CN113533307A - Method for measuring contents of calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead and zinc elements in blast furnace dust - Google Patents
Method for measuring contents of calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead and zinc elements in blast furnace dust Download PDFInfo
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Abstract
The invention discloses a method for measuring contents of calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead and zinc elements in blast furnace dust, which removes carbon and sulfur in a sample by high-temperature ignition, utilizes microwave to digest the sample, adopts an inductively coupled plasma atomic emission spectrometry to accurately and quickly measure the ten elements of calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead, zinc and the like, correspondingly reduces the use of medicines and manpower, reduces the operating cost of instruments, improves the detection efficiency, reduces the analysis cost and provides quick and powerful data support for scientific research and production.
Description
Technical Field
The invention relates to the technical field of metallurgical analysis, in particular to a method for measuring contents of calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead and zinc elements in blast furnace dust.
Background
According to the standard literature data, no standard analysis method is available for measuring the content of the ten elements such as calcium, magnesium, copper, aluminum, titanium, manganese, potassium, sodium, lead, zinc and the like in the blast furnace dust. The routine detection of potassium, sodium, copper, lead and zinc in the blast furnace dust is a flame atomic absorption spectrophotometry which is a method for detecting elements in cited slag; the method for detecting calcium, magnesium, aluminum, manganese and titanium in blast furnace dust is a method for detecting elements in reference slag, and the XRF-1800 fluorescence spectrometer is used for measuring the content of each element. Therefore, two instruments and two detection methods are needed to detect the content of the ten elements.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a method for measuring the contents of calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead and zinc in blast furnace dust, which removes carbon and sulfur in a sample by high-temperature ignition, utilizes microwave to digest the sample, adopts an inductively coupled plasma atomic emission spectrometry to accurately and quickly measure the ten elements of calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead, zinc and the like, correspondingly reduces the use of medicines and manpower, reduces the operating cost of instruments, improves the detection efficiency, reduces the analysis cost and provides quick and powerful data support for scientific research and production.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention relates to a method for measuring contents of calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead and zinc elements in blast furnace dust, which comprises the following steps:
weighing a blast furnace dust sample in a porcelain boat, placing the porcelain boat in a 600-plus 800 ℃ muffle furnace, slightly opening a furnace door during firing to keep air entering, firing for 1-6 minutes to remove carbon and sulfur, taking out the porcelain boat, transferring the sample into a microwave digestion tank after slightly cooling, firstly adding a small amount of water into a water washing bottle for wetting, then adding aqua regia, covering a sealing cover according to the operating specification of the microwave digestion instrument, placing the porcelain boat into the microwave digestion instrument, connecting a temperature sensor, setting a reaction method according to the number of pressure containers according to microwave digestion conditions, carrying out microwave digestion, taking out the digestion tank after digestion is finished, transferring a digestion solution into a plastic volumetric flask, and determining by using a plasma atomic emission spectrometer after the volume is fixed by pure water;
carrying out a blank test along with the sample, and replacing the sample with high-purity iron to carry out the test so as to ensure that the iron content is consistent with that in the sample to be tested;
drawing a working curve by mixing the standard solutions, respectively adding the standard solutions of the elements to be detected with gradient contents into a 100ml series plastic volumetric flask containing an iron matrix with the same amount as the sample according to the approximate contents of the elements to be detected in the sample to prepare the working curve of the standard solutions with corresponding content ranges, wherein the environment of the mixed standard solutions is matched with that of the sample solutions;
drawing a working curve of the standard sample, selecting 3-4 iron ore standard substances (the iron-based content of which is close to that of the sample) to manufacture the working curve of the standard sample according to the content of each element to be detected in the sample, wherein the dissolving method of the standard sample is the same as that of the sample;
introducing a calibration curve solution from low to high, a blank solution and an iron ore standard substance or a standard addition recovery sample solution and a sample solution into an inductively coupled plasma emission spectrometer to measure the signal intensity of an element to be measured, drawing a calibration solution working curve by taking the signal intensity of the element to be measured as a vertical coordinate and the mass percent of ions as a horizontal coordinate, and calculating the mass percent of the element to be measured by using the calibration curve with known mass percent;
the result calculation formula is as follows:
W(component to be measured)=Wi-W0
In the formula: w(component to be measured)The content and the mass fraction of the element to be detected in the analyte are shown;
Withe content of elements to be measured in the sample solution is the mass percentage;
W0the content and the mass fraction of the element to be detected in the blank solution are shown.
Furthermore, the microwave digestion instrument adopts an MARS microwave digestion instrument, and the model of the pressure vessel is XP 1500.
Further, the detection range is as follows: ca%: 0.100% -10.00%; mg%: 0.050% -5.00%; cu%: 0.001% -3.00%; al%: 0.020% -5.00%; mn%: 0.020% -3.00%; ti%: 0.010 percent to 1.50 percent; k: 0.010-20.00%; na: 0.010-20.00%; pb: 0.100-10.00%; zn: 0.005-10.00 percent.
Compared with the prior art, the invention has the beneficial technical effects that:
1) preparing a calibration solution working curve matched with a sample solution by using a mixed standard solution by using high-purity iron as a bottoming matrix; or 3-4 iron ore standard samples (the iron base content of which is close to that of the sample) are selected to manufacture the standard sample working curve, and the two working curve preparation methods can eliminate the interference of matrix elements. In actual detection, one of the working curves can be selected according to the content of the sample, the linear range of the curve is wide, the range of the curve basically covers the content range of each element in the fly ash, and when the content of the sample is high, the test solution does not need to be diluted, and the content of ten elements can be measured simultaneously, so that the measurement time is short, and the measurement result is accurate and reliable.
2) Placing the sample in a muffle furnace at 600-800 ℃ for burning to remove carbon and sulfur, and adding aqua regia for microwave digestion to achieve the purpose of complete decomposition; the reagent is taken from the same reagent bottle, and the same amount of the reagent is added, so that the pollution of elements such as sodium, zinc and the like is effectively controlled. The measuring range of each element is given, and the content range of each element in the daily coming sample dedusting ash is basically covered.
3) The method adopts an ICP-AES method to simultaneously, accurately and rapidly measure the ten elements such as calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead, zinc and the like in the blast furnace dust. The recovery rate of the added standard is 95.4-104.2%, the precision RSD is 4.84% at most, and powerful and reliable data support can be provided for scientific research and production.
Detailed Description
A method for measuring the contents of calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead and zinc elements in blast furnace dust includes the following steps:
1 brief summary of the method
Burning in a muffle furnace to remove carbon and sulfur in the sample, adding aqua regia for microwave digestion, and measuring by using an inductively coupled plasma emission spectrometer.
2 main instruments and working parameters
2.1 OPTIMA5300DV inductively coupled plasma spectrometer (manufactured by PE corporation, USA). The working parameters of the instrument are as follows: see table 1.
TABLE 1 operating parameters
2.2MARS microwave digestion apparatus (manufactured by CEM corporation, USA), pressure vessel model: XP 1500.
3 reagent and Standard solution
Unless otherwise stated, only reagent of superior purity and pure water of secondary and above in accordance with the provisions of GB/T6682 were used in the analysis.
3.1 high purity iron with purity > 99.99.
3.2 hydrochloric acid,. rho.1.19 g/mL.
3.3 nitric acid,. rho.1.42 g/mL.
3.4 aqua regia, hydrochloric acid and nitric acid which are 3+1 are prepared in situ.
3.5 calcium Standard solution, 1000. mu.g/mL (medium 5% HCl), national Standard solution.
3.6 magnesium Standard solution, 1000. mu.g/mL (medium 5% HCl), national Standard solution.
3.7 copper Standard solution, 1000. mu.g/mL (Medium 1% HNO)3) National standard solution.
3.8 aluminum Standard solution, 1000. mu.g/mL (Medium 10% HCl), national Standard solution.
3.9 manganese Standard solution, 1000. mu.g/mL (Medium 10% HNO)3) National standard solution.
3.10 titanium standard solution, 1000. mu.g/mL (medium 10% HNO3+ 2% HF), national standard solution.
3.11 Potassium Standard solution, 1000. mu.g/mL (Medium H)2O), national standard solution.
3.12 sodium Standard solution, 1000. mu.g/mL (Medium H)2O), national standard solution.
3.13 lead Standard solution, 1000. mu.g/mL (Medium 10% HNO)3) National standard solution.
3.14 Zinc standard solution, 1000. mu.g/mL (medium 10% HCl), national standard solution.
4 analytical step
4.1 preparation of sample solutions
Weighing 0.1000g of blast furnace dust sample in a porcelain boat, putting the porcelain boat in a muffle furnace at 600-800 ℃, slightly opening a furnace door during firing to keep air entering, firing for 1-6 minutes to remove carbon and sulfur, taking out the porcelain boat, slightly cooling, transferring the sample into a microwave digestion tank, firstly adding a small amount of water into a water washing bottle for wetting, then adding 10.00mL of aqua regia (3.4), covering a sealing cover according to the operation specification of the microwave digestion instrument, putting the container into the microwave digestion instrument, connecting a temperature sensor (a temperature probe must be completely inserted below the liquid level), according to the number of pressure containers (a CEM instrument can automatically adjust power, but the matching relation between a power platform and the number of the containers is still required in the process of setting the method), setting a reaction method according to the microwave digestion conditions in the table 2, carrying out microwave digestion, taking out a digestion tank after digestion is finished, transferring the digestion solution into a 100mL plastic volumetric flask, and carrying out determination by using a plasma atomic emission spectrometer after the volume is fixed by pure water.
TABLE 2 optimal working conditions for microwave digestion of samples
4.2 blank test and validation test
And carrying out a blank test along with the sample, and replacing the sample with high-purity iron (3.1) to carry out the test so as to ensure that the iron content is consistent with that in the sample to be tested. Because no blast furnace dust standard substance exists, the iron ore standard substance can be selected to equally replace the blast furnace dust along with the sample, or a standard recovery test is adopted to verify the correctness of the method. The reagents used should be taken from the same reagent bottle and added in equal amounts (blank and low carbon and sulfur samples do not have to be burned).
4.3 determination
4.3.1 calibration Curve
4.3.1.1 drawing working curve of mixed standard solution
In a 100ml series plastic volumetric flask containing iron matrix with the same amount as the sample, adding a standard solution of elements to be detected with gradient content according to the approximate content of the elements to be detected in the sample to prepare a working curve of the standard solution with corresponding content range, wherein the environment of the mixed standard solution is matched with the sample solution.
4.3.1.2 drawing working curve of standard sample
According to the content of each element to be measured in the sample, 3-4 iron ore standard substances (the iron-based content of which is close to that of the sample) are selected to manufacture a standard sample working curve, and the dissolving method of the standard sample is the same as that of the sample (the sample with low carbon and sulfur does not need to be burnt).
4.3.2 measurement
Referring to the working parameter modulation instrument conditions in Table 1, Ca 317.933, Mg 285.213, Cu 324.754, Al 396.153, Mn 257.610, Ti 334.941, K766.490 nm, Na 589.592nm, Pb 220.353nm, Zn 202.548nm are selected as analysis lines of each element, a calibration curve solution (4.3.1.1 or 4.3.1.2) is introduced into an inductively coupled plasma emission spectrometer from low to high, a blank solution and an iron ore standard substance or a standard recovery sample solution (4.2) are introduced to determine the signal intensity of the element to be determined, the signal intensity of the element to be determined is taken as a vertical coordinate, the ion mass percent is taken as a horizontal coordinate, a calibration solution working curve is drawn, and the mass percent of the element to be determined is determined by the calibration curve of known mass percent.
4.4 calculation of results
4.4.1 results show
W(component to be measured)=Wi-W0
In the formula: w(component to be measured)The content and the mass fraction of the element to be detected in the analyte are shown;
Withe content of elements to be measured in the sample solution is the mass percentage;
W0the content and the mass fraction of the element to be detected in the blank solution are shown.
4.4.2 conversion factor of oxide
The conversion factors of the element concentration and the oxide concentration are shown in table 3.
5 Co-existing element interference and selection of analysis lines
Taking a plurality of analysis spectral lines of ten elements such as calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead, zinc and the like, respectively scanning ten element standard solutions of which the concentration is 10 mu g/mL, investigating the mutual interference condition of coexisting elements, selecting a plurality of optional analysis lines of the same element from the ten element standard solutions, and selecting the optimal analysis spectral line with low interference and high signal-to-back ratio. According to experimental results, the selected spectral line signal is strong, the interference is less, the background is simple, and the test requirements can be completely met.
Adding 10 mug/mL standard solutions of Ca, Mg, Al and Ti into the four iron-based solutions of 0, 1, 2 and 3mg/mL respectively, and measuring under the selected working conditions respectively. Experiments show that the intensity ratio of each element analysis spectral line is increased along with the increase of the iron-based concentration, which indicates that the iron matrix has certain interference on the element to be measured, so that the same amount of high-purity iron powder can be added to simulate the composition of actual sample components when a calibration solution is prepared, so as to counteract the spectral interference caused by the matrix element and the physical interference caused by sample extraction and atomization, and simultaneously, the background interference caused by reagent blank and stray light can be eliminated by utilizing the background correction function of the instrument.
6 precision of analytical method
The same samples were tested in parallel 7 times according to analytical procedure 4, the relative standard deviations of which are shown in Table 4.
TABLE 3 conversion of element content to oxide content coefficient
Element(s) | Oxide compound | Conversion coefficient |
Ca | CaO | 1.3992 |
Mg | MgO | 1.6583 |
Cu | CuO | 1.2518 |
Al | Al2O3 | 1.8895 |
Mn | MnO | 1.2912 |
Ti | TiO2 | 1.6683 |
K | K2O | 1.2046 |
Na | Na2O | 1.3480 |
Pb | PbO | 1.0772 |
Zn | ZnO | 1.2447 |
TABLE 4 analytical methods precision (n ═ 7)
Element(s) | Ca | Mg | Cu | Al | Mn | Ti | K | Na | Pb | Zn |
RSD | 1.82 | 0.88 | 0.86 | 0.79 | 1.03 | 1.43 | 4.84 | 4.68 | 3.44 | 1.56 |
As can be seen from the data in Table 4, the RSD of the same sample measured in parallel 7 times is 4.84% at the highest, and is less than 5% at the highest, which indicates that the method of the present invention has high precision.
7 recovery rate test
A certain amount of each element standard solution was added to each sample of known value, and the recovery rate was calculated by the method of the present invention, as shown in Table 5.
TABLE 5 spiking recovery experiment
As can be seen from Table 5, the recovery rate of the spiked sample by the method of the present invention is 95.4-104.2%, so the method of the present invention has good accuracy.
8 conclusion
According to the precision experimental data, the maximum relative standard deviation RSD of each element measured for 7 times on the same sample is 4.84%, and the maximum relative standard deviation RSD is less than 5%, which indicates that the invention has higher precision. According to the recovery rate experimental data, the adding standard recovery rate is 95.4-104.2%, so that the method has better accuracy. Therefore, the method can simultaneously and accurately measure the contents of the ten elements such as calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead, zinc and the like in the blast furnace dust.
9 tolerance difference
The allowable difference of the ten elements such as calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead, zinc and the like in the blast furnace dust is shown in Table 6.
TABLE 6 allowable differences
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (3)
1. A method for measuring the contents of calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead and zinc elements in blast furnace dust is characterized by comprising the following steps:
weighing a blast furnace dust sample in a porcelain boat, placing the porcelain boat in a 600-plus 800 ℃ muffle furnace, slightly opening a furnace door during firing to keep air entering, firing for 1-6 minutes to remove carbon and sulfur, taking out the porcelain boat, transferring the sample into a microwave digestion tank after slightly cooling, firstly adding a small amount of water into a water washing bottle for wetting, then adding aqua regia, covering a sealing cover according to the operating specification of the microwave digestion instrument, placing the porcelain boat into the microwave digestion instrument, connecting a temperature sensor, setting a reaction method according to the number of pressure containers according to microwave digestion conditions, carrying out microwave digestion, taking out the digestion tank after digestion is finished, transferring a digestion solution into a plastic volumetric flask, and determining by using a plasma atomic emission spectrometer after the volume is fixed by pure water;
carrying out a blank test along with the sample, and replacing the sample with high-purity iron to carry out the test so as to ensure that the iron content is consistent with that in the sample to be tested;
drawing a working curve by mixing the standard solutions, respectively adding the standard solutions of the elements to be detected with gradient contents into a 100ml series plastic volumetric flask containing an iron matrix with the same amount as the sample according to the approximate contents of the elements to be detected in the sample to prepare the working curve of the standard solutions with corresponding content ranges, wherein the environment of the mixed standard solutions is matched with that of the sample solutions;
drawing a working curve of the standard sample, selecting 3-4 iron ore standard substances (the iron-based content of which is close to that of the sample) to manufacture the working curve of the standard sample according to the content of each element to be detected in the sample, wherein the dissolving method of the standard sample is the same as that of the sample;
introducing a calibration curve solution from low to high, a blank solution and an iron ore standard substance or a standard addition recovery sample solution and a sample solution into an inductively coupled plasma emission spectrometer to measure the signal intensity of an element to be measured, drawing a calibration solution working curve by taking the signal intensity of the element to be measured as a vertical coordinate and the mass percent of ions as a horizontal coordinate, and calculating the mass percent of the element to be measured by using the calibration curve with known mass percent;
the result calculation formula is as follows:
W(component to be measured)=Wi-W0
In the formula: w(component to be measured)The content and the mass fraction of the element to be detected in the analyte are shown;
Withe content of elements to be measured in the sample solution is the mass percentage;
W0the content and the mass fraction of the element to be detected in the blank solution are shown.
2. The method for determining the contents of calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead and zinc in the blast furnace dust according to claim 1, wherein the microwave digestion instrument adopts an MARS microwave digestion instrument, and the model of the pressure vessel is XP 1500.
3. The method for determining the contents of calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead and zinc in the blast furnace dust according to claim 1, wherein the detection range is as follows: ca%: 0.100% -10.00%; mg%: 0.050% -5.00%; cu%: 0.001% -3.00%; al%: 0.020% -5.00%; mn%: 0.020% -3.00%; ti%: 0.010 percent to 1.50 percent; k: 0.010-20.00%; na: 0.010-20.00%; pb: 0.100-10.00%; zn: 0.005-10.00 percent.
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Application publication date: 20211022 |
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RJ01 | Rejection of invention patent application after publication |