CN104535708A - Method for determination of total aluminum in aluminum-based composite slag forming agent - Google Patents
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Abstract
The invention discloses a method for determination of total aluminum in an aluminum-based composite slag forming agent. The method comprises the steps: melting a mixture of the aluminum-based composite slag forming agent, sodium carbonate, sodium peroxide and sodium hydroxide to obtain a molten mixture; heating and boiling an extract liquid obtained after extracting the molten mixture with boiling water, then diluting, metering volume, filtering, and separating the liquid to obtain a to-be-measured solution; adding an EDTA standard solution into the to-be-measured solution; titrating the to-be-measured solution with a copper sulfate standard solution, and indicating a titration end point by using a PAN indicator; titrating a blank sample with the copper sulfate standard solution, and indicating a titration end point by using the PAN indicator; and according to the titration volumes of the copper sulfate standard solution, adopting an equation described in the specification to obtain the mass percentage content of the total aluminum in the aluminum-based composite slag forming agent.
Description
Technical field
The present invention relates to metallurgical analysis field, specifically, relate to a kind of full Al-single crystal method in aluminum-base composite slag former.
Background technology
Aluminum-base composite slag former is mainly used in the efficient CSP CSP continuous casting LF stove short period and produces in smelting process, can meet Q345 Q235 the need of production of the steel grade such as SS400.It can not only rapid slagging, deoxidation desulfuration, shortens smelting cycle, reduces departures oxygen position, can also reduce the consumption such as aluminum steel, ferrosilicon, reduce power consumption, reduce ton steel cost.Aluminum-base composite slag former is primarily of compositions such as aluminium and oxide, calcium oxide, magnesium oxide, silicon dioxide.Wherein, the exact level of aluminium plays very important effect.At present, in aluminum-base composite slag former, the analysis of full aluminium there is no method.In addition, in prior art, dissolve not exclusively when taking acid-soluble method to dissolve aluminium base composite fluxing medium sample, easily wear filter solute effect during acid dissolve aftertreatment residue also undesirable.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of full Al-single crystal method in aluminum-base composite slag former, has good preci-sion and accuracy.
Technical scheme of the present invention is as follows:
In a kind of aluminum-base composite slag former, full Al-single crystal method, is characterized in that, comprising: the potpourri melting of aluminum-base composite slag former, sodium carbonate, sodium peroxide and NaOH is obtained molten mixture; Extract heating after described molten mixture extracting in boiling water boiled, then dilution, constant volume, filtration, obtains solution to be measured after separatory; EDTA standard solution is added in described solution to be measured; With solution to be measured described in the titration of copper sulphate standard solution, adopt PAN indicator instruction titration end-point; With the blank sample of copper sulphate standard solution titration, adopt PAN indicator instruction titration end-point; According to the volume of the described copper sulphate standard solution of titration, adopt
obtain the mass percentage of full aluminium in aluminum-base composite slag former, wherein V
0represent be blank sample described in titration time the volume of described copper sulphate standard solution that consumes, the volume of the described copper sulphate standard solution that what V represented consume when being solution to be measured described in titration, what T represented is described copper sulphate standard solution to the titer of aluminium, the quality of what m represented the is described aluminum-base composite slag former that described solution to be measured is corresponding.
Further: the process of solution to be measured described in the titration of described copper sulphate standard solution is carry out under the condition of 4.5 in pH value.
Further, described pH value be the condition of 4.5 by following process implementation: in the solution described to be measured adding described EDTA standard solution, add Congored test paper; Hydrochloric acid is added until described Congored test paper becomes blueness in described solution to be measured; In described solution to be measured, add acetic acid-ammonium acetate buffer solution and boil.
Further, described in the titration of described copper sulphate standard solution, the process of solution to be measured comprises: in the solution described to be measured after boiling, add described PAN indicator; Become purple with solution to be measured to described solution to be measured described in described copper sulphate standard solution first time titration, the volume of the described copper sulphate standard solution of consumption does not remember reading; In described solution to be measured, add sodium fluoride solid, after boiling, add described PAN indicator; Purple is become, the volume V of the described copper sulphate standard solution that record second time consumes with solution to be measured to described solution to be measured described in the titration of described copper sulphate standard solution second time.
Further: the quality of described aluminum-base composite slag former is 0.1500 ~ 0.2000g, the quality of described sodium carbonate is 1 ~ 2g, and the quality of described sodium peroxide is 2g, and the quality of described NaOH is 8g, the temperature of described melting is 680 ~ 700 DEG C, and the time of described melting is 10 ~ 15min.
Further: described aluminum-base composite slag former and the ratio of described boiling water extracted are 1.5-2.5g/L, the ratio of the described extract after described aluminum-base composite slag former and constant volume is 0.8g/L.
Further: the concentration of described EDTA standard solution is 0.017 ~ 0.019mol/L.
Further: described hydrochloric acid is the volume ratio of HCl and water is the hydrochloric acid of 1:1; The volume ratio of described acetic acid-ammonium acetate buffer solution and described solution to be measured is 1:1.
Further: the concentration of described copper sulphate standard solution is 0.017 ~ 0.019mol/L, the concentration of described PAN indicator is 1%.
Further: after boiling described acetic acid-ammonium acetate buffer solution, to add described PAN indicator 8 ~ 10; The ratio of described sodium fluoride and described solution to be measured is 40 ~ 60g/L, adds described PAN indicator 3 ~ 5 after boiling described sodium fluoride.
Technique effect of the present invention is as follows:
In aluminum-base composite slag former of the present invention, full Al-single crystal method adopts the content of aluminium in highly basic melting sample, EDTA volumetric determination aluminum-base composite slag former, has good precision, accuracy, can meet modern production and scientific research needs completely.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is described in further detail.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
In aluminum-base composite slag former of the present invention, the step of full Al-single crystal method is as follows:
Step S1: the potpourri melting of aluminum-base composite slag former, sodium carbonate, sodium peroxide and NaOH is obtained molten mixture.
Particularly, the quality of aluminum-base composite slag former is 0.1500 ~ 0.2000g, and the quality of sodium carbonate is 1 ~ 2g, and the quality of sodium peroxide is 2g, and the quality of NaOH is 8g.The temperature of melting is 680 ~ 700 DEG C, and the time of melting is 10 ~ 15min.Reactant can be placed in crucible by step S1 to carry out at muffle furnace, and certain the application, not as limit, also can adopt other suitable device.
The object of step S1 be with sodium carbonate, sodium peroxide and highly basic NaOH by the aluminium melting in aluminum-base composite slag former and with the element sepatation such as iron, manganese, titanium, calcium and magnesium.
Step S2: the extract heating after molten mixture extracting in boiling water is boiled, then obtains solution to be measured after dilution, constant volume, filtration, separatory.
Particularly, aluminum-base composite slag former and the ratio of boiling water extracted are 1.5-2.5g/L, are preferably 2g/L, and the ratio of the extract after aluminum-base composite slag former and constant volume is 0.8g/L.The process of step S2 extracting in boiling water can be carried out in beaker, and certain the application, not as limit, also can adopt other suitable device.The step of step S2 constant volume is preferably carried out in volumetric flask, and certain the application, not as limit, also can adopt other suitable device.
The object of step S2 is extracted by aluminium in solution so that follow-up titrimetry.
Step S3: add EDTA standard solution in solution to be measured.
Particularly, the concentration of EDTA standard solution is 0.017 ~ 0.019mol/L, is preferably 0.018mol/L.The addition of EDTA is determined according to the content of aluminium in solution to be measured.
The object of step S3 is by adding excessive EDTA in solution to be measured, makes it the aluminium coordination completely and in solution to be measured.
Step S4: with copper sulphate standard solution titration solution to be measured, adopts PAN indicator instruction titration end-point.
Particularly, step S4 carries out under the condition of 4.5.Wherein, pH value be the condition of 4.5 by following process implementation:
Step S41: add Congored test paper in the solution to be measured adding EDTA standard solution.
Particularly, this Congored test paper is one piece.
Step S42: add hydrochloric acid until Congored test paper becomes blueness in solution to be measured.
Particularly, hydrochloric acid is the volume ratio of HCl and water is the hydrochloric acid of 1:1.During by hydrochloric acid adjustment acidity, as solutions turbid, show that EDTA standard solution addition is not enough, alkalescence can be adjusted to again and add appropriate EDTA standard solution.
Step S43: add acetic acid-ammonium acetate buffer solution and boil in solution to be measured.
Particularly, the volume ratio of acetic acid-ammonium acetate buffer solution and solution to be measured is 1:1.Maintaining liquid volume in the process of boiling is 100 ~ 150mL.The time of boiling suitably can adjust according to liquid volume consumption degree, and for making sodium fluoride and aluminium complexing completely, the time of boiling after adding acetic acid-ammonium acetate buffer solution is generally not less than 3min.Preferably the collocation method of this acetic acid-ammonium acetate buffer solution is: after water-soluble for 77g ammonium acetate, add 80mL acetic acid, be diluted to scale, shake up in 1000mL volumetric flask.The pH=4.5 of this acetic acid-ammonium acetate buffer solution.
Particularly, the process of step S4 specifically comprises following step:
Step S44: add PAN indicator in the solution to be measured after boiling.
Step S45: become purple with copper sulphate standard solution first time titration solution to be measured to solution to be measured, do not remember the volume consuming copper sulphate standard solution in this step.
Step S46: add sodium fluoride solid in solution to be measured, add PAN indicator after boiling.
Step S47: become purple to solution to be measured with copper sulphate standard solution second time titration solution to be measured, the volume V of the copper sulphate standard solution that record second time consumes.
Wherein, the object of step S44 and S45 take PAN as indicator, with the EDTA that copper sulphate standard solution residual titration is excessive.The object of step S46 is the EDTA adding sodium fluoride release and aluminium coordination.The object of step S47 is with the titration of copper sulphate standard solution, according to standard solution consumption, calculates the mass percent of full aluminium.
Particularly, the concentration of this copper sulphate standard solution is 0.017 ~ 0.019mol/L, and be preferably 0.018mol/L, the concentration of this PAN indicator is 1% (namely the PAN of 0.1g is dissolved in the absolute ethyl alcohol of 100ml).PAN indicator 8 is added in step S44.In step S46, the ratio of sodium fluoride and solution to be measured is 40 ~ 60g/L.Maintaining liquid volume in the process of boiling is 100 ~ 150mL.The time of boiling suitably can adjust according to liquid volume consumption degree, and the time of boiling in step S46 is generally no less than 3min.Add PAN indicator 3 ~ 5, be preferably 3.
Step S5: according to the volume of the copper sulphate standard solution of titration, adopts
obtain the mass percentage of full aluminium in aluminum-base composite slag former, wherein V
0represent be titration blank sample time the volume of copper sulphate standard solution that consumes, the volume of the copper sulphate standard solution consumed during titration that what V represented is solution to be measured, what T represented is the titer of copper sulphate standard solution to aluminium, the quality of what m represented the is described aluminum-base composite slag former that solution to be measured is corresponding.Wherein, blank sample is from aluminum-base composite slag former sample melting step to titrimetry synchronous operation.
The present invention, by the complete molten aluminum matrix composite fluxing medium of highly basic melting sample, by the aluminium in EDTA volumetric determination aluminum-base composite slag former, has good accuracy.
This method is further illustrated below by experiments such as sample decomposition method, sample melted temperature, sample melted time, co-existing element interference.
1, the Selection experiment of aluminum-base composite slag former method is decomposed
Take aluminum-base composite slag former sample 0.2000g tetra-parts, adopt following four kinds of methods to carry out dissolving or melting experiment respectively:
Method one: add 10mL hydrochloric acid (volume ratio of HCl and water is 1:1), several H
2o
2, be heated to H
2o
2decompose completely, filter and carry out residue treatment.
Method two: add 10mL hydrochloric acid (volume ratio of HCl and water is 1:1), 3mLHNO
3dissolved samples, 3mLHClO
4smolder dry to the greatest extent, add hydrochloric acid (volume ratio of HCl and water is 1:1) dissolved salts, filter and carry out residue treatment.
Method three: add 20mLNaOH (mass concentration 20%) dissolved samples.
Method four: add 1gNa
2cO
3, 2gNa
2o
2, 8gNaOH melting 680 DEG C ~ 700 DEG C time.
The result that above-mentioned four kinds of methods decompose aluminium base slag former is as shown in table 1.
Table 1 four kinds of methods decompose the result of aluminium base slag former
As can be known from the results of Table 1, to decompose the effect of aluminium base slag former best for employing method four (i.e. method of the present invention).
2, the test of the temperature of molten aluminum matrix slag former
Take aluminum-base composite slag former sample 0.2000g, carry out the test of sample melt temperature by method of the present invention, result is as shown in table 2.
Table 2 melt temperature test findings
As can be known from the results of Table 2, the decomposition of melt temperature to aluminum-base composite slag former has a certain impact, 680 DEG C ~ 700 DEG C time, sample decomposing state is good, determination data accurately and reliably.
3, the test of melting time
Take aluminum-base composite slag former sample 0.2000g, carry out the test of sample melting time by method of the present invention, result is as shown in table 3.
Table 3 melting time test findings
As shown in Table 3, the decomposition of melting time to aluminum-base composite slag former has a certain impact, and when 10min ~ 15min, sample melts in good condition, determination data accurately and reliably.
4, co-existing element interference test
Take rafifinal (99.99%) 0.1000g two parts, be placed in 1, No. 2 crucible respectively, wherein, in No. 1 crucible, be added with MgO (10wt%), CaO (5wt%), SiO
2(3wt%), Na is not added
2cO
3; MgO (10wt%), CaO (5wt%), SiO is added with in No. 2 crucibles
2(3wt%), 1gNa is added
2cO
3; Carry out sample control test by method of the present invention, result is as shown in table 4.
Table 4 co-existing element interference test findings
As can be known from the results of Table 4, Na is added during melting sample
2cO
3the interference of coexistence elements to measurement result can be eliminated.
5, the precision test of method of the present invention
Adopt aluminum-base composite slag former sample, carry out Precision Experiment (n=9) result by method of the present invention as shown in table 5.
The Precision test result of table 5 method of the present invention
Measure precision result as can be seen from table 5, the relative standard deviation (RSD, relative standard deviation) of method of the present invention is all less than 5%, and therefore method of the present invention has good precision.
6, the accuracy test of method of the present invention
Accurately take 0.1000g aluminum-base composite slag former sample specimens two parts, add benchmark alundum (Al2O3) 0.0500g, 0.0800g respectively, by method test of the present invention, carry out determination of recovery rates, result is as shown in table 6.
The accuracy test of table 6 method of the present invention
As can be seen from the test findings of table 6, method of the present invention has the higher recovery, can ensure the accuracy of testing result.
7, the content range that method of the present invention is suitable for measuring is tested
In aluminum-base composite slag former sample, add aluminium mark liquid (1.0mg/mL), carry out the lower limit experiment of the content of Al mensuration by method of the present invention; In aluminum-base composite slag former sample, add benchmark alundum (Al2O3), carry out the upper limit experiment of the content of Al mensuration by method of the present invention, result is as shown in table 7.
Table 7 method of the present invention is suitable for the content range experiment measured
From the results shown in Table 7, method of the present invention can measure the aluminium content of in aluminum-base composite slag former 20% ~ 60%.
With a specific embodiment, method of the present invention is described further below.
In aluminium base slag former sample in this embodiment, the mass percentage of full aluminium is 18.52%, get two parts of samples, add the benchmark alundum (Al2O3) that aluminium content is respectively 26.46%, 42.34% respectively, after mark-on, aluminium content is equivalent to 44.98%, 60.86% respectively.Idiographic flow is as follows:
Take the aluminium base slag former sample (being accurate to 0.0001g) of 0.2000g and be placed in nickel crucible, add 1g sodium carbonate and sample mixes, then, cover 2g sodium peroxide successively above, 8g NaOH, melting 10 ~ 15min in the muffle furnace of 680 ~ 700 DEG C, takes out cooling.Crucible outer wall filter paper puts into 300mL beaker after cleaning, and adds 100mL extracting in boiling water, cleans crucible, obtains extract.Extract heating is boiled, cooled, moves in 250mL volumetric flask, be diluted to scale, shake up, obtain solution to be measured.
After above-mentioned solution to be measured is filtered, point getting 50.00mL solution to be measured is placed in 500mL triangular flask, add the EDTA standard solution 50mL that concentration is 0.018mol/L, add Congored test paper one piece, be adjusted to test paper with the hydrochloric acid that the volume ratio of HCl and water is 1:1 and become blueness (now the pH of system is 4.5).During by hydrochloric acid adjustment acidity, as solutions turbid to be measured, show that EDTA standard solution addition is not enough, alkalescence can be adjusted to again and add appropriate EDTA standard solution.Then add 50mL acetic acid-ammonium acetate buffer solution, boil 3min, take off, add the PAN indicator that 8 concentration are 1%, be titrated to solution to be measured with the copper sulphate standard solution that concentration is 0.018mol/L and become purple (this process does not remember reading).Add 2 ~ 3g sodium fluoride solid, 3min is boiled in heating, adds the PAN indicator 3 that concentration is 1%, is titrated to solution to be measured becomes purple with the standard solution that concentration is 0.018mol/L, the copper sulphate standard solution volume that record consumes.
Adopt
obtain the mass percentage of full aluminium in aluminum-base composite slag former.
Wherein, W (Al) %---the massfraction of aluminium, %;
V---the volume of the copper sulphate standard solution consumed during titration solution to be measured, mL;
V
0---the volume of the copper sulphate standard solution consumed during titration blank sample, mL;
T---copper sulphate standard solution to the titer of aluminium, g/mL;
The quality of m---the aluminum-base composite slag former that solution to be measured is corresponding, g.
Wherein, the method for the blank sample of titration is identical with the method for titration of the present invention solution to be measured.
Wherein, concentration is that the titer of the copper sulphate standard solution of 0.018mol/L is adopted and obtained with the following method:
Source according to this aluminium base slag former sample is seen, the roughly content of aluminium can be pre-determined, therefore, the fine aluminium (99.99%) two part close with the percentage composition of aluminium in aluminium base slag former sample can be taken, with the synchronous operation of aluminium base slag former sample, the volume of two parts of solution consumption copper sulphate standard solution is averaged.The titer of copper sulphate standard solution to aluminium is calculated as follows:
Wherein, in formula: T---copper sulphate standard solution to the titer of aluminium, g/mL;
M---the quality of fine aluminium (99.99%) to be measured, g;
V
1---the mean value of the copper sulphate standard solution volume that titration fine aluminium test solution consumes, mL;
V
0---consume the volume of copper sulphate standard solution when titration is blank.
Through the mensuration of method of the present invention, show that aluminium content is respectively 44.89%, 60.76%, the recovery is respectively 99.66%, 99.76%, illustrates that the method has good accuracy.Measure two aluminium base slag former samples respectively, the RSD value obtaining two groups of experimental datas is respectively 0.197%, 0.249%, is all less than 5%, illustrates that the method has good precision.
In sum, full Al-single crystal method in aluminum-base composite slag former of the present invention, adopt sodium carbonate, sodium peroxide and highly basic NaOH molten aluminum matrix composite fluxing medium by aluminium and Separation of interferential elements, add excessive EDTA, make EDTA completely with aluminium coordination, to return droplet with copper sulphate standard solution, obtain the content of full aluminium, for steel-making Composition Control process provides accurate data, modern production and scientific research needs can be met.This invention simplifies the operation steps of molten sample, Separation of interferential elements, improve detection efficiency.Aluminum-base composite slag former is applied very extensive in smelting process, and wherein, the exact level of aluminium plays very important effect, and therefore, method of the present invention can widespread use, and benefit has good prospects.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a full Al-single crystal method in aluminum-base composite slag former, is characterized in that, comprising:
The potpourri melting of aluminum-base composite slag former, sodium carbonate, sodium peroxide and NaOH is obtained molten mixture;
Extract heating after described molten mixture extracting in boiling water boiled, then dilution, constant volume, filtration, obtains solution to be measured after separatory;
EDTA standard solution is added in described solution to be measured;
With solution to be measured described in the titration of copper sulphate standard solution, adopt PAN indicator instruction titration end-point;
With the blank sample of copper sulphate standard solution titration, adopt PAN indicator instruction titration end-point;
According to the volume of the described copper sulphate standard solution of titration, adopt
obtain the mass percentage of full aluminium in aluminum-base composite slag former, wherein V
0represent be blank sample described in titration time the volume of described copper sulphate standard solution that consumes, the volume of the described copper sulphate standard solution that what V represented consume when being solution to be measured described in titration, what T represented is described copper sulphate standard solution to the titer of aluminium, the quality of what m represented the is described aluminum-base composite slag former that described solution to be measured is corresponding.
2. full Al-single crystal method in aluminum-base composite slag former as claimed in claim 1, is characterized in that: the process of solution to be measured described in the titration of described copper sulphate standard solution is carry out under the condition of 4.5 in pH value.
3. full Al-single crystal method in aluminum-base composite slag former as claimed in claim 2, is characterized in that, described pH value be the condition of 4.5 by following process implementation:
Congored test paper is added in the solution described to be measured adding described EDTA standard solution;
Hydrochloric acid is added until described Congored test paper becomes blueness in described solution to be measured;
In described solution to be measured, add acetic acid-ammonium acetate buffer solution and boil.
4. full Al-single crystal method in aluminum-base composite slag former as claimed in claim 3, it is characterized in that, described in the titration of described copper sulphate standard solution, the process of solution to be measured comprises:
Described PAN indicator is added in the solution described to be measured after boiling;
Purple is become with solution to be measured to described solution to be measured described in described copper sulphate standard solution first time titration;
In described solution to be measured, add sodium fluoride solid, after boiling, add described PAN indicator;
Purple is become, the volume V of the described copper sulphate standard solution that record second time consumes with solution to be measured to described solution to be measured described in the titration of described copper sulphate standard solution second time.
5. full Al-single crystal method in aluminum-base composite slag former as claimed in claim 1, it is characterized in that: the quality of described aluminum-base composite slag former is 0.1500 ~ 0.2000g, the quality of described sodium carbonate is 1 ~ 2g, the quality of described sodium peroxide is 2g, the quality of described NaOH is 8g, the temperature of described melting is 680 ~ 700 DEG C, and the time of described melting is 10 ~ 15min.
6. full Al-single crystal method in aluminum-base composite slag former as claimed in claim 1, it is characterized in that: described aluminum-base composite slag former and the ratio of described boiling water extracted are 1.5-2.5g/L, the ratio of the described extract after described aluminum-base composite slag former and constant volume is 0.8g/L.
7. full Al-single crystal method in aluminum-base composite slag former as claimed in claim 1, is characterized in that: the concentration of described EDTA standard solution is 0.017 ~ 0.019mol/L.
8. full Al-single crystal method in aluminum-base composite slag former as claimed in claim 3, is characterized in that: described hydrochloric acid is the volume ratio of HCl and water is the hydrochloric acid of 1:1; The volume ratio of described acetic acid-ammonium acetate buffer solution and described solution to be measured is 1:1.
9. full Al-single crystal method in the aluminum-base composite slag former as described in any one of claim 1 ~ 8, it is characterized in that: the concentration of described copper sulphate standard solution is 0.017 ~ 0.019mol/L, the concentration of described PAN indicator is 1%.
10. full Al-single crystal method in aluminum-base composite slag former as claimed in claim 4, is characterized in that: add described PAN indicator 8 ~ 10 after boiling described acetic acid-ammonium acetate buffer solution; The ratio of described sodium fluoride and described solution to be measured is 40 ~ 60g/L, adds described PAN indicator 3 ~ 5 after boiling described sodium fluoride.
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CN107621519A (en) * | 2017-09-26 | 2018-01-23 | 首钢集团有限公司 | A kind of assay method to metal aluminum content in magnesia carbon brick |
CN109633081A (en) * | 2019-01-31 | 2019-04-16 | 江苏中宜生物肥料工程中心有限公司 | A kind of measuring method of the organic fertilizer content of organic matter |
CN113267419A (en) * | 2021-06-15 | 2021-08-17 | 山西太钢不锈钢股份有限公司 | Detection method of aluminum deoxidizer |
CN114354836A (en) * | 2021-12-13 | 2022-04-15 | 包头钢铁(集团)有限责任公司 | Analysis method for determining total aluminum content in titanium alloy |
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