CN112304724A - Analysis method of niobium and titanium in radioactive organic phase - Google Patents
Analysis method of niobium and titanium in radioactive organic phase Download PDFInfo
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910052758 niobium Inorganic materials 0.000 title claims abstract description 62
- 239000010955 niobium Substances 0.000 title claims abstract description 62
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000010936 titanium Substances 0.000 title claims abstract description 62
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 62
- 239000012074 organic phase Substances 0.000 title claims abstract description 37
- 238000004458 analytical method Methods 0.000 title claims abstract description 27
- 230000002285 radioactive effect Effects 0.000 title claims abstract description 25
- 238000000120 microwave digestion Methods 0.000 claims abstract description 40
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 22
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 18
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims abstract description 17
- 235000002906 tartaric acid Nutrition 0.000 claims abstract description 17
- 239000011975 tartaric acid Substances 0.000 claims abstract description 17
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 17
- 230000003595 spectral effect Effects 0.000 claims description 13
- 238000004321 preservation Methods 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 11
- 238000012360 testing method Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 230000029087 digestion Effects 0.000 claims description 7
- 239000012086 standard solution Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000005485 electric heating Methods 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 239000012498 ultrapure water Substances 0.000 claims description 4
- 238000005070 sampling Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 2
- 238000005259 measurement Methods 0.000 abstract description 6
- 238000009616 inductively coupled plasma Methods 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract 1
- 229910052770 Uranium Inorganic materials 0.000 description 5
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 238000004380 ashing Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 238000000209 wet digestion Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GMVPEJUTFFCKDK-UHFFFAOYSA-N [Nb].[U] Chemical compound [Nb].[U] GMVPEJUTFFCKDK-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002901 radioactive waste Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
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Abstract
The invention provides an analysis method of niobium and titanium in a radioactive organic phase, which is characterized in that an organic phase to be measured is digested by nitric acid, hydrofluoric acid and tartaric acid through a microwave digestion instrument, is removed and transferred, and is subjected to constant volume to a certain volume to prepare a solution to be measured, and the solution is directly fed into an inductively coupled plasma spectrometer for measurement. The method can solve the problems of difficult determination of the content of the easily-hydrolyzed elements in the radioactive organic matters, low standard recovery rate and the like, improves the stability of the analysis result, and has simple sample pretreatment and accurate analysis result.
Description
Technical Field
The invention relates to analysis of content of metal elements in an organic phase in a uranium mining and metallurgy uranium extraction process, belongs to the field of analytical chemistry, and particularly relates to an analysis method of niobium and titanium in a radioactive organic phase.
Background
In the technological process of extracting uranium from a certain uranium niobium ore in Huayang city in China, the uranium in the leachate is extracted through TBP/P204, and the impurity elements in the organic phase need to be analyzed and determined so as to avoid influencing the quality of subsequent uranium products, wherein the impurity elements mainly comprise characteristic metal elements such as niobium, titanium and the like. In the aspect of testing, testing methods such as spectrophotometry, AAS and inductively coupled plasma emission spectrometry are generally adopted. The spectrophotometry and the AAS method can only measure single elements, and the inductively coupled plasma emission spectrometry has unique advantages in measuring the content of metal ions: and simultaneously measuring a plurality of metal elements. However, the organic phase is insoluble in water, has no special organic system, cannot directly enter an instrument for measurement, and is easy to generate the problems of unstable plasma flame, carbon deposition in a rectangular tube and the like even if an organic sample injection system is provided, so that the organic phase generally needs to be pretreated and then measured.
At present, the pretreatment means for analysis and detection mainly includes a high-temperature ashing method and a wet digestion method. The high-temperature ashing method easily causes volatilization loss of elements to be measured in the ashing process. The wet digestion method mainly uses the oxidation of strong oxidizing acid or strong oxidizer to destroy the organic sample, and has the problems of volatilization loss of elements to be detected, long digestion time, high blank value caused by adding a large amount of reagent and the like, thereby influencing the accuracy of the result.
Therefore, there is an urgent need for an improved method for analyzing the content of metal elements in an organic phase.
Disclosure of Invention
The invention mainly aims to provide a method for analyzing niobium and titanium in a radioactive organic phase.
The technical scheme adopted by the invention is as follows:
a method for analyzing niobium and titanium in a radioactive organic phase, comprising the steps of:
(1) sampling: according to the content of niobium and titanium in the radioactive organic phase, using a liquid transfer device to transfer a certain amount of organic phase into a microwave digestion tank;
(2) adding a digesting agent: adding a certain volume of concentrated nitric acid, concentrated hydrofluoric acid and tartaric acid into a microwave digestion tank;
(3) microwave digestion: and (4) putting the microwave digestion tank into the microwave digestion instrument, covering the microwave digestion tank with a cover, and closing the door and the window of the digestion instrument. Setting a microwave digestion program, digesting power 800W, and first step: keeping the temperature for 10-20min at the room temperature of 150 ℃ for 4-10 min; the second step is that: keeping the temperature from 150 ℃ to 180 ℃ for 5-10min, and keeping the temperature for 10-20 min; the third step: keeping the temperature for 20-40min from 180 ℃ to 210 ℃ for 5-10 min;
(4) acid removal: after the reaction is finished, taking out the microwave digestion tank when the temperature of the microwave digestion tank is reduced to 30-50 ℃, opening the cover, placing the microwave digestion tank in an acid expeller, continuing heating at the temperature of 120-;
(5) preparing a solution to be detected: adding 1-5mL of nitric acid, slightly heating on an electric heating plate, adding 0.1-0.5mL of HF, 0.1-0.5mL of tartaric acid with the concentration of 150g/L and a small amount of high-purity water to dissolve the precipitate, cooling to room temperature, transferring into a 25mL volumetric flask, fixing the volume, shaking up, and testing;
(6) selecting an analysis spectral line: respectively selecting three analysis spectral lines of niobium and titanium, and determining an optimal analysis line;
(7) drawing a standard curve: the mass concentrations of niobium are respectively 0, 0.1, 0.2, 0.5, 1, 2 and 10mg/L, the mass concentrations of titanium are respectively 0, 0.1, 0.2, 0.5, 1, 2 and 10mg/L, and a standard curve is drawn by taking the concentrations of niobium and titanium as abscissa and the spectral intensities corresponding to the concentrations of niobium and titanium as ordinate;
(8) and (3) determination: and (4) measuring the liquid to be measured under the same condition, checking the concentrations of niobium and titanium in the liquid to be measured from the standard curve, and then calculating the concentrations of niobium and titanium in the radioactive organic phase.
Wherein the volume of the organic phase removed in the step (1) is 0.3-1 mL.
In the step (2), the volume of the concentrated nitric acid is 8mL, the volume of the concentrated hydrofluoric acid is 1mL, the concentration of the tartaric acid is 150g/L, and the volume is 0.2 mL.
In the step (3), the first step of heating is carried out for 5min, and the heat preservation time is 15 min; the second step is that the heating time is 8min, and the heat preservation time is 15 min; and the third step, the heating time is 8min, and the heat preservation time is 30 min.
And (4) reducing the temperature of the microwave digestion tank to 40 ℃, and driving up the heating temperature of the acid catcher to 150 ℃.
In the step (5), the volume of nitric acid is 1.25mL, the volume of hydrofluoric acid is 0.2mL, and the volume of tartaric acid with the concentration of 150g/L is 0.2 mL.
The analytical line of niobium in the step (6) is 269.706nm, and the analytical line of titanium is 336.121 nm.
In the step (7), the linear correlation coefficients of the curves of the niobium standard solution and the titanium standard solution are both 0.9999.
And (4) in the step (8), the working condition of the liquid to be detected during the determination is the same as that of the standard curve, and the concentration of the liquid to be detected is within the range of the standard curve.
The invention establishes an analysis method of niobium and titanium in a radioactive organic phase, and has the following advantages:
1) the pretreatment time is short;
2) the dosage of the reagent is less;
3) the digestion effect is good, and the solution after microwave digestion can directly enter an instrument for measurement;
4) the stability of the analysis result is improved, the pretreatment of the sample is simple, and the analysis result is accurate.
Drawings
FIG. 1 is a graph showing the results of a nitric acid dosage test;
FIG. 2 is a graph showing the results of a hydrofluoric acid usage test;
FIG. 3 is a graph showing the results of a tartaric acid dosage test;
FIG. 4 is a graph showing the results of the incubation time test.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
As shown in fig. 1 to 4, the present invention provides a method for analyzing niobium and titanium in a radioactive organic phase, comprising the steps of:
(1) sampling: according to the content of niobium and titanium in the radioactive organic phase, using a liquid transfer device to transfer a certain amount of organic phase into a microwave digestion tank;
(2) adding a digesting agent: adding a certain volume of concentrated nitric acid, concentrated hydrofluoric acid and tartaric acid into a microwave digestion tank;
(3) microwave digestion: and (4) putting the microwave digestion tank into the microwave digestion instrument, covering the microwave digestion tank with a cover, and closing the door and the window of the digestion instrument. Setting a microwave digestion program, digesting power 800W, and first step: keeping the temperature for 10-20min at the room temperature of 150 ℃ for 4-10 min; the second step is that: keeping the temperature from 150 ℃ to 180 ℃ for 5-10min, and keeping the temperature for 10-20 min; the third step: keeping the temperature for 20-40min from 180 ℃ to 210 ℃ for 5-10 min;
(4) acid removal: after the reaction is finished, taking out the microwave digestion tank when the temperature of the microwave digestion tank is reduced to 30-50 ℃, opening the cover, placing the microwave digestion tank in an acid expeller, continuing heating at the temperature of 120-;
(5) preparing a solution to be detected: adding 1-5mL of nitric acid, slightly heating on an electric heating plate, adding 0.1-0.5mL of HF, 0.1-0.5mL of tartaric acid with the concentration of 150g/L and a small amount of high-purity water to dissolve the precipitate, cooling to room temperature, transferring into a 25mL volumetric flask, fixing the volume, shaking up, and testing;
(6) selecting an analysis spectral line: respectively selecting three analysis spectral lines of niobium and titanium, and determining an optimal analysis line;
(7) drawing a standard curve: the mass concentrations of niobium are respectively 0, 0.1, 0.2, 0.5, 1, 2 and 10mg/L, the mass concentrations of titanium are respectively 0, 0.1, 0.2, 0.5, 1, 2 and 10mg/L, and a standard curve is drawn by taking the concentrations of niobium and titanium as abscissa and the spectral intensities corresponding to the concentrations of niobium and titanium as ordinate;
(8) and (3) determination: and (4) measuring the liquid to be measured under the same condition, checking the concentrations of niobium and titanium in the liquid to be measured from the standard curve, and then calculating the concentrations of niobium and titanium in the radioactive organic phase.
Wherein the volume of the organic phase removed in the step (1) is 0.3-1 mL.
In the step (2), the volume of the concentrated nitric acid is 8mL, the volume of the concentrated hydrofluoric acid is 1mL, and the volume of the 150g/L tartaric acid is 0.2 mL.
In the step (3), the first step of heating is carried out for 5min, and the heat preservation time is 15 min; the second step is that the heating time is 8min, and the heat preservation time is 15 min; and the third step, the heating time is 8min, and the heat preservation time is 30 min.
And (4) reducing the temperature of the microwave digestion tank to 40 ℃, and driving up the heating temperature of the acid catcher to 150 ℃.
In step (5), nitric acid (1.25 mL), hydrofluoric acid (0.2 mL), and tartaric acid (150 g/L) were added in an amount of 0.2 mL.
The analytical line of niobium in the step (6) is 269.706nm, and the analytical line of titanium is 336.121 nm.
In the step (7), the linear correlation coefficients of the curves of the niobium standard solution and the titanium standard solution are both 0.9999.
9, the working conditions of the liquid to be detected in the step (8) are the same as the working conditions of the standard curve, and the concentration of the liquid to be detected is within the range of the standard curve.
The invention establishes an analysis method of niobium and titanium in a radioactive organic phase, and has the following advantages:
1) the pretreatment time is short;
2) the dosage of the reagent is less;
3) the digestion effect is good, and the solution after microwave digestion can directly enter an instrument for measurement;
4) the stability of the analysis result is improved, the pretreatment of the sample is simple, and the analysis result is accurate.
Example 1
(1) The instrument parameters of the invention are as follows: radio frequency power 1300W; the plasma gas flow is 15L/min; auxiliary gas flow, 0.2L/min; the flow rate of the atomizer is 0.8L/min; the washing time is 1.5 min; the pump speed is 2.5 mL/min; the observation height is 15 mm; the number of repetitions was 2.
(2) Determination of microwave digestion agent: the dosage of the nitric acid is 5-10mL respectively; the dosage of hydrofluoric acid is 0.1-2.0mL respectively; the dosage of tartaric acid is 0.1-0.3mL respectively, and other conditions are unchanged. As shown in fig. 1 to 3, the optimum amount of the digesting agent was obtained by measuring niobium and titanium: the dosage of the nitric acid is 8mL, and the dosage of the hydrofluoric acid is 1 mL; the amount of tartaric acid used was 0.2 mL.
(3) As shown in fig. 4, the microwave digestion program determines: and (4) putting the microwave digestion tank into the microwave digestion instrument, covering the microwave digestion tank with a cover, and closing the door and the window of the digestion instrument. Setting a microwave digestion program, digesting power 800W, and first step: keeping the temperature for 10-20min at the room temperature of 150 ℃ for 4-10 min; the second step is that: keeping the temperature from 150 ℃ to 180 ℃ for 5-10min, and keeping the temperature for 10-20 min; the third step: keeping the temperature for 5-10min from 180 ℃ to 210 ℃ for 20-40min, and keeping other conditions unchanged. Through the measurement of niobium and titanium, an optimal microwave digestion program is obtained: the first step is heating for 5min, and the heat preservation time is 15 min; the second step is that the heating time is 8min, and the heat preservation time is 15 min; and the third step, the heating time is 8min, and the heat preservation time is 30 min.
(4) Acid-removing temperature determination: after the reaction is finished, taking out the microwave digestion tank when the temperature of the microwave digestion tank is reduced to 30-50 ℃, opening the cover, placing the microwave digestion tank in an acid expeller, continuing heating at the temperature of 120-180 ℃, and evaporating to dryness without changing other conditions. Considering the acid-expelling speed, the optimal acid-expelling temperature is determined: at 150 ℃.
(5) Determination of a dissolving agent for preparing a solution to be detected: adding 1-5mL of nitric acid, slightly heating on an electric heating plate, adding 0.1-0.5mL of HF, 0.1-0.5mL of tartaric acid with the concentration of 150g/L and a small amount of high-purity water to dissolve the precipitate, cooling to room temperature, transferring into a 25mL volumetric flask, and keeping other conditions unchanged. The best dissolving agent for preparing the solution to be tested is obtained by testing niobium and titanium: 1.25mL of nitric acid, 0.2mL of hydrofluoric acid and 0.2mL of 150g/L of tartaric acid.
(6) And (3) analyzing a spectral line to determine: three analysis spectral lines of niobium and titanium are respectively selected, and other conditions are unchanged. By measuring niobium and titanium, the optimum analysis line is determined: the analytical line of niobium is 269.706nm, and the analytical line of titanium is 336.121 nm;
(7) drawing a standard curve: the mass concentrations of niobium were 0, 0.1, 0.2, 0.5, 1, 2, and 10mg/L, respectively, the mass concentrations of titanium were 0, 0.1, 0.2, 0.5, 1, 2, and 10mg/L, respectively, and a standard curve was drawn with the concentrations of niobium and titanium as abscissa and the spectral intensities corresponding to the concentrations of niobium and titanium as ordinate, with the other conditions being unchanged. By drawing a standard curve, the titanium and niobium concentrations and the spectral intensity (cps) have a good linear relation, and the linear equation of niobium is as follows: y is 21910x +2598.3, the linear equation y of titanium is 3298x +74.1, the linear correlation coefficients of niobium and titanium are both 0.9999, and the concentration of niobium and titanium in the liquid to be detected is in the range of a standard curve;
(8) the contents of niobium and titanium in the treated solution were measured by ICP-AES, and the measurement result was 0.227mg/L for niobium and 0.712mg/L for titanium. Through a linear equation, the niobium concentration in the organic phase was calculated to be 5.68mg/L and the titanium concentration was calculated to be 17.8 mg/L.
(9) The analyzed solution is collected in a special radioactive waste liquid barrel and is treated in a centralized way.
Claims (9)
1. A method for analyzing niobium and titanium in a radioactive organic phase is characterized in that: the method comprises the following steps:
(1) sampling: according to the content of niobium and titanium in the radioactive organic phase, using a liquid transfer device to transfer a certain amount of organic phase into a microwave digestion tank;
(2) adding a digesting agent: adding a certain volume of concentrated nitric acid, concentrated hydrofluoric acid and tartaric acid into a microwave digestion tank;
(3) microwave digestion: and (4) putting the microwave digestion tank into the microwave digestion instrument, covering the microwave digestion tank with a cover, and closing the door and the window of the digestion instrument. Setting a microwave digestion program, digesting power 800W, and first step: keeping the temperature for 10-20min at the room temperature of 150 ℃ for 4-10 min; the second step is that: keeping the temperature from 150 ℃ to 180 ℃ for 5-10min, and keeping the temperature for 10-20 min; the third step: keeping the temperature for 20-40min from 180 ℃ to 210 ℃ for 5-10 min;
(4) acid removal: after the reaction is finished, taking out the microwave digestion tank when the temperature of the microwave digestion tank is reduced to 30-50 ℃, opening the cover, placing the microwave digestion tank in an acid expeller, continuing heating at the temperature of 120-;
(5) preparing a solution to be detected: adding 1-5mL of nitric acid, slightly heating on an electric heating plate, adding 0.1-0.5mL of HF, 0.1-0.5mL of tartaric acid with the concentration of 150g/L and a small amount of high-purity water to dissolve the precipitate, cooling to room temperature, transferring into a 25mL volumetric flask, fixing the volume, shaking up, and testing;
(6) selecting an analysis spectral line: respectively selecting three analysis spectral lines of niobium and titanium, and determining an optimal analysis line;
(7) drawing a standard curve: the mass concentrations of niobium are respectively 0, 0.1, 0.2, 0.5, 1, 2 and 10mg/L, the mass concentrations of titanium are respectively 0, 0.1, 0.2, 0.5, 1, 2 and 10mg/L, and a standard curve is drawn by taking the concentrations of niobium and titanium as abscissa and the spectral intensities corresponding to the concentrations of niobium and titanium as ordinate;
(8) and (3) determination: and (4) measuring the liquid to be measured under the same condition, checking the concentrations of niobium and titanium in the liquid to be measured from the standard curve, and then calculating the concentrations of niobium and titanium in the radioactive organic phase.
2. The method for analyzing niobium and titanium in a radioactive organic phase according to claim 1, wherein: the volume of the organic phase removed in the step (1) is 0.3-1 mL.
3. The method for analyzing niobium and titanium in a radioactive organic phase according to claim 1, wherein: the volume of the concentrated nitric acid in the step (2) is 8 mL; the volume of the concentrated hydrofluoric acid is 1 mL; the concentration of tartaric acid was 150g/L, and the volume was 0.2 mL.
4. The method for analyzing niobium and titanium in a radioactive organic phase according to claim 1, wherein: the first step in the step (3) is heating for 5min, and the heat preservation time is 15 min; the second step is that the heating time is 8min, and the heat preservation time is 15 min; and the third step, the heating time is 8min, and the heat preservation time is 30 min.
5. The method for analyzing niobium and titanium in a radioactive organic phase according to claim 1, wherein: and (4) reducing the temperature of the microwave digestion tank to 40 ℃, and driving up the heating temperature of the acid catcher to 150 ℃.
6. The method for analyzing niobium and titanium in a radioactive organic phase according to claim 1, wherein: in the step (5), the volume of nitric acid is 1.25mL, the volume of hydrofluoric acid is 0.2mL, and the volume of tartaric acid with the concentration of 150g/L is 0.2 mL.
7. The method for analyzing niobium and titanium in a radioactive organic phase according to claim 1, wherein: the analytical line of niobium in the step (6) is 269.706nm, and the analytical line of titanium is 336.121 nm.
8. The method for the analysis of niobium and titanium in radioactive organic phase according to claim 1, characterized in that: and (3) in the step (7), the linear correlation coefficients of the curves of the niobium standard solution and the titanium standard solution are both 0.9999.
9. The method for the analysis of niobium and titanium in radioactive organic phase according to claim 1, characterized in that: and (4) in the step (8), the working condition of the liquid to be detected during the detection is the same as that of the standard curve, and the concentration of the liquid to be detected is within the range of the standard curve.
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