Analytical method for direct determination of fluoride ion content in rare earth carbonate by fluoride ion electrode method

Abstract

The invention discloses an analytical method for directly measuring fluorine ion content in carbonic acid rare earth by using a fluorine ion electrode method, and belongs to a detection method of rare earth analysis. According to the invention, analysis on the action of perchloric acid in a distillation process, the property of a fluorine ion, a measuring principle of a fluoride ion selective electrode and the like are the basis of the analytic method, and the method is provided by taking inspection on the influence of matrix concentration, sampling dissolving manner and other aspects on measurement of the fluoride ion as an experiment orientation; the analytical method for directly measuring the fluoride ion content in the carbonic acid rare earth by using the fluorine ion electrode method is capable of removing a perchloric acid distillation link, a condition that a few of organic P507 which is clamped in the perchloric acid and the carbonic acid rare earth causes an exploding potential safety hazard is eliminated, the analysis cost is reduced, and the analysis process is stable, rapid, safe and environment-friendly.

Description

Technical field: [0001] The invention relates to an analysis method for directly measuring the fluoride ion content in rare earth carbonate by a fluoride ion electrode method, which belongs to the rare earth analysis and detection method. technical background: [0002] The level of fluoride ion content in rare earth directly affects the effect of rare earth extraction and separation. The accurate determination of fluoride ion plays a decisive role in production. However, the current national standard method GB / T16480.3-1996 uses perchloric acid distillation --- fluoride ion Both the electrode method and the industry standard perchloric acid distillation --- alizarin complex colorimetric method cannot avoid the perchloric acid distillation link. The analysis process is to add 30mL concentrated perchloric acid to control the distillation temperature at about 130°C after weighing the rare earth carbonate sample. After 50 minutes, the distillate distilled out was taken at a cons...

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Problems solved by technology

[0002] The level of fluoride ion content in rare earth directly affects the effect of rare earth extraction and separation. The accurate determination of fluoride ion plays a decisive role in production. However, the current national standard method GB / T16480.3-1996 uses perchloric acid distillation --- fluoride ion Both the electrode method and the industry standard perchloric acid distillation --- alizarin complex colorimetric method cannot avoid the perchloric acid distillation link. The analysis process is to add 30mL concentrated perchloric acid to control the distillation temperature at about 130°C after weighing the rare earth carbonate sample. After 50 minutes, the distillate distilled out was taken at a constant volume and measured with a fluoride ion electrode method or added to a colorimetric tube with alizarin complexing agent for 30 minutes and then used for colorimetry with a spectrophotometer. half an hour

This method has low analysis efficiency and high analysis cost, and cannot meet the requirement of providing timely and accurate analysis data for production.

The most important thing is that there is a great safety risk in the distillation link in the above method, that is, concentrated perchloric acid is a strong oxidant, which is prone to explosion in the high temperature process, and a small amount of organic P507 entrained in rare earth carbonate is more likely to cause explosion. Corrosion of the latex tube by strong acid will cause the leakage of perchloric acid gas, which will have a certain impact on the environment, and add a high risk factor to the analysis process. At the same time, it will use electricity and steam for nearly an hour It consumes energy and also brings potential safety hazards

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