CN107121426A - Clear up the method for vanadium chromium titanium alloy and the detection method of digestion solution - Google Patents
Clear up the method for vanadium chromium titanium alloy and the detection method of digestion solution Download PDFInfo
- Publication number
- CN107121426A CN107121426A CN201710287873.9A CN201710287873A CN107121426A CN 107121426 A CN107121426 A CN 107121426A CN 201710287873 A CN201710287873 A CN 201710287873A CN 107121426 A CN107121426 A CN 107121426A
- Authority
- CN
- China
- Prior art keywords
- titanium alloy
- chromium titanium
- vanadium chromium
- solution
- vanadium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
Abstract
The invention belongs to test and analyze technical field, and in particular to a kind of method and detection method for clearing up vanadium chromium titanium alloy.The method for clearing up vanadium chromium titanium alloy comprises the following steps：Hydrochloric acid, nitric acid and water are mixed in digestive reagent, vanadium chromium titanium alloy and add digestive reagent, heating is boiled solution reaction and no longer reduced to solid；Then reduction temperature is reacted to remaining solid material and cleared up completely, cool down, produce digestion solution to hydrofluoric acid, keeping temperature is added after 65~75 DEG C.This method realizes the quick and complete of vanadium chromium titanium alloy sample and cleared up and while determine contained secondary amounts alloying element and micro impurity element, with efficient quick easy to operate, disturbing factor less accurately and reliably, testing process is short, speed is fast the features such as.
Description
Technical field
The invention belongs to test and analyze technical field, and in particular to a kind of method and digestion solution for clearing up vanadium chromium titanium alloy
Detection method.Specifically, the present invention relates to one kind be used to determining in vanadium chromium titanium alloy material mass fraction be 2.5~
5.5% secondary amounts alloying elements cr, Ti, and mass fraction is 0.001~0.25% micro impurity element Al, As, Co,
Cu, Fe, Mg, Mn, Ni, P, Pb, Si, Sn, W, Zn, Zr and mass fraction are that 0.005~0.25%K, Na sample solution are cleared up
The detection method of preparation method and contained elemental composition.
Background technology
Vanadium chromium titanium alloy (reference element V-4Cr-4Ti) is important fusion reactor candidate structure material, usual V-
Using raw material based on the vanadium metal and hundreds of μm~1mm hafnium metal powfers and metallic titanium powder of high-purity more than Cr-Ti alloys, press
Produce and prepare in methods such as magnetic levitation melting, powder metallurgy, vacuum consumable electric arc remeltings (VAR) according to V-4.5Cr-4Ti proportionings.
VAR methods use the vanadium metal, chromium and titanium of high-purity to prepare electrode for raw material and carry out vacuum melting, the rare costliness of high pure metal raw material
V-Cr-Ti alloy productions cost is caused to remain high.Positive research domestic at present uses V2O5、Cr2O3、TiO2Deng the original of relative moderate
The new technology of material reduction melting V-Cr-Ti alloys, but be due to V2O5、Cr2O3To be relatively higher than Deng impurity content in raw material
The high pure metals such as vanadium, chromium, and using multicomponent reducing agent also increase impurity element in V-Cr-Ti alloys and its content can
Can property, therefore one of its Key Technology for Development difficult point is to ensure that the content and ratio and reduction impurity content of alloying element chromium titanium
Product purity is ensured, is also to ensure that the quality for the V-Cr-Ti alloy products that inexpensive new technology is produced disclosure satisfy that nuclear energy
The requirement of the field such as industry high standard, reaches and traditional high cost smelting technology identical product quality, it is especially desirable to the research palm
Alloying element chromium titanium and more than 10 kind trace impurity high precision test technologies in V-4Cr-4Ti vanadium-base alloy are held, to be closed for vanadium
The process exploitation of gold provides " industrial eyes ", is that process of producing product control and production assurance provide detection support technology hand
Section.
The Specimen eliminating preparation method and elemental composition detection method of existing vanadium alloy material are primarily adapted for use in vanadium iron, vanadium aluminium
Deng sample, mainly with HCl ︰ HNO3=1 ︰ 1 or HCl ︰ HNO3The grade composite reagents of=2 ︰ 1 clear up preparation sample detection solution, then
Fe, Si, W, Mn, Mg, Ni, Pb, Sn, As, Cr, Co, Cu, B, P, Mo etc. are determined with inductively coupled plasma emission spectrography micro-
The method for measuring impurity content.The problem of such method is maximum is only to be suitable for that quick and complete to clear up crystal structure relatively simple
It is single and the material samples such as the vanadium iron and vananum of matrix component are only made up of the ease of solubility element such as vanadium, iron, aluminium, it is impossible to use
In clearing up the vanadium chromium titanium three that alloy structure is more complicated He matrix component includes high level slightly solubility elemental chromium, titanium is formed
The sample detection solution of first alloy material, greatly prolongs even if the reaction time and is also difficult to ensure clearing up completely for vanadium chromium titanium sample.
Moreover, the ICP-OES detection methods of existing vanadium iron, vanadium aluminium are only suitable for the micro impurity element in determination sample, usual secondary amounts is closed
Gold element needs to be measured using chemical analysis methods such as titrations, it is impossible to meets and determines secondary in vanadium chromium titanium alloy material simultaneously
The need for measuring alloying elements cr, Ti and micro impurity element.
The content of the invention
The problem of existing for prior art, is applied to determine V-Cr-Ti ternary alloy three-partalloys simultaneously the invention provides one kind
Secondary amounts alloying elements cr, Ti and other micro impurity elements in material clear up preparation method and elemental composition detection side
Method.
The present invention includes for ternary alloy three-partalloy crystal structure and its matrix component more complicated in vanadium chromium titanium alloy material
There are high level refractory element chromium, titanium and need to detect not only slightly solubility and the impurity member easily condensed or hydrolyzed such as silicon, tungsten
Plain the characteristics of, the component that have developed corresponding vanadium chromium titanium alloy sample digestive reagent is constituted and its addition opportunity and reaction temperature bar
Part etc., and optimize the proportionate relationship between sample quality and reagent dosage, it is ensured that the Specimen eliminating preparation method formulated
Quick and complete without loss it can clear up vanadium chromium titanium alloy sample, and the sample matter optimized in Specimen eliminating preparation method
The Instrument working parameter that is optimized in amount, reagent dosage, dilution ratio, reaction condition etc. and ICP-OES element determination methods,
Suitable sensitivity analysis spectral line etc., it is ensured that method can meet the need for determining secondary amounts alloying element and micro impurity element simultaneously
Will, operating efficiency is not only substantially increased, round of visits is shortened, and the influence factors such as matrix effect are reduced, improve element
The degree of accuracy of content detection result and precision level, meet and meanwhile determine vanadium chromium titanium alloy material in secondary amounts alloying element and
The need for micro impurity element.
First technical problem to be solved by this invention is to provide a kind of method for clearing up vanadium chromium titanium alloy.This method bag
Include following steps：Hydrochloric acid, nitric acid and water are mixed in digestive reagent, vanadium chromium titanium alloy and add digestive reagent, heating is boiled
Solution reaction is no longer reduced to solid；Then reduction temperature is to hydrofluoric acid is added after 65~75 DEG C, and keeping temperature is reacted to residue
Solid matter is cleared up completely, cooling, produces digestion solution.
It is preferred that, in the above-mentioned method for clearing up vanadium chromium titanium alloy, every 0.2~0.4g vanadium chromium titanium alloy adds 30~60mL and disappeared
Solve reagent.Further, 15mL digestive reagents are added per 0.1g vanadium chromium titanium alloy.
It is preferred that, in the above-mentioned method for clearing up vanadium chromium titanium alloy, count by volume, the ︰ 2 of Yan Suan ︰ Xiao Suan ︰ water=2~3 ︰ 1~
Three's mixing is prepared digestive reagent by 3.It is preferred that, the Yan Suan ︰ Xiao Suan ︰ water=︰ 2 of 2 ︰ 1.
It is preferred that, in the above-mentioned method for clearing up vanadium chromium titanium alloy, the mass concentration of the nitric acid is 65~68%；Hydrochloric acid
Mass concentration is 36~38%；The mass concentration of the hydrofluoric acid is 40~47%.
It is preferred that, in the above-mentioned method for clearing up vanadium chromium titanium alloy, every 0.2~0.4g vanadium chromium titanium alloy adds 0.5~1mL hydrogen
Fluoric acid.
The digestion solution prepared by the above-mentioned method for clearing up vanadium chromium titanium alloy, in order to detect Cr therein, Ti,
Al, As, Co, Cu, Fe, Mg, Mn, Ni, P, Pb, Si, Sn, W, Zn, Zr, K, Na equal size, can be by a variety of methods to above-mentioned member
Cellulose content is measured, such as AAS, atomic absorption spectrography (AAS), inductively coupled plasma atomic emission spectrometry, electricity
Feel the methods such as coupled plasma mass to determine one or more components in the digestion solution.According to the detection side of selection
Method, come decide whether with water it is further to digestion solution dilution, dilution how much, be disposably to detect all elements to be measured also
It is to detect in batches.
Second technical problem to be solved by this invention is to provide the above-mentioned method for clearing up vanadium chromium titanium alloy and prepared
Digestion solution.
3rd technical problem to be solved by this invention is to provide the detection method of above-mentioned digestion solution.The detection method
Comprise the following steps：
A, preparation standard curve：The standard liquid that element to be measured is added in vanadium standard liquid is configured to the molten of various concentrations
Liquid, is then detected using inductively coupled plasma atomic emission spectrometry to the solution of variant concentration, draws curve,
Obtain concentration-strength criterion curve of each metal；
B, same use inductively coupled plasma atomic emission spectrometry are detected to gained digestion solution to be measured, are obtained
To each metal ion intensity, concentration is drawn by corresponding concentration-strength criterion curve, content is finally drawn.
It is preferred that, in the detection method step A of above-mentioned digestion solution, when detecting Cr or Ti, compound concentration scope is 2.5
~5.5% various concentrations solution；When detecting Al, As, Co, Cu, Fe, Mg, Mn, Ni, P, Pb, Si, Sn, W, Zn or Zr, match somebody with somebody
Concentration range processed is 0.001%~0.25% various concentrations solution；When detecting K or Na, compound concentration scope is 0.005%
~0.25% various concentrations solution.
It is preferred that, in detection method the step A or B of above-mentioned digestion solution, the inductively coupled plasma atomic emissions
Spectroscopic methodology parameter is set to：Radio-frequency power 1150W, secondary air amount (Ar) 1.0L/min, nebulizer pressure 0.24MPa, wriggle
Pump pump speed 50r/min, height of observation 11.8mm, detection time 15s.
It is preferred that, in detection method the step A or B of above-mentioned digestion solution, the inductively coupled plasma atomic emissions
The analysis spectral line of spectroscopic methodology is：Cr 283.563nm, Ti 337.280nm, Al 396.152nm, Co 230.786nm, Cu
324.754nm, Fe 239.562nm, K 766.490nm, Mg 285.213nm, Mn 293.930nm, Na 589.592nm, Ni
231.604nm, P 178.284nm, Pb 220.353nm, Si 251.611nm, Sn 189.989nm, W 207.911nm, Zn
206.200nm, Zr 339.198nm.
The method that the present invention clears up vanadium chromium titanium alloy not only ensures Specimen eliminating entirely without residue, and element to be measured is all lossless
Lost territory enters detection solution and improves the measurement result degree of accuracy, and substantially reduces Check-Out Time and improve Product checking efficiency.
The Specimen eliminating preparation method of the vanadium chromium titanium alloy material of the present invention realize quick and completely by vanadium in ternary-alloy material,
Chromium, Titanium base Main elements and residual impurity element are cleared up and enter solution, solve the matrix components such as the Gao Ge of indissoluble, high titanium
And the rapid-digestion of the impurity composition such as silicon, tungsten, it is to avoid long-time High-temperature Digestion reacts and causes the elements such as arsenic impurities to be measured
The cohesion loss of the element such as volatile loss and silicon；And the reagent dosage of the ratio not only ensures the quick, complete of sample
Clear up, and reduce the influence that acidity effect is determined to further element as far as possible, while avoiding high titanium in Low acid medium
The problem of matrix is also easy to produce hydrolysis.Meanwhile, sample quality, dilution ratio for being optimized in Specimen eliminating preparation method etc. are anti-
Answer the Instrument working parameter optimized in condition and ICP-OES element determination methods, suitable sensitivity analysis spectral line, calibration mark
The testing conditions such as quasi- solution preparation, it is ensured that each element to be measured including secondary amounts alloying elements cr, Ti including higher concentration content
Detection signal intensity in the convenient horizontal extent of ICP-OES analysis methods, reached at the same meet determine secondary amounts close
The need for gold element and micro impurity element, substantially increase operating efficiency, shorten round of visits, eliminate spectra1 interfer- and
Reduce matrix effect influence.
Embodiment
The present invention is cleared up in the method for vanadium chromium titanium alloy, is usually avoided the samples such as high chromium matrix from producing passivation with nitric acid and is made
With and hinder this or delay to clear up proceeding for reaction, it is general main use clearing up instead for by main agents of hydrochloric acid progress sample
Should, but the present inventor's experiment finds that concentration ratio of the appropriate increase nitric acid in combination digestive reagent on the contrary can be more efficient
Ground destroys the crystal structure of V-Cr-Ti ternary alloy three-partalloys, is conducive to accelerating the speed that vanadium chromium titanium alloy sample is cleared up reaction by acid reagent
Sample preparation Element detection solution is cleared up in degree, guarantee quick and completely within a short period of time.Meanwhile, to ensure V-Cr-Ti samples
In secondary amounts matrix element titanium and the indissoluble such as silicon tungsten and easily condense or the element to be measured of hydrolysis can be by quick without loss
Clear up and enter solution, and avoid heavy dose from clearing up sample reagent influence further element and determine and corrosion instrument and equipment, the present invention
Digestion procedure using different digestive reagents and controls different reaction conditions to be divided into two reactions steps progress V-Cr- respectively
Ti ternary alloy samples matrix and the quick and complete of impurity element are cleared up, specifically：
First step, with the nitric acid of certain concentration ratio, hydrochloric acid and water (Yan Suan ︰ Xiao Suan ︰ water=2~︰ 2~3 of 3 ︰ 1；It is preferred that
HNO3︰ HCl ︰ H2The ︰ 2 of O=2 ︰ 1) mixed as digestive reagent with alloy sample, by primary sample in the case of ebuillition of heated
Grain is dissolved and carries out solution and vanish from sight, the only remaining a small amount of powdered sample residue in solution bottom, and in solution not
See that sample and acid reaction produce the minute bubbles caused by gas, the homogeneous atmosphere bubble only produced by boiling water, the step is by vanadium
Matrix, secondary amounts alloying element chromium matrix and most of impurity element are cleared up and enter solution；Second step, reduces and keeps matrix
Solution temperature promotes the indissolubles such as remnants secondary amounts alloying element Titanium base and silicon, tungsten to addition hydrofluoric acid under the conditions of 65~75 DEG C
Impurity element is cleared up completely enters solution.
The method have the advantages that first first step reaction is carried out under the conditions of solution boiling, to make by high temperature
Enter solution with post promoting most of sample to be resolved, be then just maintained under 65~75 DEG C of cryogenic conditions and hydrofluoric acid is situated between
Continue to react in matter, not only ensure that Gold Samples belong to the indissoluble such as titanium, silicon, tungsten material and effectively cleared up reaction completely, and keep away
Exempt from the impurity to be measured such as silicon under hot conditions to escape with the volatilization of ocratation form, and by the complexing of fluorine ion in hydrofluoric acid
Stabilization avoids silicon from generating the hydrolysis formation Precipitations such as orthosilicic acid, tungsten generation wolframic acid and influence the accurate of testing result
Reliability；Meanwhile, the hydrofluoric acid consumption of optimization ensure that the abundant complex reactions of sample element such as remaining fluorine ion and titanium, silicon, tungsten
Stable complex ion is formed, free hydrofluoric acid is greatly reduced to operating personnel and the corrosiveness of detecting instrument.With different
Digestive reagent and reaction condition points of 2 step sample introduction row vanadium alloy samples clear up preparations, and reagent dosage is small and is heated at high temperature
Decompose or evaporation removes portion of reagent, be simply and effectively reduced the factors such as reagent blank background, acidity effect to trace impurity
The interference of element determination.
In the following embodiments, the dense nitre that the mass percent concentration for having used top pure grade rank is 65%~68%
The hydrofluoric acid that concentrated hydrochloric acid that acid, mass percent concentration are 36%~38%, mass percent concentration are 40%~47%, water is
The distilled water of the two grades of water requirements in laboratory is met, and according to HNO3︰ HCl ︰ H2The ︰ 2 of O=2 ︰ 1 proportionate relationship mixed preparing sample
Combine digestive reagent；Equipment is：Match Mo Feishier company iCAP6300 type inductively coupled plasma atomic emission spectrometry instrument in the U.S.
(ICP-OES), but it is not limited to this.
Embodiment 1
The sample detection solution of vanadium chromium titanium alloy clears up preparation
0.2 vanadium chromium titanium alloy sample (No. 1 sample) is weighed, 30mL digestive reagents is added, is placed in ebuillition of heated on electric hot plate
Reaction to sample particle is dissolved only remaining a small amount of residue and solution produces homogeneous atmosphere bubble (first clears up step)；Reduce and protect
Solution temperature is held to 65~75 DEG C, 0.5mL hydrofluoric acid is added and clears up sample residue completely, solution is cooled to after room temperature to be diluted with water
Constant volume is well mixed (second clears up step) to be measured in 100mL volumetric flasks.
The content of secondary amounts alloying element and micro impurity element in solution is detected with ICP-OES determination samples
Using inductively coupled plasma atomic emissions spectrum (ICP-OES) as detection means, directly by prepared vanadium chromium
Titanium sample detection solution is imported in ICP-OES instruments, while 2.5%~5.5% secondary amounts alloying elements cr, Ti are determined, and
0.001%~0.25% micro impurity element Al, As, Co, Cu, Fe, Mg, Mn, Ni, P, Pb, Si, Sn, W, Zn, Zr and
0.005%~0.25% K, Na content.
ICP-OES determination steps are carried out in the usual way, and the ICP-OES parameter that predominantly detects is set to：Radio-frequency power
1150W, secondary air amount (Ar) 1.0L/min, nebulizer pressure 0.24MPa, peristaltic pump pump speed 50r/min, height of observation
11.8mm, detection time 15s.Element analysis spectrum line to be measured is：Cr 283.563nm, Ti 337.280nm, Al 396.152nm,
Co 230.786nm, Cu 324.754nm, Fe 239.562nm, K 766.490nm nm, Mg 285.213nm, Mn
293.930nm, Na589.592nm, Ni 231.604nm, P 178.284nm, Pb 220.353nm, Si 251.611nm, Sn
189.989nm, W 207.911nm, Zn 206.200nm, Zr 339.198nm.
Wherein, use using 1.84g/L vanadium standard liquid as vanadium Matrix Match bottom liquid, then add the mark of element to be measured
Quasi- solution be configured to impurity element concentration be respectively 0.00%, 0.001%, 0.002%, 0.005%, 0.010%, 0.100%,
0.250%, and secondary amounts alloying elements cr, Ti concentration are respectively 0.0%, 2.50%, 3.00%, 3.50%, 4.00%,
4.50%th, 5.50% is in concentration gradient, and with the sample solution matrix group of the vanadium chromium titanium ternary-alloy material such as V-4Cr-4Ti
Into 7 consistent series standard solution, ICP-OES instruments and drawing curve are calibrated with this.
Embodiment 2
0.3 vanadium chromium titanium alloy sample (No. 2 samples) is weighed, 45mL sample combinations digestive reagent is proportionally added into and carries out first
Step clears up reaction, then adds the reaction that disappears that 0.8mL hydrofluoric acid carries out second step, in addition, according to embodiment 1
Method identical method prepare the vanadium chromium titanium sample solution and secondary amounts alloying element and micro miscellaneous in solution determined with ICP-OES
The content of matter.
Embodiment 3
0.4 vanadium chromium titanium alloy sample (No. 3 samples) is weighed, 60mL sample combinations digestive reagent is proportionally added into and carries out first
Step clears up reaction, then adds the reaction that disappears that 1.0mL hydrofluoric acid carries out second step, in addition, according to embodiment 1
Method identical method prepare the vanadium chromium titanium sample solution and secondary amounts alloying element and micro miscellaneous in solution determined with ICP-OES
The content of matter.
Embodiment 4
0.2 chromium titanium alloy sample (No. 4 samples) is weighed, 30mL sample combinations digestive reagent is proportionally added into and carries out the first step
Rapid clears up reaction, then adds the reaction that disappears of 1.0mL hydrofluoric acid progress second step, in addition, according to embodiment 1
Method identical method prepares the vanadium chromium titanium sample solution and determines secondary amounts alloying element and trace impurity in solution with ICP-OES
Content.
The precision of embodiment 5 is assessed
Repetition carries out 8 independent sample solutions to embodiment 1 and embodiment 3 and clears up preparation and element determination respectively, right
Statistics calculates the average value and relative standard deviation (RSD) of 8 measurements, to assess the detection precision level of this method.As a result
It is shown in Table 1.
Table 1
Table 1 is visible, content in vanadium-titanium-chromium alloy sample>The RSD of the secondary amounts alloying element of 1% constant level<1%, content<
The RSD of the micro impurity element of 0.2% minor levels<10%, even below the contents level of method Monitoring lower-cut 0.001%
RSD shows that multiple measurement result is consistent again smaller than 15%, and repeatability, the repeatability of method are good, and method has higher precision
Degree level.
The rate of recovery of embodiment 6 is assessed
Recovery test has been carried out to No. 2 samples and No. 4 samples.Measured respectively by embodiment 2 and embodiment 4 first
The content of secondary amounts alloying element and micro impurity element in No. 2 samples and No. 4 samples；Then divide in No. 2 samples and No. 4 samples
The standard liquid of element to be measured is not added, and the sample detection solution for repeating embodiment 2 and embodiment 4 is prepared and element determination behaviour
Make.By calculate to the rate of recovery assessment to verify the present invention sample solution preparation method and its detection method it is accurate
Degree.It the results are shown in Table 2.
The recovery test of table 2
Table 2 is visible, and method determines content>1% alloying elements cr, the Ti rate of recovery 97%~102%, 1%~0.1%
The micro- rate of recovery 90%~110%, the rate of recovery of 0.1%~0.001% trace element shows also 80%~120%
Analysis result has higher accuracy and reliability.
Embodiment 7 is compareed with traditional chemical routes result
Secondary amounts alloying element in vanadium chromium titanium alloy material is determined using this method, its measurement result is respectively with using aluminium flake
Reduction-ferric ammonium sulfate titration measuring titanium amount, the traditional classical of ammonium persulfate oxidation-ferrous ammonium sulfate titration chromium content
Chemical analysis method compareed, to verify this method determine high content secondary amounts alloying element accuracy.As a result see
Table 3.
Table 3
Table 3 is visible, as a result compares basically identical, shows this method testing result accurately and reliably.
Claims (10)
1. clear up the method for vanadium chromium titanium alloy, it is characterised in that：Comprise the following steps：Hydrochloric acid, nitric acid and water are mixed and disappeared
Solve and digestive reagent is added in reagent, vanadium chromium titanium alloy, heating is boiled solution reaction and no longer reduced to solid；Then temperature is reduced extremely
Hydrofluoric acid is added after 65~75 DEG C, keeping temperature is reacted to remaining solid material and cleared up completely, cooling produces digestion solution.
2. the method according to claim 1 for clearing up vanadium chromium titanium alloy, it is characterised in that：Every 0.2~0.4g vanadium chromium titanium is closed
Gold adds 30~60mL digestive reagents；Further, 15mL digestive reagents are added per 0.1g vanadium chromium titanium alloy.
3. the method according to claim 1 for clearing up vanadium chromium titanium alloy, it is characterised in that：The preparation side of the digestive reagent
Method is：Count by volume, three is mixed and prepares digestive reagent by Yan Suan ︰ Xiao Suan ︰ water=2~︰ 2~3 of 3 ︰ 1；It is preferred that, salt
The Suan ︰ Xiao Suan ︰ water=︰ 2 of 2 ︰ 1.
4. the method according to claim 1 for clearing up vanadium chromium titanium alloy, it is characterised in that：The mass concentration of the nitric acid is
65~68%；The mass concentration of hydrochloric acid is 36~38%；The mass concentration of the hydrofluoric acid is 40~47%.
5. the method according to claim 1 for clearing up vanadium chromium titanium alloy, it is characterised in that：Every 0.2~0.4g vanadium chromium titanium is closed
Gold adds 0.5~1mL hydrofluoric acid.
6. the digestion solution that the method that vanadium chromium titanium alloy is cleared up as described in any one of Claims 1 to 5 is prepared.
7. the detection method of digestion solution, it is characterised in that：Comprise the following steps：
A, preparation standard curve：The standard liquid that element to be measured is added in vanadium standard liquid is configured to the solution of various concentrations,
Then the solution of variant concentration is detected using inductively coupled plasma atomic emission spectrometry, draws curve, obtain
To concentration-strength criterion curve of each metal；
B, same use inductively coupled plasma atomic emission spectrometry are examined to the digestion solution described in claim 6
Survey, obtain each metal ion intensity, concentration is drawn by corresponding concentration-strength criterion curve, content is finally drawn.
8. the detection method of digestion solution according to claim 7, it is characterised in that：In step A, as detection Cr or Ti
When, compound concentration scope is 2.5~5.5% various concentrations solution；When detection Al, As, Co, Cu, Fe, Mg, Mn, Ni, P, Pb,
When Si, Sn, W, Zn or Zr, compound concentration scope is 0.001%~0.25% various concentrations solution；When detecting K or Na, match somebody with somebody
Concentration range processed is 0.005%~0.25% various concentrations solution.
9. the detection method of digestion solution according to claim 7, it is characterised in that：In step A or B, the inductance coupling
Plasma atomic emission spectrometry parameter is closed to be set to：Radio-frequency power 1150W, secondary air amount 1.0L/min, atomizer pressure
Power 0.24MPa, peristaltic pump pump speed 50r/min, height of observation 11.8mm, detection time 15s.
10. the detection method of digestion solution according to claim 7, it is characterised in that：In A or B, described inductive etc.
The analysis spectral line of plasma-atomic emission spectroscopic methodology is：Cr 283.563nm, Ti 337.280nm, Al 396.152nm, Co
230.786nm, Cu 324.754nm, Fe 239.562nm, K 766.490nm, Mg 285.213nm, Mn 293.930nm, Na
589.592nm, Ni 231.604nm, P 178.284nm, Pb 220.353nm, Si 251.611nm, Sn 189.989nm, W
207.911nm, Zn 206.200nm, Zr 339.198nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710287873.9A CN107121426B (en) | 2017-04-27 | 2017-04-27 | Clear up the method for vanadium chromium titanium alloy and the detection method of digestion solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710287873.9A CN107121426B (en) | 2017-04-27 | 2017-04-27 | Clear up the method for vanadium chromium titanium alloy and the detection method of digestion solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107121426A true CN107121426A (en) | 2017-09-01 |
| CN107121426B CN107121426B (en) | 2019-12-03 |
Family
ID=59725361
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710287873.9A Active CN107121426B (en) | 2017-04-27 | 2017-04-27 | Clear up the method for vanadium chromium titanium alloy and the detection method of digestion solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107121426B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108344730A (en) * | 2018-02-07 | 2018-07-31 | 四川星明能源环保科技有限公司 | The assay method of trace impurity content in a kind of high-concentration sulfuric acid vanadyl solution |
| CN108693014A (en) * | 2018-03-22 | 2018-10-23 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of microwave digestion method and its elemental composition detection method of vanadium chromium titanium alloy material |
| CN110057810A (en) * | 2019-05-16 | 2019-07-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Clear up vanadium titanium blast furnace gas mud/ash method and detection method |
| CN111551541A (en) * | 2020-06-29 | 2020-08-18 | 攀钢集团研究院有限公司 | Method for detecting content of rare and noble elements in slag sample |
| CN111879845A (en) * | 2020-07-24 | 2020-11-03 | 宁波江丰电子材料股份有限公司 | Mixed acid for dissolving chromium-tantalum-titanium alloy and preparation method and application thereof |
| CN112432941A (en) * | 2020-10-29 | 2021-03-02 | 中化地质矿山总局地质研究院 | Method for measuring silicate content in salt lake brine |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101315316A (en) * | 2008-07-01 | 2008-12-03 | 攀钢集团研究院有限公司 | Digestion method and detection method of titanium-rich material |
| CN102928425A (en) * | 2012-10-31 | 2013-02-13 | 攀枝花钢城集团瑞钢工业有限公司 | Method for determining vanadium in silicon-vanadium alloy |
| CN103604800A (en) * | 2013-10-25 | 2014-02-26 | 中国航空工业集团公司北京航空材料研究院 | Analysis method for determining titanium, vanadium, tungsten, manganese and silicon in K25 chromium-base high temperature alloy |
| CN103616472A (en) * | 2013-12-09 | 2014-03-05 | 中国兵器工业第五二研究所 | Chemical analysis method for determination of zirconium content in alloy containing various interference elements |
| CN105548164A (en) * | 2015-12-25 | 2016-05-04 | 北京有色金属研究总院 | Measuring method for content of titanium in titanium silicon |
| CN105842021A (en) * | 2016-03-14 | 2016-08-10 | 攀钢集团研究院有限公司 | Method for determining contents of impurity elements in alloy, and preparation method for sample solution |
-
2017
- 2017-04-27 CN CN201710287873.9A patent/CN107121426B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101315316A (en) * | 2008-07-01 | 2008-12-03 | 攀钢集团研究院有限公司 | Digestion method and detection method of titanium-rich material |
| CN102928425A (en) * | 2012-10-31 | 2013-02-13 | 攀枝花钢城集团瑞钢工业有限公司 | Method for determining vanadium in silicon-vanadium alloy |
| CN103604800A (en) * | 2013-10-25 | 2014-02-26 | 中国航空工业集团公司北京航空材料研究院 | Analysis method for determining titanium, vanadium, tungsten, manganese and silicon in K25 chromium-base high temperature alloy |
| CN103616472A (en) * | 2013-12-09 | 2014-03-05 | 中国兵器工业第五二研究所 | Chemical analysis method for determination of zirconium content in alloy containing various interference elements |
| CN105548164A (en) * | 2015-12-25 | 2016-05-04 | 北京有色金属研究总院 | Measuring method for content of titanium in titanium silicon |
| CN105842021A (en) * | 2016-03-14 | 2016-08-10 | 攀钢集团研究院有限公司 | Method for determining contents of impurity elements in alloy, and preparation method for sample solution |
Non-Patent Citations (1)
| Title |
|---|
| 高颂 等: "电感耦合等离子体原子发射光谱法测定TG6钛合金中镁钒铬铁钴铜锰钼钨", 《冶金分析》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108344730A (en) * | 2018-02-07 | 2018-07-31 | 四川星明能源环保科技有限公司 | The assay method of trace impurity content in a kind of high-concentration sulfuric acid vanadyl solution |
| CN108693014A (en) * | 2018-03-22 | 2018-10-23 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of microwave digestion method and its elemental composition detection method of vanadium chromium titanium alloy material |
| CN110057810A (en) * | 2019-05-16 | 2019-07-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Clear up vanadium titanium blast furnace gas mud/ash method and detection method |
| CN111551541A (en) * | 2020-06-29 | 2020-08-18 | 攀钢集团研究院有限公司 | Method for detecting content of rare and noble elements in slag sample |
| CN111879845A (en) * | 2020-07-24 | 2020-11-03 | 宁波江丰电子材料股份有限公司 | Mixed acid for dissolving chromium-tantalum-titanium alloy and preparation method and application thereof |
| CN112432941A (en) * | 2020-10-29 | 2021-03-02 | 中化地质矿山总局地质研究院 | Method for measuring silicate content in salt lake brine |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107121426B (en) | 2019-12-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107121426B (en) | Clear up the method for vanadium chromium titanium alloy and the detection method of digestion solution | |
| CN105842021B (en) | Measure the method for impurity content and the preparation method of sample solution in alloy | |
| CN102965541B (en) | Ti80 titanium alloy standard substance and preparation method thereof | |
| CN103808558B (en) | The digestion procedure of vanadium nitrogen ferrotitanium hybrid alloys core-spun yarn and detection method | |
| CN106596518B (en) | The measuring method of zirconium and impurity content in a kind of uranium zircaloy | |
| CN101135617B (en) | Vanadium-nitrogen alloy resolution method | |
| CN101825530B (en) | Method for preparing titanium metal sample solution and detection method using same | |
| CN102565026A (en) | Method for determination of silicon content in ferro-aluminum manganese | |
| CN104807813A (en) | Rapid analysis method for content of manganese in ferromanganese iron | |
| CN108872203A (en) | The detection method of elemental composition in a kind of vanadium chromium slag and its digestion procedure and a kind of measurement vanadium chromium slag | |
| CN105842043B (en) | Measure the method and its sample digestion method of elemental composition in sulphur cobalt concentrate | |
| CN101315334A (en) | Method for measuring trace amount calcium in steel | |
| CN106770199A (en) | A kind of method that application ICP AES determine W content in molybdenum-iron | |
| CN102914534B (en) | Method for measuring calcium and magnesium in vanadium-nitrogen alloy | |
| CN108693014A (en) | A kind of microwave digestion method and its elemental composition detection method of vanadium chromium titanium alloy material | |
| CN110133025A (en) | The fusion preparation method of vanadium iron fuse piece | |
| CN107632011B (en) | Method for measuring content of impurity elements in high-purity bismuth | |
| CN109883810A (en) | The digestion procedure and detection method of titanium slag or vanadium slag | |
| CN102928271A (en) | Sample treatment method for measuring niobium, tungsten and zirconium in steel | |
| CN110361441B (en) | Method for detecting trace impurity elements in tungsten carbide powder | |
| CN111257097A (en) | Vanadium carbide sample to be tested manufacturing method and impurity content analysis method thereof | |
| CN102661991A (en) | Method for measuring content of acid-solvable boron in steel | |
| CN105738347B (en) | A kind of method of elemental lithium in measurement magnesium lithium alloy | |
| CN111272737B (en) | Method for measuring percentage content of multiple elements in high-silicon aluminum alloy by microwave digestion-ICP-OES and application thereof | |
| CN101526497B (en) | Method for preparing sample solution for detecting titanium tetrachloride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |