CN110231333A - A kind of measuring method of Impurities In Alumina element - Google Patents
A kind of measuring method of Impurities In Alumina element Download PDFInfo
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Abstract
The invention belongs to metal detection analysis technical fields, more particularly to a kind of measuring method of Impurities In Alumina element, this method mainly uses Anhydrous potassium carbonate and boric acid to melt sample, different from existing coloured professional standard YS/T630.-2007 " the measurement inductively coupled plasma atomic emission spectrometry of alumina impurity content ", the present invention melts the sample-smelting method of sample using potassium carbonate-boric acid, carry out the melting of sample, then the iron in aluminium oxide is measured with inductively coupled plasma emission spectrometry, sodium, calcium, silicon, lithium equal size, method is simple, it can be used for the measurement of Impurities In Alumina element.
Description
Technical field
The invention belongs to metal detection analysis technical fields, and in particular to a kind of measurement side of Impurities In Alumina element
Method.
Background technique
The measurement of Impurities In Alumina element used for aluminium electrolysis is formulated again in recent years in addition to traditional chemical analysis method
The method and inductive coupling plasma emission spectrum method of spectrofluorimetry, wherein inductive coupling plasma emission spectrum method, main
The method of micro-wave digestion is borrowed to carry out sample treatment, because microwave dissolver specification is different, then needs to find sample dissolution again
Condition, and Microwave Digestion, when sample size is larger, is limited to clear up because there are larger safety, while in the industrial production
Instrument counteracting tank and digestion time, efficiency are lower.The lithium content in domestic aluminium oxide is enriched in electrolysis production in recent years, enterprise
Industry increasingly payes attention to lithium content control.
Summary of the invention
For above-mentioned problems of the prior art and deficiency, the present invention provides a kind of survey of Impurities In Alumina element
Determine method.
To achieve the above object, the invention provides the following technical scheme:
A kind of measuring method of Impurities In Alumina element, this method be respectively prepare aluminum substrate standard solution, iron standard solution,
Silicon standard solution, sodium standard solution, calcium standard solution and lithium standard solution, by the aluminum substrate standard solution, iron standard solution, silicon
Series standard solution is made in standard solution, sodium standard solution, calcium standard solution and lithium standard solution, draws the series standard solution
Working curve, dissolve alumina sample, obtain the solution for dissolving in the sample, measure the sample solution, then, pass through different members
The atom of element is in excitation or ionization, the power for the characteristic spectral line launched, to measure the content of corresponding element.
The above method specifically sequentially includes the following steps:
Step 1: weighing 5.2873g rafifinal, volume ratio 1:1 nitric acid solution 400ml dissolution is added, last constant volume to 500ml holds
Measuring bottle obtains the aluminium base liquid solution of 20mg/ml；
0.864 gram of ammonium ferric sulfate is weighed, water is dissolved in, adds 10 milliliter of 25% sulfuric acid solution, is moved into 1000 milliliters of volumetric flasks, is diluted
To scale, the iron standard solution of 0.1mg/ml is obtained；
0.1000 gram of silicon is weighed, is placed in platinum crucible, 3.5000 grams of Anhydrous potassium carbonates are added, is uniformly mixed, is heated in 1000 degree
It is cooling to complete melting, it is dissolved in water, moves into 1000 milliliters of volumetric flasks, is diluted to scale, the silicon standard for obtaining 0.1mg/ml is molten
Liquid；
0.2540 gram of calcination is weighed to the sodium chloride of constant weight, water is dissolved in, moves into 1000 milliliters of volumetric flasks, be diluted to scale, obtain
The sodium standard solution of 0.1mg/ml；
0.367 gram of CALCIUM CHLORIDE DIHYDRATE is weighed, water is dissolved in, is moved into 1000 milliliters of volumetric flasks, is diluted to scale, obtains 0.1mg/ml
Calcium standard solution；
0.5323g lithium carbonate is weighed, water 150ml is added, volume ratio 1:3 nitric acid solution to lithium carbonate is slowly added to and dissolves completely, boil
Boiling removes carbon dioxide, and cooling moves back people's 1000mI volumetric flask, is diluted with water to scale, shakes up, obtain the lithium standard of 0.1mg/ml
Solution；
Step 2: weighing boric acid 0.8000g, potassium carbonate 1.5000g hexad is placed in platinum crucible, heat 5 at 850 DEG C
Minute, it takes out after cooling, adds suitable quantity of water, electric discharge hot plate is heated to boric carbonic potassium and is completely dissolved, pours into and fill 30ml volume
It than the politef beaker of 1:3 nitric acid solution, boils, is then transferred to 250ml volumetric flask, be separately added into step 1 obtained
10ml aluminium base liquid solution, then the iron standard solution of 0ml, 2.5ml, 5ml, 10ml, 15ml, 20ml obtained respectively plus in step 1,
Silicon standard solution, sodium standard solution, calcium standard solution and lithium standard solution after constant volume, move into polyvinyl chloride volumetric flask, to draw
Working curve series standard solution；
Step 3: using ICP-AES Inductively coupled plasma optical emission spectrometer, cooling gas flow 12L/min, atomization gas flow
For 0.8L/min, secondary air amount 0.75L/min, radio-frequency power 1400W, sample volume is the instrument condition of 1.5mL/min
Under series standard solution obtained in step 2 is detected, detection obtain Fe wavelength 259.93nm, sodium wavelength 589.93nm,
Silicon wavelength 253.13nm, calcium wavelength 396.847nm, lithium wavelength 670.780nm, and with series standard solution obtained in step 3
Draw standard curve；
Step 4: weighing 0.8000g boric acid, 0.2000g alumina sample and 1.5000g potassium carbonate respectively and be placed in platinum crucible
Stir evenly, heating platinum crucible simultaneously dissolves boric acid, aluminium oxide and potassium carbonate, be added into platinum crucible a small amount of boiling boil so that
Sample after melting dissolves to form sample solution, and sample solution is poured into and fills 25ml volume ratio as poly- the four of 1:3 nitric acid solution
Vinyl chloride beaker, and solution will be washed after washing platinum crucible with the nitric acid solution that 5ml volume ratio is 1:3 and be added to poly- four chloroethene
Alkene beaker, and boiled into politef beaker plus after 100ml water, solution in politef beaker is moved into after cooling
Plastics volumetric flask is moved into after 250ml volumetric flask constant volume, is solution to be measured, and using atomic absorption instrument, reagent blank is reference, measurement
The power of the characteristic spectral line of solution to be measured, to measure the content of corresponding element.
Compared with prior art, the beneficial effects of the present invention are:
The present invention adds the sampler-dissolving method of boric acid using potassium carbonate, the complete melting of sample is realized, using inductively coupled plasma
Emission spectrometry, which realizes while measuring the impurity contents such as the iron in alumina sample, sodium, silicon, calcium, lithium, carries out Accurate Determining
Method meets reliability and accuracy that Impurities In Alumina elemental iron, sodium, silicon, calcium, lithium measure.
Detailed description of the invention
Fig. 1 is the iron working curve diagram for the series standard solution drawn in the embodiment of the present invention；
Fig. 2 is the sodium working curve diagram for the series standard solution drawn in the embodiment of the present invention；
Fig. 3 is the silicon working curve diagram for the series standard solution drawn in the embodiment of the present invention；
Fig. 4 is the calcium working curve diagram for the series standard solution drawn in the embodiment of the present invention；
Fig. 5 is the lithium working curve diagram for the series standard solution drawn in the embodiment of the present invention.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
The present invention adds the sampler-dissolving method of boric acid using potassium carbonate, the complete melting of sample is realized, using inductive coupling etc.
Ion emission spectroscopy method realizes while measuring the iron in alumina sample, sodium, silicon, calcium, lithium impurity content and carries out accurately
Method for measuring meets reliability and accuracy that Impurities In Alumina elemental iron, sodium, silicon, calcium, lithium measure, this method tool
Body sequentially includes the following steps:
Step 1: weighing 5.2873g rafifinal, volume ratio 1:1 nitric acid solution 400ml dissolution is added, last constant volume to 500ml holds
Measuring bottle obtains the aluminium base liquid solution of 20mg/ml；
0.864 gram of ammonium ferric sulfate is weighed, water is dissolved in, adds 10 milliliter of 25% sulfuric acid solution, is moved into 1000 milliliters of volumetric flasks, is diluted
To scale, the iron standard solution of 0.1mg/ml is obtained；
0.1000 gram of silicon is weighed, is placed in platinum crucible, 3.5000 grams of Anhydrous potassium carbonates are added, is uniformly mixed, is heated in 1000 degree
It is cooling to complete melting, it is dissolved in water, moves into 1000 milliliters of volumetric flasks, is diluted to scale, the silicon standard for obtaining 0.1mg/ml is molten
Liquid；
0.2540 gram of calcination is weighed to the sodium chloride of constant weight, water is dissolved in, moves into 1000 milliliters of volumetric flasks, be diluted to scale, obtain
The sodium standard solution of 0.1mg/ml；
0.367 gram of CALCIUM CHLORIDE DIHYDRATE is weighed, water is dissolved in, is moved into 1000 milliliters of volumetric flasks, is diluted to scale, obtains 0.1mg/ml
Calcium standard solution；
0.5323g lithium carbonate is weighed, water 150ml is added, volume ratio 1:3 nitric acid solution to lithium carbonate is slowly added to and dissolves completely, boil
Boiling removes carbon dioxide, and cooling moves back people's 1000mI volumetric flask, is diluted with water to scale, shakes up, obtain the lithium standard of 0.1mg/ml
Solution；
Step 2: weighing boric acid 0.8000g, potassium carbonate 1.5000g hexad is placed in platinum crucible, heat 5 at 850 DEG C
Minute, it takes out after cooling, adds suitable quantity of water, electric discharge hot plate is heated to boric carbonic potassium and is completely dissolved, pours into and fill 30ml volume
It than the politef beaker of 1:3 nitric acid solution, boils, is then transferred to 250ml volumetric flask, be separately added into step 1 obtained
10ml aluminium base liquid solution, then the iron standard solution of 0ml, 2.5ml, 5ml, 10ml, 15ml, 20ml obtained respectively plus in step 1,
Silicon standard solution, sodium standard solution, calcium standard solution and lithium standard solution after constant volume, move into polyvinyl chloride volumetric flask, to draw
Working curve series standard solution；
Step 3: using ICP-AES Inductively coupled plasma optical emission spectrometer, cooling gas flow 12L/min, atomization gas flow
For 0.8L/min, secondary air amount 0.75L/min, radio-frequency power 1400W, sample volume is the best instrument item of 1.5mL/min
Solution is detected under part, wherein Fe wavelength (259.93nm), sodium (589.93nm) silicon (253.13nm), calcium
Serial standard liquid in (396.847nm), lithium (670.780nm) determination step 2, draws analysis curve, and curvilinear regression coefficient is big
In 0.996 or more；
Step 4: weighing 0.8000g boric acid, 0.2000g alumina sample and 1.5000g potassium carbonate respectively and be placed in platinum crucible
Stir evenly, heating platinum crucible simultaneously dissolves boric acid, aluminium oxide and potassium carbonate, be added into platinum crucible a small amount of boiling boil so that
Sample after melting dissolves to form sample solution, and sample solution is poured into and fills 25ml volume ratio as poly- the four of 1:3 nitric acid solution
Vinyl chloride beaker, and solution will be washed after washing platinum crucible with the nitric acid solution that 5ml volume ratio is 1:3 and be added to poly- four chloroethene
Alkene beaker, and boiled into politef beaker plus after 100ml water, solution in politef beaker is moved into after cooling
Plastics volumetric flask is moved into after 250ml volumetric flask constant volume, is solution to be measured, and using atomic absorption instrument, reagent blank is reference, measurement
The power of the characteristic spectral line of solution to be measured, to measure the content of corresponding element.
Actual verification is carried out with regard to analysis method Instrumental operating condition, various reagents and dosage of the present invention etc. below:
1) instrument operating condition is tested
Fe259.941, Na589.592, Si252.411 is selected to reconcile plasma power 1000w, 1200w, 1400w, 1600w etc.
Its intensity is surveyed, while adjusting nebulizer flow, revolution speed, it is final to determine complete general direct-reading plasma emission spectrometer (Spetro
Arcos) the plasma power 1.4KW of instrument, revolution speed 30RPM, cooling gas flow 12l/min, 0.80 l/ of secondary air amount
Min, 0.75 l/min of nebulizer flow.
2) determination of dissolving condition of sample, flux amount
600 DEG C, 850 DEG C, 1000 DEG C have been carried out respectively and has carried out molten sample, and molten sample test effect comparison see the table below 1.
Table 1 melts sample test effect contrast table
By test, determine that molten sample temperature at 850 DEG C, melts 30 minutes sample time, is determined as most preferably melting the sample time.
With 0.3g sample, molten sample measure numerical evaluation as a result, molten sample time 30min, to determine amount of reagent, when measurement
Amount of reagent is shown in Table 2.
Amount of reagent when table 2 measures
1.5g potassium carbonate is finally determined by many experiments and 0.8g boric acid is best flux amount, while example weight determines
In 0.2-0.3g.
3) selection of elemental analysis line
In addition to selecting each 1 grade of wavelength line of analytical element, each element has selected multiple wavelength lines, by 1.5 grams of potassium carbonate, 0.8 gram of boron
Acid melts sample, is measured, and then therefrom the spectral line of regression coefficient > 0.996 or more is selected to be adjusted, final to determine
Aluminium oxide analysis optimal wavelength be respectively as follows: Fe:259.941nm, Si:251.612nm, Na:589.592nm, Ca:396.847nm,
Li:670.780nm is optimized analysis spectral line.
4) sour selection
In ICP emission spectrographic analysis, due to the change of solution viscosity, surface tension and density can cause solution sample rate,
The variation of the factors such as nebulization efficiency, solution elevating amount, so as to cause the variation of the intensity of spectral line, as physical disturbance.General sulfuric acid
It is the acid that plasma atomic emission spectroscopy is not used with phosphoric acid, because the viscosity of sulfuric acid and phosphoric acid is too big, causes sample introduction molten
Liquid mist low efficiency.Hydrochloric acid, nitric acid and its nitration mixture are the common acids that plasma atomic emission spectroscopy carries out sample pretreatment, therefore
In test we carry out the acidification of sample with nitric acid.It is final to determine that addition 25ml volume ratio 1:3 nitric acid is molten and through testing
Liquid.
5) it the determination of final sample melting method: is determined through many experiments: accurately weighing 0.8000g boric acid and platinum earthenware is added
Crucible, then weighs 0.2000g alumina sample, finally weighs 1.5000g potassium carbonate and is stirred and evenly mixed with stirring silk, is closed the lid,
It is placed in Muffle furnace, is melted 30 minutes at 850 DEG C, after taking out cooling, a small amount of boiling boiling is added in platinum crucible, it is molten to sample
Solution, is poured into the politef beaker for filling the 250ml of 25ml volume ratio 1:3 nitric acid solution by Xie Hou, and with 5ml volume ratio
The nitric acid solution of 1:3 washs crucible, is being washed with water later, 100ml water is finally added into politef beaker, in electric hot plate
On boil, after cooling, move into 250ml volumetric flask constant volume, move into plastics volumetric flask, be solution to be measured.
6) precision test
Randomly select iron in measurement aluminium oxide standard specimen, silicon, sodium, calcium, lithium basic, normal, high value carry out precision test.In method
Defined content range, same instrument in batches measure 8 low middle quasi- samples 11 times, and precision the results are shown in Table 3.
The comparison of 3 Precision Experiment effect data of table
The accuracy of the method for the present invention and precision are high, and method is reliable, iron, sodium silicon, calcium, lithium etc. in energy Accurate Determining aluminium oxide
Element.
Embodiment
5.2873g rafifinal is weighed, volume ratio 1:1 nitric acid solution 400ml dissolution, last constant volume to 500ml capacity is added
Bottle, obtains the aluminium base liquid solution of 20mg/ml；
0.864 gram of ammonium ferric sulfate is weighed, water is dissolved in, adds 10 milliliter of 25% sulfuric acid solution, is moved into 1000 milliliters of volumetric flasks, is diluted
To scale, the iron standard solution of 0.1mg/ml is obtained；
0.1000 gram of silicon is weighed, is placed in platinum crucible, 3.5000 grams of Anhydrous potassium carbonates are added, is uniformly mixed, is heated in 1000 degree
It is cooling to complete melting, it is dissolved in water, moves into 1000 milliliters of volumetric flasks, is diluted to scale, the silicon standard for obtaining 0.1mg/ml is molten
Liquid；
0.2540 gram of calcination is weighed to the sodium chloride of constant weight, water is dissolved in, moves into 1000 milliliters of volumetric flasks, be diluted to scale, obtain
The sodium standard solution of 0.1mg/ml；
0.367 gram of CALCIUM CHLORIDE DIHYDRATE is weighed, water is dissolved in, is moved into 1000 milliliters of volumetric flasks, is diluted to scale, obtains 0.1mg/ml
Calcium standard solution；
0.5323g lithium carbonate is weighed, water 150ml is added, volume ratio 1:3 nitric acid solution to lithium carbonate is slowly added to and dissolves completely, boil
Boiling removes carbon dioxide, and cooling moves back people's 1000mI volumetric flask, is diluted with water to scale, shakes up, obtain the lithium standard of 0.1mg/ml
Solution；
Weigh boric acid 0.8000g, potassium carbonate 1.5000g hexad is placed in platinum crucible, heat 5 minutes, take at 850 DEG C
Out after cooling, add suitable quantity of water, electric discharge hot plate is heated to boric carbonic potassium and is completely dissolved, pours into and fill 30ml volume ratio 1:3 nitre
The politef beaker of acid solution, boils, and is then transferred to 250ml volumetric flask, is separately added into 10ml aluminium base obtained in step 1
Liquid solution, then the iron standard solution of 0ml, 2.5ml, 5ml, 10ml, 15ml, 20ml obtained, silicon standard are molten respectively plus in step 1
Liquid, sodium standard solution, calcium standard solution and lithium standard solution after constant volume, move into polyvinyl chloride volumetric flask, to draw working curve
With series standard solution；
Using ICP-AES Inductively coupled plasma optical emission spectrometer, cooling gas flow 12L/min, atomization gas flow is 0.8L/
Min, secondary air amount 0.75L/min, radio-frequency power 1400W, sample volume be 1.5mL/min instrument condition under to step
Series standard solution obtained is detected in 2, and detection obtains Fe wavelength 259.93nm, sodium wavelength 589.93nm, silicon wavelength
253.13nm, calcium wavelength 396.847nm, lithium wavelength 670.780nm, drawing as shown in figure 1-5 this using existing method is
The working curve of column standard solution.
0.8000g boric acid, 0.2000g alumina sample and 1.5000g potassium carbonate is weighed respectively to be placed in platinum crucible and stir
It mixes uniformly, heat platinum crucible and dissolves boric acid, aluminium oxide and potassium carbonate, a small amount of boiling is added into platinum crucible and boils so that molten
Sample after melting dissolves to form sample solution, and sample solution is poured into the poly- tetrachloro for filling that 25ml volume ratio is 1:3 nitric acid solution
Ethylene beaker, and solution will be washed after washing platinum crucible with the nitric acid solution that 5ml volume ratio is 1:3 and be added to politef
Beaker, and boiled into politef beaker plus after 100ml water, solution in politef beaker is moved into after cooling
Plastics volumetric flask is moved into after 250ml volumetric flask constant volume, is solution to be measured, using ICP-AES inductive coupling plasma emission spectrum
Instrument, reagent blank are reference, measure the power of the characteristic spectral line of solution to be measured, to measure the content of corresponding element.
Claims (2)
1. a kind of measuring method of Impurities In Alumina element, which is characterized in that prepare aluminum substrate standard solution, iron standard respectively
Solution, silicon standard solution, sodium standard solution, calcium standard solution and lithium standard solution, the aluminum substrate standard solution, iron standard is molten
Series standard solution is made in liquid, silicon standard solution, sodium standard solution, calcium standard solution and lithium standard solution, draws series mark
The working curve of quasi- solution dissolves alumina sample, obtains the solution for dissolving in the sample, measure the sample solution, then, pass through
The atom of different elements is in excitation or ionization, the power for the characteristic spectral line launched, to measure the content of corresponding element.
2. a kind of measuring method of Impurities In Alumina element as described in claim 1, which is characterized in that the measuring method
It carries out as steps described below:
Step 1: weighing 5.2873g rafifinal, volume ratio 1:1 nitric acid solution 400ml dissolution is added, last constant volume to 500ml holds
Measuring bottle obtains the aluminium base liquid solution of 20mg/ml；
0.864 gram of ammonium ferric sulfate is weighed, water is dissolved in, adds 10 milliliter of 25% sulfuric acid solution, is moved into 1000 milliliters of volumetric flasks, is diluted
To scale, the iron standard solution of 0.1mg/ml is obtained；
0.1000 gram of silicon is weighed, is placed in platinum crucible, 3.5000 grams of Anhydrous potassium carbonates are added, is uniformly mixed, is heated in 1000 degree
It is cooling to complete melting, it is dissolved in water, moves into 1000 milliliters of volumetric flasks, is diluted to scale, the silicon standard for obtaining 0.1mg/ml is molten
Liquid；
0.2540 gram of calcination is weighed to the sodium chloride of constant weight, water is dissolved in, moves into 1000 milliliters of volumetric flasks, be diluted to scale, obtain
The sodium standard solution of 0.1mg/ml；
0.367 gram of CALCIUM CHLORIDE DIHYDRATE is weighed, water is dissolved in, is moved into 1000 milliliters of volumetric flasks, is diluted to scale, obtains 0.1mg/ml
Calcium standard solution；
0.5323g lithium carbonate is weighed, water 150ml is added, volume ratio 1:3 nitric acid solution to lithium carbonate is slowly added to and dissolves completely, boil
Boiling removes carbon dioxide, and cooling moves back people's 1000mI volumetric flask, is diluted with water to scale, shakes up, obtain the lithium standard of 0.1mg/ml
Solution；
Step 2: weighing boric acid 0.8000g, potassium carbonate 1.5000g hexad is placed in platinum crucible, heat 5 at 850 DEG C
Minute, it takes out after cooling, adds suitable quantity of water, electric discharge hot plate is heated to boric carbonic potassium and is completely dissolved, pours into and fill 30ml volume
It than the politef beaker of 1:3 nitric acid solution, boils, is then transferred to 250ml volumetric flask, be separately added into step 1 obtained
10ml aluminium base liquid solution, then the iron standard solution of 0ml, 2.5ml, 5ml, 10ml, 15ml, 20ml obtained respectively plus in step 1,
Silicon standard solution, sodium standard solution, calcium standard solution and lithium standard solution after constant volume, move into polyvinyl chloride volumetric flask, to draw
Working curve series standard solution；
Step 3: using ICP-AES Inductively coupled plasma optical emission spectrometer, cooling gas flow 12L/min, atomization gas flow
For 0.8L/min, secondary air amount 0.75L/min, radio-frequency power 1400W, sample volume is the instrument condition of 1.5mL/min
Under series standard solution obtained in step 2 is detected, detection obtain Fe wavelength 259.93nm, sodium wavelength 589.93nm,
Silicon wavelength 253.13nm, calcium wavelength 396.847nm, lithium wavelength 670.780nm, and with series standard solution obtained in step 3
Draw standard curve；
Step 4: weighing 0.8000g boric acid, 0.2000g alumina sample and 1.5000g potassium carbonate respectively and be placed in platinum crucible
Stir evenly, heating platinum crucible simultaneously dissolves boric acid, aluminium oxide and potassium carbonate, be added into platinum crucible a small amount of boiling boil so that
Sample after melting dissolves to form sample solution, and sample solution is poured into and fills 25ml volume ratio as poly- the four of 1:3 nitric acid solution
Vinyl chloride beaker, and solution will be washed after washing platinum crucible with the nitric acid solution that 5ml volume ratio is 1:3 and be added to poly- four chloroethene
Alkene beaker, and boiled into politef beaker plus after 100ml water, solution in politef beaker is moved into after cooling
Plastics volumetric flask is moved into after 250ml volumetric flask constant volume, is solution to be measured, and using atomic absorption instrument, reagent blank is reference, measurement
The power of the characteristic spectral line of solution to be measured, to measure the content of corresponding element.
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