CN105424685A - Method for detecting content of manganese in manganous-rich slag - Google Patents
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Abstract
The invention discloses a method for detecting the content of manganese in manganous-rich slag. The method comprises the steps of sample pretreatment, sample dissolving, oxidizing, titration, standard titration solution preparation and content calculating. According to the method, no national standard or industrial standard exists at present; on the aspect of the accuracy of a detecting result, through the analysis steps and parameter setting adopted in the method, a sample can be completely dissolved, no residue exists, heterogeneous medium interference is avoided, experimental errors are reduced, and the detecting result is good in stability, reproducibility and accuracy. On the aspect of detecting speed, the method has the advantages of being high in analyzing speed, short in detecting period and high in analyzing efficiency. Detecting time is saved, the labor intensity of testing and analyzing personnel is relieved, energy consumption is reduced, and cost reducing and benefit increasing of an enterprise are facilitated. On the aspect of the detecting procedure, the method is easy to operate and easy to learn and understand, the requirement for the testing and analyzing personnel is not high, and good application and popularization prospects are achieved.
Description
Technical field
The invention belongs to detection technique field, be specifically related to the detection method of Fe content in a kind of Mn-rich slag.
Background technology
In smelting iron and steel is produced, secondary product when Mn-rich slag is a kind of is employing acid slag pracitice, slant acidity slag method produces high carbon ferromanganese, because wherein manganese, silicone content are higher, are the utilization factor improving resource, the manganese in Mn-rich slag can be extract or be used with manganese compound.
Because the content of manganese in Mn-rich slag and silicon is higher, and when smelting manganese silicon alloy due to recovery problem, require that the content of manganese in its raw material is greater than 40%, the content of silicon also requires higher, therefore Mn-rich slag can be used as the raw material of smelting manganese silicon alloy completely, it can also be used as the raw material producing manganese metal simultaneously, also can be used as the batching of producing blast furnace ferromanganese, electric furnace ferromanganese and low-carbon ferromanganese.For optimizing the Design of Chemical Composition smelted and produce, it is enterprise's cost efficiency.Therefore extremely important production practical significance is had to the mensuration of Fe content in Mn-rich slag.
Mn-rich slag principal ingredient is C, Si, Mn, S, P equal size.Therefore, be necessary to research and develop a kind of accuracy high, good stability, analytical cycle is short, and testing cost is low, is particularly useful for the detection method of the Mn-rich slag sample of Fe content >=10%, smelts production to upgrading, the active demand of falling basis, synergy to adapt to modernization.
Summary of the invention
The object of the present invention is to provide the detection method of Fe content in a kind of Mn-rich slag.
The object of the present invention is achieved like this, comprises the following steps:
A, sample is crushed to granularity≤0.125mm, at 105 ~ 110 DEG C of drying 1.5 ~ 2.5h to constant weight, take 0.2000g sample, add 28 ~ 32ml hydrochloric acid and the mixing of 0.2 ~ 0.5ml hydrofluorite, being heated to sample in 80 ~ 100 DEG C dissolves completely, naturally 2 ~ 3min is cooled, add 10 ~ 14ml phosphoric acid and 18 ~ 22ml perchloric acid, continue at 80 ~ 100 DEG C to be heated to the minute bubbles that liquid level presents and to disappear completely, take off and be cooled to 70 ~ 80 DEG C, add the abundant dissolved salts of 40 ~ 60ml water shake 1 ~ 2min, flowing water is cooled to 20 ~ 25 DEG C and obtains test solution a;
B, test solution a iron ammonium sulfate standard titration solution is titrated to solution pinkiness, drip 5 N-benzene for clever aminobenzoic acid solution, it be bright green is terminal that continuation iron ammonium sulfate standard titration solution is titrated to solution, write down the milliliter number of consumed iron ammonium sulfate standard titration solution, be calculated as follows and obtain Fe content in sample:
In formula:
C---iron ammonium sulfate standard titration solution concentration, unit is (mol/L);
M---the sample mass in step B, unit is g;
V
0---titration blank test solution consumption iron ammonium sulfate standard titration solution volume, unit is ml;
V---titration sample solution consumes iron ammonium sulfate standard titration solution volume, and unit is ml;
54.938---the molal weight of manganese, unit is gram every mole (g/mol).
Measure the content of manganese in Mn-rich slag thus.Described method has good accuracy, reappearance and stability, and the Mn-rich slag Fe content being specially adapted to Fe content >=10% detects.
The analytical procedure that the method for the invention adopts and setting parameter, be conducive to sample and dissolve completely, noresidue, without heterogeneous interference, decreases experimental error, and testing result has good stability, reappearance and accuracy.In detection speed, it is fast that the method for the invention has analysis speed, and sense cycle is short, the feature that analysis efficiency is high, has not only saved detection time, alleviates the labour intensity of test analysis personnel, also reduces energy consumption, is conducive to enterprise's cost efficiency.In testing process, the method for the invention is simple to operate, easily learns well and understands, to test analysis personnel without excessive demand, has good popularizing application prospect.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but limited the present invention never in any form, and any conversion done based on training centre of the present invention or replacement, all belong to protection scope of the present invention.
The detection method of Fe content in Mn-rich slag of the present invention, comprises the following steps:
A, sample is crushed to granularity≤0.125mm, at 105 ~ 110 DEG C of drying 1.5 ~ 2.5h to constant weight, take 0.2000g sample, add 28 ~ 32ml hydrochloric acid and the mixing of 0.2 ~ 0.5ml hydrofluorite, being heated to sample in 80 ~ 100 DEG C dissolves completely, naturally 2 ~ 3min is cooled, add 10 ~ 14ml phosphoric acid and 18 ~ 22ml perchloric acid, continue at 80 ~ 100 DEG C to be heated to the minute bubbles that liquid level presents and to disappear completely, take off and be cooled to 70 ~ 80 DEG C, add the abundant dissolved salts of 40 ~ 60ml water shake 1 ~ 2min, flowing water is cooled to 20 ~ 25 DEG C and obtains test solution a;
B, test solution a iron ammonium sulfate standard titration solution is titrated to solution pinkiness, drip 5 N-benzene for clever aminobenzoic acid solution, it be bright green is terminal that continuation iron ammonium sulfate standard titration solution is titrated to solution, write down the milliliter number of consumed iron ammonium sulfate standard titration solution, be calculated as follows and obtain Fe content in sample:
In formula:
C---iron ammonium sulfate standard titration solution concentration, unit is (mol/L);
M---the sample mass in step B, unit is g;
V
0---titration blank test solution consumption iron ammonium sulfate standard titration solution volume, unit is ml;
V---titration sample solution consumes iron ammonium sulfate standard titration solution volume, and unit is ml;
54.938---the molal weight of manganese, unit is gram every mole (g/mol).
The mass percentage concentration of the hydrochloric acid described in step A is 36 ~ 38%.
The mass percentage concentration of the hydrofluorite described in step A is 49 ~ 51%.
The mass percentage concentration of the phosphoric acid described in step A is 83 ~ 98%.
The mass percentage concentration of the perchloric acid described in step A is 70 ~ 72%.
N-benzene described in step B is 2g/L for the solution concentration of clever aminobenzoic acid solution.
The detection method of Fe content in Mn-rich slag of the present invention, specifically comprises sample pretreatment, sample dissolving, oxidation, titration, standard titration solution preparation and cubage operation, specifically comprises:
A, sample pretreatment: sample is crushed to granularity≤0.125mm, in 105-110 DEG C of dry 1.5-2.5h, be placed in exsiccator and be cooled to room temperature.
B, sample dissolve: take 0.2000g sample, be placed in 300ml conical flask, add 30.0ml hydrochloric acid and 5 hydrofluorite mixings, are heated to sample and dissolve completely, take off in 80-100 DEG C, slightly cold, obtain test solution.
C, oxidation processes: step B gained test solution is added 12.0ml phosphoric acid and 2.0ml perchloric acid, continue to be heated to the minute bubbles that liquid level presents to disappear completely, take off, be cooled to 70-80 DEG C, slowly add 50ml water along bottle wall, shake conical flask, fully dissolve the low salt of conical flask bottle, flowing water is cooled to room temperature, obtains test solution.
D, titration: step C gained test solution iron ammonium sulfate standard titration solution is titrated to solution pinkiness, drip 5 N-stupid generations adjacent amino stupid formic acid solution, it be bright green is terminal that continuation iron ammonium sulfate standard titration solution is titrated to solution, writes down the milliliter number of consumed iron ammonium sulfate standard titration solution.
E, standard titration solution are prepared: take 13.72g iron ammonium sulfate and be placed in the 400ml beaker filling 200ml sulfuric acid (1+1), dissolve completely until iron ammonium sulfate, move in 1000ml volumetric flask, be diluted with water to scale, shake up, obtain standard solution a;
Take 1.7150g in advance at 140-150 DEG C of dry 2h and the potassium dichromate (standard reagent) being cooled to room temperature in exsiccator in 250ml beaker, be dissolved in water, move in 1000 volumetric flasks, be diluted with water to scale and shake up.Obtain standard solution b, this concentration of standard solution is 0.0350mol/L;
Demarcate:
Pipette standard solution b25.00ml in 300ml conical flask, add 25.0ml water, add 5.0ml sulfuric acid (1+1), add 2.0ml phosphoric acid, it is light yellow for being titrated to solution with iron ammonium sulfate standard titration solution, drips 5 N-stupid generations adjacent amino stupid formic acid solutions, and it be bright green is terminal that continuation iron ammonium sulfate standard titration solution is titrated to solution, demarcate three parts simultaneously, consume iron ammonium sulfate standard titration solution milliliter number be not more than 0.1ml.
The concentration of iron ammonium sulfate standard titration solution is calculated as follows:
In formula:
C
1the concentration of-iron ammonium sulfate standard titration solution, unit is (mol/L);
C
2the concentration of-potassium dichromate standard solution, unit is (mol/L);
V
1-titration potassium dichromate standard solution consumes the volume of iron ammonium sulfate standard titration solution, and unit is ml;
V
2-pipetting the volume of potassium dichromate standard solution, unit is ml;
F, cubage: in sample, Fe content is calculated as follows:
In formula:
C---iron ammonium sulfate standard titration solution concentration, unit is (mol/L);
M---the sample mass in step B, unit is g;
V
0---titration blank test solution consumption iron ammonium sulfate standard titration solution volume, unit is ml;
V---titration sample solution consumes iron ammonium sulfate standard titration solution volume, and unit is ml;
54.938---the molal weight of manganese, unit is gram every mole (g/mol).
In described steps A, sample is crushed to granularity≤0.125mm.
In described step B, take 0.2000g sample, with hydrochloric acid and hydrofluorite in low temp. electric hot plate dissolution in low temperature sample.
In described step B and step C, hydrochloric acid, hydrofluorite, phosphoric acid and perchloric acid are concentrated acid, adopt the conical flask of 300ml.
In described step D and step e, sulfuric acid (1+1), phosphoric acid (ρ 1.70g/mL), N-stupid generation adjacent amino stupid formic acid solution 2g/L, in iron ammonium sulfate vitriolization (1+1), described iron ammonium sulfate standard titration solution preparation is prepared by sulfuric acid (1+1), and be diluted with water to volume, potassium dichromate standard solution is by the water-soluble solution of potassium dichromate, and being diluted to volume by water-soluble solution, in N-stupid generation, adjacent amino stupid formic acid solution was dissolved in the hot sodium carbonate liquor 2g/L of 100ml by 0.2gN-stupid generation adjacent amino stupid formic acid.
In described step e, it is analytical reagent that standard titration solution a prepares iron ammonium sulfate used, and it is standard reagent that standard solution b prepares potassium dichromate used.
In described step B, the slightly cold triangular flask that refers to takes off from electric furnace and places 2-3min, in step C, is cooled to room temperature and refers to and be cooled to 20-25 DEG C.
In described step C, in phosphoric acid medium, with perchloric acid, bivalent manganese is oxidized to manganic.
In described step D, buret is the 50ml base buret that school was examined under normal temperature.
Described detection method is specially adapted to the mensuration of the sample of manganese >=10% in Mn-rich slag.
Here is that the present invention will be further described for concrete case study on implementation:
Embodiment 1
---the detection of Fe content in Mn-rich slag
(1) preparation of experiment reagent and demarcation
Take 13.72g iron ammonium sulfate, add 200ml by volume ratio 1:1 98% sulfuric acid and the sulfuric acid solution that mixes of distilled water, after iron ammonium sulfate dissolves completely, move in 1000ml volumetric flask, be settled to scale with distilled water, mixing, obtains iron ammonium sulfate standard solution.
Take 1.7150g and in exsiccator, be cooled to the potassium dichromate of room temperature at 140 ~ 150 DEG C of dry 2h in advance, adding distil water dissolves, and moves in 1000ml volumetric flask, is settled to scale with distilled water, mixing, obtains the potassium dichromate standard solution that concentration is 0.0350mol/L.
Take 0.2gN-benzene for ortho-aminobenzoic acid, be dissolved in the sodium carbonate liquor of 80-90 DEG C of 100ml2g/L, obtaining concentration is that the N-benzene of 2g/L is for o-amino benzoyl acid solution.
Pipette the potassium dichromate standard solution 25.00ml of 0.0350mol/L, add 25.00ml distilled water successively, 5.00ml by volume ratio 1:1 98% sulfuric acid and the sulfuric acid solution that mixes of distilled water, 2.00ml1.70g/ml phosphoric acid, it is light yellow for being titrated to solution with iron ammonium sulfate standard solution after mixing, the N-benzene adding 5 2g/L, for o-amino benzoyl acid solution, continues with above-mentioned iron ammonium sulfate standard solution that to be titrated to solution be bright green is terminal.Demarcate three parts, the volume≤0.1ml of the iron ammonium sulfate standard solution consumed simultaneously.The calculating of described iron ammonium sulfate concentration of standard solution is undertaken by following formula:
In formula:
C
1---the concentration of iron ammonium sulfate standard solution, mol/L;
C
2---the concentration of potassium dichromate standard solution, 0.0350mol/L;
V
1---the volume of the iron ammonium sulfate standard solution that titration potassium dichromate standard solution consumes, 25.06ml;
V
2---pipette the volume of potassium dichromate standard solution, 25.00ml;
(2) detection of Fe content
Sample is crushed to granularity≤0.125mm, at 105 ~ 110 DEG C of drying 1.5 ~ 2.5h to constant weight, take 0.2000g sample, add 28 ~ 32ml hydrochloric acid and the mixing of 0.2 ~ 0.5ml hydrofluorite, being heated to sample in 80 ~ 100 DEG C dissolves completely, naturally 2 ~ 3min is cooled, add 10 ~ 14ml phosphoric acid and 18 ~ 22ml perchloric acid, continue at 80 ~ 100 DEG C to be heated to the minute bubbles that liquid level presents and to disappear completely, take off and be cooled to 70 ~ 80 DEG C, add the abundant dissolved salts of 40 ~ 60ml water shake 1 ~ 2min, flowing water is cooled to 20 ~ 25 DEG C and obtains test solution a; Test solution a iron ammonium sulfate standard titration solution is titrated to solution pinkiness, drip 5 N-benzene for clever aminobenzoic acid solution, it be bright green is terminal that continuation iron ammonium sulfate standard titration solution is titrated to solution, writes down the milliliter number of consumed iron ammonium sulfate standard titration solution.
Be calculated as follows and obtain Fe content in sample::
In formula:
C---the concentration of iron ammonium sulfate standard solution, 0.03492mol/L;
The quality of M---sample, 0.2000g;
V
0---the volume of the iron ammonium sulfate standard solution that the blank test solution of titration consumes, 0.00ml;
The volume of the iron ammonium sulfate standard solution that V---titration test solution b consumes, 18.30ml;
54.938---the molal weight of manganese, g/mol.
Embodiment 2
---the detection of Fe content in Mn-rich slag
The preparation of experiment reagent and demarcation are with embodiment 1.
The detection of Fe content is with embodiment 1.
In described Mn-rich slag sample, the calculating of Fe content is undertaken by following formula:
In formula:
C---the concentration of iron ammonium sulfate standard solution, 0.03492mol/L;
The quality of M---sample, 0.2000g;
V
0---the volume of the iron ammonium sulfate standard solution that the blank test solution of titration consumes, 0.00ml;
The volume of the iron ammonium sulfate standard solution that V---titration test solution b consumes, 26.45ml;
54.938---the molal weight of manganese, g/mol.
Embodiment 3
---the detection of Fe content in Mn-rich slag
The preparation of experiment reagent and demarcation are with embodiment 1.
The detection of Fe content is with embodiment 1.
In described Mn-rich slag sample, the calculating of Fe content is undertaken by following formula:
In formula:
C---the concentration of iron ammonium sulfate standard solution, 0.03492mol/L;
The quality of M---sample, 0.2000g;
V
0---the volume of the iron ammonium sulfate standard solution that the blank test solution of titration consumes, 0.00ml;
The volume of the iron ammonium sulfate standard solution that V---titration test solution b consumes, 34.30ml;
54.938---the molal weight of manganese, g/mol.
Embodiment 4
---the detection of Fe content in Mn-rich slag
The preparation of experiment reagent and demarcation are with embodiment 1.
The detection of Fe content is with embodiment 1.
In described Mn-rich slag sample, the calculating of Fe content is undertaken by following formula:
In formula:
C---the concentration of iron ammonium sulfate standard solution, 0.03492mol/L;
The quality of M---sample, 0.2000g;
V
0---the volume of the iron ammonium sulfate standard solution that the blank test solution of titration consumes, 0.00ml;
The volume of the iron ammonium sulfate standard solution that V---titration test solution b consumes, 40.20ml;
54.938---the molal weight of manganese, g/mol.
Embodiment 5
---the precision of detection method of the present invention, accuracy, recovery experiment
(1) Precision Experiment
Experimental technique: select 5 Mn-rich slag samples, carry out manganese content test respectively by detection method of the present invention, calculate relative standard deviation, experimental result is in table 1.
The Precision Experiment result of table 1 detection method of the present invention
Sample | Measured value (%) | Mean value (%) | Relative standard deviation RSD |
Sample 1 | 17.55,17.60,17.51,17.46,17.65 | 17.55 | 0.42 |
Sample 2 | 25.23,25.18,25.32,25.37,25.47 | 25.31 | 0.45 |
Sample 3 | 32.71,32.80,32.95,33.04,32.85 | 32.87 | 0.39 |
Sample 4 | 38.37,38.46,38.65,38.61,38.51 | 38.52 | 0.29 |
Sample 5 | 42.59,42.73,42.73,42.83,42.64 | 42.70 | 0.22 |
(2) accuracy experiment
Experimental technique: experimental technique: select 4 standard models, carry out manganese content test by detection method of the present invention respectively, each sample parallel measures 5 times, and experimental result is in table 2.
The accuracy experimental result of table 2 detection method of the present invention
(3) recovery experiment
Experimental technique: select 1 Mn-rich slag sample, add the manganese of different amount respectively, measure by detection method of the present invention, each sample parallel analyzes 4 times, averages, and trying to achieve the recovery is 98.7 ~ 101.4%, and experimental result is in table 3.
The recovery experimental result of table 3 detection method of the present invention
From above-mentioned experimental result, the analysis result deviation of detection method of the present invention is little, precision, and the recovery all can meet analyzes requirement, and analysis speed is fast, simple to operate, easily grasps, has higher application value.
Claims (6)
1. the detection method of Fe content in Mn-rich slag, is characterized in that comprising the following steps:
A, sample is crushed to granularity≤0.125mm, at 105 ~ 110 DEG C of drying 1.5 ~ 2.5h to constant weight, take 0.2000g sample, add 28 ~ 32ml hydrochloric acid and the mixing of 0.2 ~ 0.5ml hydrofluorite, being heated to sample in 80 ~ 100 DEG C dissolves completely, naturally 2 ~ 3min is cooled, add 10 ~ 14ml phosphoric acid and 18 ~ 22ml perchloric acid, continue at 80 ~ 100 DEG C to be heated to the minute bubbles that liquid level presents and to disappear completely, take off and be cooled to 70 ~ 80 DEG C, add the abundant dissolved salts of 40 ~ 60ml water shake 1 ~ 2min, flowing water is cooled to 20 ~ 25 DEG C and obtains test solution a;
B, test solution a iron ammonium sulfate standard titration solution is titrated to solution pinkiness, drip 5 N-benzene for clever aminobenzoic acid solution, it be bright green is terminal that continuation iron ammonium sulfate standard titration solution is titrated to solution, write down the milliliter number of consumed iron ammonium sulfate standard titration solution, be calculated as follows and obtain Fe content in sample:
Mn(%)=
In formula:
C---iron ammonium sulfate standard titration solution concentration, unit is (mol/L);
M---the sample mass in step B, unit is g;
V
0---titration blank test solution consumption iron ammonium sulfate standard titration solution volume, unit is ml;
V---titration sample solution consumes iron ammonium sulfate standard titration solution volume, and unit is ml;
54.938---the molal weight of manganese, unit is gram every mole (g/mol).
2. the detection method of Fe content in rich manganese manganese slag according to claim 1, is characterized in that the mass percentage concentration of the hydrochloric acid described in step A is 36 ~ 38%.
3. the detection method of Fe content in Mn-rich slag according to claim 1, is characterized in that the mass percentage concentration of the hydrofluorite described in step A is 49 ~ 51%.
4. the detection method of Fe content in Mn-rich slag according to claim 1, is characterized in that the mass percentage concentration of the phosphoric acid described in step A is 83 ~ 98%.
5. the detection method of Fe content in Mn-rich slag according to claim 1, is characterized in that the mass percentage concentration of the perchloric acid described in step A is 70 ~ 72%.
6. the detection method of Fe content in Mn-rich slag according to claim 1, is characterized in that the N-benzene described in step B is 2g/L for the solution concentration of clever aminobenzoic acid solution.
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