CN105158234A - Method for measuring contents of lanthanum, cerium and yttrium elements in multi-component nodulizing agent by applying ICP-AES method - Google Patents
Method for measuring contents of lanthanum, cerium and yttrium elements in multi-component nodulizing agent by applying ICP-AES method Download PDFInfo
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Abstract
The invention belongs to the field of analysis of element content and relates to a method for contents of lanthanum, cerium and yttrium elements in a multi-component nodulizing agent by applying an ICP-AES method, which has the characteristics of accuracy, rapidness, convenient operation and the like, and is suitable for production and detection. The technical scheme provided by the invention has the beneficial effects that according to the method for the contents of lanthanum, cerium and yttrium elements in a multi-component nodulizing agent by applying the ICP-AES method, few technical flows are needed, the detection period is greatly shortened, and meanwhile, the detection blank is filled; the microelements in the nodulizing agent are measured by applying the ICP-AES method, the detection range is enlarged, and a new detection method is explored, thus providing analysis basis is provided for the problems such as product defects; the content ranges of the lanthanum, cerium and yttrium elements are measured to be 0.0001%-4.00% by applying the method, the analysis result is accurate, and the recovery rate is 97.2%-99.7%; due to the application of the ICP-AES method, the analysis result is accurate, the analysis requirements on the contents of lanthanum, cerium and yttrium can be met, and the casting quality can be guaranteed.
Description
Technical field
The invention belongs to constituent content analysis field, be specifically related to a kind of method that inductively coupled plasma atomic emission spectrometry method (ICP-AES) measures lanthanum in polycompound nodulizer, cerium and yttrium content.
Background technology
Nodularization, inoculated technology are the gordian techniquies that large-scale ductile iron part is produced, the features such as efficient multicomponent composite nodulizer has purifying molten iron, nodularization, anti-decaying spheroidisation, anti-graphite morphology ability is strong, chilling tendency is little, refinement matrix, the scope of application are wide.Wherein Ce, La and Y can promote graphite spheroidizing, graphite nodule generated or increases, and are effective nodularization elements.Therefore the mensuration of modulizer constituent content has vital effect to monitoring nodularization effect.
The mensuration of the essential element in modulizer 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 carry out single element mensuration, is 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 lanthanum, cerium and yttrium in ICP-AES method mensuration modulizer does not also have pertinent literature to report so far.
Summary of the invention
For the deficiency that prior art exists, the invention provides a kind of method that ICP-AES method measures lanthanum, cerium and yttrium content in polycompound nodulizer, application ICP-AES method measures lanthanum, cerium and yttrium content in polycompound nodulizer and has accurately, fast, the feature such as simple operation, be applicable to produce and detection.
For solving prior art Problems existing, the invention provides a kind of method that ICP-AES method measures lanthanum, cerium and yttrium content in polycompound nodulizer, the steps include:
Step one, takes 0.5000g sample, adds in beaker with water-wet, add 10mL nitric acid, drip 5-8mL hydrofluorite with plastic tube, after intense reaction stops, add 8mL perchloric acid, be heated to emit perchloric acid cigarette, rinse wall of cup with water, continuing heating smolders to surplus 2mL ~ 3mL solution, cooling a period of time, adds 25mL hydrochloric acid, heating for dissolving salt, is cooled to room temperature, is moved into by solution in the volumetric flask of 500mL, scale is diluted to, mixing with ultrapure water;
Step 2, configuration standard curve solution: take many parts with the high purity iron of sample to be tested Matrix Match as iron-based body original pattern, wherein, described iron-based body original pattern comprises identical matrix composition with sample to be tested, but the content that described iron-based body original pattern does not comprise lanthanum, cerium and yttrium or wherein lanthanum, cerium and yttrium is known, successively respectively to adding the lanthanum of the 0.2mg/ml-8.0mg/ml concentration of suitable gradient, cerium and yttrium standard solution in many parts of iron-based body original patterns, production standard curve solution;
Step 3, typical curve solution is measured on inductive coupling plasma emission spectrograph, respectively with the concentration of the lanthanum in typical curve solution, cerium and yttrium for horizontal ordinate, the intensity of emission spectra of lanthanum, cerium and yttrium in the typical curve solution measured is ordinate drawing curve, wherein, the analysis spectral line measuring the lanthanum selected is 398.852nm, and the analysis spectral line of cerium is 413.764nm, and the analysis spectral line of yttrium is 371.029nm;
Described inductive coupling plasma emission spectrograph, its running parameter is: radio-frequency power 1300W, and assisted gas flow is 0.2L/min, and plasma flow is 15L/min, fog chamber pressure 0.55psi, pump speed 1.50r/min, multiplicity 3 times;
Step 4, the intensity of emission spectra of lanthanum, cerium and yttrium 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 lanthanum, cerium and yttrium in test solution to be measured, then calculate the content ω of lanthanum, cerium and yttrium in sample to be tested according to following formula
m.
Wherein, represent the concentration of lanthanum, cerium and yttrium in test solution to be measured, unit is mcg/ml (μ g/mL); V represents the volume of test solution to be measured, and unit is milliliter (mL); M represents the quality of sample to be tested, and unit is gram (g).
The beneficial effect of technical scheme of the present invention is: the detection method sample pretreating process that the present invention's application ICP-AES method measures lanthanum, cerium and yttrium content in modulizer is simple, and flow process is few, and sense cycle significantly shortens, and fills up simultaneously and detects blank; Application ICP-AES method, for the mensuration of modulizer medium trace element, has been expanded detection faces, has been opened up new detection method, for some problems such as product defects provide analysis foundation; The scope that application this method measures lanthanum, cerium and yttrium content is 0.0001% ~ 4.00%, its analysis result is accurate, and the recovery is at 97.2%-99.7%, and application ICP-AES method analysis result is accurate, lanthanum in modulizer, cerium and yttrium can be met containing quantitative analysis requirement, ensure casting quality.
Embodiment
In order to make those skilled in the art better understand technical scheme of the present invention, in conjunction with reality, the present invention is described in further detail.
A kind of ICP-AES method of the present invention measures the method for lanthanum, cerium and yttrium content in polycompound nodulizer, comprises the following steps:
Step one, take 0.5000g sample in 200mL polytetrafluoroethylene beaker, use a small amount of water-wet, add 10mL nitric acid, carefully drip 5-8mL hydrofluorite with plastic tube, stop to intense reaction, add 8mL perchloric acid, low-temperature heat, to emitting perchloric acid cigarette, rinses wall of cup with water, continues low-temperature heat and smolders to surplus 2mL ~ 3mL solution.Slightly cold, add 25mL hydrochloric acid (1:3), heating for dissolving salt, is cooled to room temperature.Test solution is moved in 500mL volumetric flask, be diluted to scale with ultrapure water, mixing.
Step 2, configuration standard curve solution: take many parts with the high purity iron of sample to be tested Matrix Match as iron-based body original pattern, wherein, described iron-based body original pattern comprises identical matrix composition with sample to be tested, but the content that described iron-based body original pattern does not comprise lanthanum, cerium and yttrium or wherein lanthanum, cerium and yttrium is known, successively respectively to adding the lanthanum of the 0.2mg/ml-8.0mg/ml concentration of suitable gradient, cerium and yttrium standard solution in many parts of iron-based body original patterns, production standard curve.
Step 3, typical curve solution is measured on inductive coupling plasma emission spectrograph, respectively with the concentration of the lanthanum in typical curve solution, cerium and yttrium for horizontal ordinate, the intensity of emission spectra of lanthanum, cerium and yttrium in the typical curve solution measured is ordinate drawing curve, wherein, the analysis spectral line measuring the lanthanum selected is 398.852nm, and the analysis spectral line of cerium is 413.764nm, and the analysis spectral line of yttrium is 371.029nm.
Described inductive coupling plasma emission spectrograph, its running parameter is: radio-frequency power 1300W, and assisted gas flow is 0.2L/min, and plasma flow is 15L/min, fog chamber pressure 0.55psi, pump speed 1.50r/min, multiplicity 3 times.
Step 4, measures test solution to be measured with the condition determination that step 3 is same, checks in the concentration of lanthanum, cerium and yttrium in test solution to be measured from described working curve, then calculates the content ω of lanthanum, cerium and yttrium in sample to be tested according to following formula
m.
Wherein, represent the concentration of lanthanum, cerium and yttrium in test solution to be measured, unit is mcg/ml (μ g/mL); V represents the volume of test solution to be measured, and unit is milliliter (mL); M represents the quality of sample to be tested, and unit is gram (g).
The detection method sample pretreating process that the present invention's application ICP-AES method measures lanthanum, cerium and yttrium content in modulizer is simple, and flow process is few, and sense cycle significantly shortens, and fills up simultaneously and detects blank; Application ICP-AES method, for the mensuration of modulizer medium trace element, has been expanded detection faces, has been opened up new detection method, for some problems such as product defects provide analysis foundation; The scope that application this method measures lanthanum, cerium and yttrium content is 0.0001% ~ 4.00%, its analysis result is accurate, and the recovery is at 97.2%-99.7%, and application ICP-AES method analysis result is accurate, lanthanum in modulizer, cerium and yttrium can be met containing quantitative analysis requirement, ensure casting quality.
Be described in detail the technical scheme that the application provides above, apply embodiment herein and set forth the principle of the application and embodiment, the explanation of above embodiment is just for helping method and the core concept thereof of understanding the application; Meanwhile, for one of ordinary skill in the art, according to the thought of the application, all will change in specific embodiments and applications, in sum, this description should not be construed as the restriction to the application.
Claims (2)
1. ICP-AES method measures a method for lanthanum, cerium and yttrium content in polycompound nodulizer, the steps include:
Step one, takes 0.5000g sample, adds in beaker with water-wet, add 10mL nitric acid, drip 5-8mL hydrofluorite with plastic tube, after intense reaction stops, add 8mL perchloric acid, be heated to emit perchloric acid cigarette, rinse wall of cup with water, continuing heating smolders to surplus 2mL ~ 3mL solution, cooling a period of time, adds 25mL hydrochloric acid, heating for dissolving salt, is cooled to room temperature, is moved into by solution in the volumetric flask of 500mL, scale is diluted to, mixing with ultrapure water;
Step 2, configuration standard curve solution: take many parts with the high purity iron of sample to be tested Matrix Match as iron-based body original pattern, wherein, described iron-based body original pattern comprises identical matrix composition with sample to be tested, but the content that described iron-based body original pattern does not comprise lanthanum, cerium and yttrium or wherein lanthanum, cerium and yttrium is known, successively respectively to adding the lanthanum of the 0.2mg/ml-8.0mg/ml concentration of suitable gradient, cerium and yttrium standard solution in many parts of iron-based body original patterns, production standard curve solution;
Step 3, typical curve solution is measured on inductive coupling plasma emission spectrograph, respectively with the concentration of the lanthanum in typical curve solution, cerium and yttrium for horizontal ordinate, the intensity of emission spectra of lanthanum, cerium and yttrium in the typical curve solution measured is ordinate drawing curve, wherein, the analysis spectral line measuring the lanthanum selected is 398.852nm, and the analysis spectral line of cerium is 413.764nm, and the analysis spectral line of yttrium is 371.029nm;
Step 4, the intensity of emission spectra of lanthanum, cerium and yttrium 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 lanthanum, cerium and yttrium in test solution to be measured, then calculate the content ω of lanthanum, cerium and yttrium in sample to be tested according to following formula
m;
Wherein, represent the concentration of lanthanum, cerium and yttrium in test solution to be measured, unit is mcg/ml (μ g/mL); V represents the volume of test solution to be measured, and unit is milliliter (mL); M represents the quality of sample to be tested, and unit is gram (g).
2. a kind of ICP-AES method according to claim 1 measures the method for lanthanum, cerium and yttrium content in polycompound nodulizer, it is characterized in that: described inductive coupling plasma emission spectrograph, its running parameter is: radio-frequency power 1300W, assisted gas flow is 0.2L/min, plasma flow is 15L/min, fog chamber pressure 0.55psi, pump speed 1.50r/min, multiplicity 3 times.
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| CN108613970A (en) * | 2018-05-08 | 2018-10-02 | 中国航发北京航空材料研究院 | A kind of method of rhenium element in measurement Rare-earth Elements Treated Nodular Iron |
| CN108709882A (en) * | 2018-08-14 | 2018-10-26 | 武汉钢铁有限公司 | Measure the method for element silicon and phosphorus element content in low-silicon nodulizer |
| CN109557081A (en) * | 2018-10-19 | 2019-04-02 | 大冶特殊钢股份有限公司 | The detection method of yttrium in a kind of nickel-base alloy |
| CN112033951A (en) * | 2020-08-20 | 2020-12-04 | 中航金属材料理化检测科技有限公司 | Method for determining cerium content in iron-based sample based on ICP-AES method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108613970A (en) * | 2018-05-08 | 2018-10-02 | 中国航发北京航空材料研究院 | A kind of method of rhenium element in measurement Rare-earth Elements Treated Nodular Iron |
| CN108709882A (en) * | 2018-08-14 | 2018-10-26 | 武汉钢铁有限公司 | Measure the method for element silicon and phosphorus element content in low-silicon nodulizer |
| CN109557081A (en) * | 2018-10-19 | 2019-04-02 | 大冶特殊钢股份有限公司 | The detection method of yttrium in a kind of nickel-base alloy |
| CN112033951A (en) * | 2020-08-20 | 2020-12-04 | 中航金属材料理化检测科技有限公司 | Method for determining cerium content in iron-based sample based on ICP-AES method |
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