CN103852462A - Detection method for simultaneously determining contents of calcium and phosphorus in calcium-silicon alloy - Google Patents
Detection method for simultaneously determining contents of calcium and phosphorus in calcium-silicon alloy Download PDFInfo
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- CN103852462A CN103852462A CN201210515282.XA CN201210515282A CN103852462A CN 103852462 A CN103852462 A CN 103852462A CN 201210515282 A CN201210515282 A CN 201210515282A CN 103852462 A CN103852462 A CN 103852462A
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Abstract
The invention discloses a detection method for simultaneously determining contents of calcium and phosphorus in calcium-silicon alloy. The detection method comprises the steps of by sampling the prepared to-be-determined solution and prepared standard test solution, determining the standard test solution through inductively coupled plasma emission spectrum to establish a calcium and phosphorus working curve, then determining the to-be-determined solution and finding the contents of calcium and phosphorus in the to-be-determined solution, thus realizing the determination on the contents of calcium and phosphorus in calcium-silicon alloy. The detection method can realize simultaneous determination on contents of calcium and phosphorus in calcium-silicon alloy, is simple and convenient to operate, low in labor intensity, high in detection automation degree, short in detection period, high in detection accuracy, and has the advantages of low detection cost and small environment pollution.
Description
Technical field
The present invention relates to a kind of constituent content analysis method in analytical chemistry field, particularly a kind of detection method of simultaneously measuring calcium phosphorus content in calcium-silicon.
Background technology
Calcium and silicon and oxygen have strong affinity.Particularly calcium, not only has very strong affinity with oxygen, and has very strong affinity with sulphur, nitrogen, so calcium-silicon is a kind of comparatively ideal double deoxidizer, desulfurizing agent.Calcium-silicon not only deoxidizing capacity is strong, and deoxidation products is easy to floating, is easy to discharge, and can also improves the performance of steel, improves plasticity, the toughness of steel.At present, calcium-silicon is applied in high-quality steel, special steel and specific alloy production.The specific alloys such as steel grade and nickel-base alloy, titanium-base alloy such as such as rail steel, mild carbon steel, stainless steel, all available calcium-silicon is made deoxidizer, desulfurizing agent, denitrifier and alloying constituent.Calcium-silicon is also applicable to being used as the heating agent in pneumatic steelmaking workshop, also can be used as the inovulant of cast iron and the spheroidal-graphite cast iron adjuvant in producing, and makes in iron Graphite Distribution even, reduces chilling tendency, and can increase silicon, desulfurization, improves improving cast iron quality.Calcium-silicon is one of starting material that smelting industry is conventional, and the quality of calcium-silicon can directly affect the quality of smelting molten steel.Therefore, the Accurate Determining of its silico-calcium elemental composition can, for formulating in smelting process reasonably proportioning, be to reduce waste product to occur, and valid data foundation is provided for improving the quality of products etc.Calcium-silicon is one of deoxidation the most frequently used while smelting high-quality steel and special steel alloy and desulfurizing agent, is that continuous casting steel is particularly processed alloy containing aluminum steel continuous casting for preventing the calcium that casting nozzle dross (cover eye) must be used.In steelmaking process, Xiang Gangzhong adds the condition that can change residual snotter in steel after calcium-silicon, reduces the content of steel inclusion, improves the mechanical property of steel, and it is the cleanser of high purity steel production use.Most important two indexs of calcium-silicon are exactly calcium and phosphorus content, deoxidation in calcium content height direct steelmaking process, desulfurized effect, and phosphorus content likely enters molten steel in adition process, reduces steel quality.Therefore it is very necessary measuring calcium and phosphorus content in calcium-silicon.Patent " determination method of silico-calcium constituent content in calcium-silicon " is although CN201110085892.6 has announced the assay method of silicon and calcium in calcium-silicon, but this patent adopts the molten high-temperature melting method of alkali to decompose sample, this disposal route is decomposed sample and is related to a large amount of chemical reagent, complex operation, after processing, in sample solution, salts substances content is higher simultaneously, be not suitable for Minor element and detect (for example phosphorus), then adopt traditional chemical analysis method to measure the content of silicon and calcium in calcium-silicon, this measuring method operation is also very complicated, detection speed is slow, be difficult to meet modern enterprise production requirement.
Summary of the invention
For addressing the above problem, the invention discloses a kind of detection method of simultaneously measuring calcium phosphorus content in calcium-silicon, have simple to operately, determination efficiency is high, and sense cycle is short, when having realized calcium phosphorus content, measure, effectively reduce the laboratory detection efficiency of product, thereby can meet the requirement of the High-efficient Production of modern enterprise, there is chemical reagent consumption amount little simultaneously, testing cost is low, pollutes low environment close friend.
The related solution density of the detection method of simultaneously measuring calcium phosphorus content in calcium-silicon disclosed by the invention is all at the status of criterion (STP:273K or 298K, 1 standard atmospheric pressure QNE) lower mensuration, comprise the steps: one, solution to be measured preparation, take 0.2000g sample and be placed in 50mL counteracting tank, then add 10mL nitric acid (1.40g/mL) and 5mL hydrofluorite (1.14g/mL) in counteracting tank; Counteracting tank is put into Hyperfrequency waves eliminating stove, and 25 ℃ of digestion conditions, clear up pressure 2.0MPa, digestion time 10min; Clear up complete being cooled to after room temperature, solution is transferred to 150mL polytetrafluoroethylene beaker from counteracting tank, and after adding 5mL perchloric acid (1.67g/mL) to stir evenly to be fuming, be cooled to room temperature, add again 20mL deionized water, then be diluted to 100mL with deionized water with 100mL volumetric flask and make solution to be measured; Two, standard solution preparation, a, takes 0.1000g iron and is placed in 50mL counteracting tank, then adds 10mL nitric acid (1.40g/mL) and 5mL hydrofluorite (1.14g/mL) in counteracting tank; B, counteracting tank is put into Hyperfrequency waves eliminating stove, 25 ℃ of digestion conditions, clear up pressure 2.0MPa, digestion time 10min; C, clear up complete being cooled to after room temperature, solution is transferred to 150mL polytetrafluoroethylene beaker from counteracting tank, and after adding 5mL perchloric acid (1.67g/mL) to stir evenly to be fuming, is cooled to room temperature, add again 20mL deionized water, then be diluted to 100mL with 100mL volumetric flask and make solution to be measured; Get respectively again 6 parts of 10mL solution and be placed in 6 100mL volumetric flasks, in volumetric flask, respectively add respectively again calcium standard solution (the 1000mg/L of 0.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL, with Ca metering) and phosphorus standard solution (10mg/L, with P metering), and be diluted to scale mark with deionized water; Three, assay, utilizes the concentration data of calcium in the standard sample that inductively coupled plasma emission spectrometer records or phosphorus, and makes working curve, then liquid to be measured is measured, and on working curve, search the content that obtains each calcium in sample and phosphorus, i.e. m
1calculate calcium in sample and the content of phosphorus according to formula (1),
in formula (1): W
ca, P(%): represent calcium or phosphorus content in sample, represent with massfraction; m
1: sample is searched the mass number obtaining from working curve, the mg of unit; m
0: sample sample weighting amount, the g of unit.
The detection method of simultaneously measuring calcium phosphorus content in calcium-silicon disclosed by the invention, have simple to operate, determination efficiency is high, sense cycle is short, when having realized calcium phosphorus content, measure, effectively reduce the laboratory detection efficiency of product, thereby can meet the requirement of the High-efficient Production of modern enterprise, there is chemical reagent consumption amount little simultaneously, pollute low, operation detection safety, testing cost is low, pollution low environment close friend, guarantee fully the quality of calcium-silicon, be conducive to improve the production efficiency of iron and steel enterprise, reduce production costs, guarantee the quality of product.
Embodiment
Below in conjunction with embodiment, further illustrate the present invention, should understand following embodiment and only be not used in and limit the scope of the invention for the present invention is described.
The related solution density of the detection method of simultaneously measuring calcium phosphorus content in calcium-silicon disclosed by the invention is all at the status of criterion (STP:273K or 298K, 1 standard atmospheric pressure QNE) lower mensuration, comprise the steps: one, solution to be measured preparation, take 0.2000g sample and be placed in 50mL counteracting tank, then add 10mL nitric acid (1.40g/mL) and 5mL hydrofluorite (1.14g/mL) in counteracting tank; Counteracting tank is put into Hyperfrequency waves eliminating stove, and 25 ℃ of digestion conditions, clear up pressure 2.0MPa, digestion time 10min; Clear up complete being cooled to after room temperature, solution is transferred to 150mL polytetrafluoroethylene beaker from counteracting tank, and after adding 5mL perchloric acid (1.67g/mL) to stir evenly to be fuming, be cooled to room temperature, add again 20mL deionized water, then be diluted to 100mL with deionized water with 100mL volumetric flask and make solution to be measured; Two, standard solution preparation, a, takes 0.1000g iron and is placed in 50mL counteracting tank, then adds 10mL nitric acid (1.40g/mL) and 5mL hydrofluorite (1.14g/mL) in counteracting tank; B, counteracting tank is put into Hyperfrequency waves eliminating stove, 25 ℃ of digestion conditions, clear up pressure 2.0MPa, digestion time 10min; C, clear up complete being cooled to after room temperature, solution is transferred to 150mL polytetrafluoroethylene beaker from counteracting tank, and after adding 5mL perchloric acid (1.67g/mL) to stir evenly to be fuming, is cooled to room temperature, add again 20mL deionized water, then be diluted to 100mL with 100mL volumetric flask and make solution to be measured; Get respectively again 6 parts of 10mL solution and be placed in 6 100mL volumetric flasks, in volumetric flask, respectively add respectively again calcium standard solution (the 1000mg/L of 0.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL, with Ca metering) and phosphorus standard solution (10mg/L, with P metering), and be diluted to scale mark with deionized water; Three, assay, utilizes the concentration data of calcium in the standard sample that inductively coupled plasma emission spectrometer records or phosphorus, and makes working curve, then liquid to be measured is measured, and on working curve, search the content that obtains each calcium in sample and phosphorus, i.e. m
1calculate calcium in sample and the content of phosphorus according to formula (1),
in formula (1): W
ca, P(%): represent calcium or phosphorus content in sample, represent with massfraction; m
1: sample is searched the mass number obtaining from working curve, the mg of unit; m
0: sample sample weighting amount, the g of unit.
Specific embodiment
The water that the present embodiment adopts is deionized water.Related iron, nitric acid, hydrofluorite and the perchloric acid of the present embodiment is conventional commercially available prod simultaneously.Preferably grade is pure for analyzing.
Solution to be measured preparation: accurately take on request calcium-silicon sample 0.2000g that (" taking and preparing of ferroalloy chemical analysis sample " GB/T 4010-1994) prepare in the counteracting tank of 50 milliliters, add 10ml nitric acid (ρ 1.40g/cm3) and 5ml hydrofluorite (ρ 1.14g/cm3), counteracting tank is put into Hyperfrequency waves eliminating stove, it is 25 ℃ that digestion condition is set, and clearing up pressure is that 2.0MPa, digestion time are 10min.After clearing up, cool to room temperature, takes out counteracting tank, and counteracting tank solution is transferred in 150ml polytetrafluoroethylene beaker, add 5ml perchloric acid (ρ 1.67g/cm3) and stir evenly and smolder, take off slightly coldly, add 20ml water, transfer in 100ml volumetric flask, be diluted with water to scale, shake up.Divide again and get 10ml solution in 100ml volumetric flask, be diluted with water to scale, shake up, be prepared into solution to be measured.
Standard solution preparation: accurately take 0.1000g iron in the counteracting tank of 50 milliliters, add 10ml nitric acid (ρ 1.40g/cm3) and 5ml hydrofluorite (ρ 1.14g/cm3), counteracting tank is put into Hyperfrequency waves eliminating stove, and it is that 2.0MPa, digestion time are 10min that pressure is cleared up in setting.After clearing up, cool to room temperature, takes out counteracting tank, and counteracting tank solution is transferred in 150ml polytetrafluoroethylene beaker, add 5ml perchloric acid (ρ 1.67g/cm3) and smolder, take off slightly coldly, add 20ml water, transfer in 100ml volumetric flask, be diluted with water to scale, shake up.Divide again and get 6 parts of 10ml solution in 6 100ml volumetric flasks, and the corresponding calcium standard solution (1000mg/L that adds 0.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00ml respectively, in calcium) and isopyknic phosphorus standard solution (10mg/L, in phosphorus), be diluted with water to scale, shake up preparation standard test solution.
Calcium and phosphorus detection: adopt inductively coupled plasma emission spectrometer to measure respectively calcium and phosphorus intensity in working curve solution and sample solution, calculate content in sample.Concrete steps are, start shooting and equipment is reached after steady state (SS) according to instrument and equipment instructions, then measure calcium and P elements intensity in working curve solution, according to adding calcium and phosphorus standard solution content, be prepared into respectively working curve and the phosphorus content working curve to calcium intensity of calcium content to calcium intensity, secondly measure calcium and phosphorus intensity in solution to be measured, then in working curve, search the content that calculates calcium and phosphorus in solution according to element-intensities, finally calculate the content of calcium and phosphorus in sample according to lower formula (1).Repeat twice of aforesaid operations.Recording calcium content mean value in sample for twice is 40.78%, and phosphorus content mean value is 0.048%.
The detection method of simultaneously measuring calcium phosphorus content in calcium-silicon disclosed by the invention, have simple to operate, determination efficiency is high, sense cycle is short, when having realized calcium phosphorus content, measure, effectively reduce the laboratory detection efficiency of product, thereby can meet the requirement of the High-efficient Production of modern enterprise, there is chemical reagent consumption amount little simultaneously, pollute low, operation detection safety, testing cost is low, pollution low environment close friend, guarantee fully the quality of calcium-silicon, be conducive to improve the production efficiency of iron and steel enterprise, reduce production costs, guarantee the quality of product.
The disclosed technological means of the present invention program is not limited only to the disclosed technological means of above-mentioned technological means, also comprises the technical scheme being made up of above technical characterictic combination in any.The above is the specific embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (1)
1. measure the detection method of calcium phosphorus content in calcium-silicon for one kind simultaneously, it is characterized in that: the related solution density of the described detection method of simultaneously measuring calcium phosphorus content in calcium-silicon is all at the status of criterion (STP:273K or 298K, 1 standard atmospheric pressure QNE) lower mensuration, comprise the steps: one, solution to be measured preparation, take 0.2000g sample and be placed in 50mL counteracting tank, then add 10mL nitric acid (1.40g/mL) and 5mL hydrofluorite (1.14g/mL) in counteracting tank; Counteracting tank is put into Hyperfrequency waves eliminating stove, and 25 ℃ of digestion conditions, clear up pressure 2.0MPa, digestion time 10min; Clear up complete being cooled to after room temperature, solution is transferred to 150mL polytetrafluoroethylene beaker from counteracting tank, and after adding 5mL perchloric acid (1.67g/mL) to stir evenly to be fuming, be cooled to room temperature, add again 20mL deionized water, then be diluted to 100mL with deionized water with 100mL volumetric flask and make solution to be measured; Two, standard solution preparation, a, takes 0.1000g iron and is placed in 50mL counteracting tank, then adds 10mL nitric acid (1.40g/mL) and 5mL hydrofluorite (1.14g/mL) in counteracting tank; B, counteracting tank is put into Hyperfrequency waves eliminating stove, 25 ℃ of digestion conditions, clear up pressure 2.0MPa, digestion time 10min; C, clear up complete being cooled to after room temperature, solution is transferred to 150mL polytetrafluoroethylene beaker from counteracting tank, and after adding 5mL perchloric acid (1.67g/mL) to stir evenly to be fuming, is cooled to room temperature, add again 20mL deionized water, then be diluted to 100mL with 100mL volumetric flask and make solution to be measured; Get respectively again 6 parts of 10mL solution and be placed in 6 100mL volumetric flasks, in volumetric flask, respectively add respectively again calcium standard solution (the 1000mg/L of 0.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL, with Ca metering) and phosphorus standard solution (10mg/L, with P metering), and be diluted to scale mark with deionized water; Three, assay, utilizes the concentration data of calcium in the standard sample that inductively coupled plasma emission spectrometer records or phosphorus, and makes working curve, then liquid to be measured is measured, and on working curve, search the content that obtains each calcium in sample and phosphorus, i.e. m
1calculate calcium in sample and the content of phosphorus according to formula (1),
in formula (1): W
ca, P(%): represent calcium or phosphorus content in sample, represent with massfraction; m
1: sample is searched the mass number obtaining from working curve, the mg of unit; m
0: sample sample weighting amount, the g of unit.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106370510A (en) * | 2016-10-21 | 2017-02-01 | 天津大学 | Method for microwave digestion of glass body |
| CN109507012A (en) * | 2018-12-25 | 2019-03-22 | 广电计量检测（湖南）有限公司 | The full potassium digestion procedure of total Phosphorus In Soil and detection method |
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