CN1074542C - Process for preparing solution for atomic absorption detecting total aluminium in iron and steel - Google Patents
Process for preparing solution for atomic absorption detecting total aluminium in iron and steelInfo
- Publication number
- CN1074542C CN1074542C CN 97121891 CN97121891A CN1074542C CN 1074542 C CN1074542 C CN 1074542C CN 97121891 CN97121891 CN 97121891 CN 97121891 A CN97121891 A CN 97121891A CN 1074542 C CN1074542 C CN 1074542C
- Authority
- CN
- China
- Prior art keywords
- sample
- acid
- steel
- phosphoric acid
- total aluminium
- 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.)
- Expired - Fee Related
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Abstract
The present invention relates to a method for preparing solution for measuring the total aluminium content in steel through atomic absorption or plasma spectrometry. After a test sample is dissolved by using acids, such as HCl, HClO4 and HNO3, or diluted hydrochloric acid and an intense reaction is finished, phosphoric acid of 4 to 40 ml/g as a specimen and V2O5 as auxiliary solvent which accounts for more than 6% of the test sample are added, and the test sample is put in a microwave oven, heated and dissolved at high temperature at the atmospheric pressure of 10 to 40 Pa. Because the reaction at high pressure at high temperature in the present invention is fast and the sample is dissolved by adding the phosphoric acid, the sample can be successfully dissolved once by adding the V2O5 as auxiliary solvent, and the total aluminium content is directly measured. By using the method, the analytical cycle can be shortened, the work efficiency is enhanced, and the sample consumption is reduced; blank spaces are reduced, the measured value is identical to the standard value, and the precision conforms to the requirements.
Description
The present invention relates to a kind of preparation method that material analysis is measured the solution of total aluminium content in the steel with method, particularly atomic absorption method or the inductive coupling high-frequency plasma method (ICP) of solution for preparing.
Aluminium in the iron and steel comprises that acid soluble aluminium and the aluminium that is insoluble to acid (as are insoluble in sour A1N, α-Al
2O
3Deng), at home, in the external analysis, various standards (such as GB, JK, ISO, ASTM, JIS etc.) all will be dissolved through peracid when analyzing total aluminium.At present, the solution manufacturing method with total aluminium in the atomic absorption method analysis steel generally was divided into for two steps: 1. acid is molten: at first adopt HCl+HClO
4, HCl+HNO
3, HCl+H
2O
2The dissolving acid dissolubility aluminium such as acid obtain main liquid, 2. residue treatment with this solution with Filter paper filtering then: namely the residue on the filter paper is collected, washed back and forth until the yellow disappearance of iron chloride on the filter paper is washed 3～4 times with warm water with thermohaline acid again; Filter paper is put into platinum crucible together, and calcination in coal gas waits whole filter paper to become to put into behind the carbide 1100 ℃ of Muffle furnace ashing half an hour, adds potassium pyrophosphate melting residue after the cooling 20 minutes.This residue is incorporated in the main liquid that filters, and cooling was diluted with water to scale again after heating for dissolving fused mass, clean platinum crucible were concentrated to required dosage again, measured total aluminium with atomic absorption method or plasma spectroscopy then.The prior art is in sour course of dissolution, and is very high to the temperature control requirement of electric furnace pan, and temperature is too high to cause sample not molten complete and again analyze easily, therefore need to have the personnel of certain practical experience to operate.The residue treatment Period Process is long, efficient is low, use platinum crucible, and the reagent consumption that adds the melting agent is big.The analytical chemistry field extensively adopts microwave close dissolving technology to prepare chemical analysis solution in recent years, but yet there are no report about the method for preparing the solution of total aluminium in the atomic absorption method analysis iron and steel with microwave close dissolving technology.
Purpose of the present invention prepares the method that atomic absorption method is analyzed the solution of total aluminium in the steel, can once dissolve total aluminium in the iron and steel by adopting microwave close dissolving technology, analyzes accurately, and operating efficiency is improved.
For achieving the above object, the technical solution of the present invention's proposition is:
A kind of method for preparing total aluminum solutions in Atomic absorption or the plasma spectrum mensuration iron and steel uses acid such as HCl, HClO
4, HNO
3Or watery hydrochloric acid treats that with after the sample dissolving vigorous reaction is complete, adds the flux V of phosphoric acid and 〉=6% (weight) sample of 4～40ml/ gram sample
2O
5, place in the micro-wave oven and dissolve certain hour under the certain pressure.
Flux V
2O
5Consumption be 〉=10% sample.
Solubilizing reaction pressure is 10～40 atmospheric pressure.
The solubilizing reaction time is 10～30 minutes.
Phosphoric acid can be replaced by phosphoric acid+sulfuric acid.
Below the present invention is done and be described in further detail.
When preparation Atomic absorption or plasma spectrum are measured in the iron and steel total aluminum solutions, generally 200 ℃ of sample dissolution, because the acid of adopting other is to α-Al
2O
3The solvability deficiency, be difficult to reach disposable dissolving, the solvability of phosphoric acid is stronger than general acid, but phosphoric acid namely generates pyrophosphoric acid at 270 ℃ in course of dissolution, its piece class is difficult for dissolving, causes to analyze to lose efficacy, and temperature is controlled at 200～270 ℃ of relatively difficulties in the very short operating time.The present invention adopts the airtight molten sample of microwave phosphoric acid, and uses and use less phosphoric acid to dissolve in the atomic absorption detecting, produces high pressure, high temperature under microwave action, can avoid above-mentioned deficiency.And can enlarge the analyst coverage of atomic absorption analysis, and suitable cosolvent V in addition
2O
5Can further improve solvability.Phosphoric acid among the present invention can add sulfuric acid by phosphoric acid and replace, but owing to add sulfuric acid, produces a large amount of heats, can cause damage to the material of dissolving cup, therefore adopts phosphoric acid to add sulfuric acid and can dissolve α-Al
2O
3, but it is effective to be not so good as phosphoric acid.
The present invention learns by a series of experiment, with V
2O
5Compare, total aluminium content that other cosolvent obtains is on the low side, and this shows that its hydrotropy effect is not enough strong, can not reach the requirement of standard.Compare V with other cosolvent
2O
5Stable reaction, effect continue, and the hurried rising of pressure can not occur, surpass the phenomenon that microwave limits pressure.V
2O
5Consumption be sample (weight) greater than 6%,＜6%, dissolve insufficiently, measured value is on the low side.
Introduce embodiments of the invention below in conjunction with effect.
Present embodiment uses the MK-1 type optical fiber pressure automatic control closed microwave stove of the new microwave technology Applied Research Laboratory development in Shanghai, and weighing 0.5 gram sample places the molten sample cup of teflon, adds 2mlHCl, 2mlHNO
3, treat that vigorous reaction is complete after, add again 4mlH
3PO
4(dense H
3PO
4, proportion 1.0～1.7) and 0.05 gram V
2O
5, cover capping, place in the dissolves one kind of pots under high pressure.Adjust the program of microwave sample dissolving: 15 minutes time, pressure is 20 atmospheric pressure, shut the fire door of micro-wave oven, under 100% microwave power, start operation, automatically stop after 15 minutes, the cooling, with the solution constant volume in the molten sample cup to 100ml, use atomic spectrophotometer, wavelength=309.3nm measures the total aluminium in the iron and steel.Present embodiment is also to the cosolvent V of different content
2O
5Impact to measurement result is tested, and its result such as table 1 show, work as V
2O
5During＜0.01g, measured value is on the low side; V
2O
5〉=0.03～0.07 o'clock.Measured value is normal.
The measurement result of the method for the present invention and prior art sees Table 2,3,4.
Table 2 has provided the employing standard sample and has measured, and the value that the inventive method is measured is consistent with standard value.
Table 3 is the method for employing prior art and the contrast of method measured value of the present invention.
Table 4 is analyzed for adopting standard sample (GB8911-06 sample, standard value are 0.034%) to carry out 10 times, and with the prior art determination process comparison, show that method of the present invention meets related standards fully to the requirement of precision.
Preparing Atomic absorption or plasma spectrum in prior art measures in the iron and steel in total aluminum solutions, because insoluble aluminium belongs to difficult oxide, the nitride that decomposes more, to could decompose after the melting under 1100 ℃ of high temperature with potassium pyrosulfate, consuming time more, and solvent, piece class salt cause certain difficulty to Atomic absorption or plasma spectrum mensuration in a large number.The present invention is owing to reaction speed under high temperature, the high pressure is fast, and molten sample once successfully can directly be measured total aluminium.Can find out that from table 2,3,4 result the present invention is owing to adopt microwave-oven-heating, H
3PO
4Dissolving and V
2O
5Hydrotropy, molten sample under high temperature, high pressure, can realize once clearing up and satisfy multielement mensuration and once clear up a plurality of samples, reduce the complicated processes in analyzing, speed can improve several times to tens times, improved operating efficiency, be convenient to grasp, reduce reagent consumption, reduce blank, measured value is consistent with standard value, and precision meets the requirements.
Table 1
| V 2O 5Amount (g) | Standard value (total aluminium %) | Microwave measurement value (total aluminium) % | Microwave measurement mean value % | ||||
| 1 | 2 | 3 | 4 | 5 | |||
| 0.01 | GB8911-1 0.057％ | 0.0521 | 0.0502 | 0.0512 | 0.0482 | 0.0491 | 0.0505 |
| 0.03 | 0.0562 | 0.0571 | 0.0580 | 0.0573 | 0.0568 | 0.0570 | |
| 0.05 | 0.0576 | 0.0574 | 0.0578 | 0.0571 | 0.0570 | 0.0574 | |
| 0.07 | 0.0571 | 0.0569 | 0.0581 | 0.0578 | 0.0568 | 0.0573 | |
Table 2
| Specimen coding | Standard value (%) | The measured value of the inventive method (%) | ||
| 1 (GB8911-6) | 0.034 | 0.0343 | 0.0338 | 0.0342 |
| 2 (GB8911-1) | 0.057 | 0.0576 | 0.0574 | 0.0578 |
| 3 | 0.042 | 0.041 | 0.0423 | 0.0417 |
Table 3
| Specimen coding | Prior art measured value (%) | Measured value of the present invention (%) | The difference ratio |
| 1 | 0.024 | 0.024 | 0.000 |
| 2 | 0.035 | 0.0347 | -0.0003 |
| 3 | 0.037 | 0.0361 | -0.0009 |
| 4 | 0.034 | 0.034 | 0.000 |
| 5 | 0.04 | 0.0398 | -0.0002 |
| Mean value | 0.034 | 0.03372 | Total deviation Σ d=0.00028 standard deviation d=0.00037 |
Table 4
Claims (3)
1. the preparation method of sample solution during total aluminium of measuring in the iron and steel, with acid such as HCl, HClO
4, HNO
3Or watery hydrochloric acid is with after the sample dissolving, place close dissolving in the micro-wave oven, it is characterized in that: solubilizing reaction pressure is 10～40 atmospheric pressure, the solubilizing reaction time is 10～30 minutes, when above-mentioned acid dissolving, treat that vigorous reaction is complete, add the phosphoric acid of 4～10ml/ gram sample and the flux V of 6-14% weight sample
2O
5
2. preparation method according to claim 1 is characterized in that: described flux V
2O
5Consumption be 〉=sample of 10%-14%.
3. preparation method according to claim 1 is characterized in that: described phosphoric acid can be replaced by phosphoric acid and sulfuric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97121891 CN1074542C (en) | 1997-12-11 | 1997-12-11 | Process for preparing solution for atomic absorption detecting total aluminium in iron and steel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97121891 CN1074542C (en) | 1997-12-11 | 1997-12-11 | Process for preparing solution for atomic absorption detecting total aluminium in iron and steel |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1187623A CN1187623A (en) | 1998-07-15 |
| CN1074542C true CN1074542C (en) | 2001-11-07 |
Family
ID=5176518
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 97121891 Expired - Fee Related CN1074542C (en) | 1997-12-11 | 1997-12-11 | Process for preparing solution for atomic absorption detecting total aluminium in iron and steel |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1880946B (en) * | 2005-06-14 | 2010-05-05 | 中国科学院金属研究所 | Analysis method for phosphor in high temperature alloy |
| CN101446556B (en) * | 2007-05-25 | 2010-09-01 | 中国石化扬子石油化工有限公司 | Method for determining the platinum content in the catalytic reforming catalysts through the micro-wave digestion ICP method |
| CN101324520B (en) * | 2007-06-13 | 2010-08-11 | 中国船舶重工集团公司第七二五研究所 | Method for rapidly detecting micro trace quantity lead in ship hull steel with graphite oven atomic absorption |
| CN101936830A (en) * | 2009-07-01 | 2011-01-05 | 上海宝钢工业检测公司 | Sample-dissolving cup for dissolving surface coating of substrate and method for testing thickness of coating |
| CN101915692B (en) * | 2010-09-16 | 2011-11-16 | 攀钢集团钢铁钒钛股份有限公司 | Fusion agent for fusing stainless acid resistant steel as well as preparation method, application and using method thereof |
| CN102478504A (en) * | 2010-11-26 | 2012-05-30 | 湖南晟通科技集团有限公司 | Method for detecting content of aluminium and aluminium alloy oxide inclusions |
| CN102507854A (en) * | 2011-10-18 | 2012-06-20 | 攀钢集团江油长城特殊钢有限公司 | Diluted hydrochloric acid leaching-EDTA (ethylenediaminetetraacetic acid) volumetric method for determining metal aluminum content in steelmaking exothermic agent |
| CN102507853B (en) * | 2011-10-18 | 2014-12-10 | 攀钢集团江油长城特殊钢有限公司 | Method for determining metal aluminum content in steelmaking exothermal agent |
| CN102393386A (en) * | 2011-10-28 | 2012-03-28 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of calcium, magnesium and silicon in aluminum-based compound deoxidizing slagging constituent |
| CN103196780A (en) * | 2013-03-20 | 2013-07-10 | 邢台钢铁有限责任公司 | Method for determining aluminium oxide content of aluminum-manganese ball |
| CN110836810A (en) * | 2019-11-27 | 2020-02-25 | 中国电子科技集团公司第四十三研究所 | Sample dissolving method for testing trace elements of aluminum nitride powder |
-
1997
- 1997-12-11 CN CN 97121891 patent/CN1074542C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1187623A (en) | 1998-07-15 |
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Owner name: BAOSHAN IRON & STEEL CO., LTD. Free format text: FORMER NAME OR ADDRESS: SHANGHAI BAO STEEL GROUP IRON AND STEEL CO LTD Owner name: SHANGHAI BAO STEEL GROUP IRON AND STEEL CO LTD Free format text: FORMER NAME OR ADDRESS: BAOSHAN STEEL GROUP IRON AND STEEL CO LTD |
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Address after: 201900, Fujin Road, Shanghai, Baoshan District orchard Patentee after: BAOSHAN IRON & STEEL Co.,Ltd. Address before: 200122 No. 370 Pu circuit, Shanghai, Pudong New Area Patentee before: BAOSHAN IRON & STEEL CO.,LTD. Address after: 200122 No. 370 Pu circuit, Shanghai, Pudong New Area Patentee after: BAOSHAN IRON & STEEL CO.,LTD. Address before: 201900 No. 1, Middle Road, Baoshan District, Shanghai Patentee before: Baosteel Group Corporation |
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Granted publication date: 20011107 Termination date: 20121211 |