CN108956586A - The rapid assay methods of lithia, potassium oxide, sodium oxide molybdena in continuous casting covering slag - Google Patents

The rapid assay methods of lithia, potassium oxide, sodium oxide molybdena in continuous casting covering slag Download PDF

Info

Publication number
CN108956586A
CN108956586A CN201810820554.4A CN201810820554A CN108956586A CN 108956586 A CN108956586 A CN 108956586A CN 201810820554 A CN201810820554 A CN 201810820554A CN 108956586 A CN108956586 A CN 108956586A
Authority
CN
China
Prior art keywords
covering slag
solution
continuous casting
lithia
potassium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810820554.4A
Other languages
Chinese (zh)
Inventor
王文焱
郭健
冯晴晴
张军
郑迅燕
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tangshan Iron and Steel Group Co Ltd
HBIS Co Ltd Tangshan Branch
Original Assignee
Tangshan Iron and Steel Group Co Ltd
HBIS Co Ltd Tangshan Branch
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tangshan Iron and Steel Group Co Ltd, HBIS Co Ltd Tangshan Branch filed Critical Tangshan Iron and Steel Group Co Ltd
Priority to CN201810820554.4A priority Critical patent/CN108956586A/en
Publication of CN108956586A publication Critical patent/CN108956586A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/73Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches

Landscapes

  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Plasma & Fusion (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention discloses the rapid assay methods of lithia, potassium oxide, sodium oxide molybdena in a kind of continuous casting covering slag, the described method comprises the following steps: 1) continuous casting covering slag resolution process;2) prepared by covering slag sample solution;3) standard solution of component to be measured is prepared;4) calibration curve is drawn;5) each component content in covering slag sample is measured.The present invention has many advantages, such as that the range of linearity is wide, accuracy is high, easy to operate, quick, sensitive, reagent dosage is few; laboratory pollution can be reduced; the measurement period is shortened using plasma spectrometer, meets the incoming test of continuous casting covering slag and the analysis requirement of production scene practical application.

Description

The rapid assay methods of lithia, potassium oxide, sodium oxide molybdena in continuous casting covering slag
Technical field
The invention belongs to chemical analysis technical fields, and in particular to refer to lithia, potassium oxide, oxygen in a kind of continuous casting covering slag Change the rapid assay methods of sodium.
Background technique
In the casting process of molten steel, covering slag, which is added, can be improved slab quality, prevent Longitudinal Surface Cracks, absorption dissolution from The field trash of steel slag circle, cleaning molten steel are floated in molten steel, and can completely cut off air, effectively prevent secondary oxidation of steel and heat It scatters and disappears.The guarantor of different type, property and purposes is derived under the conditions of different steel grade, different casting machines, different continuous casting process Protect slag.Ingredient by changing covering slag can control the performances such as crystallinity and the thermal resistance of slag film, to efficiently control slab The generation of surface defect, therefore, the chemical component of Accurate Determining covering slag have a very important significance.
Currently, no national standard considerably less for the detection means of lithia, potassium oxide and sodium oxide content in covering slag Method and standard substance.Flame atomic absorption method and inductively coupled plasma emission spectrography are only used, wherein lithia Measurement use flame atomic absorption method, searching document finds no using inductively coupled plasma emission spectrography;Oxidation Sodium, potassium oxide mostly use industry standard methods and inductively coupled plasma emission spectrography.Due to atomic absorption analysis method Need to measure lithium, sodium, potassium element respectively compared with inductively coupled plasma emission spectrography, analytical procedure is cumbersome, the period It is longer, it is not suitable with the current demand quickly analyzed and produced.
The present invention develops the rapid assay methods of lithia, potassium oxide, sodium oxide molybdena in a kind of continuous casting covering slag, using electricity Feel coupled plasma optical emission spectroscopic methodology and measures the fast of lithia in continuous casting covering slag containing lithium, potassium oxide and sodium oxide molybdena ingredient simultaneously Fast analysis method, limitation, the analytical procedure for overcoming atomic absorption method are cumbersome, same without lithia, potassium oxide and sodium oxide molybdena When method for measuring problem, solve high temperature sintering except the relatively time consuming cumbersome and sample loss that is may cause of the operating procedure of carbon is asked Topic meets the real work requirement of covering slag product composition quality control and production scene, is the production of covering slag standard substance Formulation with standard method provides reference.
Summary of the invention
The technical problem to be solved in the present invention is to provide lithia in a kind of continuous casting covering slag, potassium oxide, sodium oxide molybdena it is fast Fast measuring method, limitation, the analytical procedure for solving atomic absorption method are cumbersome, simultaneously without lithia, potassium oxide and sodium oxide molybdena Method for measuring problem.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: lithia, oxidation in a kind of continuous casting covering slag The rapid assay methods of potassium, sodium oxide molybdena, the described method comprises the following steps:
(1) it continuous casting covering slag resolution process: accurately weighs continuous casting covering slag sample (being accurate to mg) and is put into polytetrafluoroethylene beaker In, be added 5~6mL nitric acid, 5~6mL hydrochloric acid, 4~5mL hydrofluoric acid, 5~6mL perchloric acid on low temperature electric hot plate heat resolve, It is closely dry to emit perchloric acid cigarette, removes, cooled to room temperature;
(2) prepared by covering slag sample solution: hydrochloric acid is added in beaker after the cooling period and dissolves by heating salt on low temperature electric hot plate, Beaker is removed, is cooled to room temperature with flowing water, solution is moved into plastics volumetric flask, V is added 4ML yttrium standard solution is dilute with water It releases to scale, mixes, be filled into plastic funnel, Medium speed filter paper in the plastic containers of other dried and clean, obtain covering slag Sample solution;
(3) prepare the standard solution of component to be measured: standard stock solution lithium, sodium, potassium, yttrium concentration are 1000 μ g/mL, and the used time will Lithium standard stock solution is diluted to 100 μ g/mL standard solution, and potassium standard stock solution is diluted to 100 μ g/mL standard solution, Yttrium standard stock solution is diluted to 10 μ g/mL standard solution;
(4) it draws calibration curve: being separately added into V at least five plastics volumetric flask4ML yttrium standard solution, then be separately added into not Lithium, sodium, the potassium standard solution of same volume, are prepared into calibration serial solution, are converted into the concentration of lithia, sodium oxide molybdena, potassium oxide, Draw out calibration curve;
The wavelength for selecting each calibration list of target element, measures each calibration solution respectively on the ICP spectrometer after having optimized Object element spectral line is to the relative intensity of yttrium, using each calibration solution concentration as abscissa, the relative line intensities of object element For ordinate, instrument automatic returning draws out series of calibration curve;
(5) it measures each component content in covering slag sample: carrying out the survey of covering slag sample after the measurement of completion step (4) at once Amount guarantees that calibration curve is identical as the measuring condition of sample, measures each target in covering slag sample solution respectively in ICP spectrometer The spectral line of element calculates each component content in covering slag sample according to calibration curve to the relative intensity of yttrium.
Covering slag sample is 105~110 DEG C of 1.5~2 h of drying and the cooling in drier in the step (1) of the present invention To room temperature, the granularity of sample grinding preparation is less than 0.097mm.
Covering slag sample sample weighting amount is 0.1000~0.2000g in the step (1) of the present invention.
In the step (1) of the present invention on low temperature electric hot plate 150~200 DEG C be heated to covering slag sample decomposition.
4~5mL of hydrochloric acid is added in step (2) of the present invention in substance after cooling.
Hydrochloric acid is added in step (2) of the present invention in substance after cooling to heat on 150~200 DEG C of low temperature electric hot plates To dissolved salts.
The concentration range that lithia calibration solution is prepared in step (4) of the present invention is 0.00-2.16%, sodium oxide molybdena school The concentration range that quasi- solution is prepared is 0.00-13.50%, and it is 0.00-1.20% that potassium oxide, which calibrates the concentration range that solution is prepared,.
Vessel used in the method for the invention using it is preceding impregnated with (1+9) dilute hydrochloric acid solution >=for 24 hours, and with ultrapure Drying for standby after water cleaning.
The method of the invention is ultrapure water with water, resistivity >=18M Ω cm.
In step (3) of the present invention, yttrium, lithium, potassium standard solution preparation method are as follows: 10 μ g/mL yttrium standard solution are matched Method processed: it is 1000 μ g/mL yttrium standard stock solutions into 100mL volumetric flask that pipette, which pipettes 10.00mL concentration, is diluted with water To scale, mix;Again from 10.00mL solution is pipetted in this volumetric flask into 100mL volumetric flask, it is diluted with water to scale, is mixed It is spare;
The preparation method of 100 μ g/mL lithium standard solution: it is that 1000 μ g/mL lithium standards reserve is molten that pipette, which pipettes 10.00mL concentration, Liquid is diluted with water to scale into 100mL volumetric flask, mixes spare;
The preparation method of 100 μ g/mL potassium standard solution: it is that 1000 μ g/mL potassium standards reserve is molten that pipette, which pipettes 10.00mL concentration, Liquid is diluted with water to scale into 100mL volumetric flask, mixes spare.
The present invention passes through the comparison of external standard method and standard addition method, to the accuracy of measurement of lithia, potassium oxide, sodium oxide molybdena Verified, verified using accuracy of measurement of the covering slag reference material to sodium oxide molybdena, and carried out method precision, Recovery test, it is determined that external standard method establishes standard curve determination lithia, potassium oxide and sodium oxide molybdena ingredient.
The beneficial effects of adopting the technical scheme are that the 1, present invention is inductively coupled plasma spectrometry Method can measure various ingredients simultaneously, while several times have also been enlarged in the range for measuring element, to realize single-time measurement guarantor Protect the various ingredients content in slag.2, measurement result of the present invention is accurate and reliable, easy to operate, and reagent dosage is greatly reduced, analysis Speed improves 70% or more, shortens the measurement period, meets the comprehensive utilization and production scene real work requirement of covering slag. 3, the present invention passes through the carbon for being simply and rapidly filtered to remove high-content in sample, prevents that sample introduction can be blocked after importing ICP spectrometer System removes carbon ratio with high temperature sintering, and sample can be prevented because high temperature sintering loses, easy to operate quick, improves the accurate of measurement Property.4, the present invention is found by experiment that, after yttrium standard liquid is added, is compensated for since instrument operating condition, nebulization efficiency and matrix are imitated The interference of non-spectral caused by should waiting, effectively improves the preci-sion and accuracy that main component measures in covering slag.5, this hair It is bright to have many advantages, such as that the range of linearity is wide, accuracy is high, easy to operate, quick, sensitive, reagent dosage is few, laboratory dirt can be reduced Dye shortens the measurement period using plasma spectrometer, and incoming test and the production scene for meeting continuous casting covering slag are practical The analysis requirement of application.
Detailed description of the invention
Fig. 1 is the calibration graph of sodium element;
Fig. 2 is the calibration graph of potassium element;
Fig. 3 is the calibration graph of elemental lithium.
Specific embodiment
The present invention is described in further detail in the following with reference to the drawings and specific embodiments.
Key instrument involved in embodiment and reagent are as follows:
1) key instrument: Optima 4300DV type composes direct-reading Bidirectional observation plasma emission spectrometer (PE company of the U.S.) entirely, SCD detector, echelle grating, axial-radial Bidirectional observation.
2) main agents: hydrochloric acid, about 1.19 g/mL of ρ;Nitric acid, ρ about 1.42g/mL;Hydrofluoric acid, ρ about 1.15g/mL;High chlorine Acid, ρ about 1.76g/mL, agents useful for same are that analysis is pure.
3) covering slag reference material (commercially available): number YSBC26801-2013.
Embodiment 1
Lithia in a kind of continuous casting covering slag of the present embodiment, potassium oxide, sodium oxide molybdena rapid assay methods the following steps are included:
(1) continuous casting covering slag resolution process: covering slag sample is 105~110 DEG C of 1.5~2 h of drying and the cooling in drier To room temperature, grinding is prepared as granularity≤0.097mm protection slag sample;
0.1000g protection slag sample is weighed in 500mL polytetrafluoroethylene beaker, with 20mL ultrapure water walls of beaker, is added 5mL nitric acid, 5mL hydrochloric acid, 5mL hydrofluoric acid, 5mL perchloric acid on low temperature electric hot plate heat resolve, to emit perchloric acid cigarette closely dry, remove It is cooling;
(2) prepared by covering slag sample solution: the 150 DEG C of heating on low temperature electric hot plate of 5mL hydrochloric acid being added in beaker after the cooling period Dissolved salts remove beaker, are cooled to room temperature with flowing water, and solution is moved into 100mL plastics volumetric flask, and 10.00mL is added Yttrium (concentration is 10 μ g/mL) standard solution, is diluted to scale with ultrapure water, mixes, be filled into separately with plastic funnel, Medium speed filter paper In the plastic containers of outer dried and clean, covering slag sample solution is obtained;
(3) standard solution of component to be measured is prepared:
The preparation method of 10 μ g/mL yttrium standard solution: it is that 1000 μ g/mL yttrium standards reserve is molten that pipette, which pipettes 10.00mL concentration, Liquid is diluted with water to scale into 100mL volumetric flask, mixes;10.00mL solution is pipetted from this volumetric flask again to 100mL appearance In measuring bottle, it is diluted with water to scale, is mixed spare;
The preparation method of 100 μ g/mL lithium standard solution: it is that 1000 μ g/mL lithium standards reserve is molten that pipette, which pipettes 10.00mL concentration, Liquid is diluted with water to scale into 100mL volumetric flask, mixes spare;
The preparation method of 100 μ g/mL potassium standard solution: it is that 1000 μ g/mL potassium standards reserve is molten that pipette, which pipettes 10.00mL concentration, Liquid is diluted with water to scale into 100mL volumetric flask, mixes spare.
(4) preparation of calibration curve serial solution: it is molten in 5 100mL plastics volumetric flasks to be separately added into 10mL yttrium standard Liquid is separately added into the lithium, sodium, potassium standard solution of different volumes by table 1, adds 5mL hydrochloric acid (ρ about 1.19g/mL), use is ultrapure Water is diluted to scale, mixes, is prepared into calibration serial solution, simple substance element is converted into the corresponding mass fraction of oxide, oxygen The concentration range for changing lithium calibration solution is 0.00-2.16%, and the concentration range that sodium oxide molybdena calibrates solution is 0.00-13.50%, oxidation The concentration range that potassium calibrates solution is 0.00-1.20%;Draw calibration curve.
Each component standard curve is as follows: lithium y=41542x+2376(R2=1);Sodium y=46403x+1052(R2=1);Sodium y= 15399x+45.02(R2=1)
1 lithium of table, sodium, potassium series of calibration solution concentration
(5) drafting of calibration curve: unlatching ICP spectrometer, the operating condition optimized by table 2,3 element correspondence analysis line of table, according to Relative intensity of the object element spectral line to yttrium in secondary measurement calibration serial solution:
The operating condition of 2 ICP spectrometer of table
3 element of table recommends analytical line
Using the concentration of each calibration solution as abscissa, the relative intensity for corresponding to object element spectral line is ordinate, and instrument is automatic Calibration curve is drawn out in recurrence, as shown in Figure 1, Figure 2, Figure 3 shows;
(6) it measures each component content in covering slag sample: having measured calibration curve on ICP spectrometer, measured covering slag immediately The relative line intensity of each object element in sample solution guarantees that it is consistent with the calibration curve test condition of drafting, according to mark Quasi- working curve calculates the percentage composition of each component in covering slag.
(7) precision and accuracy test are carried out to sample: is measured in parallel 10 times, the results are shown in Table according to above-mentioned test procedure 4, relative standard deviation (RSD%) is respectively less than 4.0%, and precision is good, meets detection needs, and using standard addition method to this Sample is verified, and potassium oxide measured by two methods, lithia result are consistent as shown in Table 4.
Lithia, potassium oxide, sodium oxide molybdena precision, accuracy testing result in 4 continuous casting covering slag sample of table
(8) precision, accuracy test: selection one covering slag reference material close with sample to be tested sodium oxide content, It is measured in parallel 10 times according to above-mentioned test procedure, calculates the average value and relative standard deviation (RSD%) of sodium oxide molybdena, the results are shown in Table 5, the deviation of measured value and asserting value is 0.03%, and for relative standard deviation less than 1.00%, accuracy and precision are fine.
5 sodium oxide molybdena ingredient precision of table, accuracy validation result
Embodiment 2
Lithia in a kind of continuous casting covering slag of the present embodiment, potassium oxide, sodium oxide molybdena rapid assay methods the following steps are included:
(1) continuous casting covering slag resolution process: covering slag sample is 105~110 DEG C of 1.5~2 h of drying and the cooling in drier To room temperature, grinding is prepared as granularity≤0.097mm protection slag sample;
0.2000g protection slag sample is weighed in 500mL polytetrafluoroethylene beaker, with 15mL ultrapure water walls of beaker, is added 6mL nitric acid, 6mL hydrochloric acid, 5mL hydrofluoric acid, 6mL perchloric acid on low temperature electric hot plate heat resolve, to emit perchloric acid cigarette closely dry, remove It is cooling;
(2) prepared by covering slag sample solution: the 200 DEG C of heating on low temperature electric hot plate of 5mL hydrochloric acid being added in beaker after the cooling period Dissolved salts remove beaker, are cooled to room temperature with flowing water, and solution is moved into 100mL plastics volumetric flask, and 10.00mL is added Yttrium (concentration is 10 μ g/mL) standard solution, is diluted to scale with ultrapure water, mixes, be filled into separately with plastic funnel, Medium speed filter paper In the plastic containers of outer dried and clean, covering slag sample solution is obtained;
(3) standard solution of component to be measured is prepared:
The preparation method of 10 μ g/mL yttrium standard solution: it is that 1000 μ g/mL yttrium standards reserve is molten that pipette, which pipettes 10.00mL concentration, Liquid is diluted with water to scale into 100mL volumetric flask, mixes;10.00mL solution is pipetted from this volumetric flask again to 100mL appearance In measuring bottle, it is diluted with water to scale, is mixed spare;
The preparation method of 100 μ g/mL lithium standard solution: it is that 1000 μ g/mL lithium standards reserve is molten that pipette, which pipettes 10.00mL concentration, Liquid is diluted with water to scale into 100mL volumetric flask, mixes spare;
The preparation method of 100 μ g/mL potassium standard solution: it is that 1000 μ g/mL potassium standards reserve is molten that pipette, which pipettes 10.00mL concentration, Liquid is diluted with water to scale into 100mL volumetric flask, mixes spare.
(5) preparation of calibration curve serial solution: it is molten in 5 100mL plastics volumetric flasks to be separately added into 10mL yttrium standard Liquid is separately added into the lithium, sodium, potassium standard solution of different volumes by table 1, adds 5mL hydrochloric acid (ρ about 1.19g/mL), use is ultrapure Water is diluted to scale, mixes, is prepared into calibration serial solution, simple substance element is converted into the corresponding mass fraction of oxide, oxygen The concentration range for changing lithium calibration solution is 0.00-2.16%, and the concentration range that sodium oxide molybdena calibrates solution is 0.00-13.50%, oxidation The concentration range that potassium calibrates solution is 0.00-1.20%;Draw calibration curve (see Table 1).
Each component standard curve is as follows: lithium y=41542x+2376(R2=1);Sodium y=46403x+1052(R2=1);Sodium y= 15399x+45.02(R2=1)
(5) drafting of calibration curve: unlatching ICP spectrometer, the operating condition optimized by table 2,3 element correspondence analysis line of table, according to Relative intensity of the object element spectral line to yttrium in secondary measurement calibration serial solution;
Using the concentration of each calibration solution as abscissa, the relative intensity for corresponding to object element spectral line is ordinate, and instrument is automatic Calibration curve is drawn out in recurrence, as shown in Figure 1, Figure 2, Figure 3 shows;
(6) it measures each component content in covering slag sample: having measured calibration curve on ICP spectrometer, measured covering slag immediately The relative line intensity of each object element in sample solution guarantees that it is consistent with the calibration curve test condition of drafting, according to mark Quasi- working curve calculates the percentage composition of each component in covering slag.
(7) sample is tested: is measured in parallel 10 times according to above-mentioned test procedure, the results are shown in Table 6, relative standard deviation (RSD%) it is respectively less than 4.0%, as shown in Table 6 in the condition and range that method allows, changes reagent dosage and sample weighing quality, Same sample is measured, measured potassium oxide, lithia, sodium oxide molybdena results change are little, it was demonstrated that the precision of method It is fine with stability.
Lithia, potassium oxide testing result in 6 continuous casting covering slag sample of table
Above-described embodiment illustrates the rapid assay methods of lithia, potassium oxide, sodium oxide molybdena in continuous casting covering slag of the present invention, has line Property the advantages that range is wide, accuracy is high, easy to operate, quick, sensitive, reagent dosage is few, laboratory pollution can be reduced, applied Plasma spectrometer shortens the measurement period, meets the incoming test of continuous casting covering slag and point of production scene practical application Analysis requires.
The above embodiments are only used to illustrate and not limit the technical solutions of the present invention, although referring to above-described embodiment to this hair It is bright to be described in detail, those skilled in the art should understand that: still the present invention can be modified or be waited With replacement, without departing from the spirit or scope of the invention, or any substitutions, should all cover in power of the invention In sharp claimed range.

Claims (10)

1. the rapid assay methods of lithia, potassium oxide, sodium oxide molybdena in a kind of continuous casting covering slag, which is characterized in that the method The following steps are included:
(1) continuous casting covering slag resolution process: accurately weighing continuous casting covering slag sample and be put into polytetrafluoroethylene beaker, and addition 5~ 6mL nitric acid, 5~6mL hydrochloric acid, 4~5mL hydrofluoric acid, 5~6mL perchloric acid on low temperature electric hot plate heat resolve, emit perchloric acid cigarette It is close dry, it removes, cooled to room temperature;
(2) prepared by covering slag sample solution: hydrochloric acid is added in beaker after the cooling period and dissolves by heating salt on low temperature electric hot plate, Beaker is removed, is cooled to room temperature with flowing water, solution is moved into plastics volumetric flask, V is added 4ML yttrium standard solution is dilute with water It releases to scale, mixes, be filled into plastic funnel, Medium speed filter paper in the plastic containers of other dried and clean, obtain covering slag Sample solution;
(3) prepare the standard solution of component to be measured: standard stock solution lithium, sodium, potassium, yttrium concentration are 1000 μ g/mL, and the used time will Lithium standard stock solution is diluted to 100 μ g/mL standard solution, and potassium standard stock solution is diluted to 100 μ g/mL standard solution, Yttrium standard stock solution is diluted to 10 μ g/mL standard solution;
(4) it draws calibration curve: being separately added into V at least five plastics volumetric flask4ML yttrium standard solution, then it is separately added into difference Lithium, sodium, the potassium standard solution of volume, are prepared into calibration serial solution, are converted into the concentration of lithia, sodium oxide molybdena, potassium oxide, draw Produce calibration curve;
The wavelength for selecting each calibration list of target element, measures each calibration solution respectively on the ICP spectrometer after having optimized Object element spectral line is to the relative intensity of yttrium, using each calibration solution concentration as abscissa, the relative line intensities of object element For ordinate, instrument automatic returning draws out series of calibration curve;
(5) it measures each component content in covering slag sample: carrying out the survey of covering slag sample after the measurement of completion step (4) at once Amount guarantees that calibration curve is identical as the measuring condition of sample, measures each target in covering slag sample solution respectively in ICP spectrometer The spectral line of element calculates each component content in covering slag sample according to calibration curve to the relative intensity of yttrium.
2. the rapid assay methods of lithia, potassium oxide, sodium oxide molybdena in a kind of continuous casting covering slag according to claim 1, It is characterized in that, covering slag sample is 105~110 DEG C of 1.5~2 h of drying and is cooled in drier in the step (1) Room temperature, granularity≤0.097mm of sample grinding preparation.
3. the rapid assay methods of lithia, potassium oxide, sodium oxide molybdena in a kind of continuous casting covering slag according to claim 1, It is characterized in that, covering slag sample sample weighting amount is 0.1000~0.2000g in the step (1).
4. the rapid assay methods of lithia, potassium oxide, sodium oxide molybdena in a kind of continuous casting covering slag according to claim 1, It is characterized in that, in the step (1) on low temperature electric hot plate 150~200 DEG C be heated to covering slag sample decomposition.
5. lithia in a kind of continuous casting covering slag according to any one of claims 1-4, potassium oxide, sodium oxide molybdena is quick Measuring method, which is characterized in that 4~5mL of hydrochloric acid is added in the step (2) in substance after cooling.
6. lithia in a kind of continuous casting covering slag according to any one of claims 1-4, potassium oxide, sodium oxide molybdena is quick Measuring method, which is characterized in that hydrochloric acid is added in the step (2) in substance after cooling in 150~200 DEG C of low temperature electric hot plates On be heated to dissolved salts.
7. lithia in a kind of continuous casting covering slag according to any one of claims 1-4, potassium oxide, sodium oxide molybdena is quick Measuring method, which is characterized in that the concentration range that lithia calibration solution is prepared in the step (4) is 0.00-2.16%, oxygen Changing the concentration range that sodium calibration solution is prepared is 0.00-13.50%, and it is 0.00- that potassium oxide, which calibrates the concentration range that solution is prepared, 1.20%。
8. lithia in a kind of continuous casting covering slag according to any one of claims 1-4, potassium oxide, sodium oxide molybdena is quick Measuring method, which is characterized in that vessel used in the method using it is preceding impregnated with (1+9) dilute hydrochloric acid solution >=for 24 hours, and Drying for standby after being cleaned with ultrapure water.
9. lithia in a kind of continuous casting covering slag according to any one of claims 1-4, potassium oxide, sodium oxide molybdena is quick Measuring method, which is characterized in that the method is ultrapure water with water, resistivity >=18M Ω cm.
10. lithia in a kind of continuous casting covering slag according to any one of claims 1-4, potassium oxide, sodium oxide molybdena is fast Fast measuring method, which is characterized in that in the step (3), yttrium, lithium, potassium standard solution preparation method are as follows: 10 μ g/mL yttrium standards The preparation method of solution: it is 1000 μ g/mL yttrium standard stock solutions into 100mL volumetric flask that pipette, which pipettes 10.00mL concentration, It is diluted with water to scale, is mixed;Again from 10.00mL solution is pipetted in this volumetric flask into 100mL volumetric flask, it is diluted with water to quarter Degree mixes spare;
The preparation method of 100 μ g/mL lithium standard solution: it is that 1000 μ g/mL lithium standards reserve is molten that pipette, which pipettes 10.00mL concentration, Liquid is diluted with water to scale into 100mL volumetric flask, mixes spare;
The preparation method of 100 μ g/mL potassium standard solution: it is that 1000 μ g/mL potassium standards reserve is molten that pipette, which pipettes 10.00mL concentration, Liquid is diluted with water to scale into 100mL volumetric flask, mixes spare.
CN201810820554.4A 2018-07-24 2018-07-24 The rapid assay methods of lithia, potassium oxide, sodium oxide molybdena in continuous casting covering slag Pending CN108956586A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810820554.4A CN108956586A (en) 2018-07-24 2018-07-24 The rapid assay methods of lithia, potassium oxide, sodium oxide molybdena in continuous casting covering slag

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810820554.4A CN108956586A (en) 2018-07-24 2018-07-24 The rapid assay methods of lithia, potassium oxide, sodium oxide molybdena in continuous casting covering slag

Publications (1)

Publication Number Publication Date
CN108956586A true CN108956586A (en) 2018-12-07

Family

ID=64464595

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810820554.4A Pending CN108956586A (en) 2018-07-24 2018-07-24 The rapid assay methods of lithia, potassium oxide, sodium oxide molybdena in continuous casting covering slag

Country Status (1)

Country Link
CN (1) CN108956586A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109632771A (en) * 2019-01-11 2019-04-16 包头钢铁(集团)有限责任公司 A method of measurement coal, sludge, dedusting ash, sodium oxide molybdena in covering slag
CN109900681A (en) * 2019-03-18 2019-06-18 芜湖新兴铸管有限责任公司 The method for measuring sodium oxide content in covering slag
CN110687101A (en) * 2019-09-30 2020-01-14 马鞍山钢铁股份有限公司 Method for measuring content of lithium oxide in casting powder by ICP-AES method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102590184A (en) * 2012-02-17 2012-07-18 内蒙古包钢钢联股份有限公司 Method for determining high-content potassium and sodium in iron and dust-containing mud
CN102914532A (en) * 2012-10-12 2013-02-06 中国航空工业集团公司北京航空材料研究院 Method for detecting contents of titanium, manganese, Ferrum, nickel and tungsten in tantalum contained cobalt-base alloy
CN103529016A (en) * 2013-10-12 2014-01-22 武汉钢铁(集团)公司 Rapid determination method for multiple component contents in mold flux
CN107024468A (en) * 2017-03-17 2017-08-08 唐山钢铁集团有限责任公司 The assay method of iron, aluminium, manganese, calcium, titanium, silicon, magnesium in covering slag

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102590184A (en) * 2012-02-17 2012-07-18 内蒙古包钢钢联股份有限公司 Method for determining high-content potassium and sodium in iron and dust-containing mud
CN102914532A (en) * 2012-10-12 2013-02-06 中国航空工业集团公司北京航空材料研究院 Method for detecting contents of titanium, manganese, Ferrum, nickel and tungsten in tantalum contained cobalt-base alloy
CN103529016A (en) * 2013-10-12 2014-01-22 武汉钢铁(集团)公司 Rapid determination method for multiple component contents in mold flux
CN107024468A (en) * 2017-03-17 2017-08-08 唐山钢铁集团有限责任公司 The assay method of iron, aluminium, manganese, calcium, titanium, silicon, magnesium in covering slag

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
姜亚男等: "ICP-OES法测定保护渣中铁、铝、镁的氧化物含量 ", 《河北冶金》 *
朱立光等: "电感耦合等离子体原子发射光谱法测定保护渣中氧化钾和氧化钠", 《冶金分析》 *
李丽华等: "《仪器分析(第二版)》", 31 July 2014 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109632771A (en) * 2019-01-11 2019-04-16 包头钢铁(集团)有限责任公司 A method of measurement coal, sludge, dedusting ash, sodium oxide molybdena in covering slag
CN109900681A (en) * 2019-03-18 2019-06-18 芜湖新兴铸管有限责任公司 The method for measuring sodium oxide content in covering slag
CN110687101A (en) * 2019-09-30 2020-01-14 马鞍山钢铁股份有限公司 Method for measuring content of lithium oxide in casting powder by ICP-AES method

Similar Documents

Publication Publication Date Title
CN108956586A (en) The rapid assay methods of lithia, potassium oxide, sodium oxide molybdena in continuous casting covering slag
CN108680593A (en) A kind of X-ray fluorescence spectra quickly measures primary and secondary in granite, the method for micro constitutent
CN105842266A (en) Fluorescence analysis method for determining element content in lithium iron phosphate
CN110261420A (en) The method of x-ray fluorescence spectrometry serpentine chemical component
CN105784747A (en) Method for detecting silicon dioxide, aluminum sesquioxide, calcium oxide and magnesium oxide in acetylene sludge
CN105651799A (en) X fluorescence detection method of impurity content in quartz sand
CN108414675B (en) Method for rapidly determining low-concentration boric acid in aqueous solution by using pH meter
Ritter et al. Interlaboratory test on polymers: determination of heavy metals in polymer metrices
CN117169264B (en) Method for measuring content of lithium element in lithium-boron alloy
CN108508050A (en) The method of lanthanum, cerium and barium content in x-ray fluorescence spectrometry slag
CN110220887B (en) Method for measuring lead, zinc, tin and nickel in waste circuit board stripping material resin powder
CN106338534B (en) The method of Calcium Fluoride Content in fluorite is quickly measured using Xray fluorescence spectrometer
Máriássy et al. Link to the SI via primary direct methods
CN107655916A (en) A kind of method that mineral wool acidity coefficient is determined using dispersive spectroscopy
CN106324004A (en) Industrial strontium carbonate chemical component content detection method
CN103115881A (en) Method for evaluating and reducing uncertainty value of potassium in iron ore
Cheong et al. Improved accuracy of determination of dissolved silicate in seawater using absorption spectrometry
CN112129744B (en) Chemical phase analysis method for lithium in ore
CN114563393A (en) Method for measuring content of tungsten element in niobium-tungsten alloy
CN103353453A (en) Inductively coupled plasma-atomic emission spectrometry (ICP-AES) method for testing chemical components of blue phosphors of plasma display panel (PDP)
CN106124546A (en) A kind of measure the method for potassium content in industry potassium chlorate
CN106370775B (en) Acid dissolution-titration method for detecting iron element in battery-grade ferrous oxalate product
CN106370685A (en) Method for determining content of potassium in industrial potassium chloride
CN102854178B (en) Method for measuring atomic ratio of tellurium elements to cadmium elements in cadmium telluride
CN106093097A (en) A kind of measure the method for content of strontium in fireworks and firecrackers firework medicament

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20181207

WD01 Invention patent application deemed withdrawn after publication