CN101315316A - Digestion method and detection method of titanium-rich material - Google Patents
Digestion method and detection method of titanium-rich material Download PDFInfo
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- CN101315316A CN101315316A CNA2008101318660A CN200810131866A CN101315316A CN 101315316 A CN101315316 A CN 101315316A CN A2008101318660 A CNA2008101318660 A CN A2008101318660A CN 200810131866 A CN200810131866 A CN 200810131866A CN 101315316 A CN101315316 A CN 101315316A
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Abstract
The invention provides a method for digesting a rich titanium product and a method for detecting the rich titanium product. The method comprises the following steps: placing a sample of the rich titanium product in a container; adding nitric acid, hydrochloric acid and hydrofluoric acid into the container; sealing the container; conducting digestion with microwave to obtain a digestion solution. The method comprises the step of adopting an inductively coupled plasma atomic emission spectrometer to detect the digestion solution prepared through the above steps. According to the digesting method and the detecting method, a plurality of key impurities with the content ranging from 15% to 0.001%, which determine the quality of the rich titanium product, can be simultaneously detected. Furthermore, the accuracy, the precision and the working efficiency of detection data are greatly improved.
Description
Technical field
The present invention relates to a kind of digestion procedure and detection method of rich titanium material, be particularly related to such digestion procedure and detection method, promptly, this digestion procedure can be cleared up rich titanium material quick and completely, and this detection method simultaneously detection level scope is the impurity of 15%～0.001% the rich titanium material of multiple decision product quality.
Background technology
Utilize chloridising by TiO
2Content (weight content, down with) is that first procedure that 45%～70% ilmenite is produced titanium dioxide is that titanium is separated from the ilmenite that contains a large amount of iron and other impurity, to obtain TiO
2The what is called that content is higher, impurity element is less " rich titanium material " (TiO
2Content may be up to 95%) as the raw material of titanium industry.The method of research enrichment ilmenite is one of most active in recent years titanium emtallurgy research problem.
Exploitation is fit to the high-quality rich titanium material of chloride process titanium dioxide, and the reduction impurity of upgrading is important field of research.Therefore, need carry out detection by quantitative accurately to the plurality of impurities of content in 15%～0.001% scope in the rich titanium material such as high titanium slag.
What impurity was the most frequently used in the rich titanium material such as present detection high titanium slag is x-ray fluorescence spectrometry (XRF) method, but, xrf method is as a kind of macro-analysis method, content is at the impurity more than 1% in the rich titanium material of the low-grade high impurity in only suitable test section, impurity to the lower content of 0.5%～0.001% scope in the rich titanium material of high-grade is then powerless, and the sample pre-treatment is to adopt the expensive lithium tetraborate in the 15g left and right sides to carry out long-time fusion as flux under hot conditions more than 1000 ℃ to clear up reaction, blank background influence is big, the analysis cost height, round of visits is long.
Though inductively coupled plasma atomic emission spectrum (ICP-AES) method has possessed the ability of analyzing impurity in 15%～0.001% content range on technical feature, crucial part but is to lack at present the rich titanium material Specimen eliminating pre-treating method that is complementary with it.The mode that reaction is cleared up in the fusion that XRF is commonly used can not be used for the ICP-AES method fully, what wet method was cleared up generally employing now is with reagent such as a large amount of sulfuric acid, hydrochloric acid, hydrofluorite, the high temperature heating sample is to the mode of emitting the sulfuric acid cigarette to handle, this mode only can satisfy needing of part element detection reluctantly, fundamentally neither be a kind of the digestion procedure that requires of suitable ICP-AES check and analysis, the just expedient plan under the situation that does not have a kind of more satisfactory rich titanium material digestion procedures such as high titanium slag.Present rich titanium material digestion procedure has following shortcoming: 1. the impurity that can check is limited, because the restriction of digestion procedure, can not detect many important impurity that influence product performance index in the rich titanium material, for example should not detect the oxide Al that acid can't effectively be cleared up under the Ca, normal condition of easy generation slightly solubility sulfate
2O
3, SiO
2, Cr
2O
3Deng; 2. because high matrix Ti very easily hydrolysis form precipitation, wrap up element to be measured or stop up analytical instrument, digestion solution must replenish hydrochloric acid and keep 30% acidity, has increased blank influence and to the corrosive attack of instrument sampling system; 3. sulfuric acid density is big, viscosity is big, boiling point is high and consumption is big (needs 10mL～15mL) so serious transmission, atomizing and the launching efficiency of disturbing such as the high salt density of solution, matrix effect usually; 4. clear up effect with products material, technology, grade and difference, basically can clear up after the long-time pyroreaction of low grade titanium-riched material fully, but the actual effect of clearing up the rich titanium material of high-grade is not fully up to expectations, and grade is high more consuming time long more, even many Specimen eliminatings are incomplete.
In a word, existing rich titanium material analytical approach mainly exist the detection elements kind few, cover concentration range narrow, clear up shortcoming and limitations such as processing mode complexity, disturbing factor is many, analytical cycle is long.Application still immature, the imperfection of ICP-AES method in rich titanium material such as check and analysis high titanium slag.
Summary of the invention
One object of the present invention is to provide a kind of highly effective and safe, quick and complete the method for clearing up rich titanium material, another object of the present invention is to provide a kind of detection method that realizes the complete detection of impurity such as Al, Si in 15%～0.001% content range in the rich titanium material, Cr, Ca, Mg, Fe, Mn, V, P.
Digestion procedure according to a kind of rich titanium material of the present invention may further comprise the steps: get rich titanium material sample to be tested in container, add nitric acid, hydrochloric acid, hydrofluorite in described container, airtight then described container is cleared up with microwave, obtains digestion solution.Rich titanium material is by TiO
2Form with plurality of impurities, the weight content of every kind of impurity in the described plurality of impurities is 15%～0.001%.The concentration of the nitric acid that is adopted is 65%～68%, and the concentration of hydrochloric acid is 36%～38%, and the concentration of hydrofluorite is 40%～47%.
According to an aspect of the present invention, the step that adds nitric acid, hydrochloric acid, hydrofluorite can comprise: add nitric acid, hydrochloric acid earlier, carry out pre-reaction under room temperature environment, question response calmness, temperature of charge add hydrofluorite after near room temperature again.
According to an aspect of the present invention, rich titanium material sample to be tested is added acid to carry out micro-wave digestion and can comprise with the step that obtains digestion solution: get rich titanium material sample to be tested in container, in the rich titanium material of 0.2000g～0.5000g sample to be tested, add 4mL～7mL nitric acid, 1mL～3mL hydrochloric acid, under room temperature environment, react tranquil and do not have bubble and a NO to liquid level
2Brown cigarette produces; Then, add 1mL～2mL hydrofluorite, closed container and clear up with microwave obtains digestion solution subsequently.
According to an aspect of the present invention, the heating mode of the step of clearing up with microwave can adopt the slope to heat up, pressure in the micro-wave digestion process in the container can be below the 800psi, but micro-wave digestion process proceed step by step, that is, at first material in the container is warming up to 120 ℃～130 ℃ with 2min, is incubated 2min subsequently, and then be warming up to 170 ℃～180 ℃ with 2min, be incubated 10min～14min subsequently.
Detection method according to a kind of rich titanium material of the present invention comprises that employing ICP-AES spectrometer detects the digestion solution that the digestion procedure according to rich titanium material of the present invention prepares.If the sampling system of ICP-AES spectrometer does not have anti-corrosion capability to hydrofluorite or require to detect Si element in the rich titanium material, then this detection method also can comprise the step that adds the excessive hydrofluorite of boric acid complexing to digestion solution.Preferably, be that the form of 10%～15% boric acid aqueous solution adds boric acid with concentration.
Therefore, the digestion procedure of rich titanium material of the present invention has advantages such as less, the blank influence of reagent dosage is lower, acidity is lower, salt density is lower, test solution is simpler, has realized that sample-pretreating method and ICP-AES detection method mate preferably.The detection method of rich titanium material of the present invention has satisfied the needs that detect with impurity such as Al, Si in 15%～0.001% concentration range in the rich titanium material of the high and low grade of different material, explained hereafter, Cr, Ca, Mg, Fe, Mn, V, P comprehensively, overcome the shortcoming of original method, had and detect wide dynamic range, Specimen eliminating efficient quick, easy and simple to handle, detection elements is many, concentration range is wide, disturbing factor is few, lack detection time advantage.
Embodiment
Digestion procedure according to rich titanium material of the present invention may further comprise the steps: get rich titanium material sample to be tested in container, add nitric acid, hydrochloric acid, hydrofluorite in container, closed container is cleared up with microwave then, obtains digestion solution.Here, rich titanium material is by principal ingredient TiO
2Form with plurality of impurities, the weight content of every kind of impurity in the plurality of impurities is 15%～0.001%.
The consumption of the low more needed acid of the concentration of above-mentioned hydrofluorite, hydrochloric acid, nitric acid is many more, because the volume of microwave airtight digestion container is limited, the consumption of general reagent and the used distilled water of flushing tank skin is altogether less than 30ml, and acid concentration more the low reaction time long more, so concentrated acid of hydrofluorite, hydrochloric acid, the preferred not diluted of nitric acid, for example, preferred concentration is that 65%～68% nitric acid, concentration are that 36%～38% hydrochloric acid, concentration are 40%～47% hydrofluorite.
The step of above-mentioned adding nitric acid, hydrochloric acid, hydrofluorite can comprise: add earlier nitric acid, hydrochloric acid, carry out pre-reaction under room temperature environment, question response calmness, temperature of charge add hydrofluorite after near room temperature again.Here, how much specifically deciding of the addition of nitric acid, hydrochloric acid, hydrofluorite according to the sample weighting amount of rich titanium material sample to be tested, rich titanium material samples for 0.2000g～0.5000g, can add 4mL～7mL nitric acid earlier, add 1mL～3mL hydrochloric acid again, under room temperature environment, react tranquil and do not have bubble and a NO to liquid level
2Brown cigarette produces, and adds 1mL～2mL hydrofluorite then, and closed container and clear up with microwave obtains digestion solution subsequently.
The closed microwave of said method is cleared up and can be adopted micro-wave digestion equipment commonly used, the heating mode of clearing up with microwave can adopt the slope to heat up, pressure in the micro-wave digestion process in the container can be below the 800psi, but micro-wave digestion process proceed step by step, that is, at first material in the container is warming up to 120 ℃～130 ℃ with 2min, is incubated 2min subsequently, and then be warming up to 170 ℃～180 ℃ with 2min, be incubated 10min～14min subsequently.
Because the main matrix composition of rich titanium material such as high titanium slag is TiO
2, impurity element Si, Al etc. are many again with oxide S iO
2, Al
2O
3Form exists, so select for use nitric acid, hydrochloric acid and the hydrofluorite acting in conjunction under microwave condition of suitable consumption, ratio can decompose the Ti base, HF clears up SiO
2, HNO
3, HCl clears up all the other Al
2O
3, Cr
2O
3, CaO, MnO, impurity such as MgO, Fe, complex reaction takes place in F-and Ti simultaneously, Ti is existed with the form stable of complex anion, high concentration Ti matrix does not have the hydrolysis phenomenon yet in the solution medium of acidity less than 6%, digestion solution can keep clarification for a long time, and the airtight condition in the micro-wave digestion process has avoided Si, Cr with SiF
4, CrOCl
3Form volatilization loss.
Detection method according to rich titanium material of the present invention comprises that employing ICP-AES spectrometer detects the digestion solution that the digestion procedure according to rich titanium material of the present invention prepares.If the sampling system of ICP-AES spectrometer does not have anti-corrosion capability to hydrofluorite or require to detect Si element in the rich titanium material, detection method then of the present invention also can comprise the step that adds the excessive hydrofluorite of boric acid complexing to digestion solution, wherein, being that the form of 10%～15% boric acid aqueous solution adds boric acid with concentration preferably, is that the form of 10% boric acid aqueous solution adds boric acid with concentration further preferably.For example, as mentioned above according to digestion procedure of the present invention, earlier the rich titanium material samples to 0.2000g～0.5000g adds 4mL～7mL nitric acid, adds 1mL～3mL hydrochloric acid again, reacts tranquil and do not have bubble and a NO to liquid level under room temperature environment
2Brown cigarette produces, and adds 1mL～2mL hydrofluorite then, and closed container and clear up with microwave obtains digestion solution subsequently; If the sampling system of ICP-AES spectrometer does not have anti-corrosion capability to hydrofluorite or require to detect Si element in the rich titanium material, it is boric acid aqueous solution 0.5mL～excessive hydrofluorite of 1.0mL complexing of 10% that detection method then of the present invention can add concentration to digestion solution, constant volume detects then, if the sampling system of ICP-AES spectrometer has anti-corrosion capability to hydrofluorite and does not require the Si element that detects in the rich titanium material, then do not need to add boric acid, can directly carry out constant volume digestion solution.Therefore, use the excessive hydrofluorite of boric acid complexing as required, cause the measurement result of corroding and influencing Si to avoid sampling system (for example glass component) to detecting instrument.
Therefore, form mixing according to the digestion procedure of rich titanium material of the present invention with suitable kind, concentration, consumption and ratio and clear up reagent, in conjunction with the airtight type of heating of microwave, only needed just can apace the harmless lost territory of titanium matrix and all impurity in the rich titanium material such as high titanium slag be cleared up fully in 15 minutes～20 minutes.In addition, digestion procedure according to rich titanium material of the present invention does not use the reagent such as sulfuric acid that have a strong impact on the ICP-AES analytical performance, and reagent dosage seldom, need not to replenish reagent such as a large amount of hydrochloric acid and keep 30% highly acid medium, rely on the complexing stabilization of reagent negative ion and Ti, the acidity of only clearing up the residual reagent less than 6% of sample can be guaranteed the test solution clarification and not hydrolysis, effectively reduces blank influence and to the corrosive attack of instrument.Therefore, the test solution according to the digestion procedure of rich titanium material of the present invention and detection method is simple, salt density is low, background influence and matrix effect are little.
Below, will digestion procedure and the detection method according to the rich titanium material of the embodiment of the invention be described in detail.
The following examples have illustrated in further detail according to the digestion procedure of rich titanium material of the present invention and detection method.Yet, should be appreciated that the present invention is not subjected to the restriction of these embodiment.
Embodiment 1
It is pure that the acid that present embodiment adopted, reagent are top grade, and used microwave digestion system is produced Mars5 by U.S. CE M company, and the ICP-AES spectrometer is that the U.S.'s thermoelectric element IRIS/HR of company type is composed the direct-reading plasma spectrometer entirely.
Clearing up of rich titanium material
In the present embodiment, to TiO
2Content is that 97.55% No. 1 rich titanium material is cleared up.No. 1 rich titanium material that takes by weighing 0.2500g in micro-wave digestion jar in, along tank skin elder generation Dropwise 5 .0mL concentration is that 65%～68% nitric acid, 1.0mL concentration are 36%～38% hydrochloric acid, and the jog counteracting tank, acid is fully contacted with rich titanium material and pre-reaction to liquid level calmness and do not have bubble and NO
2Brown cigarette produces, treat to add again after temperature of charge is near room temperature in the counteracting tank 1.0mL concentration and be 40%～47% hydrofluorite, put outer jar then, build lid and tighten with torque spanner, pack in the micro-wave digestion stove by the instrumentation step, connect temperature, pressure transducer.Carry out micro-wave digestion by set micro-wave digestion heating schedule, it is to heat up in the slope that present embodiment is provided with heating schedule, pressure control is below 800psi, whole digestion process is divided into two steps to carry out, promptly, at first material in the counteracting tank is warming up to 120 ℃ and be incubated 2min with 2min, and then is warming up to 180 ℃ and be incubated 12min with 2min.
The detection of digestion solution
After clearing up EOP (end of program), utilize the air-cooled jar internal pressure that makes less than 50psi, take out counteracting tank then and the nut of slowly outwarding winding discharges surplus pressure in fuming cupboard, can add concentration subsequently and be 10% boric acid aqueous solution 0.5mL～1.0rL and the abundant complex reaction of excessive HF.Then, this digestion solution is carried out constant volume, that is, this digestion solution is transferred in the 100mL volumetric flask, adopt redistilled water to be diluted to scale, mixing.In the present embodiment, if the ICP-AES spectrometer that uses has the sampling system of anti-HF, can not add boric acid aqueous solution.
Impurity such as Al, the Si in the digestion solution behind the employing ICP-AES method detection constant volume, Cr, Ca, Mg, Fe, Mn, V, P, the content of every kind of impurity in rich titanium material in the impurity such as described Al, Si, Cr, Ca, Mg, Fe, Mn, V, P is 15%～0.001%.Basically carry out ICP-AES in the usual way and detect step, but present embodiment carries out the matrix coupling with the blunt titanium of height when the preparation working curve, further eliminate matrix effect in conjunction with synchronous background correction technology.
Ultimate analysis line to be measured can not be subjected to the disturbing effect of titanium wire, therefore need reasonably select spectral line, background correction and detect integral domain.Table 1 shows spectral line, background correction and the detection integral domain that present embodiment is selected.
Table 1
| Element | Wavelength (nm) | Left side background correction point (pixel) | Right background correction point (pixel) | Integral domain center width (pixel) | Integral measurement position (pixel) |
| Cr | 283.563 | 1 | 14 | 2 | 7 |
| Cr | 206.149 | 1 | 14 | 1 | 7 |
| Fe | 240.488 | 1 | 14 | 1 | 8 |
| Fe | 238.204 | 3 | 12 | 2 | 7 |
| Mg | 285.213 | 3 | 14 | 2 | 7 |
| Mg | 293.654 | 1 | 10 | 1 | 7 |
| Mn | 293.930 | 3 | 14 | 1 | 7 |
| Mn | 257.610 | 3 | 13 | 2 | 7 |
| P | 213.618 | 2 | 14 | 1 | 8 |
| P | 178.287 | 2 | 13 | 2 | 8 |
| V | 310.230 | 3 | 11 | 1 | 7 |
| V | 309.311 | 4 | 11 | 2 | 8 |
| Ca | 393.366 | 2 | 13 | 1 | 7 |
| Ca | 315.887 | 5 | 13 | 1 | 8 |
| Si | 251.612 | 4 | 12 | 2 | 7 |
| Si | 184.006 | 3 | 14 | 1 | 7 |
| Al | 394.401 | 4 | 15 | 2 | 7 |
| Al | 396.152 | 4 | 13 | 2 | 7 |
Embodiment 2
Except adopting TiO
2Content is that 92.12% No. 2 rich titanium material replace clearing up rich titanium material and detecting digestion solution according to the method identical with the method for embodiment 1 outside No. 1 rich titanium material.
Embodiment 3
Except adopting TiO
2Content is that 75.46% No. 3 rich titanium material (high titanium slag) replace clearing up rich titanium material and detecting digestion solution according to the method identical with the method for embodiment 1 outside No. 1 rich titanium material.
Embodiment 4
Except adopting TiO
2Content is that 74.01% No. 4 rich titanium material (high titanium slag) replace clearing up rich titanium material and detecting digestion solution according to the method identical with the method for embodiment 1 outside No. 1 rich titanium material.
Embodiment 5
Except adopting TiO
2Content is that 73.75% No. 5 rich titanium material (high titanium slag) replace clearing up rich titanium material and detecting digestion solution according to the method identical with the method for embodiment 1 outside No. 1 rich titanium material.
Embodiment 6
Except adopting TiO
2Content is that 74.77% No. 6 rich titanium material (high titanium slag) replace clearing up rich titanium material and detecting digestion solution according to the method identical with the method for embodiment 1 outside No. 1 rich titanium material.
Embodiment 7
Except adopting TiO
2Content is that 73.26% No. 7 rich titanium material (high titanium slag) replace clearing up rich titanium material and detecting digestion solution according to the method identical with the method for embodiment 1 outside No. 1 rich titanium material.
Embodiment 8
Except adopting TiO
2Content is that 99.999% No. 8 rich titanium material (high-purity titanium dioxide) replace clearing up rich titanium material and detecting digestion solution according to the method identical with the method for embodiment 1 outside No. 1 rich titanium material.
Comparative Examples
Clear up every kind of rich titanium material in above-mentioned No. 1 to No. 8 rich titanium material according to following classic method: to quality is that to add 15mL concentration be that 95%～98% the concentrated sulphuric acid and 10mL concentration are 36%～38% concentrated hydrochloric acid for every kind of rich titanium material in No. 1 to No. 8 rich titanium material of 0.2500g, be heated to then and emit the sulfuric acid cigarette, sample is cleared up in cooling subsequently.
Table 2 shows the effect of clearing up of embodiment 1 to embodiment 8 and Comparative Examples.
Table 2
As can be seen from Table 2, the present invention is actual clear up respond well, comprise that grade is that the rich titanium material of the various grades of 99.999% high-purity titanium dioxide all can be cleared up clean fully, up hill and dale, the noresidue sample, there is not insoluble residue, solution clarification has reached the present invention and has solved the target that rich titanium material such as high titanium slag is cleared up a difficult problem, is better than traditional disposal route of emitting the sulfuric acid cigarette comprehensively.Therefore, digestion procedure of the present invention has good and extensive applicability, and the rich titanium material of the different qualities that manufacture for various processes, equipment all has the good ability of clearing up.
Embodiment 9: clear up, the test of the precision of detection method
Above-mentioned No. 1 and No. 2 rich titanium material grades are higher, impurity content is relatively low, carry out precision test difficulty with this and be greater than the high low-grade sample of impurity content, and, because above-mentioned rich titanium material is taken from the production scene and is not reprocessed, rich titanium material homogeneity is relatively poor, also influenced test findings to a certain extent, but for more strictly verifying precision of the present invention, adopt method among embodiment 1 and the embodiment 2 respectively No. 1 and No. 2 rich titanium material samples to be carried out 8 times and independently clear up assay determination with ICP-AES, 8 measurement results are carried out statistical treatment, assess precision of the present invention according to relative standard deviation.Measurement result sees Table 3 and table 4, and wherein, table 3 shows the analysis result and the precision of No. 1 rich titanium material, and table 4 shows the analysis result and the precision of No. 2 rich titanium material.
Table 3
Table 4
By table 3 and table 4 as can be seen, all less than 9%, it is respond well to show that rich titanium material is cleared up, detected to method of the present invention, favorable reproducibility, precision height in 0.001% relative standard deviation that detects each element more than the lower limit.
Embodiment 10: clear up, the recovery test of detection method
Respectively No. 1 and No. 2 rich titanium material are carried out recovery test, promptly take by weighing two parts in same rich titanium material sample, and before Specimen eliminating is handled, a certain amount of standard substance of adding in a copy of it sample, and another duplicate samples does not add standard substance.Then, method according to embodiment 1 is cleared up, is detected No. 1 rich titanium material sample that does not add the standard material and No. 1 rich titanium material sample that has added standard substance respectively, method according to embodiment 2 is cleared up, is detected No. 2 rich titanium material samples that do not add the standard material and No. 2 rich titanium material samples that added standard substance respectively, estimates accuracy of the present invention by the recovery of calculating each element.Table 5 shows the recovery of clearing up with each element of detection method according to of the present invention.
Table 5
As can be seen from Table 5, the recovery of clearing up with detection method of the present invention is 91.40%～117.5%, shows that analysis result has higher accuracy.
Embodiment 11: the analysis result control test
The micro-wave digestion, ICP-AES method that uses the embodiment of the invention 1 to embodiment 7 cleared up 1,2,3,4,5,6, No. 7 rich titanium material samples respectively and detected.In addition,, as flux, melt sheet, then this glassy sample is melted sheet and carry out XRF and measure at 1000 ℃ of glassy samples of high-temperature fusion prepared in reaction with lithium tetraborate etc. for each sample in 1,2,3,4,5,6, No. 7 rich titanium material samples.The measurement result of more above-mentioned two kinds of technological means is verified the present invention's accurate detectability in the broad concentration range of 5 orders of magnitude of 15%～0.001%.Table 6 shows result's contrast of the analyzing and testing of these two kinds of technological means.
Table 6
As can be seen from Table 6, xrf method can not be finished the accurate mensuration of 1% following trace impurity, can not satisfy the needs that the rich titanium material of high-quality of high grade, that impurity content is low sample detection is analyzed; The present invention overcomes the weak point of xrf method, can directly measure the trace impurity in 1%～0.001% content range in the rich titanium material of the high-grade sample exactly simultaneously.And, adopt this method to clear up rich titanium material, the result and the xrf method measurement result basically identical of the impurity of measuring by the ICP-AES method, show that the present invention clears up, detection method and traditional detection method be accurately same and reliable, realized the multianalysis to the impurity in 15%～0.001% content range in the rich titanium material of the various places of production, type, grade.
In sum, digestion procedure of the present invention has been realized the matrix of rich titanium material such as high titanium slag and the highly effective and safe of all impurity, quick and complete clearing up, ICP-AES detection method of the present invention detection level scope simultaneously is the critical impurities of the rich titanium material of multiple decision product qualities such as 15%～0.001% Al, Si, Cr, Ca, Mg, Fe, Mn, V, P, and improved the accuracy, precision and the work efficiency that detect data greatly, had wide prospect in industrial application.
Claims (13)
1, a kind of digestion procedure of rich titanium material is characterized in that described digestion procedure may further comprise the steps:
Get rich titanium material sample to be tested in container, add nitric acid, hydrochloric acid, hydrofluorite in described container, airtight then described container is cleared up with microwave, obtains digestion solution.
2, digestion procedure as claimed in claim 1 is characterized in that described rich titanium material is by TiO
2Form with plurality of impurities, the weight content of every kind of impurity in the described plurality of impurities is 15%～0.001%.
3, digestion procedure as claimed in claim 1 is characterized in that the step that adds nitric acid, hydrochloric acid, hydrofluorite comprises: add earlier nitric acid, hydrochloric acid, carry out pre-reaction under room temperature environment, question response calmness, temperature of charge add hydrofluorite after near room temperature again.
4, digestion procedure as claimed in claim 1 is characterized in that rich titanium material sample to be tested is added acid to carry out micro-wave digestion and comprise with the step that obtains digestion solution:
Get rich titanium material sample to be tested in container,, add 4mL～7mL nitric acid, 1mL～3mL hydrochloric acid, under room temperature environment, react tranquil and do not have bubble and a NO to liquid level in the rich titanium material of 0.2000g～0.5000g sample to be tested
2Brown cigarette produces;
Then, add 1mL～2mL hydrofluorite, closed container and clear up with microwave obtains digestion solution subsequently.
5, digestion procedure as claimed in claim 1, the heating mode that it is characterized in that the step cleared up with microwave adopts the slope to heat up, pressure in the micro-wave digestion process in the container is below the 800psi, micro-wave digestion process proceed step by step, that is, at first material in the container is warming up to 120 ℃～130 ℃ with 2min, is incubated 2min subsequently, and then be warming up to 170 ℃～180 ℃ with 2min, be incubated 10min～14min subsequently.
6, digestion procedure as claimed in claim 1 is characterized in that rich titanium material sample to be tested is added acid to carry out micro-wave digestion and comprise with the step that obtains digestion solution:
Get rich titanium material sample to be tested in container,, add 5.0mL nitric acid, 1.0mL hydrochloric acid, under room temperature environment, react tranquil and do not have bubble and a NO to liquid level in the rich titanium material of 0.2500g sample to be tested
2Brown cigarette produces;
Then, add 1.0mL hydrofluorite, closed container and clear up with microwave obtains digestion solution subsequently.
7, digestion procedure as claimed in claim 6, the heating mode that it is characterized in that the step cleared up with microwave adopts the slope to heat up, pressure in the micro-wave digestion process in the container is below the 800psi, micro-wave digestion process proceed step by step, that is, at first material in the container is warming up to 120 ℃ with 2min, is incubated 2min subsequently, and then be warming up to 180 ℃ with 2min, be incubated 12min subsequently.
8, digestion procedure as claimed in claim 1, the concentration that it is characterized in that described nitric acid is 65%～68%, and the concentration of described hydrochloric acid is 36%～38%, and the concentration of described hydrofluorite is 40%～47%.
9, a kind of detection method of rich titanium material is characterized in that described detection method may further comprise the steps:
Adopt inductively coupled plasma atomic emission spectrometer that the digestion solution according to claim 1 preparation is detected.
10, detection method as claimed in claim 9, it is characterized in that then described detection method is further comprising the steps of: add the excessive hydrofluorite of boric acid complexing to digestion solution if the sampling system of inductively coupled plasma atomic emission spectrometer does not have anti-corrosion capability to hydrofluorite or require to detect Si element in the rich titanium material.
11, detection method as claimed in claim 10 is characterized in that with concentration being that the form of 10%～15% boric acid aqueous solution adds described boric acid.
12, a kind of detection method of rich titanium material is characterized in that described detection method may further comprise the steps:
Adopt inductively coupled plasma atomic emission spectrometer that the digestion solution according to any claim preparation in claim 4 and the claim 6 is detected.
13, detection method as claimed in claim 12, it is characterized in that then described detection method is further comprising the steps of if the sampling system of inductively coupled plasma atomic emission spectrometer does not have anti-corrosion capability to hydrofluorite or require to detect Si element in the rich titanium material: adding concentration to digestion solution is boric acid aqueous solution 0.5mL～excessive hydrofluorite of 1.0mL complexing of 10%.
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Cited By (19)
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|---|---|---|---|---|
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| CN103808558A (en) * | 2014-03-03 | 2014-05-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Digestion method and detection method for vanadium-nitrogen-titanium-iron mixed alloy conductor |
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2008
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| CN101598673B (en) * | 2009-07-02 | 2010-10-20 | 河北省电力研究院 | Calcium base desulfurater primary and secondary content and impurity element simultaneous determination method |
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| CN106872258A (en) * | 2017-04-27 | 2017-06-20 | 攀钢集团研究院有限公司 | Clear up the method for titanium-based denitrating catalyst and the detection method of digestion solution |
| CN107121426A (en) * | 2017-04-27 | 2017-09-01 | 攀钢集团研究院有限公司 | Clear up the method for vanadium chromium titanium alloy and the detection method of digestion solution |
| CN107121426B (en) * | 2017-04-27 | 2019-12-03 | 攀钢集团研究院有限公司 | Clear up the method for vanadium chromium titanium alloy and the detection method of digestion solution |
| CN107367505A (en) * | 2017-07-20 | 2017-11-21 | 中钢集团郑州金属制品研究院有限公司 | The ICP AES methods of niobium element content in a kind of rapid and accurate determination heat resisting steel |
| CN107367505B (en) * | 2017-07-20 | 2020-12-25 | 中钢集团郑州金属制品研究院有限公司 | ICP-AES method for rapidly and accurately determining content of niobium element in heat-resistant steel |
| CN110568123A (en) * | 2019-09-04 | 2019-12-13 | 广西蓝星大华化工有限责任公司 | Method for analyzing quality of titanium liquid after acidolysis leaching |
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