CN104807793A - Measuring method of calcium content in silicon-calcium wire - Google Patents
Measuring method of calcium content in silicon-calcium wire Download PDFInfo
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- CN104807793A CN104807793A CN201510210218.4A CN201510210218A CN104807793A CN 104807793 A CN104807793 A CN 104807793A CN 201510210218 A CN201510210218 A CN 201510210218A CN 104807793 A CN104807793 A CN 104807793A
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Abstract
The invention discloses a measuring method of a calcium content in a silicon-calcium wire. The method comprises the steps of adding a silicon-calcium wire sample with mass of m into a polytetrafluoroethylene beaker, taking another polytetrafluoroethylene beaker without a sample as a blank control, then adding a nitric acid-hydrofluoric acid mixed solution to dissolve the sample, adding perchloric acid after the sample is dissolved, continuing to heat till sulfuric acid smokes, adding hydrochloric acid and heating to dissolve salt after no smoke emits and a test solution is dry and cooled, transferring the test solution to a high-capacity bottle, diluting to a scale for constant volume, taking a certain amount of solution from the solution after the constant volume into the beakers, sequentially adding triethanolamine, water and hydroxylamine hydrochloride, adding a potassium hydroxide solution to keep pH (potential of hydrogen) to be not less than 12, adding a plurality of drops of magnesium sulfate and an appropriate amount of calcein indicator, titrating with an EDTA (Ethylene Diamine Tetraacetic Acid) standard solution with a concentration of C till fluorescent green disappears as an end point, recording the volumes as V and V0, and obtaining the calcium content as follows: W<Ca>% is equal to C(V-V0)M<Ca>100/mK*100.
Description
Technical field
The present invention relates to ferroalloy analysis field, be specifically related to the assay method of calcium content in a kind of volumetric determination silicon-calcium wire.
Background technology
Because the oxygen in calcium and molten steel, nitrogen, hydrogen, sulphur and carbon etc. have stronger affinity, so calcium-silicon is mainly used in the deoxidation of molten steel, degasification and fixed carbon.Silico-calcium produces strong exothermic effect after adding molten steel.Calcium becomes calcium steam in molten steel, produces beating action to molten steel, floats favourable to nonmetal inclusion, after calcium-silicon deoxidation, produces particle comparatively large and be easy to the nonmetal inclusion that floats, also changes shape and the character of nonmetal inclusion simultaneously.Calcium-silicon for the production of clean steel, oxygen, low-sulfur content high-quality steel.And oxygen, the special low property steel of sulphur.Add calcium-silicon and can eliminate the dross of steel at ladle nozzle making end-deoxidizer with aluminium, and the problem such as the middle pot drainage opening blocking of continuous casting steel machine.In the furnace outer refining technology of steel, carry out deoxidation, desulfurization with silico-calcium pulvis or heart yearn, the content of oxygen and sulphur in steel is reduced to very low, also can control steel medium sulphide content form, improve the utilization factor of calcium simultaneously.In Cast Iron Production, calcium-silicon, except deoxidation and clean-up effect, also plays inoculation(effect), contributes to forming particulate or globular graphite, makes Graphite Distribution in grey cast iron even, reduces chilling tendency, and can increase silicon, desulfurization, improves improving cast iron quality.Therefore the Accurate Determining carrying out calcium in silicon-calcium wire is significant.
The method large enterprise measuring calcium adopts large-scale instrument analysis mostly, but cost is high, and for small business, chemical analysis method embodies its advantage more, namely convenient, fast.Chemical analysis major part ammoniacal liquor is separated interference element, operates more loaded down with trivial details, time-consuming.
Summary of the invention
The object of the invention is to formulate a kind of operating process short, cost is low, and fast, efficient, accurately, good stability, is easy to the method for calcium content in the mensuration silicon-calcium wire grasped.Solve the mensuration of calcium content in silicon-calcium wire without standard determination method problem.
For reaching above-mentioned purpose, the assay method of calcium content in a kind of silicon-calcium wire of the present invention, its following steps:
The silicon-calcium wire sample that quality is m is added polytetrafluoroethylene beaker one, another does not add as blank, add nitrate acid and hydrofluoric acid mixed liquor dissolved samples afterwards respectively, after sample dissolves, add perchloric acid respectively, continue to be heated to perchloric acid smoked, cigarette emits only, test solution dries up, after cooling, add hydrochloric acid heating for dissolving salt respectively, respectively test solution is transferred in Large Copacity bottle, be diluted to scale constant volume, after constant volume solution, divide and get volumetric soiutions in beaker, add triethanolamine successively respectively, water, oxammonium hydrochloride, hydro-oxidation potassium solution keeps pH to be not less than 12, add several magnesium sulfate, calcein indicator is appropriate, being titrated to fluorescence green disappearance with the EDTA standard solution that concentration is C is terminal, meter lower volume is for being respectively V and V
0, obtaining calcium content is: W
ca%=C (V-V
0) M
ca100/m K × 100,
In formula: M
ca: the molal weight of calcium, g/mol;
M: sample mass, g;
K: sample divides liquor ratio, the volumetric flask volume of the Large Copacity bottle of the volumetric soiutions got after K=/transfer to;
C:EDTA concentration of standard solution, mol/L;
V: sample consumes the volume of EDTA standard solution, mL;
V
0: the blank volume consuming EDTA standard solution, mL.
Wherein said nitric acid and described hydrofluorite volumetric usage are 1:1, and concentration is respectively 67% and 40%.
Wherein said perchloric acid concentration is 70%.
Wherein said concentration of hydrochloric acid is 65%.
Wherein said triethanolamine concentrations is 12%.
Wherein said concentration of potassium hydroxide is 20%.
The invention difference from existing technology is that the present invention achieves following technique effect:
1) fast, efficiently, low cost: the method substantially reduces operating process, has saved medicine, has reduced testing cost, improve production efficiency;
2) accurately, stable: this method adopts triethanolamine to shelter interference element and is separated interference element twice with ammoniacal liquor, and both measurement results are the same.Ensure that measurement result is stablized, data are accurate.
Embodiment
Below in conjunction with embodiment, to above-mentioned being described in more detail with other technical characteristic and advantage of the present invention.
1. method summary: adopt nitric acid (67%)-hydrofluorite (40%) dissolves silicon calcium line sample in vinyon beaker, add 5mL perchloric acid (70%) to smolder, cigarette emits only, test solution dries up, after cooling, 10mL hydrochloric acid (65%) is carefully added, heating for dissolving salt along wall of cup.Test solution is transferred in 250mL volumetric flask, be diluted to scale constant volume, divide and get 50mL solution in 250mL beaker, add 50mL triethanolamine (12%), add 50mL water, add oxammonium hydrochloride a little (add the object of oxammonium hydrochloride, play further masking action equally, addition general about 0.5 gram both passable.), (as buffer solution, calcium and EDTA complexing require that pH value is greater than 12, add the pH value of potassium hydroxide (20%) guarantee system to add 30mL potassium hydroxide solution (20%).), (in order to titration end-point is sharp, terminal is good-looking to add several magnesium sulfate (0.5%).), calcein is appropriate, and being titrated to fluorescence green disappearance with EDTA standard solution is terminal.
2. reagent:
2.1 nitric acid (67%)
2.2 hydrofluorite (40%)
2.3 perchloric acid (70%)
2.4 hydrochloric acid (65%)
2.5 oxammonium hydrochlorides (solid)
2.6 triethanolamines (12%)
2.7 potassium hydroxide aqueous solutions (20%)
2.8 calcein indicator: 1g calcein and 100g dry after sodium chloride porphyrize mix, be placed in port grinding bottle for subsequent use.
2.9 EDTA standard solution C (EDTA)=0.01783mol/L
2.10 magnesium sulfate (0.5%)
3. sampling and sample preparation: get sample preparation standard according to ferroalloy and carry out sample and produce.
4. sample weighting amount: take sample 0.2500g
5. analytical procedure:
Take silicon-calcium wire sample 0.2500g in polytetrafluoroethylene beaker, add 10mL nitric acid (67%), add 10mL hydrofluorite (40%), add 5mL perchloric acid (70%), continue to be heated to perchloric acid smoked, perchloric acid cigarette emits only, cannot see one and lights a cigarette, after cooling, 10mL hydrochloric acid (65%) is carefully added along wall of cup, heating for dissolving salt, transfers to test solution in 250mL volumetric flask, is diluted to scale constant volume.From the 250mL solution after constant volume, divide and get 50mL solution in 250mL beaker, add 50mL triethanolamine (12%), add 50mL water, add oxammonium hydrochloride a little, add 30mL potassium hydroxide solution (20%), add several magnesium sulfate (0.5%), calcein indicator is appropriate, and be titrated to fluorescence green with concentration C (EDTA)=0.01783mol/L standard solution and disappear for terminal, meter lower volume is V.
Blank:
In polytetrafluoroethylene beaker, add 10mL nitric acid (67%), add 10mL hydrofluorite (40%), add 5mL perchloric acid (70%), continue to be heated to perchloric acid smoked, perchloric acid cigarette emits only, cannot see one and lights a cigarette, after cooling, 5mL hydrochloric acid (65%) is carefully added along wall of cup, heating for dissolving salt, transfers to test solution in 250mL volumetric flask, is diluted to scale constant volume.From the 250mL solution after constant volume, divide and get 50mL solution, in 250mL beaker, add 50mL triethanolamine (12%), add 50mL water, add oxammonium hydrochloride a little, add 30mL potassium hydroxide solution (20%), add several magnesium sulfate (0.5%), calcein indicator is appropriate, being titrated to fluorescence green disappearance with EDTA standard solution is terminal, and meter lower volume is V
0.
6. Analysis result calculation:
W(Ca)％＝C(V-V
0)M(Ca)100/m K×100
In formula: M (Ca): the molal weight (g/mol) of calcium
M: sample mass (g)
K: sample divides liquor ratio
C:EDTA concentration of standard solution (mol/L)
V: sample consumes the volume (mL) of EDTA standard solution
V
0: the blank volume (mL) consuming EDTA standard solution
7. standard specimen analysis of control: (because silicon-calcium wire does not have standard specimen, this method adopts calcium-silicon standard specimen to do the experiment of accuracy)
As can be seen from the above table: the data that calcium content gained in data and the ammoniacal liquor twice separation determination calcium-silicon measuring calcium content gained in calcium-silicon directly sheltered by use triethanolamine are the same, and accurately, and operating process is shorter, fast, efficient.
8. conclusion: the present invention establishes calcium content in silicon-calcium wire and carries out the assay method of quantitative test, can be applied in production preferably.Operating process is short, and cost is low, fast, accurately, efficiently, is easy to grasp.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (6)
1. the assay method of calcium content in silicon-calcium wire, is characterized in that comprising the following steps:
The silicon-calcium wire sample that quality is m is added polytetrafluoroethylene beaker one, another does not add as blank, add nitrate acid and hydrofluoric acid mixed liquor dissolved samples afterwards respectively, after sample dissolves, add perchloric acid respectively, continue to be heated to sulfuric acid to smolder, cigarette emits only, test solution dries up, after cooling, add hydrochloric acid heating for dissolving salt respectively, respectively test solution is transferred in Large Copacity bottle, be diluted to scale constant volume, after constant volume solution, divide and get volumetric soiutions in beaker, add triethanolamine successively respectively, water, oxammonium hydrochloride, hydro-oxidation potassium solution keeps pH to be not less than 12, add several magnesium sulfate, calcein indicator is appropriate, being titrated to fluorescence green disappearance with the EDTA standard solution that concentration is C is terminal, meter lower volume is for being respectively V and V
0, obtaining calcium content is: W
ca%=C (V-V
0) M
ca100/m K × 100,
In formula: M
ca: the molal weight of calcium, g/mol;
M: sample mass, g;
K: sample divides liquor ratio, the volumetric flask volume of the Large Copacity bottle of the volumetric soiutions got after K=/transfer to;
C:EDTA concentration of standard solution, mol/L;
V: sample consumes the volume of EDTA standard solution, mL;
V
0: the blank volume consuming EDTA standard solution, mL.
2. the assay method of calcium content in silicon-calcium wire according to claim 1, is characterized in that: described nitric acid and described hydrofluorite volumetric usage are 1:1, and concentration is respectively 67% and 40%.
3. the assay method of calcium content in silicon-calcium wire according to claim 1, is characterized in that: described perchloric acid concentration is 70%.
4. the assay method of calcium content in silicon-calcium wire according to claim 1, is characterized in that: described concentration of hydrochloric acid is 65%.
5. the assay method of calcium content in silicon-calcium wire according to claim 1, is characterized in that: described triethanolamine concentrations is 12%.
6. the assay method of calcium content in silicon-calcium wire according to claim 1, is characterized in that: described concentration of potassium hydroxide is 20%.
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Cited By (2)
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| CN105911049A (en) * | 2016-04-13 | 2016-08-31 | 内蒙古包钢钢联股份有限公司 | Method for determining calcium oxide in rare earth concentrate |
| CN114965862A (en) * | 2022-03-31 | 2022-08-30 | 山东鲁丽钢铁有限公司 | Method for measuring calcium content in calcium-aluminum alloy cored wire by EGTA titration method |
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| CN104483311A (en) * | 2014-12-10 | 2015-04-01 | 内蒙古包钢钢联股份有限公司 | Indicator for simultaneous measurement of calcium, barium and magnesium in silicon-calcium-barium-magnesium by adopting EDTA titration method |
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| CN101344489A (en) * | 2008-09-02 | 2009-01-14 | 武汉钢铁(集团)公司 | Method for measuring calcium constituent in silicon aluminum calcium barium alloy |
| CN104458731A (en) * | 2014-12-10 | 2015-03-25 | 内蒙古包钢钢联股份有限公司 | Method for joint measurement of calcium-barium content of silicon-barium alloy by using compleximetry |
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Cited By (2)
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| CN105911049A (en) * | 2016-04-13 | 2016-08-31 | 内蒙古包钢钢联股份有限公司 | Method for determining calcium oxide in rare earth concentrate |
| CN114965862A (en) * | 2022-03-31 | 2022-08-30 | 山东鲁丽钢铁有限公司 | Method for measuring calcium content in calcium-aluminum alloy cored wire by EGTA titration method |
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Application publication date: 20150729 |