CN103115920B - The assay method of iron calcium ratio in a kind of iron-calcium core-spun yarn - Google Patents
The assay method of iron calcium ratio in a kind of iron-calcium core-spun yarn Download PDFInfo
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- CN103115920B CN103115920B CN201310030680.7A CN201310030680A CN103115920B CN 103115920 B CN103115920 B CN 103115920B CN 201310030680 A CN201310030680 A CN 201310030680A CN 103115920 B CN103115920 B CN 103115920B
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Abstract
The invention discloses the assay method of iron calcium ratio in a kind of iron-calcium core-spun yarn, comprising: configuration standard solution, described standard solution comprises calcium standard solution and EDTA standard solution, and calculates the concentration C of EDTA standard solution; With the iron powder in magnet separation of iron calcium powder and calcium grain, in the iron powder be separated, add water and described EDTA standard solution, prepare sample solution; With sample solution described in described calcium standard solution titration, according to the concentration C of calcium standard solution concentration and EDTA standard solution, calculate the iron calcium ratio of iron calcium powder in core-spun yarn.Utilize technical solution of the present invention can iron calcium ratio in Accurate Determining iron-calcium core-spun yarn, and easy and simple to handle.
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
Along with the exploitation with new steel grade of updating of process for making, the application of novel deoxidizer for use is also more and more wider, iron-calcium core-spun yarn is exactly one wherein, current refining low-silicon steel technology controlling and process adopts iron-calcium core-spun yarn deoxidation, and therefore the iron calcium of accurate analysis iron-calcium core-spun yarn is the important step controlling final products than content.Traditional analysis complex operation step, needs to consume a large amount of chemicalss, while causing final measuring error larger, and environmental protection not enough, energy-conservation.
Summary of the invention
The object of this invention is to provide the assay method of iron calcium ratio in a kind of iron-calcium core-spun yarn, can iron calcium ratio in Accurate Determining iron-calcium core-spun yarn, and easy and simple to handle.
Technical scheme is specific as follows:
An assay method for iron calcium ratio in iron-calcium core-spun yarn, comprising:
Configuration standard solution, described standard solution comprises calcium standard solution and ethylenediamine tetraacetic acid (EthyleneDiamine Tetraacetic Acid, EDTA) standard solution, described calcium standard solution concentration is C1, and calculates the concentration C of EDTA standard solution;
With the iron powder in magnet separation of iron calcium powder and calcium grain, in the iron powder be separated, add water and described EDTA standard solution, prepare sample solution; 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, beaker bottom is placed on magnet, iron powder is separated with calcium grain, calcium grain after separation is put into the beaker of another drying, with magnet multipass separating calcium grain, to prevent from being mixed with iron powder in calcium grain, weigh the mixing iron powder after being separated and calcium grain respectively, quality is respectively G
1and G
2; In the preparation process of described sample solution, fill in the beaker of iron powder after separation and add 100mL water, when reacting phenomenon is not obvious, illustrate that in iron powder, calcium grain content is low, need first add 20mL potassium hydroxide aqueous solution; Indicator is added after reacting completely, drip EDTA standard solution again until the solution in beaker becomes stable blue look, or without white depositions in solution, then adding 5mL EDTA standard solution, the volume markings of EDTA standard solution used is V, filter immediately, filtrate puts into 500mL volumetric flask, washes 7 ~ 8 precipitations and filter paper with water, is diluted with water to scale, mixing, obtained sample solution; Divide and get 50mL sample solution in 250mL beaker, add 80mL water, 0.2g oxammonium hydrochloride, 3mL volume ratio are triethanolamine aqueous solution, the 20mL potassium hydroxide aqueous solution of 1:4,1mL magnesium sulfate solution, drip indicator, be titrated to solution with calcium standard solution and become redness, the consumption of record calcium standard solution, is labeled as V
2; 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;
C
1---the concentration of-calcium standard solution, mol/L;
V
2---the volume of the calcium standard solution consumed during-titration, mL;
The molal weight of M----calcium, 40.08g/mol;
Point 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;
G
1the quality of the mixing iron powder after----be separated, g;
W (Ca)---the calcium content in-iron powder, g;
The computing formula of iron calcium ratio:
W(Fe):[G
2+W(Ca)]；
With sample solution described in 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 and be cooled to the calcium carbonate of room temperature prior to 105 ~ 110 DEG C of dry 1h in advance, add appropriate cold boil water and drip the aqueous hydrochloric acid solution that volume ratio is 1:1, it is made to dissolve completely, then be diluted in 1000m L volumetric flask by cold boil water, be mixed with the calcium standard solution that concentration C 1 is 0.1500mol/L; In the process for preparation of described EDTA standard solution, take EDTA 186.1200 grams in 1000mL volumetric flask, add 30 grams of potassium hydroxide, be dissolved in water and be diluted with water to scale, shaking up, obtained EDTA standard solution.
Further, pipette 20.00mL calcium standard solution and be placed in 250mL beaker, add water 80mL, potassium hydroxide aqueous solution 20mL, magnesium sulfate solution 1mL, hydroxylammonium chloride 0.2g, indicator 0.5g, obtained at least two parts of mixed solutions, drop to that blue look constant is terminal respectively with above-mentioned EDTA standard solution, record EDTA standard solution consumption, and calculate the mean value of consumption, be labeled as V20;
Blank test: in the 250mL beaker of sky, add water 80mL, potassium hydroxide aqueous solution 20mL, magnesium sulfate solution 1mL, hydroxylammonium chloride 0.2g, indicator 0.5g, drop to EDTA standard solution that blue look constant is terminal, record EDTA standard solution consumption, is 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;
The volume of V1-point to get calcium standard solution, mL;
V20-titration consumes the average external volume of EDTA standard solution, mL;
V0-titer reagent blank consumes the volume of EDTA standard solution, mL.
Further, described indicator is mass ratio is the calcon-carboxylic acid of 1:100 and the potpourri of sodium chloride.
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, calcium grain most in iron calcium powder being separated with iron powder, with EDTA standard solution, the calcium grain remained in iron powder being separated with iron powder, measuring the calcium amount after being separated, by calculating the calcium ratio that taps a blast furnace with calcium standard solution.
2, environmental protection; Utilize magnet to be separated iron powder, shorten analytical procedure, saved large chemicals, there is the advantage 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 and be cooled to the calcium carbonate of room temperature prior to 105 ~ 110 DEG C of dry 1h in advance, add appropriate cold boil water and drip the aqueous hydrochloric acid solution that volume ratio is 1:1, it is made to dissolve completely, then be diluted in 1000m L volumetric flask by cold boil water, be mixed with the calcium standard solution that concentration is 0.1500mol/L.
The preparation of indicator: 1g calcon-carboxylic acid and 100g dry after sodium chloride porphyrize mix, be placed in port grinding bottle for subsequent use.
The preparation of EDTA standard solution and the calculating of concentration C thereof:
Preparation: take EDTA 186.1200 grams in 1000mL volumetric flask, add 30 grams of potassium hydroxide, be dissolved in water and be diluted with water to scale, shaking up, obtained EDTA standard solution is for subsequent use.
Demarcate: pipette three parts of 20.00mL calcium standard solutions respectively and be placed in 250mL beaker, add water 80mL, potassium hydroxide aqueous solution 20mL, magnesium sulfate solution 1mL, hydroxylammonium chloride 0.2g, indicator 0.5g, obtained three parts of mixed solutions, drop to that blue look constant is terminal respectively with above-mentioned EDTA standard solution, record EDTA standard solution consumption, and calculate the mean value of consumption, be labeled as V
20.
Blank test: in the 250mL beaker of sky, add water 80mL, potassium hydroxide aqueous solution 20mL, magnesium sulfate solution 1mL, hydroxylammonium chloride 0.2g, indicator 0.5g, drop to above-mentioned EDTA standard solution that blue look constant is terminal, record EDTA standard solution consumption, is 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-point to get the volume of calcium standard solution, mL;
V
20-titration consumes the average external volume of EDTA standard solution, mL;
V
0-titer reagent blank consumes the volume of EDTA standard solution, mL.
Step 2: be separated iron powder and calcium grain with magnet, prepare sample solution;
In the present invention, have chosen 1
#, 2
#, 3
#, 4
#, 5
#, 6
#totally 6 kinds of iron-calcium core-spun yarn samples.
Be separated iron powder and calcium grain: clip 10 ~ 20cm iron-calcium core-spun yarn, iron calcium powder in core-spun yarn taken out, weighs, be accurate to 0.01g.Iron calcium powder after weighing is poured in the beaker of 400mL drying, beaker bottom is placed on the magnet that magnetic field intensity is 1000 oersteds, iron powder is separated with calcium grain, calcium grain after separation is put into the beaker of another drying, with magnet multipass separating calcium grain, to prevent from being mixed with iron powder in calcium grain, weigh the mixing iron powder after being separated and calcium grain respectively, be accurate to 0.01g, quality is respectively G1, G2.
The preparation of sample solution: fill in the beaker of iron powder after separation and add 100mL water, when reacting phenomenon is not obvious, illustrate that in iron powder, calcium grain content is low, need first add 20mL potassium hydroxide aqueous solution.Appropriate indicator is added after reacting completely, drip EDTA standard solution again until the solution in beaker becomes stable blue look, or without white depositions in solution, then add 5mL EDTA standard solution, the volume markings of EDTA standard solution used is V, filter immediately, filtrate puts into 500mL volumetric flask, washes 7 ~ 8 precipitations and filter paper with water, is diluted with water to scale, mixing, obtained sample solution.So just obtain 1
#, 2
#, 3
#, 4
#, 5
#, 6
#totally 6 kinds of sample solutions.
Blank test: add 100mL water in empty beaker, adds the indicator with above-mentioned steps moderate, then drips EDTA standard solution until the solution in beaker becomes stable blue look, add 5mL EDTA standard solution again, put into 500mL volumetric flask, be diluted with water to scale, mixing.
Step 3: with calcium standard solution titration sample solution, and calculate the iron calcium ratio of iron calcium powder in core-spun yarn;
Divide and get 50mL sample solution in 250mL beaker, add 80mL water, 0.2g oxammonium hydrochloride, 3mL volume ratio are triethanolamine aqueous solution, the 20mL potassium hydroxide aqueous solution of 1:4,1mL magnesium sulfate solution, add appropriate indicator again, be titrated to solution with calcium standard solution and become redness, the consumption of record calcium standard solution, is 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 consumed during V2----titration, mL;
The molal weight of M----calcium, 40.08g/mol;
Point liquid proportional of K----sample solution, divides in the present embodiment and gets 50mL, so K=1/10 from 500mL sample solution.
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----is separated, 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 sample is as shown in table 1 according to the measurement result of measuring method of the present invention.
Table 1
Claims (5)
1. the assay method of iron calcium ratio in iron-calcium core-spun yarn, comprising:
Configuration standard solution, described standard solution comprises calcium standard solution and edta edta standard solution, and described calcium standard solution concentration is C
1, and calculate the concentration C of EDTA standard solution;
With the iron powder in magnet separation of iron calcium powder and calcium grain, in the iron powder be separated, add water and described EDTA standard solution, prepare sample solution A; In the preparation process of described sample solution A, 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, beaker bottom is placed on magnet, iron powder is separated with calcium grain, calcium grain after separation is put into the beaker of another drying, with magnet multipass separating calcium grain, to prevent from being mixed with iron powder in calcium grain, weigh the mixing iron powder after being separated and calcium grain respectively, quality is respectively G
1and G
2; Fill in the beaker of iron powder after separation and add 100mL water, when reacting phenomenon is not obvious, illustrate that in iron powder, calcium grain content is low, need first add 20mL potassium hydroxide aqueous solution; Indicator is added after reacting completely, drip EDTA standard solution again until the solution in beaker becomes stable blue look, or without white depositions in solution, then adding 5mL EDTA standard solution, the volume markings of EDTA standard solution used is V, filter immediately, filtrate puts into 500mL volumetric flask, washes 7 ~ 8 precipitations and filter paper with water, is diluted with water to scale, mixing, obtained sample solution A;
With sample solution A described in described calcium standard solution titration, according to 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; Divide and get 50mL sample solution A in 250mL beaker, add 80mL water, 0.2g oxammonium hydrochloride, 3mL volume ratio are triethanolamine aqueous solution, the 20mL potassium hydroxide aqueous solution of 1:4,1mL magnesium sulfate solution, drip indicator, be titrated to solution with calcium standard solution and become redness, the consumption of record calcium standard solution, is labeled as V
2; 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;
C
1---the concentration of-calcium standard solution, mol/L;
V
2---the volume of the calcium standard solution consumed during-titration, mL;
The molal weight of M----calcium, 40.08g/mol;
Point liquid proportional of K----sample solution A;
The computing formula of iron powder quality:
W(Fe)＝G
1-W(Ca)
In formula: W (Fe)---the quality of-iron powder, g;
G
1the quality of the mixing iron powder after----be separated, g;
W (Ca)---the calcium content in-iron powder, g;
The computing formula of iron calcium ratio:
W(Fe):[G
2+W(Ca)]。
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 and be cooled to the calcium carbonate of room temperature prior to 105 ~ 110 DEG C of dry 1h in advance, add appropriate cold boil water and drip the aqueous hydrochloric acid solution that volume ratio is 1:1, it is made to dissolve completely, then be diluted in 1000mL volumetric flask by cold boil water, be mixed with concentration C
1for the calcium standard solution of 0.1500mol/L; In the process for preparation of described EDTA standard solution, take EDTA 186.1200 grams in 1000mL volumetric flask, add 30 grams of potassium hydroxide, be dissolved in water and be diluted with water to scale, shaking up, obtained EDTA standard solution.
3. the assay method of iron calcium ratio in iron-calcium core-spun yarn as claimed in claim 2, it is characterized in that: pipette 20.00mL calcium standard solution and be placed in 250mL beaker, add water 80mL, potassium hydroxide aqueous solution 20mL, magnesium sulfate solution 1mL, hydroxylammonium chloride 0.2g, indicator 0.5g, obtained at least two parts of mixed solutions, drop to that blue look constant is terminal respectively with above-mentioned EDTA standard solution, record EDTA standard solution consumption, and calculate the mean value of consumption, be labeled as V
20;
Blank test; In the 250mL beaker of sky, add water 80mL, potassium hydroxide aqueous solution 20mL, magnesium sulfate solution 1mL, hydroxylammonium chloride 0.2g, indicator 0.5g, drops to that blue look constant is terminal with EDTA standard solution, and record 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-point to get the volume of calcium standard solution, mL;
V
20-titration consumes the average external volume of EDTA standard solution, mL;
V
0-titer reagent blank consumes the volume of EDTA standard solution, mL.
4. the assay method of iron calcium ratio in iron-calcium core-spun yarn as claimed in claim 3, is characterized in that: described indicator is mass ratio is the calcon-carboxylic acid of 1:100 and the potpourri of sodium chloride.
5. the assay method of iron calcium ratio in iron-calcium core-spun yarn as claimed in claim 1, is characterized in that: the value of described K is 1/10.
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| 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 |
| GB201521518D0 (en) * | 2015-12-07 | 2016-01-20 | Injection Alloys Ltd | Wire for refining molten metal |
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| 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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