CN103439324B - The rapid assay methods of iron content in continuous casting covering slag - Google Patents
The rapid assay methods of iron content in continuous casting covering slag Download PDFInfo
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- CN103439324B CN103439324B CN201310350472.5A CN201310350472A CN103439324B CN 103439324 B CN103439324 B CN 103439324B CN 201310350472 A CN201310350472 A CN 201310350472A CN 103439324 B CN103439324 B CN 103439324B
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 153
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 73
- 239000002893 slag Substances 0.000 title claims abstract description 51
- 238000009749 continuous casting Methods 0.000 title claims abstract description 24
- 238000003556 assay Methods 0.000 title claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 41
- 239000012488 sample solution Substances 0.000 claims abstract description 37
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 34
- 239000012086 standard solution Substances 0.000 claims abstract description 32
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims abstract description 24
- 229940005654 nitrite ion Drugs 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 17
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 17
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 17
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007974 sodium acetate buffer Substances 0.000 claims abstract description 13
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 24
- 239000012496 blank sample Substances 0.000 claims description 22
- 238000002835 absorbance Methods 0.000 claims description 21
- 239000000523 sample Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- BDKLKNJTMLIAFE-UHFFFAOYSA-N 2-(3-fluorophenyl)-1,3-oxazole-4-carbaldehyde Chemical compound FC1=CC=CC(C=2OC=C(C=O)N=2)=C1 BDKLKNJTMLIAFE-UHFFFAOYSA-N 0.000 claims description 3
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 230000001186 cumulative effect Effects 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 235000017281 sodium acetate Nutrition 0.000 claims description 3
- 229940087562 sodium acetate trihydrate Drugs 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 230000002829 reductive effect Effects 0.000 abstract description 7
- 239000003795 chemical substances by application Substances 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 238000006722 reduction reaction Methods 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 235000019504 cigarettes Nutrition 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 230000005477 standard model Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000008351 acetate buffer Substances 0.000 description 1
- YBCVMFKXIKNREZ-UHFFFAOYSA-N acoh acetic acid Chemical compound CC(O)=O.CC(O)=O YBCVMFKXIKNREZ-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
Landscapes
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses the rapid assay methods of iron content in a kind of continuous casting covering slag, comprise the steps: 1) prepare covering slag sample solution; 2) iron standard solution is prepared; 3) drawing standard curve; 4) iron content in sample solution is measured; 5) calculate the iron content in covering slag, step 3) and 4) in mixing nitrite ion by ascorbic acid, oxammonium hydrochloride, phenanthrolene solution, and acetic acid-sodium acetate buffer solution mixes.Ascorbic acid, oxammonium hydrochloride, phenanthrolene and acetic acid-sodium acetate buffer solution can once add by this nitrite ion, avoid the problem that the colour developing that causes because of reagent addition sequence successively problem in prior art not exclusively maybe cannot develop the color, simplify detecting step, there is sensitivity, simple to operate, analyze advantage fast; Ascorbic acid wherein and the good ascorbic acid-oxammonium hydrochloride mixing reductive agent of oxammonium hydrochloride forming property, make reduction reaction fast and stable, effectively improve the accuracy of testing result.
Description
Technical field
The present invention relates to metallurgical technology, refer to the rapid assay methods of iron content in a kind of continuous casting covering slag particularly.
Background technology
Continuous casting covering slag, be functional material important during continuous casting is produced, it is as medium interactional between crystallizer and strand, carrying out smoothly and improving 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 to the viscosity of covering slag, fusing point, and the equal physicochemical property of Crystalline have an impact, and therefore, the iron content in 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 phenanthrolene spectrophotometric method etc., all there is certain deficiency in these method of testings.Wherein, because covering slag sample has not easily keeping quality, X-fluorescence method lacks has card covering slag standard model to set up calibration curve, the standard models such as the close blast furnace slag of character, vessel slag can only be selected to set up working curve, thus have impact on the accuracy of result, in addition, as pertinent literature (Jiang Yanan, Yang Guang, field Wei .ICP-OES method measure the oxide content [J] of iron, aluminium, magnesium in covering slag. Hebei Metallurgy, 2013,205, the ICP-AES method that utilizes introduced 62-63) measures the method for iron content in covering slag, the method adopts alkali fusion method to melt sample, the mixed flux coupling adding equivalent is needed in working curve, detect and be limited to 0.012mg/L, relative standard is 1.26%, though the mensuration of multielement can be completed simultaneously, but expensive equipment, and method is not easily promoted, and phenanthrolene method spectrophotometric method is the assay method of iron content in the continuous casting covering slag of regulation in existing iron and steel industry industry standard YB/T190-2001 (continuous casting covering slag chemical analysis method), the method is in acetic acid-acetate buffer, ferrous ion and phenanthrolene generate orange red complex compound, solution absorbance is measured in 510nm place with spectrophotometer, according to the Mass Calculation iron content that typical curve checks in, but the method needs first to add reductive agent ascorbic acid when developing the color the ferric iron back in sample is become ferrous iron, then acidity is regulated with buffer solution, finally add phenanthrolene colour developing, test solution addition sequence can not be exchanged, otherwise colour developing will be caused not exclusively maybe cannot to develop the color, result in operational inconvenience and minute long.
Summary of the invention
Object of the present invention is exactly the rapid assay methods that will provide iron content in a kind of continuous casting covering slag, and the method can be quick, the easy and iron content that measures exactly 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) covering slag sample solution is prepared: be first m by quality
0covering slag sample hydrochloric acid, hydrofluorite, and do near with perchloric acid smoked after nitric acid dissolve, then leach salt with dissolving with hydrochloric acid, dilute after being cooled to room temperature, after filtering, constant volume obtains volume is V
0sample solution;
2) iron standard solution is prepared: first by Fe
2o
3calcination also, after being cooled to room temperature, adds hydrochloric acid and water, carries out heating for dissolving, obtains iron typical shelf solution, then obtain iron standard solution by after iron typical shelf solution dilution;
3) drawing standard curve: the one group of iron standard solution pipetting different volumes, in each iron standard solution, the mixing nitrite ion of equivalent is added after dilute with water, then with one group of isopyknic standard solution obtained after water constant volume, and establish blank sample, be the absorbance of the 510nm place each standard solution of detection and blank sample at wavelength with spectrophotometer, thus 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) iron content in sample solution is measured: pipetting volume is V
1sample solution, add after dilute with water with step 3) standard sample moderate mix nitrite ion, be then settled to and standard sample equal-volume with water; Be the absorbance of 510nm place test samples solution at wavelength with spectrophotometer, finding iron content from typical curve is m
1;
5) the iron content W in covering slag is calculated
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 W in covering slag can be calculated from the iron content m1 data that typical curve checks in
fe.
In described step 3), described mixing nitrite ion by concentration be the ascorbic acid of 10g/L, concentration is the oxammonium hydrochloride of 10g/L, concentration is 10g/L phenanthrolene solution, and the acetic acid-sodium acetate buffer solution of 1mol/L is 1: 0.5 ~ 2: 1 ~ 4: 18 ~ 24 to mix with volume ratio.
In described step 3), described phenanthrolene solution is dissolved in 1 volume ethanol by phenanthrolene powder, is then 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 136g sodium acetate trihydrate, then adds 57mL glacial acetic acid, and the proportions being diluted with water to 1000mL forms.
Described step 1) in; be the hydrochloric acid of 36% ~ 38% with mass percent concentration; mass percent concentration is the hydrofluorite of 40% ~ 47%; mass percent concentration is the nitric acid of 65% ~ 68%, and mass percent concentration be 70% ~ 72% perchloric acid be 10 ~ 30: 3 ~ 10: 5 ~ 20: 3 ~ 10 add and dissolve covering slag sample by volume.
Compared with prior art, tool of the present invention has the following advantages:
One, ascorbic acid in the present invention's mixing nitrite ion and the good ascorbic acid-oxammonium hydrochloride mixing reductive agent of oxammonium hydrochloride forming property, wherein, ascorbic acid is medium tenacity reductive agent, its electrode potential is+0.30V, oxammonium hydrochloride electrode potential is+0.42V, better stability is had compared with other reductive agents, use ascorbic acid-oxammonium hydrochloride mixing reductive agent, make reduction reaction fast and stable, both can ensure that ferric iron back was thorough, can avoid again ascorbic acid that other high valence ions in covering slag are reduced to divalence, effectively improve 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 mixing nitrite ion, once add, avoid the problem that the colour developing that causes because of reagent addition sequence successively problem in prior art not exclusively maybe cannot develop the color, simplify detecting step, there is sensitivity and degree of accuracy is high, simple to operate, to analyze fast, advantage that equipment cost is low.
Accompanying drawing explanation
Fig. 1 is weight of iron (m)-absorbance (A) typical curve of embodiment 1 ~ 3.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated, but the present invention is not limited to following embodiment.
For dissolving hydrochloric acid, hydrofluorite, the nitric acid of covering slag sample in following examples, and perchloric acid is commercial 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 the acetic acid-sodium acetate buffer solution prepared in following examples preferably 4 ~ 5.
Embodiment 1:
The continuous casting covering slag adopting Wuhan Iron & Steel (Group) Corp. second steel plant continuous casting production technology used is as sample.
1) first, quality m is taken
0the covering slag of=0.1000g, is placed in 300mL polytetrafluoroethylene beaker, 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 perchloric acid cigarette, continues heating and smolders near dry; After cooling, 10mL hydrochloric acid is added altogether by 9mL after first 1mL, wall of cup is rinsed with a small amount of water, heating 5min dissolved salts (controls the hydrochloric acid consumption dissolving leaching salt, the content of concentrated hydrochloric acid in solution is made to be no more than the number percent 2% of constant volume), after being cooled to room temperature, using Filter Paper Dry filtered sample solution at a slow speed, sample solution is settled to V
0=50mL;
2) calcination is in advance cooled to the 0.3574gFe of room temperature
2o
3be placed in beaker, add the hydrochloric acid that 1 ~ 2mL mass percent concentration is 36% ~ 38%, room temperature is cooled to after heating for dissolving, transfer in volumetric flask, be diluted to scale with deionized water and obtain iron typical shelf solution after mixing, by iron typical shelf solution dilution, prepare the iron standard solution of 100 μ g/mL;
3) pipetting 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL iron standard solution (100 μ g/mL) is respectively divided in 100mL volumetric flask, and blank sample is set with deionized water, respectively add 15mL mixing nitrite ion, be diluted with water to scale and mix, after room temperature places 15min, standard solution and blank sample being moved in thickness is respectively in 3cm absorption vessel, and be the absorbance A of the 510nm place each standard solution of survey and blank sample at wavelength with spectrophotometer, data are as table 1.With the quality of iron in each standard solution and blank sample for horizontal ordinate, with the absorbance of each standard solution recorded and blank sample for ordinate drawing standard curve, typical curve is as shown in a line in Fig. 1, and linear correlation degree is 0.9999.
4) divide and get V
1=20.00mL sample solution is in 50mL volumetric flask, add 15mL mixing nitrite ion, be diluted with water to scale and mix, after room temperature places 15min, it is in 3cm absorption vessel that the sample solution got after partly adding mixing nitrite ion moves into thickness, and with deionized water, blank sample is set for reference, be the absorbance A that 510nm place records sample solution with spectrophotometer at wavelength be 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 the 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 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 preferably prepare in one week use.
5) be 0.1803 according to the absorbance A of sample solution, the quality 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 dividing of sample solution gets volume, unit is milliliter (mL); m
1for the iron content checked in from typical curve, unit is microgram (μ g); m
0for covering slag sample mass, unit is gram (g).
The massfraction finally calculating iron in this continuous casting covering slag is 0.4975%.
Embodiment 2:
Adopt the continuous casting covering slag of Xi Baoye material Group Co., Ltd production as sample.
1) first, weighing m
0the covering slag of=0.2000g, is placed in 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 perchloric acid cigarette, continues heating and smolders near dry; After cooling, add 10mL hydrochloric acid altogether by 9mL after first 1mL, rinse wall of cup with a small amount of water, heating 5min dissolved salts, takes off after being cooled to room temperature, uses Filter Paper Dry filtered sample solution at a slow speed, sample solution is settled to V
0=100mL;
2) by Fe
2o
3calcination also, after being cooled to room temperature, adds hydrochloric acid and water, carries out heating for dissolving, obtains iron typical shelf solution, then will obtain the iron standard solution of 100 μ g/mL after iron typical shelf solution dilution;
3) pipetting 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL iron standard solution (100 μ g/mL) is respectively divided in five 100mL volumetric flasks, and a blank sample is set with deionized water, respectively add 25mL mixing nitrite ion, be diluted with water to scale and mix, after room temperature places 15min, get and move respectively in 2cm absorption vessel by standard solution and blank sample, be the absorbance A of the 510nm place each standard solution of survey and blank sample at wavelength with spectrophotometer, data are as table 1.With the quality of iron in each standard solution and blank sample for horizontal ordinate, with the absorbance of each standard solution recorded and blank sample for ordinate drawing standard curve, typical curve is as shown in b line in Fig. 1, and linear correlation degree is 0.9999;
4) divide and get V
1=5.00mL sample solution is in 100mL volumetric flask, add 25mL mixing nitrite ion, be diluted with water to scale and mix, after room temperature places 15min, the sample solution got after partly adding nitrite ion moves in 2cm absorption vessel, and with deionized water, blank sample is set for reference, be the absorbance A that 510nm place records sample solution with spectrophotometer at wavelength be 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 the 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) be 0.1756 according to the absorbance A of sample solution, the quality finding iron in sample solution from typical curve is m
1=308.1454 μ g, the massfraction calculating iron in this continuous casting covering slag is 3.081%.
Embodiment 3:
Adopt the continuous casting covering slag of Xi Baoye material Group Co., Ltd production as sample.
1) first, weighing m
0the covering slag of=0.5000g, is placed in 300mL polytetrafluoroethylene beaker, 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 perchloric acid cigarette, continues heating and smolders near dry; After cooling, add 10mL hydrochloric acid altogether by 9mL after first 1mL, rinse wall of cup with a small amount of water, heating 5min dissolved salts, takes off, and after being cooled to room temperature, using Filter Paper Dry filtered sample solution at a slow speed, sample solution is settled to V
0=250mL;
2) by Fe
2o
3calcination also, after being cooled to room temperature, adds hydrochloric acid and water, carries out heating for dissolving, obtains iron typical shelf solution, then will obtain the iron standard solution of 100 μ g/mL after iron typical shelf solution dilution;
3) pipetting 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL iron standard solution (100 μ g/mL) is respectively divided in five 100mL volumetric flasks, and blank sample is set with deionized water, respectively add 40mL mixing nitrite ion, be diluted with water to scale and mix, after room temperature places 15min, standard solution and blank sample being moved in thickness is respectively in the absorption vessel of 1cm, and be the absorbance A of the 510nm place each standard solution of survey and blank sample at wavelength with spectrophotometer, data are as table 1.With the quality of iron in each standard solution and blank sample for horizontal ordinate, with the absorbance of each standard solution recorded and blank sample for ordinate drawing standard curve, typical curve is as shown in c line in Fig. 1, and linear correlation degree is 0.9999.
4) divide and get V
1=10.00mL sample solution is in 250mL volumetric flask, add 40mL mixing nitrite ion, be diluted with water to scale and mix, after room temperature places 15min, getting the sample solution immigration thickness after partly adding nitrite ion is in the absorption vessel of 1cm, and with deionized water, blank sample is set for reference, be the absorbance A that 510nm place records sample solution with spectrophotometer at wavelength be 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 the 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) be 0.3817 according to the absorbance A of sample solution, the quality finding iron in sample solution from typical curve is m
1=911.7511 μ g, the massfraction calculating 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)/μg | 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 (4)
1. the rapid assay methods of iron content in continuous casting covering slag, is characterized in that: the method comprises the steps:
1) covering slag sample solution is prepared: be first m by quality
0covering slag sample hydrochloric acid, hydrofluorite, and do near with perchloric acid smoked after nitric acid dissolve, then leach salt with dissolving with hydrochloric acid, dilute after being cooled to room temperature, after filtering, constant volume obtains volume is V
0sample solution;
2) iron standard solution is prepared: first by Fe
2o
3calcination also, after being cooled to room temperature, adds hydrochloric acid and water, carries out heating for dissolving, obtains iron typical shelf solution, then obtain iron standard solution by after iron typical shelf solution dilution;
3) drawing standard curve: the one group of iron standard solution pipetting different volumes, in each iron standard solution, mixed in equal amounts nitrite ion is added after dilute with water, then with one group of isopyknic standard solution obtained after water constant volume, and establish blank sample, be the absorbance of the 510nm place each standard solution of detection and blank sample at wavelength with spectrophotometer, thus draw out " typical curve of weight of iron (m)-absorbance (A) "; Wherein, described mixing nitrite ion by concentration be the ascorbic acid of 10g/L, concentration is the oxammonium hydrochloride of 10g/L, concentration is 10g/L phenanthrolene solution, and the acetic acid-sodium acetate buffer solution of 1mol/L is 1: 0.5 ~ 2: 1 ~ 4: 18 ~ 24 to mix with volume ratio;
4) iron content in sample solution is measured: pipetting volume is V
1sample solution, adds and step 3 after dilute with water) standard sample moderate mix nitrite ion, be then settled to and standard sample equal-volume with water; Be the absorbance of 510nm place test samples solution at wavelength with spectrophotometer, finding iron content from typical curve is m
1;
5) the iron content W in covering slag is calculated
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 from the iron content m that typical curve checks in
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: described step 3) in; described phenanthrolene solution is dissolved in 1 volume ethanol by phenanthrolene powder, is then diluted with water to 5 volumes formulated.
3. the rapid assay methods of iron content in continuous casting covering slag according to claim 1; it is characterized in that: described step 3) in; described acetic acid-sodium acetate buffer solution is dissolved in 300mL water according to 136g sodium acetate trihydrate; add 57mL glacial acetic acid again, the proportions being diluted with water to 1000mL forms.
4. the rapid assay methods of iron content in continuous casting covering slag according to claim 1; it is characterized in that: described step 1) in; be the hydrochloric acid of 36% ~ 38% with mass percent concentration; mass percent concentration is the hydrofluorite of 40% ~ 47%; mass percent concentration is the nitric acid of 65% ~ 68%, and mass percent concentration be 70% ~ 72% perchloric acid be 10 ~ 30: 3 ~ 10: 5 ~ 20: 3 ~ 10 add and dissolve covering slag sample by volume.
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| CN104181272B (en) * | 2014-07-30 | 2016-08-24 | 武汉钢铁(集团)公司 | The rapid assay methods of all iron content 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 |
| CN109507181B (en) * | 2019-01-17 | 2020-06-30 | 中南大学 | A method for rapid quantitative detection of trace cobalt, nickel, iron ion concentration in zinc smelting solution |
| CN112763439A (en) * | 2020-12-28 | 2021-05-07 | 青海西钢特殊钢科技开发有限公司 | Method for determining boron element in refining slag of gear steel |
| CN113340834B (en) * | 2021-06-11 | 2023-05-16 | 成都市排水有限责任公司 | Method for rapidly determining sodium acetate content in industrial sodium acetate solution |
| CN117191769A (en) * | 2023-09-14 | 2023-12-08 | 华南理工大学 | A method for detecting total iron content in red mud |
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