CN105823821A - Determination method for contents of impurity elements in thorium tetrafluoride powder - Google Patents
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Abstract
The invention provides a determination method for the contents of impurity elements in thorium tetrafluoride powder. The determination method can determine 37 elements consisting of iron, aluminum, nickel, tin, zirconium, tungsten, silicon, arsenic, boron, calcium, cadmium, niobium, lead, magnesium, manganese, molybdenum, zinc, cobalt, chromium, copper, titanium, vanadium and rare earth element lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, terbium and yttrium. According to the method, the determination method for the contents of 37 impurity elements in thorium tetrafluoride is successively established; in virtue of experimental condition listed in the specification, the contents of the impurity elements in thorium tetrafluoride can be accurately determined; so requirements of production and scientific research for detection of the impurity elements in thorium tetrafluoride are met.
Description
Technical field
The invention belongs to set up the chemical detection method of impurity in thorium tetrafluoride powder, be specifically related to using plasma mass spectrography in thorium tetrafluoride 37 kinds of methods that impurity content is measured.
Background technology
Thorio MSR is to utilize thorium tetrafluoride and thorium anhydride as primary raw material, the height of impurity content and the quality of physical property in thorium anhydride and thorium tetrafluoride, directly influence its performance as nuclear fuel in use element, even have influence on the safe operation of nuclear reactor.Both at home and abroad about the not disclosed report of the achievement in research of impurity content assay method in thorium tetrafluoride.
Summary of the invention
It is an object of the invention to select according to thorium tetrafluoride sample dissolution, analysis condition, set up ferrum in thorium tetrafluoride, aluminum, nickel, stannum, zirconium, tungsten, arsenic, boron, calcium, cadmium, niobium, lead, magnesium, manganese, molybdenum, zinc, cobalt, chromium, copper, titanium, vanadium, the detection method that rare-earth elements of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, thulium, ytterbium, lutecium, terbium, 37 kinds of impurity contents of yttrium measure.
Realize the technical scheme of the object of the invention: impurity content assay method in a kind of thorium tetrafluoride powder, it comprises the steps:
For ferrum, aluminum, nickel, stannum, zirconium, tungsten, 7 kinds of element determinations of silicon:
Weigh 0.1～0.5 gram of thorium tetrafluoride sample to be placed in the quartz beaker of 150mL, add 50mL nitric acid, 0.5mL acetonitrile, cover quartz surfaces ware heating for dissolving on temp.-adjustable electric hot plate；
After being completely dissolved, solution is steamed to the most dry, add 2mL, c (HNO3The salpeter solution of)=3mol/L, transfers to after being cooled to room temperature to have added in the 60mL separatory funnel of 20mL extractant；Described extractant is ψ (dimethylbenzene: tributyl phosphate)=3:1；
Aqueous phase is put in 100mL volumetric flask after being layered completely by extractant, is that 1% salpeter solution is diluted to scale by percent by volume, it is thus achieved that sample solution；
Then, on icp ms, use nebulization sampling mode, add rhodium-indium mixing inner mark solution, the drift being Internal standard correction methods instrument signal with rhodium online；
Measure series standard solution, draw standard curve, measure blank solution and sample solution the most respectively, calculate the content of each element to be measured in sample.
As above impurity content assay method in a kind of thorium tetrafluoride powder, it comprises the steps: for arsenic, boron, calcium, cadmium, niobium, lead, magnesium, manganese, molybdenum, zinc, cobalt, chromium, copper, titanium, vanadium, rare-earth elements of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, thulium, ytterbium, lutecium, terbium, 30 kinds of element determinations of yttrium；
Weighing 0.1g thorium tetrafluoride sample, be placed in the quartz beaker of 150mL, add 50mL nitric acid, 0.5mL acetonitrile covers quartz surfaces ware heating for dissolving on temp.-adjustable electric hot plate；
After being completely dissolved, solution is steamed to the most dry, add 2mL, c (HNO3The salpeter solution of)=3mol/L, is transferred to after being cooled to room temperature in 100mL volumetric flask, is that 1% salpeter solution is diluted to scale by percent by volume；Take 10mL sample solution in 50mL volumetric flask, be that 1% salpeter solution is diluted to scale by percent by volume；
On icp ms, use nebulization sampling mode, add rhodium-indium mixing inner mark solution online, titanium, vanadium, chromium, nickel, copper, arsenic, zirconium with indium as internal standard, the drift that other element is Internal standard correction methods instrument signal with rhodium；
Measure series standard solution, draw standard curve, measure blank solution and sample solution the most respectively, calculate the content of each element to be measured in sample.
Impurity content assay method in a kind of thorium tetrafluoride powder as above, it interferes situation preparation series standard solution by each co-existing element interference and solution system, as shown in Table 1 and Table 2.
Table 1 series standard solution
Table 2 series standard solution
Impurity content assay method in a kind of thorium tetrafluoride powder as above,
When sampling amount is 0.1g～0.5g, the analyst coverage of each element:
As, Nb, Ni, Sn, Zn, Cr, Cu, Zr, Ti, V, W are 1 μ g/g～100 μ g/g；
B, Cd, Co, Mo, Mn are 0.1 μ g/g～10 μ g/g；
Pb is 5 μ g/g～250 μ g/g；
Al, Fe, Mg, Ca, Si are 20 μ g/g～200 μ g/g；
Sm, Eu, Gd, Dy are 0.05 μ g/g～2.5 μ g/g；
La, Ce, Pr, Nd, Ho, Er, Tm, Tb, Yb, Lu, Y are 0.5 μ g/g～25 μ g/g.
Impurity content assay method in a kind of thorium tetrafluoride powder as above, its described addition 50mL nitric acid, this nitric acid is that top grade is pure, 15.5mol/L.
Effect of the invention is that: the present invention has been successfully established the detection method of 37 kinds of impurity contents in thorium tetrafluoride, utilize the experiment condition enumerated in summary of the invention can to meet produce and the requirement of impurity content detection in scientific research thorium tetrafluoride with impurity content (scope is shown in Table 1) in Accurate Determining thorium tetrafluoride.
Detailed description of the invention
Below in conjunction with specific embodiment to impurity content assay method in a kind of thorium tetrafluoride powder of the present invention.
Embodiment 1
37 kinds of impurity content assay methods in a kind of thorium tetrafluoride powder of the present invention, it comprises the steps:
(1) for ferrum, aluminum, nickel, stannum, zirconium, tungsten, 7 kinds of element determinations of silicon
Weigh 0.3000 gram of thorium tetrafluoride sample to be placed in the quartz beaker of 150mL, add 50mL nitric acid (top grade is pure, 15.5mol/L), 0.5mL acetonitrile, cover quartz surfaces ware heating for dissolving on temp.-adjustable electric hot plate；
After being completely dissolved, solution is steamed to the most dry, add 2mL, c (HNO3The salpeter solution of)=3mol/L, transfers to after being cooled to room temperature to have added in the 60mL separatory funnel of 20mL extractant；Described extractant is ψ (dimethylbenzene: tributyl phosphate)=3:1；
Aqueous phase is put in 100mL volumetric flask after being layered completely by extractant, is diluted to scale with 1% (volume parts) salpeter solution, it is thus achieved that sample solution；
Then, on icp ms, use nebulization sampling mode, add rhodium-indium mixing inner mark solution, the drift being Internal standard correction methods instrument signal with rhodium online；
Measure series standard solution, draw standard curve, measure blank solution and sample solution the most respectively, calculate the content of each element to be measured in sample；
(2) other 30 kinds of element determinations
Arsenic, boron, calcium, cadmium, niobium, lead, magnesium, manganese, molybdenum, zinc, cobalt, chromium, copper, titanium, vanadium, rare-earth elements of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, thulium, ytterbium, lutecium, terbium, yttrium；
Weighing 0.1g thorium tetrafluoride sample, be placed in the quartz beaker of 150mL, add 50mL nitric acid, 0.5mL acetonitrile covers quartz surfaces ware heating for dissolving on temp.-adjustable electric hot plate；
After being completely dissolved, solution is steamed to the most dry, add 2mL, c (HNO3The salpeter solution of)=3mol/L, is transferred to after being cooled to room temperature in 100mL volumetric flask, is diluted to scale with 1% (volume parts) salpeter solution；Take 10mL sample solution in 50mL volumetric flask, be diluted to scale with 1% (volume parts) salpeter solution；
On icp ms, use nebulization sampling mode, add rhodium-indium mixing inner mark solution online, titanium, vanadium, chromium, nickel, copper, arsenic, zirconium with indium as internal standard, the drift that other element is Internal standard correction methods instrument signal with rhodium；
Measure series standard solution, draw standard curve, measure blank solution and sample solution the most respectively, calculate the content of each element to be measured in sample.
Situation preparation series standard solution is interfered, as shown in Table 1 and Table 2 by each co-existing element interference and solution system.
Table 1 series standard solution
Table 2 series standard solution
When sampling amount is 0.1g～0.5g, the analyst coverage of each element:
As, Nb, Ni, Sn, Zn, Cr, Cu, Zr, Ti, V, W are 1 μ g/g～100 μ g/g；
B, Cd, Co, Mo, Mn are 0.1 μ g/g～10 μ g/g；
Pb is 5 μ g/g～250 μ g/g；
Al, Fe, Mg, Ca, Si are 20 μ g/g～200 μ g/g；
Sm, Eu, Gd, Dy are 0.05 μ g/g～2.5 μ g/g；
La, Ce, Pr, Nd, Ho, Er, Tm, Tb, Yb, Lu, Y are 0.5 μ g/g～25 μ g/g.
The present invention weighs 0.1000～0.5000 gram of thorium tetrafluoride sample and carries out dissolution experiment, is respectively adopted ammonium carbonate, nitric acid and hydrochloric acid, concentrated nitric acid and perchloric acid, concentrated nitric acid, and the method such as aluminum chloride-hydrochloric acid and aluminum chloride-nitric acid carries out molten sample test.Thorium tetrafluoride in a heated condition, also can make it be completely dissolved with concentrated nitric acid, aluminum chloride-hydrochloric acid and aluminum chloride-nitric acid.But use aluminum chloride can introduce a large amount of aluminum, increase defects inspecting difficulty, thus select to use concentrated nitric acid to dissolve.
In mass spectrography detection, matrix interference is main interference.Thus, need to select suitable matrix concentration to ensure that in sample, impurity element suppression situation is stable during detection.
By to same sample, choose 0.1,0.2,0.3,0.4,0.5,1.0mg/mL different matrix concentration carry out contrast test, internal standard is more obvious by thorium matrix inhibitory effect, when 1.0mg/mL, has already decreased between 10%～25%.Matrix concentration is when 0.2mg/mL, and in sample, the impurity response rate is relatively preferable, therefore selects matrix concentration 0.2mg/mL.
Separated by matrix, by thorium matrix and separation of foreign elements, can effectively reduce matrix interference.It is respectively adopted tributyl phosphate dimethylbenzene, tributyl phosphate carbon tetrachloride extraction agent extract and separate matrix thorium, to 0.1g sample respectively under the nitric acid medium of 1mol/L, 2mol/L, 3mol/L, 4mol/L, 5mol/L, 6mol/L, 7mol/L, with 20mL extractant extract once, 20mL extractant continuous extraction twice, 40mL extractant extract once (constant volume is 10mL), thorium amount remaining after extraction is measured.This experiment finally determines that employing dimethylbenzene-TBP, as extractant, carries out the detection test of customary impurities element sepatation.5.4 internal standard elements select
ICP-MS needs to use internal standard to rectify an instrument and drifts about and matrix suppression during analyzing.Conventional internal standard element has the elements such as rhodium, indium, caesium.Different internal standard elements are different by situations such as matrix suppression, different to instrument signal calibration result, Element detection result may be had Different Effects.The impact of testing result is compared by this experiment investigation rhodium, indium and caesium as internal standard element.Test determine titanium, vanadium, chromium, nickel, copper, arsenic, zirconium with indium as internal standard, the drift that other element is Internal standard correction methods instrument signal with rhodium.
The measurement range μ g/g of impurity element in table 1 thorium tetrafluoride
Under the analysis condition that this method determines, parallel weigh 6 samples, measure 37 kinds of impurity contents.Impurity element standard solution is placed in beaker, adds 0.1g sample, the operating procedure determined by method, carry out the precision of method and add recovery test, 5 times of defects inspecting lower limits are added recovery test, 6 data of parallel assay.The precision of each element to be measured is superior to 10%.Average recovery rate, between 90%～110%, reaches expection test objective.
37 kinds of impurity contents in using plasma mass spectrometric determination thorium tetrafluoride herein.Have studied the dissolution conditions of thorium tetrafluoride sample, detection limit, matrix concentration conditions, acidity condition, nebulizer flow, internal standard element, investigated matrix interference and co-existing element interference, use extraction and separation technology to eliminate the matrix interference of Partial Elements.Each element correlation coefficient r is not less than 0.999.When sampling amount is 0.1g～0.5g, the analyst coverage of each element: As, Nb, Ni, Sn, Zn, Cr, Cu, Zr, Ti, V, W are 1 μ g/g～100 μ g/g；B, Cd, Co, Mo, Mn are 0.1 μ g/g～10 μ g/g；Pb is 5 μ g/g～250 μ g/g；Al, Fe, Mg, Ca, Si are 20 μ g/g～200 μ g/g；Sm, Eu, Gd, Dy are 0.05 μ g/g～2.5 μ g/g；La, Ce, Pr, Nd, Ho, Er, Tm, Tb, Yb, Lu, Y are 0.5 μ g/g～25 μ g/g.Method precision is superior to 10%, and average recovery rate is between 90%～110%.
Claims (5)
1. impurity content assay method in a thorium tetrafluoride powder, it is characterised in that: the method comprises the steps:
For ferrum, aluminum, nickel, stannum, zirconium, tungsten, 7 kinds of element determinations of silicon:
Weigh 0.1～0.5 gram of thorium tetrafluoride sample to be placed in the quartz beaker of 150mL, add 50mL nitric acid, 0.5mL acetonitrile, cover quartz surfaces ware heating for dissolving on temp.-adjustable electric hot plate；
After being completely dissolved, solution is steamed to the most dry, add 2mL, c (HNO3The salpeter solution of)=3mol/L, transfers to after being cooled to room temperature to have added in the 60mL separatory funnel of 20mL extractant；Described extractant is ψ (dimethylbenzene: tributyl phosphate)=3:1；
Aqueous phase is put in 100mL volumetric flask after being layered completely by extractant, is that 1% salpeter solution is diluted to scale by percent by volume, it is thus achieved that sample solution；
Then, on icp ms, use nebulization sampling mode, add rhodium-indium mixing inner mark solution, the drift being Internal standard correction methods instrument signal with rhodium online；
Measure series standard solution, draw standard curve, measure blank solution and sample solution the most respectively, calculate the content of each element to be measured in sample.
2. impurity content assay method in a thorium tetrafluoride powder, it is characterized in that: the method comprises the steps: for arsenic, boron, calcium, cadmium, niobium, lead, magnesium, manganese, molybdenum, zinc, cobalt, chromium, copper, titanium, vanadium, rare-earth elements of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, dysprosium, holmium, erbium, thulium, ytterbium, lutecium, terbium, 30 kinds of element determinations of yttrium；
Weighing 0.1g thorium tetrafluoride sample, be placed in the quartz beaker of 150mL, add 50mL nitric acid, 0.5mL acetonitrile covers quartz surfaces ware heating for dissolving on temp.-adjustable electric hot plate；
After being completely dissolved, solution is steamed to the most dry, add 2mL, c (HNO3The salpeter solution of)=3mol/L, is transferred to after being cooled to room temperature in 100mL volumetric flask, is that 1% salpeter solution is diluted to scale by percent by volume；Take 10mL sample solution in 50mL volumetric flask, be that 1% salpeter solution is diluted to scale by percent by volume；
On icp ms, use nebulization sampling mode, add rhodium-indium mixing inner mark solution online, titanium, vanadium, chromium, nickel, copper, arsenic, zirconium with indium as internal standard, the drift that other element is Internal standard correction methods instrument signal with rhodium；
Measure series standard solution, draw standard curve, measure blank solution and sample solution the most respectively, calculate the content of each element to be measured in sample.
Impurity content assay method in a kind of thorium tetrafluoride powder the most according to claim 1 and 2, it is characterised in that: interfere situation preparation series standard solution by each co-existing element interference and solution system, as shown in Table 1 and Table 2.
Table 1 series standard solution
Table 2 series standard solution
Impurity content assay method in a kind of thorium tetrafluoride powder the most according to claim 1 and 2, it is characterised in that:
When sampling amount is 0.1g～0.5g, the analyst coverage of each element:
As, Nb, Ni, Sn, Zn, Cr, Cu, Zr, Ti, V, W are 1 μ g/g～100 μ g/g；
B, Cd, Co, Mo, Mn are 0.1 μ g/g～10 μ g/g；
Pb is 5 μ g/g～250 μ g/g；
Al, Fe, Mg, Ca, Si are 20 μ g/g～200 μ g/g；
Sm, Eu, Gd, Dy are 0.05 μ g/g～2.5 μ g/g；
La, Ce, Pr, Nd, Ho, Er, Tm, Tb, Yb, Lu, Y are 0.5 μ g/g～25 μ g/g.
Impurity content assay method in a kind of thorium tetrafluoride powder the most according to claim 1 and 2, it is characterised in that: described addition 50mL nitric acid, this nitric acid is that top grade is pure, 15.5mol/L.
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