. Therefore, the proposed ETV-DBD-OES method demonstrates simplicity, suitable sensitivity, precision, and robustness, with promising application in the field for rapid water analysis for Hg.
在这项研究中，首次将一个具有复合结构的小铂化钨线圈(TC)用于液体取样电热汽化器(ETV)装置中。采用介质阻挡放电(DBD)和微型光纤光谱仪(FOS)作为光发射光谱仪，研制了一种新型直接进样汞分析仪，用于环境水中汞的灵敏测定。该ETV装置最大样品体积为100 μL，在高温脱水和灰化过程中，由于铂(Pt)和汞齐合金的形成，ETV装置完成了汞的隔离任务。优化条件下，100 μL液样中Hg的检出限(LOD)为0.1 μL -1，标准液中Hg重复测定11次的相对标准偏差(RSD)为3.2%;在0.4 ~ 100 μg L -1范围内，线性关系(r2)为> 0.999。结果表明，GBW08063样品(9.89 μ L -1)与标准物质(10 μ L -1)的标配值一致，加标回收率为94 ~ 100%，具有良好的分析准确度和精密度。总分析时间小于3 min，该小型ETV-DBD-OES系统功耗仅为~100 W，重量小于12 kg。因此，ETV-DBD-OES方法操作简便，灵敏度、精密度和鲁棒性均较好，在水中汞的快速分析中具有较好的应用前景。
{"title":"A Novel Tungsten Coil Electrothermal Vaporizer With Composite Structure Coupled With Dielectric Barrier Discharge Optical Emission Spectrometer For Direct Determination Of Trace Mercury","authors":"Jixin Liu, Xuefei Mao","doi":"10.46770/as.2023.089","DOIUrl":"https://doi.org/10.46770/as.2023.089","url":null,"abstract":": In this study, a small platinized tungsten coil (TC) with a composite structure was utilized for the first time in a liquid sampling electrothermal vaporizer (ETV) setup. A novel direct sampling mercury (Hg) analyzer coupled with a dielectric barrier discharge (DBD) and a miniature fiber optic spectrometer (FOS) as an optical emission spectrometer was fabricated for the sensitive determination of Hg in environmental water. This ETV setup displayed a maximum sample volume of 100 μL and fulfilled the task of sequestering Hg during the dehydration and ashing processes under high temperature due to the formation of a platinum (Pt) and Hg amalgam. Under optimized conditions, the limit of detection (LOD) of Hg was 0.1 μg L -1 for a 100 μL liquid sample and the relative standard deviation (RSD) of 11 repeated measurements of Hg standard solution was 3.2%; the linearity ( R 2 ) was > 0.999 in the range of 0.4-100 μg L -1 . The results for the GBW08063 sample (9.89 μg L -1 ) agreed with the certified values of certified reference materials (CRMs) (10 μg L -1 ), and the spiked recoveries were 94-100%, which proved favorable analytical accuracy and precision. The total analysis time was observed to be less than 3 min, and this small-sized ETV-DBD-OES system consumes only ~100 W of power while weighting less than 12 kg. Therefore, the proposed ETV-DBD-OES method demonstrates simplicity, suitable sensitivity, precision, and robustness, with promising application in the field for rapid water analysis for Hg.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2023-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44061279","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":"Lycoptera Fossil Elemental Imaging And Paleo-Environment Research Via Laser Ionization Time-Of-Flight Mass Spectrometry","authors":"W. Hang","doi":"10.46770/as.2023.062","DOIUrl":"https://doi.org/10.46770/as.2023.062","url":null,"abstract":"","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2023-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43703794","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}
High-temperature and High-pressure Sintering Method to Prepare Magnetite Reference Material for In-situ Microanalysis Xiao-Wen Huang, a Yu-Miao Meng, Sen Lin, * and Liang Qi a a State Key Laboratory of Ore Deposit Geochemistry, Institute of Geochemistry, Chinese Academy of Sciences, Guiyang 550081, China b Key Laboratory for High Temperature and High Pressure Study of the Earth’s Interior, Institute of Geochemistry, Chinese Academy of Sciences, Guiyang 550081, China
高温高压烧结法制备磁铁矿原位微量分析基准物质黄晓文，王宇淼，林森，*，齐亮a .中国科学院地球化学研究所矿床地球化学国家重点实验室，贵阳550081 b .中国科学院地球化学研究所地球内部高温高压研究重点实验室，贵阳550081
{"title":"High-Temperature And High-Pressure Sintering Method To Prepare Magnetite Reference Material For In-Situ Microanalysis","authors":"Sen Lin","doi":"10.46770/as.2023.012","DOIUrl":"https://doi.org/10.46770/as.2023.012","url":null,"abstract":"High-temperature and High-pressure Sintering Method to Prepare Magnetite Reference Material for In-situ Microanalysis Xiao-Wen Huang, a Yu-Miao Meng, Sen Lin, * and Liang Qi a a State Key Laboratory of Ore Deposit Geochemistry, Institute of Geochemistry, Chinese Academy of Sciences, Guiyang 550081, China b Key Laboratory for High Temperature and High Pressure Study of the Earth’s Interior, Institute of Geochemistry, Chinese Academy of Sciences, Guiyang 550081, China","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2023-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44197496","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}
: Magnetic covalent organic frameworks (COFs) were prepared using aminated Fe 3 O 4 nanoparticles as the magnetic core and 1,3,5-tris(4-aminophenyl)benzene (TPB) and 2,5-dimethoxyterephthalaldehyde (DMTA) as monomers. The resultant Fe 3 O 4 @TPB-DMTP-COF was then post-modified with 3-ethynylthiophene through the “Aza D-A reaction”. The Fe 3 O 4 @COF-thiophene composite showed a high Brunauer-Emmett-Teller surface area of 898 m 2· g -1 , as well as a high content of S (5.27 w.t.%). Trace mercury (Hg), lead (Pb), and bismuth (Bi) ions were extracted from environmental water samples, followed by inductively coupled plasma mass spectrometry (ICP-MS) detection. Extraction conditions, such as extraction pH, sample volume, adsorbent amount, extraction/desorption time and elution volume, were optimized. Under the optimal conditions, the three heavy metal ions were extracted from 150 mL of aqueous solution within 20 min and eluted with 0.1 mol L -1 HNO 3 containing 8% cysteamine hydrochloride within 20 min. The method exhibited a high enrichment factor (188) and wide linear range of 3-5000 ng·L - 1 for Hg 2+ /Pb 2+ and 2-2000 for Bi 3+ , with the detection limits of 0.41, 0.97 and 0.47 ng∙L -1 , respectively. Furthermore, the reproducibility of the method was evaluated, and the relative standard deviations of Hg 2+ , Pb 2+ and Bi 3+ were found to be 7.5, 6.8 and 6.2% (n = 7, c = 3 ng∙L -1 ), respectively. The accuracy of this method was verified by analyzing certified reference materials in environmental water, including GSB 07-1185-2000 (202047), GSB 07-1185-2000 (201239) and BY 400143 (B2003113). The application potential of this method was further evaluated by analyzing real environmental water samples. Target Hg 2+ and Pb 2+ ions concentrations were found to be 4.91 and 62.5 ng∙L -1 , respectively, in the East Lake water sample and 10.2 and 103 ng·L - 1 , respectively, in the Yangtze River water sample. The recoveries of target three metal ions were found to be 86.1-104 % in the two environmental water samples at three spiked concentration levels.
{"title":"Thiophene Functionalized Magnetic Covalent Organic Frameworks For Selective Extraction Of Trace Heavy Metals Followed By ICP-MS Detection","authors":"M. He","doi":"10.46770/as.2023.088","DOIUrl":"https://doi.org/10.46770/as.2023.088","url":null,"abstract":": Magnetic covalent organic frameworks (COFs) were prepared using aminated Fe 3 O 4 nanoparticles as the magnetic core and 1,3,5-tris(4-aminophenyl)benzene (TPB) and 2,5-dimethoxyterephthalaldehyde (DMTA) as monomers. The resultant Fe 3 O 4 @TPB-DMTP-COF was then post-modified with 3-ethynylthiophene through the “Aza D-A reaction”. The Fe 3 O 4 @COF-thiophene composite showed a high Brunauer-Emmett-Teller surface area of 898 m 2· g -1 , as well as a high content of S (5.27 w.t.%). Trace mercury (Hg), lead (Pb), and bismuth (Bi) ions were extracted from environmental water samples, followed by inductively coupled plasma mass spectrometry (ICP-MS) detection. Extraction conditions, such as extraction pH, sample volume, adsorbent amount, extraction/desorption time and elution volume, were optimized. Under the optimal conditions, the three heavy metal ions were extracted from 150 mL of aqueous solution within 20 min and eluted with 0.1 mol L -1 HNO 3 containing 8% cysteamine hydrochloride within 20 min. The method exhibited a high enrichment factor (188) and wide linear range of 3-5000 ng·L - 1 for Hg 2+ /Pb 2+ and 2-2000 for Bi 3+ , with the detection limits of 0.41, 0.97 and 0.47 ng∙L -1 , respectively. Furthermore, the reproducibility of the method was evaluated, and the relative standard deviations of Hg 2+ , Pb 2+ and Bi 3+ were found to be 7.5, 6.8 and 6.2% (n = 7, c = 3 ng∙L -1 ), respectively. The accuracy of this method was verified by analyzing certified reference materials in environmental water, including GSB 07-1185-2000 (202047), GSB 07-1185-2000 (201239) and BY 400143 (B2003113). The application potential of this method was further evaluated by analyzing real environmental water samples. Target Hg 2+ and Pb 2+ ions concentrations were found to be 4.91 and 62.5 ng∙L -1 , respectively, in the East Lake water sample and 10.2 and 103 ng·L - 1 , respectively, in the Yangtze River water sample. The recoveries of target three metal ions were found to be 86.1-104 % in the two environmental water samples at three spiked concentration levels.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2023-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41711526","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}
: MoS 2 and ZnS quantum dots (QDs) were synthesized and applied as labels in magnetic immunoassays for the determination of myeloperoxidase (MPO) and osteopontin (OPN) via single-particle mode inductively coupled plasma mass spectrometry (ICP-MS). Primary MPO antibodies and primary OPN antibodies were captured by amino-modified magnetic nanoparticles, and the target biomarkers (MPO and OPN) were extracted and then specifically labeled with MoS 2 QD-secondary MPO antibody and ZnS QD-secondary OPN antibody conjugates, respectively. MoS 2 and ZnS QDs were employed as determination signal probes for ICP-MS measurements. Under the optimized conditions, the limits of detection obtained by magnetic immunoassay for MoS 2 and ZnS QD-labeled MPO and OPN were 0.004 and 0.005 ng mL -1 , respectively. The linear ranges for MPO and OPN were 0.01–50 and 0.02–50 ng mL -1 , respectively. From six replicates, the relative standard deviations of MPO and OPN were found to be 3.5% and 3.2%, respectively. The proposed strategy was applied to determine the MPO and OPN levels in real human serum samples.
：合成了MoS2和ZnS量子点（QDs），并将其作为标记物应用于磁性免疫分析，通过单粒子模式电感耦合等离子体质谱法（ICP-MS）测定髓过氧化物酶（MPO）和骨桥蛋白（OPN）。用氨基修饰的磁性纳米颗粒捕获初级MPO抗体和初级OPN抗体，提取目标生物标志物（MPO和OPN），然后分别用MoS2 QD次级MPO抗体偶联物和ZnS QD次级OPN抗体偶联物特异性标记。MoS2和ZnS量子点被用作ICP-MS测量的测定信号探针。在优化的条件下，磁性免疫分析法对MoS2和ZnS-QD标记的MPO和OPN的检测限分别为0.004和0.005ng/mL-1。MPO和OPN的线性范围分别为0.01–50和0.02–50 ng mL-1。从六个重复中，MPO和OPN的相对标准偏差分别为3.5%和3.2%。将所提出的策略应用于测定真实人类血清样品中的MPO和OPN水平。
{"title":"Detection Of Myeloperoxidase And Osteopontin In Human Serum Using Single Particle-ICP-MS With MoS2 And ZnS Quantum Dots","authors":"Yupin Cao, Biyang Deng","doi":"10.46770/as.2023.042","DOIUrl":"https://doi.org/10.46770/as.2023.042","url":null,"abstract":": MoS 2 and ZnS quantum dots (QDs) were synthesized and applied as labels in magnetic immunoassays for the determination of myeloperoxidase (MPO) and osteopontin (OPN) via single-particle mode inductively coupled plasma mass spectrometry (ICP-MS). Primary MPO antibodies and primary OPN antibodies were captured by amino-modified magnetic nanoparticles, and the target biomarkers (MPO and OPN) were extracted and then specifically labeled with MoS 2 QD-secondary MPO antibody and ZnS QD-secondary OPN antibody conjugates, respectively. MoS 2 and ZnS QDs were employed as determination signal probes for ICP-MS measurements. Under the optimized conditions, the limits of detection obtained by magnetic immunoassay for MoS 2 and ZnS QD-labeled MPO and OPN were 0.004 and 0.005 ng mL -1 , respectively. The linear ranges for MPO and OPN were 0.01–50 and 0.02–50 ng mL -1 , respectively. From six replicates, the relative standard deviations of MPO and OPN were found to be 3.5% and 3.2%, respectively. The proposed strategy was applied to determine the MPO and OPN levels in real human serum samples.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2023-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44549605","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}
: Microplasma-induced vapor generation (μPIVG), particularly using only hydrogen, has attracted increasing attention in the field of atomic spectrometry. However, its application for field analysis of environmental samples remains limited owing to the difficulty of hydrogen storage and transportation. Herein, a non-noble metal electrode-based hydrogen evolution reaction (HER) was utilized as a safe and environment-friendly hydrogen supply method for the efficient μPIVG of Hg, Cd and Zn. Subsequently, HER-μPIVG was used for the sensitive field detection of Hg, Cd and Zn in environmental samples via miniature point discharge optical emission spectrometry (μPD-OES). In contrast to conventional hydrogen-enhanced μPIVG, hydrogen was produced in situ and in real time using a superior cathode composed of cobalt-phosphorous nanomaterial, eliminating the storage and transport of hydrogen requirements and improving the safety, sensitivity, and feasibility of μPIVG-μPD-OES. Under the optimized conditions, the limits of detection (LODs) were 0.8, 10, and 14 μg L −1 for Hg, Cd, and Zn, respectively, with relative standard deviations (RSDs) of < 4.7%. The accuracy and practicability of the proposed method were validated through Hg, Cd, and Zn determinations in two certified reference materials (CRMs) and several water samples with satisfactory results.
{"title":"Integration Of Hydrogen Evolution Reaction And Microplasma Induced Vapor Generation: A Strategy For Improving Safety And Sensitivity Of Microplasma Optical Emission Spectrometry","authors":"C. Zheng","doi":"10.46770/as.2023.091","DOIUrl":"https://doi.org/10.46770/as.2023.091","url":null,"abstract":": Microplasma-induced vapor generation (μPIVG), particularly using only hydrogen, has attracted increasing attention in the field of atomic spectrometry. However, its application for field analysis of environmental samples remains limited owing to the difficulty of hydrogen storage and transportation. Herein, a non-noble metal electrode-based hydrogen evolution reaction (HER) was utilized as a safe and environment-friendly hydrogen supply method for the efficient μPIVG of Hg, Cd and Zn. Subsequently, HER-μPIVG was used for the sensitive field detection of Hg, Cd and Zn in environmental samples via miniature point discharge optical emission spectrometry (μPD-OES). In contrast to conventional hydrogen-enhanced μPIVG, hydrogen was produced in situ and in real time using a superior cathode composed of cobalt-phosphorous nanomaterial, eliminating the storage and transport of hydrogen requirements and improving the safety, sensitivity, and feasibility of μPIVG-μPD-OES. Under the optimized conditions, the limits of detection (LODs) were 0.8, 10, and 14 μg L −1 for Hg, Cd, and Zn, respectively, with relative standard deviations (RSDs) of < 4.7%. The accuracy and practicability of the proposed method were validated through Hg, Cd, and Zn determinations in two certified reference materials (CRMs) and several water samples with satisfactory results.","PeriodicalId":8642,"journal":{"name":"Atomic Spectroscopy","volume":null,"pages":null},"PeriodicalIF":3.4,"publicationDate":"2023-04-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46453887","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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