CN104807814A - Determination method of calcium content in calcium containing ferroaluminium-manganese alloy - Google Patents
Determination method of calcium content in calcium containing ferroaluminium-manganese alloy Download PDFInfo
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- CN104807814A CN104807814A CN201510260626.0A CN201510260626A CN104807814A CN 104807814 A CN104807814 A CN 104807814A CN 201510260626 A CN201510260626 A CN 201510260626A CN 104807814 A CN104807814 A CN 104807814A
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- manganese
- calcic
- calcium content
- calcium
- aluminum
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- 239000011575 calcium Substances 0.000 title claims abstract description 41
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 35
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title abstract description 20
- 229910000914 Mn alloy Inorganic materials 0.000 title abstract 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 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
- 239000012086 standard solution Substances 0.000 claims abstract description 16
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims abstract description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 12
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 9
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 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 abstract description 8
- 229960002378 oftasceine Drugs 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims abstract description 7
- 235000019341 magnesium sulphate Nutrition 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- -1 aluminum-manganese-iron Chemical compound 0.000 claims description 18
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 17
- 238000003556 assay Methods 0.000 claims description 11
- 230000008034 disappearance Effects 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 description 26
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 25
- 239000004411 aluminium Substances 0.000 description 25
- 229910000831 Steel Inorganic materials 0.000 description 11
- 239000010959 steel Substances 0.000 description 11
- 229910000616 Ferromanganese Inorganic materials 0.000 description 7
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000009616 inductively coupled plasma Methods 0.000 description 6
- 238000009628 steelmaking Methods 0.000 description 6
- 229910000838 Al alloy Inorganic materials 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910001021 Ferroalloy Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910014779 CaAl4 Inorganic materials 0.000 description 1
- 229910004709 CaSi Inorganic materials 0.000 description 1
- 229910004706 CaSi2 Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009749 continuous casting Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000003412 degenerative effect Effects 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 238000013215 result calculation Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
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- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a determination method of the calcium content in a calcium containing ferroaluminium-manganese alloy. The method comprises the following steps of adding a calcium containing ferroaluminium-manganese alloy sample with the mass m into one beaker, enabling the other beaker to be empty so as to be used as blank control, later respectively adding hydrochloric acid, dissolving the sample on a low-temperature electric hot plate, taking out after the sample is dissolved, respectively and sequentially adding triethanolamine, water and hydroxylamine hydrochloride after cooling, adding potassium hydroxide solution to keep the pH not to be lower than 12, adding a few drops of magnesium sulfate and appropriate amount of calcein indicator, titrating by utilizing EDTA standard solution with the concentration C until the fluorescent green is disappeared as a terminal point, recording the volume as V and V0 respectively, and obtaining the calcium content as WCa% =C(V-V0)MCa100/m*100.
Description
Technical field
The present invention relates to ferroalloy analysis field, be specifically related to the assay method of calcium content in a kind of volumetric determination calcic aluminum-manganese-iron alloy.
Background technology
Deoxygenation of liquid steel is requisite process procedure in steelmaking process, and wherein the selection of deoxidizer is most important.From the history of deoxidant for steelmaking, the initial fine aluminium (generally using aluminium cake, Al content >95%) used, due to light specific gravity (2.79gPcm
3), aluminium cake not easily gos deep into molten steel inside, thus limits the effective rate of utilization of aluminium element.The ferro-silico aluminium that rear employing is made up of Si, Al Was Used replaces aluminium cake, therefore heavily increases (about 4.3gPcm
3), the effective rate of utilization of Al element is significantly improved, the consumption also corresponding reduction of deoxidant for steelmaking.
In recent years, along with steel are by the conversion of the seller to buyer's market, enterprise is forced more to focus on improving the inherent quality of steel.Double deoxidizer is strong because having deoxidizing capacity, can obviously improve the advantages such as molten steel degree of purity, naturally the common concern of numerous research institution and iron and steel enterprise is subject to, become the focus of recent deoxidizer field Study and Development, wherein especially to contain element M n, the double deoxidizer research of Ca is the most active, the selection aluminium of deoxidizer is as traditional deoxidant for steelmaking, strong and the aluminium because of aluminium and oxygen affinity, the characteristic of dissolving each other completely between iron, this also determines aluminium must status more difficult change in for a long time of ingredient as steel-making end-deoxidizer, but because aluminium adds easy formation high-melting-point deoxidation products in steel, molten steel flow is deteriorated, the castability of molten steel can be had a strong impact on, thus the direct motion that continuous casting is produced is constituted a threat to, therefore during deoxidation in steel making, the addition of aluminium is restricted.
Research shows, effectively degenerative treatments can be carried out to the high-melting-point snotter that deoxidation produces containing introducing strong deoxidant element Ca in the deoxidizer of aluminium, thus significantly improve the mobility of aluminium deoxidation molten steel, but because Ca solid solubility in aluminium alloy is extremely low, CaAl4 compound is formed with aluminium, calcium is again the superplasticity element of aluminium alloy, and the aluminium alloy of about 5% calcium and 5% manganese has superplasticity.Calcium and silicon form CaSi, are insoluble to aluminium, owing to decreasing the solid solution capacity of silicon, can slightly increase the electric conductivity of commercial-purity aluminium.Calcium can improve aluminium alloy cutting ability.CaSi2 can not make aluminium alloy heat treatment reinforcement.Micro-calcium is conducive to hydrogen in clearance liquid.
Calcic aluminium ferromanganese is best deoxidizer, desulfurizing agent in aluminum series alloy, the oxygen in steel is dropped to minimum, and the Accurate Determining therefore carrying out calcium in low calcium aluminum-manganese-iron alloy is significant.In current mensuration low calcium aluminium ferromanganese, the method for calcium adopts the instrumental analysis of ICP inductively coupled plasma mostly, but cost is high, with high content of technology, will be with a series of mark liquid simultaneously, very loaded down with trivial details.Compared to instrumental method, it is low that chemical method has cost, good stability, the features such as precision is high, quick.Be applicable to the Accurate Determining of calcium in calcic aluminum-manganese-iron alloy.
Summary of the invention
The invention provides a kind of more fast, measure the method for calcium content in calcic aluminum-manganese-iron alloy accurately and efficiently.
For reaching above-mentioned purpose, the assay method of calcium content in a kind of calcic aluminum-manganese-iron alloy of the present invention, comprises the following steps:
Add in one, beaker the calcic aluminum-manganese-iron alloy sample that quality is m, another does not add as blank, adds hydrochloric acid respectively afterwards, dissolved samples on low temp. electric hot plate, after sample dissolves, take off, after cooling, add triethanolamine, water, oxammonium hydrochloride successively respectively, hydro-oxidation potassium solution keeps pH to be not less than 12, and add several magnesium sulfate, calcein indicator is appropriate, being titrated to fluorescence green disappearance with the EDTA standard solution that concentration is C is terminal, 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 × 100;
In formula: M
ca: the molal weight of calcium, g/mol;
M: sample mass, g;
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 concentration of hydrochloric acid is 25%.
Wherein on low temp. electric hot plate at 100 DEG C dissolved samples.
Wherein said triethanolamine concentrations is 12%.
Wherein said potassium hydroxide solution concentration is 20%.
Wherein said Adlerika concentration is 0.5%.
The invention difference from existing technology is that the present invention achieves following technique effect:
1, formulated the assay method of calcium content in calcic aluminium ferromanganese, can be used for production testing, Instructing manufacture technique.
2, stable, accurate, operating process is short, and cost is low, fast, efficiently, is easy to grasp.
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: add hydrochloric acid (25%) and dissolve calcic aluminum-manganese-iron alloy sample in beaker, appropriate amount of deionized water is added in course of dissolution, sample is dissolved completely, and (course of dissolution is very fast, within general tens minutes, just can dissolve completely), take off, after cooling, add 50mL triethanolamine (12%) (must first add, to first the interference element such as iron and aluminium be sheltered), add 50mL water, add oxammonium hydrochloride a little (add the object of oxammonium hydrochloride, play further masking action equally, addition general about 0.5 gram both passable.), (as buffer solution, calcium and EDTA complexing require that pH value is greater than 12, add the pH value of potassium hydroxide (20%) guarantee system to add 30mL potassium hydroxide solution (20%).), (in order to titration end-point is sharp, terminal is good-looking to add several magnesium sulfate (0.5%).), calcein is appropriate, and being titrated to fluorescence green disappearance with EDTA standard solution is terminal.
2. reagent:
2.1 hydrochloric acid (25%)
2.2 oxammonium hydrochlorides (solid)
2.3 triethanolamines (12%)
2.4 potassium hydroxide aqueous solutions (20%)
2.5 calcein indicator: 1g calcein and 100g dry after sodium chloride porphyrize mix, be placed in port grinding bottle for subsequent use.
2.6EDTA standard solution C (EDTA)=0.01783mol/L
2.7 magnesium sulfate solutions (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 0.0500g
5. analytical procedure:
Take calcic aluminum-manganese-iron alloy sample 0.0500g in 300ml beaker, add 20mL hydrochloric acid (25%), dissolved samples on low temperature (100 DEG C) electric hot plate, appropriate amount of deionized water is added in course of dissolution, sample is dissolved completely, (course of dissolution is very fast, within general tens minutes, just can dissolve completely) take off, add 50mL triethanolamine (12%), add 50mL water, add oxammonium hydrochloride a little, add 30mL potassium hydroxide solution (20%), add several magnesium sulfate (0.5%), calcein indicator is appropriate, being titrated to fluorescence green with concentration C (EDTA)=0.01783mol/L standard solution disappears for terminal, meter lower volume is V.
Blank:
In 300ml beaker, add 20mL hydrochloric acid (25%), dissolved samples on low temperature (100 DEG C) electric hot plate, take off after sample dissolves, after cooling, add 50mL triethanolamine (12%), add 50mL water, add oxammonium hydrochloride a little, add 30mL potassium hydroxide solution (20%), add several magnesium sulfate (0.5%), calcein indicator is appropriate, being titrated to fluorescence green disappearance with EDTA standard solution is terminal, and meter lower volume is V
0.
6. Analysis result calculation:
W(Ca)％＝C(V-V
0)M(Ca)100/m×100
In formula: M (Ca): the molal weight (g/mol) of calcium
M: sample mass (g)
C:EDTA concentration of standard solution (mol/L)
V: sample consumes the volume (mL) of EDTA standard solution
V
0: the blank volume (mL) consuming EDTA standard solution
7. standard specimen analysis of control: the comparison of this method measured value and ICP plasma measured value calcium is as table 1:
Table 1 this method measured value and ICP plasma measured value calcium content
| The name of an article | This method measured value (%) | ICP plasma measured value (%) | Extreme difference (%) |
| Calcic aluminium ferromanganese 1 | 5.42 | 5.31 | 0.11 |
| Calcic aluminium ferromanganese 2 | 5.13 | 5.37 | -0.24 |
As can be seen from Table 1: this method measured value is the same with the data of ICP plasma measured value gained, and accurately, and operating process is short, fast, efficient.
Precision is as shown in table 2:
Table 2 low calcium aluminum-manganese-iron alloy sample repetitive measurement data
| The name of an article | Measured value (%) |
| Calcic aluminium ferromanganese 1 | 5.42 5.43 5.42 5.41 5.42 5.45 5.42 5.42 |
As can be seen from Table 2: precision is good.Method has good stability, can meet production requirement.
8. conclusion:
The present invention establishes calcium content in calcic aluminium ferromanganese and carries out the assay method of quantitative test, can be applied in production preferably.Operating process is short, and cost is low, fast, accurately, efficiently, is easy to grasp.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (6)
1. the assay method of calcium content in calcic aluminum-manganese-iron alloy, is characterized in that comprising the following steps:
The calcic aluminum-manganese-iron alloy sample that quality is m is added in one, beaker, another does not add as blank, adds hydrochloric acid respectively afterwards, dissolved samples on low temp. electric hot plate, after sample dissolves, take off, add triethanolamine, water, oxammonium hydrochloride successively respectively after cooling, 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 × 100;
In formula: M
ca: the molal weight of calcium, g/mol;
M: sample mass, g;
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 calcic aluminum-manganese-iron alloy according to claim 1, is characterized in that: described concentration of hydrochloric acid is 25%.
3. the assay method of calcium content in calcic aluminum-manganese-iron 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 calcic aluminum-manganese-iron alloy according to claim 1, is characterized in that: described triethanolamine concentrations is 12%.
5. the assay method of calcium content in calcic aluminum-manganese-iron alloy according to claim 1, is characterized in that: described potassium hydroxide solution concentration is 20%.
6. the assay method of calcium content in calcic aluminum-manganese-iron alloy according to claim 1, is characterized in that: described Adlerika concentration is 0.5%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510260626.0A CN104807814A (en) | 2015-05-20 | 2015-05-20 | Determination method of calcium content in calcium containing ferroaluminium-manganese alloy |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105651930A (en) * | 2016-02-26 | 2016-06-08 | 内蒙古包钢钢联股份有限公司 | Method for determining calcium content of iron-calcium cored wire |
| CN105758852A (en) * | 2016-02-26 | 2016-07-13 | 内蒙古包钢钢联股份有限公司 | Determining method for content of calcium in high-calcium line |
-
2015
- 2015-05-20 CN CN201510260626.0A patent/CN104807814A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105651930A (en) * | 2016-02-26 | 2016-06-08 | 内蒙古包钢钢联股份有限公司 | Method for determining calcium content of iron-calcium cored wire |
| CN105758852A (en) * | 2016-02-26 | 2016-07-13 | 内蒙古包钢钢联股份有限公司 | Determining method for content of calcium in high-calcium line |
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Application publication date: 20150729 |