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Method for measuring rhenium content in ammonium rhenate

A determination method, ammonium rhenate technology, applied in the field of chemical analysis, can solve the problems of long evaporation time, poor anti-interference ability, long detection time, etc.

Inactive Publication Date: 2018-02-16
TONGLING NON FERROUS METAL GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because there are errors in the measurement results of single impurity content and the accumulation of multiple impurity measurement results, this method has the problem of inaccurate measurement results, and in the measurement process, rhenium needs to be removed in the form of rhenium sulfide through repeated evaporation, and the evaporation time is long , high energy consumption
However, the tetraphenyl arsenic chloride hydrochloride precipitation gravimetric method has the defects of long detection time and poor anti-interference ability.

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  • Method for measuring rhenium content in ammonium rhenate

Examples

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Embodiment 1

[0031] A method for assaying rhenium content in ammonium rhenate, comprising the steps of:

[0032] (1) Take by weighing 0.9997g ammonium rhenate and be dissolved in 150ml water, then add 50.0ml concentration and be the sulfuric acid solution of 25g / L and 5g ammonium sulfate, after dissolving completely, be diluted to 250ml, obtain electrolyte;

[0033] (2) Boil the platinum electrode in 50vt% nitric acid for 4 minutes, take it out and rinse it with water, then boil it in boiling water for 2 minutes, take it out and soak it twice with absolute ethanol to obtain a platinum anode and a platinum cathode;

[0034] (3) Under the condition of 105°C, dry the platinum cathode for 4 minutes, cool it, and accurately weigh the mass of the platinum cathode for the first time to 19.1973g;

[0035] (4) Pour the electrolyte solution into a beaker first, then install the platinum anode and platinum cathode on the electrolysis instrument, immerse the platinum mesh or platinum sheet in the elec...

Embodiment 2

[0042] A method for assaying rhenium content in ammonium rhenate, comprising the steps of:

[0043] (1) Take by weighing 1.0040g ammonium rhenate and be dissolved in 150ml water, then add 75.0ml concentration and be the sulfuric acid solution of 25g / L and 5g ammonium sulfate, after dissolving completely, be diluted to 250ml, obtain electrolyte;

[0044] (2) Boil the platinum electrode in 50vt% nitric acid for 5 minutes, take it out and rinse it with water, then boil it in boiling water for 1 minute, take it out and soak it twice with absolute ethanol to obtain a platinum anode and a platinum cathode;

[0045] (3) Under the condition of 105°C, dry the platinum cathode for 3 minutes, cool it, and accurately weigh the mass of the platinum cathode 19.1975g for the first time;

[0046](4) Pour the electrolyte solution into a beaker first, then install the platinum anode and platinum cathode on the electrolysis instrument, immerse the platinum mesh or platinum sheet in the electroly...

Embodiment 3

[0053] A method for assaying rhenium content in ammonium rhenate, comprising the steps of:

[0054] (1) Take by weighing 1.0007g ammonium rhenate and be dissolved in 150ml water, then add 40.0ml concentration and be the sulfuric acid solution of 25g / L and 5.5g ammonium sulfate, after dissolving completely, be diluted to 250ml, obtain electrolyte;

[0055] (2) Boil the platinum electrode in 50vt% nitric acid for 5 minutes, take it out and rinse it with water, then boil it in boiling water for 2 minutes, take it out and soak it twice with absolute ethanol to obtain a platinum anode and a platinum cathode;

[0056] (3) Under the condition of 105°C, dry the platinum cathode for 5 minutes, cool it, and accurately weigh the mass of the platinum cathode for the first time to 19.1973g;

[0057] (4) Pour the electrolyte solution into a beaker first, then install the platinum anode and platinum cathode on the electrolysis instrument, immerse the platinum mesh or platinum sheet in the el...

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Abstract

The invention relates to the technical field of chemical analysis, in particular to a method for measuring the rhenium content in ammonium rhenate. The method includes steps of taking platinum electrodes as anodic-cathodic, and performing electrolysis at a certain concentration of electrolyte and a certain current density; stirring an electrolyte solution by the aid of bubbles generated from the platinum electrodes without turning on stirring and heating devices during the entire electrolytic process so that perrhenate ions (ReO4<->) is reduced to be metallic rhenium (Re) and deposited on theplatinum electrodes with known mass; performing drying and weighing to obtain the mass of rhenium deposited on the platinum electrodes; performing supplementary measurement on the trace rhenium in theresidual electrolytic solution by means of an ICP-AES method. Both the electrolytic method and the ICP-AES method are adopted at the same time, and accuracy of measuring results is guaranteed.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a method for determining rhenium content in ammonium rhenate. Background technique [0002] Rhenium is a rare metal element, its content in the earth's crust is extremely low, and only a small amount is distributed in molybdenite, rare earth ore and niobium-tantalum ore. Metal rhenium has a high melting point, and is often used as a catalyst for refining petroleum, and has a wide range of applications in superalloys, electronic tube structural materials, special alloys for aerospace, and environmental protection. Currently, the best way to prepare pure metal rhenium is to reduce its industrial compound ammonium rhenate with hydrogen. Ammonium rhenate produced in industry often contains certain impurities. The type and content of the impurities seriously affect the purity of the sample. The detection of rhenium content in ammonium rhenate is an important indicator for j...

Claims

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Application Information

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IPC IPC(8): G01N21/73G01N1/38
CPCG01N1/38G01N21/73
Inventor 钱庆长吴德珍史静倪莹江玲玲
Owner TONGLING NON FERROUS METAL GROUP CORP
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