CN105738394A - X-ray fluorescence spectrum analysis method for primary and secondary components in rubidium ore - Google Patents
X-ray fluorescence spectrum analysis method for primary and secondary components in rubidium ore Download PDFInfo
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- CN105738394A CN105738394A CN201610114140.0A CN201610114140A CN105738394A CN 105738394 A CN105738394 A CN 105738394A CN 201610114140 A CN201610114140 A CN 201610114140A CN 105738394 A CN105738394 A CN 105738394A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses an X-ray fluorescence spectrum analysis method of primary and secondary components in rubidium ores, which comprises the following specific processes: screening standard substances of rubidium-containing rock ore and soil and water system sediments, designing a standard curve, selecting a mixed flux for melting to prepare a standard sample, determining instrument analysis conditions, correcting a matrix and a spectral line overlapping effect, establishing the standard curve, and determining silicon, aluminum, calcium, iron, sodium, potassium, titanium and rubidium in the rubidium ore by using a fixed value sample to verify the accuracy and reproducibility of the method; according to the invention, a melting sample preparation is selected as a pretreatment means for rubidium ore X-ray fluorescence spectrum analysis, compared with powder pressing, the particle size effect and the matrix effect to a certain extent can be eliminated, and compared with the traditional chemical and instrument analysis methods, the method for analyzing the major and minor components of the rubidium ore by using the X-ray fluorescence spectrum is time-saving and labor-saving; the invention has the advantages of low detection limit, wide linear range, high analysis speed and the like, and the average processing time of a single ore sample is not more than 20 min.
Description
Technical field
The invention belongs to the X-ray fluorescence spectra of major and minor component in screening technical field, particularly a kind of rubidium Ore containing rubidium rock ore deposit and soil, sediments and analyze method.
Background technology
Rubidium is relatively broad in distributed in nature, but previously research thinks that it there is no independent mineral deposit and exists, and the associated resources being only used as lithium ore deposit reclaims.Rubidium be manufacture electronic device (photomultiplier tube photocell), spectrophotometer, automatically control, spectroscopic assay, cinecolour, color television, radar, laser instrument and glass, pottery, electronic clock etc. important source material；In space technology, ion propeller and thermionic energy converter need substantial amounts of rubidium；The hydride of rubidium and boride can make propellant of high energy；Radioactivity rubidium can measure the mineral age, and the compound of rubidium is also applied to pharmacy, paper-making industry in addition, is important " three is rare " Strategic mineral resources.Along with " three is rare " mineral products are looked for the pay attention to day by day that miner makees by China, the ground such as Gansu, Inner Mongol is found that a collection of Large-super Large rubidium mineral deposit, rubidium (Rb in succession2O) grade 0.004% ~ 0.29%.The associating generally requiring multiple chemical analysis, instrument analytical method is measured for analyzing of the components such as silicon, aluminum, calcium, ferrum, sodium, potassium, titanium, rubidium in rubidium Ore, in Table 1, wherein titanium needs extra alkali fusion completely for ensureing to dissolve, and need to quantitatively add alkali metal ionization buffer when analyzing rubidium according to flame atomic absorption spectrometry.
Table 1 rubidium ore deposit major and minor component common analytical methods
The range of linearity and the advantage of repeatability and multielement analysis that X-ray fluorescence spectra is outstanding make it be widely used in geological and mineral field, but there is no precedent processing this novel Mineral Resource Domain of rubidium ore deposit, therefore develop what a kind of XRF analysis method for rubidium ore deposit was a need for.
Summary of the invention
The X-ray fluorescence spectra that it is an object of the invention to develop major and minor component in a kind of rubidium Ore analyzes method, pre-treatment is selected MTG YBCO bulk to eliminate granularity effect, is carried software correction matrix and overlap of spectral lines effect by instrument with Criterion curve, thus realizing the accurate quantitative analysis to major and minor components such as silicon, aluminum, calcium, ferrum, sodium, potassium, titanium, rubidiums in rubidium Ore.
Present invention achieves above-mentioned purpose, technical scheme is as follows:
In a kind of rubidium Ore, the X-ray fluorescence spectra of major and minor component analyzes method, specifically comprises the following steps that
(1) at least 10 standard substance Criterion curves containing rubidium rock ore deposit and soil, sediments are selected；
(2) accurately weighing 8.000g mixed flux, pour in platinum yellow crucible, the mass ratio adding standard substance, mixed flux and standard substance is 1:10, adds and releasing agent, and mixed flux is 1:40 in the mass ratio of remover, stirring and evenly mixing；
(3) platinum yellow crucible is put into warmed up molten model machine, carry out molten sample, after terminating, take out natural cooling；
(4) after standard substance selected in step (1) has melted, scan each standard substance and determine element instrumental conditions to be measured；
(5) according to instrument condition analytical standard sample, Criterion curve；
(6) correction matrix and overlap of spectral lines effect, corrects the matrix effect of element to be measured beyond rubidium with Alpha Coefficient Method, and the matrix effect of rubidium then corrects with Compton scattering internal standard method, is absent from overlap of spectral lines between each component to be measured；
(7) definite value rubidium ore sample carried out MTG YBCO bulk by step (1) to (5) and analyze, the result obtained with step (6) is compared checking, if meeting requirement namely to come into operation, if result is unsatisfied with, then re-start matrix and overlap of spectral lines effect calibration.
Described mixed solvent is lithium tetraborate and lithium metaborate, lithium tetraborate: lithium metaborate=67:33.
Described releasing agent is ammonium iodide.
The Pt:Au=95:5 of described platinum yellow crucible.
Described platinum yellow crucible use before with 5 ~ 10%(volume ratio, v/v) nitric acid boils cleaning, with pure water after taking-up, 70 DEG C of dry for standby.
In step (3), the temperature that this method molten model machine used heats up is 1050 ~ 1100 DEG C.
This method molten sample equipment used is that TNRY-01C type X fluorescence spectrum analyzes the molten model machine of dedicated full-automatic, the product of Luoyang Te Nai experimental facilities company limited can be adopted, because of molten model machine model/parameter differences, revise corresponding molten sample's condition as the case may be, here molten sample program can be selected as follows: select mode of operation 1, molten sample temperature 1050 DEG C, fritting time 300s, molten sample time 300s, time of repose 30s.
Advantage of the present invention is as follows:
1.X ray fluorescence spectra, as the inorganic analysis instrument of a maturation, is widely used in the fields such as geological and mineral, petrochemical industry, environmental monitoring, has range of linearity width, high repeatability and other advantages.Silicon, aluminum, calcium, ferrum, sodium, potassium, titanium, rubidium eight component in applying X-ray fluorescence spectrum quantitative analysis rubidium ore sample of the present invention, data are accurate, simple and efficient, fully meet rubidium ore deposit and explore, select the demand of the aspects such as smelting.
2. the present invention is simple to operate, analyzes speed fast, compares traditional chemical, instrument analytical method can save a large amount of manpower and materials, and single-piece sample processing time is less than 20min.
Accompanying drawing explanation
Fig. 1 is the design flow diagram of the present invention.
Detailed description of the invention
The step that the present invention is embodied as is as follows:
First, select following 11 containing rubidium rock ore deposit and soil, sediments standard substance Criterion curve, its composition content is in Table 2.
Table 2 standard substance content
*, except being μ g/g except Rb, all the other are %.
Accurately weigh 8.0000g mixed flux (lithium tetraborate: lithium metaborate=67:33), pour in platinum yellow crucible, add 0.8000g standard substance, 0.2000 ammonium iodide, stir evenly with Glass rod.
It is as follows that TNRY-01C type X fluorescence spectrum analyzes the dedicated full-automatic molten sample program setting of molten model machine: mode of operation 1, molten sample temperature 1050 DEG C, fritting time 300s, molten sample time 300s, time of repose 30s.
Platinum yellow crucible is put into warmed up to 1050 DEG C and be incubated molten model machine more than 15min, run by setup program, after terminating, take out natural cooling.
After standard sequence has melted, scanning standard sample determines element passage to be measured, background and PHD (PulseHeightDistribution, pulse height is distributed) bound, and instrumental conditions is in Table 3.
Table 3 instrumental conditions
With table 3 Instrumental condition analysis standard sample, Criterion curve, then with SuperQ5.1 software correction matrix and overlap of spectral lines effect, the matrix effect of Rb corrects with Compton scattering internal standard method, the matrix effect of element to be measured is remained with Alpha Coefficient Method correction, overlap of spectral lines, concrete correction situation and each elemental standards curve intercept, slope it is absent from Table 4 between each component to be measured.
The correction of table 4 matrix effect
By definite value rubidium ore sample condition MTG YBCO bulk as described above, the construction method analysis of application institute, evaluation methodology accuracy and repeatability.Satisfied requirement can be come into operation immediately, if result is unsatisfied with, then re-starts matrix and overlap of spectral lines effect calibration.
Use the present invention that the rubidium composition of ores analytical standard material in the Research Institute of Chengdu is analyzed process as follows:
Accurately weigh 8.0000g mixed flux (lithium tetraborate: lithium metaborate=67:33), pour in platinum yellow crucible, add 0.8000g sample, 0.2000g releasing agent ammonium iodide, stir evenly with Glass rod.Platinum yellow crucible is put into warmed up to 1050 DEG C and be incubated molten model machine more than 15min, fritting 300s, molten sample 300s, stand 30s, melted terminate after take out, upper machine analysis after sample natural cooling.
Analyze sample with this method, result and classical way relatively in Table 5, this method accuracy fully meets the requirement of rubidium Ore routine analysis as known from Table 5.
Table 5 method validation result of the test
Carrying out precision test (8 Duplicate Samples) with No. 2 samples, result is in Table 6, and this method repeatability is good as seen from the results in Table 6.
Claims (7)
1. in a rubidium Ore, the X-ray fluorescence spectra of major and minor component analyzes method, it is characterised in that step is as follows:
(1) at least 10 standard substance Criterion curves containing rubidium rock ore deposit and soil, sediments are selected；
(2) accurately weighing 8.000g mixed flux, pour in platinum yellow crucible, the mass ratio adding standard substance, mixed flux and standard substance is 1:10, adds and releasing agent, and mixed flux is 1:40 in the mass ratio of remover, stirring and evenly mixing；
(3) platinum yellow crucible is put into warmed up molten model machine, carry out molten sample, after terminating, take out natural cooling；
(4) after standard substance selected in step (1) has melted, scan each standard substance and determine element instrumental conditions to be measured；
(5) according to instrument condition analytical standard sample, Criterion curve；
(6) correction matrix and overlap of spectral lines effect, corrects the matrix effect of element to be measured beyond rubidium with Alpha Coefficient Method, and the matrix effect of rubidium then corrects with Compton scattering internal standard method, is absent from overlap of spectral lines between each component to be measured；
(7) definite value rubidium ore sample carried out MTG YBCO bulk by step (1) to (5) and analyze, the result obtained with step (6) is compared checking, if meeting requirement namely to come into operation, if result is unsatisfied with, then re-start matrix and overlap of spectral lines effect calibration.
2. in a kind of rubidium Ore according to claim 1, the X-ray fluorescence spectra of major and minor component analyzes method, it is characterised in that: in step (2), described mixed solvent is lithium tetraborate and lithium metaborate, lithium tetraborate: lithium metaborate=67:33.
3. in a kind of rubidium Ore according to claim 1, the X-ray fluorescence spectra of major and minor component analyzes method, it is characterised in that: in step (2), described releasing agent is ammonium iodide.
4. in a kind of rubidium Ore according to claim 1, the X-ray fluorescence spectra of major and minor component analyzes method, it is characterised in that: the Pt:Au=95:5 of described platinum yellow crucible.
5. in a kind of rubidium Ore according to claim 1, the X-ray fluorescence spectra of major and minor component analyzes method, it is characterised in that: described platinum yellow crucible boils cleaning with the nitric acid of volume ratio 5 ~ 10% before using, with pure water after taking-up, 70 DEG C of dry for standby.
6. in a kind of rubidium Ore according to claim 1, the X-ray fluorescence spectra of major and minor component analyzes method, it is characterised in that: in step (3), the temperature that described molten model machine heats up is 1050 ~ 1100 DEG C.
7. in a kind of rubidium Ore according to claim 1, the X-ray fluorescence spectra of major and minor component analyzes method, it is characterized in that: in step (3), described molten model machine is that TNRY-01C type X fluorescence spectrum analyzes the molten model machine of dedicated full-automatic, molten sample program is as follows: molten sample temperature 1050 DEG C ~ 1100 DEG C, fritting time 300s, molten sample time 300s, time of repose 30s.
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Cited By (11)
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| CN106168588A (en) * | 2016-08-31 | 2016-11-30 | 广西出入境检验检疫局危险品检测技术中心 | A kind of measure the method for potassium content in potassium perchlorate used for fireworks and crackers |
| CN106290436A (en) * | 2016-08-31 | 2017-01-04 | 广西出入境检验检疫局危险品检测技术中心 | A kind of measure the method for potassium content in fireworks and firecrackers Potassium Hydrogen Phthalate |
| CN106885815A (en) * | 2017-03-22 | 2017-06-23 | 中国石油大学(华东) | A kind of method that depositional environment is differentiated based on element XRF methods in sandstone |
| CN107576680A (en) * | 2017-09-07 | 2018-01-12 | 中国地质科学院矿产综合利用研究所 | Method for analyzing niobium-tantalum ore by low dilution ratio melting X-ray fluorescence spectrum |
| CN107677529A (en) * | 2017-09-26 | 2018-02-09 | 贵研资源（易门）有限公司 | Noble Metal Rhodium, iridium and the ruthenium analysis sample-pretreating method of complicated indissoluble |
| CN109324074A (en) * | 2018-10-30 | 2019-02-12 | 湖南航天磁电有限责任公司 | The method of x-ray fluorescence spectrometry strontium permanent-magnet ferrite component content |
| CN109975384A (en) * | 2017-12-28 | 2019-07-05 | 中国科学院过程工程研究所 | A kind of method of Metal Distribution rate in detection rock |
| CN110082379A (en) * | 2019-04-09 | 2019-08-02 | 湛江出入境检验检疫局检验检疫技术中心 | The method that MTG YBCO bulk-X-ray fluorescence spectra surveys 14 kinds of major and minor components in chrome ore |
| CN110208251A (en) * | 2019-06-20 | 2019-09-06 | 安徽创谱仪器科技有限公司 | Plasma emission spectroscopy interference correction method |
| JP2020165961A (en) * | 2019-03-27 | 2020-10-08 | 住友金属鉱山株式会社 | Ore sample analysis method |
| CN115575432A (en) * | 2022-10-12 | 2023-01-06 | 山东省地质科学研究院 | Method for measuring major and minor components in alunite ore by using X-ray fluorescence spectrum |
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Cited By (13)
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| CN106168588A (en) * | 2016-08-31 | 2016-11-30 | 广西出入境检验检疫局危险品检测技术中心 | A kind of measure the method for potassium content in potassium perchlorate used for fireworks and crackers |
| CN106290436A (en) * | 2016-08-31 | 2017-01-04 | 广西出入境检验检疫局危险品检测技术中心 | A kind of measure the method for potassium content in fireworks and firecrackers Potassium Hydrogen Phthalate |
| CN106885815A (en) * | 2017-03-22 | 2017-06-23 | 中国石油大学(华东) | A kind of method that depositional environment is differentiated based on element XRF methods in sandstone |
| CN107576680A (en) * | 2017-09-07 | 2018-01-12 | 中国地质科学院矿产综合利用研究所 | Method for analyzing niobium-tantalum ore by low dilution ratio melting X-ray fluorescence spectrum |
| CN107576680B (en) * | 2017-09-07 | 2020-10-23 | 中国地质科学院矿产综合利用研究所 | Method for analyzing niobium-tantalum ore by low dilution ratio melting X-ray fluorescence spectrum |
| CN107677529A (en) * | 2017-09-26 | 2018-02-09 | 贵研资源（易门）有限公司 | Noble Metal Rhodium, iridium and the ruthenium analysis sample-pretreating method of complicated indissoluble |
| CN109975384A (en) * | 2017-12-28 | 2019-07-05 | 中国科学院过程工程研究所 | A kind of method of Metal Distribution rate in detection rock |
| CN109324074A (en) * | 2018-10-30 | 2019-02-12 | 湖南航天磁电有限责任公司 | The method of x-ray fluorescence spectrometry strontium permanent-magnet ferrite component content |
| JP2020165961A (en) * | 2019-03-27 | 2020-10-08 | 住友金属鉱山株式会社 | Ore sample analysis method |
| JP7400558B2 (en) | 2019-03-27 | 2023-12-19 | 住友金属鉱山株式会社 | Analysis method for ore samples |
| CN110082379A (en) * | 2019-04-09 | 2019-08-02 | 湛江出入境检验检疫局检验检疫技术中心 | The method that MTG YBCO bulk-X-ray fluorescence spectra surveys 14 kinds of major and minor components in chrome ore |
| CN110208251A (en) * | 2019-06-20 | 2019-09-06 | 安徽创谱仪器科技有限公司 | Plasma emission spectroscopy interference correction method |
| CN115575432A (en) * | 2022-10-12 | 2023-01-06 | 山东省地质科学研究院 | Method for measuring major and minor components in alunite ore by using X-ray fluorescence spectrum |
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