CN108303308A - The assay method of 10 kinds of impurity elements in a kind of U-Al alloy - Google Patents

The assay method of 10 kinds of impurity elements in a kind of U-Al alloy Download PDF

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CN108303308A
CN108303308A CN201711452445.3A CN201711452445A CN108303308A CN 108303308 A CN108303308 A CN 108303308A CN 201711452445 A CN201711452445 A CN 201711452445A CN 108303308 A CN108303308 A CN 108303308A
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sample
alloy
kinds
impurity elements
solution
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马妍琳
赵竹霞
董世哲
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China North Nuclear Fuel Co Ltd
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China North Nuclear Fuel Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38—Diluting, dispersing or mixing samples
    • 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

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Abstract

The present invention relates to a kind of assay method of 10 kinds of impurity elements in U-Al alloy, described 10 kinds of impurity elements are Fe, Mg, Mn, Zn, Cd, B, Ni, Ti, Cu and Li；It the described method comprises the following steps 1) sample dissolving；2) serial mixed standard solution preparation；3) sample measures；The present invention establishes the detection method of 10 kinds of impurity elements in Coupled Plasma-Atomic Emission Spectrometric Determination U-Al alloy, the content of each impurity element can be accurately measured using the experiment condition enumerated in invention content, accurate detection data has been quoted, the progress of special production has effectively been coordinated.

Description

The assay method of 10 kinds of impurity elements in a kind of U-Al alloy
Technical field
The invention belongs to chemical detection method fields, and in particular to a kind of survey of 10 kinds of impurity elements in U-Al alloy Determine method.
Background technology
U-Al alloy has in nucleus product and is widely applied as emerging nuclear fuel, and temporarily nothing domestic at present has Close the pertinent literature of defects inspecting in U-Al alloy；Due to involved in method to 10 in how many pairs of alloys of impurity content Crystallisation procedure, plasticity and improve cutting ability etc. and have a great impact, therefore, in 10 in Accurate Determining method The content of impurity element coordinates the production task of U-Al alloy, better accurate instruction technique to melt out satisfactory conjunction Gold；Investigation through condition experiment herein establishes iron in U-Al alloy, and 10 kinds of cadmium, magnesium, manganese, zinc, boron, nickel, titanium, copper, lithium etc. is miscellaneous The detection regulation of prime element.
Invention content
It is an object of the invention to：According to detection requirements of one's work, based on the existing instrument and equipment in laboratory, establish etc. Ionomer emission spectrum method measures the detection method of 10 kinds of impurity contents in U-Al alloy, meets scientific research, production detects Demand.
Technical scheme is as follows：The assay method of 10 kinds of impurity elements in a kind of U-Al alloy, described 10 kinds Impurity element is Fe, Mg, Mn, Zn, Cd, B, Ni, Ti, Cu and Li；It the described method comprises the following steps
1) sample dissolves
U-Al alloy sample 0.25g accurately is weighed, the quartz that U-Al alloy sample is placed in 100mL after weighing is burnt In cup, 15mL A hydrochloric acid solutions, 5mL A salpeter solutions is added, is dissolved by heating on temp.-adjustable electric hot plate；Wait for that sample all dissolves Afterwards, low temperature is steamed to a small amount of, is removed and is cooled to room temperature；Using B salpeter solutions as medium, the quartzy capacity of 25mL is shifted and is settled to In bottle；Above-mentioned solution 10mL is taken, added in the quartzy separatory funnel of 20mL extractants and diluent, to shake separatory funnel in 10min is stood after 30s, and water phase is transferred in the 25mL quartz beakers of drying after layering completely, it is to be measured；
2) serial mixed standard solution preparation
Respectively using salpeter solution as medium, it is molten to be configured to hybrid standard series with the standard solution of each single element to be measured Liquid is shown in Table 1：
1 impurity element standard serial solution of table
3) sample measures
After plasma emission spectrometer preheats successfully, according to File-Open-Method's in the software of equipment Sequentially, selection needs method to be used, clicks " OK " key and opens；Test front opening Results Data Set, input file Name preserves experimental data test result caused by prevent instrument or computer glitch and loses, igniting button clicked, according to as follows Step is detected：
1. analysis margin：Sample feeding pipe is put into blank, " Analyze Blank " key analysis blank is clicked；
2. analytical standard sample：Sample feeding pipe is sequentially placed into standard solution, " Analyze Standard " analysis is clicked Corresponding concentration of standard solution, midpoint " Conc " button can see the concentration of corresponding standard solution；
3. analyzing sample：Sample feeding pipe is put into sample to be tested, " Analyze Sample " is clicked and analyzes solution to be measured In each element to be measured concentration；
4. preserving result：Automatically save data；
5. the testing result that instrument exports is recorded in original record.
A hydrochloric acid solutions described in step 1) use the concentrated hydrochloric acid and water volume ratio 1 by sub-boiling distillation:1 is matched It sets.
A salpeter solutions described in step 1), for by the concentrated nitric acid of sub-boiling distillation.
Solution temperature described in step 1) is 230 DEG C~260 DEG C.
As not being completely dissolved in step 1), 2mL hydrochloric acid solutions and 1mL salpeter solutions are added, continues to dissolve by heating.
A concentration of 4.5-6.5mol/L of B salpeter solutions described in step 1).
Extractant and diluent described in step 1) are tributyl phosphate and dimethylbenzene, tributyl phosphate：Dimethylbenzene= 1:3。
PE companies of the model U.S. production of plasma emission spectrometer used in step 3) Optima5300DV。
The line wavelength of each impurity element described in step 3) is：Fe 238.204nm, B249.772nm, Cd361.051nm, Ni221.648nm, Mg285.213nm, Ti334.940nm, Mn257.610nm, Cu327.393nm, Zn330.258nm, Li670.784nm.
Instrument operating condition described in step 3) is：RF generator powers are 1100~1300W, and carrier gas flux is 0.80~0.85L/min, plasma gas flow rate are 14~16L/min, and sample introduction speed is 1.2~1.8mL/min, secondary air Amount is 0.2~0.3L/min, and observed pattern is horizontal observes.
The remarkable result of the present invention is：Establish 10 kinds of impurity in Coupled Plasma-Atomic Emission Spectrometric Determination U-Al alloy The detection method of element can accurately be measured the content of each impurity element using the experiment condition enumerated in invention content, be quoted Accurate detection data, has effectively coordinated the progress of special production.
Specific implementation mode
With reference to specific embodiment to the assay method of 10 kinds of impurity elements in a kind of U-Al alloy of the present invention It is described in further detail.
The assay method of 10 kinds of impurity elements in a kind of U-Al alloy, described 10 kinds of impurity elements are Fe, Mg, Mn, Zn, Cd, B, Ni, Ti, Cu and Li；It the described method comprises the following steps
1) sample dissolves
U-Al alloy sample 0.25g accurately is weighed, the quartz that U-Al alloy sample is placed in 100mL after weighing is burnt In cup, 15mL A hydrochloric acid solutions, 5mL A salpeter solutions is added, is dissolved by heating on temp.-adjustable electric hot plate, the solution temperature It is 230 DEG C~260 DEG C, is not completely dissolved such as, adds 2mL hydrochloric acid solutions and 1mL salpeter solutions, continue to dissolve by heating；It waits trying All after dissolving, low temperature is steamed to a small amount of sample, is removed and is cooled to room temperature；Using B salpeter solutions as medium, shifts and be settled to 25mL Quartzy volumetric flask in；Above-mentioned solution 10mL is taken, added in the quartzy separatory funnel of 20mL extractants and diluent, to be shaken in 10min is stood after separatory funnel 30s, water phase is transferred in the 25mL quartz beakers of drying after layering completely, it is to be measured；
The A hydrochloric acid solutions use the concentrated hydrochloric acid and water volume ratio 1 by sub-boiling distillation:1 is configured；Described A salpeter solutions, for by the concentrated nitric acid of sub-boiling distillation；A concentration of 4.5-6.5mol/L of the B salpeter solutions；Described Extractant and diluent are tributyl phosphate and dimethylbenzene, tributyl phosphate：Dimethylbenzene=1:3.
2) serial mixed standard solution preparation
Respectively using salpeter solution as medium, it is molten to be configured to hybrid standard series with the standard solution of each single element to be measured Liquid is shown in Table 2：
2 impurity element standard serial solution of table
3) sample measures
After plasma emission spectrometer preheats successfully, according to File-Open-Method's in the software of equipment Sequentially, selection needs method to be used, clicks " OK " key and opens；Test front opening Results Data Set, input file Name preserves experimental data test result caused by prevent instrument or computer glitch and loses, igniting button clicked, according to as follows Step is detected：
6. analysis margin：Sample feeding pipe is put into blank, " Analyze Blank " key analysis blank is clicked；
7. analytical standard sample：Sample feeding pipe is sequentially placed into standard solution, " Analyze Standard " analysis is clicked Corresponding concentration of standard solution, midpoint " Conc " button can see the concentration of corresponding standard solution；
8. analyzing sample：Sample feeding pipe is put into sample to be tested, " Analyze Sample " is clicked and analyzes solution to be measured In each element to be measured concentration；
9. preserving result：Automatically save data；
10. the testing result that instrument exports is recorded in original record.
PE companies of the model U.S. production of plasma emission spectrometer used in step 3) Optima5300DV；
The line wavelength of each impurity element described in step 3) is：Fe 238.204nm, B249.772nm, Cd361.051nm, Ni221.648nm, Mg285.213nm, Ti334.940nm, Mn257.610nm, Cu327.393nm, Zn330.258nm, Li670.784nm；
Instrument operating condition described in step 3) is：RF generator powers are 1100~1300W, and carrier gas flux is 0.80~0.85L/min, plasma gas flow rate are 14~16L/min, and sample introduction speed is 1.2~1.8mL/min, secondary air Amount is 0.2~0.3L/min, and observed pattern is horizontal observes.
Embodiment one
1) sample dissolves
U-Al alloy sample 0.25g accurately is weighed, sample is placed in the quartz beaker of 100mL after weighing, and is added 15mL hydrochloric acid solutions, 5mL salpeter solutions are dissolved by heating on 230 DEG C of temp.-adjustable electric hot plates, are not completely dissolved such as, can be added 2mL hydrochloric acid solutions and 1mL salpeter solutions), after sample all dissolving, low temperature is steamed to a small amount of, is removed, is cooled to room temperature, with The salpeter solution of 4.5mol/L is medium, shifts and is settled in the quartzy volumetric flask of 25mL.Dividing takes above-mentioned solution 10mL in In quartzy separatory funnel added with 20mL extractants.10min is stood after shaking separatory funnel 30s, by water phase after layering completely It is transferred in the 25mL quartz beakers of drying, it is to be measured.
2) serial mixed standard solution
Respectively using salpeter solution as medium, it is molten to be configured to hybrid standard series with the standard solution of each single element to be measured Liquid is shown in Table 3.
3 elemental standards serial solution to be measured of table
3) sample measures
After plasma emission spectrometer preheats successfully, according to File-Open-Method's in the software of equipment Sequentially, selection needs method to be used, clicks " OK " key and opens；Test front opening Results Data Set, input file Name preserves experimental data test result caused by prevent instrument or computer glitch and loses, igniting button clicked, according to as follows Step is detected：
1. analysis margin：Sample feeding pipe is put into blank, " Analyze Blank " key analysis blank is clicked；
2. analytical standard sample：Sample feeding pipe is sequentially placed into standard solution, " Analyze Standard " analysis is clicked Corresponding concentration of standard solution, midpoint " Conc " button can see the concentration of corresponding standard solution；
3. analyzing sample：Sample feeding pipe is put into sample to be tested, " Analyze Sample " is clicked and analyzes solution to be measured In each element to be measured concentration；
4. preserving result：Automatically save data；
5. the testing result that instrument exports is recorded in original record.
PE companies of the model U.S. production of plasma emission spectrometer used in step 3) Optima5300DV；
The line wavelength of each impurity element described in step 3) is：Fe 238.204nm, B249.772nm, Cd361.051nm, Ni221.648nm, Mg285.213nm, Ti334.940nm, Mn257.610nm, Cu327.393nm, Zn330.258nm, Li670.784nm；
Instrument operating condition described in step 3) is：RF generator powers are 1100~1300W, and carrier gas flux is 0.80~0.85L/min, plasma gas flow rate are 14~16L/min, and sample introduction speed is 1.2~1.8mL/min, secondary air Amount is 0.2~0.3L/min, and observed pattern is horizontal observes.
As a result it calculates
Impurity content is indicated with mass fraction ω in sample, and unit is μ g/g, is calculated by formula (1).
ω=ωi-ω0…………………………………………(1)
In formula：
ω --- the mass fraction of impurity element to be measured in sample, unit are every gram of microgram (μ g/g)；
ωi--- Instrument measuring goes out the mass fraction of impurity element to be measured in sample, and unit is every gram of microgram (μ g/g)；
ω0--- Instrument measuring goes out the mass fraction of impurity element to be measured in blank, and unit is every gram of microgram (μ g/g).
If the μ g/g of result >=10 retain to integer-bit；If 10 μ g/g of result ＜, retain two effective digitals.As a result it calculates
U-Al alloy is handled according to above-mentioned detection method, weighs 7 parts of same sample respectively, one group as background (content of each element to be measured is respectively less than lower limit in sample, therefore the content of each element lower limit is added on the basis of raw sample Afterwards as background)；Remaining the six parts amounts that each elemental standard solution lower-limit point to be measured is added；By two groups of samples in identical processing Under the conditions of be measured, measurement result is shown in Table 4.
4 precision of table and the rate of recovery
As seen from the above table, the method precision is better than 10%, and the rate of recovery meets detection and want between 92%~107% It asks.
Embodiment two
1) sample dissolves
U-Al alloy sample 0.25g accurately is weighed, sample is placed in the quartz beaker of 100mL after weighing, and is added 15mL hydrochloric acid solutions, 5mL salpeter solutions are dissolved by heating on 250 DEG C of temp.-adjustable electric hot plates, are not completely dissolved such as, can be added 2mL hydrochloric acid solutions and 1mL salpeter solutions), after sample all dissolving, low temperature is steamed to a small amount of, is removed, is cooled to room temperature, with The salpeter solution of 5.5mol/L is medium, shifts and is settled in the quartzy volumetric flask of 25mL.Dividing takes above-mentioned solution 10mL in In quartzy separatory funnel added with 20mL extractants.10min is stood after shaking separatory funnel 30s, by water phase after layering completely It is transferred in the 25mL quartz beakers of drying, it is to be measured.
2) serial mixed standard solution
Respectively using salpeter solution as medium, it is molten to be configured to hybrid standard series with the standard solution of each single element to be measured Liquid is shown in Table 5.
5 elemental standards serial solution to be measured of table
3) sample measures
After plasma emission spectrometer preheats successfully, according to File-Open-Method's in the software of equipment Sequentially, selection needs method to be used, clicks " OK " key and opens；Test front opening Results Data Set, input file Name preserves experimental data test result caused by prevent instrument or computer glitch and loses, igniting button clicked, according to as follows Step is detected：
1. analysis margin：Sample feeding pipe is put into blank, " Analyze Blank " key analysis blank is clicked；
2. analytical standard sample：Sample feeding pipe is sequentially placed into standard solution, " Analyze Standard " analysis is clicked Corresponding concentration of standard solution, midpoint " Conc " button can see the concentration of corresponding standard solution；
3. analyzing sample：Sample feeding pipe is put into sample to be tested, " Analyze Sample " is clicked and analyzes solution to be measured In each element to be measured concentration；
4. preserving result：Automatically save data；
5. the testing result that instrument exports is recorded in original record.
PE companies of the model U.S. production of plasma emission spectrometer used in step 3) Optima5300DV；
The line wavelength of each impurity element described in step 3) is：Fe 238.204nm, B249.772nm, Cd361.051nm, Ni221.648nm, Mg285.213nm, Ti334.940nm, Mn257.610nm, Cu327.393nm, Zn330.258nm, Li670.784nm；
Instrument operating condition described in step 3) is：RF generator powers are 1100~1300W, and carrier gas flux is 0.80~0.85L/min, plasma gas flow rate are 14~16L/min, and sample introduction speed is 1.2~1.8mL/min, secondary air Amount is 0.2~0.3L/min, and observed pattern is horizontal observes.
As a result it calculates
Impurity content is indicated with mass fraction ω in sample, and unit is μ g/g, is calculated by formula (1).
ω=ωi-ω0…………………………………………(2)
In formula：
ω --- the mass fraction of impurity element to be measured in sample, unit are every gram of microgram (μ g/g)；
ωi--- Instrument measuring goes out the mass fraction of impurity element to be measured in sample, and unit is every gram of microgram (μ g/g)；
ω0--- Instrument measuring goes out the mass fraction of impurity element to be measured in blank, and unit is every gram of microgram (μ g/g).
If the μ g/g of result >=10 retain to integer-bit；If 10 μ g/g of result ＜, retain two effective digitals.As a result it calculates
U-Al alloy is handled according to above-mentioned detection method, weighs 7 parts of same sample respectively, one group as background (content of each element to be measured is respectively less than lower limit in sample, therefore the content of each element lower limit is added on the basis of raw sample Afterwards as background)；Remaining the six parts amounts that each elemental standard solution lower-limit point to be measured is added；By two groups of samples in identical processing Under the conditions of be measured, measurement result is shown in Table 6.
6 precision of table and the rate of recovery
As seen from the above table, the method precision is better than 10%, and the rate of recovery meets detection and want between 92%~105% It asks.
Embodiment three
1) sample dissolves
U-Al alloy sample 0.25g accurately is weighed, sample is placed in the quartz beaker of 100mL after weighing, and is added 15mL hydrochloric acid solutions, 5mL salpeter solutions are dissolved by heating on 260 DEG C of temp.-adjustable electric hot plates, are not completely dissolved such as, can be added 2mL hydrochloric acid solutions and 1mL salpeter solutions), after sample all dissolving, low temperature is steamed to a small amount of, is removed, is cooled to room temperature, with The salpeter solution of 6.5mol/L is medium, shifts and is settled in the quartzy volumetric flask of 25mL.Dividing takes above-mentioned solution 10mL in In quartzy separatory funnel added with 20mL extractants.10min is stood after shaking separatory funnel 30s, by water phase after layering completely It is transferred in the 25mL quartz beakers of drying, it is to be measured.
2) serial mixed standard solution
Respectively using salpeter solution as medium, it is molten to be configured to hybrid standard series with the standard solution of each single element to be measured Liquid is shown in Table 7.
7 elemental standards serial solution to be measured of table
3) sample measures
After plasma emission spectrometer preheats successfully, according to File-Open-Method's in the software of equipment Sequentially, selection needs method to be used, clicks " OK " key and opens；Test front opening Results Data Set, input file Name preserves experimental data test result caused by prevent instrument or computer glitch and loses, igniting button clicked, according to as follows Step is detected：
1. analysis margin：Sample feeding pipe is put into blank, " Analyze Blank " key analysis blank is clicked；
2. analytical standard sample：Sample feeding pipe is sequentially placed into standard solution, " Analyze Standard " analysis is clicked Corresponding concentration of standard solution, midpoint " Conc " button can see the concentration of corresponding standard solution；
3. analyzing sample：Sample feeding pipe is put into sample to be tested, " Analyze Sample " is clicked and analyzes solution to be measured In each element to be measured concentration；
4. preserving result：Automatically save data；
5. the testing result that instrument exports is recorded in original record.
PE companies of the model U.S. production of plasma emission spectrometer used in step 3) Optima5300DV；
The line wavelength of each impurity element described in step 3) is：Fe 238.204nm, B249.772nm, Cd361.051nm, Ni221.648nm, Mg285.213nm, Ti334.940nm, Mn257.610nm, Cu327.393nm, Zn330.258nm, Li670.784nm；
Instrument operating condition described in step 3) is：RF generator powers are 1100~1300W, and carrier gas flux is 0.80~0.85L/min, plasma gas flow rate are 14~16L/min, and sample introduction speed is 1.2~1.8mL/min, secondary air Amount is 0.2~0.3L/min, and observed pattern is horizontal observes.
As a result it calculates
Impurity content is indicated with mass fraction ω in sample, and unit is μ g/g, is calculated by formula (1).
ω=ωi-ω0…………………………………………(3)
In formula：
ω --- the mass fraction of impurity element to be measured in sample, unit are every gram of microgram (μ g/g)；
ωi--- Instrument measuring goes out the mass fraction of impurity element to be measured in sample, and unit is every gram of microgram (μ g/g)；
ω0--- Instrument measuring goes out the mass fraction of impurity element to be measured in blank, and unit is every gram of microgram (μ g/g).
If the μ g/g of result >=10 retain to integer-bit；If 10 μ g/g of result ＜, retain two effective digitals.As a result it calculates
U-Al alloy is handled according to above-mentioned detection method, weighs 7 parts of same sample respectively, one group as background (content of each element to be measured is respectively less than lower limit in sample, therefore the content of each element lower limit is added on the basis of raw sample Afterwards as background)；Remaining the six parts amounts that each elemental standard solution lower-limit point to be measured is added；By two groups of samples in identical processing Under the conditions of be measured, measurement result is shown in Table 8.
8 precision of table and the rate of recovery
As seen from the above table, the method precision is better than 10%, and the rate of recovery meets detection and want between 92%~107% It asks.

Claims (10)

1. the assay method of 10 kinds of impurity elements in a kind of U-Al alloy, it is characterised in that：10 kinds of impurity elements be Fe, Mg, Mn, Zn, Cd, B, Ni, Ti, Cu and Li；It the described method comprises the following steps
1) sample dissolves
U-Al alloy sample 0.25g accurately is weighed, U-Al alloy sample is placed in the quartz beaker of 100mL after weighing, 15mL A hydrochloric acid solutions, 5mL A salpeter solutions is added, is dissolved by heating on temp.-adjustable electric hot plate；After sample all dissolving, low temperature It steams to a small amount of, removes and be cooled to room temperature；Using B salpeter solutions as medium, shifts and be settled in the quartzy volumetric flask of 25mL；It takes Solution 10mL is stated, added in the quartzy separatory funnel of 20mL extractants and diluent, to stand after shaking separatory funnel 30s in Water phase is transferred in the 25mL quartz beakers of drying by 10min after layering completely, to be measured；
2) serial mixed standard solution preparation
Respectively using salpeter solution as medium, it is configured to hybrid standard serial solution with the standard solution of each single element to be measured, is seen Table 1：
1 impurity element standard serial solution of table
3) sample measures
After plasma emission spectrometer preheats successfully, according to the sequence of File-Open-Method in the software of equipment, Selection needs method to be used, clicks " OK " key and opens；Front opening Results Data Set are tested, import file name preserves Experimental data test result caused by prevent instrument or computer glitch is lost, and is clicked igniting button, is carried out in accordance with the following steps Detection：
1. analysis margin：Sample feeding pipe is put into blank, " Analyze Blank " key analysis blank is clicked；
2. analytical standard sample：Sample feeding pipe is sequentially placed into standard solution, " Analyze Standard " analysis is clicked and corresponds to Concentration of standard solution, midpoint " Conc " button can see the concentration of corresponding standard solution；
3. analyzing sample：Sample feeding pipe is put into sample to be tested, " Analyze Sample " is clicked and analyzes in solution to be measured respectively The concentration of element to be measured；
4. preserving result：Automatically save data；
5. the testing result that instrument exports is recorded in original record.
2. the assay method of 10 kinds of impurity elements in a kind of U-Al alloy as described in claim 1, it is characterised in that：Step 1) Described in A hydrochloric acid solutions, use concentrated hydrochloric acid and the water volume ratio 1 by sub-boiling distillation:1 is configured.
3. the assay method of 10 kinds of impurity elements in a kind of U-Al alloy as described in claim 1, it is characterised in that：Step 1) Described in A salpeter solutions, for by sub-boiling distillation concentrated nitric acid.
4. the assay method of 10 kinds of impurity elements in a kind of U-Al alloy as described in claim 1, it is characterised in that：Step 1) Described in solution temperature be 230 DEG C~260 DEG C.
5. the assay method of 10 kinds of impurity elements in a kind of U-Al alloy as described in claim 1, it is characterised in that：Step 1) In as not being completely dissolved, add 2mL hydrochloric acid solutions and 1mL salpeter solutions, continue to dissolve by heating.
6. the assay method of 10 kinds of impurity elements in a kind of U-Al alloy as described in claim 1, it is characterised in that：Step 1) Described in B salpeter solutions a concentration of 4.5-6.5mol/L.
7. the assay method of 10 kinds of impurity elements in a kind of U-Al alloy as described in claim 1, it is characterised in that：Step 1) Described in extractant and diluent be tributyl phosphate and dimethylbenzene, tributyl phosphate：Dimethylbenzene=1:3.
8. the assay method of 10 kinds of impurity elements in a kind of U-Al alloy as described in claim 1, it is characterised in that：Step 3) Used in plasma emission spectrometer PE companies of the model U.S. production Optima5300DV.
9. the assay method of 10 kinds of impurity elements in a kind of U-Al alloy as described in claim 1, it is characterised in that：Step 3) Described in the line wavelength of each impurity element be：Fe 238.204nm, B249.772nm, Cd361.051nm, Ni221.648nm, Mg285.213nm, Ti334.940nm, Mn257.610nm, Cu327.393nm, Zn330.258nm, Li670.784nm。
10. the assay method of 10 kinds of impurity elements in a kind of U-Al alloy as described in claim 1, it is characterised in that：Step 3) the instrument operating condition described in is：RF generator powers are 1100~1300W, and carrier gas flux is 0.80~0.85L/min, Plasma gas flow rate is 14~16L/min, and sample introduction speed is 1.2~1.8mL/min, and secondary air amount is 0.2~0.3L/min, Observed pattern is horizontal observes.
CN201711452445.3A 2017-12-28 2017-12-28 The assay method of 10 kinds of impurity elements in a kind of U-Al alloy Pending CN108303308A (en)

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