CN108872196A - A method of measurement Titanium In Aluminum Alloy and boron content - Google Patents
A method of measurement Titanium In Aluminum Alloy and boron content Download PDFInfo
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- CN108872196A CN108872196A CN201810554754.XA CN201810554754A CN108872196A CN 108872196 A CN108872196 A CN 108872196A CN 201810554754 A CN201810554754 A CN 201810554754A CN 108872196 A CN108872196 A CN 108872196A
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- 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
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/68—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using high frequency electric fields
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Abstract
The invention discloses a kind of methods for measuring Titanium In Aluminum Alloy and boron content, and specific step is as follows：Aluminum alloy specimen is weighed first to be put into triangular flask, hydrochloric acid is added into sample to complete reaction, obtain mixed liquor a, then hydrogenperoxide steam generator is added dropwise to mixed liquor a kind, continue to be heated to the transparent no residue shape of solution, is moved into volumetric flask after cooling, be diluted with water to scale, it shakes up, obtains prepare liquid；Finally prepare liquid is placed in inductive coupling plasma emission spectrograph and is measured；A kind of method for measuring Titanium In Aluminum Alloy and boron content of the present invention, pass through the screening to analysis spectral line in operating condition, it ensure that in continuous mode not by the interference of other spectral lines, make solution rate faster by the way that sodium hydroxide is added dropwise, this method has measurement result accurate, reliable, detection process is quick, can reach energy-efficient feature.
Description
Technical field
The invention belongs to analyzing detecting method technical fields, and in particular to a kind of measurement Titanium In Aluminum Alloy and boron content
Method.
Background technique
Al-Ti-B alloy is a kind of grain refiner that aluminium product must add in the process, the aluminium titanium of China's independent research
Boron alloy has captured domestic market comprehensively, and has had already turned on international market, and present China has become maximum in the world
Al-Ti-B alloy producing country.The key index of Al-Ti-B alloy depends on the content of the alloying elements such as titanium boron in alloy, is producing
Stringent control must be carried out in the process, but since the time of Al-Ti-B alloy research and development is not grown, corresponding analyzing detecting method
Research keeps up with the paces of production not yet, therefore research and development are able to satisfy the analyzing detecting method that production control requires and become when business
It is anxious.
Summary of the invention
The object of the present invention is to provide a kind of methods for measuring Titanium In Aluminum Alloy and boron content, provide a kind of Gao Ling
The Titanium In Aluminum Alloy of sensitivity and the measuring method of boron content.
The technical scheme adopted by the invention is that a method of measurement Titanium In Aluminum Alloy and boron content are specifically pressed
Implement according to following steps：
Step 1 weighs aluminum alloy specimen and is put into triangular flask, and hydrochloric acid is added into sample to complete reaction, is mixed
Liquid a；
Hydrogenperoxide steam generator is added dropwise to mixed liquor a kind in step 2, continues to be heated to the transparent no residue shape of solution, after cooling
It moves into volumetric flask, is diluted with water to scale, shakes up, obtain prepare liquid；
Prepare liquid is placed in inductive coupling plasma emission spectrograph and is measured by step 3, detects titanium and boron
Spectral intensity obtains the content of titanium and boron in titanium alloy sample in conjunction with titanium and boron standard curve.
The features of the present invention also characterized in that
The amount of aluminum alloy specimen is 0.1~0.2g in step 1 in step 1, and triangular flask is the triangular flask of 100ml.
The concentration of hydrochloric acid solution is 5.85mol/L in step 1, and the additive amount of hydrochloric acid solution is 25ml~30ml.
The concentration of hydrogenperoxide steam generator is 10mol/L in step 2, and the additive amount of hydrogenperoxide steam generator is 6~7 drops.
The volumetric flask that volumetric flask in step 2 is 100ml.
Heating temperature in step 2 is 150 DEG C~300 DEG C.
In the operating condition of the inductive coupling plasma emission spectrograph of step 3, the analysis spectral line of titanium is
334.940nm, the analysis spectral line of boron are 249.677nm.
The beneficial effects of the invention are as follows:A kind of method for measuring Titanium In Aluminum Alloy and boron content of the present invention, by right
The screening of analysis spectral line in operating condition ensure that not by the interference of other spectral lines in continuous mode, by the way that hydroxide is added dropwise
Sodium makes solution rate faster, while the present invention is to be not added target solid etalon substance Y34 as the blank solution of boron；This method
Accurate with measurement result, reliable, detection process is quick, can reach energy-efficient feature.
Specific embodiment
The present invention is described in detail With reference to embodiment.A kind of measurement Titanium In Aluminum Alloy of the present invention and boron
The method of constituent content, is specifically implemented according to the following steps：
Step 1 weighs 0.1~0.2g of aluminum alloy specimen and is put into 100ml triangular flask, and hydrochloric acid is added into sample to complete
Reaction, obtains mixed liquor a；
Wherein the concentration of hydrochloric acid solution is 5.85mol/L, and the additive amount of hydrochloric acid solution is 25ml~30ml；
Hydrogenperoxide steam generator is added dropwise to the mixed liquor a kind in step 2, continues to be heated to the transparent no residue shape of solution, cold
But it moves into afterwards in the volumetric flask of 100ml, is diluted with water to scale, shakes up, obtain prepare liquid；
Wherein the concentration of hydrogenperoxide steam generator is 10mol/L, and additive amount is 6~7 drops, and heating temperature is 150 DEG C~300
℃。
Prepare liquid is placed in inductive coupling plasma emission spectrograph and is measured by step 3, detects titanium and boron
Emitted luminescence intensity obtains the content of titanium and boron in titanium alloy sample in conjunction with titanium and boron standard curve；Inductively coupled plasma body
In the operating condition of emission spectrometer, the analysis spectral line of titanium is 334.940nm, and the analysis spectral line of boron is 249.677nm.
The specific choice process of the analysis parameter of measuring method of the invention is as follows：
1) selection of blank solution
Method one：A high-purity aluminium (purity 99.995%) 0.0859g is weighed in the triangular flask of 100ml, is added (1+1)
Hydrochloric acid 25ml, cap upper surface ware are placed on low-temperature furnace slow heating dissolution, and cooling constant volume is in the measuring bottle of 100ml after dissolving completely
In, it shakes up, measures the analytical line intensity of titanium and boron；
Method two：The hydrochloric acid solution of 25ml (1+1) is directly added into an empty volumetric flask, constant volume measures titanium after shaking up
With the analytical line intensity of boron；
Method three：Aluminium alloy solid etalon substance Y34 0.100g is weighed, is placed in 100ml triangular flask, 25ml salt is added
Acid is complete to sample vigorous reaction, is placed on high-temperature electric resistance furnace and is heated to sample dissolution completely, and 7 drop hydrogenperoxide steam generators are added,
Continue to be heated to the transparent no residue shape of solution, is moved into the volumetric flask of 100ml after cooling, scale is diluted with water to, after shaking up
Measure the intensity of the analytical line of titanium and boron.
Three of the above method measurement titanium and boron intensity value are shown in Table 1.By table 1 compares：The blank solution of titanium and boron is equal
Method one can be used, but because fine aluminium dissolves especially slowly in hydrochloric acid solution, greatly reduce production efficiency；Therefore, titanium
Blank solution can be selected method two, i.e. blank reagent solution, and the blank solution selecting method three of boron；
1 titanium of table and boron intensity value
| Element and wavelength (nm) | Method 1. intensity | Method 2. intensity | Method 3. intensity |
| Ti 334.940 | 3858.3 | 3838.4 | 78710.7 |
| Ti 336.121 | 1713.8 | 1681.7 | 42591.7 |
| Ti 337.279 | 3150.3 | 3237.5 | 63383.1 |
| B 249.677 | 1776.7 | 11260.3 | 1010.6 |
| B 249.772 | 3177.8 | 20983.2 | 3299.0 |
| B 208.889 | 39.5 | 234.5 | 22.1 |
2) selection of standard curve serial solution preparation
According to the approximate composition range Cu of this material TiB2-7050:2.0~2.6, Mg1.9~2.6, TiB2:4~6, Zn:
5.9~7.1, Zr:0.08~0.15；
Method one：It selects high-purity aluminium (purity 99.995%), weighs 0.085g, prepared according to the method for step 1- step 3
Test solution；Fine aluminium dissolves especially slowly in hydrochloric acid solution, need to be the dissolution of heating cover surface plate 2 hours or more on low-temperature furnace；Add
Enter titanium, the amount of boron standard liquid is shown in Table 2, be prepared into standard curve serial solution.
Method two:Two parts of 0.100g of solid etalon substance Y34 are weighed, test solution is prepared by the method for step 1- step 3, adds
Enter titanium, the amount of boron standard liquid is shown in Table 2, be prepared into standard curve serial solution.
The amount of titanium, boron standard liquid is added in table 2
Standard curve is made using two methods during the application, is mutually measured the content and reality of respective titanium and boron
The content of the titanium and boron in sample TiB2-7050 is produced, sample measurement result should meet Ti：68.9%, B:31.1%；I.e. titanium with
The mass ratio of boron is approximately equal to 2.2 ratio.
A kind of method for measuring Titanium In Aluminum Alloy and boron content of the present invention, by analysis spectral line in operating condition,
The screening of evanescent voltage and the time of integration etc. ensure that in continuous mode not by the interference of other spectral lines, passes through and hydrogen-oxygen is added dropwise
Change sodium and make solution rate faster, while the present invention is molten using the blank that target aluminium alloy solid etalon substance Y34 as boron is not added
Liquid；This method has measurement result accurate, reliable, and detection process is quick, can reach energy-efficient feature.
Embodiment 1
Step 1 weighs aluminum alloy specimen 0.1 (being accurate to 0.0001g) and is put into 100ml triangular flask, is added into sample
25ml hydrochloric acid (1+1) obtains mixed liquor a to complete reaction；
Step 2 is added dropwise hydrogenperoxide steam generator 6 to the mixed liquor a kind and drips, and continues to be heated to 150 ° to make the transparent nothing of solution
Residue shape moves into the volumetric flask of 100ml after cooling, is diluted with water to scale, shakes up, obtain prepare liquid；
Prepare liquid is placed in inductive coupling plasma emission spectrograph and is measured by step 3, detects titanium and boron
Emitted luminescence intensity obtains the content of titanium and boron in titanium alloy sample in conjunction with titanium and boron standard curve；The wherein analysis spectral line of titanium
For 334.940nm, the analysis spectral line of boron is 249.677nm.
The results are shown in Table 3 for the assay of titanium and boron in embodiment 1 in sample TiB2-7050, as shown in Table 3, adopts
TiB2-7050 aluminium alloy is measured with this method, the titanium of measurement and the relative standard deviation RSD of boron content are respectively less than 6%,
Measurement result is consistent with asserting value, this illustrates this method veracity and precision with higher.
The assay result of titanium and boron in 3 embodiment of table, 1 sample TiB2-7050
Embodiment 2
1. a kind of method for measuring Titanium In Aluminum Alloy and boron content, which is characterized in that specifically real according to the following steps
It applies：
Step 1 weighs aluminum alloy specimen 0.15 and is put into 100ml triangular flask, and 26ml hydrochloric acid (1+1) is added extremely into sample
Reaction completely, obtains mixed liquor a；
Step 2 is added dropwise hydrogenperoxide steam generator 6 to the mixed liquor a kind and drips, and continues to be heated to 150 ° to make the transparent nothing of solution
Residue shape moves into the volumetric flask of 100ml after cooling, is diluted with water to scale, shakes up, obtain prepare liquid；
Prepare liquid is placed in inductive coupling plasma emission spectrograph and is measured by step 3, detects titanium and boron
Emitted luminescence intensity obtains the content of titanium and boron in titanium alloy sample in conjunction with titanium and boron standard curve；Inductively coupled plasma body
In the operating condition of emission spectrometer, the analysis spectral line of titanium is 334.940nm, and the analysis spectral line of boron is 249.677nm.
The results are shown in Table 4 for the assay of titanium and boron in embodiment 2 in sample TiB2-7050, as shown in Table 4, should
Method veracity and precision with higher.
The assay result of titanium and boron in 4 embodiment 2 of table in sample TiB2-7050
Embodiment 3
Step 1 weighs aluminum alloy specimen 0.16 and is put into 100ml triangular flask, and 27ml hydrochloric acid (1+1) is added extremely into sample
Reaction completely, obtains mixed liquor a；
Step 2 is added dropwise hydrogenperoxide steam generator 7 to the mixed liquor a kind and drips, and continues to be heated to 160 ° to make the transparent nothing of solution
Residue shape moves into the volumetric flask of 100ml after cooling, is diluted with water to scale, shakes up, obtain prepare liquid；
Prepare liquid is placed in inductive coupling plasma emission spectrograph and is measured by step 3, detects titanium and boron
Emitted luminescence intensity obtains the content of titanium and boron in titanium alloy sample in conjunction with titanium and boron standard curve；Inductively coupled plasma body
In the operating condition of emission spectrometer, the analysis spectral line of titanium is 334.940nm, and the analysis spectral line of boron is 249.677nm.
The results are shown in Table 5 for the assay of titanium and boron in embodiment 3 in sample TiB2-7050, as shown in Table 5, should
Method veracity and precision with higher.
The assay result of titanium and boron in 5 embodiment 3 of table in sample TiB2-7050
Embodiment 4
1. a kind of method for measuring Titanium In Aluminum Alloy and boron content, which is characterized in that specifically real according to the following steps
It applies：
Step 1 weighs aluminum alloy specimen 0.18 and is put into 100ml triangular flask, and 28ml hydrochloric acid (1+1) is added extremely into sample
Reaction completely, obtains mixed liquor a；
Step 2 is added dropwise hydrogenperoxide steam generator 6 to the mixed liquor a kind and drips, and continues to be heated to 180 ° to make the transparent nothing of solution
Residue shape moves into the volumetric flask of 100ml after cooling, is diluted with water to scale, shakes up, obtain prepare liquid；
Prepare liquid is placed in inductive coupling plasma emission spectrograph and is measured by step 3, detects titanium and boron
Emitted luminescence intensity obtains the content of titanium and boron in titanium alloy sample in conjunction with titanium and boron standard curve；Inductively coupled plasma body
In the operating condition of emission spectrometer, the analysis spectral line of titanium is 334.940nm, and the analysis spectral line of boron is 249.677nm.
The results are shown in Table 6 for the assay of titanium and boron in embodiment 4 in sample TiB2-7050, as shown in Table 6, should
Method veracity and precision with higher.
The assay result of titanium and boron in 6 embodiment 4 of table in sample TiB2-7050
Embodiment 5
Step 1 weighs aluminum alloy specimen 0.2 and is put into 100ml triangular flask, and 30ml hydrochloric acid (1+1) is added extremely into sample
Reaction completely, obtains mixed liquor a；
Step 2 is added dropwise hydrogenperoxide steam generator 6 to the mixed liquor a kind and drips, and continues to be heated to 300 ° to make the transparent nothing of solution
Residue shape moves into the volumetric flask of 100ml after cooling, is diluted with water to scale, shakes up, obtain prepare liquid；
Prepare liquid is placed in inductive coupling plasma emission spectrograph and is measured by step 3, detects titanium and boron
Emitted luminescence intensity obtains the content of titanium and boron in titanium alloy sample in conjunction with titanium and boron standard curve；Inductively coupled plasma body
In the operating condition of emission spectrometer, the analysis spectral line of titanium is 334.940nm, and the analysis spectral line of boron is 249.677nm.
The results are shown in Table 7 for the assay of titanium and boron in embodiment 5 in sample TiB2-7050, as shown in Table 7, should
Method veracity and precision with higher.
The assay result of titanium and boron in 7 embodiment 5 of table in sample TiB2-7050
Claims (7)
1. a kind of method for measuring Titanium In Aluminum Alloy and boron content, which is characterized in that be specifically implemented according to the following steps：
Step 1 weighs aluminum alloy specimen and is put into triangular flask, and hydrochloric acid is added into sample to complete reaction, obtains mixed liquor a；
Hydrogenperoxide steam generator is added dropwise into the mixed liquor a in step 2, continues to be heated to the transparent no residue shape of solution, after cooling
It moves into volumetric flask, is diluted with water to scale, shakes up, obtain prepare liquid；
Prepare liquid is placed in inductive coupling plasma emission spectrograph and is measured by step 3, detects the transmitting of titanium and boron
Luminous intensity obtains the content of titanium and boron in titanium alloy sample in conjunction with titanium and boron standard curve.
2. a kind of method for measuring Titanium In Aluminum Alloy and boron content according to claim 1, which is characterized in that described
The quality of aluminum alloy specimen is 0.1~0.2g in step 1, and triangular flask is the triangular flask of 100ml.
3. a kind of method for measuring Titanium In Aluminum Alloy and boron content according to claim 1, which is characterized in that described
The concentration of hydrochloric acid solution is 5.85mol/L in step 1, and the additive amount of hydrochloric acid solution is 25ml~30ml.
4. a kind of method for measuring Titanium In Aluminum Alloy and boron content according to claim 1, which is characterized in that described
The concentration of hydrogenperoxide steam generator is 10mol/L in step 2, and the additive amount of hydrogenperoxide steam generator is 6~7 drops.
5. a kind of method for measuring Titanium In Aluminum Alloy and boron content according to claim 1, which is characterized in that described
The volumetric flask that volumetric flask in step 2 is 100ml.
6. a kind of method for measuring Titanium In Aluminum Alloy and boron content according to claim 1, which is characterized in that described
Heating temperature in step 2 is 150 DEG C~300 DEG C.
7. a kind of method for measuring Titanium In Aluminum Alloy and boron content according to claim 1, which is characterized in that described
In the operating condition of the inductive coupling plasma emission spectrograph of step 3, the analysis spectral line of titanium is 334.940nm, point of boron
Analysis spectral line is 249.677nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109738419A (en) * | 2018-12-18 | 2019-05-10 | 郑州磨料磨具磨削研究所有限公司 | The measuring method of boron content in a kind of aluminum-based boron carbide material |
| CN110243853A (en) * | 2019-06-12 | 2019-09-17 | 中国华能集团有限公司 | The screening technique of constituent content in a kind of alloy |
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2018
- 2018-06-01 CN CN201810554754.XA patent/CN108872196A/en active Pending
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109738419A (en) * | 2018-12-18 | 2019-05-10 | 郑州磨料磨具磨削研究所有限公司 | The measuring method of boron content in a kind of aluminum-based boron carbide material |
| CN109738419B (en) * | 2018-12-18 | 2022-07-01 | 郑州磨料磨具磨削研究所有限公司 | Method for measuring boron content in aluminum-based boron carbide material |
| CN110243853A (en) * | 2019-06-12 | 2019-09-17 | 中国华能集团有限公司 | The screening technique of constituent content in a kind of alloy |
| CN110243853B (en) * | 2019-06-12 | 2022-02-01 | 中国华能集团有限公司 | Method for screening content of elements in alloy |
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Application publication date: 20181123 |