CN102087208A - Method for detecting content of oxide inclusion in aluminium and aluminium alloys - Google Patents
Method for detecting content of oxide inclusion in aluminium and aluminium alloys Download PDFInfo
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Abstract
The invention relates to a method for detecting content of oxide inclusion in aluminium and aluminium alloys. The method comprises the following steps: washing the specimens with absolute ethyl alcohol and propanol and drying the specimens; adding defined amount of ethanol and iodine to a reflux device and fully mixing the ethanol and iodine uniformly to ensure the concentration of iodine in ethanol to be 10-20%; weighing 1+/-0.0001g of specimens, placing the specimens into the reflux device with nitrogen as the protective gas to carry out reflux reaction at the temperature of 40-70 DEG C for 4-6 hours until the specimens are totally dissolved; filtering the solution with filter paper, abandoning the filtrate and washing the filter paper with ethanol until no iodine exists; ashing the filter paper and inclusion, adding 1-3g of alkali to fuse the ash, taking out and cooling the fused ash, adding hot water to a beaker, after the fusion cake is fully dissolved, adding hydrochloric acid while shaking the beaker, then pouring the solution into a 100ml volumetric flask and fixing the volume with water; and measuring the content of the oxide inclusion by colorimetry.
Description
One, technical field
The invention belongs to non-ferrous metal element detection range, specifically relate to oxide inclusion Determination on content analytical approach in aluminium and the aluminium alloy.
Two, background technology
The content that traditional chemical method detected and analyzed oxide inclusion in metallic aluminium or the aluminium alloy mainly adopts bromo-methyl alcohol method to measure, USSR (Union of Soviet Socialist Republics) just once adopted bromo-methyl alcohol method to measure the content of aluminium oxide in the metallic aluminium in national standard, its method is: at a certain temperature, test portion is dissolved in the bromine-methanol soln, aluminium and other alloying element all generate bromide and are dissolved among the methyl alcohol, and oxides such as silicon and aluminium oxide are insoluble, after isolated by filtration and abundant the cleaning, residue and filter paper are dried together, ashing, weigh, deduction silicon amount and filter paper weight, promptly get oxide inclusion content, but, because the reagent that molten sample adopts all is volatile poisonous chemical reagent, brings very big difficulty to analysis, simultaneously sample analysis person is brought very big actual bodily harm.Therefore, invent a kind of molten sample respond well, do not have the molten sample reagent of toxicity that inclusion analysis is had very great significance again.
Three, summary of the invention
Technical matters to be solved by this invention provides oxide inclusion Determination on content and analytical approach in a kind of aluminium and the aluminium alloy, this method is to adopt aluminium in iodo-dissolve with ethanol method dissolved aluminum and the aluminium alloy, aluminium is separated with snotter, and then by combining with colourimetry, the content of oxide inclusion in quantitative measurement aluminium and the aluminium alloy exactly.
For solving the problems of the technologies described above, technical scheme of the present invention is: oxide inclusion Determination on content analytical approach in a kind of aluminium and the aluminium alloy is characterized in that the determination and analysis step is:
A, cut aluminium flake from the ingot casting of aluminum or aluminum alloy and become the fine strip shape test portion, clean up with propyl alcohol then with absolute ethyl alcohol earlier, in exsiccator, placed 5～20 minutes or used the cold air drying test portion;
B, pour 60～100ml ethanol in reflux, add an amount of iodine, heating is dissolved in the ethanol iodine fully, and the concentration of iodine in ethanol is 10-20%;
C, take by weighing 1 ± 0.0001g test portion, put into reflux, do blanket gas with nitrogen and prevent aluminaization, back flow reaction 4～6 hours is dissolved fully until sample under 40～70 ℃ of conditions;
D, use filter paper filtering solution, discard filtrate, clean filter paper with ethanol, till not having iodine;
E, the filter paper that will have a precipitation place in the crucible, begin ashing from low temperature, rising to 600～900 ℃ of insulations took out after 20～60 minutes, cooling adds 1～3g alkali, in 650～800 ℃ of fusions, add hot-water flooding after the taking-up in beaker, the limit is shaken the beaker limit and is added hydrochloric acid, pours in the 100ml volumetric flask water constant volume then;
F, draw above-mentioned solution 10ml in the 100ml volumetric flask respectively, water dashes to the 50ml, adds 2～4% ascorbic acid, 1～3ml, shakes up, and adds the paranitrophenol indicator, with 1: 5NH
3H
2O transfers to yellow, transfers to yellow with 5% hydrochloric acid again and takes off just, adds acetate-ammonium acetate buffer solution of 10ml PH=4.4, after shaking up, adds 0.5% aluminon, 2～5ml, and the water constant volume is placed and carried out colorimetric after 3～5 hours, determines the content of oxide inclusion.
The further optimized technical scheme of the present invention is that the medical numerical control supersonic washer of KQ 250DE type is adopted in the cleaning of test portion in (A) step.
The further optimized technical scheme of the present invention is to adopt Ag in (D) step
+Detect and whether contain iodine.
The further optimized technical scheme of the present invention is that employed crucible is platinum crucible or silver crucible in (E) step.
The further optimized technical scheme of the present invention is that the colorimetric wavelength is in (F) step: 525.0nm.
The outfit of standard aluminum solution: take by weighing 0.5293g fine aluminium sheet in the 150ml beaker, add hydrochloric acid (1+1) 100ml dissolving, be punched in the 1000ml volumetric flask water constant volume, promptly get 1.000mg/ml standard inventory solution, again the standard inventory solution dilution is become 20.00 μ g/ml titers.
The method for drafting of typical curve is among the present invention: draw 0.0,10.0,20.0,30.0,40.0 respectively from standard aluminum solution, 50.0,60.0,70.0,80.0,90.0 100 microgram aluminium oxide add reagent with sample and carry out colorimetric, the drawing standard curve in the 100ml volumetric flask.
Beneficial effect of the present invention is:
1, operating process is simpler, and do not have toxic gas generation or volatilization in the entire test, bring a lot of convenience to practical operation, avoided the actual bodily harm of chemical reagent to analytical test person, be a kind of effectively and have a good method of oxide inclusion content in the detection aluminium of practical significance and the aluminium alloy.
2, carry out colorimetric detection with tintmeter again with the iodo-dissolve with ethanol, its result detects accurately, can detect the aluminium and the aluminium alloy of oxide inclusion content＞0.00020.
Four, embodiment
Describe the specific embodiment of the present invention in detail below in conjunction with the experimental data progress:
Embodiment 1:
Oxide inclusion Determination on content analytical approach in a kind of aluminium and the aluminium alloy, the determination and analysis step is:
A, cut aluminium flake, be processed into the fine strip shape test portion, clean up with propyl alcohol then with absolute ethyl alcohol earlier, in exsiccator, place 5～20 minutes dry test portions from the ingot casting of aluminum or aluminum alloy;
B, pour 60～100ml ethanol in reflux, add an amount of iodine, heating is dissolved in the ethanol iodine fully, and the concentration of iodine in ethanol is 10%;
C, take by weighing 1 ± 0.0001g test portion, put into reflux, do blanket gas with nitrogen and prevent aluminaization, back flow reaction 4～6 hours is dissolved fully until sample under 40 ℃ of conditions;
D, use filter paper filtering solution, discard filtrate, clean filter paper with ethanol, until detect with Ag+ do not have iodine till;
E, the filter paper that will have a precipitation place in the crucible, begin ashing from low temperature, rise to 600 ℃ of insulations and take out cooling after 20～60 minutes, add 1g alkali,, add hot-water flooding after the taking-up in beaker in 700 ℃ of fusions, the limit is shaken the beaker limit and is added hydrochloric acid, pours in the 100ml volumetric flask water constant volume then;
F, draw above-mentioned solution 10ml in the 100ml volumetric flask respectively, water dashes to the 50ml, adds 2% ascorbic acid 3ml, shakes up, and adds the paranitrophenol indicator, with 1: 5NH
3H
2O transfers to yellow, transfers to yellow with 5% hydrochloric acid again and takes off just, adds acetate-ammonium acetate buffer solution of 10ml PH=4.4, after shaking up, adds 0.5% aluminon, 2～5ml, and the water constant volume is placed and carried out colorimetric after 3～5 hours, determines the content of oxide inclusion.
Embodiment 2:
Oxide inclusion Determination on content analytical approach in a kind of aluminium and the aluminium alloy, the determination and analysis step is:
A, cut aluminium flake, be processed into the fine strip shape test portion, clean up in the medical numerical control supersonic washer of KQ-250DE type with propyl alcohol then with absolute ethyl alcohol earlier, use the cold air drying test portion from the ingot casting of aluminum or aluminum alloy;
B, pour 60～100ml ethanol in reflux, add an amount of iodine, heating is dissolved in the ethanol iodine, and the concentration of iodine in ethanol is 15%;
C, take by weighing 1 ± 0.0001g test portion, put into reflux, do blanket gas with nitrogen and prevent aluminaization, back flow reaction 4～6 hours is dissolved fully until sample under 50 ℃ of conditions;
D, use filter paper filtering solution, discard filtrate, clean filter paper with ethanol, until detect with silver nitrate do not have iodine till;
E, the filter paper that will have a precipitation place in the crucible, begin ashing from low temperature, rising to 700 ℃ of insulations took out after 20～60 minutes, cooling adds 2g NaOH, in 650 ℃ of fusions, add hot-water flooding after the taking-up in beaker, the limit is shaken the beaker limit and is added hydrochloric acid, pours in the 100ml volumetric flask water constant volume then;
F, draw above-mentioned solution 10ml in the 100ml volumetric flask respectively, water dashes to the 50ml, adds 3% ascorbic acid 2ml, shakes up, and adds the paranitrophenol indicator, with 1: 5NH
3H
2O transfers to yellow, transfers to yellow with 5% hydrochloric acid again and takes off just, adds acetate-ammonium acetate buffer solution of 10ml PH=4.4, after shaking up, adds 0.5% aluminon, 2～5ml, and the water constant volume is placed and carried out colorimetric after 3～5 hours, determines the content of oxide inclusion.
Embodiment 3:
Oxide inclusion Determination on content analytical approach in a kind of aluminium and the aluminium alloy, the determination and analysis step is:
A, cut aluminium flake, be processed into the fine strip shape test portion, sample is cleaned up in the medical numerical control supersonic washer of KQ-250DE type with propyl alcohol then with absolute ethyl alcohol earlier, in exsiccator, place 5～20 minutes dry test portions from the ingot casting of aluminum or aluminum alloy;
B, pour 60～100ml ethanol in reflux, add an amount of iodine, heating is dissolved in the ethanol iodine, and the concentration of iodine in ethanol is 20%;
C, take by weighing 1 ± 0.0001g test portion, put into reflux, do blanket gas with nitrogen and prevent aluminaization, back flow reaction 4～6 hours is dissolved fully until sample under 60 ℃ of conditions;
D, use filter paper filtering solution, discard filtrate, clean filter paper with ethanol, till not having iodine;
E, the filter paper that will have a precipitation place in the platinum crucible, begin ashing from low temperature, rising to 900 ℃ of insulations took out after 20～60 minutes, cooling adds 1g natrium carbonicum calcinatum and 2g NaOH, in 800 ℃ of fusions, add hot-water flooding after the taking-up in beaker, the limit is shaken the beaker limit and is added hydrochloric acid, pours in the 100ml volumetric flask water constant volume then;
F, draw above-mentioned solution 10ml in the 100ml volumetric flask respectively, water dashes to the 50ml, adds 4% ascorbic acid 2ml, shakes up, and adds the paranitrophenol indicator, with 1: 5NH
3H
2O transfers to yellow, transfers to yellow with 5% hydrochloric acid again and takes off just, adds acetate-ammonium acetate buffer solution of 10ml PH=4.4, after shaking up, adds 0.5% aluminon, 2～5ml, and the water constant volume is placed and carried out colorimetric after 3～5 hours, determines the content of oxide inclusion.
Embodiment 4:
Oxide inclusion Determination on content analytical approach in a kind of aluminium and the aluminium alloy, the determination and analysis step is:
A, cut aluminium flake, be processed into the fine strip shape test portion, clean up with propyl alcohol then with absolute ethyl alcohol earlier, in exsiccator, place 10～20 minutes dry test portions from the ingot casting of aluminum or aluminum alloy;
B, pour 60～100ml ethanol in reflux, add an amount of iodine, heating is dissolved in the ethanol iodine, and the concentration of iodine in ethanol is 18%;
C, take by weighing 1 ± 0.0001g test portion, put into reflux, do blanket gas with nitrogen and prevent aluminaization, back flow reaction 4～6 hours is dissolved fully until sample under 70 ℃ of conditions;
D, use filter paper filtering solution, discard filtrate, clean filter paper with ethanol, until detect with Ag+ do not have iodine till;
E, the filter paper that will have a precipitation place in the crucible, begin ashing from low temperature, rising to 800 ℃ of insulations took out after 20～60 minutes, cooling adds 1.5g boric acid and 1g natrium carbonicum calcinatum, in 750 ℃ of fusions, add hot-water flooding after the taking-up in beaker, the limit is shaken the beaker limit and is added hydrochloric acid, pours in the 100ml volumetric flask water constant volume then;
F, draw above-mentioned solution 10ml in the 100ml volumetric flask respectively, water dashes to the 50ml, adds 3% ascorbic acid 3ml, shakes up, and adds the paranitrophenol indicator, with 1: 5NH
3H
2O transfers to yellow, transfers to yellow with 5% hydrochloric acid again and takes off just, adds acetate-ammonium acetate buffer solution of 10ml PH=4.4, after shaking up, adds 0.5% aluminon, 2～5ml, and the water constant volume is placed and carried out colorimetric after 3～5 hours, determines the content of oxide inclusion.
Embodiment 5:
Oxide inclusion Determination on content analytical approach in a kind of aluminium and the aluminium alloy, the determination and analysis step is:
A, cut aluminium flake, be processed into the fine strip shape test portion, clean up with propyl alcohol then with absolute ethyl alcohol earlier, in exsiccator, place 15～20 minutes dry test portions from the ingot casting of aluminum or aluminum alloy;
B, pour 60～100ml ethanol in reflux, add an amount of iodine, heating is dissolved in the ethanol iodine, and the concentration of iodine in ethanol is 12%;
C, take by weighing 1 ± 0.0001g test portion, put into reflux, do blanket gas with nitrogen and prevent aluminaization, back flow reaction 4～6 hours is dissolved fully until sample under 55 ℃ of conditions;
D, use filter paper filtering solution, discard filtrate, clean filter paper with ethanol, till not having iodine;
E, the filter paper that will have a precipitation place in the platinum crucible, begin ashing from low temperature, rising to 750 ℃ of insulations took out after 20～60 minutes, cooling adds the 1.8g natrium carbonicum calcinatum, in 700 ℃ of fusions, add hot-water flooding after the taking-up in beaker, the limit is shaken the beaker limit and is added hydrochloric acid, pours in the 100ml volumetric flask water constant volume then;
F, draw above-mentioned solution 10ml in the 100ml volumetric flask respectively, water dashes to the 50ml, adds 2% ascorbic acid 1ml, shakes up, and adds the paranitrophenol indicator, with 1: 5NH
3H
2O transfers to yellow, transfers to yellow with 5% hydrochloric acid again and takes off just, adds acetate-ammonium acetate buffer solution of 10ml PH=4.4, after shaking up, adds 0.5% aluminon, 2～5ml, and the water constant volume is placed and carried out colorimetric after 3～5 hours, determines the content of oxide inclusion.
Embodiment 6:
Oxide inclusion Determination on content analytical approach in a kind of aluminium and the aluminium alloy, the determination and analysis step is:
A, cut aluminium flake, be processed into the fine strip shape test portion, clean up with propyl alcohol then with absolute ethyl alcohol earlier, in exsiccator, place 5～20 minutes dry test portions from the ingot casting of aluminum or aluminum alloy;
B, pour 60～100ml ethanol in reflux, add an amount of iodine, heating is dissolved in the ethanol iodine, and the concentration of iodine in ethanol is 10%;
C, take by weighing 1 ± 0.0001g test portion, put into reflux, do blanket gas with nitrogen and prevent aluminaization, back flow reaction 4～6 hours is dissolved fully until sample under 65 ℃ of conditions;
D, use filter paper filtering solution, discard filtrate, clean filter paper with ethanol, till not having iodine;
E, the filter paper that will have a precipitation place in the crucible, begin ashing from low temperature, rising to 650 ℃ of insulations took out after 20～60 minutes, cooling adds 1.5g boric acid, in 600 ℃ of fusions, add hot-water flooding after the taking-up in beaker, the limit is shaken the beaker limit and is added hydrochloric acid, pours in the 100ml volumetric flask water constant volume then;
F, draw above-mentioned solution 10ml in the 100ml volumetric flask respectively, water dashes to the 50ml, adds 2% ascorbic acid 2ml, shakes up, and adds the paranitrophenol indicator, with 1: 5NH
3H
2O transfers to yellow, transfers to yellow with 5% hydrochloric acid again and takes off just, adds acetate-ammonium acetate buffer solution of 10ml PH=4.4, after shaking up, adds 0.5% aluminon, 2～5ml, and the water constant volume is placed and carried out colorimetric after 3～5 hours, determines the content of oxide inclusion.
Embodiment 7:
Oxide inclusion Determination on content analytical approach in a kind of aluminium and the aluminium alloy, the determination and analysis step is:
A, cut aluminium flake, be processed into the fine strip shape test portion, clean up in the medical numerical control supersonic washer of KQ-250DE type with propyl alcohol then with absolute ethyl alcohol earlier, in exsiccator, place 5～20 minutes dry test portions from the ingot casting of aluminum or aluminum alloy;
B, pour 60～100ml ethanol in reflux, add an amount of iodine, heating is dissolved in the ethanol iodine, and the concentration of iodine in ethanol is 20%;
C, take by weighing 1 ± 0.0001g test portion, put into reflux, do blanket gas with nitrogen and prevent aluminaization, back flow reaction 4～6 hours is dissolved fully until sample under 70 ℃ of conditions;
D, use filter paper filtering solution, discard filtrate, clean filter paper with ethanol, till not having iodine;
E, the filter paper that will have a precipitation place in the silver crucible, begin ashing from low temperature, rising to 850 ℃ of insulations took out after 20～60 minutes, cooling adds 1.5g boric acid and 1.5g NaOH, in 800 ℃ of fusions, add hot-water flooding after the taking-up in beaker, the limit is shaken the beaker limit and is added hydrochloric acid, pours in the 100ml volumetric flask water constant volume then;
F, draw above-mentioned solution 10ml in the 100ml volumetric flask respectively, water dashes to the 50ml, adds 4% ascorbic acid 2ml, shakes up, and adds the paranitrophenol indicator, with 1: 5NH
3H
2O transfers to yellow, transfers to yellow with 5% hydrochloric acid again and takes off just, adds acetate-ammonium acetate buffer solution of 10ml PH=4.4, after shaking up, adds 0.5% aluminon, 2～5ml, and the water constant volume is placed and carried out after 3～5 hours, determines the content of oxide inclusion.
Claims (5)
1. oxide inclusion content detecting method in aluminium and the aluminium alloy is characterized in that the determination and analysis step is:
A, cut aluminium flake from the ingot casting of aluminum or aluminum alloy and become the fine strip shape test portion, clean up with propyl alcohol then with absolute ethyl alcohol earlier, in exsiccator, placed 5～20 minutes or used the cold air drying test portion;
B, pour 60～100ml ethanol in reflux, add an amount of iodine, heating is dissolved in the ethanol iodine, and the concentration of iodine in ethanol is 10～20%;
C, take by weighing 1 ± 0.0001g test portion, put into reflux, do blanket gas with nitrogen and prevent aluminaization, back flow reaction 4～6 hours is dissolved fully until sample under 40～70 ℃ of conditions;
D, use filter paper filtering solution, discard filtrate, clean filter paper with ethanol, till not having iodine; E, the filter paper that will have a precipitation place in the crucible, begin ashing from low temperature, being warming up to 600～900 ℃ of insulations took out after 20～60 minutes, cooling adds 1～3g alkali, in 650～800 ℃ of fusions, add hot-water flooding after the taking-up in beaker, the limit is shaken the beaker limit and is added hydrochloric acid, pours in the 100ml volumetric flask water constant volume then;
F, draw above-mentioned solution 10ml in the 100ml volumetric flask respectively, water dashes to the 50ml, adds 2～4% ascorbic acid, 1～3ml, shakes up, and adds the paranitrophenol indicator, with 1: 5NH
3H
2O transfers to yellow, transfers to yellow with 5% hydrochloric acid again and takes off just, adds acetate-ammonium acetate buffer solution of 10ml PH=4.4, after shaking up, adds 0.5% aluminon, 2～5ml, and the water constant volume is placed and carried out colorimetric after 3～5 hours, determines the content of oxide inclusion.
2. oxide inclusion content detecting method in a kind of aluminium according to claim 1 and the aluminium alloy is characterized in that, (A) the medical numerical control supersonic washer of KQ-250DE type is adopted in the cleaning of test portion in the step.
3. oxide inclusion content detecting method in a kind of aluminium according to claim 1 and the aluminium alloy is characterized in that, (D) adopts Ag in the step
+Detect and whether contain iodide ion.
4. oxide inclusion content detecting method in a kind of aluminium according to claim 1 and the aluminium alloy is characterized in that, (E) employed crucible is platinum crucible or silver crucible in the step.
5. oxide inclusion content detecting method in a kind of aluminium according to claim 1 and the aluminium alloy is characterized in that, (F) the colorimetric wavelength is in the step: 525.0nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103185717A (en) * | 2011-12-31 | 2013-07-03 | 湖南晟通科技集团有限公司 | Method for determining content of aluminum nitride in aluminum ash |
| CN109342254A (en) * | 2018-09-19 | 2019-02-15 | 中国航发北京航空材料研究院 | A kind of method of fast quantitative analysis high temperature alloy inclusion content |
| CN111521467A (en) * | 2020-06-04 | 2020-08-11 | 河北省地质实验测试中心 | Graphite detection method |
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| JP3144031B2 (en) * | 1992-03-30 | 2001-03-07 | 昭和電工株式会社 | Oxygen analysis of aluminum and aluminum alloys |
| CN1619289A (en) * | 2003-11-21 | 2005-05-25 | 兰州理工大学 | Detecting method of aluminium and aluminium alloy oxide impuring content |
| CN101256131A (en) * | 2008-04-17 | 2008-09-03 | 上海交通大学 | Apparatus for detection of foreign material in aluminum as well as aluminum alloy fondant |
| CN101643855A (en) * | 2009-08-07 | 2010-02-10 | 中国船舶重工集团公司第十二研究所 | Method for refining aluminum and aluminum alloy melt through in-situ reduction |
-
2010
- 2010-12-21 CN CN2010105982338A patent/CN102087208A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3144031B2 (en) * | 1992-03-30 | 2001-03-07 | 昭和電工株式会社 | Oxygen analysis of aluminum and aluminum alloys |
| CN1619289A (en) * | 2003-11-21 | 2005-05-25 | 兰州理工大学 | Detecting method of aluminium and aluminium alloy oxide impuring content |
| CN101256131A (en) * | 2008-04-17 | 2008-09-03 | 上海交通大学 | Apparatus for detection of foreign material in aluminum as well as aluminum alloy fondant |
| CN101643855A (en) * | 2009-08-07 | 2010-02-10 | 中国船舶重工集团公司第十二研究所 | Method for refining aluminum and aluminum alloy melt through in-situ reduction |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103185717A (en) * | 2011-12-31 | 2013-07-03 | 湖南晟通科技集团有限公司 | Method for determining content of aluminum nitride in aluminum ash |
| CN109342254A (en) * | 2018-09-19 | 2019-02-15 | 中国航发北京航空材料研究院 | A kind of method of fast quantitative analysis high temperature alloy inclusion content |
| CN111521467A (en) * | 2020-06-04 | 2020-08-11 | 河北省地质实验测试中心 | Graphite detection method |
| CN111521467B (en) * | 2020-06-04 | 2023-08-29 | 河北省地质实验测试中心 | Graphite detection method |
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Application publication date: 20110608 |