CN103439324A - Method for rapidly measuring iron content in continuous casting mold fluxes - Google Patents
Method for rapidly measuring iron content in continuous casting mold fluxes Download PDFInfo
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- CN103439324A CN103439324A CN2013103504725A CN201310350472A CN103439324A CN 103439324 A CN103439324 A CN 103439324A CN 2013103504725 A CN2013103504725 A CN 2013103504725A CN 201310350472 A CN201310350472 A CN 201310350472A CN 103439324 A CN103439324 A CN 103439324A
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Abstract
The invention discloses a method for rapidly measuring iron content in continuous casting mold fluxes. The method comprises the following steps; 1, preparing a mold flux sample solution; 2, preparing an iron standard solution; 3, drawing a standard curve; 4, measuring iron content in the sample solution; 5, calculating the iron content in the mold fluxes, wherein a mixed color developing solution in the steps 3 and 4 is formed by mixing ascorbic acid, hydroxylamine hydrochloride, an orthophenanthrolene solution and an acetic acid-sodium acetate buffer solution. According to the color developing solution, the ascorbic acid, the hydroxylamine hydrochloride, the orthophenanthrolene solution and the acetic acid-sodium acetate buffer solution can be added together, so that the problem of incomplete color development or incapability of color development in the prior art due to the problem of sequence of adding reagents, is avoided, the detection step is simplified, and the method has the advantages of flexibility, simplicity for operation and high analysis speed; an ascorbic acid and hydroxylamine hydrochloride mixed reducing agent with excellent performance is formed by the ascorbic acid and the hydroxylamine hydrochloride in the color developing solution, so that the reduction reaction is rapid and stable, and the precision of a detection result is effectively improved.
Description
Technical field
The present invention relates to metallurgical technology, refer to particularly the rapid assay methods of iron content in a kind of continuous casting covering slag.
Background technology
Continuous casting covering slag, be important functional material during continuous casting is produced, and it is as interactional medium between crystallizer and strand, carrying out smoothly and improving the slab quality impact significantly continuous casting process.In covering slag, ferro element is mainly with Fe
2o
3form exist, the size of iron content can be to viscosity, the fusing point of covering slag, and Crystalline equates that physicochemical property exert an influence, therefore, the iron content in the Accurate Determining covering slag is significant to instructing continuous casting to produce.
At present, the common assay method of continuous casting covering slag iron content has x-ray fluorescence method (XRF), inductively coupled plasma emission spectrography (ICP-AES), and the phenanthrolene spectrophotometric method etc., all there is certain deficiency in these method of testings.Wherein, because the covering slag sample has the keeping quality of being difficult for, the X-fluorescence method lacks has card covering slag standard model to set up calibration curve, can only select the standard models such as blast furnace slag that character is close, vessel slag to set up working curve, thereby affect the accuracy of result, in addition, as pertinent literature (Jiang Yanan, Yang Guang, field Wei .ICP-OES method is measured the oxide content [J] of iron, aluminium, magnesium in covering slag. Hebei Metallurgy, 2013,205, the ICP-AES method of utilizing of introducing 62-63) is measured the method for iron content in covering slag, the method adopts the molten sample of alkali fusion method, need to add the mixed flux coupling of equivalent in working curve, detect and be limited to 0.012mg/L, the relative standard is 1.26%, though can complete the mensuration of multielement simultaneously, the instrument costliness, and method is difficult for promoting, and phenanthrolene method spectrophotometric method is the assay method of iron content in the continuous casting covering slag of stipulating in existing iron and steel industry industry standard YB/T190-2001 (continuous casting covering slag chemical analysis method), the method is in acetic acid-sodium acetate buffering, ferrous ion and phenanthrolene generate orange red complex compound, measure solution absorbance in the 510nm place with spectrophotometer, the Mass Calculation iron content checked according to typical curve, yet the method need to first add the reductive agent ascorbic acid that the ferric iron in sample is reduced into to ferrous iron when colour developing, then regulate acidity with buffer solution, finally add the phenanthrolene colour developing, the test solution addition sequence can not be changed, otherwise will cause colour developing not exclusively maybe can't develop the color, caused operational inconvenience and minute long.
Summary of the invention
Purpose of the present invention is exactly the rapid assay methods that iron content in a kind of continuous casting covering slag will be provided, and the method can be quick, easy and measure exactly the iron content in covering slag.
For achieving the above object, the technical solution used in the present invention is: the rapid assay methods of iron content in a kind of continuous casting covering slag, the method comprises the steps:
1) prepare the covering slag sample solution: be at first m by quality
0covering slag is hydrochloric acid, hydrofluorite for sample, and after nitric acid dissolve with perchloric acid smoked near dry, then with dissolving with hydrochloric acid, leach salt, dilute after being cooled to room temperature, after filtering, to make volume be V to constant volume
0sample solution;
2) preparation iron standard solution: at first by Fe
2o
3calcination and be cooled to room temperature after, add hydrochloric acid and water, carry out heating for dissolving, obtain iron standard stock solution, then will iron standard stock solution obtain the iron standard solution after dilution;
3) drawing standard curve: the one group of iron standard solution that pipettes different volumes, add the mixing nitrite ion of equivalent after dilute with water in each iron standard solution, then make one group of isopyknic standard solution after the water constant volume, and establish blank sample, be the absorbance that each standard solution and blank sample detect in the 510nm place with spectrophotometer at wavelength, thereby draw out " typical curve of weight of iron (m)-absorbance (A) "; Wherein, described mixing nitrite ion is by ascorbic acid, oxammonium hydrochloride, phenanthrolene solution, and acetic acid-sodium acetate buffer solution mixes;
4) measure the iron content in sample solution: pipetting volume is V
1sample solution, add the nitrite ion that mixes with step 3) standard sample moderate after dilute with water, then water is settled to and the standard sample equal-volume; The absorbance that is 510nm place test samples solution at wavelength with spectrophotometer, finding iron content from typical curve is m
1;
5) calculate the iron content W in covering slag
fe: by the cumulative volume V of sample solution
0, volume V is got in dividing of sample solution
1, covering slag sample mass m
0, and the iron content m1 data that check in from typical curve can calculate the iron content W in covering slag
fe.
In described step 3), the oxammonium hydrochloride that the ascorbic acid that described mixing nitrite ion is 10g/L by concentration, concentration are 10g/L, concentration are 10g/L phenanthrolene solution, and acetic acid-sodium acetate buffer solution of 1mol/L be take volume ratio and mixed as 1: 0.5～2: 1～4: 18～24.
In described step 3), described phenanthrolene solution is dissolved in 1 volume ethanol by the phenanthrolene powder, then is diluted with water to 5 volumes formulated.
In described step 3), described acetic acid-sodium acetate buffer solution is dissolved in 300mL water according to the 136g sodium acetate trihydrate, then adds the 57mL glacial acetic acid, and the ratio that is diluted with water to 1000mL is formulated.
Described step 1) in; the hydrochloric acid that is 36%～38% with mass percent concentration; the hydrofluorite that mass percent concentration is 40%～47%; the nitric acid that mass percent concentration is 65%～68%, and the mass percent concentration perchloric acid that is 70%～72% is to add dissolve covering slag sample at 10～30: 3～10: 5～20: 3～10 by volume.
Compared with prior art, the present invention has following advantage:
One, ascorbic acid in the present invention's mixing nitrite ion and oxammonium hydrochloride form well behaved ascorbic acid-oxammonium hydrochloride mixing reductive agent, wherein, ascorbic acid is the medium tenacity reductive agent, its electrode potential is+0.30V, the oxammonium hydrochloride electrode potential is+0.42V, compared better stability with other reductive agents, use ascorbic acid-oxammonium hydrochloride mixing reductive agent, make the reduction reaction fast and stable, both can guarantee the ferric iron reduction thoroughly, can avoid again ascorbic acid that other high valence ions in covering slag are reduced to divalence, effectively improved the accuracy of testing result.
They are two years old, ascorbic acid, oxammonium hydrochloride, phenanthrolene and acetic acid-sodium acetate buffer solution are mixed with to the mixing nitrite ion, once add, avoided the problem that not exclusively maybe can't develop the color because of the colour developing that successively problem causes of reagent addition sequence in the prior art, simplified detecting step, there is sensitivity and degree of accuracy is high, simple to operate, the advantage analyze fast, equipment cost is low.
The accompanying drawing explanation
The weight of iron that Fig. 1 is embodiment 1～3 (m)-absorbance (A) typical curve.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated, but the present invention is not limited to following embodiment.
Hydrochloric acid, hydrofluorite, nitric acid for dissolving the covering slag sample in following examples, and perchloric acid is commercially available concentration, wherein, the mass percent concentration of hydrochloric acid is 36%～38%, the mass percent concentration of hydrofluorite is 40%～47%, the mass percent concentration of nitric acid is 65%～68%, and the mass percent concentration of perchloric acid is 70%～72%; The pH of acetic acid-sodium acetate buffer solution of preparing in following examples preferably 4～5.
Embodiment 1:
Adopt Wuhan Iron & Steel's the second steel plant continuous casting production technology continuous casting covering slag used as sample.
1) at first, take quality m
0the covering slag of=0.1000g, be placed in the 300mL polytetrafluoroethylene beaker, with after a small amount of water-wet, adds 10mL hydrochloric acid, 3mL hydrofluorite, 5mL nitric acid, low-temperature heat 30min; Then add 3mL perchloric acid, low-temperature heat, to emitting the perchloric acid cigarette, continues heating and smolders near dry; After cooling, add altogether 10mL hydrochloric acid by 9mL after first 1mL, rinse wall of cup with a small amount of water, heating 5min dissolved salts (is controlled the hydrochloric acid consumption that dissolves the leaching salt, make the content of concentrated hydrochloric acid in solution be no more than the number percent 2% of constant volume), after being cooled to room temperature, use Filter Paper Dry filtered sample solution at a slow speed, sample solution is settled to V
0=50mL;
2) by calcination in advance and be cooled to the 0.3574g Fe of room temperature
2o
3be placed in beaker, add the hydrochloric acid that 1～2mL mass percent concentration is 36%～38%, be cooled to room temperature after heating for dissolving, transfer in volumetric flask, with deionized water be diluted to scale and mix after obtain iron standard stock solution, by the dilution of iron standard stock solution, prepare the iron standard solution of 100 μ g/mL;
3) pipette respectively 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL iron standard solution (100 μ g/mL) is divided in the 100mL volumetric flask, and with deionized water, blank sample is set, respectively add 15mL mixing nitrite ion, be diluted with water to scale and mix, after room temperature is placed 15min, by standard solution and blank sample, moving respectively in thickness is in the 3cm absorption vessel, with spectrophotometer, at wavelength, is the absorbance A that the 510nm place surveys each standard solution and blank sample, and data are as table 1.The quality of iron in each standard solution and blank sample of take is horizontal ordinate, and take each standard solution of recording and the absorbance of blank sample is ordinate drawing standard curve, and typical curve is as shown in a line in Fig. 1, and the linear dependence degree is 0.9999.
4) divide and get V
1=20.00mL sample solution is in the 50mL volumetric flask, add 15mL mixing nitrite ion, be diluted with water to scale and mix, after room temperature is placed 15min, getting part, to add the sample solution mixed after nitrite ion to move into thickness be in the 3cm absorption vessel, and take deionized water and blank sample is set as reference, with spectrophotometer, at wavelength, be that the absorbance A that the 510nm place records sample solution is 0.1803;
Above-mentioned steps 3) and 4) in the mixing nitrite ion used by 1 volume ascorbic acid, 1 volume oxammonium hydrochloride, 2 volume phenanthrolene solution, and acetic acid-sodium acetate buffer solution of 20 volume 1mol/L mixes, wherein, the concentration of ascorbic acid is 10g/L; The concentration of oxammonium hydrochloride is 10g/L; The concentration of phenanthrolene solution is 10g/L, and the compound method of phenanthrolene solution is: take the 5g phenanthrolene and be dissolved in 100mL ethanol, be diluted with water to 500mL; The compound method of acetic acid-sodium acetate buffer solution is: take 136g sodium acetate trihydrate (CH
3cOONa3H
2o) be dissolved in 300mL water, add 57.0mL glacial acetic acid (ρ=1.05g/mL), mix after being diluted with water to 1000mL.This mixing nitrite ion is used in being preferably in and preparing one week.
5) according to the absorbance A of sample solution, be 0.1803, the quality of finding iron in sample solution from typical curve is m
1=198.9919 μ g, the iron content W in described covering slag
fecan be calculated as follows:
In formula, W
fefor the massfraction of iron, %; V
0for the cumulative volume of sample solution, unit is milliliter (mL); V
1for getting volume dividing of sample solution, unit is milliliter (mL); m
1for the iron content checked in from typical curve, unit is microgram (μ g); m
0for the covering slag sample mass, unit is gram (g).
The massfraction that finally calculates iron in this continuous casting covering slag is 0.4975%.
Embodiment 2:
Adopt west to protect the continuous casting covering slag of smelting material Group Co.,Ltd production as sample.
1) at first, weighing m
0the covering slag of=0.2000g, be placed in the 300mL polytetrafluoroethylene beaker, uses a small amount of water-wet, adds 20mL hydrochloric acid, 5mL hydrofluorite, 5mL nitric acid, low-temperature heat 30min; Then add 5mL perchloric acid, low-temperature heat, to emitting the perchloric acid cigarette, continues heating and smolders near dry; After cooling, by 9mL after first 1mL, add altogether 10mL hydrochloric acid, with a small amount of water, rinse wall of cup, heating 5min dissolved salts, after taking off and being cooled to room temperature, with Filter Paper Dry filtered sample solution at a slow speed, be settled to V by sample solution
0=100mL;
2) by Fe
2o
3calcination and be cooled to room temperature after, add hydrochloric acid and water, carry out heating for dissolving, obtain iron standard stock solution, then will iron standard stock solution obtain the iron standard solution of 100 μ g/mL after dilution;
3) pipette respectively 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL iron standard solution (100 μ g/mL) is divided in five 100mL volumetric flasks, and with deionized water, a blank sample is set, respectively add 25mL mixing nitrite ion, be diluted with water to scale and mix, after room temperature is placed 15min, getting standard solution and blank sample are moved respectively in the 2cm absorption vessel, is the absorbance A that the 510nm place surveys each standard solution and blank sample with spectrophotometer at wavelength, and data are as table 1.The quality of iron in each standard solution and blank sample of take is horizontal ordinate, and take each standard solution of recording and the absorbance of blank sample is ordinate drawing standard curve, and typical curve is as shown in b line in Fig. 1, and the linear dependence degree is 0.9999;
4) divide and get V
1=5.00mL sample solution is in the 100mL volumetric flask, add 25mL mixing nitrite ion, be diluted with water to scale and mix, after room temperature is placed 15min, get in the sample solution immigration 2cm absorption vessel after part adds nitrite ion, and take deionized water and blank sample is set as reference, with spectrophotometer, at wavelength, be that the absorbance A that the 510nm place records sample solution is 0.1756;
Above-mentioned steps 3) and 4) in the mixing nitrite ion used by 1 volume ascorbic acid, 0.5 volume oxammonium hydrochloride, 4 volume phenanthrolene solution, and acetic acid-sodium acetate buffer solution of 24 volume 1mol/L mixes, wherein, the concentration of ascorbic acid is 10g/L; The concentration of oxammonium hydrochloride is 10g/L; The concentration of phenanthrolene solution is 10g/L.
5) according to the absorbance A of sample solution, be 0.1756, the quality of finding iron in sample solution from typical curve is m
1=308.1454 μ g, the massfraction that calculates iron in this continuous casting covering slag is 3.081%.
Embodiment 3:
Adopt west to protect the continuous casting covering slag of smelting material Group Co.,Ltd production as sample.
1) at first, weighing m
0the covering slag of=0.5000g, be placed in the 300mL polytetrafluoroethylene beaker, with after a small amount of water-wet, adds 30mL hydrochloric acid, 10mL hydrofluorite, 20mL nitric acid, low-temperature heat 30min; Then add 10mL perchloric acid, low-temperature heat, to emitting the perchloric acid cigarette, continues heating and smolders near dry; After cooling, by 9mL after first 1mL, add altogether 10mL hydrochloric acid, with a small amount of water, rinse wall of cup, heating 5min dissolved salts, take off, and after being cooled to room temperature, uses Filter Paper Dry filtered sample solution at a slow speed, and sample solution is settled to V
0=250mL;
2) by Fe
2o
3calcination and be cooled to room temperature after, add hydrochloric acid and water, carry out heating for dissolving, obtain iron standard stock solution, then will iron standard stock solution obtain the iron standard solution of 100 μ g/mL after dilution;
3) pipette respectively 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL iron standard solution (100 μ g/mL) is divided in five 100mL volumetric flasks, and with deionized water, blank sample is set, respectively add 40mL mixing nitrite ion, be diluted with water to scale and mix, after room temperature is placed 15min, by in standard solution and the blank sample absorption vessel that to move respectively in thickness be 1cm, with spectrophotometer, at wavelength, be the absorbance A that the 510nm place surveys each standard solution and blank sample, data are as table 1.The quality of iron in each standard solution and blank sample of take is horizontal ordinate, and take each standard solution of recording and the absorbance of blank sample is ordinate drawing standard curve, and typical curve is as shown in c line in Fig. 1, and the linear dependence degree is 0.9999.
4) divide and get V
1=10.00mL sample solution is in the 250mL volumetric flask, add 40mL mixing nitrite ion, be diluted with water to scale and mix, after room temperature is placed 15min, getting part adds the sample solution after nitrite ion to move in the absorption vessel that thickness is 1cm, and take deionized water and blank sample is set as reference, with spectrophotometer, at wavelength, be that the absorbance A that the 510nm place records sample solution is 0.3817;
Above-mentioned steps 3) and 4) in the mixing nitrite ion used by 1 volume ascorbic acid, 2 volume oxammonium hydrochlorides, 1 volume phenanthrolene solution, and acetic acid-sodium acetate buffer solution of 18 volume 1mol/L mixes, wherein, the concentration of ascorbic acid is 10g/L; The concentration of oxammonium hydrochloride is 10g/L; The concentration of phenanthrolene solution is 10g/L.
5) according to the absorbance A of sample solution, be 0.3817, the quality of finding iron in sample solution from typical curve is m
1=911.7511 μ g, the massfraction that calculates iron in this continuous casting covering slag is 4.559%.
In embodiment 1-3, the absorbance A of different iron content standard solution is as shown in table 1:
Table 1
| m(Fe)/ |
200 | 400 | 600 | 800 | 1000 |
| Embodiment 1(A) | 0.1791 | 0.3881 | 0.5830 | 0.7899 | 0.9899 |
| Embodiment 2(A) | 0.1013 | 0.2388 | 0.3760 | 0.5139 | 0.6512 |
| Embodiment 3(A) | 0.0604 | 0.1505 | 0.2412 | 0.3312 | 0.4215 |
Claims (5)
1. the rapid assay methods of iron content in a continuous casting covering slag, it is characterized in that: the method comprises the steps:
1) prepare the covering slag sample solution: be at first m by quality
0covering slag is hydrochloric acid, hydrofluorite for sample, and after nitric acid dissolve with perchloric acid smoked near dry, then with dissolving with hydrochloric acid, leach salt, dilute after being cooled to room temperature, after filtering, to make volume be V to constant volume
0sample solution;
2) preparation iron standard solution: at first by Fe
2o
3calcination and be cooled to room temperature after, add hydrochloric acid and water, carry out heating for dissolving, obtain iron standard stock solution, then will iron standard stock solution obtain the iron standard solution after dilution;
3) drawing standard curve: the one group of iron standard solution that pipettes different volumes, add the mixed in equal amounts nitrite ion after dilute with water in each iron standard solution, then make one group of isopyknic standard solution after the water constant volume, and establish blank sample, be the absorbance that each standard solution and blank sample detect in the 510nm place with spectrophotometer at wavelength, thereby draw out " typical curve of weight of iron (m)-absorbance (A) "; Wherein, described mixing nitrite ion is by ascorbic acid, oxammonium hydrochloride, phenanthrolene solution, and acetic acid-sodium acetate buffer solution mixes;
4) measure the iron content in sample solution: pipetting volume is V
1sample solution, add the nitrite ion that mixes with step 3) standard sample moderate after dilute with water, then water is settled to and the standard sample equal-volume; The absorbance that is 510nm place test samples solution at wavelength with spectrophotometer, finding iron content from typical curve is m
1;
5) calculate the iron content W in covering slag
fe: by the cumulative volume V of sample solution
0, volume V is got in dividing of sample solution
1, covering slag sample mass m
0, and the iron content m checked in from typical curve
1data can calculate the iron content W in covering slag
fe.
2. the rapid assay methods of iron content in continuous casting covering slag according to claim 1; it is characterized in that: in described step 3); the oxammonium hydrochloride that the ascorbic acid that described mixing nitrite ion is 10g/L by concentration, concentration are 10g/L, concentration are 10g/L phenanthrolene solution, and acetic acid-sodium acetate buffer solution of 1mol/L be take volume ratio and mixed as 1: 0.5～2: 1～4: 18～24.
3. the rapid assay methods of iron content in continuous casting covering slag according to claim 1 and 2; it is characterized in that: in described step 3); described phenanthrolene solution is dissolved in 1 volume ethanol by the phenanthrolene powder, then is diluted with water to 5 volumes formulated.
4. the rapid assay methods of iron content in continuous casting covering slag according to claim 1 and 2; it is characterized in that: in described step 3); described acetic acid-sodium acetate buffer solution is dissolved in 300mL water according to the 136g sodium acetate trihydrate; add the 57mL glacial acetic acid, the ratio that is diluted with water to 1000mL is formulated again.
5. the rapid assay methods of iron content in continuous casting covering slag according to claim 1 and 2; it is characterized in that: described step 1); the hydrochloric acid that is 36%～38% with mass percent concentration; the hydrofluorite that mass percent concentration is 40%～47%; the nitric acid that mass percent concentration is 65%～68%, and the mass percent concentration perchloric acid that is 70%～72% is to add dissolve covering slag sample at 10～30: 3～10: 5～20: 3～10 by volume.
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| CN104181272A (en) * | 2014-07-30 | 2014-12-03 | 武汉钢铁(集团)公司 | Method for rapidly determining content of total iron in vanadium titano-magnetite |
| CN107024468A (en) * | 2017-03-17 | 2017-08-08 | 唐山钢铁集团有限责任公司 | The assay method of iron, aluminium, manganese, calcium, titanium, silicon, magnesium in covering slag |
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| US5620658A (en) * | 1995-09-11 | 1997-04-15 | Industrial Test Systems, Inc. | Colorimetric test strip |
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| CN104181272A (en) * | 2014-07-30 | 2014-12-03 | 武汉钢铁(集团)公司 | Method for rapidly determining content of total iron in vanadium titano-magnetite |
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| CN107024468A (en) * | 2017-03-17 | 2017-08-08 | 唐山钢铁集团有限责任公司 | The assay method of iron, aluminium, manganese, calcium, titanium, silicon, magnesium in covering slag |
| CN109507181A (en) * | 2019-01-17 | 2019-03-22 | 中南大学 | A kind of rapid quantitative detection zinc abstraction solution trace cobalt ferronickel ion concentration method |
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