CN102200500A - Pretreatment method for inductively coupled plasma-atomic emission spectrometry (ICP-AES) test of content of elements in quaternary alloy - Google Patents
Pretreatment method for inductively coupled plasma-atomic emission spectrometry (ICP-AES) test of content of elements in quaternary alloy Download PDFInfo
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- CN102200500A CN102200500A CN2010101317701A CN201010131770A CN102200500A CN 102200500 A CN102200500 A CN 102200500A CN 2010101317701 A CN2010101317701 A CN 2010101317701A CN 201010131770 A CN201010131770 A CN 201010131770A CN 102200500 A CN102200500 A CN 102200500A
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Abstract
The invention relates to a test of the content of elements in a quaternary alloy, in particular to an inductively coupled plasma-atomic emission spectrometry (ICP-AES) test method for the content of the elements in the quaternary alloy. In the method, by a NaOH-SVC-H2O2-HCl-SVC-H2O2 dissolving method, the quaternary alloy can be dissolved totally; and the dissolving method is combined with the ICP-AES, so conditions for testing eight elements of Si, Fe, Pb, Cd, Ti, Mg, Cu and Sn at the same time are provided.
Description
Technical field
The constituent content that the present invention relates to quaternary alloy is measured, and relates in particular to a kind of quaternary alloy constituent content ICP-AES assay method.
Background technology
Development product in 1964, it had the advantage of galvanizing by dipping and two kinds of products of hot-dip aluminizing to galvanizing by dipping aluminium alloy layer steel plate (being called for short GL), is successfully applied to a plurality of fields such as automobile, electrical equipment, building by U.S. Bethlehem Steel Company.According to this u s company's patent report: aluminium is 55% (± 2%) in the GL alloy layer, and zinc is 43.5% (± 0.5～1.0%), when silicon is 1.5% (± 0.5%), and this product reaches best Corrosion Protection and usability.
The high zinc high alumina of the high silicon rare earth quaternary alloy ingot sample that the present invention relates to, be in conjunction with actual raw material metal on the theoretical foundation of domestic and international first generation aluminium-zinc-silicon ternary alloy three-partalloy and second generation aluminium-zinc-silicon-rare earth quaternary alloy, be different from the quaternary alloy ingot of latest generation both domestic and external, multiple characteristics such as collection intensity, corrosion resistance, high-temperature oxidation, heat insulation, japanning property.Therefore, grasp and strict each the main amount composition of quaternary alloy ingot of this latest generation and the composition content of doping composition controlled well, will become very important, this is directly connected to the quality and the lumber recovery of this product.
Mainly contain Si, Fe, Pb, Cd, Ti, Mg, eight kinds of elements of Cu, Sn in the quaternary alloy, measuring the component total amount of rare earth can be referring to the national standard of existing chemical analysis, measuring other elementary composition also can be referring to the national standard of existing GDS photoelectric direct reading spectrometry method, but do not have so far both at home and abroad simultaneous determination of multiponents in the high zinc high alumina of the corresponding high silicon rare earth quaternary alloy ingot ICP-AES forensic chemistry analytic approach enclose tame standard.
Eight key components, at present can referring to method gravimetric method, spectrophotometric method, ICP-AES method and atomic absorption spectrography (AAS) etc. are arranged, these methods are used for the part compound mensuration of binary kirsite, binary aluminium alloy and ternary allumen mostly.These binary or ternary alloy three-partalloy ingot and alloy-layer product thereof relate to the complicacy of multi-component coexistence effect in the alloy and whole two importances of integrality of dissolving of soluble component of Chemical Pretreatment method all very importantly, and simultaneous determination of multiponents comprises that the chemical analysis method that complete process for chemically pretreating reaches does not have complete report at home and abroad, the quaternary alloy ingot of especially high silicon, rare earth, high zinc, high aluminium component and alloy-layer new product thereof so far in the quaternary alloy of relevant latest generation.
Summary of the invention
The present invention is intended to address the above problem, the preprocess method that provides a kind of quaternary alloy constituent content ICP-AES to measure.Method of the present invention can directly thoroughly be dissolved various elements, satisfies the needs that ICP-AES measures.
The present invention is achieved in that
Method of the present invention makes the ICP-AES method measure eight key components such as silicon in the high silicon rare earth of the high zinc of the high alumina quaternary alloy ingot and iron simultaneously becomes possibility, satisfied the analytical test requirement of the doping component of Ferrous Metallurgy alloy industry latest generation high added value alloy product, have fast, stable, accurately, multiple characteristics such as advanced person.Method of the present invention can be used for the complete dissolving of polycomponent of polynary or high first superalloy ingot sample simultaneously, needs according to determination object, but also coupling hydride generator (HG-ICP-AES) or other exact instrument, thereby this law can play important popularizing action.
Embodiment
The present invention is further illustrated below in conjunction with embodiment:
The preprocess method that a kind of quaternary alloy constituent content ICP-AES measures, described mensuration alloy contains Si, Fe, Pb, Cd, Ti, Mg, eight kinds of elements of Cu, Sn, and it is characterized in that: the preprocess method of described alloy comprises:
The weighing step: accurately take by weighing the described quaternary alloy sample of 1.0000 grams in polytetrafluoroethylene beaker,
The molten step of alkali: add 10ml concentration and be 20% NaOH liquid, heating for dissolving on electric furnace, intense reaction is treated the quaternary alloy sample dissolution to small size, granule, residue shape, when emitting vesicle, adds 5ml concentration and be 30% H
2O
2Hydrotropy;
The molten step of acid: beaker is taken off, and it is the HCl solution acidifying of 6mol/L that cold slightly back adds 20mL concentration, during to small size, drips 1ml concentration again and be 30% H
2O
2Hydrotropy, up to all dissolvings of granule, snotter and residue, this solution is the faint yellow of clarification; Wash simultaneously around clear beaker inwall and surface plate, continue heating;
The standard solution configuration step: after treating that the whole dissolvings of salt are finished, take off, cooling in the 100mL volumetric flask, is diluted with water to scale, shakes up, and it is stand-by to do overanxious carbon elimination.
The precision test
Under the same measured condition, take by weighing half 0.5000 gram of original sample amount, still press sample analysis method, in the low concentration district the carrying out of eight components such as quaternary alloy ingot sample Si and Fe measured simultaneously, the precision of having investigated to high requirement this law is (because of matrix reduces by half, analysis result can be similar to thinks the measured value of being a bit larger tham 2 times), its test findings sees Table 1.
Table 1 precision test (n=10)
By the test of above-mentioned precision, each coefficient of variation of measuring eight components in the actual sample for 10 times simultaneously drops on below 0.90% continuously, all meets the precision coefficient of variation of allowing less than 5%, so this law has higher repeatability, satisfies actual requirement.
Accuracy test
Standard reagent is made
Because the high zinc high alumina of the high silicon rare earth quaternary alloy ingot sample that this paper discusses, be on the basis of first generation aluminium zinc-silicon ternary alloy three-partalloy of inventing abroad of China, carry out the quaternary alloy ingot that is different from latest generation both domestic and external of independent research on the basis in conjunction with second generation aluminium-zinc-silicon rare earth quaternary alloy, therefore, this paper is based on this alloy pig component, carry out the synchronous matrix coupling of main content zinc-aluminium, make the serial hybrid standard reagent of approximate sample percentage concentration scope, measured the series standard reagent of the internal control of eight components as this law.
Under the same measured condition, we get a above-mentioned standard reagent, and (Mg 0.004%, Si0.60%, Ti0.004%, Fe 0.40%, Cu 0.004%, Cd 0.004%, and Sn 0.004%, and Pb 0.004%), eight components such as its Si and Fe are carried out the accuracy test of measuring simultaneously, the results are shown in Table 2
The standard model accuracy test (n=10) of table 2 concentration known
Accuracy test by above-mentioned standard model, the coefficient of variation of the mean value of each component of bioassay standard sample drops on the scope less than 1.33% simultaneously, all less than the interval range of the coefficient of variation 5% of allowing, the full dose recovery of standard model is 95.80%～101.78% simultaneously, absolute error is in 5%, the result shows that this law has higher accuracy, and the result is satisfactory.
The recovery of standard addition test of sample
Under the same measured condition, we carry out the accuracy test of recovery of standard addition at part quaternary alloy ingot sample of peeking, and the results are shown in Table 3
Accuracy test by above-mentioned recovery of standard addition, the actual recovery of measuring eight components such as Si and Fe in the quaternary alloy ingot simultaneously drops between 94.29%～105.26%, all greater than the requirement of allowing of 90% instrumental method, so this law has higher repeatability, reliable results.
The recovery of standard addition accuracy test (n=10) of table 3 sample
The contrast test of the present invention and national standard Law GDS photoelectric direct reading spectrometry method that can reference
Under this paper condition determination, our part quaternary alloy ingot sample of peeking, measure eight components such as Si and Fe simultaneously and carried out contrast test with national standard Law GDS photoelectric direct reading spectrometry method (old law) that can reference, the result sees Table 4 respectively and earlier checks the variance of judging between two methods that there was no significant difference is arranged with F then, the results are shown in Table 5 variance there was no significant differences between two methods then, also be under the situation of precision unanimity, carry out again between two kinds of methods or two groups of separate test figures between the rank test method of system error-free is arranged, the results are shown in Table 6.
Table 4 is measured two methods of eight components such as Si and Fe in the quaternary alloy ingot sample simultaneously to have a competition (n=2 * 6)
F method of inspection in the table 5 mensuration quaternary alloy ingot sample between two variances of eight components such as Si and Fe
(á＝0.05，n
1＝n
2＝6，df
1＝df
2＝n-1＝5)
The result shows, the variance there was no significant difference between two methods of this law and old law also is that precision is consistent.
There is the sum of ranks of system error-free to examine between two kinds of methods of table 6 or two groups of separate test figures
(á＝0.05)
At this moment, n
1=8, n
2=8, n=16.If national standard Law (old law) system error-free that can reference, then R
1=2+3+6+8+9+11+14+16=69 for á=0.05, looks into the sum of ranks tables of critical values, gets T
1=52, T
2=84, T is arranged
1＜R
1＜T
2So there is not significant difference in two groups of data, promptly there is not systematic error in this law for old law, i.e. the accuracy of two methods is consistent, and eight component reliable results such as Si and Fe are satisfactory in the quaternary alloy ingot sample of mensuration.
Claims (2)
1. the preprocess method measured of a quaternary alloy constituent content ICP-AES, described mensuration alloy contains Si, Fe, Pb, Cd, Ti, Mg, eight kinds of elements of Cu, Sn, and it is characterized in that: the preprocess method of described alloy comprises:
The weighing step: accurately take by weighing the described quaternary alloy sample of 1.0000 grams in polytetrafluoroethylene beaker,
The molten step of alkali: add 10ml concentration and be 20% NaOH solution, heating for dissolving on electric furnace, intense reaction is treated the quaternary alloy sample dissolution to small size, granule, residue shape, when emitting vesicle, adds 5ml concentration and be 30% H
2O
2Hydrotropy;
The molten step of acid: beaker is taken off, and it is the HCl solution acidifying of 6mol/L that cold slightly back adds 20mL concentration, during to small size, drips 1ml concentration again and be 30% H
2O
2Hydrotropy, up to all dissolvings of granule, snotter and residue, this solution is the faint yellow of clarification; Wash simultaneously around clear beaker inwall and surface plate, continue heating;
The standard solution preparation steps: after treating that the whole dissolvings of salt are finished, take off, cooling in the 100mL volumetric flask, is diluted with water to scale, shakes up, and it is stand-by to do overanxious carbon elimination.
2. the preprocess method that quaternary alloy constituent content ICP-AES according to claim 1 measures is characterized in that in molten step of described alkali and the sour molten step, described small size is meant that liquor capacity is not more than 5ml.
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Cited By (6)
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| CN103543141A (en) * | 2013-09-25 | 2014-01-29 | 中国科学院上海光学精密机械研究所 | Analytical method of trace impurity elements Fe and Cu in tin oxide electrode |
| CN103592197A (en) * | 2013-11-07 | 2014-02-19 | 铜陵有色金属集团股份有限公司 | Method for analyzing selenium content in crude selenium |
| CN105628684A (en) * | 2015-12-30 | 2016-06-01 | 河南省有色金属地质勘查总院 | Method for measuring high-content lead in lead-zinc ore by utilization of ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) method |
| CN106644643A (en) * | 2016-12-30 | 2017-05-10 | 广西玉柴机器股份有限公司 | Sample preparation method for ICP spectral analysis on tin aluminum alloy layer of engine bearing bush with double layers of materials |
| CN107643280A (en) * | 2016-07-22 | 2018-01-30 | 天津市茂联科技有限公司 | The quick determination method of trace germanium in a kind of copper, cobalt and iron alloy |
| CN110146491A (en) * | 2019-06-14 | 2019-08-20 | 山西八达镁业有限公司 | A method of verifying alloying component testing result accuracy |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103543141A (en) * | 2013-09-25 | 2014-01-29 | 中国科学院上海光学精密机械研究所 | Analytical method of trace impurity elements Fe and Cu in tin oxide electrode |
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| CN103592197A (en) * | 2013-11-07 | 2014-02-19 | 铜陵有色金属集团股份有限公司 | Method for analyzing selenium content in crude selenium |
| CN105628684A (en) * | 2015-12-30 | 2016-06-01 | 河南省有色金属地质勘查总院 | Method for measuring high-content lead in lead-zinc ore by utilization of ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) method |
| CN107643280A (en) * | 2016-07-22 | 2018-01-30 | 天津市茂联科技有限公司 | The quick determination method of trace germanium in a kind of copper, cobalt and iron alloy |
| CN106644643A (en) * | 2016-12-30 | 2017-05-10 | 广西玉柴机器股份有限公司 | Sample preparation method for ICP spectral analysis on tin aluminum alloy layer of engine bearing bush with double layers of materials |
| CN110146491A (en) * | 2019-06-14 | 2019-08-20 | 山西八达镁业有限公司 | A method of verifying alloying component testing result accuracy |
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Application publication date: 20110928 |