CN102954941A - Method for determining sodium and potassium in tantalum-containing high-temperature alloy by atomic absorption spectrometry - Google Patents
Method for determining sodium and potassium in tantalum-containing high-temperature alloy by atomic absorption spectrometry Download PDFInfo
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Abstract
The invention belongs to the technology of high-temperature alloy low-content element analysis and relates to a method for determining elements sodium and potassium in tantalum-containing high-temperature alloy by atomic absorption spectrometry. The method which is developed and established by the invention is accurate and reliable, and can reach the requirement of scientific research and production; the method has low detection limit which is 0.0005 percent; cesium chloride with lower ionization potential is added to serve as an ionization inhibitor to eliminate the ionization interference and improve the measurement sensitivity at the same time; sodium and potassium elements can be detected at the same time by one testing liquid; and the method is quick in measurement and convenient to operate, so that labor and materials can be saved greatly.
Description
Technical field
The invention belongs to the low secondary element analytical technology of high temperature alloy, relate to the method that aas determination contains elements of Na and potassium in the tantalum high temperature alloy.
Background technology
Along with the development of national defense industry, new material is constantly released, and various excellent performance materials are further strict to the requirement of its composition, and the content of impurity element is most important on the impact of material property in the low secondary element of high temperature alloy.Patents, non-patent literature investigation both at home and abroad found, the method of measuring sodium, potassium is generally atomic absorption method, in lithium sodium potassium caesium, wimet in sodium, the High Purity Rbcl in the potassium in potassium in the soluble lithium compounds or sodium, the tungsten-rhenium wire, the lithium metal. mensuration of calcium, potassium, magnesium and sodium amount etc., original method is inadaptable to contain the analysis of sodium and potassium element in the tantalum high temperature alloy.
Summary of the invention
The objective of the invention is: propose the method that a kind of aas determination with high accuracy, easy and simple to handle, that analytical cycle is short, efficient is high contains sodium and potassium in the tantalum high temperature alloy.
Technical scheme of the present invention is: adopt Atomic Absorption Spectrometer, wherein, use condition of work and the analytical line of Atomic Absorption Spectrometer as shown in the table:
| Element | Analytical line nm | Spectrum channel nm | Lamp current mA | Air mass flow L/min | Acetylene flow L/min |
| Na | 589.0 | 0.2 or 0.7 | 5～16 | 3.5 | 1.0～2.5 |
| K | 766.5 | 0.2 or 0.7 | 5～16 | 3.5 | 1.0～2.5 |
(1), employed reagent is as follows in the mensuration process:
(1.1), cesium chloride solution: ρ (Cs) ≈ 20mg/mL, spectroscopic pure;
(1.2), Na standard solution: 0.10mg/mL, potassium standard solution: 0.10mg/mL;
(1.3), Na, K mixed standard solution: 10 μ g/mL;
(1.4), ionized water is put into the pure water instrument and made ultrapure water;
(1.5), nitric acid is MOS level or high-purity;
(1.6), hydrochloric acid is MOS level or high-purity;
(1.7), chloroazotic acid;
(1.8), hydrofluorite is MOS level or high-purity;
(2), analytical procedure is as follows:
(2.1), test portion: take by weighing 1.00g and contain tantalum high temperature alloy test portion, be accurate to 0.0001g;
(2.2), preparation sample solution: test portion is placed the 150mL polytetrafluoroethylene beaker, add the 15mL chloroazotic acid, drip 10 hydrofluorite, dissolving behind the test portion dissolve complete, is cooled to room temperature, move in the 50mL plastics volumetric flask, add 1～5mL cesium chloride solution, with the water constant volume;
(2.3), preparation standard adds working curve solution
(2.3.1), preparation test portion standard adds working curve solution; Take by weighing and contain tantalum high temperature alloy test portion in the 150mL polytetrafluoroethylene beaker, add the 15mL chloroazotic acid, drip 10 hydrofluorite, dissolving is dissolved test portion fully, is chilled to room temperature, be transferred in the 50mL plastics volumetric flask, add successively 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mLNa, K mixed standard solution and 1～5mL cesium chloride solution, be diluted to scale with water, shake up;
(2.3.2), preparation reagent blank standard adds working curve solution; Prepare reagent blank with the sample operation repetitive, add successively 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mLNa, K mixed standard solution and 1～5mL cesium chloride solution, be diluted to scale with water, shake up, the standard of preparation reagent blank adds serial solution;
(2.4), measure the concentration of sodium, potassium in the test solution; Press the selected condition of work of Atomic Absorption Spectrometer, on Atomic Absorption Spectrometer, respectively at Na 589.0nm, K 766.5nm wavelength place, under Air-acetylene Flame, the absorbance of Na and K in employing Atomic Absorption Spectrometry amount reagent blank standard adding working curve solution and the test portion standard adding working curve solution, draw respectively the reagent blank standard and add working curve and test portion standard adding working curve, add the Na that working curve checks in reagent blank in the reagent blank standard, the K quality adds the Na that working curve checks in test portion in the test portion standard, the K quality; With the Na of the test portion that checks in, Na, the K quality that the K quality deducts reagent blank, with following formula convert Na in the test portion obtain getting as Atomic Absorption Spectrometry, K content;
In the formula:
m
1---the sodium that on working curve, checks in, the quality of potassium element, unit is microgram (μ g);
The quality of m---test portion, unit is gram (g).
Advantage of the present invention is:
1) aas determination set up of research contain sodium and potassium in the tantalum high temperature alloy method accurately and reliably, can satisfy the requirement of research and production;
2) method detection lower limit is low, and measurement lower limit is 0.0005%;
3) adopt the lower cesium chloride of adding ionization potential as the ionization inhibitor, eliminate ionization and disturb, sensitivity is measured in simultaneously improvement;
4) a cover test solution realization sodium, potassium element are measured simultaneously;
5) this patented method is measured fast, and is easy and simple to handle, saved a large amount of man power and materials.
Embodiment
Embodiment one
Mensuration contains sodium, potassium content among the tantalum high temperature alloy A, adopts Atomic Absorption Spectrometer (PE AAnalyst 100 Atomic Absorption Spectrometers), and condition of work and the analytical line of instrument are as shown in the table:
| Element | Analytical line nm | Spectrum channel nm | Lamp current mA | Air mass flow L/min | Acetylene flow L/min |
| Na | 589.0 | 0.7 | 6 | 3.5 | 2.0 |
| K | 766.5 | 0.7 | 6 | 3.5 | 2.0 |
(1), employed reagent is as follows in the mensuration process:
(1.1), cesium chloride solution: ρ (Cs) ≈ 20mg/mL, spectroscopic pure;
(1.2), Na standard solution: 0.10mg/mL, potassium standard solution: 0.10mg/mL;
(1.3), Na, K mixed standard solution: 10 μ g/mL;
(1.4), ionized water is put into the pure water instrument and made ultrapure water;
(1.5), nitric acid is MOS level or high-purity;
(1.6), hydrochloric acid is MOS level or high-purity;
(1.7), chloroazotic acid;
(1.8), hydrofluorite is MOS level or high-purity;
(2), analytical procedure is as follows:
(2.1), test portion: take by weighing 1.00g and contain tantalum high temperature alloy test portion, be accurate to 0.0001g;
(2.2), preparation sample solution: test portion is placed the 150mL polytetrafluoroethylene beaker, add the 15mL chloroazotic acid, drip 10 hydrofluorite, dissolving behind the test portion dissolve complete, is cooled to room temperature, move in the 50mL plastics volumetric flask, add 1～5mL cesium chloride solution, with the water constant volume;
(2.3), preparation standard adds working curve solution
(2.3.1), preparation test portion standard adds working curve solution; Take by weighing and contain tantalum high temperature alloy test portion in the 150mL polytetrafluoroethylene beaker, add the 15mL chloroazotic acid, drip 10 hydrofluorite, dissolving is dissolved test portion fully, is chilled to room temperature, be transferred in the 50mL plastics volumetric flask, add successively 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mLNa, K mixed standard solution and 1～5mL cesium chloride solution, be diluted to scale with water, shake up;
(2.3.2), preparation reagent blank standard adds working curve solution; Prepare reagent blank with the sample operation repetitive, add successively 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mLNa, K mixed standard solution and 1～5mL cesium chloride solution, be diluted to scale with water, shake up, the standard of preparation reagent blank adds serial solution;
(2.4), measure the concentration of sodium, potassium in the test solution; Press the selected condition of work of Atomic Absorption Spectrometer, on Atomic Absorption Spectrometer, respectively at Na 589.0nm, K 766.5nm wavelength place, under Air-acetylene Flame, the absorbance of Na and K in employing Atomic Absorption Spectrometry amount reagent blank standard adding working curve solution and the test portion standard adding working curve solution, draw respectively the reagent blank standard and add working curve and test portion standard adding working curve, add the Na that working curve checks in reagent blank in the reagent blank standard, the K quality adds the Na that working curve checks in test portion in the test portion standard, the K quality; With the Na of the test portion that checks in, Na, the K quality that the K quality deducts reagent blank, with following formula convert Na in the test portion obtain getting as Atomic Absorption Spectrometry, K content;
(2.5), the computation and measurement result, obtain containing Na, K content among the tantalum high temperature alloy A; The content of Na is that the content of 0.00061%, K is 0.00041%.
Embodiment two
Mensuration contains sodium, potassium content among the tantalum high temperature alloy B, adopts Atomic Absorption Spectrometer (PE AAnalyst 100 Atomic Absorption Spectrometers), and condition of work and the analytical line of instrument are as shown in the table:
| Element | Analytical line nm | Spectrum channel nm | Lamp current mA | Air mass flow L/min | Acetylene flow L/min |
| Na | 589.0 | 0.7 | 8 | 3.5 | 2.0 |
| K | 766.5 | 0.7 | 8 | 3.5 | 2.0 |
(1), employed reagent is as follows in the mensuration process:
(1.1), cesium chloride solution: ρ (Cs) ≈ 20mg/mL, spectroscopic pure;
(1.2), Na standard solution: 0.10mg/mL, potassium standard solution: 0.10mg/mL;
(1.3), Na, K mixed standard solution: 10 μ g/mL;
(1.4), ionized water is put into the pure water instrument and made ultrapure water;
(1.5), nitric acid is MOS level or high-purity;
(1.6), hydrochloric acid is MOS level or high-purity;
(1.7), chloroazotic acid;
(1.8), hydrofluorite is MOS level or high-purity;
(2), analytical procedure is as follows:
(2.1), test portion: take by weighing 1.00g and contain tantalum high temperature alloy test portion, be accurate to 0.0001g;
(2.2), preparation sample solution: test portion is placed the 150mL polytetrafluoroethylene beaker, add the 15mL chloroazotic acid, drip 10 hydrofluorite, dissolving behind the test portion dissolve complete, is cooled to room temperature, move in the 50mL plastics volumetric flask, add 1～5mL cesium chloride solution, with the water constant volume;
(2.3), preparation standard adds working curve solution
(2.3.1), preparation test portion standard adds working curve solution; Take by weighing and contain tantalum high temperature alloy test portion in the 150mL polytetrafluoroethylene beaker, add the 15mL chloroazotic acid, drip 10 hydrofluorite, dissolving is dissolved test portion fully, is chilled to room temperature, be transferred in the 50mL plastics volumetric flask, add successively 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mLNa, K mixed standard solution and 1～5mL cesium chloride solution, be diluted to scale with water, shake up;
(2.3.2), preparation reagent blank standard adds working curve solution; Prepare reagent blank with the sample operation repetitive, add successively 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mLNa, K mixed standard solution and 1～5mL cesium chloride solution, be diluted to scale with water, shake up, the standard of preparation reagent blank adds serial solution;
(2.4), measure the concentration of sodium, potassium in the test solution; Press the selected condition of work of Atomic Absorption Spectrometer, on Atomic Absorption Spectrometer, respectively at Na 589.0nm, K 766.5nm wavelength place, under Air-acetylene Flame, the absorbance of Na and K in employing Atomic Absorption Spectrometry amount reagent blank standard adding working curve solution and the test portion standard adding working curve solution, draw respectively the reagent blank standard and add working curve and test portion standard adding working curve, add the Na that working curve checks in reagent blank in the reagent blank standard, the K quality adds the Na that working curve checks in test portion in the test portion standard, the K quality; With the Na of the test portion that checks in, Na, the K quality that the K quality deducts reagent blank, with following formula convert Na in the test portion obtain getting as Atomic Absorption Spectrometry, K content;
(2.5), the computation and measurement result, obtain containing Na, K content among the tantalum high temperature alloy B; The content of Na is that the content of 0.0019%, K is 0.0019%.
Embodiment three
Mensuration contains in the tantalum high temperature alloy sodium, potassium content among the C, adopts Atomic Absorption Spectrometer (PE AAnalyst 100 Atomic Absorption Spectrometers), and condition of work and the analytical line of instrument are as shown in the table:
| Element | Analytical line nm | Spectrum channel nm | Lamp current mA | Air mass flow L/min | Acetylene flow L/min |
| Na | 589.0 | 0.2 | 5 | 4.0 | 2.5 |
| K | 766.5 | 0.2 | 5 | 4.0 | 2.5 |
(1), employed reagent is as follows in the mensuration process:
(1.1), cesium chloride solution: ρ (Cs) ≈ 20mg/mL, spectroscopic pure;
(1.2), Na standard solution: 0.10mg/mL, potassium standard solution: 0.10mg/mL;
(1.3), Na, K mixed standard solution: 10 μ g/mL;
(1.4), ionized water is put into the pure water instrument and made ultrapure water;
(1.5), nitric acid is MOS level or high-purity;
(1.6), hydrochloric acid is MOS level or high-purity;
(1.7), chloroazotic acid;
(1.8), hydrofluorite is MOS level or high-purity;
(2), analytical procedure is as follows:
(2.1), test portion: take by weighing 1.00g and contain tantalum high temperature alloy test portion, be accurate to 0.0001g;
(2.2), preparation sample solution: test portion is placed the 150mL polytetrafluoroethylene beaker, add the 15mL chloroazotic acid, drip 10 hydrofluorite, dissolving behind the test portion dissolve complete, is cooled to room temperature, move in the 50mL plastics volumetric flask, add 1～5mL cesium chloride solution, with the water constant volume;
(2.3), preparation standard adds working curve solution
(2.3.1), preparation test portion standard adds working curve solution; Take by weighing and contain tantalum high temperature alloy test portion in the 150mL polytetrafluoroethylene beaker, add the 15mL chloroazotic acid, drip 10 hydrofluorite, dissolving is dissolved test portion fully, is chilled to room temperature, be transferred in the 50mL plastics volumetric flask, add successively 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mLNa, K mixed standard solution and 1～5mL cesium chloride solution, be diluted to scale with water, shake up;
(2.3.2), preparation reagent blank standard adds working curve solution; Prepare reagent blank with the sample operation repetitive, add successively 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mLNa, K mixed standard solution and 1～5mL cesium chloride solution, be diluted to scale with water, shake up, the standard of preparation reagent blank adds serial solution;
(2.4), measure the concentration of sodium, potassium in the test solution; Press the selected condition of work of Atomic Absorption Spectrometer, on Atomic Absorption Spectrometer, respectively at Na 589.0nm, K 766.5nm wavelength place, under Air-acetylene Flame, the absorbance of Na and K in employing Atomic Absorption Spectrometry amount reagent blank standard adding working curve solution and the test portion standard adding working curve solution, draw respectively the reagent blank standard and add working curve and test portion standard adding working curve, add the Na that working curve checks in reagent blank in the reagent blank standard, the K quality adds the Na that working curve checks in test portion in the test portion standard, the K quality; With the Na of the test portion that checks in, Na, the K quality that the K quality deducts reagent blank, with following formula convert Na in the test portion obtain getting as Atomic Absorption Spectrometry, K content;
(2.5), the computation and measurement result, obtain containing Na, K content among the tantalum high temperature alloy C; The content of Na is that the content of 0.0052%, K is 0.0048%.
Claims (1)
1. an aas determination contains the method for sodium and potassium in the tantalum high temperature alloy, it is characterized in that: adopt Atomic Absorption Spectrometer, wherein, use condition of work and the analytical line of Atomic Absorption Spectrometer as shown in the table:
(1), employed reagent is as follows in the mensuration process:
(1.1), cesium chloride solution: ρ (Cs) ≈ 20mg/mL, spectroscopic pure;
(1.2), Na standard solution: 0.10mg/mL, potassium standard solution: 0.10mg/mL;
(1.3), Na, K mixed standard solution: 10 μ g/mL;
(1.4), ionized water is put into the pure water instrument and made ultrapure water;
(1.5), nitric acid is MOS level or high-purity;
(1.6), hydrochloric acid is MOS level or high-purity;
(1.7), chloroazotic acid;
(1.8), hydrofluorite is MOS level or high-purity;
(2), analytical procedure is as follows:
(2.1), test portion: take by weighing 1.00g and contain tantalum high temperature alloy test portion, be accurate to 0.0001g;
(2.2), preparation sample solution: test portion is placed the 150mL polytetrafluoroethylene beaker, add the 15mL chloroazotic acid, drip 10 hydrofluorite, dissolving behind the test portion dissolve complete, is cooled to room temperature, move in the 50mL plastics volumetric flask, add 1～5mL cesium chloride solution, with the water constant volume;
(2.3), preparation standard adds working curve solution
(2.3.1), preparation test portion standard adds working curve solution; Take by weighing and contain tantalum high temperature alloy test portion in the 150mL polytetrafluoroethylene beaker, add the 15mL chloroazotic acid, drip 10 hydrofluorite, dissolving is dissolved test portion fully, is chilled to room temperature, be transferred in the 50mL plastics volumetric flask, add successively 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mLNa, K mixed standard solution and 1～5mL cesium chloride solution, be diluted to scale with water, shake up;
(2.3.2), preparation reagent blank standard adds working curve solution; Prepare reagent blank with the sample operation repetitive, add successively 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mLNa, K mixed standard solution and 1～5mL cesium chloride solution, be diluted to scale with water, shake up, the standard of preparation reagent blank adds serial solution;
(2.4), measure the concentration of sodium, potassium in the test solution; Press the selected condition of work of Atomic Absorption Spectrometer, on Atomic Absorption Spectrometer, respectively at Na 589.0nm, K 766.5nm wavelength place, under Air-acetylene Flame, the absorbance of Na and K in employing Atomic Absorption Spectrometry amount reagent blank standard adding working curve solution and the test portion standard adding working curve solution, draw respectively the reagent blank standard and add working curve and test portion standard adding working curve, add the Na that working curve checks in reagent blank in the reagent blank standard, the K quality adds the Na that working curve checks in test portion in the test portion standard, the K quality; With the Na of the test portion that checks in, Na, the K quality that the K quality deducts reagent blank, with following formula convert Na in the test portion obtain getting as Atomic Absorption Spectrometry, K content;
In the formula:
m
1---the sodium that on working curve, checks in, the quality of potassium element, unit is microgram (μ g);
The quality of m---test portion, unit is gram (g).
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| 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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Application publication date: 20130306 |