CN105067591A - ICP-AES method for detecting beryllium content in aluminum-beryllium intermediate alloy - Google Patents
ICP-AES method for detecting beryllium content in aluminum-beryllium intermediate alloy Download PDFInfo
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Abstract
The present invention discloses an ICP-AES method for detecting beryllium content in aluminum-beryllium intermediate alloy, and technical field of chemical detection. The method includes reagent preparation, sample weighing, pretreatment dissolution, dilution, wavelength selection, preparation of series standard solutions, inductive coupling, plasma atomic emission spectrometry detection and calculation of the analysis results. The method achieves rapid dissolution in the sample pretreatment, strong operationality of preparation of the series standard solutions, easily controlled detection process and accurate and reliable detection results. The determination scope is w(Be) 0.50%-8.00%. The present invention solves the technical problem of detection method of beryllium content in aluminum-beryllium intermediate alloy, and provides a solid foundation for further research of novel products of aluminum-beryllium intermediate alloy in the industries of machinery, electronics, weapon, and nonferrous metals, and improves aluminum product quality and production efficiency, and reduces production costs in the aluminum production smelting process; and the invention provides reliable basis for the rapid and accurate quantitative analysis of beryllium content in aluminum-beryllium intermediate alloy.
Description
Technical field
The present invention relates to the ICP-AES detection method of beryllium content in a kind of aluminium beryllium intermediate alloy, in particular to the inductively coupled plasma atomic emission spectrum quantitative analysis method of beryllium content in a kind of aluminium beryllium intermediate alloy, measurement range: ω (Be) 0.50% ~ 8.00%.
Background technology
Intermediate alloy refers to makes alloy by some simple substance, make it easy to join in other alloys, to solve the problems such as scaling loss, high-melting-point alloy not easily fuse into, little special alloy is affected on starting material, in other words people's transitional alloy that can not directly use simultaneously.Aluminium beryllium intermediate alloy is one of aluminium intermediate alloy ingot or intermediate alloy, he is widely used in the melting ingredient production of a large amount of alloy product, intermediate alloy can make the new material with various characteristic and function simultaneously, is important means and approach that industrially developed country researches and develops various new material.YS/T282-2000 " aluminium intermediate alloy ingot " specify in common aluminium beryllium intermediate alloy AlBe3 to be 2.0% ~ 4.0% containing beryllium amount, also containing the impurity element such as silicon, iron, zinc.In production, special requirement accurately detect the content of beryllium, to reduce the cost of raw material, and strict control alloy product quality.
In order to meet the production requirement of Novel aluminum alloy product, strictly must control content and the addition of beryllium element in aluminium beryllium intermediate alloy, this has gone out a difficult problem to undoubtedly chemical analysis testing staff, and the exploitation for its detection technique proposes challenge.
Inquired about by Chongqing City's standard information service network, the detection technique comparative maturity of China in iron and steel and alloy, Al and Alalloy, Copper and its alloy, zinc and zinc alloy, Mg-based hydrogen storage etc., the standard detecting method going through at present to issue has an appointment 1200 kinds.
Relevant criterion has:
1. GB/T5121.17-2008 " Copper and its alloy chemical analysis method the 17th part: the mensuration of beryllium content ", measurement range: ω (Be) 0.100% ~ 2.23%;
2. GB/T13748.11-2005 " mensuration of Mg-based hydrogen storage chemical analysis method beryllium content is according to the blue R spectrophotometric method of Lay chromium cyanogen ", measurement range: ω (Be) 0.0004% ~ 0.015%;
3. GB/T20975.22-2008 " Al and Alalloy chemical analysis method the 22nd part: the mensuration of beryllium content is according to the blue R spectrophotometric method of Lay chromium cyanogen ", measurement range: ω (Be) 0.00010% ~ 0.40%;
4. YS/T470.1-2004 copper beryllium alloy chemical analysis method " inductively coupled plasma-emission spectrographic determination beryllium, cobalt, nickel, titanium, iron, aluminium, silicon, lead, magnesium amount ", measurement range: ω (Be) 0.37% ~ 2.67%;
5. YS/T470.2-2004 " copper beryllium alloy chemical analysis method sodium fluoride titration measuring beryllium amount ", measurement range: ω (Be) 3.33% ~ 4.42%;
6. GB/T7999-2007 Al and Alalloy photo-electronic directly reading emission spectrographic analysis method
But the test method in People's Republic of China's non-ferrous metal industry standard YS/T282-2000 " aluminium intermediate alloy ingot " specifies: the chemical composition umpire analysis method of alloy pig is undertaken by the regulation of GB/T6987.1 ~ 6987.24.GB/T6987.1 ~ 6987.24 standard is cancelled, performs by GB/T20975.Its GB/T20975.25-2008 " Al and Alalloy chemical analysis method the 25th part: ICP-AES ", measurement range: ω (Be) 0.0005% ~ 0.40%, can not meet the testing requirement of beryllium element in aluminium beryllium intermediate alloy.
" non-ferrous metal analysis communication " 2 phases in 1999, what adopt in paper " in aluminium beryllium intermediate alloy beryllium determination " is gravimetric method, and sample is 4.18% containing beryllium amount, and its sense cycle is tediously long, testing staff's labour intensity large, reagent consumption is many.
Do not find the country of beryllium element in aluminium beryllium intermediate alloy, industry standard assay method, do not find the ICP-AES detection method (measurement range: ω (Be) 0.50% ~ 8.00%) of beryllium content in a kind of aluminium beryllium intermediate alloy yet.In addition, in company standard method, do not find relevant applicable detection method yet.At present, as the exploitation of beryllium content ICP-AES detection method in the middle of aluminium beryllium, still belong to blank.
Summary of the invention
In view of this, the invention provides the ICP-AES detection method of beryllium content in a kind of aluminium beryllium intermediate alloy, in the method, test portion is after hydrochloric acid solution and cosolvent solution dissolve, certain volume is diluted to secondary and other water of higher level, on inductively coupled plasma atomic emission spectrometer, measure the emitted luminescence intensity of beryllium element in test solution in recommended wavelength or other suitable wavelength places, calculated the massfraction of beryllium by calibration curve.
The ICP-AES detection method of beryllium content in a kind of aluminium beryllium intermediate alloy of the present invention, comprises preparation of reagents, test portion takes, pre-treatment is dissolved, dilutes, wavelength chooses, series standard solution preparation, ICP-AES detect, the calculating of analysis result and precision.
Beneficial effect of the present invention:
In a kind of aluminium beryllium intermediate alloy of the present invention, the ICP-AES detection method of beryllium content has following features:
1. establish the quick quantitative analytic method of ICP-AES to beryllium content in aluminium beryllium intermediate alloy;
2. measurement range: ω (Be) 0.50% ~ 8.00%;
3. precision:
0.50% ~ 1.00%, tolerance 0.03%; 1.00% ~ 2.00%, tolerance 0.05%;
2.00% ~ 5.00%, tolerance 0.08%; 5.00% ~ 8.00%, tolerance 0.10%.
Accompanying drawing explanation
Below in conjunction with drawings and embodiments, the invention will be further described.
Fig. 1 is the sample solution constitutional diagram after pre-treatment of the present invention;
Fig. 2 is the instrument and equipment figure of use of the present invention.
Embodiment
Below with reference to accompanying drawing, the present invention is described in detail.
1, implementation step one: pre-treatment
With ten thousand/electronic balance, take 0.1000g test portion, be placed in 150mL conical flask.In the conical flask being loaded with aluminium beryllium intermediate alloy test portion, add 20mL hydrochloric acid solution, 2mL cosolvent solution, low-temperature heat is dissolved completely to test portion.Take off, be cooled to room temperature.It is the sample solution by being cooled to room temperature after pre-treatment dissolution process, be transferred in 100mL volumetric flask, in transfer process, insert in volumetric flask with a glass bar, conical flask bottleneck tilts near glass bar, and solution is slowly flowed into along glass bar, and glass bar lower end will near bottleneck inwall, but not too close bottleneck, in order to avoid there is solution to overflow.After solution stream is complete, by conical flask along glass bar slightly toward on carry, simultaneously upright, a solution of attachment conical flask oral area is flowed back in beaker.Remain in a little solution in conical flask, with other washing of a small amount of secondary higher level 3 ~ 4 times, cleansing solution is transferred in volumetric flask as stated above.After solution proceeds to volumetric flask, add other water of secondary higher level, be diluted to about 3/4 volume time, by volumetric flask yawing several times (be sure not reversing shake), tentatively mix.Then continue to add other water of secondary higher level, dropwise add carefully during nearly graticule, until the lower meniscus of solution and graticule tangent till.Cover tightly glass stopper.
Left index finger pins stopper, and right hand finger tip withstands a bottle feather edge, then, makes bubble rise to top the other way around the other way around by volumetric flask and wholely to swing, 10 times so repeatedly ~ 15 times, can mix.Sample solution state after pre-treatment as shown in Figure 1.
2, implementation step two: instrument condition of work is optimized
The instrument and equipment used as shown in Figure 2.According to instrument instructions, instrument condition of work is optimized, selects suitable measuring condition (as argon pressure, observed altitude, analytical line, flush time, integral time etc.).
Utilize IRISIntrepid II XSP type inductively coupled plasma atomic emission spectrometer, the optimization measuring condition of selection is as recommended work parameter.
RF power: 1150W; Atomization gas pressure: 0.2MPa (28PSI); Pump speed: 100r/min; Assisted gas flow: 0.5L/min; Plasmatorch observed altitude: 15mm; Integral time: 10s.Purity of argon: be not less than 99.99%.
3, implementation step three: determined wavelength is selected
After instrument condition of work being optimized according to instrument instructions, in element determination wavelength spectral line, consider according to sensing range, linear relationship, the recovery, testing result accuracy, select suitable mensuration wavelength.Selected mensuration wavelength is:
Be234.861{143}nm、313.042{107}nm、313.107{107}nm。
4, implementation step four: testing result is collected
Operate according to IRISIntrepid II XSP type inductively-coupled plasma spectrometer working specification, detect the content of beryllium element in sample solution.Record testing result, carries out next step analysis.
5, implementation step five: addition method is verified
According to the analytical approach optimal conditions selected, according to standard addition method, make recovery test.
6, implementation step six: synthetic standard sample is verified
(1) synthetic standard sample
The synthetic standard sample element addition of 5 aluminium beryllium intermediate alloys is in table 1.
Table 1 synthetic standard sample element addition
| Numbering | Add aluminum amount/mg | Add Be amount/mg |
| 1# | 100 | 0.50 |
| 2# | 100 | 1.00 |
| 3# | 100 | 2.00 |
| 4# | 100 | 3.00 |
| 5# | 100 | 4.00 |
(2) calibration curve preparation
In calibration curve solution, the content outline of element to be measured is higher than the content of this element in sample.The quantity of calibration curve solution is determined by precision requirement, and general (3 ~ 5) are individual, draws the standard solution of calibration curve in table 2.
The standard solution of calibration curve drawn by table 2
(3) measure
A. instrument prepares
Open ICP-AES spectrometer, more than preheating 2h.
According to instrument instructions, instrument condition of work is optimized, selects suitable measuring condition (as argon pressure, observed altitude, analytical line, flush time, integral time etc.).
Prepare the softwares such as calibration curve drafting, measurement and statistical computation.
Click plasmatorch is lighted a fire, and confirms that instrument operational factor is in normal range after igniting, atomization system and plasma torch working properly, stablize more than 15min.
B. the measurement of series of calibration curve solution and the drafting of calibration curve
On inductive coupling plasma emission spectrograph, measure the spectral intensity of serial calibration curve solution beryllium, each solution duplicate measurements 2 times ~ 3 times, calculates its mean value.Deduct zero-dose spectral intensity mean value for ordinate with each spectral intensity mean value, the concentration of series of calibration curve solution is horizontal ordinate, draws the calibration curve of beryllium respectively.
Calculate the related coefficient of calibration curve, related coefficient should be greater than more than 0.999.
C. the mensuration of sample solution
Measure the spectral intensity in sample solution, duplicate measurements 2 times ~ 3 times, calculates its mean value.The mean value that its spectral intensity mean value deducts blank solution spectral intensity is clean spectral intensity.
(4) calculating of analysis result
According to calibration curve, clean spectral intensity is converted into the mass concentration of beryllium in sample solution, represents with mg/mL.
In test portion, beryllium content is in massfraction ω (Be), calculates by formula (1):
In formula:
ρ (Be)---the numerical value of beryllium mass concentration in test solution, unit is milligram every milliliter (mg/mL);
The numerical value that V---tested liquid is long-pending, unit is milliliter (mL);
M---the numerical value of test portion quality, unit is gram (g).
7, implementation step seven: content inspection
1. for the standard addition method inspection of low content
According to the optimal conditions selected, according to standard addition method, make recovery test, the recovery=(measuring resultant-test portion content)/addition × 100%.General provision requires that the recovery is 95% ~ 105%.In a kind of aluminium beryllium intermediate alloy of the present invention, the ICP-AES detection method recovery of beryllium content is 98.75% ~ 102.0%, see table 3.This detection method measurement result is described accurately and reliably.
Table 3 recovery test result
2. for the synthetic standard sample inspection of high-load
Carry out verification operation (aluminum content is 0.1000g) by the mode synthetic standard sample of implementation step six, its evaluation is in table 4.This detection method measurement result is described accurately and reliably.
Table 4 synthetic standard sample evaluation
| Numbering | Element | Addition/mg | Content/% | Measurement result/% | Difference/% | Tolerance/% | Conclusion |
| 11# | Be | 5.00 | 5.00 | 5.05 | 0.05 | 0.10 | Meet the requirements |
| 12# | Be | 6.00 | 6.00 | 5.98 | -0.02 | 0.10 | Meet the requirements |
| 13# | Be | 7.00 | 7.00 | 7.06 | 0.06 | 0.10 | Meet the requirements |
| 14# | Be | 8.00 | 8.00 | 8.06 | 0.06 | 0.10 | Meet the requirements |
3. produce examination and analyses result
Utilize the ICP-AES detection method of beryllium cellulose content in a kind of aluminium beryllium intermediate alloy, carried out detection and precision test to sample to be tested, it produces examination and analyses result see table 5.Visible, analysis result accurately and reliably.
Examination and analyses result produced by table 5
| Numbering | Element | Measurement result ω (Be)/% | Mean value/% | Standard deviation/% |
| 21# | Be | 1.02 1.03 1.02 0.99 1.03 1.03 | 1.02 | 0.016 |
| 22# | Be | 2.98 2.99 3.02 3.00 3.03 3.05 | 3.01 | 0.026 |
| 23# | Be | 4.97 4.95 4.95 4.99 5.02 4.95 | 4.97 | 0.029 |
Claims (1)
1. the ICP-AES detection method of beryllium content in an aluminium beryllium intermediate alloy, comprise preparation of reagents, test portion take, pre-treatment is dissolved, dilute, wavelength chooses, series standard solution preparation, ICP-AES detect, the calculating of analysis result and precision, it is characterized in that:
1) preparation of reagents: utilize ultrapure water machine to prepare ultrapure water, its conductivity requires to be not more than 0.10mS/m; The preparation of hydrochloric acid solution: in 400mL beaker, add ultrapure water, then add hydrochloric acid, stir evenly with glass bar; The preparation of cosolvent solution: in 250mL beaker, add ultrapure water, then add cosolvent, stir evenly with glass bar;
2) test portion takes, and from aluminium beryllium middle sample, with ten thousand/electronic balance, takes 0.1000g test portion, is placed in 150mL conical flask;
3) pre-treatment is dissolved, and in the conical flask being loaded with test portion in the middle of aluminium beryllium, adds 20mL hydrochloric acid solution and 2mL cosolvent solution, and low-temperature heat is dissolved completely to test portion.Take off, be cooled to room temperature;
4) dilute, the sample solution of room temperature will be cooled to after pre-treatment dissolution process, be transferred in 100mL volumetric flask, in transfer process, insert in volumetric flask with a glass bar, conical flask bottleneck tilts near glass bar, solution is slowly flowed into along glass bar, glass bar lower end near bottleneck inwall, but will be too near to bottleneck, in order to avoid there is solution to overflow; After solution stream is complete, by conical flask along glass bar slightly toward on carry, simultaneously upright, make a solution of attachment conical flask oral area flow back in bottle; Remain in a little solution in conical flask, with other washing of a small amount of secondary higher level 3 ~ 4 times, cleansing solution is transferred in volumetric flask as stated above; After solution proceeds to volumetric flask, add other water of secondary higher level, be diluted to about 3/4 volume time, by volumetric flask yawing several times, tentatively mix.Then continue to add other water of secondary higher level, dropwise add carefully during nearly graticule, until the minimum point of the lower meniscus of solution and graticule tangent till, cover tightly glass stopper;
Left index finger pins glass stopper, and right hand finger tip withstands a bottle feather edge, then, makes the bubble in solution rise to top the other way around the other way around by volumetric flask and wholely to swing, 10 times so repeatedly ~ 15 times, can mix;
5) wavelength chooses, open inductively coupled plasma atomic emission spectrometer (ICP-AES), more than preheating 2h, according to instrument instructions, instrument condition of work is optimized, selects suitable measuring condition (as argon pressure, observed altitude, analytical line, flush time, integral time etc.);
Utilize IRISIntrepid II XSP type inductively coupled plasma atomic emission spectrometer, the optimization measuring condition of selection as recommended work parameter, RF power: 1150W; Atomization gas pressure: 0.2MPa (28PSI); Pump speed: 100r/min; Assisted gas flow: 0.5L/min; Plasmatorch observed altitude: 15mm; Flush time: 30s; Integral time: 10s; Purity of argon: be not less than 99.99%;
After instrument condition of work is optimized, in element determination wavelength spectral line, consider according to sensing range, linear relationship, the recovery, testing result accuracy, select suitable mensuration wavelength, selected mensuration wavelength is: Be234.861{143}nm, 313.042{107}nm, 313.107{107}nm;
6) series standard solution preparation, in calibration curve solution, the content outline of element to be measured is higher than the content of this element in sample.The quantity of calibration curve solution is determined by precision requirement, and general (3 ~ 5) are individual, draws the standard solution of calibration curve in table 1; The standard solution of calibration curve drawn by table 1
7) ICP-AES detects, and refers to softwares such as preparing calibration curve drafting, measurement and statistical computation.Click plasmatorch is lighted a fire, and confirms that instrument operational factor is in normal range after igniting, atomization system and plasma torch working properly, stablize more than 15min;
On inductive coupling plasma emission spectrograph, measure the spectral intensity of serial calibration curve solution beryllium, each solution duplicate measurements 2 times ~ 3 times, calculates its mean value.Deduct zero-dose spectral intensity mean value for ordinate with each spectral intensity mean value, the concentration of series of calibration curve solution is horizontal ordinate, draws the calibration curve of beryllium.Calculate the related coefficient of calibration curve, related coefficient should be greater than more than 0.999.
Measure the spectral intensity of sample solution in the middle of aluminium beryllium, duplicate measurements 2 times ~ 3 times, calculates its mean value.The mean value that its spectral intensity mean value deducts blank solution spectral intensity is clean spectral intensity;
8) calculating of analysis result, according to calibration curve, is converted into the mass concentration of beryllium in sample solution, represents with mg/mL by clean spectral intensity,
In test portion, beryllium content is with massfraction
meter, calculates by formula (1):
In formula:
ρ (Be)---the numerical value of the mass concentration of beryllium in test solution, unit is milligram every milliliter (mg/mL);
The numerical value that V---tested liquid is long-pending, unit is milliliter (mL);
M---the numerical value of test portion quality, unit is gram (g);
Precision, between laboratory, the difference of analysis result should be not more than tolerance numerical value listed by table 2.
Table 2 tolerance numerical value
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| CN105466909A (en) * | 2015-12-23 | 2016-04-06 | 重庆长安工业(集团)有限责任公司 | Method for fast quantitative analysis for six-element content in powder metallurgy |
| CN106596516A (en) * | 2016-11-09 | 2017-04-26 | 重庆长安工业(集团)有限责任公司 | Method of measuring trace lead content of tin bronze by means of standard addition-ICP atomic emission spectrometer |
| CN108918508A (en) * | 2018-07-25 | 2018-11-30 | 重庆长安工业(集团)有限责任公司 | The measuring method of high content iron in a kind of tin bronze |
| CN110320201A (en) * | 2018-03-30 | 2019-10-11 | 上海梅山钢铁股份有限公司 | The detection method of cobalt content in a kind of monel |
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| CN105466909A (en) * | 2015-12-23 | 2016-04-06 | 重庆长安工业(集团)有限责任公司 | Method for fast quantitative analysis for six-element content in powder metallurgy |
| CN106596516A (en) * | 2016-11-09 | 2017-04-26 | 重庆长安工业(集团)有限责任公司 | Method of measuring trace lead content of tin bronze by means of standard addition-ICP atomic emission spectrometer |
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