O. Mariichak, Y. Oleksii, G. M. Rozantsev, S. V. Radio
{"title":"含Ho(III)多氧化钨酸盐的合成、红外光谱及表面微观形貌","authors":"O. Mariichak, Y. Oleksii, G. M. Rozantsev, S. V. Radio","doi":"10.18524/2304-0947.2020.3(75).211723","DOIUrl":null,"url":null,"abstract":"nm. The technique developed in this work for the preparation of sodium decatungstoholmiate(ІІІ) is new and differs in that it allows one to synthesize a normal salt, which can be used for the synthesis of other normal salts of sodium heteropoly decatungstolanthanidates(ІІІ). As a result of attempts to synthesize salts by the interaction of holmium(III) nitrate with aqueous solutions of sodium tungstate acidified to Z = 1.17 and 1.29, X-ray amorphous solids were obtained, which most likely are mixtures of paratungstate B and holmium heptatungstate. Using the methods of chemical analysis and FTIR spectroscopy, the conditions for the formation of a sodium-holmium double salt with lacunar undecatungstate anion, derived from Keggin structure Na 2 Ho 2 [Нo 2 (H 2 O) 10 W 22 O 72 ( OH) 2 ]·46H 2 O are established. Procedure for the synthesis of holmium(III) paratungstate B Ho 10 [W 12 O 40 (OH) 2 ] 3 ·54H 2 O by the exchange reaction of holmium(ІІІ) nitrate with sodium paratungstate B was elaborated, and by the method of scanning electron microscopy it is proved to be single–phase. It was found that the grain size of the sample is in the range 200–450 nm. The absence of sodium(I) ions in the composition of the synthesized salt was proved by atomic absorption spectroscopy and EDX. Microphotographs of the salt powders Na 9 [Но(W 5 O 18 ) 2 ]·23H 2 O and Ho 10 [W 12 O 40 (OH) 2 ] 3 ·54H 2 O in the characteristic X–ray radiation show no zones with different surface morphologies, and show uniform distribution of Na, Ho, W, O is observed without segregation, which confirms the single–phase nature of the products.","PeriodicalId":19451,"journal":{"name":"Odesa National University Herald. Chemistry","volume":"2012 1","pages":""},"PeriodicalIF":0.0000,"publicationDate":"2020-09-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"SYNTHESIS, FT–IR SPECTROSCOPY AND SURFACE MICROMORPHOLOGY OF Ho(III)–CONTAINING POLYOXOTUNGSTATES\",\"authors\":\"O. Mariichak, Y. Oleksii, G. M. Rozantsev, S. V. Radio\",\"doi\":\"10.18524/2304-0947.2020.3(75).211723\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"nm. The technique developed in this work for the preparation of sodium decatungstoholmiate(ІІІ) is new and differs in that it allows one to synthesize a normal salt, which can be used for the synthesis of other normal salts of sodium heteropoly decatungstolanthanidates(ІІІ). As a result of attempts to synthesize salts by the interaction of holmium(III) nitrate with aqueous solutions of sodium tungstate acidified to Z = 1.17 and 1.29, X-ray amorphous solids were obtained, which most likely are mixtures of paratungstate B and holmium heptatungstate. Using the methods of chemical analysis and FTIR spectroscopy, the conditions for the formation of a sodium-holmium double salt with lacunar undecatungstate anion, derived from Keggin structure Na 2 Ho 2 [Нo 2 (H 2 O) 10 W 22 O 72 ( OH) 2 ]·46H 2 O are established. Procedure for the synthesis of holmium(III) paratungstate B Ho 10 [W 12 O 40 (OH) 2 ] 3 ·54H 2 O by the exchange reaction of holmium(ІІІ) nitrate with sodium paratungstate B was elaborated, and by the method of scanning electron microscopy it is proved to be single–phase. It was found that the grain size of the sample is in the range 200–450 nm. The absence of sodium(I) ions in the composition of the synthesized salt was proved by atomic absorption spectroscopy and EDX. Microphotographs of the salt powders Na 9 [Но(W 5 O 18 ) 2 ]·23H 2 O and Ho 10 [W 12 O 40 (OH) 2 ] 3 ·54H 2 O in the characteristic X–ray radiation show no zones with different surface morphologies, and show uniform distribution of Na, Ho, W, O is observed without segregation, which confirms the single–phase nature of the products.\",\"PeriodicalId\":19451,\"journal\":{\"name\":\"Odesa National University Herald. 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引用次数: 0
摘要
nm。这项工作中开发的制备十钨酸钠(ІІІ)的技术是新的,不同之处在于它可以合成一种正常的盐,这种盐可以用于合成十钨酸杂多钠的其他正常盐(ІІІ)。通过硝酸钬(III)与酸化至Z = 1.17和1.29的钨酸钠水溶液相互作用合成盐,得到了x射线无定形固体,很可能是仲钨酸B和七钨酸钬的混合物。采用化学分析和红外光谱分析的方法,确定了Keggin结构Na 2 Ho 2 [Нo 2 (h2o) 10 W 22 O 72 (OH) 2]·46h2o生成具有腔隙十一钨酸盐阴离子的钠-钬双盐的条件。阐述了硝酸钬(ІІІ)与仲钨酸钠B交换反应合成仲钨酸钬(III) bho 10 [w12 o40 (OH) 2] 3·54 h2o的工艺过程,并通过扫描电镜方法证实其为单相反应。结果表明,样品的晶粒尺寸在200 ~ 450 nm之间。通过原子吸收光谱和EDX验证了合成盐中不存在钠离子。盐粉Na 9 [Но(w5 O 18) 2]·23H 2o和Ho 10 [w12 O 40 (OH) 2] 3·54H 2o在特征x射线下的显微照片没有显示出不同的表面形貌区,Na、Ho、W、O分布均匀,没有偏析,证实了产物的单相性质。
SYNTHESIS, FT–IR SPECTROSCOPY AND SURFACE MICROMORPHOLOGY OF Ho(III)–CONTAINING POLYOXOTUNGSTATES
nm. The technique developed in this work for the preparation of sodium decatungstoholmiate(ІІІ) is new and differs in that it allows one to synthesize a normal salt, which can be used for the synthesis of other normal salts of sodium heteropoly decatungstolanthanidates(ІІІ). As a result of attempts to synthesize salts by the interaction of holmium(III) nitrate with aqueous solutions of sodium tungstate acidified to Z = 1.17 and 1.29, X-ray amorphous solids were obtained, which most likely are mixtures of paratungstate B and holmium heptatungstate. Using the methods of chemical analysis and FTIR spectroscopy, the conditions for the formation of a sodium-holmium double salt with lacunar undecatungstate anion, derived from Keggin structure Na 2 Ho 2 [Нo 2 (H 2 O) 10 W 22 O 72 ( OH) 2 ]·46H 2 O are established. Procedure for the synthesis of holmium(III) paratungstate B Ho 10 [W 12 O 40 (OH) 2 ] 3 ·54H 2 O by the exchange reaction of holmium(ІІІ) nitrate with sodium paratungstate B was elaborated, and by the method of scanning electron microscopy it is proved to be single–phase. It was found that the grain size of the sample is in the range 200–450 nm. The absence of sodium(I) ions in the composition of the synthesized salt was proved by atomic absorption spectroscopy and EDX. Microphotographs of the salt powders Na 9 [Но(W 5 O 18 ) 2 ]·23H 2 O and Ho 10 [W 12 O 40 (OH) 2 ] 3 ·54H 2 O in the characteristic X–ray radiation show no zones with different surface morphologies, and show uniform distribution of Na, Ho, W, O is observed without segregation, which confirms the single–phase nature of the products.