CN108627499A - A kind of assay method of Boron in Titanium Alloy content - Google Patents
A kind of assay method of Boron in Titanium Alloy content Download PDFInfo
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Abstract
The assay method of Boron in Titanium Alloy content disclosed by the invention, is specifically implemented according to the following steps：Step 1 sequentially adds titanium alloy sample and hydrochloric acid solution into beaker, and the hydrofluoric acid of~3 drop of 2 drop is added dropwise in heating, the first mixed liquor is obtained after titanium alloy sample is completely dissolved；Step 2, the salpeter solution that~4 drop of 3 drop is instilled into the first mixed liquor continue after heating 2min~4min, are cooled to room temperature, continue to sequentially add ethyl alcohol and yttrium standard solution into the first mixed liquor, obtain the second mixed liquor；Step 3 moves into the second mixed liquor in volumetric flask, it is diluted with water to graduation mark and shakes up, it obtains measuring liquid, measurement liquid is placed in inductive coupling plasma emission spectrograph and is measured, the spectral intensity of boron is detected, the quality of boron in titanium alloy sample is obtained in conjunction with boron standard curve, method is stable, accurate, quick, the introducing of organic reagent ethyl alcohol improves nebulization efficiency, improves sensitivity for analysis.
Description
Technical field
The invention belongs to the content analysis technical fields of titanium alloy, are related to a kind of assay method of Boron in Titanium Alloy content.
Background technology
Boron is added in alloy as boundary-strengthening element, and micro boron is added in alloy can purify crystal boundary, with
The objectionable impurities such as lead, arsenic form dystectic compound, reduce the defect of crystal boundary, make diffusion velocity of the alloying element on crystal boundary
It reduces, to improve alloy property.At present mainly using inductively coupled plasma atomic emission spectrometry to micro- in titanium alloy
The content of amount B is measured, but in continuous mode, the selection meeting pair of analytical line, the time of integration, evanescent voltage and molten sample acid etc.
Measurement result has a huge impact, it is therefore necessary to establish accurately and reliably analysis method.
Invention content
The object of the present invention is to provide a kind of assay methods of Boron in Titanium Alloy content so that the measurement result of the content of boron
It is more accurate.
The technical solution adopted in the present invention is a kind of assay method of Boron in Titanium Alloy content, specifically according to following step
It is rapid to implement：
Step 1 sequentially adds titanium alloy sample and hydrochloric acid solution into beaker, and the hydrogen fluorine of~3 drop of 2 drop is added dropwise in heating
Acid obtains the first mixed liquor after titanium alloy sample is completely dissolved；
Step 2, the salpeter solution that~4 drop of 3 drop is instilled into the first mixed liquor continue after heating 2min~4min, cooling
To room temperature, continues to sequentially add ethyl alcohol and yttrium standard solution into the first mixed liquor, obtain the second mixed liquor；
Step 3 moves into the second mixed liquor in the volumetric flask of 100ml, is diluted with water to graduation mark and shakes up, is measured
Measurement liquid is placed in inductive coupling plasma emission spectrograph and is measured, detects the spectral intensity of boron by liquid, in conjunction with
Boron standard curve obtains the quality of boron in titanium alloy sample.
The features of the present invention also characterized in that：
In step 1, the density of the hydrochloric acid solution is 1.19g/ml, and additive amount is 13ml~16ml.
In step 1, heating temperature is 80 DEG C~100 DEG C.
In step 1, the beaker is polytetrafluoroethylene beaker.
In step 2, the density of salpeter solution is 1.42g/ml.
In step 2, the additive amount of the ethyl alcohol is 3ml~4ml.
In step 2, a concentration of 0.2mg/ml of yttrium standard solution, additive amount is 1ml~4ml.
In step 2, the heating temperature is 60 DEG C~80 DEG C.
In step 3, in the operating condition of the inductive coupling plasma emission spectrograph, analysis spectral line is
249.773nm, time of integration 2s, evanescent voltage 700V.
The beneficial effects of the invention are as follows：
The assay method of the Boron in Titanium Alloy content of the present invention, by analysis spectral line, evanescent voltage, product in operating condition
Between timesharing and the screening of molten sample acid etc., it ensure that and do not interfered by other spectral lines in continuous mode, and the intensity of spectral line is moderate, salt
Acid plus hydrofluoric acid make sample solution rate faster, and assay method through the invention measures trace B in titanium alloy, passes through standard
Exactness, precision and rate of recovery experiment, the experiment of sample analysis result, relative standard deviation are less than 5%, method is stable, it is accurate,
Quickly, the introducing of organic reagent ethyl alcohol improves nebulization efficiency, reduces surface tension, improves sensitivity for analysis.
Specific implementation mode
The present invention is described in detail With reference to embodiment.
A kind of assay method of Boron in Titanium Alloy content of the present invention, is specifically implemented according to the following steps：
Step 1 sequentially adds titanium alloy sample and hydrochloric acid solution into beaker, and the hydrogen fluorine of~3 drop of 2 drop is added dropwise in heating
Acid obtains the first mixed liquor after titanium alloy sample is completely dissolved；
Wherein, beaker is polytetrafluoroethylene beaker；The density of hydrochloric acid solution is 1.19g/ml (1+1 hydrochloric acid), and additive amount is
13ml~16ml；Heating temperature is 80 DEG C~100 DEG C.
Step 2, the salpeter solution that~4 drop of 3 drop is instilled into the first mixed liquor continue after heating 2min~4min, cooling
To room temperature, continues to sequentially add ethyl alcohol and yttrium standard solution into the first mixed liquor, obtain the second mixed liquor；
Wherein, the density of salpeter solution is 1.42g/ml (1+1 nitric acid)；Heating temperature is 60 DEG C~80 DEG C；Ethyl alcohol adds
Dosage is 3ml~4ml；A concentration of 0.2mg/ml of yttrium standard solution, additive amount are 1ml~4ml.
Step 3 moves into the second mixed liquor in the plastics volumetric flask of 100ml, is diluted with water to graduation mark and shakes up, obtains
Liquid is measured, measurement liquid is placed in inductive coupling plasma emission spectrograph and is measured, detects the spectral intensity of boron, then
The quality of boron in titanium alloy sample is obtained in conjunction with boron standard curve.
Wherein, the JY70C type inductive couplings etc. of JY companies of inductive coupling plasma emission spectrograph selection France production
Ionomer emission spectrum instrument, in operating condition, analysis spectral line 249.773nm, time of integration 2s, evanescent voltage 700V；
Other operating conditions are：Radio-frequency signal generator frequency is 40.68MHz, and solution elevating amount is 1.5ml/min, power 1KW, cooling
Throughput is 12L/min, and grating is holography 4320gr/mm, and sheath throughput is 0.3L/min, and slit is 20/25 μm, carrier gas stream
Amount is 0.4L/min, and focal length 1.0m, observed altitude is 15mm above induction coil.
The drafting of boron standard curve：
1) high standard solution
0.1 gram of pure titanium valve number part is weighed, boron standard solution (0.01mg/ml) 2ml, 4ml, 6ml, 8ml, 10ml is added,
It also can be used in real work and add boron standard solution as high standard with trade mark mark steel.
2) low mark solution
Blank reagent solution, in addition to being not added with boron standard liquid, step measures its spectral intensity according to the above analysis.
Step carries out the measurement of the boron spectral intensity under different content boron according to the above analysis, draws out the quality and light of boron
The standard curve of spectral intensity；
The selection of the operating condition of inductive coupling plasma emission spectrograph：
1) selection of analytical line
Al6%, Mo5%, V1.5%, Zr2%, Fe0.1%, B0.05% is added in 0.1 gram of pure titanium, passes through spectral line wheel
Wide scanning carries out 4 analytical lines 249.773,249.678,208.959,208.893 of the matrix element with coexistence elements to boron
Interference research, in terms of the disturbed condition of spectral line, matrix titanium and element al coexists, the analytical line of Mo, V, Zr, Fe will be with boron
Analytical line can be separated preferably, and B249.678nm and B249.773nm is selected to carry out the measurement of titanium alloy B content as analytical line.
The present invention selects 249.773nm for analytical line.
2) selection of the time of integration
It is respectively 0.5s, 1s, 2s in the time of integration with 0.05mg boron standard solution, 3s, 4s, 5s, 10s are tested, real
It tests and shows the time of integration in 2s, the spectral intensity of boron is most strong.
3) selection of evanescent voltage
It is listed in table 1 in evanescent voltage with 0.05mg boron standard solution, as can be seen from Table 1, when evanescent voltage is 725V, spectrum
Line maximum intensity.But evanescent voltage cannot be too big, it can influence the service life of power tube, so 700V voltages are selected in this method,
The intensity of spectral line is not also weak, does not influence the accuracy measured.
Influence of the 1 differential declines voltage of table to boron the intensity of spectral line
| Evanescent voltage | 600 | 625 | 650 | 680 | 700 | 725 | 750 |
| The intensity of spectral line | 58.16 | 68.144 | 108.08 | 154.19 | 204.30 | 244.73 | 5.19 |
4) selection of molten sample acid
Sulfuric acid (1+1), hydrochloric acid (1+1) plus hydrofluoric acid dissolution sample, sulfuric acid (1+1) is selected to hold sample survey 0.05mg boron and obtain respectively
It is 68.114 to the intensity of spectral line, our experiments show that, sulfuric acid (1+1) weakens the intensity value of boron, and hydrochloric acid (1+1) adds hydrofluoric acid dissolution
Sample is fast, and the intensity value than sulfuric acid (1+1) is higher by very much, and sensitivity improves, so selection hydrochloric acid (1+1) plus hydrofluoric acid dissolution examination
Sample.
5) interference experiment of matrix
The boron standard solution that configuration two is 0.05mg, one plus Titanium base, another is not added with, under the same test conditions
It measures, the two difference is larger, therefore to eliminate matrix effect, and the standard series of drawing curve all carries out Matrix Match.
6) influence of organic reagent ethyl alcohol
Influence of the ethyl alcohol additive amount to spectral intensity, is shown in Table 2
Influence of 2 ethyl alcohol of table to boron intensity value
| Amount of alcohol added | 1 | 2 | 3 | 4 |
| Intensity value (I) | 231.87 | 266.33 | 268.77 | 319.64 |
As can be seen from Table 2, with the continuous increase of organic reagent amount of alcohol, the intensity of spectral line is continuously increased, because ethyl alcohol is dense
Degree, which increases, causes test solution viscosity to increase, and surface tension and density gradually reduce, and improve sample rate, and nebulization efficiency obviously increases
Add, so that the intensity of spectral line of boron is increased, improve sensitivity for analysis, but ethyl alcohol is excessive, plasma will be extinguished, 4ml is added in ethyl alcohol
It is advisable.
7) influence of internal standard element
The working conditions such as the optical system and electronic system of ICP-AES instruments occur minor change or test the acid of solution
Degree, viscosity, matrix element concentration difference can cause the variation of analytical element intensity, the addition of internal standard element that can efficiently reduce
With this spectra1 interfer- of elimination, when internal standard element not being added, experimental data fluctuation is slightly larger, after yttrium is added as internal standard, method essence
Degree increases.
Embodiment 1
Step 1 sequentially adds 0.1000g titanium alloys sample and 13ml hydrochloric acid (1+1) into beaker, in 80 DEG C of following heating
The hydrofluoric acid of~3 drop of 2 drop is added dropwise in side, and the first mixed liquor is obtained after titanium alloy sample is completely dissolved；
Step 2, the nitric acid (1+1) that~4 drop of 3 drop is instilled into the first mixed liquor continue to heat at being 60 DEG C in temperature
It after 2min, is cooled to room temperature, continues to sequentially add 3ml ethyl alcohol into the first mixed liquor and the yttrium standard of a concentration of 0.2mg/ml is molten
Liquid 1ml obtains the second mixed liquor；
Step 3 moves into the second mixed liquor in the plastics volumetric flask of 100ml, is diluted with water to graduation mark and shakes up, obtains
Liquid is measured, measurement liquid is placed in inductive coupling plasma emission spectrograph and is measured, detects the spectral intensity of boron, then
The quality of boron in titanium alloy sample is obtained in conjunction with boron standard curve.
Wherein, the JY70C type inductive couplings etc. of JY companies of inductive coupling plasma emission spectrograph selection France production
Ionomer emission spectrum instrument, in operating condition, analysis spectral line 249.773nm, time of integration 2s, evanescent voltage 700V；
Other operating conditions are：Radio-frequency signal generator frequency is 40.68MHz, and solution elevating amount is 1.5ml/min, power 1KW, cooling
Throughput is 12L/min, and grating is holography 4320gr/mm, and sheath throughput is 0.3L/min, and slit is 20/25 μm, carrier gas stream
Amount is 0.4L/min, and focal length 1.0m, observed altitude is 15mm above induction coil.
Embodiment 2
Step 1 sequentially adds 0.0940g titanium alloys sample and 14ml hydrochloric acid (1+1) into beaker, in 80 DEG C of following heating
The hydrofluoric acid of~3 drop of 2 drop is added dropwise in side, and the first mixed liquor is obtained after titanium alloy sample is completely dissolved；
Step 2, the nitric acid (1+1) that~4 drop of 3 drop is instilled into the first mixed liquor continue to heat at being 60 DEG C in temperature
It after 2min, is cooled to room temperature, continues to sequentially add 3.5ml ethyl alcohol and the yttrium standard of a concentration of 0.2mg/ml into the first mixed liquor
Solution 2ml obtains the second mixed liquor；
Step 3 moves into the second mixed liquor in the plastics volumetric flask of 100ml, is diluted with water to graduation mark and shakes up, obtains
Liquid is measured, measurement liquid is placed in inductive coupling plasma emission spectrograph and is measured, is calculated by boron standard curve
The quality of boron in titanium alloy sample；The operating condition of inductive coupling plasma emission spectrograph is the same as embodiment 1.
Embodiment 3
Step 1 sequentially adds 0.1500g titanium alloys sample and 15ml hydrochloric acid (1+1) into beaker, in 85 DEG C of following heating
The hydrofluoric acid of~3 drop of 2 drop is added dropwise in side, and the first mixed liquor is obtained after titanium alloy sample is completely dissolved；
Step 2, the nitric acid (1+1) that~4 drop of 3 drop is instilled into the first mixed liquor continue to heat at being 65 DEG C in temperature
It after 3min, is cooled to room temperature, continues to sequentially add 3.7ml ethyl alcohol and the yttrium standard of a concentration of 0.2mg/ml into the first mixed liquor
Solution 3ml obtains the second mixed liquor；
Step 3 moves into the second mixed liquor in the plastics volumetric flask of 100ml, is diluted with water to graduation mark and shakes up, obtains
Liquid is measured, measurement liquid is placed in inductive coupling plasma emission spectrograph and is measured, is calculated by boron standard curve
The quality of boron in titanium alloy sample；The operating condition of inductive coupling plasma emission spectrograph is the same as embodiment 1.
Embodiment 4
Step 1 sequentially adds 0.2000g titanium alloys sample and 15ml hydrochloric acid (1+1) into beaker, in 90 DEG C of following heating
The hydrofluoric acid of~3 drop of 2 drop is added dropwise in side, and the first mixed liquor is obtained after titanium alloy sample is completely dissolved；
Step 2, the nitric acid (1+1) that~4 drop of 3 drop is instilled into the first mixed liquor continue to heat at being 70 DEG C in temperature
It after 3min, is cooled to room temperature, continues to sequentially add 4ml ethyl alcohol into the first mixed liquor and the yttrium standard of a concentration of 0.2mg/ml is molten
Liquid 4ml obtains the second mixed liquor；
Step 3 moves into the second mixed liquor in the plastics volumetric flask of 100ml, is diluted with water to graduation mark and shakes up, obtains
Liquid is measured, measurement liquid is placed in inductive coupling plasma emission spectrograph and is measured, is calculated by boron standard curve
The quality of boron in titanium alloy sample；The operating condition of inductive coupling plasma emission spectrograph is the same as embodiment 1
Embodiment 5
Step 1 sequentially adds 0.2500g titanium alloys sample and 16ml hydrochloric acid (1+1) into beaker, in 90 DEG C of following heating
The hydrofluoric acid of~3 drop of 2 drop is added dropwise in side, and the first mixed liquor is obtained after titanium alloy sample is completely dissolved；
Step 2, the nitric acid (1+1) that~4 drop of 3 drop is instilled into the first mixed liquor continue to heat at being 70 DEG C in temperature
It after 4min, is cooled to room temperature, continues to sequentially add 4ml ethyl alcohol into the first mixed liquor and the yttrium standard of a concentration of 0.2mg/ml is molten
Liquid 4ml obtains the second mixed liquor；
Step 3 moves into the second mixed liquor in the plastics volumetric flask of 100ml, is diluted with water to graduation mark and shakes up, obtains
Liquid is measured, measurement liquid is placed in inductive coupling plasma emission spectrograph and is measured, is calculated by boron standard curve
The quality of boron in titanium alloy sample；The operating condition of inductive coupling plasma emission spectrograph is the same as embodiment 1.
The Specimen Determination of Examples 1 to 5 the results are shown in Table 3
The Specimen Determination result of 3 Examples 1 to 5 of table
| Embodiment | Measured value (%) | Average value (%) | RSD (%) |
| 1 | 0.0490 0.0510 0.0498 | 0.0499 | 1.49 |
| 2 | 0.0309 0.0291 0.0310 | 0.0303 | 1.61 |
| 3 | 0.0508 0.0505 0.0491 | 0.0501 | 2.15 |
| 4 | 0.0610 0.0596 0.0591 | 0.0587 | 1.76 |
| 5 | 0.0607 0.0625 0.0597 | 0.0610 | 3.15 |
The assay method of the Boron in Titanium Alloy content of the present invention, by analysis spectral line, evanescent voltage, product in operating condition
Between timesharing and the screening of molten sample acid etc., it ensure that and do not interfered by other spectral lines in continuous mode, and the intensity of spectral line is moderate, salt
Acid plus hydrofluoric acid make sample solution rate faster, and assay method through the invention measures trace B in titanium alloy, passes through standard
Exactness, precision and rate of recovery experiment, the experiment of sample analysis result, relative standard deviation are less than 5%, method is stable, it is accurate,
Quickly, the introducing of organic reagent ethyl alcohol improves nebulization efficiency, reduces surface tension, improves sensitivity for analysis.
Claims (9)
1. a kind of assay method of Boron in Titanium Alloy content, which is characterized in that be specifically implemented according to the following steps：
Step 1 sequentially adds titanium alloy sample and hydrochloric acid solution into beaker, and the hydrofluoric acid of~3 drop of 2 drop is added dropwise in heating,
The first mixed liquor is obtained after titanium alloy sample is completely dissolved；
Step 2, the salpeter solution that~4 drop of 3 drop is instilled into the first mixed liquor continue after heating 2min~4min, are cooled to room
Temperature continues to sequentially add ethyl alcohol and yttrium standard solution into the first mixed liquor, obtains the second mixed liquor；
Step 3 moves into the second mixed liquor in the volumetric flask of 100ml, is diluted with water to graduation mark and shakes up, and obtains measuring liquid,
Measurement liquid is placed in inductive coupling plasma emission spectrograph and is measured, the spectral intensity of boron is detected, in conjunction with boron
Standard curve obtains the quality of boron in titanium alloy sample.
2. a kind of assay method of Boron in Titanium Alloy content as described in claim 1, which is characterized in that in step 1, the salt
The density of acid solution is 1.19g/ml, and additive amount is 13ml~16ml.
3. a kind of assay method of Boron in Titanium Alloy content as described in claim 1, which is characterized in that in step 1, heating temperature
Degree is 80 DEG C~100 DEG C.
4. a kind of assay method of Boron in Titanium Alloy content as described in claim 1, which is characterized in that in step 1, the burning
Cup is polytetrafluoroethylene beaker.
5. a kind of assay method of Boron in Titanium Alloy content as described in claim 1, which is characterized in that in step 2, nitric acid is molten
The density of liquid is 1.42g/ml.
6. a kind of assay method of Boron in Titanium Alloy content as described in claim 1, which is characterized in that in step 2, the second
The additive amount of alcohol is 3ml~4ml.
7. a kind of assay method of Boron in Titanium Alloy content as described in claim 1, which is characterized in that in step 2, yttrium standard
A concentration of 0.2mg/ml of solution, additive amount are 1ml~4ml.
8. a kind of assay method of Boron in Titanium Alloy content as described in claim 1, which is characterized in that described to add in step 2
Hot temperature is 60 DEG C~80 DEG C.
9. a kind of assay method of Boron in Titanium Alloy content as described in claim 1, which is characterized in that in step 3, the electricity
In the operating condition for feeling coupled plasma optical emission spectrometer, analysis spectral line 249.773nm, time of integration 2s, decaying electricity
Pressure is 700V.
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Application publication date: 20181009 |