CN103115920A - Method for measuring iron/calcium ratio in iron-calcium core-spun yarn - Google Patents
Method for measuring iron/calcium ratio in iron-calcium core-spun yarn Download PDFInfo
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Abstract
The invention discloses a method for measuring iron/calcium ratio in an iron-calcium core-spun yarn, which comprises the following steps: preparing standard solutions which comprise a calcium standard solution and an EDTA (ethylene diamine tetraacetic acid) standard solution, and calculating the concentration C of the EDTA standard solution; separating iron powder and calcium particles in the iron-calcium powder with a magnet, and adding water and the EDTA standard solution into the separated iron powder to prepare a sample solution; and titrating the sample solution with the calcium standard solution, and calculating the iron/calcium ratio in the iron-calcium core-spun yarn according to the concentration of the calcium standard solution and the concentration C of the EDTA standard solution. The technical scheme disclosed by the invention can be used for accurately measuring the iron/calcium ratio in the iron-calcium core-spun yarn, and is simple to operate.
Description
Technical field
The present invention relates to technical field of ferrous metallurgical analysis, particularly relate to the assay method of iron calcium ratio in a kind of iron-calcium core-spun yarn.
Background technology
The exploitation with new steel grade updated along with process for making, the application of novel deoxidizer for use is also more and more wider, iron-calcium core-spun yarn is exactly wherein a kind of, refining low-silicon steel technology controlling and process adopts the iron-calcium core-spun yarn deoxidation at present, so the iron calcium ratio content of accurate analysis iron-calcium core-spun yarn is the important step of controlling final products.The traditional analysis complex operation step needs to consume a large amount of chemicalss, when causing final measuring error larger, and environmental protection not enough, energy-conservation.
Summary of the invention
The assay method that the purpose of this invention is to provide iron calcium ratio in a kind of iron-calcium core-spun yarn, the iron calcium ratio in can the Accurate Determining iron-calcium core-spun yarn, and easy and simple to handle.
Technical scheme is specific as follows:
The assay method of iron calcium ratio in a kind of iron-calcium core-spun yarn comprises:
Configuration standard solution, described standard solution comprise calcium standard solution and ethylenediamine tetraacetic acid (Ethylene Diamine Tetraacetic Acid, EDTA) standard solution, and described calcium standard solution concentration is C1, and calculate the concentration C of EDTA standard solution;
With the iron powder in magnet separation of iron calcium powder and calcium grain, add entry and described EDTA standard solution in the iron powder that separates, the preparation sample solution;
With the described sample solution of described calcium standard solution titration, according to the concentration C of calcium standard solution concentration C 1 and EDTA standard solution, obtain the iron calcium ratio of iron calcium powder in core-spun yarn.
Further, in the process for preparation of described calcium standard solution, take 15.0000g in advance prior to 105～110 ℃ of dry 1h and be cooled to the calcium carbonate of room temperature, add appropriate cold boil water and drip the aqueous hydrochloric acid solution that volume ratio is 1:1, it is dissolved fully, then be diluted in 1000m L volumetric flask with cold boil water, be mixed with concentration C 1 and be the calcium standard solution of 0.1500mol/L.
Further, in the process for preparation of described EDTA standard solution, take EDTA 186.1200 grams to the 1000mL volumetric flask, add 30 gram potassium hydroxide, be dissolved in water and be diluted with water to scale, shake up, make the EDTA standard solution.
Further, pipette the 20.00mL calcium standard solution and be placed in the 250mL beaker, add water 80mL, potassium hydroxide aqueous solution 20mL, magnesium sulfate solution 1mL, hydrochloric acid hydroxylammonium 0.2g, indicator 0.5g makes at least two parts of mixed solutions, drop to the blue look constant terminal point that is with above-mentioned EDTA standard solution respectively, record EDTA standard solution consumption, and calculate the mean value of consumption, be labeled as V20;
Blank test: in the 250mL of sky beaker, add water 80mL, potassium hydroxide aqueous solution 20mL, magnesium sulfate solution 1mL, hydrochloric acid hydroxylammonium 0.2g, indicator 0.5g, drop to the blue look constant terminal point that is with the EDTA standard solution, record EDTA standard solution consumption, be labeled as V0;
Be calculated as follows the concentration C of EDTA standard solution:
In formula: C
1The concentration of-calcium standard solution, mol/L;
V1-minute the get volume of calcium standard solution, mL;
V20-titration consumes the average external volume of EDTA standard solution, mL;
V0-titration reagent blank consumes the volume of EDTA standard solution, mL.
Further, described indicator is that mass ratio is the calcon-carboxylic acid of 1:100 and the potpourri of sodium chloride.
Further, clip 10～20cm iron-calcium core-spun yarn takes out iron calcium powder in core-spun yarn, weighs; Iron calcium powder after weighing is poured in the beaker of 400mL drying, be placed on beaker bottom with magnet, iron powder is separated with the calcium grain, calcium grain after separating is put into another dry beaker, available magnet multipass separating calcium grain, to prevent being mixed with iron powder in the calcium grain, mixing iron powder and calcium grain after weighing separates respectively, quality is respectively G
1, G
2
Further, in the preparation process of described sample solution, add 100mL water in the beaker that separates rear dress iron powder, not obvious when reacting phenomenon, illustrate that in iron powder, calcium grain content is low, need first add the 20mL potassium hydroxide aqueous solution; Add indicator after reacting completely, drip again the EDTA standard solution and stablize blue look until the solution in beaker becomes, or in solution without white depositions, then add 5mL EDTA standard solution, the volume markings of EDTA standard solution used is V, filter immediately, filtrate is put into the 500mL volumetric flask, washes 7～8 times with water and precipitates and filter paper, is diluted with water to scale, mixing makes sample solution.
Further, divide and get the 50mL sample solution in the 250mL beaker, add 80mL water, 0.2g oxammonium hydrochloride, 3mL volume ratio are triethanolamine aqueous solution, the 20mL potassium hydroxide aqueous solution of 1:4, the 1mL magnesium sulfate solution drips indicator, is titrated to solution with calcium standard solution and becomes redness, record the consumption of calcium standard solution, be labeled as V
2
Further, the computing formula of calcium content in iron powder:
W(Ca)=[(C×V）×K-(C
1×V
2)]M×1/K×10
-3
In formula: W (Ca)---the content of calcium in-mixing iron powder, g;
The concentration of C----EDTA standard solution, mol/L;
V----adds the volume of EDTA standard solution, mL;
The concentration of C1----calcium standard solution, mol/L;
The volume of the calcium standard solution that consumes during the V2----titration, mL;
The molal weight of M----calcium, 40.08g/mol;
Minute liquid proportional of K----sample solution;
The computing formula of iron powder quality:
W(Fe)=G
1-W(Ca)
In formula: W (Fe)---the quality of-iron powder, g;
The quality of the mixing iron powder after G1----separates, g;
W (Ca)---the calcium content in-iron powder, g;
The computing formula of iron calcium ratio:
W(Fe):[G
2+W(Ca)]。
Further, the value of described K is 1/10.
Beneficial effect of the present invention:
1, principle is reasonable, easy and simple to handle; With magnet, most calcium grain in the iron calcium powder is separated with iron powder, with the EDTA standard solution, calcium grain residual in iron powder is separated with iron powder, the calcium amount after separating with calcium standard solution mensuration is by calculating the calcium ratio that taps a blast furnace.
2, environmental protection; Utilize magnet to separate iron powder, shortened analytical procedure, saved large chemicals, have advantages of energy-saving and environmental protection.
Embodiment
In the present invention, agents useful for same is preferred: potassium hydroxide aqueous solution concentration is 200g/L; Magnesium sulfate solution concentration is 5g/L.
In iron-calcium core-spun yarn, the determination step of iron calcium ratio is as follows:
Step 1: configuration standard solution, and calculate EDTA concentration of standard solution C;
The preparation of calcium standard solution: take 15.0000g in advance prior to 105～110 ℃ of dry 1h and be cooled to the calcium carbonate of room temperature, add appropriate cold boil water and drip the aqueous hydrochloric acid solution that volume ratio is 1:1, it is dissolved fully, then be diluted in 1000m L volumetric flask with cold boil water, be mixed with the calcium standard solution that concentration is 0.1500mol/L.
The preparation of indicator: the sodium chloride porphyrize mixing after 1g calcon-carboxylic acid and 100g oven dry is placed in port grinding bottle standby.
The preparation of EDTA standard solution and the calculating of concentration C thereof:
Preparation: take EDTA 186.1200 grams to the 1000mL volumetric flask, add 30 gram potassium hydroxide, be dissolved in water and be diluted with water to scale, shake up, make the EDTA standard solution standby.
Demarcate: pipette respectively three parts of 20.00mL calcium standard solutions and be placed in the 250mL beaker, add water 80mL, potassium hydroxide aqueous solution 20mL, magnesium sulfate solution 1mL, hydrochloric acid hydroxylammonium 0.2g, indicator 0.5g, make three parts of mixed solutions, drop to the blue look constant terminal point that is with above-mentioned EDTA standard solution respectively, record EDTA standard solution consumption, and the mean value of calculating consumption, be labeled as V
20
Blank test: in the 250mL of sky beaker, add water 80mL, potassium hydroxide aqueous solution 20mL, magnesium sulfate solution 1mL, hydrochloric acid hydroxylammonium 0.2g, indicator 0.5g, drop to the blue look constant terminal point that is with above-mentioned EDTA standard solution, record EDTA standard solution consumption, be labeled as V
0
Be calculated as follows the concentration of EDTA standard solution:
In formula: C
1The concentration of-calcium standard solution, mol/L;
V
1-minute get the volume of calcium standard solution, mL;
V
20-titration consumes the average external volume of EDTA standard solution, mL;
V
0-titration reagent blank consumes the volume of EDTA standard solution, mL.
Step 2: separate iron powder and calcium grain with magnet, the preparation sample solution;
In the present invention, chosen 1
#, 2
#, 3
#, 4
#, 5
#, 6
#Totally 6 kinds of iron-calcium core-spun yarn samples.
Separate iron powder and calcium grain: clip 10～20cm iron-calcium core-spun yarn, iron calcium powder in core-spun yarn is taken out, weigh, be accurate to 0.01g.Iron calcium powder after weighing is poured in the beaker of 400mL drying, the magnet that is 1000 oersteds with magnetic field intensity is placed on beaker bottom, iron powder is separated with the calcium grain, calcium grain after separating is put into another dry beaker, with magnet multipass separating calcium grain, to prevent being mixed with iron powder in the calcium grain, mixing iron powder and calcium grain after weighing separates respectively, be accurate to 0.01g, quality is respectively G1, G2.
The preparation of sample solution: add 100mL water in the beaker that separates rear dress iron powder, not obvious when reacting phenomenon, illustrate that in iron powder, calcium grain content is low, need first add the 20mL potassium hydroxide aqueous solution.Add appropriate indicator after reacting completely, drip again the EDTA standard solution and stablize blue look until the solution in beaker becomes, or in solution without white depositions, then add 5mL EDTA standard solution, the volume markings of EDTA standard solution used is V, filter immediately, filtrate is put into the 500mL volumetric flask, washes 7～8 times with water and precipitates and filter paper, is diluted with water to scale, mixing makes sample solution.So just obtained 1
#, 2
#, 3
#, 4
#, 5
#, 6
#Totally 6 kinds of sample solutions.
Blank test: add 100mL water in empty beaker, add the indicator with the above-mentioned steps moderate, then drip the EDTA standard solution and stablize blue look until the solution in beaker becomes, add again 5mL EDTA standard solution, put into the 500mL volumetric flask, be diluted with water to scale, mixing.
Step 3: use calcium standard solution titration sample solution, and calculate the iron calcium ratio of iron calcium powder in core-spun yarn;
Divide and get the 50mL sample solution in the 250mL beaker, add 80mL water, 0.2g oxammonium hydrochloride, 3mL volume ratio are triethanolamine aqueous solution, the 20mL potassium hydroxide aqueous solution of 1:4, the 1mL magnesium sulfate solution, add again appropriate indicator, be titrated to solution with calcium standard solution and become redness, record the consumption of calcium standard solution, be labeled as V
2
The calculating of calcium content in iron powder:
W(Ca)=[(C×V）×K-(C
1×V
2)]M×1/K×10
-3
In formula: W (Ca)---the content of calcium in-mixing iron powder, g;
The concentration of C----EDTA standard solution, mol/L;
V----adds the volume of EDTA standard solution, mL;
The concentration of C1----calcium standard solution, mol/L;
The volume of the calcium standard solution that consumes during the V2----titration, mL;
The molal weight of M----calcium, 40.08g/mol;
Minute liquid proportional of K----sample solution divides from the 500mL sample solution in the present embodiment and gets 50mL, so K=1/10.
The calculating of iron powder quality:
W(Fe)=G
1-W(Ca)
In formula: W (Fe)---the quality of-iron powder, g;
The quality of the mixing iron powder after G1----separates, g;
W (Ca)---the calcium content in-iron powder, g.
The calculating of iron calcium ratio:
W(Fe):[G
2+W(Ca)]
Different iron-calcium core-spun yarn samples are as shown in table 1 according to the measurement result of measuring method of the present invention.
Table 1
Claims (10)
1. the assay method of iron calcium ratio in an iron-calcium core-spun yarn comprises:
Configuration standard solution, described standard solution comprise calcium standard solution and edta edta standard solution, and described calcium standard solution concentration is C
1, and the concentration C of calculating EDTA standard solution;
With the iron powder in magnet separation of iron calcium powder and calcium grain, add entry and described EDTA standard solution in the iron powder that separates, the preparation sample solution;
With the described sample solution of described calcium standard solution titration, according to the calcium standard solution concentration C
1With the concentration C of EDTA standard solution, obtain the iron calcium ratio of iron calcium powder in core-spun yarn.
2. the assay method of iron calcium ratio in iron-calcium core-spun yarn as claimed in claim 1, it is characterized in that: in the process for preparation of described calcium standard solution, take 15.0000g in advance prior to 105～110 ℃ of dry 1h and be cooled to the calcium carbonate of room temperature, add appropriate cold boil water and drip the aqueous hydrochloric acid solution that volume ratio is 1:1, it is dissolved fully, then be diluted in 1000m L volumetric flask with cold boil water, be mixed with concentration C
1Calcium standard solution for 0.1500mol/L.
3. the assay method of iron calcium ratio in iron-calcium core-spun yarn as claimed in claim 2, it is characterized in that: in the process for preparation of described EDTA standard solution, take EDTA 186.1200 grams to the 1000mL volumetric flask, add 30 gram potassium hydroxide, be dissolved in water and be diluted with water to scale, shake up, make the EDTA standard solution.
4. the assay method of iron calcium ratio in iron-calcium core-spun yarn as claimed in claim 3, it is characterized in that: pipette the 20.00mL calcium standard solution and be placed in the 250mL beaker, add water 80mL, potassium hydroxide aqueous solution 20mL, magnesium sulfate solution 1mL, hydrochloric acid hydroxylammonium 0.2g, indicator 0.5g makes at least two parts of mixed solutions, drop to the blue look constant terminal point that is with above-mentioned EDTA standard solution respectively, record EDTA standard solution consumption, and calculate the mean value of consumption, be labeled as V
20
Blank test; In the 250mL of sky beaker, add water 80mL, potassium hydroxide aqueous solution 20mL, magnesium sulfate solution 1mL, hydrochloric acid hydroxylammonium 0.2g, indicator 0.5g drops to the blue look constant terminal point that is with the EDTA standard solution, records EDTA standard solution consumption, is labeled as V
0
Be calculated as follows the concentration C of EDTA standard solution:
In formula: C
1The concentration of-calcium standard solution, mol/L;
V
1-minute get the volume of calcium standard solution, mL;
V
20-titration consumes the average external volume of EDTA standard solution, mL;
V
0-titration reagent blank consumes the volume of EDTA standard solution, mL.
5. the assay method of iron calcium ratio in iron-calcium core-spun yarn as claimed in claim 4, it is characterized in that: described indicator is that mass ratio is the calcon-carboxylic acid of 1:100 and the potpourri of sodium chloride.
6. the assay method of iron calcium ratio in iron-calcium core-spun yarn as claimed in claim 1 is characterized in that: in the preparation process of described sample solution, clip 10～20cm iron-calcium core-spun yarn takes out iron calcium powder in core-spun yarn, weighs; Iron calcium powder after weighing is poured in the beaker of 400mL drying, be placed on beaker bottom with magnet, iron powder is separated with the calcium grain, calcium grain after separating is put into another dry beaker, with magnet multipass separating calcium grain, to prevent being mixed with iron powder in the calcium grain, mixing iron powder and calcium grain after weighing separates respectively, quality is respectively G
1And G
2
7. the assay method of iron calcium ratio in iron-calcium core-spun yarn as claimed in claim 6, it is characterized in that: in the preparation process of described sample solution, add 100mL water in the beaker that separates rear dress iron powder, when reacting phenomenon not obvious, illustrate that in iron powder, calcium grain content is low, need first add the 20mL potassium hydroxide aqueous solution; Add indicator after reacting completely, drip again the EDTA standard solution and stablize blue look until the solution in beaker becomes, or in solution without white depositions, then add 5mL EDTA standard solution, the volume markings of EDTA standard solution used is V, filter immediately, filtrate is put into the 500mL volumetric flask, washes 7～8 times with water and precipitates and filter paper, is diluted with water to scale, mixing makes sample solution.
8. the assay method of iron calcium ratio in iron-calcium core-spun yarn as claimed in claim 7, it is characterized in that: divide and get the 50mL sample solution in the 250mL beaker, add 80mL water, 0.2g oxammonium hydrochloride, 3mL volume ratio are triethanolamine aqueous solution, the 20mL potassium hydroxide aqueous solution of 1:4, the 1mL magnesium sulfate solution drips indicator, is titrated to solution with calcium standard solution and becomes redness, record the consumption of calcium standard solution, be labeled as V
2
9. the assay method of iron calcium ratio in iron-calcium core-spun yarn as claimed in claim 8, it is characterized in that: in iron powder, the computing formula of calcium content is:
W(Ca)=[(C×V）×K-(C
1×V
2)]M×1/K×10
-3
In formula: W (Ca)---the content of calcium in-mixing iron powder, g;
The concentration of C----EDTA standard solution, mol/L;
V----adds the volume of EDTA standard solution, mL;
The concentration of C1----calcium standard solution, mol/L;
The volume of the calcium standard solution that consumes during the V2----titration, mL;
The molal weight of M----calcium, 40.08g/mol;
Minute liquid proportional of K----sample solution;
The computing formula of iron powder quality:
W(Fe)=G
1-W(Ca)
In formula: W (Fe)---the quality of-iron powder, g;
The quality of the mixing iron powder after G1----separates, g;
W (Ca)---the calcium content in-iron powder, g;
The computing formula of iron calcium ratio:
W(Fe):[G
2+W(Ca)]。
10. the assay method of iron calcium ratio in iron-calcium core-spun yarn as claimed in claim 9, it is characterized in that: the value of described K is 1/10.
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Cited By (7)
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| CN103411968A (en) * | 2013-07-31 | 2013-11-27 | 南京梅山冶金发展有限公司 | Method for detecting total iron content of steel slag |
| CN103512879A (en) * | 2013-09-16 | 2014-01-15 | 内蒙古包钢钢联股份有限公司 | Complexometry joint measurement method for calcium, barium and magnesium contents in silico-calcium barium magnesium alloy |
| CN106290346A (en) * | 2016-09-29 | 2017-01-04 | 浙江达美生物技术有限公司 | Mensuration reagent of superoxide dismutase and preparation method thereof |
| CN106834601A (en) * | 2015-12-07 | 2017-06-13 | 因杰克什阿卢易斯有限公司 | For the line of refining molten metal |
| CN109613172A (en) * | 2018-11-12 | 2019-04-12 | 包头钢铁（集团）有限责任公司 | Iron calcium compares measuring method in a kind of iron-calcium core-spun yarn |
| CN109612959A (en) * | 2018-11-12 | 2019-04-12 | 包头钢铁（集团）有限责任公司 | Carbon, test methods of sulphur contents in reduced iron powder in a kind of iron-calcium core-spun yarn |
| CN109612980A (en) * | 2018-11-12 | 2019-04-12 | 包头钢铁（集团）有限责任公司 | Silicon, manganese, method for measuring phosphor content in reduced iron powder in a kind of iron-calcium core-spun yarn |
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Cited By (9)
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| CN103411968A (en) * | 2013-07-31 | 2013-11-27 | 南京梅山冶金发展有限公司 | Method for detecting total iron content of steel slag |
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| CN103512879A (en) * | 2013-09-16 | 2014-01-15 | 内蒙古包钢钢联股份有限公司 | Complexometry joint measurement method for calcium, barium and magnesium contents in silico-calcium barium magnesium alloy |
| CN103512879B (en) * | 2013-09-16 | 2016-06-01 | 内蒙古包钢钢联股份有限公司 | The method of calcium, barium, Mg content in Si Si bond surveyed by a kind of complexometric titration connection |
| CN106834601A (en) * | 2015-12-07 | 2017-06-13 | 因杰克什阿卢易斯有限公司 | For the line of refining molten metal |
| CN106290346A (en) * | 2016-09-29 | 2017-01-04 | 浙江达美生物技术有限公司 | Mensuration reagent of superoxide dismutase and preparation method thereof |
| CN109613172A (en) * | 2018-11-12 | 2019-04-12 | 包头钢铁（集团）有限责任公司 | Iron calcium compares measuring method in a kind of iron-calcium core-spun yarn |
| CN109612959A (en) * | 2018-11-12 | 2019-04-12 | 包头钢铁（集团）有限责任公司 | Carbon, test methods of sulphur contents in reduced iron powder in a kind of iron-calcium core-spun yarn |
| CN109612980A (en) * | 2018-11-12 | 2019-04-12 | 包头钢铁（集团）有限责任公司 | Silicon, manganese, method for measuring phosphor content in reduced iron powder in a kind of iron-calcium core-spun yarn |
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