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Measurement method for uranium content in ammonium diuranate

A technology for ammonium diuranate and its determination method, which is applied in the field of determination of uranium content in ammonium diuranate, can solve the problems of time-consuming, unsuitable for large-scale sample analysis, and high risk of operation, and achieve precision and accuracy ideal effect

Inactive Publication Date: 2012-01-18
中核二七二铀业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] In the existing technology, the analysis steps are cumbersome (two times of weighing samples, two times of sample dissolution, and one operation of transferring solution), and the operation is highly dangerous (need to add dangerous chemicals such as concentrated perchloric acid, concentrated sulfuric acid and hydrofluoric acid, etc. sample), the analysis process takes a long time (continuous batch operation, it takes about 120 minutes for a skilled analyst to analyze a sample), and it is not suitable for large-scale sample analysis

Method used

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  • Measurement method for uranium content in ammonium diuranate

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Embodiment 1: Analyze No. 1 ammonium diuranate sample, and make six parallel samples.

[0030] The specific analysis steps are as follows:

[0031] (1). Put the ammonium diuranate sample in a weighing bottle, put it in an oven and bake it at 105°C for 2.0h, then take it out;

[0032] (2). Place in a desiccator to cool to room temperature, weigh 2.33-2.36g sample by subtraction method, weigh 6 parallel samples, accurate to 0.1mg, and place in a 300mL tall beaker;

[0033] (3). Add 40mL of concentrated phosphoric acid (85%) and 0.5ml of concentrated nitric acid to each weighed sample, cover with a watch glass, and place the beaker on a heating plate at low temperature (105°C) to dissolve the sample for 9 hours;

[0034] (4). After the sample is dissolved and clarified, remove it and cool it to room temperature, pipette 5mL of sulfuric acid solution (1+1 sulfuric acid solution) to wash the watch glass;

[0035] (5). Put the beaker on a magnetic stirrer, under stirri...

Embodiment 2

[0045] Embodiment 2: A standard sample of U3O8 was added to the ammonium diuranate sample to perform a recovery experiment to test the accuracy of the method, and 8 parallel samples were analyzed.

[0046] The specific analysis steps are as follows:

[0047] (1). Put the ammonium diuranate sample in a weighing bottle, put it in an oven and bake it at 105°C for 2.0h, then take it out;

[0048] (2). Place in a desiccator to cool to room temperature, weigh 2.33 to 2.36 g of samples by the subtraction method, accurate to 0.1 mg, place them in a 300mL tall beaker, and weigh 8 samples;

[0049] (3). Weigh 0.00-0.30 g of U3O8 standard sample by the addition method, and add it to the 6 ammonium diuranate samples;

[0050] (4). Add 40mL of concentrated phosphoric acid and 0.5ml of concentrated nitric acid to each sample, cover with a watch glass, place the beaker on a heating plate and heat at low temperature (110°C) to dissolve the sample for 10h;

[0051] (5). After the sample...

Embodiment 3

[0061] Embodiment 3: Analyze No. 2 ammonium diuranate sample, and make 6 parallel samples.

[0062] The specific analysis steps are as follows:

[0063] (1). Put the ammonium diuranate sample in a weighing bottle, put it in an oven and bake it at 105°C for 2.0h, then take it out;

[0064] (2). Place in a desiccator to cool to room temperature, weigh 2.33-2.36g sample by subtraction method, weigh 6 parallel samples, accurate to 0.1mg, and place in a 300mL tall beaker;

[0065] (3). Add 40mL of concentrated phosphoric acid (85%) and 0.5ml of concentrated nitric acid to each weighed sample, cover with a watch glass, and place the beaker on a heating plate at low temperature (105°C) to dissolve the sample for 8.5h;

[0066] (4). After the sample is dissolved and clarified, remove it and cool it to room temperature, pipette 5mL of sulfuric acid solution (1+1 sulfuric acid solution) to wash the watch glass;

[0067] (5). Put the beaker on a magnetic stirrer, under stirring, a...

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Abstract

The invention discloses a measurement method for uranium content in ammonium diuranate. The method mainly comprises the following steps of: placing an ammonium diuranate sample in a baking box to bake for 2.0 hours and then taking the sample out; placing the ammonium diuranate sample in a dryer to be cooled to room temperature; placing a beaker on an electric heating plate to dissolve at a low temperature; adding sulfamic acid solution to wash the wall of the beaker; directly adding ferrous sulfate solution and stirring; placing the beaker in a water bath; adjusting the temperature of the water bath to be 30-35 DEG C; adding oxidant solution along the inner wall of the beaker; continuously stirring and standing to diminish foams; adding vanadyl sulfate and deionized water; adding standard potassium dichromate solid into sample solution; inputting sample weight and weight of added standard potassium dichromate solid into a computer titration software interface; and automatically calculating percentage content of uranium in the sample by a computer according to an automatic potentiometric titrimeter. The method is easy, safe and quick in analytical operation and is extremely suitable for large-batch sample analysis of enterprises.

Description

technical field [0001] The invention relates to the analysis of uranium ore concentrates, in particular to a method for measuring uranium content in ammonium diuranate. Background technique [0002] Ammonium diuranate is a kind of uranium ore concentrate. At present, the domestic method for the determination of uranium in uranium ore concentrate has the national standard "GB / T 11848.1-2008: Determination of Uranium by Ferrous Sulfate Reduction-Potassium Dichromate Titration". The analytical steps of this method are: [0003] 1. Weigh 1g of sample by subtraction method, accurate to 0.1mg, and place it in a 250ml tall beaker; [0004] 2. Add 20ml of concentrated sulfuric acid (9mol / l), 1ml of concentrated nitric acid and 3ml of concentrated perchloric acid, cover with a watch glass, and heat to smoke; [0005] 3. Take it off, add 2ml of hydrofluoric acid after cooling to room temperature, and heat until the sample is completely dissolved; [0006] 4. Take it off, transf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16
Inventor 周峰杨理琼唐世根刘栋李海唐淑萍李洪唐枫
Owner 中核二七二铀业有限责任公司
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