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
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- manganese
- calcic
- calcium content
- calcium
- aluminum
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- 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%.
Priority Applications (1)
| 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 |
Applications Claiming Priority (1)
| 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 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104807814A true CN104807814A (en) | 2015-07-29 |
Family
ID=53692828
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510260626.0A Pending CN104807814A (en) | 2015-05-20 | 2015-05-20 | Determination method of calcium content in calcium containing ferroaluminium-manganese alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104807814A (en) |
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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104820061A (en) | Measuring method of calcium content in silicon-calcium-barium alloy | |
| CN104819908A (en) | Continuous measuring method of calcium and barium content in silicon-calcium-barium and silicon-aluminum-calcium-barium alloy | |
| CN104297246B (en) | Method for measuring magnesium content in aluminum magnesium alloy powder | |
| CN103115920B (en) | The assay method of iron calcium ratio in a kind of iron-calcium core-spun yarn | |
| CN102213704A (en) | Method for measuring contents of silicon-calcium elements in silicon-calcium alloy | |
| CN103760051A (en) | Method for measuring content of silicon and zirconium in silicon-zirconium alloy | |
| CN104792784A (en) | Continuous determination method for content of calcium oxide and magnesium oxide in blast furnace slag | |
| CN101750408A (en) | Method for measuring contents of aluminum, calcium, barium, strontium and phosphorus in silicon-calcium-barium alloy by ICP (inductively coupled plasma) | |
| CN102128836A (en) | Method for detecting manganese in carbon manganese alloy | |
| CN104833769A (en) | Determination method of calcium oxide content in open-hearth slag, converter slag and electro-furnace slag | |
| CN102565026A (en) | Method for measuring silicon content in aluminum manganese iron | |
| CN105738559A (en) | Method for measuring calcium oxide and magnesium oxide content of tundish covering agent | |
| CN106770512A (en) | The assay method of fluohydric acid content in a kind of nitric hydrofluoric acid type Acidwash solution | |
| CN105092496B (en) | The detection method of phosphorus content in a kind of nitridation reinforcing agent | |
| CN105223146A (en) | A kind of method adopting silicone content in silicon molybdenum blue colorimetric method for determining ferro-silico aluminium | |
| CN105067614A (en) | Method for continuous determination of content of Ca, Mg and Ba in Si-Ca-Ba-Mg alloy | |
| CN104807814A (en) | Determination method of calcium content in calcium containing ferroaluminium-manganese alloy | |
| CN104133035B (en) | Method for measuring content of metal magnesium in briquetting nodulizer by using differential method | |
| CN104819978A (en) | Measuring method of calcium content in silicon-aluminum-calcium-barium alloy | |
| CN104819982A (en) | Determination method for content of calcium in calcium-containing silicon-aluminum alloy | |
| CN104422685A (en) | Method for determining content of metal aluminum in ladle slag modifying agent | |
| CN102928425B (en) | Method for determining vanadium in silicon-vanadium alloy | |
| CN104819977A (en) | Measuring method of calcium content in silicon-calcium alloy | |
| CN108267444A (en) | Method for testing chelating ability of chelating acid to metal calcium ions | |
| CN101660995A (en) | Method of measuring total content of rare earth in rare earth chrome-manganese-silicon inoculant |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150729 |