CN102128820A - Method for analyzing impurity elements in aluminum bronze intermediate alloy - Google Patents
Method for analyzing impurity elements in aluminum bronze intermediate alloy Download PDFInfo
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- CN102128820A CN102128820A CN 201010585323 CN201010585323A CN102128820A CN 102128820 A CN102128820 A CN 102128820A CN 201010585323 CN201010585323 CN 201010585323 CN 201010585323 A CN201010585323 A CN 201010585323A CN 102128820 A CN102128820 A CN 102128820A
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Abstract
The invention provides a method for analyzing impurity elements in aluminum bronze intermediate alloy. In the method, aluminum bronze intermediate alloy is subjected to spectral analysis by taking a copper electrode as an auxiliary electrode, wherein the purity of copper in the copper electrode is over 99.999 percent. Compared with the prior art, aluminum bronze intermediate alloy is subjected to the spectral analysis by taking the copper of which the purity is over 99.999 percent as the auxiliary electrode, and the pure copper serving as the auxiliary electrode can eliminate the matrix effect of the copper in the aluminum bronze intermediate alloy and reduce the interference of the copper by being excited, so that the content of obtained impurity elements has small error and is accurate. Experiments indicate that the result of the spectral analysis of the aluminum bronze intermediate alloy by taking the copper of which the purity is over 99.999 percent as the auxiliary electrode is basically the same as that obtained by a chemical analysis process, but is more accurate.
Description
Technical field
The invention belongs to the aluminium alloy technical field, relate in particular to a kind of analytical approach of aluminum bronze intermediate alloy impurity element.
Background technology
In aluminium alloy, Cu extensively is used to improve the intensity of aluminium alloy as intensified element, have certain solid solution strengthening effect as Cu itself, the CuAl that timeliness is separated out
2Has tangible strengthening effect etc.Discover, in aluminium alloy, add the Cu element, not only can improve flowability, tensile strength and the hardness of aluminium alloy, can also improve stress corrosion resistance, cyclic strains fatigue resistance and the fracture toughness of aluminium alloy, as being to add copper in the alloy not only can improve its mechanical property at Al-Zn-Mg, can also improve its etch resistant properties.But the fusing point of Cu is 1083.4 ℃, is much higher than 660.37 ℃ of Al, 648.9 ℃ and 419.5 ℃ of Zn of Mg, needs higher smelting temperature when being the feedstock production aluminium alloy with the fine copper, and is not only higher to equipment requirements, and can increase cost.
Intermediate alloy is for ease of add one or more elements and the alloy of special configuration in casting alloy, high-melting-point alloy is fused under lower temperature, as the Al-Cu intermediate alloy of cupric 48%～52% adding temperature when the melting is 680 ℃～720 ℃, therefore, in the fusion process of aluminium alloy, be the interpolation that raw material is realized Cu generally with the Al-Cu intermediate alloy.Be that raw material is when carrying out the interpolation of Cu with the Al-Cu intermediate alloy, in order accurately to control the addition of Cu, in order to avoid excessive Cu reduces the performance of aluminium alloy or introduces other impurity elements, need the impurity element of Al-Cu intermediate alloy be analyzed as the content of Si, Fe, Mn, Mg, Zn, Ti, Ni etc.
Spectrographic method is that the intensity of the characteristic spectrum of launching under excited state according to tested atom or molecule is calculated a kind of method of constituent content because have fast, accurately, environmental protection, characteristics such as easy and simple to handle, be widely used in the impurity analysis of Al-Cu intermediate alloy.In the process of carrying out spectral analysis, general with the matrix in the sample as internal standard element, adopt internal standard method to analyze, promptly in the impurity analysis of Al-Cu intermediate alloy, generally analyze as internal standard element with Al.But, in the Al-Cu alloy, the content of Cu is generally more than 40%, and spectroanalysis instrument generally adopts electrodes such as tungsten, carbon or silver as auxiliary electrode, make that the matrix effect that Cu produces in the Al-Cu alloy is comparatively obvious, make that the impurity content that records is inaccurate, error is bigger, is unfavorable for the preparation and the use of Al-Cu intermediate alloy.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of analytical approach of aluminum bronze intermediate alloy impurity element, and analytical approach error provided by the invention is less, and accuracy is higher.
The invention provides a kind of analytical approach of aluminum bronze intermediate alloy impurity element, is that auxiliary electrode carries out spectral analysis to the aluminum bronze intermediate alloy with the copper electrode, and the purity of copper is more than 99.999% in the described copper electrode.
Preferably, the purity of copper is more than 99.9999% in the described copper electrode.
Preferably, the using plasma emission spectrometer carries out spectral analysis to described aluminum bronze intermediate alloy.
Preferably, the exciting power of described plasma emission spectrometer is 1050W～1250W.
Preferably, be the integral time of described plasma emission spectrometer: visible region 2s～5s, ultraviolet region 10s～30s.
Preferably, the atomizing pressure of described plasma emission spectrometer is 22PSI～35PSI.
Preferably, the peristaltic pump rotating speed of described plasma emission spectrometer is 100rpm～120rpm.
Preferably, described aluminum bronze intermediate alloy comprises following composition:
The Cu of 40wt%～60wt%;
Surplus is Al.
Compared with prior art, the present invention is that copper more than 99.999% carries out spectral analysis as auxiliary electrode to the aluminum bronze intermediate alloy with purity, fine copper participates in exciting as auxiliary electrode, can eliminate the matrix effect of copper in the aluminum bronze intermediate alloy, reduce the interference of copper, thereby make the impurity content error of acquisition less, comparatively accurate.Experiment shows, is copper more than 99.999% when as auxiliary electrode the aluminum bronze intermediate alloy being carried out spectral analysis with purity, and with the no significant difference as a result that chemical analysis obtains, the result is comparatively accurate.
Embodiment
The invention provides a kind of analytical approach of aluminum bronze intermediate alloy impurity element, is that auxiliary electrode carries out spectral analysis to the aluminum bronze intermediate alloy with the copper electrode, and the purity of copper is more than 99.999% in the described copper electrode.
When the impurity element in the aluminum bronze intermediate alloy being analyzed,, can form matrix effect when analyzing during as internal standard element, thereby influence result's accuracy with aluminium because copper content is higher in the aluminum bronze intermediate alloy with spectrographic method.The present invention with purity be copper more than 99.999% as auxiliary electrode, can participate in atomic excitation, eliminate the matrix effect of copper in the aluminum bronze intermediate alloy, thereby improve precision of analysis.
According to the present invention, the purity of copper is preferably more than 99.9999% in the described copper electrode, and the copper that purity is high more can reduce the interference effect of copper in the aluminium copper more as auxiliary electrode.
After auxiliary electrode in the commercially available spectroanalysis instrument replaced with copper electrode, adopt conventional method can realize analysis to the aluminum bronze intermediate alloy.Described copper electrode can be that raw material processes according to method well known to those skilled in the art with the copper rod according to the different requirement of each spectrometer.
Since plasma source have good detectability, higher analysis precision, easy and simple to handle, can realize advantage such as multielement simultaneous determination, the preferred using plasma emission spectrometer of the present invention carries out spectral analysis to described aluminum bronze intermediate alloy, specifically may further comprise the steps:
A) Al-Cu intermediate alloy standard model is dissolved in the mixed liquor of hydrochloric acid and nitric acid, behind the dissolution in low temperature, slowly adds volumetric concentration and be 33.3% hydrofluorite and mass concentration and be 5% boric acid, solution gets standard samples after the dilution;
B) described standard model solution being excited on plasma emission spectrometer, obtain the emissive porwer and the mass concentration of each element, is horizontal ordinate with the mass concentration, and corresponding emissive porwer is the standard working curve that ordinate is drawn each impurity element respectively;
C) Al-Cu intermediate alloy testing sample is dissolved in the mixed liquor of hydrochloric acid and nitric acid, behind the dissolution in low temperature, slowly adds volumetric concentration and be 33.3% hydrofluorite and mass concentration and be 5% boric acid, obtain testing sample solution after the dilution;
D) described testing sample solution is excited on plasma emission spectrometer, obtain the emissive porwer of each impurity element, the standard working curve that obtains according to step b) obtains the mass concentration of each impurity element, thereby obtains the content of each impurity element.
In order to obtain better analytical effect, described aluminum bronze intermediate alloy preferably includes following component:
The Cu of 40wt%～60wt%;
Surplus is Al.
Preferred, described aluminum bronze intermediate alloy comprises following component:
The Cu of 48wt%～52wt%;
Surplus is Al.
According to the method described above, preparation, the detection method of the preparation of standard model solution, detection method and testing sample solution are identical, for for simplicity, are called the preparation of sample solution and the detection of sample solution hereinafter.
In the aluminum bronze intermediate alloy, there is sour insoluble silicon, the present invention at first with sample dissolution in the mixed solution of hydrochloric acid and nitric acid, in solution, add volumetric concentration again and be 33.3% hydrofluorite and mass concentration and be 5% boric acid, to reduce the error of silica test.The present invention does not have particular restriction to the mixed solution of described hydrochloric acid and nitric acid, sample dissolution can be got final product.In order to prevent the hydrofluorite etching apparatus, effect is measured in the boric acid influence, and the present invention preferably controls the consumption of hydrofluorite and boric acid, and the mass volume ratio of described sample, hydrofluorite and boric acid is preferably 0.1g～0.5g: 1mL～3mL: 2mL～5mL.
Behind above-mentioned solution dilution, can obtain sample solution after, the using plasma emission spectrometer is analyzed described sample solution.In analytic process, the exciting power of described plasma emission spectrometer is preferably 950W～1350W, more preferably 1050W～1250W; Be preferably the integral time of described plasma emission spectrometer: visible region 2s～5s, ultraviolet region 10s～30s, visible region 3s～4s more preferably, ultraviolet region 15s～25s; The atomizing pressure of described plasma emission spectrometer is preferably 22PSI～35PSI, more preferably 25PSI～30PSI; The peristaltic pump rotating speed of described plasma emission spectrometer is preferably 80rpm～150rpm, more preferably 100rpm～120rpm.
Described standard model solution placed on the plasma emission spectrometer excite, can obtain the emissive porwer of each element, mass concentration with each impurity element in the standard solution is a horizontal ordinate, and the corresponding emissive porwer of its of acquisition is the standard working curve that ordinate is drawn each impurity element respectively.When carrying out the drafting of typical curve, as internal standard element, adopt internal standard method to draw and follow-up analysis with aluminium.
When adopting internal standard method to analyze and since with purity be copper electrode 99.999% or more as auxiliary electrode, the copper electrode participation excites, and can significantly reduce the matrix effect of copper in the aluminum bronze intermediate alloy, thereby make analysis result more accurate.
After obtaining the typical curve of each impurity element, can obtain the mass concentration of each impurity element according to the emissive porwer of each impurity element in the testing sample of this typical curve and acquisition, and then learn the content of each impurity element in the aluminum bronze intermediate alloy.
Compared with prior art, the present invention is that copper more than 99.999% carries out spectral analysis as auxiliary electrode to the aluminum bronze intermediate alloy with purity, fine copper participates in exciting as auxiliary electrode, can eliminate the matrix effect of copper in the aluminum bronze intermediate alloy, reduce the interference of copper, thereby make the impurity content error of acquisition less, comparatively accurate.Experiment shows, is copper more than 99.999% when as auxiliary electrode the aluminum bronze intermediate alloy being carried out spectral analysis with purity, and with the no significant difference as a result that chemical analysis obtains, the result is comparatively accurate.
In order to further specify the present invention, the analytical approach of copper-aluminium master alloy impurity element provided by the invention is described in detail below in conjunction with embodiment.
Embodiment 1
The aluminum bronze intermediate alloy standard model of 0.3g cupric 52wt% is dissolved in the mixed solution of being made up of 5mL hydrochloric acid and 10mL nitric acid, the slow adding in cooling back 2mL volumetric concentration is 33.3% hydrofluorite and 3mL boric acid, be diluted to 100mL, solution gets standard samples;
After the auxiliary electrode of Tianjin, island/ICPS-8100 inductive coupling plasma emission spectrograph is changed to copper electrode, described standard model solution is analyzed, analysis condition is as follows: exciting power is 1010W, be integral time: visible region 2s, ultraviolet region 20s, the pressure of atomizer is 25PSI, and the peristaltic pump rotating speed is 100rpm.Read the emissive porwer of Al, Si, Fe, Mn, Mg, Zn, Ti and Ni, and, utilize internal standard method to draw the standard working curve of each impurity element according to the mass concentration and the corresponding emissive porwer of each element in the above-mentioned standard model solution.
0.3g aluminum bronze intermediate alloy testing sample is dissolved in the mixed solution of being made up of 5mL hydrochloric acid and 10mL nitric acid, the slow adding in cooling back 2mL volumetric concentration is 33.3% hydrofluorite and 3mL boric acid, be diluted to 100mL, obtain testing sample solution, adopt following three kinds of methods that described testing sample solution is analyzed respectively:
(1) be that auxiliary electrode is analyzed with the Cu electrode:
The auxiliary electrode of Tianjin, island/ICPS-8100 inductive coupling plasma emission spectrograph is changed to after purity is 99.9999% copper electrode, described standard model solution is analyzed, analysis condition is as follows: exciting power is 1010W, be integral time: visible region 2s, ultraviolet region 20s, the pressure of atomizer is 25PSI, and the peristaltic pump rotating speed is 100rpm.Read the emissive porwer of Al, Si, Fe, Mn, Mg, Zn, Ti and Ni, and obtain the mass concentration of Si, Fe, Mn, Mg, Zn, Ti and Ni according to Fig. 1～typical curve shown in Figure 7, the result is referring to table 1, the impurities analysis result that table 1 provides for the embodiment of the invention;
(2) be that auxiliary electrode is analyzed with the W electrode:
With Tianjin, island/ICPS-8100 inductive coupling plasma emission spectrograph described standard model solution is analyzed, its auxiliary electrode is a tungsten electrode, analysis condition is as follows: exciting power is 1010W, be integral time: visible region 2s, ultraviolet region 20s, the pressure of atomizer is 25PSI, and the peristaltic pump rotating speed is 100rpm.Read the emissive porwer of Al, Si, Fe, Mn, Mg, Zn, Ti and Ni, and obtain the mass concentration of Si, Fe, Mn, Mg, Zn, Ti and Ni according to Fig. 1～typical curve shown in Figure 7, the result is referring to table 1, the impurities analysis result that table 1 provides for the embodiment of the invention;
(3) chemically analyze:
Adopt gravimetric method to analyze the content of Si in the described testing sample solution; Adopt the content of Fe in the described testing sample solution of phenanthrolene spectrophotometry; Adopt the content of Mn in the described testing sample solution of potassium metaperiodate spectrophotometry; Adopt the content of Mg in the described testing sample solution of CDTA titration measuring; Adopt the content of Zn in the described testing sample solution of EDTA titration measuring; Adopt the content of Ti in the described testing sample solution of hydrogen peroxide spectrophotometry; Adopt the content of Ni in the described testing sample solution of dimethylglyoxime spectrophotometry; The result is referring to table 1, the impurities analysis result that table 1 provides for the embodiment of the invention.
The impurities analysis result that table 1 embodiment of the invention provides
As shown in Table 1, compare with the W electrode impurity content that analysis obtains as auxiliary electrode, the impurity content that impurity content that the Cu electrode obtains as auxiliary electrode and chemical analysis obtain is more approaching, and deviation is littler.That is to say, be auxiliary electrode when the aluminum bronze intermediate alloy is carried out spectral analysis with Cu, and with the no significant difference as a result that chemical analysis obtains, the result is comparatively accurate.
The above only is a preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (8)
1. the analytical approach of an aluminum bronze intermediate alloy impurity element is characterized in that, is that auxiliary electrode carries out spectral analysis to the aluminum bronze intermediate alloy with the copper electrode, and the purity of copper is more than 99.999% in the described copper electrode.
2. analytical approach according to claim 1 is characterized in that, the purity of copper is more than 99.9999% in the described copper electrode.
3. analytical approach according to claim 1 is characterized in that, the using plasma emission spectrometer carries out spectral analysis to described aluminum bronze intermediate alloy.
4. analytical approach according to claim 3 is characterized in that, the exciting power of described plasma emission spectrometer is 1050W～1250W.
5. analytical approach according to claim 3 is characterized in that, be the integral time of described plasma emission spectrometer: visible region 2s～5s, ultraviolet region 10s～30s.
6. analytical approach according to claim 3 is characterized in that, the atomizing pressure of described plasma emission spectrometer is 22PSI～35PSI.
7. analytical approach according to claim 3 is characterized in that, the peristaltic pump rotating speed of described plasma emission spectrometer is 100rpm～120rpm.
8. analytical approach according to claim 1 is characterized in that, described aluminum bronze intermediate alloy comprises following composition:
The Cu of 40wt%～60wt%;
Surplus is Al.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108627501A (en) * | 2018-05-08 | 2018-10-09 | 中国航发北京航空材料研究院 | A method of measuring elemental lithium in WE43A alloys |
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|---|---|---|---|---|
| US3406308A (en) * | 1966-10-04 | 1968-10-15 | Westinghouse Electric Corp | Electron discharge device for generation of spectral radiation having an auxiliary discharge of low current |
| CN1227632A (en) * | 1996-07-01 | 1999-09-01 | 埃姆特克磁化股份有限公司 | Process and apparatus for laser-induced spectral analysis |
| US6645364B2 (en) * | 2000-10-20 | 2003-11-11 | Shipley Company, L.L.C. | Electroplating bath control |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108627501A (en) * | 2018-05-08 | 2018-10-09 | 中国航发北京航空材料研究院 | A method of measuring elemental lithium in WE43A alloys |
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Application publication date: 20110720 |