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 PDFInfo
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- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 90
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims abstract description 41
- 235000013619 trace mineral Nutrition 0.000 title claims abstract description 17
- 239000011573 trace mineral Substances 0.000 title claims abstract description 17
- 239000011734 sodium Substances 0.000 claims abstract description 110
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 28
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011591 potassium Substances 0.000 claims abstract description 27
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 claims abstract description 23
- 238000005259 measurement Methods 0.000 claims abstract description 19
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 16
- 239000000243 solution Substances 0.000 claims description 76
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 45
- 239000012086 standard solution Substances 0.000 claims description 35
- 239000003153 chemical reaction reagent Substances 0.000 claims description 30
- 239000012488 sample solution Substances 0.000 claims description 28
- 238000002360 preparation method Methods 0.000 claims description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 20
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 20
- 238000002835 absorbance Methods 0.000 claims description 20
- 239000004033 plastic Substances 0.000 claims description 20
- 229920003023 plastic Polymers 0.000 claims description 20
- 238000010521 absorption reaction Methods 0.000 claims description 19
- 238000001354 calcination Methods 0.000 claims description 10
- -1 polytetrafluoroethylene Polymers 0.000 claims description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 10
- 239000001103 potassium chloride Substances 0.000 claims description 10
- 235000011164 potassium chloride Nutrition 0.000 claims description 10
- 239000011780 sodium chloride Substances 0.000 claims description 10
- 229910052792 caesium Inorganic materials 0.000 claims description 7
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 7
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 4
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 4
- 238000013102 re-test Methods 0.000 claims description 4
- 238000001228 spectrum Methods 0.000 claims description 4
- 229910052702 rhenium Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 238000000705 flame atomic absorption spectrometry Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 238000011160 research Methods 0.000 abstract description 5
- 238000004458 analytical method Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000003112 inhibitor Substances 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000009863 impact test Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 7
- 239000012535 impurity Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- UTBYQPSPFXHANA-UHFFFAOYSA-N [K].[Na].[Li] Chemical compound [K].[Na].[Li] UTBYQPSPFXHANA-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 150000002642 lithium compounds Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000013500 performance material Substances 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- DECCZIUVGMLHKQ-UHFFFAOYSA-N rhenium tungsten Chemical compound [W].[Re] DECCZIUVGMLHKQ-UHFFFAOYSA-N 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
本发明属于纯金属痕量元素分析技术，涉及一种测定纯Re中痕量元素钠和钾的方法。本发明采用火焰原子吸收光谱法测定纯Re中痕量元素钠和钾的含量，分析范围为0.0001%～0.001%。用硝酸处理纯Re试样，优化了测量条件，着重研究干扰及其控制的方法，选择氯化铯作为电离抑制剂，对溶解酸用量和基体干扰进行影响试验并进行严格的控制，采用标准加入法测量钠和钾的含量。研究建立的测定纯Re中痕量元素Na、K的方法准确可靠，可以满足科研生产的要求；方法检测下限低，测量下限为0.0001%；采用氯化铯作为电离抑制剂，消除电离效应，同时改善测量灵敏度；该技术方法测量快速，操作简便，节约了大量人力和物力。The invention belongs to pure metal trace element analysis technology, and relates to a method for measuring trace elements sodium and potassium in pure Re. The invention adopts flame atomic absorption spectrometry to measure the content of trace elements sodium and potassium in pure Re, and the analysis range is 0.0001%-0.001%. Treat the pure Re sample with nitric acid, optimize the measurement conditions, focus on the research of interference and its control method, choose cesium chloride as the ionization inhibitor, conduct the impact test on the amount of dissolved acid and matrix interference and carry out strict control. method to measure sodium and potassium content. The established method for the determination of trace elements Na and K in pure Re is accurate and reliable, and can meet the requirements of scientific research and production; the detection limit of the method is low, and the measurement limit is 0.0001%; cesium chloride is used as an ionization inhibitor to eliminate the ionization effect, and at the same time Improve measurement sensitivity; this technical method is fast in measurement, easy to operate, and saves a lot of manpower and material resources.
Description
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:
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:
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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| CN102954941A (en) * | 2012-10-24 | 2013-03-06 | 中国航空工业集团公司北京航空材料研究院 | Method for determining sodium and potassium in tantalum-containing high-temperature alloy by atomic absorption spectrometry |
| CN103257112A (en) * | 2013-04-12 | 2013-08-21 | 中国航空工业集团公司北京航空材料研究院 | Determination method for trace element potassium in pure Hf |
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