CN102401756B - Preparation method of ferromolybdenum sample molten glass - Google Patents
Preparation method of ferromolybdenum sample molten glass Download PDFInfo
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- CN102401756B CN102401756B CN2010102764609A CN201010276460A CN102401756B CN 102401756 B CN102401756 B CN 102401756B CN 2010102764609 A CN2010102764609 A CN 2010102764609A CN 201010276460 A CN201010276460 A CN 201010276460A CN 102401756 B CN102401756 B CN 102401756B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910001309 Ferromolybdenum Inorganic materials 0.000 title claims abstract description 10
- 239000006060 molten glass Substances 0.000 title abstract 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 106
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 53
- 238000002844 melting Methods 0.000 claims abstract description 24
- 230000008018 melting Effects 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000011521 glass Substances 0.000 claims abstract description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 11
- XZXYQEHISUMZAT-UHFFFAOYSA-N 2-[(2-hydroxy-5-methylphenyl)methyl]-4-methylphenol Chemical compound CC1=CC=C(O)C(CC=2C(=CC=C(C)C=2)O)=C1 XZXYQEHISUMZAT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229940107816 ammonium iodide Drugs 0.000 claims abstract description 10
- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000004458 analytical method Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 108010038629 Molybdoferredoxin Proteins 0.000 claims description 17
- HBELESVMOSDEOV-UHFFFAOYSA-N [Fe].[Mo] Chemical compound [Fe].[Mo] HBELESVMOSDEOV-UHFFFAOYSA-N 0.000 claims description 17
- 230000004907 flux Effects 0.000 claims description 17
- 239000011435 rock Substances 0.000 claims description 10
- 241001300078 Vitrea Species 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 238000001304 sample melting Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000013467 fragmentation Methods 0.000 claims description 2
- 238000006062 fragmentation reaction Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 3
- 238000000441 X-ray spectroscopy Methods 0.000 abstract description 2
- 210000004127 vitreous body Anatomy 0.000 abstract 3
- 238000000184 acid digestion Methods 0.000 abstract 1
- 238000005259 measurement Methods 0.000 abstract 1
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 238000007493 shaping process Methods 0.000 abstract 1
- 238000004846 x-ray emission Methods 0.000 description 5
- 230000004927 fusion Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000003252 repetitive effect Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010309 melting process Methods 0.000 description 2
- 238000007500 overflow downdraw method Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910001021 Ferroalloy Inorganic materials 0.000 description 1
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a preparation method of a ferromolybdenum sample molten glass, which comprises the following steps: preparing a sample, performing acid digestion on the sample, preparing a sample by melting a vitreous body, and preparing the vitreous body by melting the vitreous body in a shaping crucible. Digesting a ferromolybdenum sample by using nitric acid, drying at low temperature, adding lithium tetraborate and ammonium iodide reagents, and melting at high temperature of 1100 ℃ to prepare a molten glass body. Provides a new melting sample preparation way for the X-ray spectrometry analysis of ferromolybdenum, and solves the difficulties in the prior art for preparing ferromolybdenum molten glass. The method has the advantages of simple and rapid operation, easy control, no damage to the platinum crucible, prolonged service life and service cycle of the platinum crucible, and reduced cost for repeatedly repairing the crucible. The formed ferromolybdenum fused glass body is glossy and transparent, meets the measurement requirement of an XRF method, and has a very strong application prospect.
Description
Technical field
The invention belongs to the chemical analysis technology field, specifically for x ray fluorescence spectrometry, analyze a kind of preparation method for ferromolybdenum sample melting glass body in the typing crucible.
Background technology
Molybdenum-iron mainly adopts wet chemistry analyzed at present, and the element sense cycle is long, complex operation, and x ray fluorescence spectrometry is measured can shorten sense cycle, makes simple to operateization.But x-ray fluorescence spectrometry molybdenum-iron only is confined to the pressed disc method sample preparation at present, and pressed disc method is subject to the impact of the effects such as granularity, mineral, and precision is poor, and the precision of fusion method sample preparation is better than pressed disc method.But molybdenum-iron is placed on the direct flux that adds in platinum crucible carries out high-temperature fusion, very easily with platinum crucible, forms the alloy of low melting point in melting process, thereby valuable vessel platinum crucible is had to heavy corrosion, and harmfulness is high.The pertinent literature of inquiry ferroalloy fusion method sample preparation: the people's such as Hou Yanbing " X-fluorescence melts the sheet method measures sial in ferro-silico aluminium and Al-Ba iron " (" metallurgical analysis " 24 volume supplementary issues in 2004).In document: first use lithium tetraborate melting wall built-up in platinum crucible, form a flux platinum crucible, the potpourri of sample and oxygenant is placed in the flux platinum crucible, first low-temperature oxidation in muffle furnace, because the fusing point of lithium tetraborate is higher, in oxidizing process, the flux platinum crucible can not melt, and the decomposition temperature of oxygenant is lower, can make the reducing substances oxidation complete, platinum crucible is not corroded.In document, time length, rotating speed speed and temperature setting in melting process are not specifically described, the experimentation operation is very strict and be difficult to control, does not have the value of popularization.Therefore for the preparation of molybdenum-iron sample melten glass body, existing sample pretreating means can't meet actual requirement.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method for ferromolybdenum sample melting glass body, especially a kind of nitric acid that utilizes first digests the molybdenum-iron sample, adds lithium tetraborate and ammonium iodide reagent after low temperature drying, prepares the method for melten glass body 1100 ℃ of high-temperature fusion.
Concrete technology method of the present invention comprises: the acid of sample preparation, sample is cleared up, melten glass system sample and melten glass system sample are made Vitrea processing step in the typing crucible.
Concrete technology of the present invention is:
1 sample preparation:
(1) will after the fragmentation of molybdenum-iron sample, be ground between the 120-200 order, sample mass is no less than 1g;
(2) sample takes: get wherein 0.3000-0.3500g of molybdenum-iron;
(3) acid of sample is cleared up:
The sample taken is placed in the 50ml platinum crucible, add the 10-15ml deionized water, slowly drip 8-10ml red fuming nitric acid (RFNA) (analysis that volumetric molar concentration is 16moL/L is pure or top grade is pure), low-temperature heat (≤100 ℃), rock sample is all dissolved, then platinum crucible first is placed on the concentrated volume in high-temperature region (200 ℃≤temperature≤400 ℃), when solution when slightly salt is separated out, need to reduce temperature (100 ℃≤temperature≤150 ℃) until sample is all dried, take off and be cooled to room temperature; Now the molybdenum-iron sample has become nitrate, and nitrate is easy to be decomposed by alkaline mixed flux high-temperature fusion, does not corrode platinum alloy crucible, and the effect that sample decomposes is played in the effect in the x ray fluorescence spectrometry analysis.
2 melten glass system samples:
(1), in the platinum crucible of drying, add lithium tetraborate flux quality 4.500-5.000g (analyzing pure), add ammonium iodide release agent 0.15-0.20g (analyzing pure), platinum crucible is tilted 30 °, and the rotation crucible mixes flux in crucible, and covers specimen surface as far as possible;
(2) platinum crucible that, will mix flux is put into rapidly the high temperature furnace of 1100 ℃, after melting 4-5min, take out, promptly shake platinum crucible, molten mass is received into the tiny blobs be scattered on inwall in molten mass, (generally this process is carried out once again to put into 1100 ℃ of high temperature furnaces, if the tiny blobs on the platinum crucible wall can't once be taken in fully, but repetitive operation is once), then melting 2-3min;
(3), take out platinum crucible, rock platinum crucible, again take in the little blobs hung on wall, then pour molten mass into the typing crucible fully rapidly, if the molten mass mobility weakens, can again add a small amount of ammonium iodide to carry out the demoulding.
Vitrea making in 3 typing crucibles:
The typing crucible of molten mass of packing into is put into the high temperature furnace melting 2-3min of 1100 ℃, the typing crucible is rocked in taking-up makes molten mass make fully to mix, when the melting rate of flow of fluid is slower, continue to shake the typing crucible and catch up with in clean molten mass bubble and shakeout, cooling rear molten mass forms bright and clean smooth vitreum at the typing crucible.
The present invention utilizes nitric acid to clear up the molybdenum-iron sample, and then low temperature drying adds lithium tetraborate and ammonium iodide reagent, prepares the method for melten glass body 1100 ℃ of high-temperature fusion.For the x-ray spectrometry analysis of molybdenum-iron provides a kind of new melting sample preparation approach.Solved the difficulty that the standby prior art of molybdenum-iron melten glass system exists.Will be as a kind of new molybdenum-iron melting method for making sample after enforcement, it is simple to operation, quick, easy to control that method has, and do not damage platinum crucible, extended life-span and the life cycle of platinum crucible, saved the cost of repeatedly repairing crucible.The molybdenum-iron melten glass body gloss formed, transparent, meet the requirement that the XRF method is measured, there is very strong application prospect.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1:
Taking granularity is 120 order molybdenum-iron sample 0.3000g.The sample of weighing is placed in the 50ml platinum crucible, add the 10ml deionized water, slowly drip 8ml red fuming nitric acid (RFNA) (analysis that volumetric molar concentration is 16moL/L is pure), 40 ℃ of low-temperature heats, rock sample is all dissolved, platinum crucible first is placed on the concentrated volume in 200 ℃ of high-temperature regions, when solution when slightly salt is separated out, need to reduce by 150 ℃ of temperature until sample is all dried, take off and be cooled to room temperature.
Add lithium tetraborate (analyzing pure) flux quality 4.5000g in the platinum crucible of drying, add ammonium iodide (analyzing pure) release agent 0.15g.Platinum crucible is tilted 30 °, and the rotation crucible mixes flux in crucible, and covers the platinum crucible inwall that hangs with sample.The platinum crucible that mixes flux is put into rapidly to the high temperature furnace of 1100 ℃, take out after melting 4min.Clamp with the platinum pliers, promptly shake platinum crucible, molten mass is received into the tiny blobs be scattered on inwall in molten mass.Again put into high temperature furnace (generally this process is carried out once, if the tiny blobs on the platinum crucible wall can't once take in fully, but repetitive operation once), then melting 2min.
Take out platinum crucible, rock platinum crucible, again take in the little blobs hung on wall, then rapidly molten mass is poured fully into to the typing crucible of Φ 35mm.If the molten mass mobility weakens, can again add a small amount of ammonium iodide to carry out the demoulding at platinum crucible, more rapidly molten mass be poured fully into to the typing crucible of Φ 35mm.
The typing crucible is put into to the high temperature furnace melting 2min again of 1100 ℃, taken out and rock molten mass and makes it fully to mix.When the melting rate of flow of fluid is slower, continues to shake the typing crucible and catch up with in clean molten mass bubble and shakeout.Can be at Φ 35mm typing crucible, the bright and clean smooth vitreum of interior formation after cooling.
Embodiment 2:
Taking granularity is 200 order molybdenum-iron sample 0.3500g.The sample of weighing is placed in the 50ml platinum crucible, add the 15ml deionized water, drip 10ml red fuming nitric acid (RFNA) (top grade that volumetric molar concentration is 16moL/L is pure), 100 ℃ of low-temperature heats, rock sample is all dissolved, platinum crucible first is placed on the concentrated volume in 400 ℃ of high-temperature regions, when solution when slightly salt is separated out, need to reduce by 100 ℃ of temperature until sample is all dried, take off and be cooled to room temperature;
Add lithium tetraborate (analyzing pure) flux quality 5.0000g in the platinum crucible of drying, add ammonium iodide (analyzing pure) release agent 0.20g.Platinum crucible is tilted 30 °, and the rotation crucible mixes flux in crucible, and covers the platinum crucible inwall that hangs with sample.The platinum crucible that mixes flux is put into rapidly to the high temperature furnace of 1100 ℃, take out after melting 5min.Clamp with the platinum pliers, promptly shake platinum crucible, molten mass is received into the tiny blobs be scattered on inwall in molten mass.Again put into high temperature furnace (generally this process is carried out once, if the tiny blobs on the platinum crucible wall can't once take in fully, but repetitive operation once), then melting 3min.
Take out platinum crucible, rock platinum crucible, again take in the little blobs hung on wall, then rapidly molten mass is poured fully into to the typing crucible of Φ 35mm.If the molten mass mobility weakens, can again add a small amount of ammonium iodide to carry out the demoulding at platinum crucible, more rapidly molten mass be poured fully into to the typing crucible of Φ 35mm.
The typing crucible is put into to the high temperature furnace melting 3min again of 1100 ℃, taken out and rock molten mass and makes it fully to mix.When the melting rate of flow of fluid is slower, continues to shake the typing crucible and catch up with in clean molten mass bubble and shakeout.Can be at Φ 35mm typing crucible, the bright and clean smooth vitreum of interior formation after cooling.
Claims (1)
1. a preparation method for ferromolybdenum sample melting glass body, it is characterized in that, the concrete technology method comprises: the acid of sample preparation, sample is cleared up, melten glass system sample and melten glass system sample are made Vitrea processing step in the typing crucible, and the concrete technology step is as follows:
1) sample preparation:
(1) will after the fragmentation of molybdenum-iron sample, be ground between the 120-200 order, sample mass is no less than 1 g;
(2) sample takes: take molybdenum-iron sample 0. 3000-0.3500g;
2) acid of sample is cleared up:
The sample taken is placed in 50 ml platinum crucibles, add 10-15 ml deionized water, slowly drip the red fuming nitric acid (RFNA) that analysis is pure or top grade is pure that 8-10 ml volumetric molar concentration is 16moL/L, be less than 100 ℃ of low-temperature heats, rock sample is all dissolved, then platinum crucible first is placed on the concentrated volume in high-temperature region of 200 ℃≤temperature T≤400 ℃, when solution when slightly salt is separated out, reduce by 100 ℃ ~ 150 ℃ of heating-up temperatures, until sample is all dried, take off and be cooled to room temperature;
3) melten glass system sample:
(1), in the platinum crucible of drying, add lithium tetraborate flux quality 4.500-5.000 g, add ammonium iodide release agent 0.15-0.20 g, platinum crucible is tilted 30 °, the rotation crucible mixes flux in crucible, and covers specimen surface;
(2) platinum crucible that, will mix flux is put into rapidly the high temperature furnace of 1100 ℃, take out after melting 4-5 min, promptly shake platinum crucible, molten mass is received into the tiny blobs be scattered on inwall in molten mass, again put into 1100 ℃ of high temperature furnaces, then melting 2-3 min;
(3), take out platinum crucible, rock platinum crucible, again take in the little blobs hung on wall, the typing crucible of then rapidly molten mass being poured into fully;
4) Vitrea making in the typing crucible:
The typing crucible of molten mass of packing into is put into the high temperature furnace melting 2-3 min of 1100 ℃, the typing crucible is rocked in taking-up makes molten mass make fully to mix, when the melting rate of flow of fluid is slower, continue to shake the typing crucible and catch up with in clean molten mass bubble and shakeout, cooling rear molten mass forms bright and clean smooth vitreum at the typing crucible.
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| CN104280415A (en) * | 2013-10-31 | 2015-01-14 | 东旭集团有限公司 | Method for accurately detecting components of raw glass sheets |
| CN106645242A (en) * | 2016-10-08 | 2017-05-10 | 山西太钢不锈钢股份有限公司 | Method for preparing molybdenum iron glass fuse pieces |
| CN111879801A (en) * | 2020-06-23 | 2020-11-03 | 邯郸钢铁集团有限责任公司 | Preparation method of glass sample for XRF analysis based on acid oxidation low alloy steel sample |
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| CN101592571A (en) * | 2009-06-19 | 2009-12-02 | 邯郸钢铁股份有限公司 | X-fluorescence fusion method is measured alloying element content method in ferrotianium, the vanadium iron |
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| JPH0625715B2 (en) * | 1988-09-20 | 1994-04-06 | 新日本製鐵株式会社 | Fluorescent X-ray analysis sample preparation method and apparatus thereof |
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| CN101008593A (en) * | 2006-01-27 | 2007-08-01 | 宝山钢铁股份有限公司 | Sample preparation method of material containing silicon carbide used for x-ray spectrometric analysis |
| CN101592571A (en) * | 2009-06-19 | 2009-12-02 | 邯郸钢铁股份有限公司 | X-fluorescence fusion method is measured alloying element content method in ferrotianium, the vanadium iron |
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