The detection method of calcium phosphorus content in a kind of calcium-silicon of mensuration simultaneously
Technical field
The present invention relates to a kind of constituent content analysis method in analytical chemistry field, particularly one and measure silico-calcium conjunction simultaneously
The detection method of calcium phosphorus content in gold.
Background technology
Calcium and silicon have strong affinity with oxygen.Particularly calcium, not only has a strongest affinity with oxygen, and with sulfur, nitrogen
There is the strongest affinity, so calcium-silicon is a kind of comparatively ideal double deoxidizer, desulfurizing agent.Calcium-silicon not only deoxidation
Ability is strong, and deoxidation products is prone to float, it is easy to discharges, and can also improve the performance of steel, improves the plasticity of steel, toughness.At present,
Calcium-silicon is applied in high-quality steel, special steel and specific alloy production.The steel grades such as such as rail steel, mild steel, rustless steel
With the specific alloy such as nickel-base alloy, titanium-base alloy, calcium-silicon is all can use to make deoxidizer, desulfurizing agent, denitrifier and alloying constituent.Silicon
Calcium alloy also is adapted for being used as the heating agent in pneumatic steelmaking workshop, also act as the inovulant of cast iron and spheroidal graphite cast-iron produce in add
Add agent, make Graphite Distribution in ferrum uniform, reduce chilling tendency, and silicon, desulfurization can be increased, improve improving cast iron quality.Calcium-silicon is smelting
One of raw material that refining industry is conventional, the quality of calcium-silicon can directly affect the quality of smelting molten steel.Therefore, its silico-calcium element
The Accurate Determining of composition can occur for reducing waste product, for improving product quality etc. for formulating rational proportioning in smelting process
Valid data foundation is provided.Calcium-silicon is to smelt high-quality steel and one of deoxidation the most frequently used during special steel alloy and desulfurizing agent,
It is that continuous casting steel particularly Aluminum steel continuous casting is for preventing casting nozzle dross (set eye) from having to use for Calcium treatment alloy.In steelmaking process,
Xiang Gangzhong can change in steel the condition remaining field trash after adding calcium-silicon, reduces the content of steel inclusion, improves steel
The mechanical property of material, it is the cleanser that high purity steel produces.The most important two indices of calcium-silicon is exactly calcium and phosphorus contains
Amount, deoxidation, desulfurized effect during calcium content height direct steelmaking, phosphorus content likely enters molten steel, fall in adition process
Low steel quality.Therefore it is the most necessary for measuring calcium and phosphorus content in calcium-silicon." in calcium-silicon, silico-calcium element contains patent
The algoscopy of amount " although CN201110085892.6 discloses silicon and calcium catalyst method in calcium-silicon, but this patent uses
The molten high-temperature melting method of alkali decomposes sample, and this processing method is decomposed sample and related to substantial amounts of chemical reagent, complex operation, locates simultaneously
After reason, in sample solution, salts substances content is higher, is not suitable for Minor element detection (such as phosphorus), then uses traditional change
Credit analysis method measures silicon and the content of calcium in calcium-silicon, and the operation of this measuring method is the most complicated, detection speed is slow, is difficult to full
Foot modern enterprise production requirement.
Summary of the invention
For solving the problems referred to above, the invention discloses the detection method of calcium phosphorus content in a kind of calcium-silicon of mensuration simultaneously,
Having simple to operate, determination efficiency is high, and the detection cycle is short, it is achieved that measures while calcium phosphorus content, significantly reduces product
Test in laboratory efficiency such that it is able to meet the requirement efficiently produced of modern enterprise, there is chemical reagent consumption amount simultaneously
Little, testing cost is low, pollutes low environment friendly.
In the calcium-silicon of mensuration simultaneously disclosed by the invention, the solution density involved by detection method of calcium phosphorus content all exists
Measure under the status of criterion (STP:273K or 298K, 1 normal atmosphere QNE), comprise the steps: one, prepared by solution to be measured,
Weigh 0.2000g sample and be placed in 50mL counteracting tank, then in counteracting tank, add 10mL nitric acid (1.40g/mL) and 5mL Fluohydric acid.
(1.14g/mL);Counteracting tank is put in Hyperfrequency waves eliminating stove, digestion condition 25 DEG C, clear up pressure 2.0MPa, digestion time
10min;Clear up complete be cooled to room temperature after, solution is transferred to 150mL polytetrafluoroethylene beaker from counteracting tank, and adds
5mL perchloric acid (1.67g/mL) stirs evenly after being fuming, and is cooled to room temperature, then adds 20mL deionized water, then uses with deionized water
100mL volumetric flask is diluted to 100mL and makes solution to be measured;Two, prepared by standard solution, a, weighs 0.1000g ferrum and is placed in 50mL and disappears
Solve tank, then in counteracting tank, add 10mL nitric acid (1.40g/mL) and 5mL Fluohydric acid. (1.14g/mL);B, counteracting tank is put into micro-
In ripple digestion furnace, digestion condition 25 DEG C, clear up pressure 2.0MPa, digestion time 10min;C, clear up complete be cooled to room temperature after,
Solution is transferred to 150mL polytetrafluoroethylene beaker from counteracting tank, and adds 5mL perchloric acid (1.67g/mL) and stir evenly and be fuming
After, it is cooled to room temperature, then adds 20mL deionized water, then be diluted to 100mL with 100mL volumetric flask and make solution to be measured;Divide again
Do not take 6 parts of 10mL solution to be placed in 6 100mL volumetric flasks, in volumetric flask respectively each addition 0.00mL, 2.00mL,
The calcium standard solution (1000mg/L measures with Ca) of 4.00mL, 6.00mL, 8.00mL, 10.00mL and phosphorus standard solution (10mg/
L, measures with P), and it is diluted to graduation mark with deionized water;Three, assay, utilizes Inductively coupled plasma optical emission spectrometer
Calcium or the concentration data of phosphorus in the standard specimen recorded, and prepared working curve, then liquid to be measured is measured, and in work song
Search on line and obtain calcium and the content of phosphorus, i.e. m in each sample1The content of the calcium in sample and phosphorus is calculated according to formula (1),In formula (1): WCa,P(%): represent calcium or phosphorus content in sample, divide by quality
Number represents;m1: sample searches the mass number obtained, unit mg from working curve;m0: sample sample weighting amount, unit g.
In the calcium-silicon of mensuration simultaneously disclosed by the invention, the detection method of calcium phosphorus content, has simple to operate, measures effect
Rate is high, and the detection cycle is short, it is achieved that measures while calcium phosphorus content, significantly reduces the test in laboratory efficiency of product, from
And disclosure satisfy that the requirement efficiently produced of modern enterprise, and there is chemical reagent consumption amount little simultaneously, pollute low, operation detection peace
Entirely, testing cost is low, pollutes low environment friendly, ensure that the quality of calcium-silicon fully, is conducive to improving iron and steel enterprise
Production efficiency, reduces production cost, it is ensured that the quality of product.
Detailed description of the invention
Below in conjunction with detailed description of the invention, it is further elucidated with the present invention, it should be understood that following detailed description of the invention is only used for
The bright present invention rather than restriction the scope of the present invention.
In the calcium-silicon of mensuration simultaneously disclosed by the invention, the solution density involved by detection method of calcium phosphorus content all exists
Measure under the status of criterion (STP:273K or 298K, 1 normal atmosphere QNE), comprise the steps: one, prepared by solution to be measured,
Weigh 0.2000g sample and be placed in 50mL counteracting tank, then in counteracting tank, add 10mL nitric acid (1.40g/mL) and 5mL Fluohydric acid.
(1.14g/mL);Counteracting tank is put in Hyperfrequency waves eliminating stove, digestion condition 25 DEG C, clear up pressure 2.0MPa, digestion time
10min;Clear up complete be cooled to room temperature after, solution is transferred to 150mL polytetrafluoroethylene beaker from counteracting tank, and adds
5mL perchloric acid (1.67g/mL) stirs evenly after being fuming, and is cooled to room temperature, then adds 20mL deionized water, then uses with deionized water
100mL volumetric flask is diluted to 100mL and makes solution to be measured;Two, prepared by standard solution, a, weighs 0.1000g ferrum and is placed in 50mL and disappears
Solve tank, then in counteracting tank, add 10mL nitric acid (1.40g/mL) and 5mL Fluohydric acid. (1.14g/mL);B, counteracting tank is put into micro-
In ripple digestion furnace, digestion condition 25 DEG C, clear up pressure 2.0MPa, digestion time 10min;C, clear up complete be cooled to room temperature after,
Solution is transferred to 150mL polytetrafluoroethylene beaker from counteracting tank, and adds 5mL perchloric acid (1.67g/mL) and stir evenly and be fuming
After, it is cooled to room temperature, then adds 20mL deionized water, then be diluted to 100mL with 100mL volumetric flask and make solution to be measured;Divide again
Do not take 6 parts of 10mL solution to be placed in 6 100mL volumetric flasks, in volumetric flask respectively each addition 0.00mL, 2.00mL,
The calcium standard solution (1000mg/L measures with Ca) of 4.00mL, 6.00mL, 8.00mL, 10.00mL and phosphorus standard solution (10mg/
L, measures with P), and it is diluted to graduation mark with deionized water;Three, assay, utilizes Inductively coupled plasma optical emission spectrometer
Calcium or the concentration data of phosphorus in the standard specimen recorded, and prepared working curve, then liquid to be measured is measured, and in work song
Search on line and obtain calcium and the content of phosphorus, i.e. m in each sample1The content of the calcium in sample and phosphorus is calculated according to formula (1),In formula (1): WCa,P(%): represent calcium or phosphorus content in sample, divide by quality
Number represents;m1: sample searches the mass number obtained, unit mg from working curve;m0: sample sample weighting amount, unit g.
Specific embodiment
The water that the present embodiment is used is deionized water.Ferrum, nitric acid, Fluohydric acid. and height involved by the present embodiment simultaneously
Chloric acid is conventional commercial product.Preferably grade is analytical pure.
Prepared by solution to be measured: accurately weigh the most on request (" taking and preparing of ferroalloy chemical analysis sample " GB/T
Calcium-silicon sample 0.2000g 4010-1994) prepared, in the counteracting tank of 50 milliliters, adds 10ml nitric acid (ρ 1.40g/
And 5ml Fluohydric acid. (ρ 1.14g/cm3) cm3), being put into by counteracting tank in Hyperfrequency waves eliminating stove, arranging digestion condition is 25 DEG C, clears up
Pressure is 2.0MPa, digestion time is 10min.After clearing up, it is cooled to room temperature, takes out counteracting tank, counteracting tank solution is turned
Move on in 150ml polytetrafluoroethylene beaker, add 5ml perchloric acid (ρ 1.67g/cm3) and stir evenly and smolder, take off the coldest, add 20ml water,
Transfer to, in 100ml volumetric flask, be diluted with water to scale, shake up.Divide again and take 10ml solution in 100ml volumetric flask, dilute with water
Release scale, shake up, be prepared as solution to be measured.
Prepared by standard solution: accurately weigh 0.1000g ferrum in the counteracting tank of 50 milliliters, adds 10ml nitric acid (ρ 1.40g/
And 5ml Fluohydric acid. (ρ 1.14g/cm3) cm3), counteracting tank is put in Hyperfrequency waves eliminating stove, arrange and clear up pressure and be 2.0MPa, disappear
The solution time is 10min.After clearing up, it is cooled to room temperature, takes out counteracting tank, counteracting tank solution is transferred to 150ml polytetrafluoro
In ethylene beaker, add 5ml perchloric acid (ρ 1.67g/cm3) and smolder, take off the coldest, add 20ml water, transfer in 100ml volumetric flask,
It is diluted with water to scale, shakes up.Divide again and take 6 parts of 10ml solution in 6 100ml volumetric flasks, and respectively correspondence add 0.00mL,
The calcium standard solution (1000mg/L, in terms of calcium) of 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00ml and isopyknic phosphorus
Standard solution (10mg/L, in terms of phosphorus), is diluted with water to scale, shakes up, prepare standard solution.
Calcium and phosphorus detection: use Inductively coupled plasma optical emission spectrometer to measure working curve solution and sample respectively
Calcium and phosphorus intensity in solution, calculate content in sample.Comprise the concrete steps that, start shooting according to instrument and equipment description and make equipment reach
After steady statue, then measure calcium and P elements intensity in working curve solution, according to adding calcium and phosphorus standard solution content, point
It is not prepared as calcium content to the working curve of calcium intensity and the phosphorus content working curve to calcium intensity, secondly measures in solution to be measured
Calcium and phosphorus intensity, then according to element-intensities search in working curve calculating solution in calcium and the content of phosphorus, finally according under
Formula (1) calculates calcium and the content of phosphorus in sample.Repeat aforesaid operations twice.Recording calcium content meansigma methods in sample for twice is
40.78%, phosphorus content meansigma methods is 0.048%.
In the calcium-silicon of mensuration simultaneously disclosed by the invention, the detection method of calcium phosphorus content, has simple to operate, measures effect
Rate is high, and the detection cycle is short, it is achieved that measures while calcium phosphorus content, significantly reduces the test in laboratory efficiency of product, from
And disclosure satisfy that the requirement efficiently produced of modern enterprise, and there is chemical reagent consumption amount little simultaneously, pollute low, operation detection peace
Entirely, testing cost is low, pollutes low environment friendly, ensure that the quality of calcium-silicon fully, is conducive to improving iron and steel enterprise
Production efficiency, reduces production cost, it is ensured that the quality of product.
Technological means disclosed in the present invention program is not limited only to the technological means disclosed in above-mentioned technological means, also includes
The technical scheme being made up of above technical characteristic combination in any.The above is the detailed description of the invention of the present invention, it should refer to
Go out, for those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to make some
Improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.