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• W2078160964 abstract "VI. SUMMARYIt is possible to bright-plate both Re and Tc metals from aqueous media in a reasonably quantitative fashion, but the deposit is not favorable for weighing. The (VII)-states in 4 M perchloric acid undergo initial 4- or 3-electron reduction-steps in polarography at the d.m.e. These waves are suitable for analyses of 10−3 — 10−4 M solutions within ± 1% if necessary precautions are taken. The four-electron coulometric reduction of pertechnetate can probably be refined to better than ± 0.5%. Several usable amperometric techniques exist for the determination of rhenium. The direct chemical reduction of some technetium (VII) in aqueous acidic media by contact with mercury is an important consideration in many electrochemical techniques.The available techniques for the determination of rhenium and technetium by redox potentiometry are not very selective. Precipitation of the tetraphenylarsonium MO4− salts remains the only good gravimetric determination which has been described for these elements; useful amperometric variants of this procedure have not been defined.Older procedures for the separation of rhenium or technetium from other materials by volatilization are often supplanted by ion-exchange or liquid-liquid extraction methods. Most ion-exchange methods involve the MO4− ions on anion-exchangers and the use of acidic media, especially nitric acid. Many different liquid-liquid extraction systems are used, the majority employing the (VII)-species. Many complexed and chelated (V)-species would be amenable to extractions, but conveniently quantitative routes to the (V)-compounds are not easily found.The normal tetrahedral MO4− species persist in aqueous media under most circumstances; their characteristic absorption in the ultraviolet region has some analytical utility, especially for the pertechnetate ion. The formation of meso-ions, MO5−3, in alkaline media is not very extensive in the case of rhenium and is virtually non-existent with technetium in aqueous media. Spectrophotometric measurement of ReCl6−2 provides a useful method; a comparable TcCl6−2 procedure would be complicated by the occurrence of photocatalyzed aquation. Study of the latter process explains some of the previous discrepancies regarding the spectrum of this ion. The (V)-thiocyanate procedures remain important for rhenium and technetium, as does the furildioxime chelate with rhenium. A number of dyes have been found to be reactive with perrhenate and extract into solvents like benzene; they have molar absorptivities that approach 105.The very unusual properties of a technetium (V) system with a substituted 8-quinolinol are described. The system has important direct applications for liquid-liquid extraction and spectrophotometry. More importantly, it is probably representative of other (V)-chelates of analytical significance. Only a start has been made toward the full elucidation of this rather complex example of such a system.Both the spark excitation of refractory solids and the volatilization of metal chelates will permit increasingly frequent application of mass spectrometry to inorganic analyses and studies of materials including rhenium and technetium. There is no question whatever that a more widespread use should be made of x-ray absorption and fluorescence methods in the routine analysis of such difficult samples as alloys containing rhenium and technetium.Activation analysis is being widely applied for the determination of low levels of both rhenium and technetium. In addition, of course, the usual occurrence of the latter element is as either Tc9 9 m or Tc9 9, which provide their own radioactivity.There remains a relative paucity of good classical gravimetric, titrimetric, simpler electrometric methods available for rhenium and technetium. But there does exist a good selection of bases for separations, for sensitive and reliable measurements by spectrophotometry, radioactivity, contemporary instrumental methods." @default.
• W2078160964 created "2016-06-24" @default.
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• W2078160964 date "1970-11-01" @default.
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• W2078160964 title "Recent Developments in the Analytical Chemistry of Rhenium and Technetium" @default.
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• W2078160964 doi "https://doi.org/10.1080/1040834ve08542738" @default.
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