THE PREPARATION AND PROPERTIES OF MAGNESIUM PERCHLORATE AND ITS USE AS A DRYING AGENT1
THE PREPARATION AND PROPERTIES OF MAGNESIUM PERCHLORATE AND ITS USE AS A DRYING AGENT1
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DOI：
10.1021/ja01431a022
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发表时间：
1922-10
影响因子：
15
通讯作者：
H. Willard;G. Smith
中科院分区：
文献类型：
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作者：
H. Willard;G. Smith
高氯酸镁首先由Serullas制备。[2] Weinland和Ensgraber对这种物质进行了更详细的研究，[3]他通过在五氧化二磷上真空干燥样品来制备水合物Mg（C104）2.6 H2O。他们没有注意到这种处理最终产生较低的水合物Mg（C104）2· 3H20，因为即使在其早期阶段，脱水也相当缓慢。文献中没有提到过这种第二水合物。高氯酸镁六水合物的制备将最纯的进口氧化镁用稍微过量的纯dil处理。高氯酸，其通过Willard的方法制备。4.蒸发由此形成的溶液，直到在表面开始结晶，并放出高氯酸的烟雾。然后加入足够的水使混合物冷却至室温，以保持晶体物质为半流体。离心排水后，将仅含有少量高氯酸的产物再溶解，重结晶，并再次离心。这样得到的针状晶体经光谱检验表明不含钙或钡，尽管在其制备过程中所用的氧化物同样显示含有微量的这些杂质。
Magnesium perchlorate was first prepared by Serullas. 2 A more de-tailed study of this substance was made by Weinlandand Ensgraber, 3 who prepared the hydrate, Mg (C104) 2.6 H20, by drying the sample in a vacuum over phosphorus pentoxide. They failed to note that this treat-ment yields finally the lower hydrate, Mg (C104) 2· 3H20, because the de-hydration is rather slow even in its early stages. No mention of this second hydrate was found in the literature.Preparation of Magnesium Perchlorate Hexahydrate The purest imported magnesium oxide was treated with a slight excess of pure dil. perchloric acid, which was prepared by the method of Willard. 4 The solution thus formed was evaporated until crystallization began at the surface and fumes of perchloric acid were being given off. The mix-ture was then allowed to cool to room temperature with the addition of sufficient water to keep thecrystal mass semifluid. After centrifugal drainage the product, containing but a slight amount of perchloric acid, was redissolved, recrystallized, and again centrifuged. The needle-like crystals thus obtained were shown by spectroscopic examination to con-tain no calcium or barium in spite of the fact that the oxide employed in their preparation was similarly shown to contain traces of these impurities.