CN112710776A - Oxidation-reduction titration detection method for uranium content in uranium tetrachloride - Google Patents
Oxidation-reduction titration detection method for uranium content in uranium tetrachloride Download PDFInfo
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Abstract
The invention belongs to the technical field of titration detection methods, and particularly relates to an oxidation-reduction titration detection method for uranium content in uranium tetrachloride, which comprises the steps of firstly, storing and weighing samples, secondly, dissolving the samples, thirdly, adding reagents, fourthly, titrating the samples, fifthly, calculating results; the invention establishes an oxidation-reduction titration detection method for uranium content in uranium tetrachloride, and the uranium content in the uranium tetrachloride can be accurately determined by using experimental conditions listed in the content of the invention, and the determination precision of the method is superior to 0.6%. The method can be used for determining the uranium content in the uranium tetrachloride, and is effectively matched with the special production.
Description
Technical Field
The invention belongs to the technical field of titration detection methods, and particularly relates to an oxidation-reduction titration detection method for uranium content in uranium tetrachloride.
Background
The uranium tetrachloride is chloride with the oxidation state of uranium being +4, can be used for separating electromagnetic elements in the uranium enrichment process, and is also a main raw material of organic uranium chemistry. Can be obtained by reacting uranium dioxide with a chlorinating agent under appropriate conditions.
At present, the standard of uranium content determination in uranium tetrachloride is temporarily absent, and the current detection method of the uranium content in uranium tetrafluoride is that concentrated phosphoric acid and potassium dichromate are used for dissolving a sample, uranium (VI) is reduced to uranium (IV) by using excessive ferrous sulfate in a concentrated phosphoric acid medium, the excessive ferrous sulfate is oxidized by nitric acid by using molybdenum (VI) as a catalyst, vanadyl sulfate is added, the uranium (IV) to the uranium (VI) are titrated by using a potassium dichromate standard solution, and the titration end point is determined by a potentiometric method.
The sample storage mode, the sample weighing mode and the sample dissolving mode of the method are not suitable for determining the uranium content in the uranium tetrachloride.
Disclosure of Invention
In view of the above disadvantages, the present invention aims to provide a method for detecting uranium tetrafluoride in uranium tetrachloride by redox titration, which is suitable for detecting the uranium content in uranium tetrafluoride, wherein uranium tetrafluoride is stable in nature in air and insoluble in water, uranium tetrachloride has strong hygroscopicity, is easy to deliquesce and is easy to dissolve in water, and storage, weighing, dissolving methods and detection conditions of a uranium tetrafluoride sample in the existing method are not suitable for the uranium tetrachloride sample.
The technical scheme of the invention is as follows:
a redox titration detection method for uranium tetrachloride uranium content comprises a first step of storing and weighing samples, a second step of dissolving the samples, a third step of adding reagents, a fourth step of titrating the samples, and a fifth step of calculating results;
step one, sample storage and weighing, including sample storage and sample weighing;
step two, sample dissolution
Adding 1-3mL of deionized water along the wall of a beaker, adding 5mL of concentrated nitric acid, heating and dissolving on an electric heating plate at 180 ℃, adding 1-3mL of deionized water and 5mL of concentrated nitric acid again after the solution is evaporated to dryness, repeatedly evaporating to dryness for three times, adding 30mL of concentrated phosphoric acid along the wall of the beaker, covering a watch glass, heating and dissolving on the electric heating plate, frequently shaking the beaker during the process, and dissolving the sample for 40-50min to completely dissolve the sample; taking down the beaker after complete dissolution, and cooling to room temperature;
step three, adding a reagent;
placing the dissolved sample solution on an electromagnetic stirrer, adding a stirrer, vertically adding 4.0mL of ferrous sulfate solution under stirring, inserting a thermometer, and reducing for at least 2 min; regulating the temperature of the solution to 35 +/-2 ℃, and sequentially adding 5mL of sulfuric acid solution, 5mL of sulfamic acid solution and 6mL of oxidant solution, wherein the solution is changed from light green to brown and then light green; continuing stirring for 2.5min, standing for 0.5min, adding 10mL vanadium sulfate acyl solution, and adding 90mL deionized water along the cup wall;
step four, titrating the sample;
inserting an electrode, stirring, keeping the potential at 350-400 mV, weighing the mass of a titration flask filled with a potassium dichromate A solution with the concentration of 9.7mg/g before titration, and accurately measuring the mass to 0.1mg, and dripping the potassium dichromate A solution from the titration flask to the potential of 450-480 mV; recording the mass of a titration bottle filled with the potassium dichromate A solution after titration is finished, and accurately measuring the mass to 0.1 mg;
continuously dropwise adding 0.5mg/mL potassium dichromate B solution into a 2mL micro burette, adding 0.10mL each time, after dropwise adding the B solution each time, washing the end part of the burette with water, and recording a potential value and a corresponding volume reading when the potential reading does not change more than 1mV within 5 s; dripping until the potential change is maximum, dripping 0.10mL of B solution after the potential exceeds the end point, and recording the corresponding potential value; calculating the volume V of the solution of the potassium dichromate B consumed by reaching an equivalent point by second-order derivative;
step five, calculating results;
measuring result of uranium content in sample by mass fraction WUExpressed in percent (%) and calculated according to formula (1):
in the formula:
ρa-mass fraction of potassium dichromate a solution in milligrams per gram (mg/g);
m5——m5＝m6-m7the titration amount of the potassium dichromate a solution is in grams (g);
m6the mass of a titration flask filled with the potassium dichromate A solution before titration is in grams (g);
m7the mass of the titration flask filled with the potassium dichromate A solution after titration is in gram (g);
ρb-the concentration of potassium dichromate B solution in milligrams per milliliter (mg/mL);
v — volume of potassium dichromate B solution consumed at endpoint in milliliters (mL);
k-conversion factor of potassium dichromate to natural uranium (K-2.4273);
g-enrichment factor for uranium-the relative atomic weight of uranium in the sample/238.029;
m4mass of sample in grams (g).
And storing the samples, namely placing a weighing bottle with the specification of 25mm multiplied by 40mm in an oven to be dried for 1h at 100 ℃, cooling and transferring to a dryer, quickly placing the uranium tetrachloride samples to be analyzed into the weighing bottle after sampling is finished, placing the weighing bottle into the dryer for temporary storage, and detecting the samples stored in the weighing bottle stored in the dryer at the first time after the preparation work before detection is finished.
And weighing 0.19900-0.20100 g of sample by a weight reduction method, accurately measuring the sample to 0.01mg, and recording the actual mass.
Putting a high waist beaker with the sample dissolved on a balance plate, peeling, putting a weighing bottle and the sample on another balance plate, and recording the mass m of the weighing bottle and the sample1Then taking the weighing bottle down from the balance, slowly leveling the weighing bottle above the high-waist beaker to ensure that the sample is uniformly distributed on the side wall of the weighing bottle, opening the cover of the weighing bottle, tapping the upper part of the bottle mouth by using the cover of the weighing bottle to ensure that the sample slowly falls into the high-waist beaker, and pouring out the sampleWhen the quantity of the sample is close to the required quantity, the bottle cap is used for tapping the upper part of the bottle opening, the weighing bottle is slowly erected while the bottle cap is used for tapping, the sample adhered on the bottle opening falls back into the weighing bottle, the bottle cap is quickly covered, and the mass m of the weighing bottle and the sample is weighed2(ii) a Wherein the mass of the sample is m1-m2。
In the second step, after the sample is dissolved for 40-50min, if the sample is not completely dissolved, the time can be prolonged until the sample is completely dissolved.
The invention has the beneficial effects that:
the invention establishes an oxidation-reduction titration detection method for uranium content in uranium tetrachloride, and the uranium content in the uranium tetrachloride can be accurately determined by using experimental conditions listed in the content of the invention, and the determination precision of the method is superior to 0.6%. The method can be used for determining the uranium content in the uranium tetrachloride, and is effectively matched with the special production.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A redox titration detection method for uranium tetrachloride uranium content comprises a first step of storing and weighing samples, a second step of dissolving the samples, a third step of adding reagents, a fourth step of titrating the samples, and a fifth step of calculating results;
step one, storing and weighing samples
1. Sample storage
And (3) placing a weighing bottle with the specification of 25mm multiplied by 40mm into an oven, drying for 1h at 100 ℃, cooling and transferring into a dryer, quickly placing a uranium tetrachloride sample to be analyzed into the weighing bottle after sampling, and placing the weighing bottle into the dryer for temporary storage. After the preparation before the detection is completed, the sample stored in the weighing bottle stored in the dryer is detected for the first time.
2. Sample weighing
0.19900 g-0.20100 g of sample is weighed by a decrement method, the precision is 0.01mg, and the actual mass is recorded.
Putting a high waist beaker with the sample dissolved on a balance plate, peeling, putting a weighing bottle and the sample on another balance plate, and recording the mass m of the weighing bottle and the sample1Then taking the weighing bottle down from the balance, slowly laying the weighing bottle flat above the high-waist beaker to enable the samples to be uniformly distributed on the side wall of the weighing bottle, opening the cover of the weighing bottle, tapping the upper part of the bottle opening by using the cover of the weighing bottle to enable the samples to slowly fall into the high-waist beaker, tapping the upper part of the bottle opening by using the cover of the weighing bottle while enabling the weighing bottle to be vertical when the amount of the poured samples is close to the required amount, enabling the samples adhered on the bottle opening to fall back into the weighing bottle, quickly covering the cover of the weighing bottle, and weighing the mass m of the weighing bottle and the samples2。
Wherein the mass of the sample is m1-m2。
Step two, sample dissolution
Adding 1-3mL of deionized water along the wall of a beaker, adding 5mL of concentrated nitric acid, heating and dissolving at 180 ℃ on an electric heating plate, adding 1-3mL of deionized water and 5mL of concentrated nitric acid again after the solution is evaporated to dryness, repeatedly evaporating to dryness for three times, adding 30mL of concentrated phosphoric acid along the wall of the beaker, covering a watch glass, heating and dissolving on the electric heating plate, frequently shaking the beaker during the process, and dissolving the sample for 40-50min to completely dissolve the sample. If the dissolution is incomplete, the time can be prolonged until the sample is completely dissolved. And taking down the beaker after complete dissolution and cooling to room temperature.
Step three, adding reagent
And (3) placing the dissolved sample solution on an electromagnetic stirrer, adding a stirrer, vertically adding 4.0mL of ferrous sulfate solution under the stirring condition, inserting a thermometer, and reducing for not less than 2 min. The temperature of the solution is adjusted to 35 +/-2 ℃, 5mL of sulfuric acid solution, 5mL of sulfamic acid solution and 6mL of oxidant solution are added in sequence, and the solution is changed from light green to brown and then light green. After stirring for 2.5min, standing for 0.5min, adding 10mL vanadyl sulfate solution, and adding 90mL deionized water along the cup wall.
Step four, sample titration
Inserting an electrode, stirring, keeping the potential at 350-400 mV, weighing the mass of a titration flask filled with a potassium dichromate A solution with the concentration of 9.7mg/g before titration, and accurately measuring the mass to 0.1mg, and dripping the potassium dichromate A solution from the titration flask to the potential of 450-480 mV; and recording the mass of the titration flask filled with the potassium dichromate A solution after titration is finished, and accurately measuring the mass to 0.1 mg.
And continuously dropwise adding 0.5mg/mL potassium dichromate B solution into a 2mL micro burette, adding 0.10mL of the solution B each time, washing the end part of the burette with water after dropwise adding the solution B each time, and recording a potential value and a corresponding volume reading when the potential reading does not change more than 1mV within 5 s. Dropping the solution until the potential changes to the maximum, dropping 0.10mL of B solution after the potential exceeds the end point, and recording the corresponding potential value. The volume V of potassium dichromate B solution consumed to reach the equivalence point was calculated as the second derivative.
Step five, calculating the result
Measuring result of uranium content in sample by mass fraction WUExpressed in percent (%) and calculated according to formula (1):
in the formula:
ρa-mass fraction of potassium dichromate a solution in milligrams per gram (mg/g);
m5——m5＝m6-m7the titration amount of the potassium dichromate a solution is in grams (g);
m6the mass of a titration flask filled with the potassium dichromate A solution before titration is in grams (g);
m7the mass of the titration flask filled with the potassium dichromate A solution after titration is in gram (g);
ρbconcentration of the potassium dichromate B solutionIn milligrams per milliliter (mg/mL);
v — volume of potassium dichromate B solution consumed at endpoint in milliliters (mL);
k-conversion factor of potassium dichromate to natural uranium (K-2.4273);
g-enrichment factor for uranium-the relative atomic weight of uranium in the sample/238.029;
m4mass of sample in grams (g).
The precision after using the method is as follows:
6 parts of the same sample are weighed respectively, analyzed according to the method, and subjected to precision experiments, and the results are shown in table 1.
TABLE 1 precision test
In the drawings of the disclosed embodiments of the invention, only methods related to the disclosed embodiments are referred to, other methods can refer to common design, and the same embodiment and different embodiments of the invention can be combined with each other without conflict;
the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that are within the spirit and principle of the present invention are intended to be included in the scope of the present invention.
Claims (7)
1. A redox titration detection method for uranium tetrachloride uranium content comprises a first step of storing and weighing samples, a second step of dissolving the samples, a third step of adding reagents, a fourth step of titrating the samples, and a fifth step of calculating results; the method is characterized in that:
step one, sample storage and weighing, including sample storage and sample weighing;
step two, sample dissolution
Adding 1-3mL of deionized water along the wall of a beaker, adding 5mL of concentrated nitric acid, heating and dissolving on an electric heating plate at 180 ℃, adding 1-3mL of deionized water and 5mL of concentrated nitric acid again after the solution is evaporated to dryness, repeatedly evaporating to dryness for three times, adding 30mL of concentrated phosphoric acid along the wall of the beaker, covering a watch glass, heating and dissolving on the electric heating plate, frequently shaking the beaker during the process, and dissolving the sample for 40-50min to completely dissolve the sample; taking down the beaker after complete dissolution, and cooling to room temperature;
step three, adding a reagent;
placing the dissolved sample solution on an electromagnetic stirrer, adding a stirrer, vertically adding 4.0mL of ferrous sulfate solution under stirring, inserting a thermometer, and reducing for at least 2 min; regulating the temperature of the solution to 35 +/-2 ℃, and sequentially adding 5mL of sulfuric acid solution, 5mL of sulfamic acid solution and 6mL of oxidant solution, wherein the solution is changed from light green to brown and then light green; continuing stirring for 2.5min, standing for 0.5min, adding 10mL vanadium sulfate acyl solution, and adding 90mL deionized water along the cup wall;
step four, titrating the sample;
inserting an electrode, stirring, keeping the potential at 350-400 mV, weighing the mass of a titration flask filled with a potassium dichromate A solution with the concentration of 9.7mg/g before titration, and accurately measuring the mass to 0.1mg, and dripping the potassium dichromate A solution from the titration flask to the potential of 450-480 mV; recording the mass of a titration bottle filled with the potassium dichromate A solution after titration is finished, and accurately measuring the mass to 0.1 mg;
continuously dropwise adding 0.5mg/mL potassium dichromate B solution into a 2mL micro burette, adding 0.10mL each time, after dropwise adding the B solution each time, washing the end part of the burette with water, and recording a potential value and a corresponding volume reading when the potential reading does not change more than 1mV within 5 s; dripping until the potential change is maximum, dripping 0.10mL of B solution after the potential exceeds the end point, and recording the corresponding potential value; calculating the volume V of the solution of the potassium dichromate B consumed by reaching an equivalent point by second-order derivative;
step five, calculating results;
measuring result of uranium content in sample by mass fraction WUExpressed in percent (%) and calculated according to formula (1):
in the formula:
ρa-mass fraction of potassium dichromate a solution in milligrams per gram (mg/g);
m5——m5＝m6-m7the titration amount of the potassium dichromate a solution is in grams (g);
m6the mass of a titration flask filled with the potassium dichromate A solution before titration is in grams (g);
m7the mass of the titration flask filled with the potassium dichromate A solution after titration is in gram (g);
ρb-the concentration of potassium dichromate B solution in milligrams per milliliter (mg/mL);
v — volume of potassium dichromate B solution consumed at endpoint in milliliters (mL);
k-conversion factor of potassium dichromate to natural uranium (K-2.4273);
g-enrichment factor for uranium-the relative atomic weight of uranium in the sample/238.029;
m4mass of sample in grams (g).
2. The redox titration detection method for uranium content in uranium tetrachloride according to claim 1, characterized in that: and storing the samples, namely placing a weighing bottle with the specification of 25mm multiplied by 40mm in an oven to be dried for 1h at 100 ℃, cooling and transferring to a dryer, quickly placing the uranium tetrachloride samples to be analyzed into the weighing bottle after sampling is finished, placing the weighing bottle into the dryer for temporary storage, and detecting the samples stored in the weighing bottle stored in the dryer at the first time after the preparation work before detection is finished.
3. The redox titration detection method for uranium content in uranium tetrachloride according to claim 1, characterized in that: and weighing 0.19900-0.20100 g of sample by a weight reduction method, accurately measuring the sample to 0.01mg, and recording the actual mass.
4. The redox titration detection method for uranium content in uranium tetrachloride according to claim 3, characterized in that: putting a high waist beaker with the sample dissolved on a balance plate, peeling, putting a weighing bottle and the sample on another balance plate, and recording the mass m of the weighing bottle and the sample1Then taking the weighing bottle down from the balance, slowly laying the weighing bottle flat above the high-waist beaker to enable the samples to be uniformly distributed on the side wall of the weighing bottle, opening the cover of the weighing bottle, tapping the upper part of the bottle opening by using the cover of the weighing bottle to enable the samples to slowly fall into the high-waist beaker, tapping the upper part of the bottle opening by using the cover of the weighing bottle while enabling the weighing bottle to be vertical when the amount of the poured samples is close to the required amount, enabling the samples adhered on the bottle opening to fall back into the weighing bottle, quickly covering the cover of the weighing bottle, and weighing the mass m of the weighing bottle and the samples2(ii) a Wherein the mass of the sample is m1-m2。
5. The redox titration detection method for uranium content in uranium tetrachloride according to claim 1, characterized in that: in the second step, after the sample is dissolved for 40-50min, if the sample is not completely dissolved, the time can be prolonged until the sample is completely dissolved.
6. The redox titration detection method for uranium content in uranium tetrachloride according to claim 1, characterized in that: the sample storage comprises the steps of placing a weighing bottle with the specification of 25mm multiplied by 40mm in an oven to be dried for 1h at 100 ℃, cooling and transferring to a dryer, quickly placing a uranium tetrachloride sample to be analyzed into the weighing bottle after sampling is finished, placing the weighing bottle into the dryer for temporary storage, and detecting the sample stored in the weighing bottle stored in the dryer at the first time after preparation work before detection is finished;
and weighing 0.19900-0.20100 g of sample by a weight reduction method, accurately measuring the sample to 0.01mg, and recording the actual mass.
7. The redox titration detection method for uranium content in uranium tetrachloride according to claim 6, characterized in that: balancePutting a high waist beaker with the sample dissolved on a balance plate, peeling, putting a weighing bottle and the sample on another balance plate, and recording the mass m of the weighing bottle and the sample1Then taking the weighing bottle down from the balance, slowly laying the weighing bottle flat above the high-waist beaker to enable the samples to be uniformly distributed on the side wall of the weighing bottle, opening the cover of the weighing bottle, tapping the upper part of the bottle opening by using the cover of the weighing bottle to enable the samples to slowly fall into the high-waist beaker, tapping the upper part of the bottle opening by using the cover of the weighing bottle while enabling the weighing bottle to be vertical when the amount of the poured samples is close to the required amount, enabling the samples adhered on the bottle opening to fall back into the weighing bottle, quickly covering the cover of the weighing bottle, and weighing the mass m of the weighing bottle and the samples2(ii) a Wherein the mass of the sample is m1-m2。
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