CN102706816B - Method for determination of trace element Na and K in pure Re - Google Patents

Method for determination of trace element Na and K in pure Re Download PDF

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CN102706816B
CN102706816B CN201210167209.8A CN201210167209A CN102706816B CN 102706816 B CN102706816 B CN 102706816B CN 201210167209 A CN201210167209 A CN 201210167209A CN 102706816 B CN102706816 B CN 102706816B
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任慧
杨春晟
叶晓英
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BEIJING INSTITUTE OF AERONAUTICAL MATERIALS CHINA AVIATION INDUSTRY GROUP Corp
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Abstract

The invention belongs to the analysis technics of trace element in pure metal, and relates to a method for determination of trace element Na and K in pure Re. A FAAS (flame atomic absorption spectrometry) is applied to the determination of the trace element Na and K in pure Re, and the analysis range is 0.0001%-0.001%. A pure Re sample is processed by nitric acid, the measurement condition is optimized, and interference and method for controlling the interference are researched as emphasis. The cesium chloride is chosen as ionization inhibitor, the influence test in the dosage of the acid for dissolution and matrix interference is carried and strict control is performed, and the standard addition method is applied to determine the content of Na and K. The method has the advantages that the established method for determination of the trace element Na and K in pure Re is accuracy and reliable, and the requirements of scientific research is also satisfied. The determination lower limit of the method is low, and is 0.0001%. The ionization effect is eliminated and the sensitivity of determination is improved by adoption of cesium chloride as the ionization inhibitor. The method is quick, the operation is simple, and labour power and material resources are saved largely.

Description

A kind of method of measuring trace element sodium and potassium in pure Re
Technical field
The present invention is a kind of method of measuring trace element sodium and potassium in pure Re, belongs to simple metal trace element analysis technology.
Background technology
Re is a kind of rare refractory metal, has high-melting-point, high strength and good plasticity and excellent mechanical stability, and its fusing point is only second to tungsten, up to 3180 ℃.Re does not have fragility critical transition temperature, under high temperature and extremely cold very hot condition, all there is good creep-resistant property, be suitable for superhigh temperature and heat-flash shake working environment, because of its a series of excellent specific properties, Re and alloy thereof are widely used in the industries such as petrochemical complex, Aero-Space and electronics industry, become one of very important new material of modern high-tech field.Along with industrial expansion, new material is constantly released, and various excellent performance materials are further strict to the requirement of its composition, and in simple metal, the content of impurity element is most important on the impact of material property.Investigation by analysis, in the document of having published, there are method, the addition method of measuring potassium in soluble lithium compounds and/or sodium content to survey in potassium in tungsten-rhenium wire, Flame Atomic Absorption Spectrometry Determination lithium metal lithium sodium potassium caesium in sodium, Flame Atomic Absorption Spectrometry Determination High Purity Rbcl, domestic standard method has the mensuration flame atomic absorption spectrometry GB/T12690.8-2003 of non-rare earth impurity chemical analysis method sodium amount in rare earth metal and oxide thereof, but they have very large difference with sodium and potassium in the pure Re of Flame Atomic Absorption Spectrometry Determination.Along with the progress of technology, be a new field about the mensuration of Determination of trace element contents in pure material, both at home and abroad all less than the method for measuring trace amounts of sodium and potassium in pure Re about flame atomic absorption spectrometry.
Summary of the invention
The present invention designs for situation in above-mentioned prior art just provides a kind of method of measuring trace element sodium and potassium in pure Re, its objective is the mensuration that solves trace element sodium and potassium content in pure Re.
The object of the invention is to be achieved through the following technical solutions:
A method of measuring trace element sodium and potassium in pure Re, is characterized in that: the reagent that the method is used in mensuration process has:
Cesium chloride solution, in solution, the quality-volumetric concentration of caesium is 20mg/mL, preparation method takes the specpure cesium chloride of 2.53g, is placed in 100mL beaker, is dissolved in water, and moves in 100mL volumetric flask, is diluted with water to scale, shakes up;
Na standard solution: quality-volumetric concentration is 0.10mg/mL, preparation method takes 0.2541g in advance through 550 ℃ of calcination 2h and be chilled to the sodium chloride of room temperature in desiccator, the massfraction of sodium chloride is not less than 99.95%, be placed in 250mL beaker, be dissolved in water, add the MOS grade hydrochloric acid of 20mL, move in 1000mL volumetric flask, be diluted with water to scale, shake up, move in dry plastic bottle and preserve;
K standard solution: quality-volumetric concentration is 0.10mg/mL, preparation method takes 0.1907g in advance through 550 ℃ of calcination 2h and be chilled to the potassium chloride of room temperature in desiccator, the massfraction of potassium chloride is not less than 99.95%, be placed in 250mL beaker, be dissolved in water, add the MOS grade hydrochloric acid of 20mL, move in 1000mL volumetric flask, be diluted with water to scale, shake up, move in dry plastic bottle and preserve;
Na, K mixed standard solution: quality-volumetric concentration is 1 μ g/mL, preparation method pipettes sodium standard solution, the each 10.00mL of potassium standard solution, is placed in 1000mL volumetric flask, is diluted with water to scale, shakes up;
Nitric acid: MOS level;
The step of the mensuration process of the method is:
(1) prepare sample solution:
Take the pure Re test portion of 0.50g, be accurate to 0.0001g, pure Re massfraction is not less than 99.99%;
Pure Re test portion is placed in to 150mL polytetrafluoroethylene beaker, adds 3~10mL nitric acid, dissolve, after dissolving completely, slightly cold, move in 25mL plastics volumetric flask;
(2) preparation standard adds working curve solution
Get the sample solution that is no less than 4 parts, add respectively Na, K mixed standard solution, wherein the addition in 3 parts of sample solutions be 0,0.5mL, 5mL, addition in other sample solution is 0.5mL~5mL, then in above-mentioned whole sample solutions, add 1~5mL cesium chloride solution, be diluted to scale with water, shake up;
(3) measurement standard adds the content of Na, K in working curve solution
Adopt atomic absorption spectrography (AAS), respectively at Na 589.0nm, K 766.5nm wavelength place, measurement standard adds the absorbance of Na, K in working curve solution successively, horizontal ordinate adds the content of Na, K in working curve solution by standard, ordinate adds the absorbance of Na, K in working curve solution by standard, drawing curve, obtains this curve and horizontal ordinate intersection value, is designated as Na1, K1;
(4) prepare reagent blank standard and add working curve solution
In 150mL polytetrafluoroethylene beaker, add 3~10mL nitric acid, move in 25mL plastics volumetric flask, get this solution that is no less than 4 parts, add respectively Na, K mixed standard solution, wherein the addition in 3 parts of sample solutions be 0,0.5mL, 5mL, addition in other sample solution is 0.5mL~5mL, then in above-mentioned whole sample solutions, add 1~5mL cesium chloride solution, be diluted to scale with water, shake up;
(5) measure the content that reagent blank standard adds Na, K in working curve solution
Adopt atomic absorption spectrography (AAS), respectively at Na 589.0nm, K 766.5nm wavelength place, measure successively the absorbance that reagent blank standard adds Na, K in working curve solution, horizontal ordinate adds the content of Na, K in working curve solution by reagent blank standard, ordinate adds the absorbance of Na, K in working curve solution by reagent blank standard, drawing curve, obtains this curve and horizontal ordinate intersection value, is designated as Na2, K2;
(6) the content WNa, the WK that calculate Na in pure Re, K element, numerical value represents with %
WNa=Na1-Na2
WK=K1-K2。
2. the method for trace element sodium and potassium in the pure Re of mensuration according to claim 1, is characterized in that: condition of work and the analytical line of Atomic Absorption Spectrometer are as follows:
Na element: analytical line 589.0nm, spectrum channel 0.2 or 0.7nm, lamp current 5~20mA, air mass flow 4.0L/min, acetylene flow 1.0~2.5L/min;
K element: analytical line 766.5nm, spectrum channel 0.2 or 0.7nm, lamp current 6~15mA, air mass flow 4.0L/min, acetylene flow 1.0~2.5L/min.
The present invention adopts the content of trace element sodium and potassium in the pure Re of Flame Atomic Absorption Spectrometry Determination, and analyst coverage is 0.0001%~0.001%.Due to sodium and potassium content low, exist matrix interference, acid to disturb and ionization interference, meanwhile, because all belonging to nature, sodium and potassium is rich in element, and ubiquitous in human body, container, laboratory, air, very easily pollute, so the present invention has optimized measuring condition, the method that research is disturbed and controlled emphatically, selective chlorination caesium is as ionization inhibitor, dissolving acid consumption and matrix are disturbed affect and test and carry out strict control, the content of employing standard addition method measurement sodium and potassium.
Advantage of the present invention is:
1) in the pure Re of mensuration that research is set up, the atomic absorption spectrography (AAS) of trace element Na, K accurately and reliably, can meet the requirement of research and production;
2) method detection lower limit is low, and measurement lower limit is 0.0001%;
3) adopt cesium chloride as ionization inhibitor, eliminate ionisation effect, improve simultaneously and measure sensitivity.
4) this technical method is measured fast, easy and simple to handle, has saved a large amount of man power and materials.
Embodiment
Embodiment mono-
Measure sodium, potassium content in pure Re1, adopt Atomic Absorption Spectrometer A(PE AAnalyst100 Atomic Absorption Spectrometer), condition of work and the analytical line of instrument are as shown below:
Figure BDA00001684533600041
The reagent that the method is used in mensuration process has:
Cesium chloride solution: in solution, the quality-volumetric concentration of caesium is 20mg/mL, preparation method takes the specpure cesium chloride of 2.53g, is placed in 100mL beaker, is dissolved in water, and moves in 100mL volumetric flask, is diluted with water to scale, shakes up;
Na standard solution: quality-volumetric concentration is 0.10mg/mL, preparation method takes 0.2541g in advance through 550 ℃ of calcination 2h and be chilled to the sodium chloride of room temperature in desiccator, the massfraction of sodium chloride is not less than 99.95%, be placed in 250mL beaker, be dissolved in water, add the MOS grade hydrochloric acid of 20mL, move in 1000mL volumetric flask, be diluted with water to scale, shake up, move in dry plastic bottle and preserve;
K standard solution: quality-volumetric concentration is 0.10mg/mL, preparation method takes 0.1907g in advance through 550 ℃ of calcination 2h and be chilled to the potassium chloride of room temperature in desiccator, the massfraction of potassium chloride is not less than 99.95%, be placed in 250mL beaker, be dissolved in water, add the MOS grade hydrochloric acid of 20mL, move in 1000mL volumetric flask, be diluted with water to scale, shake up, move in dry plastic bottle and preserve;
Na, K mixed standard solution: quality-volumetric concentration is 1 μ g/mL, preparation method pipettes sodium standard solution, the each 10.00mL of potassium standard solution, is placed in 1000mL volumetric flask, is diluted with water to scale, shakes up;
Nitric acid: MOS level;
The step of the mensuration process of the method is:
(1) prepare sample solution:
Take the pure Re1 test portion of 0.50g, be accurate to 0.0001g, pure Re 1 massfraction is not less than 99.99%;
Pure Re1 test portion is placed in to 150mL polytetrafluoroethylene beaker, adds 3mL nitric acid, dissolve, after dissolving completely, slightly cold, move in 25mL plastics volumetric flask;
(2) preparation standard adds working curve solution
Get 4 parts of sample solutions, add respectively Na, K mixed standard solution 0,0.5mL, 2mL, 5mL, then in above-mentioned whole sample solutions, add 1mL cesium chloride solution, be diluted to scale with water, shake up;
(3) measurement standard adds the content of Na, K in working curve solution
Adopt atomic absorption spectrography (AAS), respectively at Na 589.0nm, K 766.5nm wavelength place, measurement standard adds the absorbance of Na, K in working curve solution successively, horizontal ordinate adds the content of Na, K in working curve solution by standard, ordinate adds the absorbance of Na, K in working curve solution by standard, drawing curve, obtains this curve and horizontal ordinate intersection value, is designated as Na1, K1;
(4) prepare reagent blank standard and add working curve solution
In 150mL polytetrafluoroethylene beaker, add 3mL nitric acid, move in 25mL plastics volumetric flask, get 4 parts of these solution, add respectively Na, K mixed standard solution 0,0.5mL, 2mL, 5mL, then in above-mentioned whole sample solutions, add 1mL cesium chloride solution, be diluted to scale with water, shake up;
(5) measure the content that reagent blank standard adds Na, K in working curve solution
Adopt atomic absorption spectrography (AAS), respectively at Na 589.0nm, K 766.5nm wavelength place, measure successively the absorbance that reagent blank standard adds Na, K in working curve solution, horizontal ordinate adds the content of Na, K in working curve solution by reagent blank standard, ordinate adds the absorbance of Na, K in working curve solution by reagent blank standard, drawing curve, obtains this curve and horizontal ordinate intersection value, is designated as Na2, K2;
(6) the content WNa, the WK that calculate Na in pure Re1, K element, numerical value represents with %
W Na=Na1-Na2
W K=K1-K2。
Computation and measurement result, the content that the content that obtains Na in pure Re1 is 0.000128%, K is 0.000129%.
Embodiment bis-
Measure sodium, potassium content in pure Re2, adopt Atomic Absorption Spectrometer A(PE AAnalyst100 Atomic Absorption Spectrometer), condition of work and the analytical line of instrument are as shown below:
Figure BDA00001684533600061
The reagent that the method is used in mensuration process has:
Cesium chloride solution: in solution, the quality-volumetric concentration of caesium is 20mg/mL, preparation method takes the specpure cesium chloride of 2.53g, is placed in 100mL beaker, is dissolved in water, and moves in 100mL volumetric flask, is diluted with water to scale, shakes up;
Na standard solution: quality-volumetric concentration is 0.10mg/mL, preparation method takes 0.2541g in advance through 550 ℃ of calcination 2h and be chilled to the sodium chloride of room temperature in desiccator, the massfraction of sodium chloride is not less than 99.95%, be placed in 250mL beaker, be dissolved in water, add the MOS grade hydrochloric acid of 20mL, move in 1000mL volumetric flask, be diluted with water to scale, shake up, move in dry plastic bottle and preserve;
K standard solution: quality-volumetric concentration is 0.10mg/mL, preparation method takes 0.1907g in advance through 550 ℃ of calcination 2h and be chilled to the potassium chloride of room temperature in desiccator, the massfraction of potassium chloride is not less than 99.95%, be placed in 250mL beaker, be dissolved in water, add the MOS grade hydrochloric acid of 20mL, move in 1000mL volumetric flask, be diluted with water to scale, shake up, move in dry plastic bottle and preserve;
Na, K mixed standard solution: quality-volumetric concentration is 1 μ g/mL, preparation method pipettes sodium standard solution, the each 10.00mL of potassium standard solution, is placed in 1000mL volumetric flask, is diluted with water to scale, shakes up;
Nitric acid: MOS level;
The step of the mensuration process of the method is:
(1) prepare sample solution:
Take the pure Re2 test portion of 0.50g, be accurate to 0.0001g, pure Re2 massfraction is not less than 99.99%;
Pure Re2 test portion is placed in to 150mL polytetrafluoroethylene beaker, adds 5mL nitric acid, dissolve, after dissolving completely, slightly cold, move in 25mL plastics volumetric flask;
(2) preparation standard adds working curve solution
Get 5 parts of sample solutions, add respectively Na, K mixed standard solution 0,0.5mL, 1mL, 3mL, 5mL, then in above-mentioned whole sample solutions, add 2mL cesium chloride solution, be diluted to scale with water, shake up;
(3) measurement standard adds the content of Na, K in working curve solution
Adopt atomic absorption spectrography (AAS), respectively at Na 589.0nm, K 766.5nm wavelength place, measurement standard adds the absorbance of Na, K in working curve solution successively, horizontal ordinate adds the content of Na, K in working curve solution by standard, ordinate adds the absorbance of Na, K in working curve solution by standard, drawing curve, obtains this curve and horizontal ordinate intersection value, is designated as Na1, K1;
(4) prepare reagent blank standard and add working curve solution
In 150mL polytetrafluoroethylene beaker, add 5mL nitric acid, move in 25mL plastics volumetric flask, get 5 parts of these solution, add respectively Na, K mixed standard solution 0,0.5mL, 1mL, 3mL, 5mL, then in above-mentioned whole sample solutions, add 2mL cesium chloride solution, be diluted to scale with water, shake up;
(5) measure the content that reagent blank standard adds Na, K in working curve solution
Adopt atomic absorption spectrography (AAS), respectively at Na 589.0nm, K 766.5nm wavelength place, measure successively the absorbance that reagent blank standard adds Na, K in working curve solution, horizontal ordinate adds the content of Na, K in working curve solution by reagent blank standard, ordinate adds the absorbance of Na, K in working curve solution by reagent blank standard, drawing curve, obtains this curve and horizontal ordinate intersection value, is designated as Na2, K2;
(6) the content WNa, the WK that calculate Na in pure Re2, K element, numerical value represents with %
W Na=Na1-Na2
W K=K1-K2。
Computation and measurement result, the content that the content that obtains Na in pure Re2 is 0.000425%, K is 0.000424%.
Embodiment tri-
Measure sodium, potassium content in pure Re3, adopt Atomic Absorption Spectrometer A(PE AAnalyst100 Atomic Absorption Spectrometer), condition of work and the analytical line of instrument are as shown below:
The reagent that the method is used in mensuration process has:
Cesium chloride solution: in solution, the quality-volumetric concentration of caesium is 20mg/mL, preparation method takes the specpure cesium chloride of 2.53g, is placed in 100mL beaker, is dissolved in water, and moves in 100mL volumetric flask, is diluted with water to scale, shakes up;
Na standard solution: quality-volumetric concentration is 0.10mg/mL, preparation method takes 0.2541g in advance through 550 ℃ of calcination 2h and be chilled to the sodium chloride of room temperature in desiccator, the massfraction of sodium chloride is not less than 99.95%, be placed in 250mL beaker, be dissolved in water, add the MOS grade hydrochloric acid of 20mL, move in 1000mL volumetric flask, be diluted with water to scale, shake up, move in dry plastic bottle and preserve;
K standard solution: quality-volumetric concentration is 0.10mg/mL, preparation method takes 0.1907g in advance through 550 ℃ of calcination 2h and be chilled to the potassium chloride of room temperature in desiccator, the massfraction of potassium chloride is not less than 99.95%, be placed in 250mL beaker, be dissolved in water, add the MOS grade hydrochloric acid of 20mL, move in 1000mL volumetric flask, be diluted with water to scale, shake up, move in dry plastic bottle and preserve;
Na, K mixed standard solution: quality-volumetric concentration is 1 μ g/mL, preparation method pipettes sodium standard solution, the each 10.00mL of potassium standard solution, is placed in 1000mL volumetric flask, is diluted with water to scale, shakes up;
Nitric acid: MOS level;
The step of the mensuration process of the method is:
(1) prepare sample solution:
Take the pure Re3 test portion of 0.50g, be accurate to 0.0001g, pure Re3 massfraction is not less than 99.99%;
Pure Re3 test portion is placed in to 150mL polytetrafluoroethylene beaker, adds 10mL nitric acid, dissolve, after dissolving completely, slightly cold, move in 25mL plastics volumetric flask;
(2) preparation standard adds working curve solution
Get 7 parts of sample solutions, add respectively Na, K mixed standard solution 0,0.5mL, 1mL, 2mL, 3mL, 4mL, 5mL, then in above-mentioned whole sample solutions, add 5mL cesium chloride solution, be diluted to scale with water, shake up;
(3) measurement standard adds the content of Na, K in working curve solution
Adopt atomic absorption spectrography (AAS), respectively at Na 589.0nm, K 766.5nm wavelength place, measurement standard adds the absorbance of Na, K in working curve solution successively, horizontal ordinate adds the content of Na, K in working curve solution by standard, ordinate adds the absorbance of Na, K in working curve solution by standard, drawing curve, obtains this curve and horizontal ordinate intersection value, is designated as Na1, K1;
(4) prepare reagent blank standard and add working curve solution
In 150mL polytetrafluoroethylene beaker, add 10mL nitric acid, move in 25mL plastics volumetric flask, get 7 parts of these solution, add respectively Na, K mixed standard solution 0,0.5mL, 1mL, 2mL, 3mL, 4mL, 5mL, then in above-mentioned whole sample solutions, add 5mL cesium chloride solution, be diluted to scale with water, shake up;
(5) measure the content that reagent blank standard adds Na, K in working curve solution
Adopt atomic absorption spectrography (AAS), respectively at Na 589.0nm, K 766.5nm wavelength place, measure successively the absorbance that reagent blank standard adds Na, K in working curve solution, horizontal ordinate adds the content of Na, K in working curve solution by reagent blank standard, ordinate adds the absorbance of Na, K in working curve solution by reagent blank standard, drawing curve, obtains this curve and horizontal ordinate intersection value, is designated as Na2, K2;
(6) the content WNa, the WK that calculate Na in pure Re3, K element, numerical value represents with %
W Na=Na1-Na2
W K=K1-K2。
Computation and measurement result, the content that the content that obtains Na in pure Re3 is 0.000775%, K is 0.000800%.

Claims (2)

1. a method for trace element sodium and potassium in the pure Re of mensuration, is characterized in that: the reagent that the method is used in mensuration process has:
Cesium chloride solution, in solution, the quality-volumetric concentration of caesium is 20mg/mL, preparation method takes the specpure cesium chloride of 2.53g, is placed in 100mL beaker, is dissolved in water, and moves in 100mL volumetric flask, is diluted with water to scale, shakes up;
Na standard solution: quality-volumetric concentration is 0.10mg/mL, preparation method takes 0.2541g in advance through 550 ℃ of calcination 2h and be chilled to the sodium chloride of room temperature in desiccator, the massfraction of sodium chloride is not less than 99.95%, be placed in 250mL beaker, be dissolved in water, add the MOS grade hydrochloric acid of 20mL, move in 1000mL volumetric flask, be diluted with water to scale, shake up, move in dry plastic bottle and preserve;
K standard solution: quality-volumetric concentration is 0.10mg/mL, preparation method takes 0.1907g in advance through 550 ℃ of calcination 2h and be chilled to the potassium chloride of room temperature in desiccator, the massfraction of potassium chloride is not less than 99.95%, be placed in 250mL beaker, be dissolved in water, add the MOS grade hydrochloric acid of 20mL, move in 1000mL volumetric flask, be diluted with water to scale, shake up, move in dry plastic bottle and preserve;
Na, K mixed standard solution: quality-volumetric concentration is 1 μ g/mL, preparation method pipettes sodium standard solution, the each 10.00mL of potassium standard solution, is placed in 1000mL volumetric flask, is diluted with water to scale, shakes up;
Nitric acid: MOS level;
The step of the mensuration process of the method is:
(1) prepare sample solution:
Take the pure Re test portion of 0.50g, be accurate to 0.0001g, pure Re massfraction is not less than 99.99%;
Pure Re test portion is placed in to 150mL polytetrafluoroethylene beaker, adds 3~10mL nitric acid, dissolve, after dissolving completely, be cooled to room temperature, move in 25mL plastics volumetric flask;
(2) preparation standard adds working curve solution
Get the sample solution that is no less than 4 parts, add respectively Na, K mixed standard solution, wherein the addition in 3 parts of sample solutions be 0,0.5mL, 5mL, addition in other sample solution is 0.5mL~5mL, then in above-mentioned whole sample solutions, add 1~5mL cesium chloride solution, be diluted to scale with water, shake up;
(3) measurement standard adds the content of Na, K in working curve solution
Adopt atomic absorption spectrography (AAS), at Na 589.0nm, K 766.5nm wavelength place, measurement standard adds the absorbance of Na, K in working curve solution successively respectively, and horizontal ordinate adds Na, K in working curve solution by standard
Content, ordinate adds the absorbance of Na, K in working curve solution by standard, drawing curve obtains this curve and horizontal ordinate intersection value, is designated as Na1, K1;
(4) prepare reagent blank standard and add working curve solution
In 150mL polytetrafluoroethylene beaker, add 3~10mL nitric acid, move in 25mL plastics volumetric flask, get this solution that is no less than 4 parts, add respectively Na, K mixed standard solution, wherein the addition in 3 parts of sample solutions be 0,0.5mL, 5mL, addition in other sample solution is 0.5mL~5mL, then in above-mentioned whole sample solutions, add 1~5mL cesium chloride solution, be diluted to scale with water, shake up;
(5) measure the content that reagent blank standard adds Na, K in working curve solution
Adopt atomic absorption spectrography (AAS), respectively at Na 589.0nm, K 766.5nm wavelength place, measure successively the absorbance that reagent blank standard adds Na, K in working curve solution, horizontal ordinate adds the content of Na, K in working curve solution by reagent blank standard, ordinate adds the absorbance of Na, K in working curve solution by reagent blank standard, drawing curve, obtains this curve and horizontal ordinate intersection value, is designated as Na2, K2;
(6) calculate the content W of Na in pure Re, K element na, W k, numerical value represents with %
W Na=Na1-Na2
W K=K1-K2。
2. the method for trace element sodium and potassium in the pure Re of mensuration according to claim 1, is characterized in that: condition of work and the analytical line of Atomic Absorption Spectrometer are as follows:
Na element: analytical line 589.0nm, spectrum channel 0.2 or 0.7nm, lamp current 5~20mA, air mass flow 4.0L/min, acetylene flow 1.0~2.5L/min;
K element: analytical line 766.5nm, spectrum channel 0.2 or 0.7nm, lamp current 6~15mA, air mass flow 4.0L/min, acetylene flow 1.0~2.5L/min.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10319008A (en) * 1997-05-15 1998-12-04 Sumitomo Chem Co Ltd Quantitative analyzing method of element in liquid chemical
CN101109700A (en) * 2007-08-22 2008-01-23 中国石油化工股份有限公司 Method for measuring ruthenium content using ethyne-air flame atomic absorption spectrometry
CN101650301A (en) * 2009-08-10 2010-02-17 四川大学 Atomic absorption spectrometry of content of Fe and Zn impurities in yellow phosphorus

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10319008A (en) * 1997-05-15 1998-12-04 Sumitomo Chem Co Ltd Quantitative analyzing method of element in liquid chemical
CN101109700A (en) * 2007-08-22 2008-01-23 中国石油化工股份有限公司 Method for measuring ruthenium content using ethyne-air flame atomic absorption spectrometry
CN101650301A (en) * 2009-08-10 2010-02-17 四川大学 Atomic absorption spectrometry of content of Fe and Zn impurities in yellow phosphorus

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
ICP-AES法测定新型镍基高温合金中微量硼;叶晓英等;《2008年中国机械工程学会年会暨甘肃省学术年会文集》;20081231;90-93页 *
叶晓英等.ICP-AES法测定新型镍基高温合金中微量硼.《2008年中国机械工程学会年会暨甘肃省学术年会文集》.2008,
火焰原子吸收光谱法测定高纯氯化铷中的钠、钾;王晓辉等;《化学分析计量》;20050430;第14卷(第2期);48-49页 *
王晓辉等.火焰原子吸收光谱法测定高纯氯化铷中的钠、钾.《化学分析计量》.2005,第14卷(第2期),
王长华等.电感耦合等离子体质谱法测定高纯钨中15种痕量杂质元素.《质谱学报》.2011,第32卷(第4期),
电感耦合等离子体质谱法测定高纯钨中15种痕量杂质元素;王长华等;《质谱学报》;20110731;第32卷(第4期);216-221页 *

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