CN102519941A - Method for measuring vanadium element in titanium alloy - Google Patents
Method for measuring vanadium element in titanium alloy Download PDFInfo
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- CN102519941A CN102519941A CN2011103338232A CN201110333823A CN102519941A CN 102519941 A CN102519941 A CN 102519941A CN 2011103338232 A CN2011103338232 A CN 2011103338232A CN 201110333823 A CN201110333823 A CN 201110333823A CN 102519941 A CN102519941 A CN 102519941A
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Abstract
The invention discloses a method for measuring vanadium element in titanium alloy. The method comprises the following steps of: dissolving a sample by using sulfuric acid; adding a few drops of nitric acid; adding pure water to prepare sample solution; preparing standard solution containing vanadium of different concentrations; determining spectral line intensity of the standard solution by using an inductively coupled plasma emission spectrometer, and drawing a working curve by taking vanadium element concentration as an abscissa and the spectral line intensity as an ordinate; determining the spectral line intensity of the sample solution by using the inductively coupled plasma emission spectrometer; calculating the concentration of the vanadium element according to the working curve; and selecting an analytical spectral line as 290.880 nm in a process of determining the spectral line intensity by using the inductively coupled plasma emission spectrometer.
Description
Technical field
The present invention relates to the measuring method of v element in a kind of titanium alloy, specifically, relate to a kind of method that can measure the v element of high-load in the titanium alloy quickly and accurately.
Background technology
Many advantages such as that titanium and alloy thereof have is in light weight, intensity is big, thermotolerance is strong, corrosion-resistant are described as " following metal ", are the new structural materials with development prospect.Titanium and alloy thereof not only have crucial application in aviation, universe aircraft industry, and have begun widespread use in many industrial sectors such as chemical industry, oil, light industry, metallurgy, generating.
The main secondary element in the titanium alloy and the content of interstitial impurity element are very big to the mechanical property influence of titanium material; Along with the change of these constituent contents, its mechanical property and hardness also change thereupon, simultaneously plasticity, toughness is corresponding changes; Different according to its impurity content; Can form the titanium material of the different trades mark, in industry, produce different purposes, the value that is produced also has very big difference.TB5 is the good a kind of titanium alloy of present home market prospect.Its product technology condition sees the following form 1:
Table 1TB5 product technology condition
It and other titanium alloy evident difference are exactly that content of vanadium is high especially.At present, the detection to v element in the titanium alloy mainly contains three kinds: traditional chemical analytic approach, inductively coupled plasma emission spectrography, atomic absorption spectrography (AAS).The traditional chemical analytic approach mainly contains: ferrous ammonium sulfate titration, and its sample pre-treatment time is long, complex operation, analysis speed is slow, and precision is poor.That atomic absorption spectrography (AAS) has is simple to operate, detect lower limit low, disturb little, result to wait characteristics accurately and reliably; But it is slower for multielement analysis; Can only analyze a kind of element at every turn; The sensing range of its analytical element is accurately measured for the element of high-load is then very difficult generally at several PPb to tens PPm.Inductively coupled plasma emission spectrography can be accomplished in a sample solution simultaneously to its contained disposable measuring of multiple element; Have simple to operate, detect that lower limit is low, analysis speed is fast, the range of linearity is wide, the result waits characteristics accurately and reliably, having developed rapidly becomes a kind of conventional method of analysis of extensively and generally adopting.Its shortcoming is the spectral line serious interference.At present, inductively coupled plasma emission spectrography is measured the content of V all below 10%, be higher than 10% after, its precision and accuracy are just very poor.
Therefore, need a kind of method that can measure the v element of high-load in the titanium alloy quickly and accurately.
Summary of the invention
Each side of the present invention provides the measuring method of v element in a kind of titanium alloy, and said method comprises the steps: to use sulfuric acid with sample dissolution, adds several nitric acid then, adds pure water and is configured to sample solution; Utilize the matrix composition quite and not to contain vanadium or content of vanadium is few and the titanium alloy original pattern of known its content of vanadium in add variable concentrations the preparation of v element standard solution contain the standard solution of variable concentrations vanadium; Utilizing line strength of inductive coupling plasma emission spectrograph bioassay standard solution, is horizontal ordinate with the v element concentration in the titanium alloy, is ordinate drawing curve with line strength; Utilize inductive coupling plasma emission spectrograph to measure line strength of sample solution, calculate v element concentration according to working curve, utilizing inductive coupling plasma emission spectrograph to measure in the process of line strength, the selection analysis spectral line is 290.880nm.
According to an aspect of the present invention, in the step that adds nitric acid with add and also can comprise between the step of pure water preparation sample solution and make its volume less than 10mL the sample solution boiling.
According to an aspect of the present invention; The analytical parameters of inductive coupling plasma emission spectrograph is: high frequency power 1100-1400W, atomization gas flow 0.65-0.85L/min, secondary air amount 0.15-0.25L/min; Sample lifting capacity 1.2-1.8mL/min, observed pattern are axial.
According to an aspect of the present invention, in the step with the sulfuric acid dissolution sample, the concentration of the sulfuric acid of adding is 1+1 to 1+3.
Embodiment
To describe in detail according to exemplary embodiment of the present invention below.
Measuring method according to v element in the titanium alloy of the embodiment of the invention comprises the steps: to use sulfuric acid with sample dissolution, adds several nitric acid then, adds pure water and is configured to sample solution; Utilize the matrix composition quite and not to contain vanadium or content of vanadium is few and the titanium alloy original pattern of known its content of vanadium in add variable concentrations the preparation of v element standard solution contain the standard solution of variable concentrations vanadium; Utilizing line strength of inductive coupling plasma emission spectrograph bioassay standard solution, is horizontal ordinate with the v element concentration in the titanium alloy, is ordinate drawing curve with line strength; Utilize inductive coupling plasma emission spectrograph to measure line strength of sample solution, calculate v element concentration according to working curve.
Utilizing inductive coupling plasma emission spectrograph to measure in the process of line strength, the selection analysis spectral line is 290.880nm.Usually, the spectral line of inductive coupling plasma emission spectrograph mensuration vanadium has 290.880nm, 310.230nm, 309.310nm, 292.402nm, 311.071nm etc.When choosing spectral line 290.880nm, its line strength is big and other element interference is very little.When choosing spectral line 310.230nm, line strength is taken second place, and other element disturbs less.When choosing spectral line 309.310nm, disturbed by the spectrum of Al and Nb element, line strength is placed in the middle.When choosing spectral line 292.402nm, other element disturbs less but line strength is very little.When choosing spectral line 311.071nm, disturbed by the spectrum of Be and Nb element, line strength is less.Therefore, according to one embodiment of present invention, the selection analysis spectral line is 290.880nm, thereby can obtain analysis result more accurately.
Sulfuric acid is joined in the sample, thereby the titanium alloy sample can generate corresponding soluble salt with sulfuric acid reaction and be dissolved in the sulfuric acid.The concentration that those skilled in the art have grasped along with sulfuric acid increases; Metal can dissolve more easily; And when sulfuric acid concentration is too high; May be owing to the metal surface form the further reaction that passivation layer stops metal and sulfuric acid, the characteristic of sulfuric acid dissolution metal is well known to a person skilled in the art, therefore no longer carries out detailed description at this.Those skilled in the art can select suitable sulfuric acid concentration and consumption in conjunction with actual conditions according to the characteristic of sulfuric acid and metal reaction.
According to one embodiment of present invention, preferably, the sulfuric acid concentration of adding is (1+1-1+3), when sulfuric acid concentration＞1+1, makes the sample passivation easily, makes to dissolve the chronic even dissolved samples fully of appearance.When sulfuric acid concentration＜1+3, the concentration of sulfuric acid is lower, and along with the rising of temperature, water progressively evaporates, and after the water evaporation was a certain amount of, test solution was emitted a large amount of heat and made the titanium alloy dissolving, dissolved a kind time lengthening like this.
According to one embodiment of present invention, when the weight of sample was 0.1000g, the consumption of sulfuric acid was 5-30mL, and when sulfuric acid amount＜5mL, solution is difficult for dissolved samples very little.When sulfuric acid amount＞30mL, because the viscosity of sulfuric acid is big, when liquid acidity to be measured was big, the easy blocking atomizer reduced instrumental sensitivity.
Use sulfuric acid with after the sample dissolution, also can in solution, add several nitric acid, make solution titanyl at a middle or low price change into the high price titanium.After adding nitric acid, can more easily observe the dissolving situation of sample, thereby help the carrying out of subsequent step.
According to one embodiment of present invention, after using sulfuric acid and nitric acid dissolve sample,, make its volume less than 10mL the sample solution boiling if the sample solution volume greater than 10mL, also can carry out boiling to sample solution and handle.Through improving the precision of detection significantly after the boiling processing.
According to one embodiment of present invention; The analytical parameters of inductive coupling plasma emission spectrograph is: high frequency power 1100-1400W, atomization gas flow 0.65-0.85L/min, secondary air amount 0.15-0.25L/min; Sample lifting capacity 1.2-1.8mL/min, observed pattern are axial.Utilize above-mentioned analytical parameters to measure and to obtain measurement result accurately apace, yet the invention is not restricted to this, can suitably adjust the analytical parameters of inductive coupling plasma emission spectrograph according to actual needs.
To the measuring method according to v element in the titanium alloy of the present invention be described with reference to concrete example below.
(1) takes by weighing 0.1000g (being accurate to 0.0001g) sample in the 200mL conical flask; Add 5-30mL sulfuric acid (1+1-1+3), low-temperature heat to sample dissolves fully basically, adds several nitric acid oxidations titanium at a low price and is the high price titanium; Continue low-temperature heat to decomposing fully, the boiling test solution makes its volume less than 10mL.Be cooled to room temperature, solution quantitatively is transferred in the 200mL volumetric flask, be diluted to scale with high purity water, mixing obtains sample solution.
(2) take by weighing that the contained matrix composition of 0.1000g (being accurate to 0.0001g) quite and not contains vanadium or content of vanadium is few and 5 parts of the titanium alloy original patterns of known its content of vanadium; Place 5 200mL conical flasks, add the 1mg/mL vanadium standard solution of 0mL, 5mL, 10mL, 15mL, 20mL successively.Method dissolving according to step (1) is settled to 200mL, obtains standard serial solution.With 290.880 as analysis spectral line, utilize inductive coupling plasma emission spectrograph successively standard serial solution to be scanned, just obtain standard working curve.
(3) utilize inductive coupling plasma emission spectrograph to measure line strength of sample solution, calculate v element concentration according to working curve.
Example 1
The titanium alloy sample that takes by weighing 0.1000g (being accurate to 0.0001g) content of vanadium 15.10% adds 10mL sulfuric acid (1+1) in the 200mL conical flask, low-temperature heat to sample dissolves fully basically, adds several nitric acid, continues low-temperature heat to decomposing fully, and the test solution boiling is to 5mL.Be cooled to room temperature, solution quantitatively is transferred in the 200mL volumetric flask, be diluted to scale with high purity water, mixing obtains solution to be measured.With solution to be measured at following analysis condition: analysis spectral line is 290.880nm, high frequency power 1300W, atomization gas flow 0.75L/min, secondary air amount 0.20L/min, sample lifting capacity 1.6mL/min, observed pattern: axially; Utilizing inductive coupling plasma emission spectrograph to measure line strength is 3016500.2, confirms that according to standard working curve its v element concentration is 15.03% (standard code tolerance≤0.25%).
Example 2
The titanium alloy sample that takes by weighing 0.1000g (being accurate to 0.0001g) content of vanadium 15.10% adds 15mL sulfuric acid (1+1) in the 200mL conical flask, low-temperature heat to sample dissolves fully basically, adds several nitric acid, continues low-temperature heat to decomposing fully, and the test solution boiling is to 8mL.Be cooled to room temperature, solution quantitatively is transferred in the 200mL volumetric flask, be diluted to scale with high purity water, mixing obtains solution to be measured.With solution to be measured at following analysis condition: analysis spectral line is 290.880nm, high frequency power 1300W, atomization gas flow 0.80L/min, secondary air amount 0.20L/min, sample lifting capacity 1.7mL/min, observed pattern: axially; Utilizing inductive coupling plasma emission spectrograph to measure line strength is 3031668.0, confirms that according to standard working curve its v element concentration is 15.11% (standard code tolerance≤0.25%).
Visible through above concrete example, v element concentration and the actual value of utilizing method of the present invention to measure differ very little, and its error is all above 0.1%, this in the standard defined be less than or equal to 0.25% error.Therefore, the v element concentration that obtains according to the method for the invention is reliable.
Utilization can be measured the content of vanadium in the titanium alloy exactly according to measuring method of the present invention, can shorten greatly simultaneously and measure the required time, therefore can measure the v element of high-load in the titanium alloy quickly and accurately.
Though combined exemplary embodiment the present invention has been described; But those skilled in the art should understand that; Under the situation that does not break away from the spirit and scope of the present invention; Can carry out the various changes on form and the details to these embodiment, scope of the present invention is limited claims and equivalent thereof.
Claims (4)
1. the measuring method of v element in the titanium alloy, said method comprises the steps:
Use sulfuric acid with sample dissolution, add several nitric acid then, add pure water and be configured to sample solution;
Utilize the matrix composition quite and not to contain vanadium or content of vanadium is few and the titanium alloy original pattern of known its content of vanadium in add variable concentrations the preparation of v element standard solution contain the standard solution of variable concentrations vanadium;
Utilizing line strength of inductive coupling plasma emission spectrograph bioassay standard solution, is horizontal ordinate with the v element concentration in the titanium alloy, is ordinate drawing curve with line strength;
Utilize inductive coupling plasma emission spectrograph to measure line strength of sample solution, calculate v element concentration according to working curve;
Utilizing inductive coupling plasma emission spectrograph to measure in the process of line strength, the selection analysis spectral line is 290.880nm.
2. the measuring method of v element as claimed in claim 1 wherein, also comprises making its volume less than 10mL the sample solution boiling between the step of step that adds nitric acid and adding pure water preparation sample solution.
3. the measuring method of v element as claimed in claim 1; Wherein, The analytical parameters of inductive coupling plasma emission spectrograph is: high frequency power 1100-1400W, atomization gas flow 0.65-0.85L/min, secondary air amount 0.15-0.25L/min; Sample lifting capacity 1.2-1.8mL/min, observed pattern are axial.
4. the measuring method of v element as claimed in claim 1, wherein, in the step with the sulfuric acid dissolution sample, the concentration of the sulfuric acid of adding is 1+1 to 1+3.
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Cited By (6)
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| CN102866145A (en) * | 2012-09-27 | 2013-01-09 | 东方电气集团东方汽轮机有限公司 | Method for measuring total vanadium concentration in all vanadium redox flow battery electrolyte |
| CN103424399A (en) * | 2013-07-19 | 2013-12-04 | 中国船舶重工集团公司第七二五研究所 | Analytic method for simultaneously determining percentage content of nine impurity elements in titanium sponge |
| CN103424398A (en) * | 2013-07-19 | 2013-12-04 | 中国船舶重工集团公司第七二五研究所 | Method for measuring barium percentage composition in titanium sponge |
| CN104713870A (en) * | 2013-12-12 | 2015-06-17 | 陕西宏远航空锻造有限责任公司 | Method for determining trace elements in Ti-AL-V-base titanium alloy |
| CN106556591A (en) * | 2016-12-01 | 2017-04-05 | 青海聚能钛业股份有限公司 | A kind of electron beam cold hearth single melting TC4 titan alloy casting ingot chemical composition methods of inspection |
| CN113063774A (en) * | 2021-03-12 | 2021-07-02 | 中航金属材料理化检测科技有限公司 | Method for measuring contents of multiple elements in titanium alloy |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102866145A (en) * | 2012-09-27 | 2013-01-09 | 东方电气集团东方汽轮机有限公司 | Method for measuring total vanadium concentration in all vanadium redox flow battery electrolyte |
| CN103424399A (en) * | 2013-07-19 | 2013-12-04 | 中国船舶重工集团公司第七二五研究所 | Analytic method for simultaneously determining percentage content of nine impurity elements in titanium sponge |
| CN103424398A (en) * | 2013-07-19 | 2013-12-04 | 中国船舶重工集团公司第七二五研究所 | Method for measuring barium percentage composition in titanium sponge |
| CN103424399B (en) * | 2013-07-19 | 2015-06-24 | 中国船舶重工集团公司第七二五研究所 | Analytic method for simultaneously determining percentage content of nine impurity elements in titanium sponge |
| CN103424398B (en) * | 2013-07-19 | 2015-08-05 | 中国船舶重工集团公司第七二五研究所 | A kind of assay method for barium percentage composition in titanium sponge |
| CN104713870A (en) * | 2013-12-12 | 2015-06-17 | 陕西宏远航空锻造有限责任公司 | Method for determining trace elements in Ti-AL-V-base titanium alloy |
| CN104713870B (en) * | 2013-12-12 | 2017-06-06 | 陕西宏远航空锻造有限责任公司 | A kind of method of trace element in measure Ti AL V series titanium alloys |
| CN106556591A (en) * | 2016-12-01 | 2017-04-05 | 青海聚能钛业股份有限公司 | A kind of electron beam cold hearth single melting TC4 titan alloy casting ingot chemical composition methods of inspection |
| CN113063774A (en) * | 2021-03-12 | 2021-07-02 | 中航金属材料理化检测科技有限公司 | Method for measuring contents of multiple elements in titanium alloy |
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Application publication date: 20120627 |