CN101750408A - Method for measuring contents of aluminum, calcium, barium, strontium, and phosphorus in silicon-calcium-barium alloy by ICP (inductively coupled plasma) - Google Patents
Method for measuring contents of aluminum, calcium, barium, strontium, and phosphorus in silicon-calcium-barium alloy by ICP (inductively coupled plasma) Download PDFInfo
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- CN101750408A CN101750408A CN200810229714A CN200810229714A CN101750408A CN 101750408 A CN101750408 A CN 101750408A CN 200810229714 A CN200810229714 A CN 200810229714A CN 200810229714 A CN200810229714 A CN 200810229714A CN 101750408 A CN101750408 A CN 101750408A
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Abstract
The invention relates to the technical field of ferrous metallurgical analysis, in particular to a method for measuring contents of aluminum, calcium, barium, strontium, and phosphorus in silicon-calcium-barium alloy by ICP (inductively coupled plasma). The method comprises the following steps of: dissolving a sample with nitric acid and hydrofluoric acid, fuming with sulfuric acid, diluting to a certain volume, and introducing an atomized solution into an inductive coupling plasma atomic emission spectrometer to measure the intensity of a spectral line to be measured; and solving the concentration of elements corresponding to substances to be measured based on the measured spectral line intensity of known concentration standard substances. The method has the advantages of no pollution and capability of analyzing and determining the content of the calcium, the barium, the aluminum, the phosphorus and the strontium in the silicon-calcium-barium alloy and meanwhile, separating the barium and the strontium which can not be separated by a chemical analytical method.
Description
Technical field
The present invention relates to a kind of technical field of ferrous metallurgical analysis, is the method that a kind of ICP measures aluminium, calcium, barium, strontium, phosphorus content in the calsibar alloy.
Background technology
Calsibar alloy is deoxidizer, the desulfurizing agent of steel-making, also has the effect of dephosphorization (BaP2, BaP3) concurrently, is the inovulant and the alterant of casting.In a large amount of aluminium-deoxidized molten steel, add calsibar alloy, can remove the alundum (Al snotter that exists in the steel, can improve the same tropism of steel, good processing characteristics and mechanical property are arranged.
Barium in the calsibar alloy reduces the vapour pressure of calcium effectively in the steel-making temperature range, increase the solubleness of calcium in molten steel, compare with calcium-silicon, add in the molten steel as the calcium source with calsibar alloy, even add a half of calcium amount calcium-silicon addition, the content of calcium but is about 2 times of calcium-silicon in the molten steel, and calcium stability also significantly improves in the molten steel.Because calcium has been protected in the existence of barium effectively in the alloy, reduce the volatilization oxidation of calcium, thereby reach the purpose that molten steel calcium is handled.Calsibar alloy can replace silicon barium, silico-calcium that molten steel is carried out deep deoxidation, can reduce cost effectively and improve the quality of products.
At present, the chemical analysis method of calcium barium aluminium phosphorus strontium element in the domestic existing calsibar alloy comprises: the barium amount in the YB/T109.2 barium sulphate gravimetric determination Si-Ba alloy; Aluminium amount in the YB/T109.3EDTA volumetric determination Si-Ba alloy; The YB/T109.5 molybdenum blue spectrophotometry is measured the phosphorus amount in the Si-Ba alloy; Calcium amount in the GB/T4700.2EDTA volumetric determination calcium-silicon.Wherein the barium amount in the barium sulphate gravimetric determination Si-Ba alloy is that barium adds the strontium resultant, because barium is close with the strontium chemical property, the two can't be separated with chemical method.The said method analytical cycle is long, complex operation, and consumes a large amount of chemicalss.
Summary of the invention
The purpose of this invention is to provide a kind of inductively coupled plasma atomic emission (being called for short the ICP method) and measure the method for calcium, barium, aluminium, phosphorus, strontium element content in the calsibar alloy, this methods analyst speed is fast, accuracy is high, once molten sample is measured multiple element simultaneously, and reduces the right environmental pollution of a lot of chemicalss.
The present invention is achieved through the following technical solutions:
ICP measures the method for aluminium, calcium, barium, strontium, phosphorus content in the calsibar alloy, it is characterized in that, this method is with sample nitric acid, hydrofluoric acid dissolution, sulfuric acid is fuming, be diluted to certain volume, atomized soln is introduced inductively coupled plasma atomic emission spectrometer, measure line strength of element to be measured; According to line strength that the concentration known standard substance records, obtain the concentration of test substance corresponding element.
Advantage of the present invention is:
1) fast, accurately: the once molten sample of ICP method can be measured the content of calsibar alloy aluminium, calcium, barium, strontium, phosphorus simultaneously, and traditional chemical analysis method can only be measured a kind of element by once molten sample.
2) energy-saving and environmental protection: adopt traditional chemical analysis method need add certain chemicals, the acidity of control solution, the kind of comparing chemicals with the ICP method is all relative with consumption more, and step is also loaded down with trivial details relatively.The ICP method only needs sample is processed into transparent solution, can measure its result.
3) solve difficult problems: barium and strontium all are the elements of second main group, and chemical property is very approaching, adopt gravimetric determination, can't analyze barium, strontium content separately.And the ICP method can be separated the two.
Embodiment
1. method summary
Sample nitric acid, hydrofluoric acid dissolution, sulfuric acid is fuming, and is diluted to certain volume, and atomized soln is introduced inductively coupled plasma atomic emission spectrometer, measures element spectral line intensity to be measured.According to line strength that the concentration known standard substance records, obtain the concentration of test substance corresponding element.
2 reagent
2.1 nitric acid: ρ 1.42g/ml
2.2 hydrofluorite: ρ 1.13g/ml
2.3 sulfuric acid: 1: 1 aqueous solution
2.4 nitric acid: 1: 1 aqueous solution
2.5 strontium mark liquid (100 μ g/ml): take by weighing 0.3043g strontium chloride (SrCl26H2O), place the 250mL beaker, after being dissolved in water, move in the people 1000mL volumetric flask, be diluted with water to scale, mixing.
2.6 aluminium mark liquid: (1mg/ml): take by weighing 1.0000g fine aluminium (＞99.9%) and place polytetrafluoroethylene beaker, add 40mL sodium hydroxide solution (10%), heating for dissolving in water-bath.Add water 100mL again, dripping hydrochloric acid (1+1) to solution is acid and excessive 10mL then, and cooling moves in the 1L volumetric flask, is diluted with water to scale, mixing.
2.7 phosphorus mark liquid (1mg/ml): take by weighing 4.3940g earlier through 105 ℃ of potassium dihydrogen phosphates of drying,, add 10mL nitric acid (4.1), move in the 1L volumetric flask, be diluted with water to scale, mixing with the suitable quantity of water dissolving to constant.
But stepwise dilution during use.
2.8 calcium mark liquid (1mg/ml): take by weighing 2.4972g at 105 ℃ of pure lime carbonate of top grade that dry by the fire to constant, place the 250mL beaker, add 20mL water, dripping hydrochloric acid (4.5) adds 10mL hydrochloric acid (4.5) again to dissolving fully then, boils and removes carbon dioxide, be cooled to room temperature, move in the 1L volumetric flask, be diluted with water to scale, mixing.
2.9 barium mark liquid: (1mg/ml): take by weighing 1.7787g barium chloride (BaCl22H2O), be dissolved in the water that boiled on a small quantity, the cooling back moves in the 1L volumetric flask, is diluted with water to scale, mixing.
3 key instruments
3.1 the IRIS Intrepid II of U.S. Thermo company type high resolving power, high sensitivity are composed the direct-reading inductive coupling plasma emission spectrograph entirely; TEVA software (version: 1.5.0).
3.2 instrument parameter: the radio-frequency generator operating power is 1150W, and the sample determination number of times is 3 times, flush time 30s, long wave 5s integral time, shortwave 20s integral time, peristaltic pump speed 130rpm, sample size 2.40ml/min.
3.3 the analysis of line wavelength of element to be measured is:
3.4 minimum short-term precision
Measure the absolute or relative light intensity 10 times of the denseest calibration curve solution of each element emission, calculate its standard deviation, relative standard deviation should be less than 0.9%.
3.5 the linearity of curve
The linearity of calibration curve checks that by calculating related coefficient related coefficient must be greater than 0.999.
4 analytical procedures
The 0.2000g sample is placed the 250ml polytetrafluoroethylene beaker, add 5ml nitric acid (2.1) and 5ml hydrofluorite (2.2), heating, after treating sample dissolution, add 10ml sulfuric acid (2.3), behind the sulfuric acid cigarette, take off cold slightly, add 5ml nitric acid (2.4), make the salt dissolving, the cooling back moves in the 100ml volumetric flask, is diluted to scale with water, shake up phosphorus to be measured, aluminium, content of strontium.
Draw above-mentioned test solution 10.00ml and place the 100ml volumetric flask, be diluted with water to scale, shake up, calcium to be measured, barium content.
The preparation of 5 standard solution
5.1 prepare 5 100ml volumetric flasks, press the standard solution that table 1 regulation adds analytical element, add coexistence elements by table 1 simultaneously and do matrix.
Table 1
5.2 prepare 5 100mL volumetric flasks, press the standard solution that table 2 regulation adds analytical element, add coexistence elements by table 2 simultaneously and do matrix.
Table 2
6, sample analysis
Table 3
Table 4
Table 5
Claims (1)
1.ICP the method for aluminium, calcium, barium, strontium, phosphorus content in the mensuration calsibar alloy, it is characterized in that, this method is with sample nitric acid, hydrofluoric acid dissolution, sulfuric acid is fuming, be diluted to certain volume, atomized soln is introduced inductively coupled plasma atomic emission spectrometer, measure line strength of element to be measured; According to line strength that the concentration known standard substance records, obtain the concentration of test substance corresponding element.
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| CN200810229714A CN101750408A (en) | 2008-12-15 | 2008-12-15 | Method for measuring contents of aluminum, calcium, barium, strontium, and phosphorus in silicon-calcium-barium alloy by ICP (inductively coupled plasma) |
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| CN200810229714A CN101750408A (en) | 2008-12-15 | 2008-12-15 | Method for measuring contents of aluminum, calcium, barium, strontium, and phosphorus in silicon-calcium-barium alloy by ICP (inductively coupled plasma) |
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| CN102128822A (en) * | 2010-12-21 | 2011-07-20 | 安徽六国化工股份有限公司 | Method for simultaneously determining contents of phosphorus, magnesium, iron and aluminum in phosphate ores by using ICP (inductively coupled plasma) method |
| CN102419325A (en) * | 2011-07-27 | 2012-04-18 | 中国科学院青海盐湖研究所 | Method for determining strontium calcium barium in strontium carbonate |
| CN102507538A (en) * | 2011-10-28 | 2012-06-20 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of lanthanum and cerium in rare earth silicon-calcium-barium |
| CN102507535A (en) * | 2011-10-28 | 2012-06-20 | 内蒙古包钢钢联股份有限公司 | Determination method of lanthanum and cerium content in rare earth silicon aluminum iron |
| CN102565027A (en) * | 2010-12-15 | 2012-07-11 | 鞍钢股份有限公司 | Method for measuring content of acid-soluble aluminum in ferroboron |
| CN102565176A (en) * | 2010-12-17 | 2012-07-11 | 鞍钢股份有限公司 | Method for simultaneously determining harmful elements in iron ore |
| CN102928400A (en) * | 2012-10-15 | 2013-02-13 | 深圳市谱尼测试科技有限公司 | Method for measuring content of heavy metal in polymer |
| CN103293144A (en) * | 2013-06-26 | 2013-09-11 | 天津虹炎科技有限公司 | ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) measurement of content of impurity phosphorus in steel |
| 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 |
| CN103852462A (en) * | 2012-12-05 | 2014-06-11 | 南京梅山冶金发展有限公司 | Detection method for simultaneously determining contents of calcium and phosphorus in calcium-silicon alloy |
| CN104048951A (en) * | 2014-07-04 | 2014-09-17 | 武钢集团昆明钢铁股份有限公司 | Method for measuring contents of silicon, calcium and aluminum in additives and co-solvents of permanent magnetic ferrites through ICP (Inductively Coupled Plasma) emission spectroscopy |
| CN104297226A (en) * | 2014-10-16 | 2015-01-21 | 宁夏共享集团有限责任公司 | Method for detecting content of aluminum and calcium in nodulizing agent by ICP-AES process |
| CN109030465A (en) * | 2018-08-17 | 2018-12-18 | 南京云开合金有限公司 | The detection method of the content of strontium, iron, barium, magnesium, calcium in a kind of zinc strontium alloy |
| CN113295676A (en) * | 2021-04-06 | 2021-08-24 | 包头钢铁（集团）有限责任公司 | Method for measuring calcium, aluminum and barium in deoxidizer |
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2008
- 2008-12-15 CN CN200810229714A patent/CN101750408A/en active Pending
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| CN102565027A (en) * | 2010-12-15 | 2012-07-11 | 鞍钢股份有限公司 | Method for measuring content of acid-soluble aluminum in ferroboron |
| CN102565176A (en) * | 2010-12-17 | 2012-07-11 | 鞍钢股份有限公司 | Method for simultaneously determining harmful elements in iron ore |
| CN102128822A (en) * | 2010-12-21 | 2011-07-20 | 安徽六国化工股份有限公司 | Method for simultaneously determining contents of phosphorus, magnesium, iron and aluminum in phosphate ores by using ICP (inductively coupled plasma) method |
| CN102128822B (en) * | 2010-12-21 | 2012-07-04 | 安徽六国化工股份有限公司 | Method for simultaneously determining contents of phosphorus, magnesium, iron and aluminum in phosphate ores by using ICP (inductively coupled plasma) method |
| CN102419325A (en) * | 2011-07-27 | 2012-04-18 | 中国科学院青海盐湖研究所 | Method for determining strontium calcium barium in strontium carbonate |
| CN102419325B (en) * | 2011-07-27 | 2013-07-03 | 中国科学院青海盐湖研究所 | Method for determining strontium calcium barium in strontium carbonate |
| CN102507538A (en) * | 2011-10-28 | 2012-06-20 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of lanthanum and cerium in rare earth silicon-calcium-barium |
| CN102507535A (en) * | 2011-10-28 | 2012-06-20 | 内蒙古包钢钢联股份有限公司 | Determination method of lanthanum and cerium content in rare earth silicon aluminum iron |
| CN102928400A (en) * | 2012-10-15 | 2013-02-13 | 深圳市谱尼测试科技有限公司 | Method for measuring content of heavy metal in polymer |
| CN103852462B (en) * | 2012-12-05 | 2016-09-28 | 南京梅山冶金发展有限公司 | The detection method of calcium phosphorus content in a kind of calcium-silicon of mensuration simultaneously |
| CN103852462A (en) * | 2012-12-05 | 2014-06-11 | 南京梅山冶金发展有限公司 | Detection method for simultaneously determining contents of calcium and phosphorus in calcium-silicon alloy |
| CN103293144A (en) * | 2013-06-26 | 2013-09-11 | 天津虹炎科技有限公司 | ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) measurement of content of impurity phosphorus in steel |
| 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 |
| 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 |
| CN104048951A (en) * | 2014-07-04 | 2014-09-17 | 武钢集团昆明钢铁股份有限公司 | Method for measuring contents of silicon, calcium and aluminum in additives and co-solvents of permanent magnetic ferrites through ICP (Inductively Coupled Plasma) emission spectroscopy |
| CN104048951B (en) * | 2014-07-04 | 2017-02-15 | 武钢集团昆明钢铁股份有限公司 | Method for measuring contents of silicon, calcium and aluminum in additives and co-solvents of permanent magnetic ferrites through ICP (Inductively Coupled Plasma) emission spectroscopy |
| CN104297226A (en) * | 2014-10-16 | 2015-01-21 | 宁夏共享集团有限责任公司 | Method for detecting content of aluminum and calcium in nodulizing agent by ICP-AES process |
| CN109030465A (en) * | 2018-08-17 | 2018-12-18 | 南京云开合金有限公司 | The detection method of the content of strontium, iron, barium, magnesium, calcium in a kind of zinc strontium alloy |
| CN109030465B (en) * | 2018-08-17 | 2021-06-11 | 南京云开合金有限公司 | Method for detecting content of strontium, iron, barium, magnesium and calcium in zinc-strontium alloy |
| CN113295676A (en) * | 2021-04-06 | 2021-08-24 | 包头钢铁（集团）有限责任公司 | Method for measuring calcium, aluminum and barium in deoxidizer |
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Open date: 20100623 |