CN111307784A - Method for determining content of impurity elements in uranium boride solid sample - Google Patents
Method for determining content of impurity elements in uranium boride solid sample Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000012535 impurity Substances 0.000 title claims abstract description 40
- QPXOIGGWJBMJIH-UHFFFAOYSA-N bis(boranylidyne)uranium Chemical compound B#[U]#B QPXOIGGWJBMJIH-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000007787 solid Substances 0.000 title claims abstract description 23
- 238000000605 extraction Methods 0.000 claims abstract description 38
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052796 boron Inorganic materials 0.000 claims abstract description 30
- 229910052770 Uranium Inorganic materials 0.000 claims abstract description 27
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011159 matrix material Substances 0.000 claims abstract description 25
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 19
- 239000010453 quartz Substances 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000005303 weighing Methods 0.000 claims abstract description 10
- 238000004090 dissolution Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000010025 steaming Methods 0.000 claims abstract description 7
- 238000004366 reverse phase liquid chromatography Methods 0.000 claims abstract description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 18
- 238000004458 analytical method Methods 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 239000012086 standard solution Substances 0.000 claims description 9
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052791 calcium Inorganic materials 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000003085 diluting agent Substances 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 239000008096 xylene Substances 0.000 claims description 5
- 230000003595 spectral effect Effects 0.000 claims description 4
- RWLALWYNXFYRGW-UHFFFAOYSA-N 2-Ethyl-1,3-hexanediol Chemical compound CCCC(O)C(CC)CO RWLALWYNXFYRGW-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000013582 standard series solution Substances 0.000 claims description 3
- 238000013375 chromatographic separation Methods 0.000 claims 2
- 238000001514 detection method Methods 0.000 abstract description 16
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000008188 pellet Substances 0.000 abstract description 3
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- 239000011575 calcium Substances 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 238000005259 measurement Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 3
- 230000000717 retained effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000003671 uranium compounds Chemical class 0.000 description 2
- 150000001639 boron compounds Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 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
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
-
- 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to a method for determining the content of impurity elements in a uranium boride solid sample, which comprises the following steps: step one, sample dissolution; weighing 1.0g of sample, placing the sample in a 150mL quartz beaker, adding 5-10mL of concentrated nitric acid solution, heating and dissolving the sample, after the sample is completely dissolved, steaming the sample to 2-3mL at low temperature, taking down the sample, and cooling the sample to room temperature; step two, separating a uranium matrix; separating uranium matrix in the sample by an extraction method-reversed phase chromatography column method; step three, separating the boron matrix; separating the boron matrix by an extraction method; step four, measuring a sample; the samples were measured by the standard curve method using ICP-AES. The method for determining the content of the impurity element in the uranium boride powder or the pellet by the plasma emission spectrometry is successfully established, the content of the impurity element can be accurately determined by using the experimental conditions listed in the content of the invention, accurate detection data are reported, a method is provided for relevant detection of uranium boride in the future, and the method is effectively matched with the special production.
Description
Technical Field
The invention belongs to the field of chemical detection, and particularly relates to a method for determining the content of impurity elements in a uranium boride solid sample.
Background
BoronizingThe uranium compounds are of various types, with UB2、UB4、UB12Several boron compounds have high melting points, related chemical detection methods about uranium boride are not found at home and abroad through research and study, and meanwhile, research on the preparation process and performance of uranium boride fuels is not systematically carried out at home, so that correct data can be provided for scientific research and production units carrying out process experiments, process support is provided, and a foundation is laid for detection and production of uranium compounds after detection.
During the method establishment, problems mainly exist in the aspects of investigation of sample dissolution conditions, investigation of instrument conditions and elimination of interference of a uranium matrix and a boron matrix.
Disclosure of Invention
The invention aims to: according to the requirement of detection work, a method for determining the content of impurity elements in uranium boride powder or pellets by plasma emission spectrometry is established based on the existing instruments and equipment in a laboratory. The requirements of scientific research and production detection are met.
The technical scheme of the invention is as follows: a method for determining the content of impurity elements in a uranium boride solid sample comprises the following steps:
step one, sample dissolution;
weighing 1.0g of sample, placing the sample in a 150mL quartz beaker, adding 5-10mL of concentrated nitric acid solution, heating and dissolving the sample, after the sample is completely dissolved, steaming the sample to 2-3mL at low temperature, taking down the sample, and cooling the sample to room temperature;
step two, separating a uranium matrix;
separating uranium matrix in the sample by an extraction method-reversed phase chromatography column method;
step three, separating the boron matrix;
separating the boron matrix by an extraction method;
step four, measuring a sample;
the samples were measured by the standard curve method using ICP-AES.
Further, the uranium boride solid sample is a uranium boride solid sample.
Further, in the first step, the concentrated nitric acid is superior pure concentrated nitric acid purified by sub-boiling distillation.
Further, in the first step, the heating temperature is 230-260 ℃.
And further, in the second step, the extraction method-reversed phase chromatography column method is used for separating the uranium matrix, firstly, 30-40mL of uranium extraction reagent is adopted to separate uranium in a sample under the medium of 5.5-10mol/L nitric acid solution, standing is carried out for 10min, the lower layer clear liquid is placed in a well balanced chromatography column, 10mL of volumetric flask is used for receiving leacheate to reach the scale, constant volume is realized, and shaking is carried out uniformly.
Furthermore, the uranium extraction reagent is prepared by taking TBP as an extracting agent and xylene as a diluent according to the proportion of 1: 3.
Further, in the third step, the extraction method is used for separating the boron substrate, the received sample is poured into a separating funnel filled with 30-40mL of boron extraction reagent, the separating funnel is shaken for 30s and then stands for 10min, then liquid below the separating funnel is placed into a second separating funnel filled with 30-40mL of boron extraction reagent, the separating funnel is shaken for 30s and then stands for 10min, and the lower layer clear liquid is collected into a 10mL quartz volumetric flask to be measured.
Further, the boron extraction reagent is prepared by taking xylene as a diluent and 2-ethyl-1, 3-hexanediol as an extracting agent according to the proportion of 1: 1.
Further, in the fourth step, the ICP-AES was manufactured by PE with model number Optima5300 DV.
Further, in the fourth step, the ICP-AES working condition, as shown in Table 1,
TABLE 1 working conditions of the apparatus
| Item | Require that | Item | Require that |
| RF generator power | 1100-1300W | Flow of carrier gas | 0.80-0.85L/min |
| Flow rate of plasma gas | 14-16L/min | Sample introduction speed | 1.2-1.8mL/min |
| Auxiliary gas flow | 0.2-0.3L/min | Observation mode | Horizontal observation |
；
In the fourth step, the elements to be measured are Fe, Ni, Cu, Mg, Ca, Mn, Si and Al, the concentration of the standard series solution is shown in Table 2,
TABLE 2 Standard solutions of elements to be tested
In the fourth step, the analysis line of the element to be measured is shown in table 3,
TABLE 3 analysis lines for elements to be tested
The invention has the following remarkable effects: the method for determining the content of the impurity element in the uranium boride powder or the pellet by the plasma emission spectrometry is successfully established, the content of the impurity element can be accurately determined by using the experimental conditions listed in the content of the invention, accurate detection data are reported, a method is provided for the related detection of uranium boride in the future, and the method is effectively matched with the special production.
Detailed Description
The method for determining the content of impurity elements in a uranium boride solid sample according to the present invention is further described in detail with reference to the following specific examples.
A method for determining the content of impurity elements in a uranium boride solid sample comprises the following steps:
step one, sample dissolution;
weighing 1.0g of sample, placing the sample in a 150mL quartz beaker, adding 5-10mL of concentrated nitric acid solution, heating and dissolving the sample, after the sample is completely dissolved, steaming the sample to 2-3mL at low temperature, taking down the sample, and cooling the sample to room temperature;
step two, separating a uranium matrix;
separating uranium matrix in the sample by an extraction method-reversed phase chromatography column method;
step three, separating the boron matrix;
separating the boron matrix by an extraction method;
step four, measuring a sample;
the samples were measured by the standard curve method using ICP-AES.
Further, the uranium boride solid sample is a uranium boride solid sample.
Further, in the first step, the concentrated nitric acid is superior pure concentrated nitric acid purified by sub-boiling distillation.
Further, in the first step, the heating temperature is 230-260 ℃.
And further, in the second step, the extraction method-reversed phase chromatography column method is used for separating the uranium matrix, firstly, 30-40mL of uranium extraction reagent is adopted to separate uranium in a sample under the medium of 5.5-10mol/L nitric acid solution, standing is carried out for 10min, the lower layer clear liquid is placed in a well balanced chromatography column, 10mL of volumetric flask is used for receiving leacheate to reach the scale, constant volume is realized, and shaking is carried out uniformly.
Furthermore, the uranium extraction reagent is prepared by taking TBP as an extracting agent and xylene as a diluent according to the proportion of 1: 3.
Further, in the third step, the extraction method is used for separating the boron substrate, the received sample is poured into a separating funnel filled with 30-40mL of boron extraction reagent, the separating funnel is shaken for 30s and then stands for 10min, then liquid below the separating funnel is placed into a second separating funnel filled with 30-40mL of boron extraction reagent, the separating funnel is shaken for 30s and then stands for 10min, and the lower layer clear liquid is collected into a 10mL quartz volumetric flask to be measured.
Further, the boron extraction reagent is prepared by taking xylene as a diluent and 2-ethyl-1, 3-hexanediol as an extracting agent according to the proportion of 1: 1.
Further, in the fourth step, the ICP-AES was manufactured by PE with model number Optima5300 DV.
Further, in the fourth step, the ICP-AES working condition, as shown in Table 1,
TABLE 1 working conditions of the apparatus
| Item | Require that | Item | Require that |
| RF generator power | 1100-1300W | Flow of carrier gas | 0.80-0.85L/min |
| Flow rate of plasma gas | 14-16L/min | Sample introduction speed | 1.2-1.8mL/min |
| Auxiliary gas flow | 0.2-0.3L/min | Observation mode | Horizontal observation |
；
In the fourth step, the elements to be measured are Fe, Ni, Cu, Mg, Ca, Mn, Si and Al, the concentration of the standard series solution is shown in Table 2,
TABLE 2 Standard solutions of elements to be tested
In the fourth step, the analysis line of the element to be measured is shown in table 3,
TABLE 3 analysis lines for elements to be tested
| Element(s) | Wavelength of spectral line nm | Observation mode | Element(s) | Wavelength of spectral line nm | Observation mode |
| Fe | 23204 | Level of | Ca | 317.933 | Level of |
| Mg | 27077 | Level of | Cu | 324.752 | Level of |
| Ni | 231.604 | Level of | Mn | 257.610 | Level of |
。
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example one
1 sample dissolution
Weighing 1.0g of sample, placing the sample in a 150mL quartz beaker, adding 5mL of concentrated nitric acid solution, heating and dissolving on a temperature-adjusting electric hot plate at 230-260 ℃, after the sample is completely dissolved, steaming at low temperature to about 3mL, taking down, and cooling to room temperature.
2 separating uranium substrates
The beaker is washed three times by taking 5.5mol/L nitric acid solution as a medium, and the sample is transferred to a quartz separating funnel added with 30mL uranium extraction reagent. Shaking the separating funnel for 30s, standing for 10min, placing the lower layer clear liquid in a balanced reversed phase chromatographic column, receiving the leacheate to a scale with a 10mL quartz volumetric flask, metering the volume, and shaking up.
3 separating the boron matrix
And pouring the received sample into a separating funnel filled with 30mL of boron extraction reagent, shaking the separating funnel for 30s, standing for 10min, putting the liquid below the separating funnel into a second separating funnel filled with 30mL of boron extraction reagent, shaking the separating funnel for 30s, standing for 10min, and collecting the lower layer clear liquid into a 10mL quartz volumetric flask to be tested.
4 preparation of Standard solution
Preliminarily determining that each element to be detected and the analysis range thereof are iron: 10 mu g/g-100 mu g/g; nickel, copper, manganese, calcium, magnesium: 5.0 mu g/g-50 mu g/g.
TABLE 2 Standard solutions of elements to be tested
5 sample detection
The samples were measured by the standard curve method using a plasma emission spectrometer ICP-AES, model Optima5300DV, manufactured by PE.
TABLE 3 analysis lines for elements to be tested
TABLE 4 working conditions of the apparatus
| Item | Require that | Item | Require that |
| RF generator power | 1100 | Flow of carrier gas | 0.80L/min |
| Flow rate of plasma gas | 14L/min | Sample introduction speed | 1.2mL/min |
| Auxiliary gas flow | 0.2L/min | Observation mode | Horizontal observation |
6 calculation of results
The content of impurity elements in the sample is expressed in mass fraction omega in units of micrograms per gram (mu g/g) and is calculated according to the formula (1).
ω＝ωi-ω0…………………………………………(1)
In the formula:
omega-mass fraction of impurity elements in the sample, unit is microgram per gram (mu g/g);
ωi-the mass fraction of impurity elements in the sample is determined by the instrument in units of microgram per gram (μ g/g);
ω0-the mass fraction of impurity elements in the blank is determined by the instrument in micrograms per gram (μ g/g).
If the result is more than or equal to 10 mu g/g, keeping the integer number; if the result is less than 10 mug/g, two significant digits are retained.
7 precision test
Weighing 12 parts of the same sample respectively, and dividing the sample into two groups, wherein one group is used as a background; a lower limit amount of the impurity element to be added; the results of the measurements performed on both sets of samples under the same treatment conditions are given below:
TABLE 5 lower limit recovery and precision of impurity element method
The measurement result shows that the average recovery rate of each element to be detected is between 90% and 110%, the precision is better than 10%, and the detection requirement is met.
Example two
1 sample dissolution
Weighing 1.0g of sample, placing the sample in a 150mL quartz beaker, adding 7.5mL of concentrated nitric acid solution, heating and dissolving on a temperature-adjusting electric hot plate at 230-260 ℃, after the sample is completely dissolved, steaming at low temperature to about 3mL, taking down, and cooling to room temperature.
2 separating uranium substrates
The beaker is washed three times by using 8mol/L nitric acid solution as a medium, and a sample is transferred to a quartz separating funnel added with 35mL uranium extraction reagent. Shaking the separating funnel for 30s, standing for 10min, placing the lower layer clear liquid in a balanced reversed phase chromatographic column, receiving the leacheate to a scale with a 10mL quartz volumetric flask, metering the volume, and shaking up.
3 separating the boron matrix
And pouring the received sample into a separating funnel filled with 35mL of boron extraction reagent, shaking the separating funnel for 30s, standing for 10min, putting the liquid below the separating funnel into a second separating funnel filled with 35mL of boron extraction reagent, shaking the separating funnel for 30s, standing for 10min, and collecting the lower layer clear liquid into a 10mL quartz volumetric flask to be tested.
4 preparation of Standard solution
Preliminarily determining that each element to be detected and the analysis range thereof are iron: 10 mu g/g-100 mu g/g; nickel, copper, manganese, calcium, magnesium: 5.0 mu g/g-50 mu g/g.
TABLE 6 Standard solutions of elements to be tested
5 sample detection
The samples were measured by the standard curve method using a plasma emission spectrometer ICP-AES, model Optima5300DV, manufactured by PE.
TABLE 7 analysis lines for elements to be tested
TABLE 8 Instrument operating conditions
| Item | Require that | Item | Require that |
| RF generator power | 1200W | Flow of carrier gas | 0.83L/min |
| Flow rate of plasma gas | 15L/min | Sample introduction speed | 1.5mL/min |
| Auxiliary gas flow | 0.25L/min | Observation mode | Horizontal observation |
6 calculation of results
The content of impurity elements in the sample is expressed in mass fraction omega in units of micrograms per gram (mu g/g) and is calculated according to the formula (1).
ω＝ωi-ω0…………………………………………(2)
In the formula:
omega-mass fraction of impurity elements in the sample, unit is microgram per gram (mu g/g);
ωi-the mass fraction of impurity elements in the sample is determined by the instrument in units of microgram per gram (μ g/g);
ω0-the mass fraction of impurity elements in the blank is determined by the instrument in micrograms per gram (μ g/g).
If the result is more than or equal to 10 mu g/g, keeping the integer number; if the result is less than 10 mug/g, two significant digits are retained.
7 precision test
Weighing 12 parts of the same sample respectively, and dividing the sample into two groups, wherein one group is used as a background; one group was added with 5 times the lower limit amount of the impurity element, and the two groups of samples were measured under the same treatment conditions, and the results are shown below:
TABLE 9 lower limit recovery and precision of impurity element method
The measurement result shows that the average recovery rate of each element to be detected is between 90% and 110%, the precision is better than 10%, and the detection requirement is met.
EXAMPLE III
1 sample dissolution
Weighing 1.0g of sample, placing the sample in a 150mL quartz beaker, adding 10mL of concentrated nitric acid solution, heating and dissolving on a temperature-adjusting electric hot plate at 230-260 ℃, after the sample is completely dissolved, steaming at low temperature to about 3mL, taking down, and cooling to room temperature.
2 separating uranium substrates
The beaker is washed three times by taking a 10mol/L nitric acid solution as a medium, and a sample is transferred to a quartz separating funnel added with 40mL uranium extraction reagent. Shaking the separating funnel for 30s, standing for 10min, placing the lower layer clear liquid in a balanced reversed phase chromatographic column, receiving the leacheate to a scale with a 10mL quartz volumetric flask, metering the volume, and shaking up.
3 separating the boron matrix
And pouring the received sample into a separating funnel filled with 40mL of boron extraction reagent, shaking the separating funnel for 30s, standing for 10min, putting the liquid below the separating funnel into a second separating funnel filled with 40mL of boron extraction reagent, shaking the separating funnel for 30s, standing for 10min, and collecting the lower layer clear liquid into a 10mL quartz volumetric flask to be tested.
4 preparation of Standard solution
Preliminarily determining that each element to be detected and the analysis range thereof are iron: 10 mu g/g-100 mu g/g; nickel, copper, manganese, calcium, magnesium: 5.0 mu g/g-50 mu g/g.
TABLE 10 Standard solutions of elements to be tested
5 sample detection
The samples were measured by the standard curve method using a plasma emission spectrometer ICP-AES, model Optima5300DV, manufactured by PE.
TABLE 11 analysis lines for elements to be tested
TABLE 12 working conditions of the apparatus
| Item | Require that | Item | Require that |
| RF generator power | 1300W | Flow of carrier gas | 0.85L/min |
| Flow rate of plasma gas | 16L/min | Sample introduction speed | 1.8mL/min |
| Auxiliary gas flow | 0.3L/min | Observation mode | Horizontal observation |
6 calculation of results
The content of impurity elements in the sample is expressed in mass fraction omega in units of micrograms per gram (mu g/g) and is calculated according to the formula (1).
ω＝ωi-ω0…………………………………………(3)
In the formula:
omega-mass fraction of impurity elements in the sample, unit is microgram per gram (mu g/g);
ωi-the mass fraction of impurity elements in the sample is determined by the instrument in units of microgram per gram (μ g/g);
ω0-the mass fraction of impurity elements in the blank is determined by the instrument in micrograms per gram (μ g/g).
If the result is more than or equal to 10 mu g/g, keeping the integer number; if the result is less than 10 mug/g, two significant digits are retained.
7 precision test
Weighing 12 parts of the same sample respectively, and dividing the sample into two groups, wherein one group is used as a background; the amount of the upper limit point of the added impurity element in one group and the measurement of the two groups of samples under the same treatment condition have the following results:
TABLE 13 lower limit recovery and precision of impurity element method
The measurement result shows that the average recovery rate of each element to be detected is between 90% and 110%, the precision is better than 10%, and the detection requirement is met.
Claims (10)
1. The method for determining the content of impurity elements in the uranium boride solid sample is characterized by comprising the following steps of:
step one, sample dissolution;
weighing 1.0g of sample, placing the sample in a 150mL quartz beaker, adding 5-10mL of concentrated nitric acid solution, heating and dissolving the sample, after the sample is completely dissolved, steaming the sample to 2-3mL at low temperature, taking down the sample, and cooling the sample to room temperature;
step two, separating a uranium matrix;
separating uranium matrix in the sample by an extraction method-reversed phase chromatography column method;
step three, separating the boron matrix;
separating the boron matrix by an extraction method;
step four, measuring a sample;
the samples were measured by the standard curve method using ICP-AES.
2. The method for determining the content of impurity elements in a uranium boride solid sample as claimed in claim 1, wherein: the uranium boride solid sample is a uranium boride solid sample.
3. The method for determining the content of impurity elements in a uranium boride solid sample as claimed in claim 1, wherein: in the first step, the concentrated nitric acid is superior pure concentrated nitric acid purified by sub-boiling distillation.
4. The method for determining the content of impurity elements in a uranium boride solid sample as claimed in claim 1, wherein: in the first step, the heating temperature is 230-260 ℃.
5. The method for determining the content of impurity elements in a uranium boride solid sample as claimed in claim 1, wherein: in the second step, the extraction method-reversed phase chromatographic separation column method is used for separating the uranium matrix, firstly, 30-40mL of uranium extraction reagent is adopted to separate uranium in a sample in 5.5-10mol/L nitric acid solution medium, standing is carried out for 10min, the lower layer clear liquid is placed in a well balanced chromatographic separation column, 10mL of volumetric flask is used for receiving leacheate to reach the scale, constant volume is carried out, and shaking is carried out uniformly.
6. The method for determining the content of impurity elements in a uranium boride solid sample according to claim 5, wherein: the uranium extraction reagent is prepared by taking TBP as an extracting agent and xylene as a diluent according to the proportion of 1: 3.
7. The method for determining the content of impurity elements in a uranium boride solid sample as claimed in claim 1, wherein: and in the third step, the extraction method is used for separating the boron matrix, the received sample is poured into a separating funnel filled with 30-40mL of boron extraction reagent, the separating funnel is shaken for 30s and then stands for 10min, then the liquid below the separating funnel is put into a second separating funnel filled with 30-40mL of boron extraction reagent, the separating funnel is shaken for 30s and then stands for 10min, and the lower layer clear liquid is collected into a 10mL quartz volumetric flask to be tested.
8. The method for determining the content of impurity elements in a uranium boride solid sample according to claim 7, wherein: the boron extraction reagent is prepared by taking dimethylbenzene as a diluent and 2-ethyl-1, 3-hexanediol as an extracting agent according to the proportion of 1: 1.
9. The method for determining the content of impurity elements in a uranium boride solid sample as claimed in claim 1, wherein: in the fourth step, the ICP-AES is manufactured by PE with model number Optima5300 DV.
10. The method for determining the content of impurity elements in a uranium boride solid sample as claimed in claim 1, wherein: in the fourth step, the ICP-AES working conditions, as shown in Table 1,
TABLE 1 working conditions of the apparatus
；
In the fourth step, the elements to be measured are Fe, Ni, Cu, Mg, Ca, Mn, Si and Al, the concentration of the standard series solution is shown in Table 2,
TABLE 2 Standard solutions of elements to be tested
In the fourth step, the analysis line of the element to be measured is shown in table 3,
TABLE 3 analysis lines for elements to be tested
。
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