CN105738349A - Method for measuring content of vanadium in rare earth alloy - Google Patents
Method for measuring content of vanadium in rare earth alloy Download PDFInfo
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Abstract
The invention discloses a method for measuring the content of vanadium in rare earth alloy, and belongs to the technical field of metallurgical analysis methods. The method aims at solving the problem that a suitable method for measuring the content of the vanadium in the rare earth alloy does not exist. The method includes the following steps of 1, preparing sample solutions; 2, preparing working standard curve solutions of the vanadium; 3, online measuring the content of the vanadium. The method is rapid is analysis speed, good in precision degree and high in accuracy degree, and the requirement of scientific research and the requirement of production can be completely met; the method is suitable for rapidly measuring the content of the vanadium in the rare earth alloy.
Description
Technical field
Present invention relates particularly to the assay method of content of vanadium in a kind of rare earth alloy, belong to metallurgical analysis method and technology field.
Background technology
Rare earth has the title of industry " gold ", has the physical characteristics such as excellent photoelectromagnetic due to it, new material that can be different, various in style with other materials component property, and its most significant function is exactly the quality and the performance that increase substantially other products.Such as increase substantially the tactical qualities for manufacturing tank, aircraft, the steel of guided missile, aluminium alloy, magnesium alloy, titanium alloy.And, rare earth is many high-tech lubricants such as electronics, laser, nuclear industry, superconduction equally.Rare earth alloy mainly has: tungsten and rear earth alloy, rare earth aluminium alloy, rare earth ferrosilicon conjunction etc..
Vanadium has physical property and the chemical property of numerous excellence, thus the purposes of vanadium is very extensive, has the title of metal " vitamin ".Initial vanadium is applied to iron and steel mostly, by refining tissue and the crystal grain of steel, improves grain coarsening temperature, thus playing the increase intensity of steel, toughness and wearability.Later, people were found that again the vanadium excellent improving effect in titanium alloy gradually, and were applied to aerospace field, so that aerospace industry achieves breakthrough progress.Along with developing by leaps and bounds of scientific and technological level, the requirement of new material is improved by the mankind day by day.The vanadium application in non-steel field is more and more extensive, and its scope covers the various fields such as Aero-Space, chemistry, battery, pigment, glass, optics, medicine.
The mensuration of content of vanadium has several reference method, but the mensuration of these methods are not directly applicable in rare earth alloy content of vanadium, not yet there are national standard method, rower and enterprise's mark method for the analysis detection of content of vanadium in rare earth alloy.
Summary of the invention
Therefore, it is an object of the invention to the problem for solving not to be suitable for the content of vanadium assay method of rare earth alloy, it is provided that the assay method of content of vanadium in a kind of rare earth alloy, said method comprising the steps of:
Step one: prepare sample solution
Sample is put in polytetrafluoroethylene beaker, add nitric acid, Fluohydric acid., heating for dissolving, add perchloric acid smoked near dry, add hydrochloric acid after taking off beaker cooling and reheat dissolving, be transferred in volumetric flask after cooling, be diluted to scale constant volume with pure water；
Step 2: prepare vanadium Working calibration curve solution
Vanadium Working calibration curve solution is prepared with the rare earth alloy sample without vanadium and vanadium standard solution；
Step 3: on content of vanadium, machine measures
On inductively-coupled plasma spectrometer, vanadium working curve standard solution and sample solution measuring the spectral intensity of vanadium simultaneously, computer automatic returning calculates analysis result.
Further, described step one is particularly as follows: claim 0.1 0.2g rare earth alloy sample, it is accurate to 0.1mg, put in polytetrafluoroethylene beaker, add 10 15mL nitric acid, 5mL Fluohydric acid., on electric hot plate, low-temperature heat is dissolved, and adds 5mL perchloric acid smoked near dry, takes off cooling, add 10mL (1+1) hydrochloric acid, again heating for dissolving on electric hot plate, is transferred in 100mL volumetric flask after taking off cooling, be diluted to 100mL volumetric flask scale with pure water, shake up, do blank test solution in company with sample solution.
Further, described step 2 is particularly as follows: with the vanadium standard solution of 1000 μ g/mL, dilution is configured to 100.0 μ g/mL, 10.0 the vanadium standard solution of μ g/mL, when content of vanadium≤0.050% in sample, claim the 0.2000g 5 parts of the same kind rare earth alloy sample without vanadium, sample dissolution is carried out by step one, shift respectively after cooling in 5 100mL volumetric flasks, it is separately added into 10.0 μ g/mL vanadium mark liquid and is configured to content of vanadium respectively 0%, 0.005%, 0.010%, 0.020%, the working curve standard solution of 5 points of 0.050%, the addition of vanadium amount respectively 0mL, 1.00mL, 2.00mL, 4.00mL, 10.00mL；As content of vanadium > 0.050%, claim the 0.1000g 5 parts of the same kind rare earth alloy sample without vanadium, sample dissolution is carried out by step one, shift respectively after cooling in 5 100mL volumetric flasks, be separately added into 100.0 μ g/mL vanadium mark liquid be configured to content of vanadium respectively 0%, 0.100%, 0.500%, 1.00%, 2.00% the working curve standard solution of 5 points, the addition of vanadium amount respectively 0mL, 1.00mL, 5.00mL, 10.00mL, 20.00mL.
Further, in described method step three:
Selecting Optima5300DV inductively-coupled plasma spectrometer, select the optimized analysis spectral line 311.071nm of vanadium, main working parameters includes, higher frequency: 40.68MHZ, power: 1300W, plasma gas flow rate: 15L/min, assisted gas flow: 0.2L/min, carrier gas flux: 0.8L/min, solution elevating amount: 1.5mL/min, washing time: 8s, prespark period: 45s, the time of integration: 2～10s are automatic, reading time delay: 30s, observed altitude: 15mm, observed pattern: axially.
Further, the reagent used in described method includes, and nitric acid: ρ 1.42, top grade is pure；Hydrochloric acid: ρ 1.19, top grade is pure；Fluohydric acid.: ρ 1.13, top grade is pure；Perchloric acid: ρ 1.68, top grade is pure；Hydrochloric acid (1+1), formulated in proportion with top grade pure hydrochloric acid and high purity water.
The beneficial effects of the present invention is: the assay method of content of vanadium in a kind of rare earth alloy of the present invention, after adopting acid dissolved samples, inductively-coupled plasma spectrometer is utilized directly to measure vanadium amount in rare earth alloy, inspection range is wider is 0.002 2.00%, analyzes method simple and fast, and agents useful for same is less, analysis speed is fast, precision is good, and accuracy is high, it is possible to fully meet the demand of research and production.The content of vanadium being suitable in rare earth alloy quickly measures.
Accompanying drawing explanation
Fig. 1 is the flow chart of the assay method of content of vanadium in a kind of rare earth alloy of the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is illustrated:
The method step of this detailed description of the invention as it is shown in figure 1, in detailed description below, agents useful for same particularly as follows:
Nitric acid: ρ 1.42, top grade is pure；Hydrochloric acid: ρ 1.19, top grade is pure；Fluohydric acid.: ρ 1.13, top grade is pure；Perchloric acid: ρ 1.68, top grade is pure；Hydrochloric acid (1+1), formulated in proportion with top grade pure hydrochloric acid and high purity water, experimental water is two grades of pure water.
Concrete operation step is as follows: claims 0.1 0.2g rare earth alloy sample, is accurate to 0.1mg, puts in polytetrafluoroethylene beaker, adding 10 15mL nitric acid, 5mL Fluohydric acid., with 100 DEG C of heating for dissolving of low temperature on electric hot plate, add 5mL perchloric acid smoked near dry, take off cooling, add 10mL (1+1) hydrochloric acid, again heating for dissolving on electric hot plate, it is transferred in 100mL volumetric flask after taking off cooling, it is diluted to 100mL volumetric flask scale with pure water, shakes up, do blank test solution in company with sample solution.Vanadium standard solution with 1000 μ g/mL, dilution is configured to 100.0 μ g/mL, 10.0 the vanadium standard solution of μ g/mL, when content of vanadium≤0.050% in sample, claim the 0.2000g 5 parts of the same kind rare earth alloy sample without vanadium, sample dissolution is carried out by step one, shift respectively after cooling in 5 100mL volumetric flasks, it is separately added into 10.0 μ g/mL vanadium mark liquid and is configured to content of vanadium respectively 0%, 0.005%, 0.010%, 0.020%, the working curve standard solution of 5 points of 0.050%, the addition of vanadium amount respectively 0mL, 1.00mL, 2.00mL, 4.00mL, 10.00mL；As content of vanadium > 0.050%, claim the 0.1000g 5 parts of the same kind rare earth alloy sample without vanadium, sample dissolution is carried out by step one, shift respectively after cooling in 5 100mL volumetric flasks, be separately added into 100.0 μ g/mL vanadium mark liquid be configured to content of vanadium respectively 0%, 0.100%, 0.500%, 1.00%, 2.00% the working curve standard solution of 5 points, the addition of vanadium amount respectively 0mL, 1.00mL, 5.00mL, 10.00mL, 20.00mL.
Selecting Optima5300DV inductively-coupled plasma spectrometer, select the optimized analysis spectral line 311.071nm of vanadium, main working parameters includes, higher frequency: 40.68MHZ, power: 1300W, plasma gas flow rate: 15L/min, assisted gas flow: 0.2L/min, carrier gas flux: 0.8L/min, solution elevating amount: 1.5mL/min, washing time: 8s, prespark period: 45s, the time of integration: 2～10s are automatic, reading time delay: 30s, observed altitude: 15mm, observed pattern: axially.On inductively-coupled plasma spectrometer, vanadium working curve standard solution and sample solution measuring the spectral intensity of vanadium simultaneously, computer automatic returning calculates analysis result.Performance characteristics according to different inductively-coupled plasma spectrometers, it is also possible to select other glitch-free vanadium analytical line to be analyzed.
To rare earth alloy sample, carry out the test of precision, accuracy by the assay method of the present invention.Result of the test in Table 1,
Table 1
As can be seen from Table 1, the inventive method has higher precision and good accuracy, can meet the needs of production and scientific research, great application value.
The above is the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, under the premise without departing from principle of the present invention; can also making some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (5)
1. the assay method of content of vanadium in a rare earth alloy, it is characterised in that said method comprising the steps of:
Step one: prepare sample solution
Sample is put in polytetrafluoroethylene beaker, add nitric acid, Fluohydric acid., heating for dissolving, add perchloric acid smoked near dry, add hydrochloric acid after taking off beaker cooling and reheat dissolving, be transferred in volumetric flask after cooling, be diluted to scale constant volume with pure water；
Step 2: prepare vanadium Working calibration curve solution
Vanadium Working calibration curve solution is prepared with the rare earth alloy sample without vanadium and vanadium standard solution；
Step 3: on content of vanadium, machine measures
On inductively-coupled plasma spectrometer, vanadium working curve standard solution and sample solution measuring the spectral intensity of vanadium simultaneously, computer automatic returning calculates analysis result.
2. the assay method of content of vanadium in rare earth alloy as claimed in claim 1, it is characterised in that described step one particularly as follows:
Claim 0.1 0.2g rare earth alloy sample, be accurate to 0.1mg, put in polytetrafluoroethylene beaker, adding 10 15mL nitric acid, 5mL Fluohydric acid., on electric hot plate, low-temperature heat is dissolved, add 5mL perchloric acid smoked near dry, take off cooling, add 10mL (1+1) hydrochloric acid, again heating for dissolving on electric hot plate, it is transferred in 100mL volumetric flask after taking off cooling, it is diluted to 100mL volumetric flask scale with pure water, shakes up, do blank test solution in company with sample solution.
3. the assay method of content of vanadium in rare earth alloy as claimed in claim 1, it is characterised in that described step 2 particularly as follows:
Vanadium standard solution with 1000 μ g/mL, dilution is configured to 100.0 μ g/mL, 10.0 the vanadium standard solution of μ g/mL, when content of vanadium≤0.050% in sample, claim the 0.2000g 5 parts of the same kind rare earth alloy sample without vanadium, sample dissolution is carried out by step one, shift respectively after cooling in 5 100mL volumetric flasks, it is separately added into 10.0 μ g/mL vanadium mark liquid and is configured to content of vanadium respectively 0%, 0.005%, 0.010%, 0.020%, the working curve standard solution of 5 points of 0.050%, the addition of vanadium amount respectively 0mL, 1.00mL, 2.00mL, 4.00mL, 10.00mL；As content of vanadium > 0.050%, claim the 0.1000g 5 parts of the same kind rare earth alloy sample without vanadium, sample dissolution is carried out by step one, shift respectively after cooling in 5 100mL volumetric flasks, be separately added into 100.0 μ g/mL vanadium mark liquid be configured to content of vanadium respectively 0%, 0.100%, 0.500%, 1.00%, 2.00% the working curve standard solution of 5 points, the addition of vanadium amount respectively 0mL, 1.00mL, 5.00mL, 10.00mL, 20.00mL.
4. the assay method of content of vanadium in rare earth alloy as claimed in claim 1, it is characterised in that in described method step three:
Selecting Optima5300DV inductively-coupled plasma spectrometer, select the optimized analysis spectral line 311.071nm of vanadium, main working parameters includes, higher frequency: 40.68MHZ, power: 1300W, plasma gas flow rate: 15L/min, assisted gas flow: 0.2L/min, carrier gas flux: 0.8L/min, solution elevating amount: 1.5mL/min, washing time: 8s, prespark period: 45s, the time of integration: 2～10s are automatic, reading time delay: 30s, observed altitude: 15mm, observed pattern: axially.
5. the assay method of content of vanadium in rare earth alloy as claimed in claim 1, it is characterised in that the reagent used in described method includes, and nitric acid: ρ 1.42, top grade is pure；Hydrochloric acid: ρ 1.19, top grade is pure；Fluohydric acid.: ρ 1.13, top grade is pure；Perchloric acid: ρ 1.68, top grade is pure；Hydrochloric acid (1+1), formulated in proportion with top grade pure hydrochloric acid and high purity water.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106290314A (en) * | 2016-08-02 | 2017-01-04 | 内蒙古包钢钢联股份有限公司 | The assay method of content of niobium in rare earth alloy |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101750405A (en) * | 2008-12-15 | 2010-06-23 | 鞍钢股份有限公司 | Method for measuring rare earth component in rare earth magnesium alloy |
| CN102519942A (en) * | 2011-10-28 | 2012-06-27 | 内蒙古包钢钢联股份有限公司 | Method for determining content of lanthanum and cerium of rare-earth silico-calcium alloy |
-
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- 2016-02-26 CN CN201610104514.0A patent/CN105738349A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101750405A (en) * | 2008-12-15 | 2010-06-23 | 鞍钢股份有限公司 | Method for measuring rare earth component in rare earth magnesium alloy |
| CN102519942A (en) * | 2011-10-28 | 2012-06-27 | 内蒙古包钢钢联股份有限公司 | Method for determining content of lanthanum and cerium of rare-earth silico-calcium alloy |
Non-Patent Citations (4)
| Title |
|---|
| 卢文琪 等: "火焰原子吸收光谱法测定稀土钙镁硅铁合金中的钙和镁", 《光谱仪器与分析》 * |
| 彭银仙: "《工业分析》", 31 January 2014, 哈尔滨工程大学出版社，第一版 * |
| 徐盘明 等: "《实用金属材料分析方法》", 31 May 2015, 中国科学技术大学出版社，第2版 * |
| 杨忠梅 等: "电感耦合等离子体原子发射光谱法测定钢中低含量钒和铌", 《冶金分析》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106290314A (en) * | 2016-08-02 | 2017-01-04 | 内蒙古包钢钢联股份有限公司 | The assay method of content of niobium in rare earth alloy |
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Application publication date: 20160706 |