CN108051468A - X-ray fluorescence spectrum method for simultaneously analyzing fluorite, barite and celestite - Google Patents
X-ray fluorescence spectrum method for simultaneously analyzing fluorite, barite and celestite Download PDFInfo
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- CN108051468A CN108051468A CN201810063776.6A CN201810063776A CN108051468A CN 108051468 A CN108051468 A CN 108051468A CN 201810063776 A CN201810063776 A CN 201810063776A CN 108051468 A CN108051468 A CN 108051468A
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- 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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Abstract
The invention discloses an X-ray fluorescence spectrum method for simultaneously and quantitatively analyzing fluorite, barite and celestite in ores, which comprises the following specific steps: mixing barite standard substance, fluorite standard substance, rare earth ore standard substance, strontium sulfate and strontium carbonate to prepare artificial standard, melting by using mixed flux (lithium tetraborate: lithium metaborate =12:22), scanning the obtained standard sample to determine instrument conditions, and establishing a standard curve after correcting matrix effect; after a sample to be detected is treated by a strontium-containing acetic acid solution, filtering, separating and interfering, adding a mixed flux (lithium tetraborate: lithium metaborate =12:22) for melting after precipitation and filter paper ashing, and analyzing by a standard curve in the previous process; the invention selects X-ray fluorescence spectrum as an analytical instrument, simplifies the pretreatment operation, realizes the simultaneous quantitative analysis of three components of fluorite, barite and celestite in the ore, and is suitable for the mineral product analysis which is independent or contains fluorite, barite and celestite.
Description
Technical field
It is particularly a kind of to analyze fluorite, barite simultaneously the present invention relates to the analysis method of fluorite, barite and celestine
And the X-ray fluorescence spectra method of celestine, fluorite in ore, barite and celestine can be measured by the method for the present invention simultaneously
Content.
Background technology
Fluorite is industrial the most useful fluorine mineral, is usually used in metallurgical and chemical industry.Barite is as baric sulfate
Mineral, are the essential industry raw mineral materials for producing barium and barium compound, while the also exacerbation as oil, gas drilling mud
Agent.One of the key industry mineral of celestine as strontium, it is all kinds of containing strontium compound for refining and preparing.Dechang, the west of the country
The nonmetal mineral resources such as fluorite, barite, celestine are associated in the rare earth mineral deposit of the ground such as prosperous part, it is after Mineral separation to assign more
It is stored in rare-earth tailing, recycling above-mentioned resource by hydrometallurgical flowsheets is conducive to improve mineral products comprehensive utilization ratio, but also to dividing
Analysis test job proposes challenge.
It need to individually be sampled using classical way analysis fluorite, barite, celestine, again with EDTA capacity after separation is disturbed
Method or FAAS/ICP-OES analyses measure, and cumbersome, flow is tediously long.Calcium, strontium, barium are all alkaline-earth metal, and property is close, it is difficult to
Separation is complete, causes to analyze CaF using EDTA volumetric methods2Generally require supplement correction；With flame atomic absorption spectrometry
（FAAS）Or inductively coupled plasma spectrometry method（ICP-OES）Measure BaSO4Middle Ba or SrSO4It is both needed to filter twice before middle Sr
Separation, time and effort consuming.
For x ray fluorescence spectrometry, the outstanding range of linearity, good reappearance make it be obtained in geological and mineral field
Extensive use has been arrived, but has analyzed CaF in sample simultaneously by XRF2、BaSO4And SrSO4Analysis method there is no precedent.
The content of the invention
The present invention's provides X-ray fluorescence spectra method that is a kind of while analyzing fluorite, barite and celestine, the party
Method be by the existing barite of mixing portion, fluorite Standard Reference Materials for Determination, laboratory internal rare earth ore standard substance and
Strontium sulfate, strontium carbonate etc. prepare labor standard substance, and standard sample of photo, designated instrument condition is made after labor standard material melts
Scanning obtains each element response intensity to be measured, and standard curve is established with it；Sample to be tested is handled by containing strontium acetic acid solution, separation
Impurity is disturbed, is melted after precipitation and filter paper ashing with mixed flux, machine is analyzed on gained print, can be simultaneously by the method for the present invention
Measure the content of fluorite, barite and celestine in ore.The present invention analyzes CaF in sample by XRF simultaneously2、BaSO4And
SrSO4, hence it is evident that simplify operating procedure, shorten the pre-treatment time, reduce reagent consumption, be conducive to fluorite, barite and
The utilization of its spar resource, therefore it is studied and promotes meaningful.
The present invention realizes above-mentioned purpose, and idiographic flow is as follows：
First, barite ore Standard Reference Materials for Determination GBW07812, GBW07813, fluorite Standard Reference Materials for Determination are selected
GBW07251, GBW07253, laboratory internal rare earth ore standard substance, strontium sulfate, strontium carbonate mixed preparing labor standard object
Matter；Then, standard sample of photo being made with mixed flux melting labor standard substance, scanning standard print determines instrumental conditions,
Whole standard sample of photo are analyzed with this condition one by one, by 5.1 software systems correction of matrix effect of SuperQ, establish standard curve；
Sample to be tested is separated by filtration interference, is melted after precipitation and filter paper ashing with mixed flux, gained sample to contain the dissolving of strontium acetic acid solution
On piece machine is analyzed, and can measure the content of fluorite in ore, barite and celestine simultaneously.
The concrete analysis step of the above method is as follows：
（1）Select barite ore Standard Reference Materials for Determination GBW07812, GBW07813, fluorite Standard Reference Materials for Determination
GBW07251, GBW07253, laboratory internal rare earth ore standard substance and strontium sulfate (spectroscopic pure), strontium carbonate (spectroscopic pure)
Mixed preparing labor standard substance.
（2）Accurately weigh 8.0000 g lithium borate salt mixed fluxs（Lithium tetraborate：Lithium metaborate=12:22）, pour into platinum yellow
Crucible [Pt:Au=95:5] [platinum yellow crucible is using preceding with 5 ~ 10% in（Volume ratio, v/v）Hydrochloric acid boils cleaning, with pure water after taking-up
Washing, 70 DEG C are dried for standby], labor standard substance, 0.1000 g releasing agent ammonium iodides described in 0.8000 g are added in, with glass
Stick stirs and evenly mixs.
（3）Platinum yellow crucible is put into the molten model machine for having warmed up to 1100 DEG C and keeping the temperature more than 15 min, by setup program
Operation, after take out treat its natural cooling.
It sample equipment is melted used in this method analyzes dedicated full-automatic for TNRY-01C types X fluorescence spectrum and melt model machine [Luoyang spy is resistance to
Experimental facilities Co., Ltd, can be suitably modified to molten sample's condition in this method because melting model machine model/parameter differences], melt sample program
It is as follows：Operating mode 1 is selected, melts 1100 DEG C, fritting time 300s of sample temperature, melts sample time 300s, time of repose 20s.
（4）After the completion for the treatment of that labor standard substance melts, scanning gained print determines element instrumental conditions to be measured.
（5）The instrumental conditions determined with step 4 scan each standard substance print one by one, obtain each element response to be measured
Intensity establishes standard curve with it.By 5.1 software correction matrix effects of SuperQ, fundamental parameters method correction is carried with system
Each element matrix effect to be measured in addition to Sr, Ba, two element matrix effect of Sr, Ba are then corrected with theoretical coefficient method.
Actual sample needs to exclude the interference of the potential impurity such as calcium carbonate, strontium carbonate, barium carbonate and calcium sulfate, stream before melting
Journey is as follows：
0.8000 g samples to be tested accurately are weighed in 100 mL glass beakers, add in 25 mL acetic acid solutions containing strontium, are capped surface
Ware, 30 min of slightly boiling, during which rocks mixing every 10 min, after with deionization to wash surface plate and wall of cup [after purging molten
About 30 ~ 40 mL of liquid total volume], 35 mL ethyl alcohol are added, are stirred evenly with glass bar, stand 30 min.Pass through quantitative filter paper mistake at a slow speed
Filter is washed beaker with deionized water and is precipitated each 5 ~ 6 times, then filter paper and precipitation is transferred in platinum yellow crucible, low temperature drying
After being warming up to 800 DEG C of ashing in Muffle furnace, 8.0000 g mixed fluxs and 0.1 g releasing agent ammonium iodides are added in after cooling, after
Continue the same standard substance of melting operation, machine is analyzed on gained print, and analysis can obtain the content of fluorite, barite and celestine.
Present invention provide that under conditions of, calcirm-fluoride at most dissolves 5 mg in acetic acid solution containing strontium, therefore is calculating sample
Middle CaF2This part should be included in during %.
The preparation of the acetic acid solution containing strontium：It weighs 0.1000 g anhydrous strontium chlorides to pour into 1000 mL glass beakers, add in
100 mL distilled water with glass bar stirring and dissolving, are added in 50 mL acetic acid, then add distilled water to 500 mL, stirred with glass bar
It is even, it is transferred to spare in tool plug vial, the solution as acetic acid solution containing strontium.
Advantage of the present invention is as follows：
The present invention is realized by MTG YBCO bulk-X-ray fluorescence spectra analysis method to fluorite, barite and celestine in ore
It is measured while three kinds of components, first handles sample to be tested, selective dissolution wherein carbonate, calcium sulfate etc. to contain strontium acetic acid solution
Impurity is then separated by filtration, and is precipitated with filter paper directly in MTG YBCO bulk with being ashed in platinum yellow crucible, is added mixed flux and the demoulding
Agent MTG YBCO bulk simplifies operating procedure compared to classical way, shortens the pre-treatment time, reduces reagent consumption, can be simultaneously
Three kinds of fluorite, barite and celestine components in determination sample possess stronger innovative and practicability.
Description of the drawings
Fig. 1 is the method flow schematic diagram of the present invention.
Specific embodiment
Select barite ore Standard Reference Materials for Determination GBW07812, GBW07813, fluorite Standard Reference Materials for Determination
GBW07251, GBW07253, laboratory rare earth ore standard substance and strontium sulfate, strontium carbonate（Spectroscopic pure）It is mixed with certain proportion
It closes, prepares labor standard substance, composition see the table below 1.
1 standard substance of table forms
Each component unit is % in table 1.
Weigh 8.0000 g mixed fluxs（Lithium tetraborate：Lithium metaborate=12:22）, pour into platinum yellow crucible, add in
0.8000 g standard substances, 0.1000 g releasing agent ammonium iodides, are stirred and evenly mixed with glass bar.
Platinum yellow crucible is put into 1100 DEG C of molten model machines, by following procedure MTG YBCO bulk：Operating mode 1 is selected, during fritting
Between be arranged to 300 s, melt 300 s of the sample time, 20 s of time of repose, after take out platinum yellow crucible, natural cooling.
After the completion of 15 labor standard material melts, scanning gained print determines instrumental conditions, is shown in Table 2.
2 instrumental conditions of table
* because of difference between instrument, more than 2 θ only referred to the setting of background angle.
The * element Channel scan times to be measured（Except La, Ce are 40+20 s, at 2 θ angles+background angle at outside）It is 20+
10 s。
With 2 Instrumental analysis condition of table scanning standard print one by one, each element response intensity to be measured is recorded, thus establishes mark
Directrix curve.Carry out basal image by 5.1 software systems of SuperQ, respectively to be treated beyond fundamental parameters method correction Sr, Ba
Element matrix effect is surveyed, Sr, Ba element matrix effect are then corrected with theoretical coefficient method.
0.8000 g samples to be tested accurately are weighed in 100 mL glass beakers, add in 25 mL acetic acid solutions containing strontium, capping
Surface plate, 30 min of slightly boiling, during which rocks mixing every 10 min, after surface plate and wall of cup [purging washed with deionization
About 30 ~ 40 mL of overall solution volume afterwards], 35 mL ethyl alcohol are added, are stirred evenly with glass bar, stand 30 min.By quantitatively filtering at a slow speed
Paper filters, and washs beaker with deionized water and precipitates each 5 ~ 6 times, then filter paper and precipitation is transferred in platinum yellow crucible, low temperature
Drying adds in 8.0000 g mixed fluxs and 0.1 g releasing agent iodate after being warming up to 800 DEG C of ashing in Muffle furnace after cooling
Ammonium, subsequent melt operate same standard substance, and machine is analyzed on gained print.Analysis gained CaO%, SrO%, BaO%, convert in proportion
That is CaF2%=（1.3924CaO%+0.60）%、SrSO4%=（1.7727SrO%）%、BaSO4%=（1.5252BaO%）%.
The sample voluntarily prepared with inventor investigates this method accuracy, is shown in Table 3；With actual sample（n=4）Investigation method
Precision is shown in Table 4.
3 accuracy experimental result of table
4 Precision Experiment result of table
From table 3,4 result of table, the method for the present invention analysis result is accurate, and precision is good.
Claims (7)
1. analyzing the X-ray fluorescence spectra method of fluorite, barite and celestine simultaneously, characterization step is as follows：
First, barite ore Standard Reference Materials for Determination GBW07812, GBW07813, fluorite Standard Reference Materials for Determination are selected
GBW07251, GBW07253, laboratory internal rare earth ore standard substance, strontium sulfate, strontium carbonate mixed preparing labor standard object
Matter；Then, standard sample of photo being made with mixed flux melting labor standard substance, scanning standard print determines instrumental conditions,
Whole standard sample of photo are analyzed with this condition one by one, by 5.1 software systems correction of matrix effect of SuperQ, establish standard curve；
Sample to be tested is separated by filtration interference, is melted after precipitation and filter paper ashing with mixed flux, gained sample to contain the dissolving of strontium acetic acid solution
On piece machine is analyzed, and can measure the content of fluorite in ore, barite and celestine simultaneously.
2. X-ray fluorescence spectra method that is according to claim 1 while analyzing fluorite, barite and celestine, special
Sign is：When the selection mixed flux melting prepares standard sample of photo, the dilution ratio of mixed flux and labor standard substance is
10：1, melting temperature is 1100 DEG C.
3. X-ray fluorescence spectra method that is according to claim 1 while analyzing fluorite, barite and celestine, special
Sign is：The mixed flux is lithium borate salt mixed flux, is specially lithium tetraborate：Lithium metaborate=12:22.
4. the X-ray fluorescence spectra of fluorite, barite and celestine is analyzed while according to claim 1-3 any one
Method, it is characterised in that be as follows：
（1）Select barite ore Standard Reference Materials for Determination GBW07812, GBW07813, fluorite Standard Reference Materials for Determination
GBW07251, GBW07253, laboratory internal rare earth ore standard substance and strontium sulfate, strontium carbonate mixed preparing labor standard
Substance；
（2）Lithium borate salt mixed flux is weighed, is poured into platinum yellow crucible, adds in labor standard substance and releasing agent ammonium iodide, with
Glass bar stirs and evenly mixs；Lithium borate salt mixed flux, labor standard substance, the ratio of releasing agent ammonium iodide are 8:0.8:0.1；
（3）Platinum yellow crucible is put into the molten model machine for having warmed up to 1100 DEG C and keeping the temperature more than 15 min, transported by setup program
Row, after take out treat its natural cooling；
（4）After the completion for the treatment of that labor standard substance melts, scanning gained print determines element instrumental conditions to be measured；
（5）Step（4）In the instrumental conditions that determine scan each standard sample of photo one by one, obtain each element response intensity to be measured,
Standard curve is established with it；By 5.1 software correction matrix effects of SuperQ, with system carry fundamental parameters method correction except Sr,
Each element matrix effect to be measured outside Ba, two element matrix effect of Sr, Ba are then corrected with theoretical coefficient method；
（6）0.8000 g samples to be tested accurately are weighed in 100 mL glass beakers, add in 25 mL acetic acid solutions containing strontium, capping
Surface plate, 30 min of slightly boiling, during which rocks mixing every 10 min, after surface plate and wall of cup washed with deionization, add
35 mL ethyl alcohol, are stirred evenly with glass bar, stand 30 min；It is filtered, beaker is washed with deionized water and sunk by quantitative filter paper at a slow speed
It forms sediment each 5 ~ 6 times, then filter paper and precipitation is transferred in platinum yellow crucible, low temperature drying is after being warming up to 800 DEG C of ashes in Muffle furnace
Change, 8.0000 g mixed fluxs and 0.1 g releasing agent ammonium iodides are added in after cooling, subsequent melt operates same standard substance, gained
Machine is analyzed on print, while measures the content of fluorite in ore, barite and celestine.
5. X-ray fluorescence spectra method that is according to claim 4 while analyzing fluorite, barite and celestine, special
Sign is：The platinum yellow crucible boils cleaning using preceding with the hydrochloric acid of volume ratio 5 ~ 10%, with pure water, 70 DEG C of bakings after taking-up
It is dry spare.
6. X-ray fluorescence spectra method that is according to claim 4 while analyzing fluorite, barite and celestine, special
Sign is：The molten sample equipment analyzes dedicated full-automatic for TNRY-01C types X fluorescence spectrum and melts model machine, and it is as follows to melt sample program：Choosing
Operating mode 1 is selected, melts 1100 DEG C, 300 s of fritting time of sample temperature, melts 300 s of sample time, 20 s of time of repose.
7. X-ray fluorescence spectra method that is according to claim 4 while analyzing fluorite, barite and celestine, special
Sign is：The preparation of the acetic acid solution containing strontium：It weighs 0.1000 g anhydrous strontium chlorides to pour into 1000 mL glass beakers, add
Enter 100 mL distilled water, with glass bar stirring and dissolving, add in 50 mL acetic acid, distilled water is then added to 500 mL, with glass bar
It stirs evenly, is transferred to spare in tool plug vial, the solution as acetic acid solution containing strontium.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956674A (en) * | 2018-06-28 | 2018-12-07 | 中国石油天然气股份有限公司 | Method and device for representing reservoir clay mineral conversion |
| CN108982563A (en) * | 2018-08-03 | 2018-12-11 | 武汉科技大学 | Method for preparing glass sheet for XRF analysis of release aid effect |
| CN109406616A (en) * | 2018-09-30 | 2019-03-01 | 中国地质大学（武汉） | A method of sulfate mineral sulfur isotope is measured by standard specimen of YF-2 barite |
| CN110530852A (en) * | 2019-10-16 | 2019-12-03 | 国家地质实验测试中心 | A method of inductively-coupled plasma spectrometer, which is decomposed, with mixed flux analyzes barite |
| CN110987903A (en) * | 2019-12-11 | 2020-04-10 | 华中科技大学 | LIBS matrix effect correction method and application thereof |
-
2018
- 2018-01-23 CN CN201810063776.6A patent/CN108051468A/en active Pending
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956674A (en) * | 2018-06-28 | 2018-12-07 | 中国石油天然气股份有限公司 | Method and device for representing reservoir clay mineral conversion |
| CN108982563A (en) * | 2018-08-03 | 2018-12-11 | 武汉科技大学 | Method for preparing glass sheet for XRF analysis of release aid 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 |
| CN109406616A (en) * | 2018-09-30 | 2019-03-01 | 中国地质大学（武汉） | A method of sulfate mineral sulfur isotope is measured by standard specimen of YF-2 barite |
| CN110530852A (en) * | 2019-10-16 | 2019-12-03 | 国家地质实验测试中心 | A method of inductively-coupled plasma spectrometer, which is decomposed, with mixed flux analyzes barite |
| CN110987903A (en) * | 2019-12-11 | 2020-04-10 | 华中科技大学 | LIBS matrix effect correction method and application thereof |
| CN110987903B (en) * | 2019-12-11 | 2021-06-11 | 华中科技大学 | LIBS matrix effect correction method and application thereof |
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