CN105424681A - Assay method of chemical elements in Mg-Zn-Re intermediate alloy - Google Patents
Assay method of chemical elements in Mg-Zn-Re intermediate alloy Download PDFInfo
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- CN105424681A CN105424681A CN201510981355.8A CN201510981355A CN105424681A CN 105424681 A CN105424681 A CN 105424681A CN 201510981355 A CN201510981355 A CN 201510981355A CN 105424681 A CN105424681 A CN 105424681A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention provides an assay method of chemical elements in Mg-Zn-Re intermediate alloy and belongs to the field of analysis and measurement. The assay method includes the steps of: preparing a to-be-assayed solution, preparing a standard curve solution and making a working curve; and assaying the working curve of the to-be-assayed solution. In the invention, a unique method is employed with usage of an ICP emission spectrometer. The method can be used for assaying the contents of Zn, Si, Cu, Ni, Mn and Fe in the Mg-Zn-Re intermediate alloy at the same time, is less in required reagent, can save time and can satisfy production timely.
Description
Technical field
The invention belongs to analysis to measure field, particularly relate to the assay method of chemical element in a kind of Mg-Zn-Re intermediate alloy.
Background technology
Mg-Zn-Re alloy has good casting fluidity, excellent greenhouse mechanical property and high-temperature creep resistance, plays serviceability temperature and can reach more than 300 DEG C, be widely used on the engine of aircraft and automobile, gear box casing.The Properties Control of essential element assay to Mg-Zn-Re alloy wherein in Mg-Zn-Re alloy is most important, in Mg-Zn-Re alloy, essential element now adopts classical chemical analysis method, classical chemical analysis method must through the chemical treatment of complexity, analytical cycle is long, complex operation, application reagent is many, and can only single element mensuration be carried out, be subject to the impact of some disturbing factors and external condition, can not meet the requirement of ironcasting to high-purity raw and auxiliary material impurity analysis, the detection therefore for trace element contained in modulizer adopts classical analysis method to realize.
Current ICP-AES is in the high-end analytical test field widespread use of China, it has higher evaporation-atomization-excite and ionizing power, Matrix effects level is low, precision is good, the typical curve range of linearity is wider and the advantages such as efficient and sensible, is particularly useful for the analysis of Minor element, is that a kind of cost is few, pollute few, flow process is short, has the rapid analysis of the feature of environmental protection, and is suitable for the Simultaneously test of all multielements.And the content applying the essential element that ICP-AES method measures in Mg-Zn-Re alloy does not also have pertinent literature to report so far.
Summary of the invention
For solving the problems of the technologies described above, the invention provides the assay method of chemical element in a kind of Mg-Zn-Re intermediate alloy.
The present invention is achieved by the following technical programs.
The assay method of chemical element in a kind of Mg-Zn-Re intermediate alloy provided by the invention, comprises the following steps:
1) take sample to be tested 0.1gMg-Zn-Re intermediate alloy, slowly add after hydrochloric acid dissolves completely to sample in beaker, then add hydrofluorite, heating is boiled, and is diluted to 100ml after taking off cooling, makes night to be measured;
2) configuration standard curve solution, take the Mg-Zn-Re intermediate alloy of many parts of known Zn, Si, Cu, Ni, Mn, Fe content as basic original pattern, use step 1) method make solution, and add Zn, Si, Cu, Ni, Mn, Fe standard solution of the 0.1mg/ml-5.0mg/ml concentration of suitable gradient, production standard curve solution;
3) say that typical curve solution measures on inductive coupling plasma emission spectrograph, respectively with the concentration of Zn, Si, Cu, Ni, Mn, the Fe in typical curve solution for horizontal ordinate, the intensity of emission spectra of Zn, Si, Cu, Ni, Mn, Fe in the typical curve solution of mensuration is ordinate drawing curve;
4) intensity of emission spectra of Zn, Si, Cu, Ni, Mn, Fe in test solution to be measured is measured with the condition determination same with step 3, and from described working curve, check in the concentration of Zn, Si, Cu, Ni, Mn, Fe in test solution to be measured, then calculate the content ω M of Zn, Si, Cu, Ni, Mn, Fe in sample to be tested according to following formula.
Further, described concentration of hydrochloric acid is 35 ~ 40%, and addition is that every gram of sample to be tested heavily adds 80 ~ 120ml.
Further, described hydrofluoric acid concentration is 20 ~ 25%, and addition is that every gram of sample to be tested heavily adds 30 ~ 60ml.
Further, described inductive coupling plasma emission spectrograph, its running parameter is: radio-frequency power 1400W, and assisted gas flow is 0.15L/min, and plasma flow is 14L/min, fog chamber pressure 0.5psi, pump speed 2.50r/min, multiplicity 5 times.
Beneficial effect of the present invention is: the present invention uses unique method, and use ICP plasma emission spectrometer, can in Simultaneously test Mg-Zn-Re intermediate alloy in the content of zinc (Zn), silicon (Si), copper (Cu), nickel (Ni), manganese (Mn) and iron (Fe), required reagent is few, save time, meet in time and produce.
Embodiment
Further describe technical scheme of the present invention below, but described in claimed scope is not limited to.
Embodiment one
The assay method of chemical element in a kind of Mg-Zn-Re intermediate alloy provided by the invention, comprises the following steps:
1) take sample to be tested 0.1gMg-Zn-Re intermediate alloy, slowly add after hydrochloric acid dissolves completely to sample in beaker, then add hydrofluorite, heating is boiled, and is diluted to 100ml after taking off cooling, makes night to be measured; Described concentration of hydrochloric acid is 35%, and addition is 8ml; Described hydrofluoric acid concentration is 25%, and addition is 6ml;
2) configuration standard curve solution, take the Mg-Zn-Re intermediate alloy of many parts of known Zn, Si, Cu, Ni, Mn, Fe content as basic original pattern, use step 1) method make solution, and add Zn, Si, Cu, Ni, Mn, Fe standard solution of the 0.1mg/ml-5.0mg/ml concentration of suitable gradient, production standard curve solution;
3) say that typical curve solution measures on inductive coupling plasma emission spectrograph, respectively with the concentration of Zn, Si, Cu, Ni, Mn, the Fe in typical curve solution for horizontal ordinate, the intensity of emission spectra of Zn, Si, Cu, Ni, Mn, Fe in the typical curve solution of mensuration is ordinate drawing curve;
Described inductive coupling plasma emission spectrograph, its running parameter is: radio-frequency power 1400W, and assisted gas flow is 0.15L/min, and plasma flow is 14L/min, fog chamber pressure 0.5psi, pump speed 2.50r/min, multiplicity 5 times
4) intensity of emission spectra of Zn, Si, Cu, Ni, Mn, Fe in test solution to be measured is measured with the condition determination same with step 3, and from described working curve, check in the concentration of Zn, Si, Cu, Ni, Mn, Fe in test solution to be measured, then calculate the content ω M of Zn, Si, Cu, Ni, Mn, Fe in sample to be tested according to following formula.
Embodiment three
The assay method of chemical element in a kind of Mg-Zn-Re intermediate alloy provided by the invention, comprises the following steps:
1) take sample to be tested 0.1gMg-Zn-Re intermediate alloy, slowly add after hydrochloric acid dissolves completely to sample in beaker, then add hydrofluorite, heating is boiled, and is diluted to 100ml after taking off cooling, makes night to be measured; Described concentration of hydrochloric acid is 38%, and addition is 12ml; Described hydrofluoric acid concentration is 23%, addition 5ml;
2) configuration standard curve solution, take the Mg-Zn-Re intermediate alloy of many parts of known Zn, Si, Cu, Ni, Mn, Fe content as basic original pattern, use step 1) method make solution, and add Zn, Si, Cu, Ni, Mn, Fe standard solution of the 0.1mg/ml-5.0mg/ml concentration of suitable gradient, production standard curve solution;
3) say that typical curve solution measures on inductive coupling plasma emission spectrograph, respectively with the concentration of Zn, Si, Cu, Ni, Mn, the Fe in typical curve solution for horizontal ordinate, the intensity of emission spectra of Zn, Si, Cu, Ni, Mn, Fe in the typical curve solution of mensuration is ordinate drawing curve;
Described inductive coupling plasma emission spectrograph, its running parameter is: radio-frequency power 1400W, and assisted gas flow is 0.15L/min, and plasma flow is 14L/min, fog chamber pressure 0.5psi, pump speed 2.50r/min, multiplicity 5 times
4) intensity of emission spectra of Zn, Si, Cu, Ni, Mn, Fe in test solution to be measured is measured with the condition determination same with step 3, and from described working curve, check in the concentration of Zn, Si, Cu, Ni, Mn, Fe in test solution to be measured, then calculate the content ω M of Zn, Si, Cu, Ni, Mn, Fe in sample to be tested according to following formula.
Claims (4)
1. the assay method of chemical element in Mg-Zn-Re intermediate alloy, is characterized in that: comprise the following steps:
1) take sample to be tested 0.1gMg-Zn-Re intermediate alloy, slowly add after hydrochloric acid dissolves completely to sample in beaker, then add hydrofluorite, heating is boiled, and is diluted to 100ml after taking off cooling, makes night to be measured;
2) configuration standard curve solution, take the Mg-Zn-Re intermediate alloy of many parts of known Zn, Si, Cu, Ni, Mn, Fe content as basic original pattern, use step 1) method make solution, and add Zn, Si, Cu, Ni, Mn, Fe standard solution of the 0.1mg/ml-5.0mg/ml concentration of suitable gradient, production standard curve solution;
3) say that typical curve solution measures on inductive coupling plasma emission spectrograph, respectively with the concentration of Zn, Si, Cu, Ni, Mn, the Fe in typical curve solution for horizontal ordinate, the intensity of emission spectra of Zn, Si, Cu, Ni, Mn, Fe in the typical curve solution of mensuration is ordinate drawing curve;
4) intensity of emission spectra of Zn, Si, Cu, Ni, Mn, Fe in test solution to be measured is measured with the condition determination same with step 3, and from described working curve, check in the concentration of Zn, Si, Cu, Ni, Mn, Fe in test solution to be measured, then calculate the content ω M of Zn, Si, Cu, Ni, Mn, Fe in sample to be tested according to following formula.
2. the assay method of chemical element in Mg-Zn-Re intermediate alloy as claimed in claim 1, it is characterized in that: described concentration of hydrochloric acid is 35 ~ 40%, addition is that every gram of sample to be tested heavily adds 80 ~ 120ml.
3. the assay method of chemical element in Mg-Zn-Re intermediate alloy as claimed in claim 1, it is characterized in that: described hydrofluoric acid concentration is 20 ~ 25%, addition is that every gram of sample to be tested heavily adds 30 ~ 60ml.
4. the assay method of chemical element in Mg-Zn-Re intermediate alloy as claimed in claim 1, it is characterized in that: described inductive coupling plasma emission spectrograph, its running parameter is: radio-frequency power 1400W, assisted gas flow is 0.15L/min, plasma flow is 14L/min, fog chamber pressure 0.5psi, pump speed 2.50r/min, multiplicity 5 times.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0579983A (en) * | 1991-09-20 | 1993-03-30 | Sumitomo Electric Ind Ltd | Analyzing method for rare earth element in glass |
| US7768639B1 (en) * | 2007-09-26 | 2010-08-03 | The United States Of America As Represented By The United States Department Of Energy | Methods for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry |
| CN102854047A (en) * | 2012-09-29 | 2013-01-02 | 清华大学 | Method for detecting content of heavy metal in sand casting powder |
| CN102914532A (en) * | 2012-10-12 | 2013-02-06 | 中国航空工业集团公司北京航空材料研究院 | Method for detecting contents of titanium, manganese, Ferrum, nickel and tungsten in tantalum contained cobalt-base alloy |
| CN102928364A (en) * | 2012-10-25 | 2013-02-13 | 中国地质科学院矿产综合利用研究所 | Method for measuring trace impurity elements of sodium, magnesium, calcium, iron and lead in high-purity boric acid |
| CN104502277A (en) * | 2014-12-15 | 2015-04-08 | 贵州安吉航空精密铸造有限责任公司 | Spectral analysis method |
-
2015
- 2015-12-23 CN CN201510981355.8A patent/CN105424681A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0579983A (en) * | 1991-09-20 | 1993-03-30 | Sumitomo Electric Ind Ltd | Analyzing method for rare earth element in glass |
| US7768639B1 (en) * | 2007-09-26 | 2010-08-03 | The United States Of America As Represented By The United States Department Of Energy | Methods for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry |
| CN102854047A (en) * | 2012-09-29 | 2013-01-02 | 清华大学 | Method for detecting content of heavy metal in sand casting powder |
| CN102914532A (en) * | 2012-10-12 | 2013-02-06 | 中国航空工业集团公司北京航空材料研究院 | Method for detecting contents of titanium, manganese, Ferrum, nickel and tungsten in tantalum contained cobalt-base alloy |
| CN102928364A (en) * | 2012-10-25 | 2013-02-13 | 中国地质科学院矿产综合利用研究所 | Method for measuring trace impurity elements of sodium, magnesium, calcium, iron and lead in high-purity boric acid |
| CN104502277A (en) * | 2014-12-15 | 2015-04-08 | 贵州安吉航空精密铸造有限责任公司 | Spectral analysis method |
Non-Patent Citations (1)
| Title |
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| 陶美娟 等: "电感耦合等离子体原子发射光谱法测定镁及镁合金中17种元素", 《理化检验（化学分册）》 * |
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