CN113281458A - Analysis method for free total calcium content of steel slag - Google Patents
Analysis method for free total calcium content of steel slag Download PDFInfo
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- CN113281458A CN113281458A CN202110669129.1A CN202110669129A CN113281458A CN 113281458 A CN113281458 A CN 113281458A CN 202110669129 A CN202110669129 A CN 202110669129A CN 113281458 A CN113281458 A CN 113281458A
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- steel slag
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 43
- 239000010959 steel Substances 0.000 title claims abstract description 43
- 239000002893 slag Substances 0.000 title claims abstract description 42
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000011575 calcium Substances 0.000 title claims abstract description 37
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 37
- 238000004458 analytical method Methods 0.000 title abstract description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 67
- 239000000243 solution Substances 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 26
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000004448 titration Methods 0.000 claims abstract description 17
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 11
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000292 calcium oxide Substances 0.000 claims abstract description 10
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- 239000012086 standard solution Substances 0.000 claims abstract description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 8
- 229960003531 phenolsulfonphthalein Drugs 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- DEGAKNSWVGKMLS-UHFFFAOYSA-N calcein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC(CN(CC(O)=O)CC(O)=O)=C(O)C=C1OC1=C2C=C(CN(CC(O)=O)CC(=O)O)C(O)=C1 DEGAKNSWVGKMLS-UHFFFAOYSA-N 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229960002378 oftasceine Drugs 0.000 claims description 4
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- BELBBZDIHDAJOR-UHFFFAOYSA-N Phenolsulfonephthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2S(=O)(=O)O1 BELBBZDIHDAJOR-UHFFFAOYSA-N 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 235000010333 potassium nitrate Nutrition 0.000 claims description 2
- 239000004323 potassium nitrate Substances 0.000 claims description 2
- DIZZDZCUMBBRSG-UHFFFAOYSA-J tetrasodium;2-[[5-[3-[3-[[bis(carboxylatomethyl)amino]methyl]-4-hydroxy-2-methyl-5-propan-2-ylphenyl]-1,1-dioxo-2,1$l^{6}-benzoxathiol-3-yl]-2-hydroxy-6-methyl-3-propan-2-ylphenyl]methyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CC1=C(O)C(C(C)C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C(=C(CN(CC([O-])=O)CC([O-])=O)C(O)=C(C(C)C)C=2)C)=C1C DIZZDZCUMBBRSG-UHFFFAOYSA-J 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000003556 assay Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000004568 cement Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- BDRTVPCFKSUHCJ-UHFFFAOYSA-N molecular hydrogen;potassium Chemical compound [K].[H][H] BDRTVPCFKSUHCJ-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- XHCCWBJFZUXJBV-UHFFFAOYSA-K trisodium 2-[(2-oxido-5-sulfophenyl)diazenyl]-3,6-disulfonaphthalene-1,8-diolate Chemical compound C1=CC(=C(C=C1S(=O)(=O)O)N=NC2=C(C3=C(C=C(C=C3C=C2S(=O)(=O)O)S(=O)(=O)O)[O-])[O-])[O-].[Na+].[Na+].[Na+] XHCCWBJFZUXJBV-UHFFFAOYSA-K 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The patent relates to the chemical analysis field of the content of free total calcium in steel slag. Dissolving calcium in a steel slag sample in an ethylene glycol solution, adding triethanolamine to shield the influence of compounds except the calcium in the ethylene glycol solution, then adding strong base to adjust the pH value to be more than 13, adding a mixed indicator under shaking, titrating by using an EDTA standard solution until green fluorescence completely disappears and is red after the green fluorescence appears, and consuming the volume of the EDTA standard titration solution/the quality of the steel slag sample when the steel slag free total calcium content =100% and the EDTA standard titration solution titrates the titer of calcium oxide. The method effectively overcomes the defects in the analysis process of the content of free total calcium in the steel slag.
Description
Technical Field
The patent relates to the chemical analysis field of the content of free total calcium in steel slag.
Background
The control of the free total calcium content in the steel slag is beneficial to the resource utilization of the steel slag. The analysis of the content of free total calcium in the steel slag is very important. At present, a laboratory of a processing plant adopts a method of a steel slag free calcium oxide content determination method YB/T4328-2012 to analyze, and the method has two defects, which seriously influences the accuracy of an analysis result. Firstly, after a sample is dissolved, solid-liquid separation by using a centrifugal machine is not easy to control, and test errors are easily caused; and secondly, the chrome blue K is adopted as the calcium indicator, the end point is easy to fluctuate, and repeated titration causes test errors.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the analysis method aims to provide an analysis method of the steel slag free total calcium content, which can realize solid-liquid rapid separation, is easy to observe a titration end point and has complete reaction, and solves the problems of poor solid-liquid analysis and end point fluctuation of a calcium indicator in the original method, so that the analysis result is accurate and reliable.
The technical scheme adopted by the invention is as follows: a method for analyzing the free total calcium content of steel slag includes such steps as dissolving calcium in the steel slag sample in glycol solution, adding triethanolamine to shield the influence of compounds except calcium in the ethylene glycol solution, adding strong base to adjust the pH value to be more than 13, adding calcein-phenol red mixed indicator or calcein-methyl thymol blue-phenolphthalein mixed indicator under shaking until green fluorescence appears, titrating the steel slag with an EDTA standard solution to completely disappear green fluorescence and show red by using a black background, wherein the steel slag contains free total calcium =100% and the titer of the EDTA standard titration solution to calcium oxide consumes the volume of the EDTA standard titration solution/the mass of the steel slag sample during titration, the unit of the titer of the EDTA standard titration solution to calcium oxide is mg/ml, the unit of the volume of the EDTA standard titration solution is ml, and the unit of the mass of the steel slag sample is kg.
Dissolving calcium in the steel slag sample in the glycol solution means that 0.3g of the steel slag sample is weighed and placed in a dry conical flask, 30ml of glycol is added, and the temperature is controlled to be 80-90 ℃ to magnetically stir for 20 min.
Dissolving calcium in a steel slag sample in an ethylene glycol solution, carrying out suction filtration, precipitation washing and solution volume metering, then adding triethanolamine to shield the influence of compounds except the calcium in the ethylene glycol solution, wherein the specific processes of suction filtration, precipitation washing and solution volume metering are that rapid quantitative filter paper is used for filtration, a suction filter is used for improving the filtration speed, absolute ethyl alcohol is used for washing the precipitate for 7-8 times, the ethylene glycol solution is cleaned, and water is added to enable the volume of the solution to be 100 milliliters.
The calcein-phenol red mixed indicator is prepared by weighing 1 g of calcein, adding 50-100 g of potassium chloride, mixing, grinding, placing into a ground bottle, weighing 0.05 g of phenol red, dissolving in 30ml of anhydrous ethanol, adding into the ground bottle, and diluting with water to 100 ml.
The calcein-methyl thymol blue-phenolphthalein mixed indicator is prepared by weighing 1 g calcein, 1 g methyl thymol blue, 0.20 g phenolphthalein and 50 g potassium nitrate dried at 105-110 deg.C, mixing, grinding, filling into ground bottle, and diluting with water to 100 ml.
Adding triethanolamine to shield the influence of compounds except calcium in the ethylene glycol solution, then adding strong base to adjust the pH value to be more than 13, and specifically preparing hydrochloric acid with the volume ratio of 39% and water in a ratio of 1:1 into dilute hydrochloric acid; adding 2 drops of dilute hydrochloric acid into the ethylene glycol solution, then adding 5mL of triethanolamine, adding potassium hydroxide while stirring to adjust the pH value of the solution, and stopping adding the potassium hydroxide when the pH value is more than 13.
The invention has the beneficial effects that: the method effectively overcomes the defects in the analysis process of the content of free total calcium in the steel slag, realizes the rapid solid-liquid separation in the analysis process of the sample, and ensures that the end point is easy to observe and the reaction is complete in the end point process, thereby ensuring that the analysis result is accurate and reliable.
Detailed Description
Example one
The method has the advantages of effect verification and sample assay accuracy analysis: the analysis adopts a standard substance cement clinker free calcium oxide component analysis standard sample (GSB 08-2145-2016) as a basis. The content of free calcium oxide in the standard substance was 3.08%.
The above assay method and the same standard steel material were repeated 5 times, and the assay data were as follows:
the test results are as follows:
as can be seen by examination, the P value is far greater than 0.05, and 3.07 percent is in a confidence interval (3.05322, 3.09478), which indicates that the result is accurate and reliable by using the method.
Example two
Weighing 0.3g of steel slag sample, weighing two steel slag samples at the same time, placing the two steel slag samples in a dry conical flask, adding 30mL of ethylene glycol, heating the mixture on a magnetic stirrer at the temperature of 80-90 ℃, and magnetically stirring the mixture for 20 min. Filtering with rapid quantitative filter paper, increasing the filtering speed with suction filter, washing the precipitate with anhydrous ethanol for 7-8 times, washing with ethylene glycol solution, and adding water to desired volume of 100 mL. Adding 2 drops of hydrochloric acid with the ratio of 1:1, adding 5mL of triethanolamine, adding potassium hydroxide while stirring to adjust the pH value of the solution to be more than 13, and checking by using a pH test paper. Under the condition of shaking, a proper amount of calcium blue indicator (calcein-methyl thymol blue-phenolphthalein mixed indicator) is added into the solution until green fluorescence appears, and then the EDTA standard solution is used for titration with a black background until the green fluorescence completely disappears and is red, the consumption milliliter number of the standard solution is read, and the calcium content is calculated according to a calculation formula.
EXAMPLE III
Weighing 0.3g of steel slag sample, weighing two steel slag samples at the same time, placing the two steel slag samples in a dry conical flask, adding 30mL of ethylene glycol, heating the mixture on a magnetic stirrer at the temperature of 80-90 ℃, and magnetically stirring the mixture for 20 min. Filtering with rapid quantitative filter paper, increasing the filtering speed with suction filter, washing the precipitate with anhydrous ethanol for 7-8 times, washing with ethylene glycol solution, and adding water to desired volume of 100 mL. Adding 2 drops of hydrochloric acid with the ratio of 1:1, adding 5mL of triethanolamine, adding total potassium hydrogen while stirring to adjust the pH value of the solution to be more than 13, and checking by using a pH test paper.
Under shaking, add appropriate calcein-phenol red mixed indicator and 3 drops of phenol red to the solution until green fluorescence appears, titrate with EDTA standard solution with black background until green fluorescence disappears completely and appears red. Reading the consumption milliliter number of the standard solution, and calculating the nickel content according to a calculation formula. The data are as follows
In the examples of this patent, the titer of EDTA standard titration solution to calcium oxide was 0.8460.
Claims (6)
1. A method for analyzing the content of free total calcium in steel slag is characterized by comprising the following steps: dissolving calcium in a steel slag sample in an ethylene glycol solution, adding triethanolamine to shield the influence of compounds except the calcium in the ethylene glycol solution, then adding strong base to adjust the pH value to be more than 13, adding a calcein-phenol red mixed indicator or a calcein-methyl thymol blue-phenolphthalein mixed indicator under shaking, titrating the mixed indicator with an EDTA standard solution until the green fluorescence is completely disappeared and the mixed indicator is red by using a black background after the green fluorescence appears, titrating the standard titration solution until the green fluorescence is completely disappeared, wherein the free total calcium content of the steel slag =100% and the titer of the EDTA standard titration solution to the calcium oxide consumes the volume of the EDTA standard titration solution/the mass of the steel slag sample when titrating the titer of the EDTA standard titration solution to the calcium oxide, wherein the unit of the titer of the EDTA standard titration solution to the calcium oxide is milligram/milliliter, the unit of the volume of the EDTA standard titration solution is milliliter, and the unit of the mass of the steel slag sample is kilogram.
2. The method for analyzing the content of free total calcium in steel slag according to claim 1, wherein the method comprises the following steps: dissolving calcium in the steel slag sample in the glycol solution means that 0.3g of the steel slag sample is weighed and placed in a dry conical flask, 30ml of glycol is added, and the temperature is controlled to be 80-90 ℃ to magnetically stir for 20 min.
3. The method for analyzing the content of free total calcium in steel slag according to claim 2, wherein the method comprises the following steps: dissolving calcium in a steel slag sample in an ethylene glycol solution, carrying out suction filtration, precipitation washing and solution volume metering, then adding triethanolamine to shield the influence of compounds except the calcium in the ethylene glycol solution, wherein the specific processes of suction filtration, precipitation washing and solution volume metering are that rapid quantitative filter paper is used for filtration, a suction filter is used for improving the filtration speed, absolute ethyl alcohol is used for washing the precipitate for 7-8 times, the ethylene glycol solution is cleaned, and water is added to enable the volume of the solution to be 100 milliliters.
4. The method for analyzing the content of free total calcium in steel slag according to claim 3, wherein the method comprises the following steps: the calcein-phenol red mixed indicator is prepared by weighing 1 g of calcein, adding 50-100 g of potassium chloride, mixing, grinding, placing into a ground bottle, weighing 0.05 g of phenol red, dissolving in 30ml of anhydrous ethanol, adding into the ground bottle, and diluting with water to 100 ml.
5. The method for analyzing the content of free total calcium in steel slag according to claim 3, wherein the method comprises the following steps: the calcein-methyl thymol blue-phenolphthalein mixed indicator is prepared by weighing 1 g calcein, 1 g methyl thymol blue, 0.20 g phenolphthalein and 50 g potassium nitrate dried at 105-110 deg.C, mixing, grinding, filling into ground bottle, and diluting with water to 100 ml.
6. The method for analyzing the content of free total calcium in steel slag according to claim 3, wherein the method comprises the following steps: adding triethanolamine to shield the influence of compounds except calcium in the ethylene glycol solution, then adding strong base to adjust the pH value to be more than 13, and specifically preparing hydrochloric acid with the volume ratio of 39% and water in a ratio of 1:1 into dilute hydrochloric acid; adding 2 drops of dilute hydrochloric acid into the ethylene glycol solution, then adding 5mL of triethanolamine, adding potassium hydroxide while stirring to adjust the pH value of the solution, and stopping adding the potassium hydroxide when the pH value is more than 13.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114280223A (en) * | 2021-12-22 | 2022-04-05 | 安徽华好阳光乳业有限公司 | Method for determining calcium in pasteurized milk |
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| CN105738362A (en) * | 2016-02-26 | 2016-07-06 | 内蒙古包钢钢联股份有限公司 | Method for measuring contents of calcium oxide and magnesia in iron ore |
| CN106404997A (en) * | 2016-10-14 | 2017-02-15 | 山西太钢不锈钢股份有限公司 | Method for determining content of calcium in calcium-silicon alloy by potentiometric titration |
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2021
- 2021-06-17 CN CN202110669129.1A patent/CN113281458A/en active Pending
Patent Citations (4)
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| CN102401822A (en) * | 2010-09-07 | 2012-04-04 | 鞍钢股份有限公司 | Determination method of free calcium oxide in furnace slag |
| CN102213704A (en) * | 2011-03-30 | 2011-10-12 | 太原重工股份有限公司 | Method for measuring contents of silicon-calcium elements in silicon-calcium alloy |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114280223A (en) * | 2021-12-22 | 2022-04-05 | 安徽华好阳光乳业有限公司 | Method for determining calcium in pasteurized milk |
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