CN103512879B - The method of calcium, barium, Mg content in Si Si bond surveyed by a kind of complexometric titration connection - Google Patents
The method of calcium, barium, Mg content in Si Si bond surveyed by a kind of complexometric titration connection Download PDFInfo
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Abstract
The present invention discloses the method that a kind of complexometric titration connection surveys calcium in Si Si bond, barium, Mg content, comprising: sample solution and the blank solution as a comparison preparing described alloy; Volumetric soiutions and blank titration solution is prepared respectively by described sample solution and described blank solution; Described volumetric soiutions comprises calcium volumetric soiutions, calcium and barium volumetric soiutions, calcium and magnesium volumetric soiutions; Described blank titration solution comprises calcium blank titration solution, calcium and barium blank titration solution, calcium and magnesium blank titration solution; With EDTA standardized solution volumetric soiutions and described blank titration solution described in titration respectively, according to the consumption of described EDTA standardized solution, calculate the content of calcium, barium, magnesium in described alloy respectively. Molten sample only need to be carried out once by method provided by the invention, just can under same solution, the content of Simultaneously test calcium, barium, magnesium three kinds of elements, easy and simple to handle.
Description
Technical field
The present invention relates to steel and alloy analysis technical field, particularly relate to the method that a kind of complexometric titration connection surveys calcium, barium, Mg content in Si?Si bond.
Background technology
Si?Si bond is a kind of new and effective composite deoxidant, sweetening agent, is mainly used in molten steel deoxidation, dephosphorization. It can effectively remove the impurity in steel by ball or refinement steel inclusion, changes the character of steel inclusion, reduces the deleterious effect of non-metallic inclusion. Make molten steel purifying, it is to increase the quality of steel. The smelting of high-quality steel is played an important role. Metallurgical industry has applications well prospect. Therefore measure calcium, barium, Mg content in Si?Si bond to have a very important role
At present, the content measuring barium in Si-Ca-Ba-Mg generally adopts weighting method, and does not have unified international standard measuring method, and weighting method operation is loaded down with trivial details, and analysis process is long, can not meet requirement fast and accurately in production. The mensuration of calcium contents generally adopts ethylenediamine tetraacetic acid (EDTA) (EthyleneDiamineTetraaceticAcid, EDTA) complexometry, adopts Atomic Emission SpectrometerAES (ICP) to measure the content of magnesium. Needing the many posies of many people to carry out during mensuration, consuming cost is big, and length consuming time, and labor intensive is big.
Summary of the invention
It is an object of the invention to provide the method that a kind of complexometric titration connection surveys calcium, barium, Mg content in Si?Si bond, only need to carry out once molten sample, just can under same solution, the content of Simultaneously test calcium, barium, magnesium three kinds of elements, easy and simple to handle.
Technical scheme is specific as follows:
A method for calcium, barium, Mg content in Si?Si bond surveyed by complexometric titration connection, comprising:
Prepare sample solution and the blank solution as a comparison of described alloy;
Volumetric soiutions and blank titration solution is prepared respectively by described sample solution and described blank solution; Described volumetric soiutions comprises calcium volumetric soiutions, calcium and barium volumetric soiutions, calcium and magnesium volumetric soiutions; Described blank titration solution comprises calcium blank titration solution, calcium and barium blank titration solution, calcium and magnesium blank titration solution;
The compound method of described calcium volumetric soiutions: divide and get sample solution described in 50mL in the beaker of 250mL, add 50mL water, 0.2g oxammonium hydrochloride, 5mL triethanolamine solution, 10mL potassium sulfate solution, place 10 minutes, add 40mL potassium hydroxide solution and calconcarboxylic acid again, obtain described calcium volumetric soiutions; With calcium volumetric soiutions described in described EDTA standardized solution titration, the consumption of described EDTA standardized solution is VCa; Divide and get blank solution described in 50mL, according to the compound method of described calcium volumetric soiutions, obtain described calcium blank titration solution; With calcium blank titration solution described in described EDTA standardized solution titration, the consumption of described EDTA standardized solution is V01;
The compound method of described calcium and barium volumetric soiutions: divide and get sample solution described in 50mL in the beaker of 250mL, add 50mL water, 0.2g oxammonium hydrochloride, 5mL triethanolamine solution, 40mL potassium hydroxide solution and fluorexon mixture indicator, obtain described calcium and barium volumetric soiutions; With calcium and barium volumetric soiutions described in described EDTA standardized solution titration, the consumption of described EDTA standardized solution is VCa+Ba; Divide and get blank solution described in 50mL, according to the compound method of described calcium and barium volumetric soiutions, obtain described calcium and barium blank titration solution; With calcium and barium blank titration solution described in described EDTA standardized solution titration, the consumption of described EDTA standardized solution is V02;
The compound method of described calcium and magnesium volumetric soiutions: divide and get sample solution described in 50mL in the beaker of 250mL, add 50mL water, 0.2g oxammonium hydrochloride, 5mL triethanolamine solution, 10mL potassium sulfate solution, place 10 minutes, add 10mL ammonia-chloride buffer solution and o-cresolphthalein indicator again, obtain described calcium and magnesium volumetric soiutions; With calcium and magnesium volumetric soiutions described in described EDTA standardized solution titration, the consumption of described EDTA standardized solution is VCa+Mg; Divide and get blank solution described in 50mL, according to the compound method of described calcium and magnesium volumetric soiutions, obtain described calcium and magnesium blank titration solution; With calcium and magnesium blank titration solution described in described EDTA standardized solution titration, the consumption of described EDTA standardized solution is V03;
With EDTA standardized solution volumetric soiutions and described blank titration solution described in titration respectively, consumption according to described EDTA standardized solution, the calculation formula calculating the content of calcium, barium, magnesium in alloy described in the content of calcium, barium, magnesium in described alloy respectively is respectively:
Wherein: the concentration of c---EDTA standardized solution, mol/L; M---sample mass, g; K---sample divides liquid proportional; MCa---the molar mass of calcium; MBa---the molar mass of barium; MMg---the molar mass of magnesium.
Further: the compound method of described sample solution: to take 0.2500g alloy sample in 250mL polytetrafluoroethylene beaker, in polytetrafluoroethylene beaker, add nitric acid 10mL, hydrochloric acid 5mL, shake lower and add hydrofluoric acid 8mL, make described sample dissolution; Add perchloric acid 10mL again, heat the solution in described polytetrafluoroethylene beaker, make perchloric acid smoked, and make solution evaporation to dry, obtain salt thing, cooling; Adding hydrochloric acid and isopyknic water 10mL altogether in described polytetrafluoroethylene beaker, heating makes described salt thing dissolve, and is proceeded in 400mL beaker, and the volume adding water to solution in beaker is 150mL; Dripping in beaker and add ammonia soln to pH value 6��7, heated and boiled, filters; Wash beaker 4-5 time with ammonium chloride solution and precipitate 9-10 time, dilute filtrate to 250mL with water, mixed even, obtain described sample solution; According to the compound method of described sample solution, do not add described sample, prepare described blank solution.
Further: the compound method of described calconcarboxylic acid: 1g standard calcium indicator mixes after grinding with the Repone K after 100g oven dry.
Further: the compound method of described fluorexon mixture indicator: fluorexon 1g, the Repone K after alizarin 1g and 100g oven dry mixes after grinding.
Further: the compound method of described ammonia-chloride buffer solution: 67g ammonium chloride is dissolved in 200mL water, then add in ammoniacal liquor that 570mL density is 0.90g/mL, mixing.
Further: described in described EDTA standardized solution titration during calcium volumetric soiutions, it is terminal that described calcium volumetric soiutions turns into blueness from redness;
Described in described EDTA standardized solution titration when calcium and barium volumetric soiutions, it is terminal that the color of described calcium and barium volumetric soiutions turns into orange red;
Described in described EDTA standardized solution titration when calcium and magnesium volumetric soiutions, it is terminal that the color of described calcium and magnesium volumetric soiutions turns into brilliant white.
The useful effect of the present invention:
1, fast, accurately: traditional method can only once survey a kind of element by molten sample, and operate loaded down with trivial details, and the present invention only need to carry out once molten sample, just can complete the Simultaneously test of calcium, barium, magnesium three kinds of elements under same solution, the rapid and accurate determination of calcium, barium, magnesium in Si-Ca-Ba-Mg in daily production can be met completely.
2, analysis cost reduces: calcium, barium, magnesium three kinds of elements need the many people in many posies to carry out when measuring respectively simultaneously. And the present invention only needs to carry out once molten sample, adopt a kind of complexometric titration agent just can complete the Simultaneously test of three kinds of elements, save manpower and cost.
Embodiment
Total thinking of the present invention: adopt nitric acid-hydrochloric acid-hydrofluoric acid dissolution sample, add perchloric acid to strengthen capacity of decomposition, smolder remaining nitric acid, hydrochloric acid, hydrofluoric acid after catching up with most reaction, by EDTA volumetry after the interference elements such as ammoniacal liquor separation of iron, aluminium, the buffer system of pH=10 measures calcium magnesium resultant, calcium and calcium barium resultant is measured respectively, it is achieved that dissolved samples Simultaneously test calcium, barium, magnesium three kinds of elements when the buffer system of pH=12.
In the present invention, agents useful for same is preferred:
The density of nitric acid is 1.42g/mL; The density of hydrofluoric acid is 1.15g/mL; The density of hydrochloric acid is 1.19g/mL; The density of perchloric acid is 1.67g/mL; Oxammonium hydrochloride used is solid; In triethanolamine solution, the volume ratio of trolamine and water is 1:4; The ammoniacal liquor of ammonia soln to be density be 0.90g/mL mixes with isopyknic water. The concentration of potassium hydroxide solution is 200g/L; The concentration of ammonium chloride solution is 10g/L; The concentration of potassium sulfate solution is 100g/L; The concentration of EDTA standardized solution is 0.007mol/L;
The compound method of the ammonia of pH=10-chloride buffer solution: 67g ammonium chloride is dissolved in 200mL water, adds in the ammoniacal liquor that 570mL density is 0.90g/mL, mixed even;
The compound method of fluorexon mixture indicator: take fluorexon 1g, the Repone K after alizarin 1g and 100g oven dry grinds thin mixed even;
The compound method of calconcarboxylic acid: 1g standard calcium indicator and 100g dry after Repone K grind thin mixed even.
The method steps that complexometric titration connection surveys calcium, barium, Mg content in Si?Si bond is as follows:
According to QJH/BG-01-02, sample is carried out pre-treatment, make sample become the homogeneous powder powder sample of easily decomposition.
Step 1: the solution of preparation Si?Si bond sample and blank solution;
Take 0.2500g Si?Si bond sample in 250mL polytetrafluoroethylene beaker, in polytetrafluoroethylene beaker, add nitric acid 10mL, hydrochloric acid 5mL, shake lower and add about 8mL hydrofluoric acid and dissolve completely to sample, then add perchloric acid 10mL; Polytetrafluoroethylene beaker is placed on Low-temp. electrothermal plate and heats, make perchloric acid smoked, and make the solution evaporation in polytetrafluoroethylene beaker to dry, take off slightly cold. Adding hydrochloric acid and isopyknic water 10mL altogether in polytetrafluoroethylene beaker, heating makes salt dissolve, and takes off, is proceeded in 400mL beaker, add water, and in control beaker, the volume of solution is about 150mL. Drip in beaker and add ammonia soln and be neutralized to pH value 6��7, heated and boiled, filter with middling speed qualitative filter paper while hot. Wash beaker 4-5 time with the ammonium chloride solution of heat and precipitate 9-10 time, abandon precipitation, be diluted with water to 250mL, mixed even, obtain sample solution.
Blank test: add nitric acid 10mL in the polytetrafluoroethylene beaker of sky, hydrochloric acid 5mL, hydrofluoric acid 8mL, perchloric acid 10mL; Polytetrafluoroethylene beaker is placed on Low-temp. electrothermal plate and heats, make perchloric acid smoked, and make the solution evaporation in polytetrafluoroethylene beaker to dry, take off slightly cold. Adding hydrochloric acid and isopyknic water 10mL altogether in polytetrafluoroethylene beaker, take off, proceeded in 400mL beaker, add water after heating, in control beaker, the volume of solution is about 150mL. Drip in beaker and add ammonia soln, be adjusted to pH value 6��7, heated and boiled, filter with middling speed qualitative filter paper while hot. Wash beaker 4-5 time with the ammonium chloride solution of heat and precipitate 9-10 time, abandon precipitation, be diluted with water to 250mL, mixed even, obtain blank solution.
Step 2: prepare volumetric soiutions and blank titration solution by sample solution and blank solution respectively, with EDTA standardized solution titration volumetric soiutions and blank titration solution respectively, and calculates the content of calcium, barium, magnesium;
The preparation of calcium volumetric soiutions: divide and get 50mL sample solution in the beaker of 250mL, add 50mL water, 0.2g oxammonium hydrochloride, 5mL triethanolamine solution, 10mL potassium sulfate solution, place 10 minutes, add 40mL potassium hydroxide solution and appropriate calconcarboxylic acid again, obtain calcium volumetric soiutions; With EDTA standardized solution titration calcium volumetric soiutions, it is terminal that solution turns into blueness from redness, and the consumption of its EDTA standardized solution is VCa��
The preparation of calcium blank titration solution: divide and get 50mL blank solution in the beaker of 250mL, add 50mL water, 0.2g oxammonium hydrochloride, 5mL triethanolamine solution, 10mL potassium sulfate solution, place 10 minutes, add 40mL potassium hydroxide solution and appropriate calconcarboxylic acid again, obtain calcium blank titration solution; With EDTA standardized solution titration calcium blank titration solution, it is terminal that solution turns into blueness from redness, and the consumption of its EDTA standardized solution is V01��
The preparation of calcium and barium volumetric soiutions: divide and get 50mL sample solution in the beaker of 250mL, add 50mL water, 0.2g oxammonium hydrochloride, 5mL triethanolamine solution, 40mL potassium hydroxide solution and appropriate fluorexon mixture indicator, obtain calcium and barium volumetric soiutions; With EDTA standardized solution titration calcium and barium volumetric soiutions, turning into orange red to solution colour is terminal, and the consumption of its EDTA standardized solution is VCa+Ba��
The preparation of calcium and barium blank titration solution: divide and get 50mL blank solution in the beaker of 250mL, add 50mL water, 0.2g oxammonium hydrochloride, 5mL triethanolamine solution, 40mL potassium hydroxide solution and appropriate fluorexon mixture indicator, obtain calcium and barium blank titration solution; With EDTA standardized solution titration calcium and barium blank titration solution, turning into orange red to solution colour is terminal, and the consumption of its EDTA standardized solution is V02��
The preparation of calcium and magnesium volumetric soiutions: divide and get 50mL sample solution in the beaker of 250mL, add 50mL water, 0.2g oxammonium hydrochloride, 5mL triethanolamine solution, 10mL potassium sulfate solution, place 10 minutes, add 10mL ammonia-chloride buffer solution and a little o-cresolphthalein indicator again, obtain calcium and magnesium volumetric soiutions; With EDTA standardized solution titration calcium and magnesium volumetric soiutions, turning into brilliant white to solution colour is terminal, and the consumption of its EDTA standardized solution is VCa+Mg��
The preparation of calcium and magnesium blank titration solution: divide and get 50mL blank solution in the beaker of 250mL, add 50mL water, 0.2g oxammonium hydrochloride, 5mL triethanolamine solution, 10mL potassium sulfate solution, place 10 minutes, add 10mL ammonia-chloride buffer solution and a little o-cresolphthalein indicator again, obtain calcium and magnesium blank titration solution; With EDTA standardized solution titration calcium and magnesium blank titration solution, turning into brilliant white to solution colour is terminal, and the consumption of its EDTA standardized solution is V03��
According to formula below, calculate the content of calcium, barium, magnesium respectively:
In above-mentioned formula: the concentration of c---EDTA standardized solution, mol/L;
VCa---titration sample solution is consumed the volume of EDTA standardized solution, mL during calcium;
VCa+Ba---titration sample solution is consumed the volume of EDTA standardized solution, mL when calcium, barium;
VCa+Mg---titration sample solution is consumed the volume of EDTA standardized solution, mL when calcium, magnesium;
M---sample mass, g;
K---sample divides liquid proportional, divides and get 50mL in the present embodiment from 250mL sample solution, so K=1/5;
V01---titration blank solution is consumed the volume of EDTA standardized solution, mL during calcium;
V02---titration blank solution is consumed the volume of EDTA standardized solution, mL when calcium, barium;
V03---titration blank solution is consumed the volume of EDTA standardized solution, mL when calcium, magnesium;
MCa---the molar mass (40.08g/mol) of calcium;
MBa---the molar mass (37.33g/mol) of barium;
MMg---the molar mass (24.30g/mol) of magnesium.
Measuring Si?Si bond sample according to measuring method of the present invention, its measuring result is as shown in table 1��3.
The mensuration of Ca in table 1 Si?Si bond
The mensuration of Mg in table 2 Si?Si bond
The mensuration of Ba in table 3 Si?Si bond
By table 1��3 it may be seen that the measuring result (measured value) obtained by measuring method of the present invention differs less with standard value, illustrate and can realize calcium in Si-Ca-Ba-Mg, barium, magnesium connection cls analysis fast and accurately by the method for complexometric titration.
Claims (6)
1. a method for calcium, barium, Mg content in Si?Si bond surveyed by complexometric titration connection, comprising:
Prepare sample solution and the blank solution as a comparison of described alloy;
Volumetric soiutions and blank titration solution is prepared respectively by described sample solution and described blank solution; Described volumetric soiutions comprises calcium volumetric soiutions, calcium and barium volumetric soiutions, calcium and magnesium volumetric soiutions; Described blank titration solution comprises calcium blank titration solution, calcium and barium blank titration solution, calcium and magnesium blank titration solution;
The compound method of described calcium volumetric soiutions: divide and get sample solution described in 50mL in the beaker of 250mL, add 50mL water, 0.2g oxammonium hydrochloride, 5mL triethanolamine solution, 10mL potassium sulfate solution, place 10 minutes, add 40mL potassium hydroxide solution and calconcarboxylic acid again, obtain described calcium volumetric soiutions; With calcium volumetric soiutions described in edta edta standardized solution titration, the consumption of described EDTA standardized solution is VCa; Divide and get blank solution described in 50mL, according to the compound method of described calcium volumetric soiutions, obtain described calcium blank titration solution; With calcium blank titration solution described in described EDTA standardized solution titration, the consumption of described EDTA standardized solution is V01;
The compound method of described calcium and barium volumetric soiutions: divide and get sample solution described in 50mL in the beaker of 250mL, add 50mL water, 0.2g oxammonium hydrochloride, 5mL triethanolamine solution, 40mL potassium hydroxide solution and fluorexon mixture indicator, obtain described calcium and barium volumetric soiutions; With calcium and barium volumetric soiutions described in described EDTA standardized solution titration, the consumption of described EDTA standardized solution is VCa+Ba; Divide and get blank solution described in 50mL, according to the compound method of described calcium and barium volumetric soiutions, obtain described calcium and barium blank titration solution; With calcium and barium blank titration solution described in described EDTA standardized solution titration, the consumption of described EDTA standardized solution is V02;
The compound method of described calcium and magnesium volumetric soiutions: divide and get sample solution described in 50mL in the beaker of 250mL, add 50mL water, 0.2g oxammonium hydrochloride, 5mL triethanolamine solution, 10mL potassium sulfate solution, place 10 minutes, add 10mL ammonia-chloride buffer solution and o-cresolphthalein indicator again, obtain described calcium and magnesium volumetric soiutions; With calcium and magnesium volumetric soiutions described in described EDTA standardized solution titration, the consumption of described EDTA standardized solution is VCa+Mg; Divide and get blank solution described in 50mL, according to the compound method of described calcium and magnesium volumetric soiutions, obtain described calcium and magnesium blank titration solution; With calcium and magnesium blank titration solution described in described EDTA standardized solution titration, the consumption of described EDTA standardized solution is V03;
With EDTA standardized solution volumetric soiutions and described blank titration solution described in titration respectively, according to the consumption of described EDTA standardized solution, calculate the content of calcium, barium, magnesium in described alloy respectively; In described alloy, the calculation formula of the content of calcium, barium, magnesium is respectively:
Wherein: the concentration of c---EDTA standardized solution, mol/L; M---sample mass, g; K---sample divides liquid proportional; MCa---the molar mass of calcium; MBa---the molar mass of barium; MMg---the molar mass of magnesium.
2. the method for calcium, barium, Mg content in Si?Si bond surveyed by complexometric titration connection as claimed in claim 1, it is characterized in that, the compound method of described sample solution: take 0.2500g alloy sample in 250mL polytetrafluoroethylene beaker, nitric acid 10mL is added in polytetrafluoroethylene beaker, hydrochloric acid 5mL, shake lower and add hydrofluoric acid 8mL, make described sample dissolution; Add perchloric acid 10mL again, heat the solution in described polytetrafluoroethylene beaker, make perchloric acid smoked, and make solution evaporation to dry, obtain salt thing, cooling; Adding hydrochloric acid and isopyknic water 10mL altogether in described polytetrafluoroethylene beaker, heating makes described salt thing dissolve, and is proceeded in 400mL beaker, and the volume adding water to solution in beaker is 150mL; Dripping in beaker and add ammonia soln to pH value 6��7, heated and boiled, filters; Wash beaker 4-5 time with ammonium chloride solution and precipitate 9-10 time, dilute filtrate to 250mL with water, mixed even, obtain described sample solution;
According to the compound method of described sample solution, do not add described sample, prepare described blank solution.
3. the method for calcium, barium, Mg content in Si?Si bond surveyed by complexometric titration connection as claimed in claim 1, it is characterised in that, the compound method of described calconcarboxylic acid: 1g standard calcium indicator mixes after grinding with the Repone K after 100g oven dry.
4. the method for calcium, barium, Mg content in Si?Si bond surveyed by complexometric titration connection as claimed in claim 1, it is characterized in that, the compound method of described fluorexon mixture indicator: fluorexon 1g, the Repone K after alizarin 1g and 100g oven dry mixes after grinding.
5. the method for calcium, barium, Mg content in Si?Si bond surveyed by complexometric titration connection as claimed in claim 1, it is characterized in that, the compound method of described ammonia-chloride buffer solution: 67g ammonium chloride is dissolved in 200mL water, then add in ammoniacal liquor that 570mL density is 0.90g/mL, mixing.
6. the method for calcium, barium, Mg content in Si?Si bond surveyed by complexometric titration connection as claimed in claim 1, it is characterised in that, described in described EDTA standardized solution titration during calcium volumetric soiutions, it is terminal that described calcium volumetric soiutions turns into blueness from redness;
Described in described EDTA standardized solution titration when calcium and barium volumetric soiutions, it is terminal that the color of described calcium and barium volumetric soiutions turns into orange red;
Described in described EDTA standardized solution titration when calcium and magnesium volumetric soiutions, it is terminal that the color of described calcium and magnesium volumetric soiutions turns into brilliant white.
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