CN106645242A - Method for preparing molybdenum iron glass fuse pieces - Google Patents
Method for preparing molybdenum iron glass fuse pieces Download PDFInfo
- Publication number
- CN106645242A CN106645242A CN201610872488.6A CN201610872488A CN106645242A CN 106645242 A CN106645242 A CN 106645242A CN 201610872488 A CN201610872488 A CN 201610872488A CN 106645242 A CN106645242 A CN 106645242A
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- molybdenum
- iron
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- platinum crucible
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention relates to the technical field of quantitative analysis of X-ray fluorescence spectrums, and discloses a method for preparing molybdenum iron sample glass fuse pieces. The method includes the process steps: grinding samples; performing pre-oxidation for the samples; preparing glass molten mass. The method particularly includes the steps: paving the bottom with mixed flux of lithium tetraborate and lithium metaborate; directly mixing lithium carbonate, sodium nitrate and molybdenum iron samples; gradually rising the temperature and oxidizing at the temperature lower than 700 DEG C; adding ammonium bromide reagents; preparing the glass fuse pieces at the temperature of 1100 DEG C. According to the method, the excellent molybdenum iron glass fuse pieces are simply, conveniently and rapidly prepared, use requirements of an X-ray fluorescence analysis method are met, and large-batch actual production inspection is rapidly finished in a high-quality manner.
Description
Technical field
The present invention relates to X-ray fluorescence spectra quantitative analysis tech field.
Background technology
At present molybdenum-iron is mainly measured using chemical analysis method, particularly host element Mo, Element detection cycle length, step
It is rapid loaded down with trivial details, and adopt x ray fluorescence spectrometry measurement then to shorten detection cycle, it is easy to operate.But current XRF light
Spectrometry determines molybdenum-iron and is confined to pressed disc method sample preparation, and due to the impact of test sample matrix effect and granularity effect, analysis result is accurate
Degree is poor；And glass melting method sample preparation, the degree of accuracy of x-ray fluorescence spectrometry can match in excellence or beauty with chemical analysis method, but
Molybdenum-iron is placed in crucible into directly addition flux carries out high-temperature fusion, and easily low melting point is formed with platinum crucible in melting process
Alloy, so as to heavy corrosion platinum crucible, use cost is very high.
（1）Patent CN 102401756A provide method be：The processing step of vitreum, profit are made in sizing crucible
Molybdenum-iron sample is cleared up with nitric acid, low temperature drying is subsequently adding lithium tetraborate and iodate ammonium reagent, in 1100 DEG C of high-temperature fusions.
Shortcoming：Its nitric acid clears up post-drying needs the temperature at 100 DEG C or so to carry out, and process slowly, spends the time
Also it is longer；During high-temperature fusion, the solute on crucible side need to be repeatedly collected, if operation is not careful, be easily caused sample damage
Lose.
（2）The method that patent CN 10183289A is provided is carried out in the steps below：Platinum crucible wall built-up, prepares oxide；
Iron alloy samples are pre-oxidized；Iron alloy samples MTG YBCO bulk.
Shortcoming：One is to need platinum yellow gold crucible wall built-up, strict to wall built-up operation, is slightly slipped up, and will result in valuable platinum yellow
Golden crucible heavy corrosion；Two be adopt this method ultimately form solute in glass melt ratio it is too little, need add
Demoulding dosage is big, affects testing result.
（3）CN103149074A discloses a kind of MTG YBCO bulk mode of x-ray fluorescence analysis molybdenum-iron, including following step
Suddenly：A, to weigh lithium tetraborate, lithium carbonate and sample mixed uniform, wraps up glomeration；B, material is put into the rebasing earthenware of graphite powder
In crucible, high temperature pre-oxidation.
Shortcoming：It is cumbersome；Graphite powder for protecting crucible decomposes not exclusively can impact analysis result.
There is different degrees of defect in said method.Using existing sample pretreating and analytical technology, it is impossible to meet real
The requirement of border production cycle.
The content of the invention
The technical problem to be solved is：When how a kind of analysis molybdenum-iron for x ray fluorescence spectrometry is provided
The method for preparing mother glass fuse piece.
The technical solution adopted in the present invention is：A kind of method for preparing molybdenum-iron bead, enters according to the steps
OK
Step one, molybdenum-iron is crushed after cross 200 mesh sieve, make diameter be less than 0.074mm；
Step 2, configuration oxidant are Li2CO3And NaNO3Mixture, Li2CO3Quality be 5 times of molybdenum-iron, NaNO3Quality
For 2-3 times of molybdenum-iron,
Step 3, mixed flux is laid on platinum crucible bottom and madial wall, with the speed less than 15 DEG C/min by platinum crucible
300 DEG C are warmed up to, after being then well mixed molybdenum-iron and oxidant platinum crucible is put into, it is to avoid molybdenum-iron and oxidant and platinum earthenware
Crucible directly contact；
Step 4, platinum crucible is warmed up into 650 DEG C with the speed less than 15 DEG C/min, insulation 10min makes molybdenum-iron and oxidant
React completely；
Step 5, platinum crucible is cooled to room temperature, adds 100mg-140mg concentration for the NH of 400mg/mL4The Br aqueous solution, so
After be heated to 1100 DEG C insulation 5min-6min, be finally cooled to room temperature and obtain molybdenum-iron bead.
As a kind of preferred embodiment：Mixed flux compares metaboric acid by lithium metaborate and lithium tetraborate according to quality in step 3
Lithium：Lithium tetraborate=1：2 mixing.
As a kind of preferred embodiment：Heating and thermal insulation is carried out in fusion apparatus in step 5, in insulating process, platinum earthenware
Crucible stand in fusion apparatus heating 2min, then crucible rotation and incline shake heating 3 ~ 4min, 30 ° ~ 45 ° of angle of inclination.
The invention has the beneficial effects as follows：Present invention achieves the simple, fast molybdenum-iron bead for preparing high-quality, meets
The use requirement of x-ray fluorescence analysis methods, high-quality is rapidly completed large batch of production inspection.
Specific embodiment
A kind of method for preparing molybdenum-iron bead, is carried out according to the steps
Step one, weigh 0.2g molybdenum-iron samples, by molybdenum-iron sample it is broken after, ground 200 mesh sieve makes diameter be less than 0.074mm；
Step 2, configuration oxidant are Li2CO3And NaNO3Mixture, Li2CO3Quality be 1g, NaNO3Quality be 0.6 gram；
Step 3,5-6 gram of mixed flux is laid on into platinum crucible bottom and madial wall, platinum crucible is put into Muffle furnace, with little
Platinum crucible is warmed up into 300 DEG C in the speed of 15 DEG C/min, platinum earthenware is put into after being then well mixed molybdenum-iron and oxidant
Crucible, it is to avoid molybdenum-iron and oxidant and platinum crucible directly contact, mixed flux is by lithium metaborate and lithium tetraborate according to mass ratio
Lithium metaborate：Lithium tetraborate=1：2 mixing；
Step 4, platinum crucible is warmed up into 650 DEG C with the speed less than 15 DEG C/min, insulation 10min makes molybdenum-iron and oxidant
React completely, while the also part fusing of the mixed flux in the bottom of a pan；
Step 5, platinum crucible is cooled to room temperature, adds 100mg-140mg concentration for the NH of 400mg/mL4The Br aqueous solution, so
After be heated to 1100 DEG C insulation 5min-6min, be finally cooled to room temperature and obtain molybdenum-iron bead, carry out in fusion apparatus plus
Heat insulation, in insulating process, platinum crucible stands in fusion apparatus heating 2min, then crucible rotation and incline shake add
3 ~ 4min of heat, 30 ° ~ 45 ° of angle of inclination.
The fusing point of molybdenum trioxide is that boiling point is relatively low, and its fusing point is 795 DEG C, and boiling point is 1155 DEG C, and molybdenum-iron is oxidized to three
Molybdenum oxide, just has started to before melting distillation, when temperature is up to 900 ~ 1100 DEG C, evaporates quite fast.Alkali and alkaline earth metal ions
Stable molybdate can be defined with its reaction before molybdenum trioxide volatilization, these molybdates are difficult in molybdenum trioxide distillation interval
Decompose.Therefore, we have selected the carbonate and nitrate of alkali metal Li and Na as oxidant, respectively Li2CO3With
NaNO3, can effectively suppress the volatilization of molybdenum trioxide.
306.8 DEG C of sodium nitrate fusing point, lithium carbonate fusing point is 618 DEG C, and the fusing point of lithium tetraborate and lithium metaborate mixture is about
For 700 DEG C, therefore, the key operation of pre-oxidation is as follows：Initial temperature is 300 DEG C, is then to slowly warm up to 650 DEG C, and heat up speed
Degree is less than 15 DEG C/min, and oxidation 10min is then kept at 650 DEG C.Now, molybdenum-iron sample is complete with oxidant reaction, and
At this temperature, mix with the mixed flux of the bottom of a pan part fusing, it is ensured that the almost free of losses of molybdenum-iron sample.
Operating process of the present invention is simple, it is easy to control, it is not necessary to add extra safeguard measure, need to only control oxidation temperature
Degree, you can ensure the complete oxidation of sample.
Molybdenum-iron glass melt homogeneous transparent made by the present invention, meets the requirement of XRF detections；X-ray for molybdenum-iron is glimmering
Light spectrum analysis provides a kind of new, easy sample preparation approach.
Present invention reduces testing cost：While ensure that platinum crucible not by alloy corrosion, molybdenum-iron point is shortened
The cycle of analysis, with good application prospect.
Claims (3)
1. a kind of method for preparing molybdenum-iron bead, it is characterised in that：Carry out according to the steps
Step one, molybdenum-iron is crushed after cross 200 mesh sieve, make diameter be less than 0.074mm；
Step 2, configuration oxidant are Li2CO3And NaNO3Mixture, Li2CO3Quality be 5 times of molybdenum-iron, NaNO3Quality
For 2-3 times of molybdenum-iron,
Step 3, mixed flux is laid on platinum crucible bottom and madial wall, with the speed less than 15 DEG C/min by platinum crucible
300 DEG C are warmed up to, after being then well mixed molybdenum-iron and oxidant platinum crucible is put into, it is to avoid molybdenum-iron and oxidant and platinum earthenware
Crucible directly contact；
Step 4, platinum crucible is warmed up into 650 DEG C with the speed less than 15 DEG C/min, insulation 10min makes molybdenum-iron and oxidant
React completely；
Step 5, platinum crucible is cooled to room temperature, adds 100mg-140mg concentration for the NH of 400mg/mL4The Br aqueous solution, so
After be heated to 1100 DEG C insulation 5min-6min, be finally cooled to room temperature and obtain molybdenum-iron bead.
2. a kind of method for preparing molybdenum-iron bead according to claim 1, it is characterised in that：Mix in step 3 molten
Agent compares lithium metaborate by lithium metaborate and lithium tetraborate according to quality：Lithium tetraborate=1：2 mixing.
3. a kind of method for preparing molybdenum-iron bead according to claim 1, it is characterised in that：In melting in step 5
Heating and thermal insulation is carried out in equipment, in insulating process, platinum crucible stands heating 2min, then crucible rotation in fusion apparatus
And incline shake heating 3 ~ 4min, 30 ° ~ 45 ° of angle of inclination.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610872488.6A CN106645242A (en) | 2016-10-08 | 2016-10-08 | Method for preparing molybdenum iron glass fuse pieces |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610872488.6A CN106645242A (en) | 2016-10-08 | 2016-10-08 | Method for preparing molybdenum iron glass fuse pieces |
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| CN106645242A true CN106645242A (en) | 2017-05-10 |
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| CN201610872488.6A Pending CN106645242A (en) | 2016-10-08 | 2016-10-08 | Method for preparing molybdenum iron glass fuse pieces |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108982563A (en) * | 2018-08-03 | 2018-12-11 | 武汉科技大学 | The preparation method of the XRF analysis sheet glass of demolding aids effect |
| CN109270101A (en) * | 2018-09-10 | 2019-01-25 | 自贡硬质合金有限责任公司 | A method of utilizing lanthanum content in x-ray fluorescence spectrometry molybdenum product |
| CN111879802A (en) * | 2020-07-17 | 2020-11-03 | 南京钢铁股份有限公司 | Preparation and analysis method of X-ray fluorescence fuse piece for measuring molybdenum content in molybdenum oxide |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101526488A (en) * | 2008-03-03 | 2009-09-09 | 湖南华菱湘潭钢铁有限公司 | Method for analyzing components of iron ore by using X-ray fluorescence spectrum |
| CN101832891A (en) * | 2010-02-22 | 2010-09-15 | 河北钢铁股份有限公司邯郸分公司 | Iron alloy fusing sample preparation method for X-ray fluorescence spectrum analysis |
| CN102401756A (en) * | 2010-09-07 | 2012-04-04 | 鞍钢股份有限公司 | Preparation method for ferromolybdenum sample melting glass body |
| CN102426122A (en) * | 2011-09-07 | 2012-04-25 | 河北钢铁股份有限公司邯郸分公司 | Sample preparation method by fusing medium-carbon ferrochrome and high-carbon ferrochrome |
| CN102607934A (en) * | 2012-03-07 | 2012-07-25 | 河北钢铁股份有限公司邯郸分公司 | X-ray fluorescence spectroscopy analysis fusion sample preparation method of aluminum, manganese, calcium and iron alloy |
| CN103149074A (en) * | 2013-02-28 | 2013-06-12 | 攀钢集团攀枝花钢钒有限公司 | Molten sample preparation method of molybdenum, manganese, vanadium or chromium iron alloy sample for X-ray fluorescence spectroscopy |
-
2016
- 2016-10-08 CN CN201610872488.6A patent/CN106645242A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101526488A (en) * | 2008-03-03 | 2009-09-09 | 湖南华菱湘潭钢铁有限公司 | Method for analyzing components of iron ore by using X-ray fluorescence spectrum |
| CN101832891A (en) * | 2010-02-22 | 2010-09-15 | 河北钢铁股份有限公司邯郸分公司 | Iron alloy fusing sample preparation method for X-ray fluorescence spectrum analysis |
| CN102401756A (en) * | 2010-09-07 | 2012-04-04 | 鞍钢股份有限公司 | Preparation method for ferromolybdenum sample melting glass body |
| CN102426122A (en) * | 2011-09-07 | 2012-04-25 | 河北钢铁股份有限公司邯郸分公司 | Sample preparation method by fusing medium-carbon ferrochrome and high-carbon ferrochrome |
| CN102607934A (en) * | 2012-03-07 | 2012-07-25 | 河北钢铁股份有限公司邯郸分公司 | X-ray fluorescence spectroscopy analysis fusion sample preparation method of aluminum, manganese, calcium and iron alloy |
| CN103149074A (en) * | 2013-02-28 | 2013-06-12 | 攀钢集团攀枝花钢钒有限公司 | Molten sample preparation method of molybdenum, manganese, vanadium or chromium iron alloy sample for X-ray fluorescence spectroscopy |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108982563A (en) * | 2018-08-03 | 2018-12-11 | 武汉科技大学 | The preparation method of the XRF analysis sheet glass of demolding aids effect |
| CN108982563B (en) * | 2018-08-03 | 2021-02-19 | 武汉科技大学 | Method for preparing glass sheet for XRF analysis of release aid effect |
| CN109270101A (en) * | 2018-09-10 | 2019-01-25 | 自贡硬质合金有限责任公司 | A method of utilizing lanthanum content in x-ray fluorescence spectrometry molybdenum product |
| CN111879802A (en) * | 2020-07-17 | 2020-11-03 | 南京钢铁股份有限公司 | Preparation and analysis method of X-ray fluorescence fuse piece for measuring molybdenum content in molybdenum oxide |
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