CN104819908A - Continuous measuring method of calcium and barium content in silicon-calcium-barium and silicon-aluminum-calcium-barium alloy - Google Patents
Continuous measuring method of calcium and barium content in silicon-calcium-barium and silicon-aluminum-calcium-barium alloy Download PDFInfo
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Abstract
The invention discloses a continuous measuring method of calcium and barium content in silicon-calcium-barium and silicon-aluminum-calcium-barium alloy. The method includes: a silicon-calcium-barium or silicon-aluminum-calcium-barium alloy sample with the mass of m is added into a beaker, another beaker without the silicon-calcium-barium or silicon-aluminum-calcium-barium alloy sample serves as blank control, nitric acid-hydrofluoric acid mixture is respectively added into the two beakers to dissolve the sample, sulfuric acid is added until smoke is generated, hydrochloric acid dissolving salts are respectively added when the sample is in a wet salt state, water and hydroxylamine hydrochloride are added, heating is performed until yellow solution becomes colorless, the solution is filtered and placed into a large-capacity bottle, sediments are washed by dilute sulfuric acid and water, the sediments and filter paper are placed into a ceramic crucible, ashing, burning and weighing are performed, the mass of barium sulfate obtained from the sample and the blank is respectively m1 and m2, and barium content is achieved; volumetric solutions are taken from constant-volume solutions and respectively added into beakers, triethanolamine, water, hydroxylamine hydrochloride and potassium hydroxide solution are respectively sequentially added into the beakers, a few drops of magnesium sulfate are added, appropriate amount of calcein indicator is added, EDTA standard solution with concentration of C is used for titration until fluorescent green disappears, the volume is respectively recorded as V and V0, and calcium content is achieved.
Description
Technical field
The invention belongs to ferroalloy analysis field, be specifically related to the method for continuously measuring of calcium, barium content in a kind of volumetric determination Si-Ca-Ba, silicon aluminum calcium barium alloy.
Background technology
Calsibar alloy is new high-efficiency composite alloy in barium system alloy, is deoxidizer, the desulfurizing agent of practicing steel, also has dephosphorization (BaP concurrently
2, BaP
3) effect: be the inovulant in casting and alterant.
Si-Ca-Ba is good deoxidizer and desulfurizing agent, silicon in deoxidation process, calcium, and barium three kinds of elements promote mutually, effectively improve utilization factor.It is minimum that Si-Ca-Ba can make oxygen content in steel drop to, silicon, calcium, and the recovery of barium is higher than the recovery rate of other alloy.Other complex oxides of formation can be made easily to float from molten steel, the multiple molten steel of purification, improves impact flexibility and the processing characteristics of steel simultaneously.Barium effectively reduces the vapor pressure of calcium in steel-making temperature range, increase the solubleness of calcium in molten steel, compare with calcium-silicon, add in slag with alloy as calcium source, add in molten steel as calcium source with calsibar alloy, even a half of the calcium amount calcium-silicon addition added, the calcium content in molten steel is but about the twice of calcium-silicon, the recovery of calcium is apparently higher than calcium-silicon, and in molten steel, the stability of calcium also significantly improves.This illustrates that barium effectively protects volatilization and the oxidation that calcium decreases calcium in slag, thus reaches the object to molten steel process, and it has following characteristics: 1: deoxidizing capacity is strong, and fluidity molten steel well thoroughly solves the dross problem of continous casting sprue; 2: significantly improve silicon, the recovery of manganese etc. and minimizing carbon dust addition; 3: desulfurized effect is obvious, shorten the steel-making cycle; 4: applied widely, all or by technological requirement part can replace aluminum steel, Si-Al-Ba alloy, ferro-silico aluminium, deoxidation material in the steel-making such as silicon-calcium wire, reduces deoxidation cost.Therefore the Accurate Determining carrying out calcium and barium in Si-Ca-Ba, silicon aluminum calcium barium alloy is significant.
The method large enterprise measuring calcium and barium 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 calcium and barium major part adopt assay method respectively, consuming time, waste material.Calcium catalyst major part ammoniacal liquor is separated interference element, operates more loaded down with trivial details, time-consuming.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method for continuously measuring measuring calcium in Si-Ca-Ba, silicon aluminum calcium barium alloy, barium content more fast, accurately and efficiently.
For reaching above-mentioned purpose, the method for continuously measuring of calcium, barium content in a kind of Si-Ca-Ba of the present invention, silicon aluminum calcium barium alloy, comprises the following steps:
The Si-Ca-Ba or silicon aluminum calcium barium alloy sample that quality is m is added polytetrafluoroethylene beaker one, another does not add as blank, add nitrate acid and hydrofluoric acid mixed liquor respectively afterwards, dissolved samples on low temp. electric hot plate, after sample dissolves, add sulfuric acid respectively, continue to be heated to sulfuric acid to smolder, treat that sample is wet salt shape, take off, after cooling, add hydrochloric acid heating for dissolving salt respectively, to add water and hydroxylammonium chloride heating are boiled to solution and become colorless by yellow, take off, place, use filter paper at a slow speed afterwards, filter in Large Copacity bottle, precipitation dilute sulfuric acid dip 6-8 time, then 9-10 time is washed with water, precipitation is put into porcelain crucible together with filter paper, ashing, calcination, weigh, sample and the blank quality m obtaining barium sulphate respectively
1and m
2, barium content is: W
ba%=100 (m
1-m
2) 0.5884/m,
In formula: m
1: barium sulphate quality, g;
M
2: blank quality, g;
M: sample mass, g;
After constant volume solution, divide and get volumetric soiutions in beaker, add triethanolamine, water, oxammonium hydrochloride successively respectively, hydro-oxidation potassium solution keeps pH to be not less than 12, add several magnesium sulfate, calcein indicator is appropriate, and being titrated to fluorescence green disappearance with the EDTA standard solution that concentration is C is terminal, and 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 on low temp. electric hot plate at 100 DEG C dissolved samples.
Wherein said sulfuric acid concentration is 5%.
Wherein said dilute sulfuric acid concentration is 1%.
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 mensuration calcium adopts triethanolamine to shelter interference element and is separated interference element twice with ammoniacal liquor, and both measurement results are the same.Barium adopts gravimetric method, and 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: the Si-Ca-Ba adopting nitric acid (67%)-hydrofluorite (40%) to dissolve in vinyon beaker or silicon aluminum calcium barium alloy sample, add sulfuric acid to smolder wet salt shape, take off, after cooling, 5mL hydrochloric acid (65%) is carefully added, heating for dissolving salt along wall of cup.Test solution is added 150mL water, add a little hydroxylammonium chloride (this step is for sheltering iron) heating and boil and become colorless by yellow to solution, take off, place 1 hour, with filter paper at a slow speed, (add feet, barium sulphate is crystalline precipitate, particle is very thin, and not adding feet can wear filter, affects the measurement result of barium.) filter in 250mL volumetric flask, precipitation is washed 6-8 time with 1% sulfuric acid, then washes 9-10 time with water, precipitation is put into porcelain crucible together with filter paper, ashing, calcination, weigh.Obtain barium sulphate quality; Filtrate is diluted to scale constant volume, from the 250mL solution after constant volume, divides and get 50mL solution in 250mL beaker, add 50mL triethanolamine (12%), add 50mL water, add oxammonium hydrochloride a little (further masking action, addition general about 0.5 gram both passable.), (be 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%).), (titration end-point is sharp, and terminal is good-looking to add several magnesium sulfate (0.5%).), calcein indicator 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 sulfuric acid (5%) (1%)
2.4 hydrochloric acid (65%)
2.5 oxammonium hydrochlorides (solid)
2.6 triethanolamines (12%)
2.7 potassium hydroxide 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 Si-Ca-Ba or Si-Al-Ca-Ba sample m0.2500g in polytetrafluoroethylene beaker, add 10mL nitric acid (67%), add 10mL hydrofluorite (40%), at the upper dissolved samples of low temp. electric hot plate (100 DEG C), after sample dissolves, add 20mL sulfuric acid (5%), continue to be heated to sulfuric acid to smolder, test solution is wet salt shape, and (this walks key, test solution is that wet salt shape just takes off, the not too long time, otherwise, form indissoluble pyrosulfuric acid calcium and pyrosulfuric acid barium, to next step with dissolving with hydrochloric acid not, affect measurement result.) take off, after cooling, carefully add 5mL hydrochloric acid (65%) along wall of cup, heating for dissolving salt.Test solution is added 150mL water, add a little hydroxylammonium chloride (solid) (this step for sheltering iron) heating to boil to solution and become colorless by yellow, take off, place 1 hour, with filter paper at a slow speed, (add feet, barium sulphate is crystalline precipitate, and particle is very thin, do not add feet and can wear filter, affect the measurement result of barium.) filter in 250mL volumetric flask, precipitation is washed 6-8 time with 1% sulfuric acid, and then wash 9-10 time with water, precipitation is put into porcelain crucible together with filter paper, in muffle furnace 600 DEG C of ashing, 800-850 DEG C of calcination, weighs.Obtain the content m of barium sulphate
1.Filtrate is 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 30mL potassium hydroxide solution (20%), add several magnesium sulfate (0.5%), calcein indicator is appropriate, and be titrated to fluorescence green with 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%), at the upper dissolved samples of low temp. electric hot plate (100 DEG C), after sample dissolves, add 20mL sulfuric acid (5%), continue to be heated to sulfuric acid and smolder, test solution is wet salt shape, take off, after cooling, carefully add 5mL hydrochloric acid (65%) along wall of cup, heating for dissolving salt.Test solution is added 150mL water, add a little hydroxylammonium chloride (solid), heating is boiled, take off, place 1 hour, (add feet with filter paper at a slow speed, the same with sample, consistent blank can be controlled) to filter in 250mL volumetric flask, precipitation is washed 6-8 time with 1% sulfuric acid, then washes 9-10 time with water, precipitation is put into porcelain crucible together with filter paper, in muffle furnace 600 DEG C of ashing, 800-850 DEG C of calcination, weighs.The content m obtained
2.Filtrate 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, be titrated to fluorescence green with C (EDTA)=0.01783mol/L standard solution to disappear for terminal, 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; 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 (mL) of EDTA standard solution;
V
0: the blank volume (mL) consuming EDTA standard solution;
W(Ba)％＝100(m
1-m
2)0.5884/m；
M
1: barium sulphate quality (g);
M
2: blank quality (g);
M: sample mass (g);
0.5884: barium sulphate is converted into the reduction coefficient of barium;
7. standard specimen analysis of control:
The comparison of calcium:
As can be seen from the above table: the data that calcium content gained in data and the ammoniacal liquor twice separation determination calsibar alloy measuring calcium content gained in Si-Ca-Ba, silicon aluminum calcium barium alloy directly sheltered by use triethanolamine are the same, and accurately, and operating process is short, fast, efficient.
The accuracy of barium:
As can be seen from the above table: measurement result is accurate, and operating process is short, fast, efficient.
8. conclusion:
By this method, METHOD FOR CONTINUOUS DETERMINATION calcium and barium content in Si-Ca-Ba, silicon aluminum calcium barium alloy can be gone out accurately.Substantially reduce the running time, reduce energy consumption.Make determination data accurately and reliably, application obtains good effect aborning.
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 (8)
1. the method for continuously measuring of calcium, barium content in Si-Ca-Ba, silicon aluminum calcium barium alloy, is characterized in that comprising the following steps:
The Si-Ca-Ba or silicon aluminum calcium barium alloy sample that quality is m is added polytetrafluoroethylene beaker one, another does not add as blank, add nitrate acid and hydrofluoric acid mixed liquor respectively afterwards, dissolved samples on low temp. electric hot plate, after sample dissolves, add sulfuric acid respectively, continue to be heated to sulfuric acid to smolder, treat that sample is wet salt shape, take off, after cooling, add hydrochloric acid heating for dissolving salt respectively, to add water and hydroxylammonium chloride heating are boiled to solution and become colorless by yellow, take off, place, use filter paper at a slow speed afterwards, filter in Large Copacity bottle, precipitation dilute sulfuric acid dip 6-8 time, then 9-10 time is washed with water, precipitation is put into porcelain crucible together with filter paper, ashing, calcination, weigh, sample and the blank quality m obtaining barium sulphate respectively
1and m
2, barium content is: W
ba%=100 (m
1-m
2) 0.5884/m,
In formula: m
1: barium sulphate quality, g;
M
2: blank quality, g;
M: sample mass, g;
After constant volume solution, divide and get volumetric soiutions in beaker, add triethanolamine, water, oxammonium hydrochloride successively respectively, hydro-oxidation potassium solution keeps pH to be not less than 12, add several magnesium sulfate, calcein indicator is appropriate, and being titrated to fluorescence green disappearance with the EDTA standard solution that concentration is C is terminal, and 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 calsibar alloy 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 calsibar alloy according to claim 1, is characterized in that: on low temp. electric hot plate at 100 DEG C dissolved samples.
4. the assay method of calcium content in calsibar alloy according to claim 1, is characterized in that: described sulfuric acid concentration is 5%.
5. the assay method of calcium content in calsibar alloy according to claim 1, is characterized in that: described dilute sulfuric acid concentration is 1%.
6. the assay method of calcium content in calsibar alloy according to claim 1, is characterized in that: described concentration of hydrochloric acid is 65%.
7. the assay method of calcium content in calsibar alloy according to claim 1, is characterized in that: described triethanolamine concentrations is 12%.
8. the assay method of calcium content in calsibar alloy according to claim 1, is characterized in that: described concentration of potassium hydroxide is 20%.
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| CN105651931A (en) * | 2016-02-26 | 2016-06-08 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of calcium oxide and magnesium oxide in refined slag |
| CN105738559A (en) * | 2016-02-26 | 2016-07-06 | 内蒙古包钢钢联股份有限公司 | Method for measuring calcium oxide and magnesium oxide content of tundish covering agent |
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| CN109270210A (en) * | 2018-10-10 | 2019-01-25 | 新兴铸管股份有限公司 | The method of barium content in barium sulfate precipitate-EDTA volumetric determination Si-Al-Ba alloy and Si-Ca-Ba |
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| CN108593488A (en) * | 2018-05-15 | 2018-09-28 | 沈阳铸造研究所有限公司 | The joint measurement method of silicon, aluminium and calcium element content in a kind of Alsical |
| CN109030275A (en) * | 2018-09-11 | 2018-12-18 | 芜湖新兴铸管有限责任公司 | Seamless pure calcium line calcic measuring method |
| CN109270210A (en) * | 2018-10-10 | 2019-01-25 | 新兴铸管股份有限公司 | The method of barium content in barium sulfate precipitate-EDTA volumetric determination Si-Al-Ba alloy and Si-Ca-Ba |
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Application publication date: 20150805 |