CN104458731A - Method for joint measurement of calcium-barium content of silicon-barium alloy by using compleximetry - Google Patents
Method for joint measurement of calcium-barium content of silicon-barium alloy by using compleximetry Download PDFInfo
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- CN104458731A CN104458731A CN201410751333.8A CN201410751333A CN104458731A CN 104458731 A CN104458731 A CN 104458731A CN 201410751333 A CN201410751333 A CN 201410751333A CN 104458731 A CN104458731 A CN 104458731A
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Abstract
The invention relates to a method for joint measurement of calcium-barium content of a silicon-barium alloy by using compleximetry. The method is characterized by comprising the following steps: dissolving a sample by using nitric acid and hydrofluoric acid; adding perchloric acid until smoke is generated; steaming until the sample is dried; dissolving salts by using hydrochloric acid, fixing volume by using water, then taking two samples, and adding a masking agent into the two samples respectively to eliminate interference elements; then mixing calcein with an indicator; performing titration by using EDTA (ethylene diamine tetraacetic acid) as a standard solution to measure the calcium-barium content and the calcium content respectively; and performing subtractive calculation to obtain the barium content. The method has the following advantages: by virtue of joint measurement, simultaneous measurements by one time of sample dissolving are realized, and successive measurements by two times of sample dissolving are not needed, so that the operation time is greatly shortened, and the operation is quick and accurate; by one time of sample dissolving, the labor capacity of workers is reduced, the added types and added amount of chemicals are greatly reduced, the cost is saved, the use frequency of a electric hot plate is reduced, and the energy consumption is reduced.
Description
Technical field
The invention belongs to technical field of analytical chemistry, relate to the quantitative analysis method of calcium in a kind of Si-Ba alloy-barium translocation.
Background technology
Si-Ba alloy is a kind of new and effective double deoxidizer, silicon in deoxidation process, calcium, and barium three kinds of elements promote mutually, effectively improve the utilization factor of adjuvant.It is mainly used in deoxidation in molten steel, dephosphorization.Other complex oxides of formation can be made easily to float from molten steel, cleaning molten steel, improve impact flexibility and the processing characteristics of steel.Oxygen content in steel can be made to drop to minimum.Make molten steel purifying, improve the quality of steel.Applications well prospect is had in metallurgical industry.Therefore fast, in Accurate Determining Si-Ba alloy, calcium, barium content have a very important role.
At present, measuring calcium, barium two kinds of elements in Si-Ba alloy needs molten sample respectively to detect respectively.Measure calcium in Si-Ba alloy and mainly adopt EDTA compleximetry.Sample is through the molten sample of nitrate acid and hydrofluoric acid, and sulfuric acid is smoldered, and after dissolved salts, regulate pH value to be separated interference element, dividing and get part solution, is that indicator carries out titration with calcon-carboxylic acid.The mensuration of Barium in Silico-Barium Alloy mainly adopts gravimetric method, needs secondary precipitate, long flow path, and drug variety is many, consumes large, can not measure very soon.
Summary of the invention
The object of the invention is to measure to distinguish molten sample when overcoming calcium, barium in existing method mensuration Si-Ba alloy, it is many that medicine adds kind, length consuming time, the problem of complex operation, a kind of easy, once calcium, barium two kinds of elements in molten sample translocation Si-Ba alloy are accurately and rapidly provided, thus reduce manpower and materials cost, shorten the method for calcium-barium content in operation steps and the complexometry translocation Si-Ba alloy of running time.
Method of the present invention is realized by following steps:
Sample is through the molten sample of nitrate acid and hydrofluoric acid, perchloric acid smoked, be evaporated to dry, after dissolving with hydrochloric acid salt, get two parts of samples with after water constant volume point, after adding screening agent elimination interference element respectively, use calcein mixed indicator, carry out titration with EDTA as standard solution, measure the content of calcium barium resultant and calcium respectively, difference subtracts the content calculating barium, and computing formula is as follows:
；
；
Wherein:
The concentration of c---EDTA standard solution, mol/L;
M---sample mass, g;
K---sample divides liquid proportional;
V
ca---in titration sample solution during calcium consume the volume of EDTA standard solution, mL;
V
ca+Ba---in titration sample solution when calcium, barium consume the volume of EDTA standard solution, mL;
V
01---in titration blank solution during calcium consume the volume of EDTA standard solution, mL;
V
02---in titration blank solution when calcium, barium consume the volume of EDTA standard solution, mL;
M
ca---the molal weight of calcium;
M
ba---the molal weight of barium.
Described screening agent is triethanolamine solution, oxammonium hydrochloride, potassium sulfate solution and potassium hydroxide solution, or is triethanolamine solution, oxammonium hydrochloride and potassium hydroxide solution.
Advantage of the present invention is:
1) fast, accurately: achieve once molten sample Simultaneously test by translocation, successively need not measure by twice molten sample, this substantially reduces the running time, fast, accurately.
2) energy-conservation, efficient: once molten sample decreases the labor capacity of personnel, what greatly reduce medicine adds kind and addition, has saved cost, decreases the frequency of utilization of electric hot plate, reduces energy consumption.This method has efficient, energy-conservation advantage.
Embodiment
1. method summary:
Get Si-Ba alloy sample, through the molten sample of nitrate acid and hydrofluoric acid, perchloric acid smoked, after dissolving with hydrochloric acid salt, divide with water constant volume and get aliquot, after adding screening agent elimination interference element, use EDTA to carry out titration as standard solution, measure the content of calcium barium resultant and calcium respectively.Difference subtracts the content calculating barium.
2. reagent:
Nitric acid (density 1.42 g/mL)
Hydrofluorite: (density 1.15g/mL)
Perchloric acid: (density 1.67g/mL);
Hydrochloric acid: (density is that the hydrochloric acid of 1.19g/mL mixes with isopyknic water);
Triethanolamine solution: (volume ratio of triethanolamine and water is 1:4);
Oxammonium hydrochloride (solid);
Ammoniacal liquor (density is that the ammoniacal liquor of 0.90g/mL mixes with isopyknic water);
Potassium hydroxide solution: (200g/L);
Potassium sulfate solution: (100g/L);
Calcein mixed indicator: take the potassium chloride porphyrize mixing after calcein 1g, alizarin 1g and 100g oven dry;
EDTA concentration of standard solution (0.007mol/L)
4. sample size
Take sample 0.2500g.
5. analytical procedure
Take 0.2500g Si-Ba alloy sample and (carry out blank test in company with sample) in 250mL polytetrafluoroethylene beaker, add nitric acid 10mL(density 1.42g/mL), drip about 8mL hydrofluorite (density 1.15g/mL) under shake to dissolve completely to sample, add perchloric acid 10mL (density 1.67g/mL), on low temp. electric hot plate, perchloric acid cigarette is emitted in heating, and be evaporated to dry, take off slightly cold.Add hydrochloric acid 10mL (density is that the hydrochloric acid of 1.19g/mL mixes with isopyknic water), heating makes salt dissolve, and takes off.(if any insolubles, need to filter, with rinsing residue to non-iron-ion and chlorion, filter paper and residue be placed in platinum crucible ashing, with sodium carbonate-boric acid mixed solvent melting, decompose completely and leach in filtrate).Solution is transferred to 250mL volumetric flask, with water dilution scale, shakes up.
Divide and get 50mL filtrate in 250mL beaker, add water 50mL, add 0.2g oxammonium hydrochloride (solid), 5mL triethanolamine (volume ratio of triethanolamine and water is 1:4), 10 mL potassium sulfate solutions (100g/L), place 10 minutes, add 40mL potassium hydroxide (200g/L), add a little calcein mixed indicator, it is orange red for terminal for being titrated to solution with EDTA standard solution (0.007mol/L), and its EDTA consumption is V
ca; Divide and get 50mL filtrate in 250mL beaker, add water 50mL, add 0.2g oxammonium hydrochloride (solid), 5mL triethanolamine (volume ratio of triethanolamine and water is 1:4), add 40mL potassium hydroxide (200g/L), add a little calcein mixed indicator, it is orange red for terminal for being titrated to solution with EDTA standard solution (0.007mol/L), and its EDTA consumption is V
(Ca+Ba).
6. Analysis result calculation:
；
；
Wherein:
The concentration of c---EDTA standard solution, mol/L;
M---sample mass, g;
K---sample divides liquid proportional;
V
ca---in titration sample solution during calcium consume the volume of EDTA standard solution, mL;
V
ca+Ba---in titration sample solution when calcium, barium consume the volume of EDTA standard solution, mL;
V
01---in titration blank solution during calcium consume the volume of EDTA standard solution, mL;
V
02---in titration blank solution when calcium, barium consume the volume of EDTA standard solution, mL;
M
ca---the molal weight of calcium;
M
ba---the molal weight of barium.
7. sample analysis contrast
The measurement result (measured value) obtained by measuring method of the present invention differs less with standard value, illustrates and can realize calcium in Si-Ba alloy, barium translocation analysis fast and accurately by the method for complexometry.
8. conclusion
By this method, calcium in Si-Ba alloy, barium content can be determined fast and accurately.Avoid two kinds of methods molten sample respectively when measuring calcium barium two kinds of elements respectively, the trouble processed respectively.Save material consumption and manpower expenditure.Substantially increase the detection efficiency of chemical method, energy-conserving and environment-protective, be applicable to the express-analysis of gross sample.
Claims (3)
1. the method for calcium-barium content in a complexometry translocation Si-Ba alloy, it is characterized in that: sample is through the molten sample of nitrate acid and hydrofluoric acid, and perchloric acid smoked, is evaporated to dry, after dissolving with hydrochloric acid salt, get two parts of samples with after water constant volume point, after adding screening agent elimination interference element respectively, use calcein mixed indicator, titration is carried out as standard solution with EDTA, measure the content of calcium barium resultant and calcium respectively, difference subtracts the content calculating barium, and computing formula is as follows:
；
；
Wherein:
The concentration of c---EDTA standard solution, mol/L;
M---sample mass, g;
K---sample divides liquid proportional;
V
ca---in titration sample solution during calcium consume the volume of EDTA standard solution, mL;
V
ca+Ba---in titration sample solution when calcium, barium consume the volume of EDTA standard solution, mL;
V
01---in titration blank solution during calcium consume the volume of EDTA standard solution, mL;
V
02---in titration blank solution when calcium, barium consume the volume of EDTA standard solution, mL;
M
ca---the molal weight of calcium;
M
ba---the molal weight of barium.
2. the method for calcium-barium content in complexometry translocation Si-Ba alloy according to claim 1, it is characterized in that: described screening agent is triethanolamine solution, oxammonium hydrochloride, potassium sulfate solution and potassium hydroxide solution, or be triethanolamine solution, oxammonium hydrochloride and potassium hydroxide solution.
3. the method for calcium-barium content in complexometry translocation Si-Ba alloy according to claim 1, is characterized in that: the compound method of calcein mixed indicator be take calcein 1g, alizarin 1g and 100g dry after the mixing of potassium chloride porphyrize.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104807793A (en) * | 2015-04-29 | 2015-07-29 | 内蒙古包钢钢联股份有限公司 | Measuring method of calcium content in silicon-calcium wire |
| CN104820061A (en) * | 2015-04-29 | 2015-08-05 | 内蒙古包钢钢联股份有限公司 | Measuring method of calcium content in silicon-calcium-barium alloy |
| CN104819977A (en) * | 2015-04-29 | 2015-08-05 | 内蒙古包钢钢联股份有限公司 | Measuring method of calcium content in silicon-calcium alloy |
| CN104819908A (en) * | 2015-04-29 | 2015-08-05 | 内蒙古包钢钢联股份有限公司 | Continuous measuring method of calcium and barium content in silicon-calcium-barium and silicon-aluminum-calcium-barium alloy |
| CN104819978A (en) * | 2015-04-29 | 2015-08-05 | 内蒙古包钢钢联股份有限公司 | Measuring method of calcium content in silicon-aluminum-calcium-barium alloy |
| CN104833675A (en) * | 2015-05-20 | 2015-08-12 | 内蒙古包钢钢联股份有限公司 | Determination method of content of calcium oxide in iron ore |
| CN104833769A (en) * | 2015-05-20 | 2015-08-12 | 内蒙古包钢钢联股份有限公司 | Determination method of calcium oxide content in open-hearth slag, converter slag and electro-furnace slag |
| CN104964976A (en) * | 2015-06-12 | 2015-10-07 | 内蒙古包钢钢联股份有限公司 | Method of measuring calcium hydroxide content in slaked lime |
| CN105092569A (en) * | 2015-08-21 | 2015-11-25 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of calcium hydroxide in carbide slag |
| CN105158405A (en) * | 2015-08-21 | 2015-12-16 | 内蒙古包钢钢联股份有限公司 | Method for continuously determining content of calcium oxide and magnesium oxide in bentonite |
| CN109596611A (en) * | 2019-01-21 | 2019-04-09 | 湖北紫荆生物技术有限公司 | A kind of water body calcium content test agent and water body calcium content measurement method |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104807793A (en) * | 2015-04-29 | 2015-07-29 | 内蒙古包钢钢联股份有限公司 | Measuring method of calcium content in silicon-calcium wire |
| CN104820061A (en) * | 2015-04-29 | 2015-08-05 | 内蒙古包钢钢联股份有限公司 | Measuring method of calcium content in silicon-calcium-barium alloy |
| CN104819977A (en) * | 2015-04-29 | 2015-08-05 | 内蒙古包钢钢联股份有限公司 | Measuring method of calcium content in silicon-calcium alloy |
| CN104819908A (en) * | 2015-04-29 | 2015-08-05 | 内蒙古包钢钢联股份有限公司 | Continuous measuring method of calcium and barium content in silicon-calcium-barium and silicon-aluminum-calcium-barium alloy |
| CN104819978A (en) * | 2015-04-29 | 2015-08-05 | 内蒙古包钢钢联股份有限公司 | Measuring method of calcium content in silicon-aluminum-calcium-barium alloy |
| CN104833675A (en) * | 2015-05-20 | 2015-08-12 | 内蒙古包钢钢联股份有限公司 | Determination method of content of calcium oxide in iron ore |
| CN104833769A (en) * | 2015-05-20 | 2015-08-12 | 内蒙古包钢钢联股份有限公司 | Determination method of calcium oxide content in open-hearth slag, converter slag and electro-furnace slag |
| CN104964976A (en) * | 2015-06-12 | 2015-10-07 | 内蒙古包钢钢联股份有限公司 | Method of measuring calcium hydroxide content in slaked lime |
| CN105092569A (en) * | 2015-08-21 | 2015-11-25 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of calcium hydroxide in carbide slag |
| CN105158405A (en) * | 2015-08-21 | 2015-12-16 | 内蒙古包钢钢联股份有限公司 | Method for continuously determining content of calcium oxide and magnesium oxide in bentonite |
| CN105092569B (en) * | 2015-08-21 | 2019-06-04 | 内蒙古包钢钢联股份有限公司 | The measuring method of calcium hydroxide content in carbide slag |
| CN109596611A (en) * | 2019-01-21 | 2019-04-09 | 湖北紫荆生物技术有限公司 | A kind of water body calcium content test agent and water body calcium content measurement method |
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