CN104330521A - Method for determining content of calcium oxide in raw and auxiliary metallurgical materials - Google Patents
Method for determining content of calcium oxide in raw and auxiliary metallurgical materials Download PDFInfo
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- CN104330521A CN104330521A CN201410609306.7A CN201410609306A CN104330521A CN 104330521 A CN104330521 A CN 104330521A CN 201410609306 A CN201410609306 A CN 201410609306A CN 104330521 A CN104330521 A CN 104330521A
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Abstract
The invention discloses a method for determining the content of calcium oxide in raw and auxiliary metallurgical materials. The method comprises the following steps: firstly, according to the sample name of the calcium oxide in the raw and auxiliary materials needing to be determined, selecting a plurality of standard samples of which the variety is the same as that of the sample; secondly, selecting one of the standard samples, and determining the content of the calcium oxide by virtue of a fully-automatic potentiometric titrator, selecting the other standard samples respectively, and determining the content of the calcium oxide in the same way to obtain respective calcium oxide content determination values; thirdly, automatically determining a regression curve equation of a correction value by virtue of linear regression calculation software according to obtained standard calcium oxide content values in the standard samples and the respective calcium oxide content determination values; finally, operating a to-be-determined sample according to the steps, inputting various obtained data into the regression curve equation of the correction value, so that a content correction value of the calcium oxide in a to-be-determined calcium-containing sample can be obtained by calculation. The practice proves that the method is easy to operate and a determination result is high in accuracy.
Description
Technical field
The invention belongs to metallurgical material analysis technical field, specifically refer to the assay method of calcium oxide content in a kind of metallurgical raw and auxiliary material.
Background technology
Calcium, magnesium exist mainly with compounds such as carbonate, sulfate, silicate, phosphate, fluorides at nature.During metallurgical material is analyzed, the mensuration of content of calcium and magnesium accounts for very consequence.Measurement result as content of calcium and magnesium in the lime stone in flux for metallurgy, rauhkalk provides calcium magnesium grade foundation accurately for the knot valency of raw material and auxiliary material; The fire resistive material that metallurgy high furnace is used, the desulfurizing agent in metallurgical process, the coverture in auxiliary material, covering slag etc., calcium, magnesium determination result are material proportions in metallurgical technology, material balance and control the important parameter of the technology controlling and process such as sintering, blast furnace basicity.Therefore, in field of steel metallurgy, in starting material, the analysis of calcium-magnesium content has a very important role.
In metallurgical material is analyzed, in raw and auxiliary material, the content of calcium, magnesium is higher, and its measurement result often calculates with calcium oxide and magnesium oxide and represents.At present, high-load calcium oxide in metallurgical supplementary material is measured and method of magnesium oxide mainly contains visual compleximetry and automatic potentiometric titration.
With reference to the visual compleximetry of GB/T 3286.1-2012 " the mensuration compleximetry of lime stone and rauhkalk chemical analysis method calcium oxide and content of magnesia and atomic spetrophtometry method ", it is the classical titration method of visual titration calcium oxide and content of magnesia, its principle is under different pH value, calcium in EDTA and calcium oxide and magnesium oxide, magnesium complexing, utilize formula:
Calculate the content of calcium oxide, in formula, c is the concentration (unit: mol/L) of EDTA, and V is the titration volumes (unit: mL) of EDTA, the molal weight of 56.08 calcium oxide, (unit: g/mol), V
1test solution constant volume (unit: mL), V
2pipette the volume (unit: mL) of titration test solution, m is the quality (unit: g) taking sample.But for the sample of the matrix such as slag and fire resistive material more complicated, in measurement operation, color change near terminal hop is difficult to the naked eye accurately judge, according to the impact of the reason such as experience difference, indicator addition, ambient light, co-existing element interference of operating personnel, easy generation error, cause the accuracy of analysis result and precision poor.
And automatic potentiometric titration adopts the mode of potential break to obtain terminal, highly sensitive, instrument automatic decision, Repeatability and Reproducibility is all better than visual titrimetry, and automaticity is high, has liberated labour.Automatic potentiometric titration is based on chemical reaction, and the absorbance of different colours change when luminosity electrode measures equivalent point, or absorbance is converted into electric potential signal, determines equivalent point by first order derivative differentiate.In the titration of metallurgical raw and auxiliary material calcium oxide content, during due to judgement to variable color terminal, in potentiometric titration there is certain deviation in the judgement terminal of luminosity electrode and the endpoint of visual titrimetry, cause the titration results of automatic potentiometric titration on the low side, thus the accuracy of impact analysis result.
Summary of the invention
Object of the present invention is exactly for the deficiencies in the prior art, and provide the assay method of calcium oxide content in a kind of metallurgical supplementary material, the method is simple to operate, and measurement result accuracy is high.
For achieving the above object, the assay method of calcium oxide content in metallurgical supplementary material of the present invention, comprises the following steps successively:
An assay method for calcium oxide content in metallurgical supplementary material, comprises the following steps successively:
1) according to the sample ID of calcium oxide in required mensuration raw and auxiliary material, select the standard model of kind of the same race with it several, described standard model all has respective calcium oxide content standard value;
2) get wherein a kind of standard model, quality is m, adds solvent or flux is fully decomposed to form solution to be measured, and being then settled to volume is V
1;
3) pipetting volume is V
2solution to be measured, add highly basic regulate solution PH>=12.5;
4) in solution to be measured, calcon-carboxylic acid is added, autopotentiometric titrator is adopted to carry out calcium oxide content mensuration, adopt concentration to be that the EDTA standard solution of c mol/L carries out titration during mensuration, when the equivalent point that instrument judges automatically, drip EDTA standard solution volume be VmL;
5) calculating calcium oxide content measured value in standard model of getting is:
6) get other several standard models respectively, adopt step 2) ~ 5) mode measure, draw respective calcium oxide content measured value;
7) according to calcium oxide content standard value in gained some groups of standard models and respective calcium oxide content measured value, the regression curve equation formula of calcium oxide content corrected value is automatically obtained with linear regression software for calculation:
W
corrected value=aW
measured valueregression coefficient a and b value in+b,
Thus determine calcium oxide content corrected value and automatic potentiometric titration drip EDTA standard solution volume to be regression equation between V be:
8) testing sample is got, according to abovementioned steps 2) ~ 4) operate, then by various for gained data input step 7) in formula, the normalization value of calcium oxide in calcic sample to be measured can be calculated.
Preferably, step 1) in get containing calcium oxide standard model be more than five kinds or five kinds.
Further, step 3) described in highly basic be NaOH or potassium hydroxide.
Again further, step 4) described in calcon-carboxylic acid be calcium carboxylates.
In metallurgical supplementary material of the present invention, the assay method of calcium oxide content is on autopotentiometric titrator, utilizes luminosity electrode, carries out automatic Titration and automatically draws analysis result.Simultaneously, method of the present invention utilizes and the standard model several (described standard model all has respective calcium oxide content standard value) that need measure the sample ID of calcium oxide kind of the same race in raw and auxiliary material, detect on the same stage, according to the regression coefficient of the measured value determination corrected value regression curve that its theoretical oxidation calcium content standard value and automatical potentiometric titrimeter detect, as correction coefficient, thus determine the variable relation between testing sample measured value and corrected value, draw the normalization value of calcium oxide in calcic sample to be measured, accuracy of analysis is improved.In addition, assay method of the present invention is simple to operate, fast, accurately, effectively can improve accuracy and the precision of analysis result.
Embodiment
Below in conjunction with specific embodiment, calcium oxide content assay method in metallurgical raw and auxiliary material of the present invention is described in further details.
Embodiment 1
The mensuration of calcium oxide content in certain lime stone sample to be measured.
1) find out the standard model 3 of lime stone standard model 2, rauhkalk, its standard No. and calcium oxide content standard value see the following form 1.
2) get wherein YSBC28724-934# lime stone standard model 0.5000mg, according to the sample decomposition step 3.5.4.1 in GB/T 3286.1-2012, sample is adopted 4g mixed flux (weight ratio sodium carbonate: boric acid=2; 1) fusion and decomposition, watery hydrochloric acid leaches, and constant volume, in 250mL volumetric flask, obtains test solution to be measured;
3) pipette test solution 25.00mL to be measured in 300mL titration cup, add 100mL water, 5mL triethanolamine solution, hydro-oxidation potassium solution (concentration is 200g/L), regulate the pH value 13 making vs;
4) with calcon-carboxylic acid (1g calcon-carboxylic acid and the grinding of 100g sodium chloride, mixing) 0.1g; DP5 luminosity electrode is inserted in solution, connect DL50 autopotentiometric titrator, the optimum determining parameter of setting this method instrument as measurement point density be 4, minimum may increment be 20 μ L, signal drift 50mv/min time, under relevant work program on automatical potentiometric titrimeter, when sample weighting amount m is 0.5000g, constant volume V
1for 250mL, pipette titration volumes V
2when concentration c for 25.00mL, EDTA standard titration solution is 0.01000mol/L, calculate the theoretical calculation formula of oxidation calcium oxide content
in constant coefficient be
computing formula is W
measured value=1.1216 × V%, input equation coefficients 1.1216, with automatical potentiometric titrimeter titration under the analysis bank of the above-mentioned coefficient of input, consuming EDTA volume is 25.83ml, show that sample tests value is W
measured value=28.97%.
6) get other four standard models respectively, adopt step 2) ~ 5) mode measure, draw respective calcium oxide content measured value.The measured value of 5 standard models is in table 1.
Table 1: lime stone, rauhkalk standard model content and potentiometric titrimeter titrate the analysis result (%)
7) according to table 1 Plays value and measured value, regression curve equation formula W is automatically obtained with linear regression software for calculation
corrected value=aW
measured valuethe regression coefficient a of+b and b value:
a＝1.00923，b＝－0.0005556，
Thus determine that the regression equation between corrected value and automatic potential titrator tests definite value V is:
That is: W
corrected value=1.00923 × 1.1216 × V%-0.0005556, is input to computing formula coefficient 1.00923 × 1.1216=1.1320 and-0.0005556 and step 4) in potentiometric titrimeter identical parameters another group analysis group in corresponding computing formula program under preserve.
8) by lime stone sample to be measured according to step 2) ~ 4) operation, carry out automatic titration, consuming EDTA titration volumes is 48.238mL, and its analysis result is:
W
corrected value=1.1320 × V%-0.0005556=54.55%.
The manual titration validation value content of calcium oxide in limestone of sample chemistry in GB/T3286.1-2012 is adopted to be 54.63% to the lime stone sample to be measured of the present embodiment.
Then the inventive method measurement result and national standard method measurement result relative error are (54.55%-54.63%)/54.63% × 100%=-0.15%.
Embodiment 2
Be numbered the mensuration of calcium oxide content in BH0120-3Wa lime stone standard model to certain, in this BH0120-3Wa lime stone standard model known, calcium oxide content is 53.93%, and assay method is:
Step 1) ~ 7) with embodiment 1;
8) by lime stone sample to be measured according to step 2) ~ 4) operation, carry out automatic titration, consuming EDTA titration volumes is 47.769mL, and its analysis result is:
W
corrected value=1.1320 × V%-0.0005556=54.02%.
Then the inventive method measurement result and standard value relative error are (54.02%-53.93%)/53.93% × 100%=0.17%.
Embodiment 3
The mensuration of calcium oxide content in certain slag to be measured.
1) find out 5, the slag inner quality standard sample that calcium oxide content becomes gradient to distribute, its standard No. and calcium oxide content standard value see the following form 2.
2) get wherein L-1# slag standard model 0.5000mg, according to the sample decomposition step 3.5.4.1 in GB/T 3286.1-2012, sample is adopted 4g mixed flux (weight ratio sodium carbonate: boric acid=2; 1) fusion and decomposition, watery hydrochloric acid leaches, and constant volume, in 250mL volumetric flask, obtains test solution to be measured;
3) pipette test solution 25.00mL to be measured in 300mL titration cup, add 100mL water, 5mL triethanolamine solution, hydro-oxidation potassium solution (concentration is 200g/L), regulate the pH value 13.5 making vs, obtain calcium oxide content liquid to be measured;
4) with calcon-carboxylic acid (1g calcon-carboxylic acid and the grinding of 100g sodium chloride, mixing) 0.1g; DP5 luminosity electrode is inserted in solution, connect DL50 autopotentiometric titrator, the optimum determining parameter of setting this method instrument as measurement point density be 4, minimum may increment be 20 μ L, signal drift 50mv/min time, under relevant work program on automatical potentiometric titrimeter, when sample weighting amount m is 0.5000g, constant volume V
1for 250mL, pipette titration volumes V
2when concentration c for 25.00mL, EDTA standard titration solution is 0.01000mol/L, calculate the theoretical calculation formula of oxidation calcium oxide content
in constant coefficient be
computing formula is w
caO=1.1216 × V%, input equation coefficients 1.1216.With automatical potentiometric titrimeter titration under the analysis bank of the above-mentioned coefficient of input, consuming EDTA volume is 18.281ml, show that sample tests value is W
measured value=20.50%.
6) get other four standard models respectively, adopt step 2) ~ 5) mode measure, draw respective calcium oxide content measured value.The measured value of 5 standard models is in table 2.
Table 2: g of slag sample standard content and potentiometric titrimeter titrate the analysis result (%)
7) according to table 1 Plays value and measured value, regression curve equation formula W is automatically obtained with linear regression software for calculation
corrected value=aW
measured valuethe regression coefficient a of+b and b value:
a＝1.00402，b＝0.0014779。
That is: W
corrected value=1.00402 × 1.1216 × V%+0.0014779, is input to computing formula coefficient 1.00402 × 1.1216=1.12611 and+0.0014779 and step 4) in potentiometric titrimeter identical parameters another group analysis group in corresponding computing formula program under preserve.
8) by g of slag sample to be measured according to step 2) ~ 4) operation, carry out automatic titration, consuming EDTA titration volumes is 23.942ml, and its analysis result is:
W
corrected value=1.12611 × 23.942%+0.0014779=27.11%.
Adopt calcium oxide content in the manual titration validation value slag of sample chemistry in GB/T3286.1-2012 to be 27.01% to the g of slag sample to be measured of the present embodiment.
Then the inventive method measurement result and national standard method measurement result relative error are (27.11%-27.01%)/27.01% × 100%=0.37%.
Embodiment 4
Calcium oxide content in another kind of slag is measured.
Determination step 1) ~ 7) with embodiment 3;
8) by g of slag sample to be measured according to step 2) ~ 4) operation, carry out automatic titration, consuming EDTA titration volumes is 36.089ml, and its analysis result is:
W
corrected value=1.12611 × 36.089%+0.0014779=40.79%.
Adopt calcium oxide content in the manual titration validation value slag of sample chemistry in GB/T3286.1-2012 to be 40.85% to the g of slag sample to be measured of the present embodiment.
Then the inventive method measurement result and national standard method measurement result relative error are (40.79%-40.85%)/40.85% × 100%=-0.15%.
Claims (4)
1. the assay method of calcium oxide content in metallurgical supplementary material, is characterized in that: the method comprises the following steps successively:
1) according to the sample ID of calcium oxide in required mensuration raw and auxiliary material, select the standard model of kind of the same race with it several, described standard model all has respective calcium oxide content standard value;
2) get wherein a kind of standard model, quality is m, adds solvent or flux is fully decomposed to form solution to be measured, and being then settled to volume is V
1;
3) pipetting volume is V
2solution to be measured, add highly basic regulate solution PH>=12.5;
4) in solution to be measured, calcon-carboxylic acid is added, autopotentiometric titrator is adopted to carry out calcium oxide content mensuration, adopt concentration to be that the EDTA standard solution of c mol/L carries out titration during mensuration, when the equivalent point that instrument judges automatically, drip EDTA standard solution volume be V mL;
5) calculating calcium oxide content measured value in standard model of getting is:
6) get other several standard models respectively, adopt step 2) ~ 5) mode measure, draw respective calcium oxide content measured value;
7) according to calcium oxide content standard value in gained some groups of standard models and respective calcium oxide content measured value, the regression curve equation formula of calcium oxide content corrected value is automatically obtained with linear regression software for calculation:
W
corrected value=aW
measured valueregression coefficient a and b value in+b,
Thus determine calcium oxide content corrected value and automatic potentiometric titration drip EDTA standard solution volume to be regression equation between V be:
8) testing sample is got, according to abovementioned steps 2) ~ 4) operate, then by various for gained data input step 7) in formula, the normalization value of calcium oxide in calcic sample to be measured can be calculated.
2. the assay method of calcium oxide content in metallurgical supplementary material according to claim 1, is characterized in that: step 1) in what get is more than five kinds or five kinds containing calcium oxide standard model.
3. the assay method of calcium oxide content in metallurgical supplementary material according to claim 1 and 2, is characterized in that: step 3) described in highly basic be NaOH or potassium hydroxide.
4. the assay method of calcium oxide content in metallurgical supplementary material according to claim 1 and 2, is characterized in that: step 4) described in calcon-carboxylic acid be calcium carboxylates.
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Cited By (4)
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| CN104977385A (en) * | 2015-06-12 | 2015-10-14 | 内蒙古包钢钢联股份有限公司 | Method for continuous determination of calcium oxide and magnesium oxide content of limestone and dolomite |
| CN106546443A (en) * | 2016-11-08 | 2017-03-29 | 攀钢集团攀枝花钢钒有限公司 | The assay method of calcium-magnesium content in Inactivate granular magnesium |
| CN111239331A (en) * | 2020-03-20 | 2020-06-05 | 莱芜泰禾生化有限公司 | Method for detecting content of calcium oxide in quick lime |
| CN113640454A (en) * | 2021-07-30 | 2021-11-12 | 华能国际电力股份有限公司上海石洞口第一电厂 | Method for rapidly testing content of calcium oxide in limestone |
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