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Analysis and detection method for uranium content in natural triuranium octaoxide

A technology for the detection of U3O8 and its detection method, which is applied in the field of analysis and detection of uranium content in natural U3O8, and can solve the complex volume calculation process of potassium dichromate solution, which is not suitable for large-scale sample analysis and analysis process operation Complicated and other issues, to improve the security of the analysis, easy to operate, and improve the efficiency of the analysis

Pending Publication Date: 2022-04-12
中核二七二铀业有限责任公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The operation of the analysis process is complicated, there are human errors in the end point control, and the calculation process of the volume of potassium dichromate solution consumed is complicated, so it is not suitable for large-scale sample analysis

Method used

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  • Analysis and detection method for uranium content in natural triuranium octaoxide
  • Analysis and detection method for uranium content in natural triuranium octaoxide
  • Analysis and detection method for uranium content in natural triuranium octaoxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Analyze the No. 1 U3O8 sample, make 6 parallel samples, and calculate the relative standard deviation RSD of the precision of the method.

[0035] The specific analysis steps are as follows:

[0036] (1) Weigh 2.0g of the sample, accurate to 0.1mg, and place it in a 300mL tall beaker; add 40mL of concentrated phosphoric acid and 0.5mL of concentrated nitric acid, shake to mix the sample and acid solution; cover the watch glass, and put the beaker Put it on a hot plate and heat to dissolve the sample at (130±2)°C.

[0037] (2) After the sample is dissolved, remove it and cool it to room temperature; take 5mL of 1+1 sulfuric acid solution to wash the watch glass. Put a magnetic stirring bar, place the beaker on the magnetic stirrer, under stirring, take 5mL of 150g / L sulfamic acid solution and add it along the wall of the cup, add 17mL of 280g / L ferrous sulfate solution, and stir for 1.5min.

[0038] When adding ferrous sulfate solution, it should be added directly to t...

Embodiment 2

[0051] Two inspectors in laboratory A and B independently measure the same U3O8 sample, each of them weighs 6 parallel samples, and performs indoor repetitive experiments according to the same operation.

[0052] The specific analysis steps are as follows:

[0053] (1) Weigh 2.0g of the sample, accurate to 0.1mg, and place it in a 300mL tall beaker; add 40mL of concentrated phosphoric acid and 0.5mL of concentrated nitric acid, shake to mix the sample and acid solution; cover the watch glass, and put the beaker Put it on a hot plate and heat to dissolve the sample at (130±2)°C.

[0054] (2) After the sample is dissolved, remove it and cool it to room temperature; take 5mL of 1+1 sulfuric acid solution to wash the watch glass. Put a magnetic stirring bar, place the beaker on the magnetic stirrer, under stirring, take 5mL of 150g / L sulfamic acid solution and add it along the wall of the cup, add 17mL of 280g / L ferrous sulfate solution, and stir for 1.5min.

[0055] Note: When ...

Embodiment 3

[0069] This method was compared with the national standard "GB / T 11848.1 Determination of uranium in uranium ore concentrate---ferrous sulfate reduction / potassium dichromate oxidation titration method", and the same person measured 6 parallel samples.

[0070] The specific analysis steps are as follows:

[0071] (1) Weigh 2.0g of the sample, accurate to 0.1mg, and place it in a 300mL tall beaker; add 40mL of concentrated phosphoric acid and 0.5mL of concentrated nitric acid, shake to mix the sample and acid solution; cover the watch glass, and put the beaker Put it on a hot plate and heat to dissolve the sample at (130±2)°C.

[0072] (2) After the sample is dissolved, remove it and cool it to room temperature; take 5mL of 1+1 sulfuric acid solution to wash the watch glass. Put a magnetic stirring bar, place the beaker on the magnetic stirrer, under stirring, take 5mL of 150g / L sulfamic acid solution and add it along the wall of the cup, add 17mL of 280g / L ferrous sulfate solu...

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Abstract

The invention belongs to the technical field of uranium mining and metallurgy analysis and detection, and particularly relates to an analysis and detection method for uranium content in natural triuranium octaoxide. The method comprises the following steps: weighing a triuranium octoxide sample, adding phosphoric acid and nitric acid, and dissolving at low temperature; adding a sulfuric acid solution to clean the watch glass, adding a sulfamic acid solution to wash the cup wall, directly adding a ferrous sulfate solution, and stirring; adding an oxidant solution along the inner wall of the beaker; adding a vanadyl sulfate solution; the method comprises the following steps: adding a potassium dichromate standard substance solid into a sample solution, titrating with a 10g / L potassium dichromate standard solution to a termination potential, automatically switching to a 0.6 g / L potassium dichromate standard solution, titrating to an excessive amount, carrying out first-order derivative data processing on a titration curve by automatic potentiometric titrator software to obtain a titration end-point potential, and determining the titration end-point potential according to the titration end-point potential. And calculating the percentage content of uranium in the sample according to the consumed potassium dichromate solid and the two potassium dichromate standard solutions. The method is simple, safe, rapid and automatic in analysis operation, and is very suitable for large-batch sample analysis of enterprises.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection of uranium mining and metallurgy, and in particular relates to an analysis and detection method of uranium content in natural U3O8. Background technique [0002] Natural U3O8 is an important uranium ore concentrate. At present, the national standard for the determination of uranium content in U3O8 is the national standard "GB / T 11848.1-2008: Analytical Methods for Uranium Ore Concentrate Part 1: Ferrous Sulfate Reduction - Determination of Uranium by Potassium Dichromate Titration". [0003] In the prior art, the sample is dissolved in two stages, and two highly dangerous chemical reagents, perchloric acid and hydrofluoric acid, are used. After the sample is dissolved, it is necessary to weigh and divide the sample solution again. Manual titration, and finally manual calculation of the results. The operation of the analysis process is complicated, there are human errors in the end...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N1/38G01N1/44G01N21/78G01N31/16
Inventor 周峰杨理琼吴敏刘栋陈洁彭海英王婷婷
Owner 中核二七二铀业有限责任公司
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