{"title":"评估金属有机框架浸渍材料的两步萃取法。","authors":"Mizuki Mukai, Reetu Rani, Nao Iwanaga, Kentaro Saeki, Kei Toda, Shin-Ichi Ohira","doi":"10.1007/s44211-024-00608-5","DOIUrl":null,"url":null,"abstract":"<div><p>Metal–organic frameworks (MOFs) are widely used for gas adsorption, separation, and sensing materials. In most cases, MOFs are not used in their crystal form but as impregnated materials because the fine crystals result in high-pressure drops. One key characteristic of MOF-impregnated materials is the amount of MOF in the material. This is evaluated using the wet digestion method; however, it is limited to determining only the metal content. Moreover, some metal, denoted as free metal, will not react with ligands to form MOFs. Additionally, it is crucial to determine the ligand amount, which cannot be determined using wet digestion. In the present study, a two-step extraction method for copper (II) benzene-1,3,5-tricarboxylate (Cu-BTC MOF) impregnated materials was developed to determine the MOF formed and free metals and ligands. Various solvents were applied to evaluate the extraction efficiencies. The results led to the selection of ethanol (EtOH) for extracting free Cu<sup>2+</sup> and BTC, while 0.3 M HNO<sub>3</sub> was chosen to extract MOF-formed Cu<sup>2+</sup> and BTC. The MOF-impregnated sample material was first extracted using EtOH and then 0.3 M HNO<sub>3</sub>. The Cu<sup>2+</sup> and BTC in the obtained extract solutions, as well as EtOH and HNO<sub>3</sub>, were analyzed using flame atomic absorption spectroscopy and high-performance liquid chromatography, respectively. In standard addition tests, free and MOF-formed Cu<sup>2+</sup> and BTC were quantitatively extracted from MOF-impregnated materials. The developed two-step analysis method was successfully applied to Cu-BTC-impregnated materials used in gas sensing.</p><h3>Graphical abstract</h3>\n<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":7802,"journal":{"name":"Analytical Sciences","volume":null,"pages":null},"PeriodicalIF":1.8000,"publicationDate":"2024-05-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Two-step extraction for the evaluation of metal–organic framework impregnated materials\",\"authors\":\"Mizuki Mukai, Reetu Rani, Nao Iwanaga, Kentaro Saeki, Kei Toda, Shin-Ichi Ohira\",\"doi\":\"10.1007/s44211-024-00608-5\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>Metal–organic frameworks (MOFs) are widely used for gas adsorption, separation, and sensing materials. In most cases, MOFs are not used in their crystal form but as impregnated materials because the fine crystals result in high-pressure drops. One key characteristic of MOF-impregnated materials is the amount of MOF in the material. This is evaluated using the wet digestion method; however, it is limited to determining only the metal content. Moreover, some metal, denoted as free metal, will not react with ligands to form MOFs. Additionally, it is crucial to determine the ligand amount, which cannot be determined using wet digestion. In the present study, a two-step extraction method for copper (II) benzene-1,3,5-tricarboxylate (Cu-BTC MOF) impregnated materials was developed to determine the MOF formed and free metals and ligands. Various solvents were applied to evaluate the extraction efficiencies. The results led to the selection of ethanol (EtOH) for extracting free Cu<sup>2+</sup> and BTC, while 0.3 M HNO<sub>3</sub> was chosen to extract MOF-formed Cu<sup>2+</sup> and BTC. The MOF-impregnated sample material was first extracted using EtOH and then 0.3 M HNO<sub>3</sub>. The Cu<sup>2+</sup> and BTC in the obtained extract solutions, as well as EtOH and HNO<sub>3</sub>, were analyzed using flame atomic absorption spectroscopy and high-performance liquid chromatography, respectively. In standard addition tests, free and MOF-formed Cu<sup>2+</sup> and BTC were quantitatively extracted from MOF-impregnated materials. The developed two-step analysis method was successfully applied to Cu-BTC-impregnated materials used in gas sensing.</p><h3>Graphical abstract</h3>\\n<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>\",\"PeriodicalId\":7802,\"journal\":{\"name\":\"Analytical Sciences\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":1.8000,\"publicationDate\":\"2024-05-29\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Analytical Sciences\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://link.springer.com/article/10.1007/s44211-024-00608-5\",\"RegionNum\":4,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"CHEMISTRY, ANALYTICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Analytical Sciences","FirstCategoryId":"92","ListUrlMain":"https://link.springer.com/article/10.1007/s44211-024-00608-5","RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
Two-step extraction for the evaluation of metal–organic framework impregnated materials
Metal–organic frameworks (MOFs) are widely used for gas adsorption, separation, and sensing materials. In most cases, MOFs are not used in their crystal form but as impregnated materials because the fine crystals result in high-pressure drops. One key characteristic of MOF-impregnated materials is the amount of MOF in the material. This is evaluated using the wet digestion method; however, it is limited to determining only the metal content. Moreover, some metal, denoted as free metal, will not react with ligands to form MOFs. Additionally, it is crucial to determine the ligand amount, which cannot be determined using wet digestion. In the present study, a two-step extraction method for copper (II) benzene-1,3,5-tricarboxylate (Cu-BTC MOF) impregnated materials was developed to determine the MOF formed and free metals and ligands. Various solvents were applied to evaluate the extraction efficiencies. The results led to the selection of ethanol (EtOH) for extracting free Cu2+ and BTC, while 0.3 M HNO3 was chosen to extract MOF-formed Cu2+ and BTC. The MOF-impregnated sample material was first extracted using EtOH and then 0.3 M HNO3. The Cu2+ and BTC in the obtained extract solutions, as well as EtOH and HNO3, were analyzed using flame atomic absorption spectroscopy and high-performance liquid chromatography, respectively. In standard addition tests, free and MOF-formed Cu2+ and BTC were quantitatively extracted from MOF-impregnated materials. The developed two-step analysis method was successfully applied to Cu-BTC-impregnated materials used in gas sensing.
期刊介绍:
Analytical Sciences is an international journal published monthly by The Japan Society for Analytical Chemistry. The journal publishes papers on all aspects of the theory and practice of analytical sciences, including fundamental and applied, inorganic and organic, wet chemical and instrumental methods.
This publication is supported in part by the Grant-in-Aid for Publication of Scientific Research Result of the Japanese Ministry of Education, Culture, Sports, Science and Technology.