CN112710779B - EDTA titration detection method for gadolinium oxide content in uranium dioxide containing gadolinium - Google Patents
EDTA titration detection method for gadolinium oxide content in uranium dioxide containing gadolinium Download PDFInfo
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- CN112710779B CN112710779B CN202011345565.5A CN202011345565A CN112710779B CN 112710779 B CN112710779 B CN 112710779B CN 202011345565 A CN202011345565 A CN 202011345565A CN 112710779 B CN112710779 B CN 112710779B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Abstract
The invention belongs to the technical field of chemical detection, and particularly relates to an EDTA titration detection method for gadolinium oxide content in gadolinium-containing uranium dioxide, which comprises the steps of preparing and weighing a sample, dissolving the sample, separating uranium, controlling acidity and titrating a solution, and fifthly, and Fe 3+ Eliminating interference, namely calculating a result; the method is superior to 1% in precision by selecting the weighing amount, the dissolution experiment of the sample, the separation experiment of uranium, the control of acidity, the selection of the addition amount of buffer solution, the experimental ratio and the like, and counting 1.0g of gadolinium-containing uranium dioxide sample. The method is accurate and reliable, and meets the technical index requirement of the project analysis. The method greatly improves the precision of the detection result, has relatively simple process, and can meet the experimental requirements of accuracy and precision.
Description
Technical Field
The invention belongs to the technical field of chemical detection, and particularly relates to an EDTA titration detection method for gadolinium oxide content in gadolinium-containing uranium dioxide.
Background
The gadolinium-containing uranium dioxide is used as an emerging nuclear fuel, has been widely applied to nuclear products, but only an X fluorescence method is searched in domestic literature on measuring the content of gadolinium oxide in the gadolinium-containing uranium dioxide at present, a related chemical detection method is not found, even a chemical analysis method of gadolinium element is seldom referred to, and a EDTA titration detection method for the content of gadolinium oxide in the gadolinium-containing uranium dioxide is finally established through researches of a large number of conditional experiments.
In the measurement of gadolinium oxide, an analysis method such as atomic absorption spectrometry, atomic emission spectrometry, or inductively coupled plasma mass spectrometry is generally used depending on the amount of gadolinium in a sample and the properties of the sample.
The instrument analysis method is generally higher in detection precision of low-content elements, and the detection precision of the constant analysis method cannot meet the detection precision requirement; the instrument analysis method has the advantages of smaller sample weighing amount, relatively poor representativeness, larger result error and incapability of meeting the precision manufacturing requirement of the existing uranium dioxide nuclear fuel.
Disclosure of Invention
Aiming at the defects, the invention aims to provide the EDTA titration detection method for the gadolinium oxide content in the uranium dioxide containing gadolinium, and the EDTA titration detection method for the gadolinium oxide content in the uranium dioxide containing gadolinium is established, wherein the gadolinium oxide content is determined to be 5% -10% from the range, so that the requirements of scientific research and production detection are met.
The technical scheme of the invention is as follows:
a EDTA titration detection method for gadolinium oxide content in gadolinium-containing uranium dioxide comprises the steps of preparing and weighing a sample, dissolving the sample, separating uranium, controlling acidity and titrating a solution, and fifth and Fe 3+ Eliminating interference, namely calculating a result;
step one, preparing and weighing a sample;
the uranium dioxide pellets containing gadolinium are required to be ground and sieved, the granularity is smaller than 154 mu m, and the uranium dioxide pellets are stored in a dry and clean polyethylene bottle, and the sample weighing amount is 1.0g and is accurate to 0.0001g;
step two, dissolving a sample;
dissolving a sample by using a hydrochloric acid (1+1) solution;
when 10mL of hydrochloric acid (1+1) is added, the sample is completely dissolved, and the solution is bright yellow, which indicates that uranium is completely converted into uranyl nitrate, heating is continued, the temperature is controlled at 200-250 ℃, the solution is heated and evaporated until the solution is taken down when the solution is 1-1.5 mL, and then cooling is carried out to room temperature;
step three, separating uranium;
separating and removing uranium by using TBP as an extractant, selecting dimethylbenzene as a diluent, and mixing the materials according to TBP: xylene = 1:3, mixing the materials in a nitric acid system of 5.0 to 5.5mol/L; v (V) Water and its preparation method ：V Has the following components According to the following steps of 1:2, extracting for two times according to a 1g sample weighing meter to separate 99.99% uranium;
step four, controlling acidity and titrating the solution;
the acidity is controlled to be pH=5-6, hydrochloric acid-hexamethylenetetramine is selected as a buffer solution, and the volume of the buffer solution is 5mL; adding 1 drop of methyl orange indicator into a conical flask, regulating the solution to turn yellow by using ammonia water and hydrochloric acid, and adding 5mL of hexamethylenetetramine buffer solution; adding 2 drops of xylenol orange indicator, and titrating with EDTA until the solution changes from red to yellow to obtain a titration end point;
step five, fe 3+ Interference cancellation
If the sample contains Fe 3+ At higher content, adding ascorbic acid to obtain Fe 3+ Adding aminosalicylic acid to mask after reduction;
step six, calculating the result
The content of gadolinium oxide in the sample is expressed in percentage (%) by mass fraction W, and is calculated according to formula (1):
wherein:
w is the mass fraction of gadolinium oxide in the sample, and the unit is percentage content (%);
C EDTA -calibrated EDTA concentration in moles per liter (mol/L);
V EDTA EDTA volume is consumed in milliliters (mL)
m-weighing the mass (g) of the sample;
0.8674 the mass fraction of gadolinium in gadolinium oxide;
the calculation results retain the last two bits of the decimal point.
In the second step, the heating temperature of the electric heating plate is 200 ℃.
In the second step, 5mL of hydrochloric acid solution was added.
And step three, TBP is in the range of 29% -31%.
And step three, transferring the dissolved solution to a separating funnel containing 10mL of extractant by using 5.5mol/L nitric acid solution.
Step five, when Fe in the sample 3+ The content is more than 0.02%, ascorbic acid is added into the conical flask, and then aminosalicylic acid is added.
The content of gadolinium oxide in the uranium dioxide is 8+/-1%.
The invention has the beneficial effects that:
the invention successfully establishes the EDTA titration detection method for the gadolinium oxide content in the uranium dioxide containing gadolinium, can accurately measure the gadolinium oxide content in the uranium dioxide containing gadolinium by utilizing the experimental conditions listed in the invention content, reports accurate detection data, and effectively matches with the special production.
The method is superior to 1% in precision by selecting the weighing amount, the dissolution experiment of the sample, the separation experiment of uranium, the control of acidity, the selection of the addition amount of buffer solution, the experimental ratio and the like, and counting 1.0g of gadolinium-containing uranium dioxide sample. The method is accurate and reliable, and meets the technical index requirement of the project analysis.
The method greatly improves the precision of the detection result, has relatively simple process, and can meet the experimental requirements of accuracy and precision.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
An EDTA titration detection method for gadolinium oxide content in uranium dioxide containing gadolinium, which comprises the following steps:
step one, sample preparation and weighing
The uranium dioxide pellets containing gadolinium are required to be ground and sieved, the granularity is smaller than 154 mu m, and the uranium dioxide pellets are stored in a dry and clean polyethylene bottle, and the sample weighing amount is 1.0g and is accurate to 0.0001g;
the method has the advantages that the gadolinium oxide content in the uranium dioxide containing gadolinium is 8+/-1%, the method belongs to constant analysis, the sample weighing amount is not too small, the method is representative and cannot be too large, the larger the sample weighing amount is, the slower the dissolution speed is, the dissolution difficulty is increased, the larger sample weighing amount can cause complicated uranium separation process due to high uranium matrix content, and the risk of solution loss is increased in the process, so that the accuracy of a detection result is influenced.
Step two, dissolving the sample
The uranium and gadolinium are dissolved in nitric acid and hydrochloric acid, the reaction speed of dissolution in hydrochloric acid (1+1) solution is high, and the dissolution is sufficient.
When 10mL of hydrochloric acid (1+1) is added, the sample is completely dissolved, and the solution is bright yellow, which indicates that uranium is completely converted into uranyl nitrate, heating is continued, the temperature is controlled at 200-250 ℃, the solution is heated and evaporated until the solution is taken down at 1-1.5 mL, and then the solution is cooled to room temperature. If too much sample solution is left, the acidity will be increased, which is unfavorable for the separation of uranium in later stage.
Step three, uranium separation
The metal uranium in the sample containing gadolinium uranium dioxide and EDTA can also produce complex reaction, if direct titration is carried out, the judgment of the titration end point color is not facilitated, and the detection result is lower. According to the method, TBP is used as an extractant to separate and remove uranium, when the TBP is 29% -31%, the extraction effect of the TBP on uranium is optimal, xylene is used as a diluent, and the TBP is used as follows: xylene = 1:3, and when the nitric acid system is 5.0-5.5 mol/L, the extraction rate of uranium can reach more than 98%. V (V) Water and its preparation method ：V Has the following components According to the following steps of 1:2, extracting according to a sample weighing amount of 1g, and separating out 99.99% uranium after extracting twice.
Step four, acidity control and solution titration
The acidity is controlled to be pH=5-6 in the reaction condition of the method, hydrochloric acid-hexamethylenetetramine is selected as a buffer solution, and the volume of the buffer solution is 5mL; adding 1 drop of methyl orange indicator into a conical flask, regulating the solution to turn yellow by using ammonia water and hydrochloric acid, and adding 5mL of hexamethylenetetramine buffer solution; 2 drops of xylenol orange indicator were added and the solution was titrated with EDTA to the endpoint of the titration from red to yellow.
Gadolinium and EDTA react at pH=5-6, the complexation is complete, hydrochloric acid-hexamethylenetetramine is selected as buffer solution in order to control the acidity in a proper range, and the recovery rate is 95-110% when 5mL of buffer solution is added.
Step five, fe 3+ Interference cancellation
If the sample contains Fe 3+ At higher content, adding ascorbic acid to obtain Fe 3+ Reducing, adding amino salicylic acid to mask, and adding amino salicylic acid to mask Fe effectively 3+ And does not interfere with the results.
When Fe in the sample 3+ The content is more than 0.02%, a certain amount of ascorbic acid is added into the conical flask, and a certain amount of aminosalicylic acid is added.
Step six, calculating the result
The content of gadolinium oxide in the sample is expressed in percentage (%) by mass fraction W, and is calculated according to formula (1):
wherein:
w is the mass fraction of gadolinium oxide in the sample, and the unit is percentage (%).
C EDTA The nominal EDTA concentration is expressed in moles per liter (mol/L).
V EDTA EDTA volume is consumed in milliliters (mL)
m-the mass (g) of the sample is weighed.
0.8674 the mass fraction of gadolinium in gadolinium oxide.
The calculation results retain the last two bits of the decimal point.
Example 1:
step one, sample preparation and weighing
The uranium dioxide pellets containing gadolinium are subjected to grinding and sieving, the granularity is smaller than 154 mu m, and the pellets are stored in a dry and clean polyethylene bottle, and the sample weighing amount is 1.0g;
step two, dissolving the sample
1.0g of a sample is weighed, accurate to 0.0001g, 5mL of hydrochloric acid solution is added, the mixture is placed on an electric heating plate (200 ℃) for heating and dissolution, hydrogen peroxide is dripped until the mixture is a bright yellow solution, and the mixture is taken down when the mixture is steamed to the volume (1-1.5) mL and is slightly cooled for standby.
Step three, uranium separation
Transferring the dissolved solution to a separating funnel containing 10mL of extractant by using 5.5mol/L nitric acid solution, vigorously shaking, standing, transferring to a 300mL conical flask after the solution is completely layered, repeating the extraction process once, and adding water to 20mL.
Step four, acidity control and solution titration
1 drop of methyl orange indicator was added to the conical flask, the solution was adjusted to yellow with ammonia and hydrochloric acid, then 5mL of hexamethylenetetramine buffer solution was added, 2 drops of xylenol orange indicator was added, and the solution was titrated with EDTA until the solution turned from red to yellow, the titration endpoint, and the result was calculated.
Step five, fe 3+ Interference cancellation
If the sample contains Fe 3+ At higher content, adding ascorbic acid to obtain Fe 3+ Reducing, adding amino salicylic acid to mask, and adding amino salicylic acid to mask Fe effectively 3+ And does not interfere with the results.
Step six, calculating the result
The content of gadolinium oxide in the sample is expressed in percentage (%) by mass fraction W, and is calculated according to formula (1):
wherein:
w is the mass fraction of gadolinium oxide in the sample, and the unit is percentage (%).
C EDTA The nominal EDTA concentration is expressed in moles per liter (mol/L).
V EDTA EDTA volume is consumed in milliliters (mL)
m-the mass (g) of the sample is weighed.
0.8674 the mass fraction of gadolinium in gadolinium oxide.
The calculation results retain the last two bits of the decimal point.
In the disclosed embodiments of the present invention, only the methods related to the embodiments of the present disclosure are referred to, and other methods may refer to the general design, so that the same embodiment and different embodiments of the present invention may be combined with each other without collision;
the foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (6)
1. A EDTA titration detection method for gadolinium oxide content in gadolinium-containing uranium dioxide comprises the steps of preparing and weighing a sample, dissolving the sample, separating uranium, controlling acidity and titrating a solution, and fifth and Fe 3+ Eliminating interference, namely calculating a result;
the method is characterized in that:
step one, preparing and weighing a sample;
the uranium dioxide pellets containing gadolinium are required to be ground and sieved, the granularity is smaller than 154 mu m, and the uranium dioxide pellets are stored in a dry and clean polyethylene bottle, and the sample weighing amount is 1.0g and is accurate to 0.0001g;
step two, dissolving a sample;
dissolving a sample by using a hydrochloric acid (1+1) solution;
when 10mL of hydrochloric acid (1+1) is added, the sample is completely dissolved, and the solution is bright yellow, which indicates that uranium is completely converted into uranyl nitrate, heating is continued, the temperature is controlled at 200-250 ℃, the solution is heated and evaporated until the solution is taken down when the solution is 1-1.5 mL, and then cooling is carried out to room temperature;
step three, separating uranium;
separating and removing uranium by using TBP as an extractant, selecting dimethylbenzene as a diluent, and mixing the materials according to TBP: xylene = 1:3, mixing the materials in a nitric acid system of 5.0 to 5.5mol/L; v (V) Water and its preparation method ：V Has the following components According to the following steps of 1:2, extracting for two times according to a 1g sample weighing meter to separate 99.99% uranium;
step four, controlling acidity and titrating the solution;
the acidity is controlled to be pH=5-6, hydrochloric acid-hexamethylenetetramine is selected as a buffer solution, and the volume of the buffer solution is 5mL; adding 1 drop of methyl orange indicator into a conical flask, regulating the solution to turn yellow by using ammonia water and hydrochloric acid, and adding 5mL of hexamethylenetetramine buffer solution; adding 2 drops of xylenol orange indicator, and titrating with EDTA until the solution changes from red to yellow to obtain a titration end point;
step five, fe 3+ Interference cancellation
If the sample contains Fe 3+ At higher content, adding ascorbic acid to obtain Fe 3+ Adding aminosalicylic acid to mask after reduction;
step six, calculating the result
The content of gadolinium oxide in the sample is expressed in percentage (%) by mass fraction W, and is calculated according to formula (1):
wherein:
w is the mass fraction of gadolinium oxide in the sample, and the unit is percentage content (%);
C EDTA -calibrated EDTA concentration in moles per liter (mol/L);
V EDTA EDTA volume is consumed in milliliters (mL)
m-weighing the mass (g) of the sample;
0.8674 the mass fraction of gadolinium in gadolinium oxide;
the calculation result keeps two positions after the decimal point;
in the second step, the heating temperature of the electric heating plate is 200 ℃.
2. The EDTA titration detection method for the content of gadolinium oxide in uranium dioxide containing gadolinium according to claim 1, wherein the method comprises the following steps: in the second step, 5mL of hydrochloric acid solution was added.
3. The EDTA titration detection method for the content of gadolinium oxide in uranium dioxide containing gadolinium according to claim 1, wherein the method comprises the following steps: and step three, TBP is in the range of 29% -31%.
4. The EDTA titration detection method for the content of gadolinium oxide in uranium dioxide containing gadolinium according to claim 1, wherein the method comprises the following steps: and step three, transferring the dissolved solution to a separating funnel containing 10mL of extractant by using 5.5mol/L nitric acid solution.
5. The EDTA titration detection method for the content of gadolinium oxide in uranium dioxide containing gadolinium according to claim 1, wherein the method comprises the following steps: step five, when Fe in the sample 3+ The content is more than 0.02%, ascorbic acid is added into the conical flask, and then aminosalicylic acid is added.
6. An EDTA titration detection method for the content of gadolinium oxide in uranium dioxide containing gadolinium according to any of claims 1 to 5, characterized in that: the content of gadolinium oxide in the uranium dioxide is 8+/-1%.
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