CN109632771A - A method of measurement coal, sludge, dedusting ash, sodium oxide molybdena in covering slag - Google Patents
A method of measurement coal, sludge, dedusting ash, sodium oxide molybdena in covering slag Download PDFInfo
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- CN109632771A CN109632771A CN201910027268.7A CN201910027268A CN109632771A CN 109632771 A CN109632771 A CN 109632771A CN 201910027268 A CN201910027268 A CN 201910027268A CN 109632771 A CN109632771 A CN 109632771A
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Abstract
The invention discloses a kind of methods of sodium oxide molybdena in measurement coal, sludge, dedusting ash, covering slag; include the following steps: the oxygen-enriched calcination of high-temperature sample except after carbon; it decomposed using hydrochloric acid, hydrofluoric acid, closely done to wet salt; dissolving with hydrochloric acid salt is used after cooling; constant volume 100mL utilizes the measurement of sodium oxide molybdena in ICP-AES progress coal, sludge, dedusting ash, covering slag.The present invention is wide using the ICP-AES range of linearity; the high feature of accuracy; a kind of high sensitivity is provided; finding speed is fast; it is easy to operate and small relative to other methods interference; have good selectivity simultaneously, can be provided to smelt Composition Control process the ICP-AES measurement coal of accurate data, sludge, dedusting ash, in covering slag sodium oxide molybdena method.
Description
Technical field
The present invention relates to oxygen in Ferrous Metallurgy analysis field more particularly to a kind of measurement coal, sludge, dedusting ash, covering slag
Change the method for sodium.
Background technique
Iron enterprise can generate a large amount of sludge, dedusting ash, and main component is iron and carbon, recycle as raw materials for sintering
It is feasible.But the enrichment of element such as sodium endanger sintered ironmaking production in dedusting ash, sludge, influence blast fumance direct motion.Therefore, it needs
Accurate Determining is carried out to sodium oxide content in sludge, dedusting ash, different sintering is respectively adopted for different mud, dedusting ash
Ingredient, processing method achieve the purpose that energy-saving and emission-reduction, comprehensive utilization.
Due in coal, sludge, dedusting ash, covering slag carbon content 10% or more, sodium oxide content 0.1~20% it
Between, although fourth is red etc. to discuss " potassium, sodium in atomic absorption spectroscopy determination ion dust mud contaning ", due to atomic absorption spectrometry
The range of linearity is narrow, and sample higher for content needs to dilute step by step after dissolution, standard that is cumbersome, reducing measurement result
Exactness；And the method uses hydrochloric acid, hydrofluoric acid, the direct sample dissolution of perchloric acid, but carbon in the ion dust mud contanings such as sludge, dedusting ash
Content is higher, if do not pre-processed carbon, perchloric acid is added in when molten sample, and sample can burn, to make the measurement knot of sodium oxide molybdena
Fruit is relatively low.Li Huaquan has studied " ICP-AES method measures trace impurity copper, zinc, cadmium, nickel, lead in sludge ", and the method uses
Microwave Digestion is cleared up for the sludge of sewage treatment plant, ICP-AES method measure trace impurity copper in sludge, zinc,
Cadmium, nickel, lead.Tian Wenli etc. studied " measurement and influence factor of potassium, sodium content in coal ash ", and sample is through perchloric acid, hydrofluoric acid
Afterwards, using atomic absorption spectroscopy determination.The above several method is not all satisfied coal of the carbon content 10% or more, dirt
Mud, dedusting ash, in covering slag sodium oxide molybdena analysis demand.
Summary of the invention
In order to solve the above-mentioned technical problem, the present invention is wide using the ICP-AES range of linearity, and the high feature of accuracy provides
A kind of high sensitivity, finding speed is fast, easy to operate and small relative to other methods interference, while having good selectivity,
The ICP-AES that accurate data can be provided to smelt Composition Control process measures coal, sludge, dedusting ash, sodium oxide molybdena in covering slag
Method.
In order to solve the above technical problems, the present invention adopts the following technical scheme:
A method of measurement coal, sludge, dedusting ash, sodium oxide molybdena in covering slag include the following steps: high-temperature sample richness
It after oxygen calcination removes carbon, decomposed using hydrochloric acid, hydrofluoric acid, closely done to wet salt, use dissolving with hydrochloric acid salt after cooling, constant volume 100mL,
Utilize the measurement of sodium oxide molybdena in ICP-AES progress coal, sludge, dedusting ash, covering slag.
Further, the specific steps are as follows:
Step 1: weighing 0.1000g sample in clean, drying cupel, be then placed in the cupel equipped with sample
750 DEG C of Muffle furnace, after oxygen-enriched calcination 30min, taking-up is cooled to room temperature in drier.
Step 2: sample after cooling is transferred to respectively in 200mL polytetrafluoroethylene beaker, sequentially add 15mL hydrochloric acid,
5mL hydrofluoric acid is closely done to wet salt, is removed, be cooled to room temperature after 250 DEG C of low temperature dissolve sample.
Step 3: after 5mL dissolving with hydrochloric acid salt is added in sample after cooling, 15mL high purity water is added, moves into 100mL plastics and holds
In measuring bottle, it is diluted to scale with high purity water, is shaken up, machine in waiting；
Step 4: configuration standard calibration curve solution, for making standard curve；Concrete configuration process is as follows:
Sodium, calcium, silicon, aluminium, magnesium single element standard solution: concentration is 1000 μ g/mL, derives from State center for standard matter；
In order to reduce matrix effect, 6 parts of purity are weighed greater than 99.9% high purity iron 0.050g and are respectively placed in 300mL beaker
In, addition 2mL hydrochloric acid, 3mL nitric acid, 20mL high purity water move into 100mL plastics volumetric flask respectively after dissolving by heating makes solution
Middle mer weight is TFe50%, and calcium, silicon, aluminium, magnesium standard solution is added, and is configured in solution containing CaO5.0%, SiO210.0%,
Al2O33.0%, MgO22.0%, then it is separately added into different amounts of sodium standard solution, so that Na in solution2O content is respectively 0,
0.050%, 0.10%, 1.0%, 5.0%, 10.0%, 25.0%, it is diluted to scale with high purity water, is shaken up；
Step 5, select determining instrument for Optima7300V, the determination of Instrument working parameter: in ICP-AES analytic process,
High-frequency emission power, carrier gas flux directly affect the sensitivity and precision of Instrument measuring, so the running parameter of determining instrument
It is as shown in the table:
| Parameter name | Numerical value |
| RF power (W) | 1300 |
| Cooling gas flow (mL/min) | 15 |
| Secondary air amount (mL/min) | 0.2 |
| Atomization gas flow (mL/min) | 0.8 |
| Input mode | Peristaltic pump sample introduction |
| Sample mode | Peak mode is jumped to sample |
| Number of repetition | 3 |
| Observed pattern | Vertical Observation |
| Washing time (s) | 30 |
| (calculating) mode of integral | PeakArea； |
Step 6: selection spectral line determines that Na589.592nm does analytical line by consulting spectral line library；
Step 7: drawing calibration curve: standards calibration curve solution and blank sample solution are introduced into inductively coupled plasma
Body emission spectrometer measures the signal strength to measured ion, and using mass percent as abscissa, the signal strength of ion is vertical sits
Plotting Na2O calibration curve；
Step 8: specimen sample solution, blank sample solution introduce inductive coupling plasma emission spectrograph, measurement to
The signal strength of measured ion, according to the Na of known quality percentage2O standard solution calibration curve, finds out Na in sample solution2O's
Content；
Na in sample2The content of O is calculated as follows:
W%=Wi-W0；
In formula: the mass percentage of element in W- sample；W0- element mass percent in blank solution to be measured；Wi-
Mass percent of the element in sample to be measured；
This method detection range is 0.010at~25.0at%.
Compared with prior art, advantageous effects of the invention:
Measurement of the present invention for sodium oxide molybdena in coal, sludge, dedusting ash, covering slag, by the high-temperature oxygen-enriched calcination of sample
After carbon, surveyed using the measurement of sodium oxide molybdena in ICP-AES progress sludge, dedusting ash, covering slag using Vertical Observation mode
Determine the range of sodium oxide molybdena: Na2O0.010at~25.0at%, is more suitable for the higher coal of sodium oxide molybdena, carbon content, sludge, dedusting
The analysis of ash, covering slag sample.The present invention passes through the multiple inspection to coal, sludge, dedusting ash, covering slag sample, application effect
Well.The present invention eliminates Matrix effects using Matrix Match, has the range of linearity wide, and high sensitivity is easy to operate, analyzes result
Accurately, feature reliably provides reliable data for the recycling and reusing of sludge, dedusting ash.
In addition, being conducive to environmental protection present invention substantially reduces hydrochloric acid, hydrofluoric acid equal solvent usage amount.
Specific embodiment
1, in the embodiment of the present invention, agents useful for same is preferred:
Hydrochloric acid: excellent pure grade；
Hydrofluoric acid: excellent pure grade；
Sodium, silicon, calcium, magnesium, aluminium single element standard solution: concentration is 1000 μ g/mL, derives from State center for standard matter；
Sodium oxide molybdena standard substance；
High purity iron (purity is 99.9% or more)；
100mL plastics volumetric flask；200mL polytetrafluoroethylene beaker；Argon gas: purity of argon >=99.9%.
Compressed air
2, preferably inductive coupling plasma emission spectrograph model PE company Optima7300V；ICP-AES instrument work
It is as follows to make parameter:
| Parameter name | Numerical value |
| RF power (W) | 1300 |
| Cooling gas flow (mL/min) | 15 |
| Secondary air amount (mL/min) | 0.2 |
| Atomization gas flow (mL/min) | 0.8 |
| Input mode | Peristaltic pump sample introduction |
| Sample mode | Peak mode is jumped to sample |
| Number of repetition | 3 |
| Observed pattern | Vertical Observation |
| Washing time (s) | 30 |
| (calculating) mode of integral | PeakArea； |
3, sample analysis
Blank assay: weighing 0.080g di-iron trioxide, does blank assay in company with sample.
It weighs 0.1000g sample to be placed in cupel, after 750 DEG C of Muffle furnace, oxygen-enriched calcination 30min, take out in drying
It is cooled to room temperature in device.
Sample after cooling is transferred to respectively in 200mL polytetrafluoroethylene beaker, 15mL hydrochloric acid, 5mL hydrogen are sequentially added
Fluoric acid is closely done to wet salt, is removed, be cooled to room temperature after 250 DEG C of low temperature dissolve sample.
After 5mL dissolving with hydrochloric acid salt is added in sample after cooling, 15mL high purity water is added, moves into 100mL plastics volumetric flask,
It is diluted to scale with high purity water, is shaken up, machine in waiting.
The configuration of standards calibration curve solution:
6 parts of high purity irons (purity be greater than 99.9%) 0.050g is weighed in 300mL beaker, be added 2mL hydrochloric acid, 3mL nitric acid,
20mL high purity water moves into 100mL plastics volumetric flask after dissolving by heating makes in solution mer weight be TFe50%, be added calcium, silicon,
Aluminium, magnesium standard solution are configured in solution containing CaO5.0%, SiO210.0%, Al2O33.0%, MgO22.0%, then add respectively
Enter different amounts of sodium standard solution so that in solution Na2O content be respectively 0,0.050%, 0.10%, 1.0%, 5.0%,
10.0%, 25.0%, it is diluted to scale with high purity water, is shaken up.This solution makes standard curve and uses.
Na589.592nm is selected to do analytical line.Draw calibration curve: by standards calibration curve solution and blank sample solution
Inductive coupling plasma emission spectrograph is introduced, the signal strength to measured ion is measured, using mass percent as abscissa, from
The signal strength of son is that ordinate draws Na2O calibration curve.Specimen sample solution, blank sample solution introduce inductive coupling etc.
Ionomer emission spectrum instrument measures the signal strength to measured ion, according to the Na of known quality percentage2The calibration of O standard solution
Curve finds out Na in sample solution2The content of O.
Na in sample2The content of O is calculated as follows:
W%=Wi-W0
In formula: the mass percentage of element in W- sample；
W0- element mass percent in blank solution to be measured；
Mass percent of the Wi- element in sample to be measured；
This method detection range: 0.010at~25.0at%.
Embodiment 1
Working curve is made according to the above method, and curve correlation coefficient r is greater than 0.999, prepares 11 parts of blank by experimental method
Solution, which divides 3 times, to be measured, the detection limit formula CL=3Sb/ defined according to International Union of Pure and Applied Chemistry (IUPAC)
K (Sb be blank standard deviation, k be corresponding Slope of Calibration Curve) calculate method detection be limited to 0.001%.
Embodiment 2
Weigh potassium feldspar (GBW03116), containing symplesite (YSBC14721-98), bloodstone (YSBC28756-2008), sodium
Feldspar (GBW03134), soda-lime-silica glass (GBW03117) are measured according to the above method, the results are shown in Table 1.
1 standard sample measurement result of table
Embodiment 3
Weigh mild-clay (GBW03115), albite (GBW03134), soda-lime-silica glass (GBW03117) standard sample
Sodium oxide molybdena standard substance is added in several pieces and mud sample, covering slag sample, dedusting ash sample, is measured according to the above method,
It the results are shown in Table 2.
The measurement result of 2 standard sample mark-on reclaims of table
Embodiment 4
Claim coal 2# sample, sludge 3# sample, dedusting ash 2#, 3# sample, covering slag 2#, 3# sample is surveyed according to the above method
It is fixed, it the results are shown in Table 3.
3 sample specimens measurement result of table
Therefore, pass through the verifying of above-mentioned embodiment, it can be seen that coal of the present invention, dedusting ash, aoxidizes in covering slag sludge
The measurement of sodium, using Vertical Observation mode, measures oxygen by the high-temperature oxygen-enriched calcination of sample except being measured after carbon using ICP-AES
Change the range of sodium: Na2O 0.010at~25.0at%.The present invention by coal, sludge, dedusting ash, covering slag sample it is multiple
It examines, application effect is good.The present invention eliminates Matrix effects using Matrix Match, has the range of linearity wide, high sensitivity, operation
Simplicity, accurate, the reliable feature of analysis result, provides reliable data for the recycling and reusing of sludge, dedusting ash, can produce
Middle popularization, use.
Embodiment described above is only that preferred embodiment of the invention is described, and is not carried out to the scope of the present invention
It limits, without departing from the spirit of the design of the present invention, those of ordinary skill in the art make technical solution of the present invention
Various changes and improvements, should all fall into claims of the present invention determine protection scope in.
Claims (4)
1. a kind of method of sodium oxide molybdena in measurement coal, sludge, dedusting ash, covering slag, which comprises the steps of: will
It after the oxygen-enriched calcination of high-temperature sample removes carbon, decomposed, closely done to wet salt using hydrochloric acid, hydrofluoric acid, use dissolving with hydrochloric acid salt after cooling,
Constant volume 100mL utilizes the measurement of sodium oxide molybdena in ICP-AES progress coal, sludge, dedusting ash, covering slag.
2. the method for sodium oxide molybdena in measurement coal according to claim 1, sludge, dedusting ash, covering slag, which is characterized in that
Specific step is as follows:
Step 1: it weighs sample and is placed in clean, drying cupel, the cupel equipped with sample is then placed in Muffle furnace, it is rich
After oxygen calcination, taking-up is cooled to room temperature in drier；
Step 2: sample after cooling being transferred in polytetrafluoroethylene beaker, hydrochloric acid, hydrofluoric acid, 250 DEG C of low temperature are sequentially added
After sample is dissolved, closely does to wet salt, remove, be cooled to room temperature；
Step 3: after dissolving with hydrochloric acid salt is added in sample after cooling, high purity water is added, moves into plastics volumetric flask, it is dilute with high purity water
It releases to scale, shakes up, machine in waiting；
Step 4: configuration standard calibration curve solution, for making standard curve；
Step 5, select determining instrument for Optima7300V；
Step 6: selection spectral line determines that Na589.592nm does analytical line by consulting spectral line library；
Step 7: drawing calibration curve: standards calibration curve solution and blank sample solution are introduced into inductively coupled plasma body hair
Spectrometer is penetrated, measures the signal strength to measured ion, using mass percent as abscissa, the signal strength of ion is drawn for ordinate
Na processed2O calibration curve；
Step 8: specimen sample solution, blank sample solution introduce inductive coupling plasma emission spectrograph, measure it is to be measured from
The signal strength of son, according to the Na of known quality percentage2O standard solution calibration curve, finds out Na in sample solution2O's contains
Amount；
Na in sample2The content of O is calculated as follows:
W%=Wi-W0；
In formula: the mass percentage of element in W- sample；W0- element mass percent in blank solution to be measured；Wi- element
Mass percent in sample to be measured；
This method detection range is 0.010at~25.0at%.
3. the method for sodium oxide molybdena in measurement coal according to claim 1, sludge, dedusting ash, covering slag, which is characterized in that
Detailed process is as follows for configuration standard calibration curve solution in the step 4:
Sodium, calcium, silicon, aluminium, magnesium single element standard solution: concentration is 1000 μ g/mL, derives from State center for standard matter；
In order to reduce matrix effect, weighs 6 parts of purity and be respectively placed in 300mL beaker greater than 99.9% high purity iron 0.050g, added
Enter 2mL hydrochloric acid, 3mL nitric acid, 20mL high purity water to move into respectively in 100mL plastics volumetric flask after dissolving by heating and make matrix in solution
Amount is TFe50%, and calcium, silicon, aluminium, magnesium standard solution is added, and is configured in solution containing CaO5.0%, SiO210.0%,
Al2O33.0%, MgO22.0%, then it is separately added into different amounts of sodium standard solution, so that Na in solution2O content is respectively 0,
0.050%, 0.10%, 1.0%, 5.0%, 10.0%, 25.0%, it is diluted to scale with high purity water, is shaken up.
4. the method for sodium oxide molybdena in measurement coal according to claim 1, sludge, dedusting ash, covering slag, which is characterized in that
The running parameter of the determining instrument is as shown in the table:
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| CN113533307A (en) * | 2021-06-10 | 2021-10-22 | 包头钢铁（集团）有限责任公司 | Method for measuring contents of calcium, magnesium, copper, aluminum, manganese, titanium, potassium, sodium, lead and zinc elements in blast furnace dust |
| CN114062359A (en) * | 2021-11-09 | 2022-02-18 | 西安热工研究院有限公司 | A method for rapid detection of soluble Na content in coal |
| CN114674771A (en) * | 2022-04-20 | 2022-06-28 | 新疆八一钢铁股份有限公司 | Method for measuring trace elements in European smelter precipitator dust |
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Application publication date: 20190416 |