CN111024463A - Preparation process of multi-element mixed standard solution for nuclear fuel analysis - Google Patents
Preparation process of multi-element mixed standard solution for nuclear fuel analysis Download PDFInfo
- Publication number
- CN111024463A CN111024463A CN201910983107.5A CN201910983107A CN111024463A CN 111024463 A CN111024463 A CN 111024463A CN 201910983107 A CN201910983107 A CN 201910983107A CN 111024463 A CN111024463 A CN 111024463A
- Authority
- CN
- China
- Prior art keywords
- standard solution
- solution
- mixed standard
- group
- prepared
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
- G01N1/34—Purifying; Cleaning
-
- 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
- G01N1/38—Diluting, dispersing or mixing samples
-
- 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
- G01N2001/2893—Preparing calibration standards
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to the technical field of nuclear fuel analysis, and particularly discloses a preparation process of a multi-element mixed standard solution for nuclear fuel analysis, which comprises the following steps: step 1: selecting raw materials; step 2: purifying raw materials; and step 3: preparing a single element standard solution with intermediate concentration; and 4, step 4: verifying the concentration of the single element standard solution; and 5: preparing a multi-element mixed standard solution; step 6: performing primary uniformity detection; and 7: and (6) subpackaging. The multi-element mixed standard solution prepared by the process has good uniformity effect and complete element types, and can meet the analysis and use requirements of impurity elements in nuclear fuel products.
Description
Technical Field
The invention belongs to the technical field of nuclear fuel analysis, and particularly relates to a preparation process of a multi-element mixed standard solution for nuclear fuel analysis.
Background
The nuclear fuel circulation relates to products such as triuranium octoxide, uranium dioxide powder, uranium dioxide pellet and uranium tetrafluoride, uranium hexafluoride, wherein there are thirty kinds of impurity elements such as Al, B, Ca, Fe, Mg, Mo, Ti, Th, V, W and need detect.
The detection method which is universal in the world and the country mainly adopts the spectrum method and the mass spectrometry method to carry out the multi-element simultaneous determination, and if the single-element standard solution is adopted to carry out calibration curve and quality control, great difficulty and unnecessary trouble are often caused to the actual work. Through the investigation of the domestic existing mixed standard solution, the existing product is found to have too little element content and only contain a plurality of common elements. Even if the product contains more elements, the contained elements still can not completely cover the range of impurity elements required to be detected by the nuclear fuel and nuclear material products in China, and the magnitude level is not consistent with the technical indexes of the nuclear fuel and nuclear material products in China.
Therefore, the development of the multi-element mixed standard solution meeting the use requirements of nuclear fuels and nuclear material products in China is very necessary.
Disclosure of Invention
The invention aims to provide a preparation process of a multi-element mixed standard solution for nuclear fuel analysis, which is used for monitoring the quantity value transfer and measuring process of impurity elements in nuclear fuel and nuclear material products in China.
The technical scheme of the invention is as follows:
a preparation process of a multi-element mixed standard solution for nuclear fuel analysis comprises the following steps:
step 1: selection of raw materials
Selecting and purchasing high-purity metal oxide or ammonium salt as a raw material;
step 2: purification of raw materials
For the high-purity reagent which cannot be purchased in the current market, the low-purity reagent needs to be purified, so that the content of impurity elements cannot cause the change of the content of main elements;
and step 3: preparation of intermediate concentration Unit element Standard solution
Preparing the raw materials selected in the step 1 and the step 2 or the purified reagent into a single element standard solution with intermediate concentration;
and 4, step 4: verification of concentration of single element standard solution
Respectively detecting the single element standard solution prepared in the step 3 by adopting an ICP-AES method or an ICP-MS method, and if the detection result is basically consistent with the theoretical preparation concentration, determining that the reagent is abnormal and meets the requirements;
if the detection result is not consistent with the theoretical preparation concentration, returning to the step 1;
and 5: preparation of Multi-element Mixed Standard solution
Preparing the single-element standard solution which meets the requirements verified in the step (4) into a multi-element mixed standard solution which meets an expected target value, and uniformly mixing;
step 6: uniformity preliminary examination
Randomly extracting samples from each group of the multi-element mixed standard solution prepared in the step 5, measuring each sample for three times, and performing uniformity initial detection by adopting a spectrum method;
then, evaluating the uniformity of the standard substance by adopting an analysis of variance method, namely an F test method, wherein the calculated F value is less than a critical value, and the sample is uniform and qualified; if the value is larger than or equal to the critical value, the sample is unqualified and can only be discarded;
and 7: dispensing
And (5) subpackaging the samples qualified in the initial inspection, covering the cover, and sealing and packaging.
In step 1, the purity of the selected raw materials and reagents is shown in table 1;
TABLE 1 raw material List
In the step 1, after preliminary detection, the content of barium ions in the selected raw material strontium nitrate is overhigh, and the content of total impurities in thorium nitrate is overhigh;
the step 2 specifically comprises the following steps:
2.1 purifying the strontium nitrate step by adopting a precipitation method;
2.2 purifying the thorium nitrate step by adopting an extraction method.
In the step 3, the prepared single element standard solution with the intermediate concentration is shown in a table 2;
TABLE 2 preparation concentrations of the Single element Standard solutions
In step 5, the preparation of the first set of standard solutions comprises the following steps:
respectively transferring 40mL of 5000 mug/mL first group of single element standard solutions to a 1000mL volumetric flask, and performing constant volume by using 3mol/L nitric acid to obtain a first group of mixed standard solutions with the element concentrations of 200 mug/mL;
respectively transferring 50mL of 2000 mu g/mL second group of single element standard solutions to a 1000mL volumetric flask, and performing constant volume by using 3mol/L nitric acid to obtain a second group of mixed standard solutions with the element concentrations of 100 mu g/mL;
respectively transferring 50mL of 1000 mu g/mL third group of single element standard solution to a 1000mL volumetric flask, and performing constant volume by using 4mol/L hydrochloric acid to obtain a third group of mixed standard solution with the element concentration of 50 mu g/mL;
each of the above mixed standard solutions was prepared in 34 bottles.
In step 5, a second set of standard solutions is prepared, comprising the steps of:
respectively transferring 10mL of 5000 mug/mL first group of single element standard solutions to a 1000mL volumetric flask, and performing constant volume by using 3mol/L nitric acid to obtain a first group of mixed standard solutions with element concentrations of 50 mug/mL;
respectively transferring 10mL of 2000 mu g/mL second group of single element standard solutions to a 1000mL volumetric flask, and performing constant volume by using 3mol/L nitric acid to obtain a second group of mixed standard solutions with the element concentrations of 20 mu g/mL;
respectively transferring 10mL of 1000 mu g/mL third group of single element standard solution to a 1000mL volumetric flask, and performing constant volume by using 4mol/L hydrochloric acid to obtain a third group of mixed standard solution with each element concentration of 10 mu g/mL;
each of the above mixed standard solutions was prepared in 34 bottles.
Step 2.1, purifying the strontium nitrate step by adopting a precipitation method, and specifically comprises the following steps:
1) dissolving spectrally pure strontium nitrate in high-purity water, and heating to 80 ℃;
2) according to the preliminary detection result, calculating the sulfuric acid amount required by barium in the precipitated strontium nitrate, slowly adding a 10% sulfuric acid solution, and continuously stirring;
3) standing for half an hour, filtering, and adding excessive sodium acetate, 2-3 drops of acetic acid and 1mL of potassium dichromate solution into the filtrate;
4) if the filtrate is not turbid, the barium ions are completely precipitated, otherwise, the previous steps are repeated;
5) heating and evaporating the filtered filtrate to density of 1.45g/cm3Cooling until crystallization is separated out;
6) filtering out crystals, drying the crystals to constant weight, and crystallizing to obtain high-purity strontium nitrate;
detection shows that the content of barium in the purified strontium nitrate is reduced, and the use requirement is met.
Step 2.2, purifying thorium nitrate step by adopting an extraction method, and specifically comprising the following steps:
1) dissolving analytically pure thorium nitrate by using 30 percent nitric acid, and carrying out precision filtration to remove insoluble substances to obtain a clear thorium nitrate solution;
2) removing trace metal uranium in 5 percent TBP kerosene and thorium nitrate solution by 6-stage countercurrent extraction;
3) extracting thorium from the extract by 10-grade countercurrent extraction with 30% TBP/kerosene to make most of thorium enter an organic phase;
4) washing the organic phase with a 30% nitric acid solution to remove impure thorium solution entrained in the organic phase;
5) carrying out 8-stage countercurrent back extraction on the organic phase subjected to impurity removal by using high-purity water at a proper temperature to obtain a high-purity thorium nitrate solution;
6) trace oil in the high-purity thorium nitrate solution is collected by carbon tetrachloride, so that pollution of organic matters to final products is avoided;
7) finally evaporating and concentrating the high-purity thorium nitrate solution to a proper concentration, and cooling and crystallizing to obtain a thorium nitrate tetrahydrate product;
through detection, the purified thorium nitrate has low content of impurity elements and meets the use requirement.
And 7, subpackaging the samples qualified in the primary inspection into cleaned polyethylene bottles.
And 6, randomly drawing 12 bottles of samples from each group of the multi-element mixed standard solution prepared in the step 5 for primary uniformity detection.
The invention has the following remarkable effects:
the invention establishes a preparation process of the multi-element mixed standard solution for nuclear fuel analysis, the prepared multi-element mixed standard solution has good uniformity effect and complete element types, and can meet the analysis and use requirements of impurity elements in nuclear fuel products.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
A preparation process of a multi-element mixed standard solution for nuclear fuel analysis comprises the following steps:
step 1: selection of raw materials
Selecting high-purity metal oxide or ammonium salt as a raw material, wherein the purity of the selected raw material and reagent is shown in table 1, and after primary detection, the content of barium ions in strontium nitrate is overhigh and the content of total impurities in thorium nitrate is overhigh;
TABLE 1 raw material List
Step 2: purification of raw materials
For the high-purity reagent which cannot be purchased in the current market, the low-purity reagent needs to be purified, so that the content of impurity elements cannot cause the change of the content of main elements;
2.1 purifying the strontium nitrate step by adopting a precipitation method;
1) dissolving spectrally pure strontium nitrate in high-purity water, and heating to 80 ℃;
2) according to the preliminary detection result, calculating the sulfuric acid amount required by barium in the precipitated strontium nitrate, slowly adding a 10% sulfuric acid solution, and continuously stirring;
3) standing for half an hour, filtering, and adding excessive sodium acetate, 2-3 drops of acetic acid and 1mL of potassium dichromate solution into the filtrate;
4) if the filtrate is not turbid, the barium ions are completely precipitated, otherwise, the previous steps are repeated;
5) heating and evaporating the filtered filtrate to density of 1.45g/cm3Cooling until crystallization is separated out;
6) filtering out crystals, drying the crystals to constant weight, and crystallizing to obtain high-purity strontium nitrate;
detection shows that the content of barium in the purified strontium nitrate is reduced, and the use requirement is met;
2.2 purifying thorium nitrate step by adopting an extraction method;
1) dissolving analytically pure thorium nitrate by using 30 percent nitric acid, and carrying out precision filtration to remove insoluble substances to obtain a clear thorium nitrate solution;
2) removing trace metal uranium in 5 percent TBP kerosene and thorium nitrate solution by 6-stage countercurrent extraction;
3) extracting thorium from the extract by 10-grade countercurrent extraction with 30% TBP/kerosene to make most of thorium enter an organic phase;
4) washing the organic phase with a 30% nitric acid solution to remove impure thorium solution entrained in the organic phase;
5) carrying out 8-stage countercurrent back extraction on the organic phase subjected to impurity removal by using high-purity water at a proper temperature to obtain a high-purity thorium nitrate solution;
6) trace oil in the high-purity thorium nitrate solution is collected by carbon tetrachloride, so that pollution of organic matters to final products is avoided;
7) finally evaporating and concentrating the high-purity thorium nitrate solution to a proper concentration, and cooling and crystallizing to obtain a thorium nitrate tetrahydrate product;
through detection, the purified thorium nitrate has low content of impurity elements and meets the use requirement;
and step 3: preparation of intermediate concentration Unit element Standard solution
Preparing the raw materials selected in the step 1 and the step 2 or the purified reagent into a single element standard solution with intermediate concentration, which is shown in a table 2;
TABLE 2 preparation concentrations of the Single element Standard solutions
And 4, step 4: verification of concentration of single element standard solution
Respectively detecting the single element standard solution prepared in the step 3 by adopting an ICP-AES method or an ICP-MS method, and if the detection result is basically consistent with the theoretical preparation concentration, determining that the reagent is abnormal and meets the requirements;
if the detection result is not consistent with the theoretical preparation concentration, returning to the step 1;
and 5: preparation of Multi-element Mixed Standard solution
Preparing the single-element standard solution which meets the requirements verified in the step (4) into a multi-element mixed standard solution which meets an expected target value, and uniformly mixing;
5.1 preparation of the first set of Standard solutions
Respectively transferring 40mL of 5000 mug/mL first group of single element standard solutions to a 1000mL volumetric flask, and performing constant volume by using 3mol/L nitric acid to obtain a first group of mixed standard solutions with the element concentrations of 200 mug/mL;
respectively transferring 50mL of 2000 mu g/mL second group of single element standard solutions to a 1000mL volumetric flask, and performing constant volume by using 3mol/L nitric acid to obtain a second group of mixed standard solutions with the element concentrations of 100 mu g/mL;
respectively transferring 50mL of 1000 mu g/mL third group of single element standard solution to a 1000mL volumetric flask, and performing constant volume by using 4mol/L hydrochloric acid to obtain a third group of mixed standard solution with the element concentration of 50 mu g/mL;
preparing 34 bottles of the mixed standard solutions in each group;
5.2 preparation of the second set of Standard solutions
Respectively transferring 10mL of 5000 mug/mL first group of single element standard solutions to a 1000mL volumetric flask, and performing constant volume by using 3mol/L nitric acid to obtain a first group of mixed standard solutions with element concentrations of 50 mug/mL;
respectively transferring 10mL of 2000 mu g/mL second group of single element standard solutions to a 1000mL volumetric flask, and performing constant volume by using 3mol/L nitric acid to obtain a second group of mixed standard solutions with the element concentrations of 20 mu g/mL;
respectively transferring 10mL of 1000 mu g/mL third group of single element standard solution to a 1000mL volumetric flask, and performing constant volume by using 4mol/L hydrochloric acid to obtain a third group of mixed standard solution with each element concentration of 10 mu g/mL;
preparing 34 bottles of the mixed standard solutions in each group;
step 6: uniformity preliminary examination
Randomly extracting 12 bottles of samples from each group of multi-element mixed standard solution prepared in the step 5, measuring each sample for three times, and performing uniformity initial detection by adopting a spectrum method;
then, evaluating the uniformity of the standard substance by adopting an analysis of variance method, namely an F test method, wherein the calculated F value is less than a critical value, and the sample is uniform and qualified; if the value is larger than or equal to the critical value, the sample is unqualified and can only be discarded;
and 7: dispensing
And (5) subpackaging the samples qualified in the primary inspection into cleaned polyethylene bottles, covering the polyethylene bottles with covers, and sealing and packaging the polyethylene bottles.
Example 1
Preparing 1L of one-level multi-element mixed standard solution standard substance in which expected magnitudes and extended uncertainties of element species are as shown in Table 3 below;
table 3 types of elements and their content levels (including factor k ═ 2) in the mixed standard solutions to be developed
Step 1: selection of raw materials
Selecting high-purity metal oxide or ammonium salt as a raw material, wherein the purity of the selected raw material and reagent is shown in table 1, and after primary detection, the content of barium ions in strontium nitrate is overhigh and the content of total impurities in thorium nitrate is overhigh;
step 2: purification of raw materials
For the high-purity reagent which cannot be purchased in the current market, the low-purity reagent needs to be purified, so that the content of impurity elements cannot cause the change of the content of main elements;
2.1 purification of strontium
The content of barium in the raw material, namely the spectral pure strontium nitrate, used for the commercial strontium is higher and exceeds 2 mu g/mL through detection, and the barium element is the main element in the project, so the content of the barium needs to be reduced by adopting a purification mode. According to the fact that the solubility of barium sulfate is lower than that of strontium sulfate, barium sulfate is precipitated before strontium sulfate is precipitated, and the strontium nitrate is purified by adopting a sulfuric acid precipitation method in the project. Dissolving spectrally pure strontium nitrate in high-purity water, heating to 80 ℃, calculating the sulfuric acid amount required by barium in the precipitated strontium nitrate according to a primary detection result, slowly adding a 10% sulfuric acid solution, and continuously stirring. Standing for half an hour, filtering, taking the filtered filtrate, adding excessive sodium acetate, 2-3 drops of acetic acid and 1mL of potassium dichromate solution, and if the filtrate is not turbid, indicating that barium ions are completely precipitated. Otherwise, the previous steps are repeated. Heating and evaporating the filtered filtrate to a density of about 1.45g/cm3In the process, the mixture is cooled until crystals are separated out, and the crystals are filtered out and dried to constant weight. Crystallizing to obtain high-purity strontium nitrate. The detection shows that the content of barium in the purified strontium nitrate is reduced, and the using requirement of the project is met.
The purified strontium nitrate was detected according to the method for detecting impurity elements, and the detection results are shown in table 4.
TABLE 4 comparison of the results of the detection before and after purification of strontium nitrate
2.2 purification of thorium
When analyzing the commercial analytical pure thorium nitrate, the total impurity content is too high, and is 5860 mu g/g. The analytical pure thorium nitrate is purified step by an extraction method, the thorium reagent obtained by purification by the method can reach nuclear purity, and the specific purification process is as follows:
1) dissolving analytically pure thorium nitrate by using 30 percent nitric acid, and carrying out precision filtration to remove insoluble substances to obtain a clear thorium nitrate solution.
2) Removing trace metal uranium in 5 percent TBP kerosene and thorium nitrate solution by 6-stage countercurrent extraction.
3) The extraction liquid is used for 10-grade countercurrent extraction of thorium by 30% TBP/kerosene, so that most of thorium enters the organic phase.
4) The organic phase was washed with a 30% nitric acid solution to remove the impure thorium solution entrained in the organic phase.
5) And (4) carrying out 8-stage countercurrent back extraction on the organic phase subjected to impurity removal by using high-purity water at a proper temperature to obtain a high-purity thorium nitrate solution.
6) And the carbon tetrachloride is used for collecting trace oil in the high-purity thorium nitrate solution, so that the pollution of organic phase to final products is avoided.
7) And finally evaporating and concentrating the high-purity thorium nitrate solution to a proper concentration, and cooling and crystallizing to obtain a thorium nitrate tetrahydrate product.
The purified thorium nitrate was retested by the method for detecting impurity elements in the raw material, and the results are shown in table 5.
TABLE 5 detection results of purified thorium nitrate (unit: ug/g)
And step 3: preparation of intermediate concentration Unit element Standard solution
Preparing the selected raw materials or the purified reagent into a single element standard solution with intermediate concentration, and showing in the following table;
the preparation method of each single element standard solution is as follows.
(1) Preparation of standard solution of aluminum (Al):
5.0000g of high-purity aluminum wire (5N, Shanghai chemical reagent purchasing and supplying station) is weighed, 50mL of concentrated hydrochloric acid is added into a quartz beaker for slight heating dissolution, and 3mol/L of hydrochloric acid is used for constant volume to reach a 1000mL volumetric flask, so that 5000 mug/mL of aluminum standard solution is obtained.
(2) Preparation of standard arsenic (As) solutions:
5.0000g of metal arsenic (4N, Shanghai chemical reagent purchasing and supplying station) is weighed, concentrated nitric acid is added continuously for micro-thermal dissolution, 3mol/L nitric acid is used for constant volume to a 1000mL volumetric flask, and 5000 mug/mL arsenic standard solution is obtained.
(3) Preparation of copper (Cu) standard solution:
5.0000g of high-purity copper sheet (5N, Shanghai chemical reagent station subpackaging factory) (surface oxide is treated by dilute nitric acid in advance), 10mL of dilute nitric acid (5mol/L) is added for slightly heating and dissolving, and the volume is determined to be 1000mL of volumetric flask by 3mol/L of nitric acid, so that 5000 mug/mL of copper standard solution is obtained.
(4) Preparation of chromium (Cr) standard solution:
38.4760g of spectrally pure chromium nitrate (Cr (NO) were weighed out3)3·9H2O) (4N, Special chemical reagent development center in North China) is placed in a quartz beaker, dissolved in high-purity water, and the volume is determined to be 1000mL by using 3mol/L nitric acid to obtain a chromium standard solution of 5000 mug/mL.
(5) Preparation of iron (Fe) standard solution:
5.0000g of high-purity iron powder (4N, Ningjin, Ministry of Fine chemical research in Jinke) is weighed and placed in a quartz beaker, 20mL of dilute nitric acid (1+1) is added for slight heating dissolution, and the volume is determined to be 1000mL of volumetric flask by 3mol/L of nitric acid, so as to obtain 5000 mug/mL of iron standard solution.
(6) Preparation of tantalum (Ta) standard solution:
10.8355g of high-purity potassium fluotantalate (K) are weighed2TaF7) (Alfa Aesar) is placed in a quartz beaker, 10mL of hydrofluoric acid (1+1) is added for micro-heating dissolution, and the volume is determined to be 1000mL of a volumetric flask by using 3mol/L of nitric acid, so that a tantalum standard solution with the volume of 5000 mug/mL is obtained.
(7) Preparation of vanadium (V) standard solution:
11.4800g of high-purity ammonium metavanadate (NH) were weighed4VO3) Putting the mixture into a quartz beaker, adding 20mL of water for dissolving, and metering the volume of the mixture into a 1000mL volumetric flask by using 3mol/L of nitric acid to obtain a vanadium standard solution with the volume of 5000 mu g/mL.
(8) Preparation of zinc (Zn) standard solution:
5.0000g of high-purity zinc particles (5N, subpackaged by Shanghai chemical reagent stations) are weighed and placed in a quartz beaker, 20mL of dilute nitric acid (1+1) is added for micro-heating dissolution, and the volume is determined to be 1000mL of volumetric flask by using 3mol/L of nitric acid, so that 5000 mug/mL of zinc standard solution is obtained.
(9) Preparation of silver (Ag) standard solution:
2.0000g of high-purity silver powder (4N, China chemical reagent, Sanko) is weighed and placed in a quartz beaker, 20mL of dilute nitric acid (1+1) is added for slightly heating and dissolving, and the volume is determined to be 1000mL of volumetric flask by 3mol/L of nitric acid, so that 2000 mu g/mL of silver standard solution is obtained.
(10) Preparation of boron (B) standard solution:
11.4380g of high purity boric acid (H) were weighed out3BO3) (4N) placing the mixture into a quartz beaker, adding 20mL of water for dissolving, and metering the volume of the mixture into a 1000mL volumetric flask by using 3mol/L nitric acid to obtain 2000 mu g/mL boron standard solution.
(11) Preparation of barium (Ba) standard solution:
2.9080g of high purity barium carbonate (BaCO) was weighed3) (4N, Special chemical reagent development center in North China) is placed in a quartz beaker, 20mL of dilute nitric acid (1+1) is added for slightly heating dissolution, and the volume is determined to be 1000mL of volumetric flask by using 3mol/L of nitric acid, so that 2000 mu g/mL of barium standard solution is obtained.
(12) Preparation of bismuth (Bi) standard solution:
weighing 2.0000g of high-purity bismuth powder (5N, chemical reagent of national drug group, Ltd.) and placing the high-purity bismuth powder into a quartz beaker, adding 20mL of dilute nitric acid (1+1) for slightly heating and dissolving, and using 3mol/L nitric acid to fix the volume into a volumetric flask of 1000mL to obtain a 2000 mu g/mL bismuth standard solution.
(13) Preparation of cadmium (Cd) standard solution:
2.0000g of high-purity cadmium sheet (5N, chemical reagent of national drug group, Ltd.) (oxide is treated by dilute nitric acid in advance) is weighed and placed in a quartz beaker, 20mL of dilute nitric acid (1+1) is added for slight heating dissolution, and the volume is fixed to a 1000mL volumetric flask by 3mol/L of nitric acid to obtain 2000 mu g/mL of cadmium standard solution.
(14) Preparation of cobalt (Co) standard solution:
2.0000g of high-purity cobalt particles (5N, a first-level chemical metering station of the national defense department Committee) are weighed and placed in a quartz beaker, 20mL of dilute nitric acid (1+1) is added for slightly heating dissolution, and the volume is determined to be 1000mL of a volumetric flask by using 3mol/L of nitric acid, so that 2000 mu g/mL of cobalt standard solution is obtained.
(15) Preparation of manganese (Mn) standard solution:
2.0000g of high-purity manganese flakes (Alfa, 4N) (oxide is shown by being treated by dilute nitric acid in advance) are weighed and placed in a quartz beaker, 20mL of dilute nitric acid (1+1) is added for micro-heating dissolution, and the volume is determined to be 1000mL of a volumetric flask by 3mol/L of nitric acid, so that 2000 mu g/mL of manganese standard solution is obtained.
(16) Preparation of molybdenum (Mo) standard solution:
3.6800g of ammonium molybdate ((NH) were weighed out4)6Mo7O24·4H2O) (4N, Beijing chemical reagent company) is put into a quartz beaker, added with 20mL of water for dissolving, and is added with 3mol/L nitric acid for constant volume to a 1000mL volumetric flask, thus obtaining 2000 mug/mL molybdenum standard solution.
(17) Preparation of niobium (Nb) standard solution:
2.8610g of high-purity niobium pentoxide is weighed in a polytetrafluoroethylene beaker, 10mL of hydrofluoric acid and 20mL of dilute nitric acid (1+1) are added for slightly heating and dissolving, and 3mol/L of nitric acid is used for fixing the volume to a 1000mL volumetric flask, thus obtaining 2000 mug/mL of niobium standard solution.
(18) Preparation of nickel (Ni) standard solution:
2.0000g of high-purity sponge nickel (Shanghai reagent factory I) is weighed and placed in a quartz beaker, 20mL of dilute nitric acid (1+1) is added for micro-heating dissolution, and the volume is determined to be 1000mL of volumetric flask by using 3mol/L of nitric acid, so that 2000 mu g/mL of nickel standard solution is obtained.
(19) Preparation of lead (Pb) standard solution:
2.0000g of high-purity lead granules (5N, China chemical reagent, III Co., Ltd.) (oxide is shown by being treated by dilute nitric acid in advance) are weighed and placed in a quartz beaker, 20mL of dilute nitric acid (1+1) is added for slight heating dissolution, and the volume is fixed to a 1000mL volumetric flask by using 3mol/L of nitric acid to obtain 2000 mu g/mL of lead standard solution.
(20) Preparation of tin (Sn) standard solution:
2.0000g of high-purity tin sheet (5N, Shenyang Standard research institute) is weighed and placed in a quartz beaker, 2mL of hydrofluoric acid and 0.5mL of nitric acid are added, and after dissolution, the volume is determined to be 1000mL of volumetric flask by using 3mol/L of nitric acid, so that 2000 mu g/mL of tin standard solution is obtained.
(21) Preparation of strontium (Sr) standard solution:
4.8306g of purified strontium nitrate (Sr (NO) was weighed3)2) Putting the mixture into a quartz beaker, dissolving the mixture in water, and metering the volume of the mixture into a 1000mL volumetric flask by using 3mol/L nitric acid to obtain 2000 mu g/mL strontium standard solution.
(22) Preparation of thorium (Th) standard solution:
2.3795g of purified thorium nitrate (Th (NO) were weighed out3)4·4H2O) is put into a quartz beaker, dissolved by water and added with 3mol/L nitric acid to be constant volume into a 1000mL volumetric flask, thus obtaining 2000 mug/mL thorium standard solution.
(23) Preparation of titanium (Ti) standard solution:
8.2651g of ammonium fluorotitanate ((NH) was weighed out4)Ti6F6) (4N, Alfa Aesar) is placed in a quartz beaker, 0.5mL of hydrofluoric acid is dripped in the quartz beaker, the solution is dissolved by slight heating, and the volume is determined to be 1000mL of a volumetric flask by 3mol/L of nitric acid, so that 2000 mu g/mL of titanium standard solution is obtained.
(24) Preparation of dysprosium (Dy) standard solution:
1.1477g of high-purity dysprosium oxide (Dy) was weighed2O3) (5N) placing the mixture into a quartz beaker, adding 20mL of dilute hydrochloric acid (1+1) for slightly heating and dissolving, and metering the volume into a 1000mL volumetric flask by using 4mol/L hydrochloric acid to obtain 1000 mu g/mL dysprosium standard solution.
(25) Preparation of europium (Eu) standard solution:
1.1579g of high-purity europium oxide (Eu) is weighed2O3) (6N) placing the europium powder in a quartz beaker, adding 20mL of dilute hydrochloric acid (1+1) for slightly heating and dissolving, and metering the volume to a 1000mL volumetric flask by using 4mol/L hydrochloric acid to obtain 1000 mu g/mL europium standard solution.
(26) Preparation of gadolinium (Gd) standard solution:
1.1526g of high-purity gadolinium oxide (Gd) is weighed2O3) (5N) placing the mixture into a quartz beaker, adding 20mL of dilute hydrochloric acid (1+1) for slightly heating and dissolving, and metering the volume into a 1000mL volumetric flask by using 4mol/L of hydrochloric acid to obtain 1000 mu g/mL of gadolinium standard solution.
(27) Preparation of ruthenium (Ru) standard solution:
3.2890g of ammonium chlorotritinate ((NH) was weighed out4)2Ru(H2O)Cl5) (Alfa Aesar) was placed in a quartz beaker, and 20mL of dilute hydrochloric acid (1+1) was added thereto to dissolve the solution in a slight heat, and the solution was taken up in a 1000 mL-volume bottle with 4mol/L hydrochloric acid to obtain a 1000. mu.g/mL ruthenium standard solution.
(28) Preparation of antimony (Sb) standard solution:
2.3944g of high-purity antimony oxide (Sb) was weighed2O3) (4N, Special chemical reagent development center in North China) is placed in a quartz beaker, 20mL of concentrated hydrochloric acid is added for slightly heating dissolution, and 6mol/L of hydrochloric acid is used for metering volume to a 1000mL volumetric flask to obtain 1000 mu g/mL of antimony standard solution.
(29) Preparation of samarium (Sm) standard solution:
2.3186g of high-purity samarium oxide (Sm) are weighed2O3) Placing the solution into a quartz beaker, adding 20mL of dilute hydrochloric acid (1+1) for micro-heating dissolution, and using 4mol/L hydrochloric acid to fix the volume into a 1000mL volumetric flask to obtain 1000 mu g/mL of samarium standard solution.
(30) Preparation of zirconium (Zr) standard solution:
3.5327g of high-purity zirconium oxychloride (ZrOCl) was weighed2·8H2O) (4N, Special chemical reagent development center in North China) is placed in a quartz beaker, dissolved in water, and is added with 4mol/L hydrochloric acid to be constant volume in a 1000mL volumetric flask, thus obtaining 1000 mug/mL zirconium standard solution.
And 4, step 4: verification of concentration of single element standard solution
And (3) respectively detecting the single element standard solution prepared in the step (3) by adopting an ICP-AES method or an ICP-MS method, and the detection results are listed in Table 6. As can be seen from the data in Table 6, the detection results are substantially consistent with the theoretical preparation concentrations, and it can be determined that the reagent is not abnormal.
TABLE 6 concentration verification of the Standard solution of Single element
And 5: preparation of Multi-element Mixed Standard solution
Preparing the single-element standard solution which meets the requirements verified in the step (4) into a multi-element mixed standard solution which meets an expected target value, and uniformly mixing;
5.1 preparation of the first set of Standard solutions
Transferring 40mL of the first group of single element standard solutions (5000 mug/mL) to 1000mL volumetric flasks respectively, and fixing the volume with 3mol/L nitric acid to obtain the first group of mixed standard solutions with the element concentrations of 200 mug/mL.
5.2 preparation of the second set of Standard solutions
Respectively transferring 50mL of second group of single element standard solution (2000 mu g/mL) to a 1000mL volumetric flask, and fixing the volume by using 3mol/L nitric acid to obtain a second group of mixed standard solution with the element concentration of 100 mu g/mL.
5.3 preparation of the third set of Standard solutions
And respectively transferring 50mL of the third group of single element standard solution (1000 mu g/mL) to a 1000mL volumetric flask, and fixing the volume by using 4mol/L hydrochloric acid to obtain a third group of mixed standard solution with the element concentration of 50 mu g/mL.
Step 6: uniformity preliminary examination
Randomly extracting 12 bottles of samples from each group of multi-element mixed standard solution prepared in the step 5, measuring each sample for three times, and performing primary uniformity detection by adopting a spectroscopy method, wherein the detection elements and the detection method of each group are shown in a table 7.
TABLE 7 elements and methods for uniformity testing
And evaluating the uniformity of the standard substance by using an analysis of variance method, namely an F test method, wherein the calculated F value is less than a critical value, and the sample is uniform.
And 7: dispensing
And (4) subpackaging the samples qualified in the primary inspection into cleaned 30mL polyethylene bottles, covering the polyethylene bottles with covers, and sealing and packaging the polyethylene bottles.
Example 2
A1L two-level multi-element mixed standard solution standard substance was prepared, in which expected magnitudes and spread uncertainties of the element species are as follows in Table 8:
table 8 types of elements and their content levels (including factor k ═ 2) in the mixed standard solutions to be developed
Step 1: selection of raw materials
Selecting high-purity metal oxide or ammonium salt as a raw material, wherein the purity of the selected raw material and reagent is shown in table 1, and after primary detection, the content of barium ions in strontium nitrate is overhigh and the content of total impurities in thorium nitrate is overhigh;
step 2: purification of raw materials
For the high-purity reagent which cannot be purchased in the current market, the low-purity reagent needs to be purified, so that the content of impurity elements cannot cause the change of the content of main elements; the specific purification procedure is shown in step 2 of example 1.
And step 3: preparation of intermediate concentration Unit element Standard solution
Preparing the selected raw materials or the purified reagent into a single element standard solution with intermediate concentration, and showing in the following table;
the preparation of each single element standard solution is described in step 3 of example 1.
And 4, step 4: verification of concentration of single element standard solution
And (3) respectively detecting the single element standard solution prepared in the step (3) by adopting an ICP-AES method or an ICP-MS method, wherein the detection result is basically consistent with the theoretical preparation concentration, and the reagent can be determined to be abnormal, specifically shown in the step (4) in the example 1.
And 5: preparation of Multi-element Mixed Standard solution
Preparing the single-element standard solution which meets the requirements verified in the step (4) into a multi-element mixed standard solution which meets an expected target value, and uniformly mixing;
5.1 preparation of the first set of Standard solutions
10mL of the first group of single element standard solution (5000 mu g/mL) is respectively transferred to a 1000mL volumetric flask, and the volume is determined by 3mol/L nitric acid. Obtaining a first group of mixed standard solutions with the concentration of each element being 50 mug/mL.
5.2 preparation of the second set of Standard solutions
10mL of the second group of single element standard solution (2000. mu.g/mL) is respectively transferred to a 1000mL volumetric flask, and the volume is determined by 3mol/L nitric acid. Obtaining a second group of mixed standard solutions with the concentration of each element being 20 mug/mL.
5.3 preparation of the third set of Standard solutions
10mL of the third group of single element standard solution (1000. mu.g/mL) is transferred to a 1000mL volumetric flask and is made to the constant volume with 4mol/L hydrochloric acid. And obtaining a third group of mixed standard solution with the element concentration of 10 mu g/mL.
Step 6: uniformity preliminary examination
Randomly extracting 12 bottles of samples from each group of multi-element mixed standard solution prepared in the step 5, and determining each sample for three times in a table 7, and performing primary uniformity detection by adopting a spectral method;
and evaluating the uniformity of the standard substance by using an analysis of variance method, namely an F test method, wherein the calculated F value is less than a critical value, and the sample is uniform.
And 7: dispensing
And (4) subpackaging the samples qualified in the primary inspection into cleaned 30mL polyethylene bottles, covering the polyethylene bottles with covers, and sealing and packaging the polyethylene bottles.
Claims (10)
1. A preparation process of a multi-element mixed standard solution for nuclear fuel analysis is characterized by comprising the following steps: the method comprises the following steps:
step 1: selection of raw materials
Selecting and purchasing high-purity metal oxide or ammonium salt as a raw material;
step 2: purification of raw materials
For the high-purity reagent which cannot be purchased in the current market, the low-purity reagent needs to be purified, so that the content of impurity elements cannot cause the change of the content of main elements;
and step 3: preparation of intermediate concentration Unit element Standard solution
Preparing the raw materials selected in the step 1 and the step 2 or the purified reagent into a single element standard solution with intermediate concentration;
and 4, step 4: verification of concentration of single element standard solution
Respectively detecting the single element standard solution prepared in the step 3 by adopting an ICP-AES method or an ICP-MS method, and if the detection result is basically consistent with the theoretical preparation concentration, determining that the reagent is abnormal and meets the requirements;
if the detection result is not consistent with the theoretical preparation concentration, returning to the step 1;
and 5: preparation of Multi-element Mixed Standard solution
Preparing the single-element standard solution which meets the requirements verified in the step (4) into a multi-element mixed standard solution which meets an expected target value, and uniformly mixing;
step 6: uniformity preliminary examination
Randomly extracting samples from each group of multi-element mixed standard solution prepared in the step 5, measuring each sample for three times, and performing uniformity initial detection by adopting a spectrometry;
then, evaluating the uniformity of the standard substance by adopting an analysis of variance method, namely an F test method, wherein the calculated F value is less than a critical value, and the sample is uniform and qualified; if the value is larger than or equal to the critical value, the sample is unqualified and can only be discarded;
and 7: dispensing
And (5) subpackaging the samples qualified in the initial inspection, covering the cover, and sealing and packaging.
2. The process of claim 1, wherein the multi-element mixed standard solution is prepared by the following steps: in step 1, the purity of the selected raw materials and reagents is shown in table 1;
TABLE 1 raw material List
3. The process of claim 2, wherein the multi-element mixed standard solution is prepared by the following steps: in the step 1, after preliminary detection, the content of barium ions in the selected raw material strontium nitrate is overhigh, and the content of total impurities in thorium nitrate is overhigh;
the step 2 specifically comprises the following steps:
2.1 purifying the strontium nitrate step by adopting a precipitation method;
2.2 purifying the thorium nitrate step by adopting an extraction method.
4. The process of claim 3, wherein the multi-element mixed standard solution is prepared by the following steps: in the step 3, the prepared single element standard solution with the intermediate concentration is shown in a table 2;
TABLE 2 preparation concentrations of the Single element Standard solutions
5. The process of claim 4, wherein the multi-element mixed standard solution is prepared by the following steps: in step 5, the preparation of the first set of standard solutions comprises the following steps:
respectively transferring 40mL of 5000 mug/mL first group of single element standard solutions to a 1000mL volumetric flask, and performing constant volume by using 3mol/L nitric acid to obtain a first group of mixed standard solutions with the element concentrations of 200 mug/mL;
respectively transferring 50mL of 2000 mu g/mL second group of single element standard solutions to a 1000mL volumetric flask, and performing constant volume by using 3mol/L nitric acid to obtain a second group of mixed standard solutions with the element concentrations of 100 mu g/mL;
respectively transferring 50mL of 1000 mu g/mL third group of single element standard solution to a 1000mL volumetric flask, and performing constant volume by using 4mol/L hydrochloric acid to obtain a third group of mixed standard solution with the element concentration of 50 mu g/mL;
each of the above mixed standard solutions was prepared in 34 bottles.
6. The process of claim 5, wherein the multi-element mixed standard solution is prepared by the following steps: in step 5, a second set of standard solutions is prepared, comprising the steps of:
respectively transferring 10mL of 5000 mug/mL first group of single element standard solutions to a 1000mL volumetric flask, and performing constant volume by using 3mol/L nitric acid to obtain a first group of mixed standard solutions with element concentrations of 50 mug/mL;
respectively transferring 10mL of 2000 mu g/mL second group of single element standard solutions to a 1000mL volumetric flask, and performing constant volume by using 3mol/L nitric acid to obtain a second group of mixed standard solutions with the element concentrations of 20 mu g/mL;
respectively transferring 10mL of 1000 mu g/mL third group of single element standard solution to a 1000mL volumetric flask, and performing constant volume by using 4mol/L hydrochloric acid to obtain a third group of mixed standard solution with each element concentration of 10 mu g/mL;
each of the above mixed standard solutions was prepared in 34 bottles.
7. The process of claim 6, wherein the multi-element mixed standard solution is prepared by the following steps: step 2.1, purifying the strontium nitrate step by adopting a precipitation method, and specifically comprises the following steps:
1) dissolving spectrally pure strontium nitrate in high-purity water, and heating to 80 ℃;
2) according to the preliminary detection result, calculating the sulfuric acid amount required by barium in the precipitated strontium nitrate, slowly adding a 10% sulfuric acid solution, and continuously stirring;
3) standing for half an hour, filtering, and adding excessive sodium acetate, 2-3 drops of acetic acid and 1mL of potassium dichromate solution into the filtrate;
4) if the filtrate is not turbid, the barium ions are completely precipitated, otherwise, the previous steps are repeated;
5) heating and evaporating the filtered filtrate to density of 1.45g/cm3Cooling until crystallization is separated out;
6) filtering out crystals, drying the crystals to constant weight, and crystallizing to obtain high-purity strontium nitrate;
detection shows that the content of barium in the purified strontium nitrate is reduced, and the use requirement is met.
8. The process of claim 7, wherein the multi-element mixed standard solution is prepared by the following steps: step 2.2, purifying thorium nitrate step by adopting an extraction method, and specifically comprising the following steps:
1) dissolving analytically pure thorium nitrate by using 30 percent nitric acid, and carrying out precision filtration to remove insoluble substances to obtain a clear thorium nitrate solution;
2) carrying out 6-stage countercurrent extraction on 5% TBP kerosene and thorium nitrate solution to remove trace metal uranium;
3) extracting thorium from the extract by 10-grade countercurrent extraction with 30% TBP/kerosene to make most of thorium enter into organic phase;
4) washing the organic phase with a 30% nitric acid solution to remove impure thorium solution entrained in the organic phase;
5) carrying out 8-stage countercurrent back extraction on the organic phase subjected to impurity removal by using high-purity water at a proper temperature to obtain a high-purity thorium nitrate solution;
6) trace oil in the high-purity thorium nitrate solution is collected by carbon tetrachloride, so that pollution of organic matters to final products is avoided;
7) finally evaporating and concentrating the high-purity thorium nitrate solution to a proper concentration, and cooling and crystallizing to obtain a thorium nitrate tetrahydrate product;
through detection, the purified thorium nitrate has low content of impurity elements and meets the use requirement.
9. The process of claim 8, wherein the multi-element mixed standard solution is prepared by the following steps: and 7, subpackaging the samples qualified in the primary inspection into cleaned polyethylene bottles.
10. The process of claim 9, wherein the multi-element mixed standard solution is prepared by the following steps: and 6, randomly drawing 12 bottles of samples from each group of the multi-element mixed standard solution prepared in the step 5 for primary uniformity detection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910983107.5A CN111024463A (en) | 2019-10-16 | 2019-10-16 | Preparation process of multi-element mixed standard solution for nuclear fuel analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910983107.5A CN111024463A (en) | 2019-10-16 | 2019-10-16 | Preparation process of multi-element mixed standard solution for nuclear fuel analysis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111024463A true CN111024463A (en) | 2020-04-17 |
Family
ID=70200903
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910983107.5A Pending CN111024463A (en) | 2019-10-16 | 2019-10-16 | Preparation process of multi-element mixed standard solution for nuclear fuel analysis |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111024463A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103738998A (en) * | 2013-12-24 | 2014-04-23 | 杨建荣 | Method for preparing low-barium strontium nitrate |
| CN106629807A (en) * | 2016-11-25 | 2017-05-10 | 中核北方核燃料元件有限公司 | Method for preparing nuclear-pure thorium tetrafluoride from thorium oxalate through purification |
| CN109443874A (en) * | 2018-11-22 | 2019-03-08 | 核工业北京化工冶金研究院 | Uranium and impurity element standard substance preparation method in a kind of triuranium octoxide |
| CN110255577A (en) * | 2019-06-05 | 2019-09-20 | 核工业北京化工冶金研究院 | The pure grade boric acid standard substance preparation process of one seed nucleus |
-
2019
- 2019-10-16 CN CN201910983107.5A patent/CN111024463A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103738998A (en) * | 2013-12-24 | 2014-04-23 | 杨建荣 | Method for preparing low-barium strontium nitrate |
| CN106629807A (en) * | 2016-11-25 | 2017-05-10 | 中核北方核燃料元件有限公司 | Method for preparing nuclear-pure thorium tetrafluoride from thorium oxalate through purification |
| CN109443874A (en) * | 2018-11-22 | 2019-03-08 | 核工业北京化工冶金研究院 | Uranium and impurity element standard substance preparation method in a kind of triuranium octoxide |
| CN110255577A (en) * | 2019-06-05 | 2019-09-20 | 核工业北京化工冶金研究院 | The pure grade boric acid standard substance preparation process of one seed nucleus |
Non-Patent Citations (2)
| Title |
|---|
| 李晓红等: "多元素混合标准溶液中铜的不确定度评定", 《化学分析计量》 * |
| 郭国龙等: "核燃料分析用多元素混合标准溶液的研制", 《化学分析计量》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Rao et al. | Dissolution of uranium oxides and electrochemical behavior of U (VI) in task specific ionic liquid | |
| CN109443874B (en) | Preparation method of standard substance of uranium and impurity elements in triuranium octoxide | |
| Reichel et al. | Concentration and determination of trace impurities in copper by atomic absorption spectrophotometry | |
| White et al. | Separation of antimony by solvent extraction | |
| CN114572960B (en) | Preparation method of graphite oxide alkyne membrane material for adsorption separation of uranium | |
| CN105300961A (en) | Separation and enrichment determination method for Ir, Rh, Pt, Pd and Au in secondary resource material | |
| Itagaki et al. | Determination of trace amounts of gold and silver in high-purity iron and steel by electrothermal atomic absorption spectrometry after reductive coprecipitation | |
| CN111024463A (en) | Preparation process of multi-element mixed standard solution for nuclear fuel analysis | |
| Inman | Determination of manganese in high-purity niobium, tantalum, molybdenum and tungsten metals with pan | |
| CN106645101B (en) | The measuring method of impurity element in a kind of zirconium diboride | |
| CN111679031A (en) | Method for measuring antimony in crude lead by precipitation separation-carbon reduction cerium sulfate volumetric method | |
| Shilimkar et al. | Rapid extraction of lead (II) from succinate media with n-octylaniline in toluene | |
| CN109896540A (en) | The method for preparing the powder of particle containing triuranium octoxide and plutonium dioxide particle | |
| Mane et al. | Extraction behaviour of 2-octylaminopyridine towards lead (II) from succinate media and its separation from other toxic metals | |
| CN103508481A (en) | Method of preparing spectrally-pure superfine silver chloride | |
| Tian et al. | Auto-deposition of 210Bi and 210Po on nickel discs and their application in the analysis of natural waters | |
| CN111650192A (en) | Method for removing lead in lead-bismuth alloy and method for measuring tellurium in lead-bismuth alloy | |
| Horton et al. | Remote Control Determination of Corrosion Products and Additives in Homogeneous Reactor Fuel | |
| Nagara et al. | Quantification of trace and ultra-trace impurities in U-Zr alloy by inductively couple plasma time of flight mass spectrometry (ICP-TOF-MS) after simultaneous separation of U and Zr | |
| CN114141400B (en) | Method for separating antimony from fission products | |
| CN116929865A (en) | Preparation method of heavy metal element standard substance in diuranate | |
| Shilmkar et al. | Liquid–liquid extraction of gallium (III) with n-octylaniline from succinate media | |
| Albwght et al. | A chemical concentration x-ray determination of selenium in copper-, nickel-and iron-base alloys | |
| Marangoni et al. | Gravimetric determination of uranium (VI) with pyridine-2, 6-dicarboxylic acid | |
| Salyer et al. | Determination of Small Amounts of Cobalt in Steels and Nickel Alloys By the Isotope Dilution-Anodic Deposition Method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200417 |
|
| RJ01 | Rejection of invention patent application after publication |