CN108732160A - A kind of quick method for analyzing lithium content in spodumene sample of hydrofluoric acid resistant - Google Patents
A kind of quick method for analyzing lithium content in spodumene sample of hydrofluoric acid resistant Download PDFInfo
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- CN108732160A CN108732160A CN201810554232.XA CN201810554232A CN108732160A CN 108732160 A CN108732160 A CN 108732160A CN 201810554232 A CN201810554232 A CN 201810554232A CN 108732160 A CN108732160 A CN 108732160A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/69—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence specially adapted for fluids, e.g. molten metal
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Abstract
A kind of quick method for analyzing lithium content in spodumene sample of hydrofluoric acid resistant, including：Spodumene sample is added to high-purity HNO3And HF, the resolution in 3-5 stage is carried out, the temperature in each stage gradually rises, and temperature range is 130 DEG C -180 DEG C, and each stage digestion time is 10min-40min；Then ultra-pure water constant volume is used, solution to be measured is respectively taken identical two parts, a certain amount of lithium standard solution is added in a copy of it, two parts of solution are diluted to certain multiple, control solution acidity is percent by volume 1%, then it is measured using embedded liquid cathode glow discharge spectrometry, the lithium content in spodumene sample is obtained using standard addition method.The present invention shortens the molten mine time using micro-wave digestion, since Seal treatment reduces air pollution, since instrument uses resistance to HF systems, therefore it is omitted and catches up with the sour redissolution stage, it improves work efficiency, the equipments such as electric hot plate is saved, to more environment-friendly, test speed is fast, has in small-size laboratory or field and is extremely widely applied foreground.
Description
Technical field
The present invention relates to a kind of analysis methods, specifically, being related to one kind being based on embedded liquid cathode glow discharge
The method that spectrometer quickly measures lithium content in spodumene sample.
Background technology
Lithium is widely present in salt lake bittern, seawater, subsurface brine and lithium ore.China's lithium ore resources are abundant, wherein opening
Adopt using it is most be spodumene.China's spodumene ore resources are mainly distributed on the remote districts such as Sichuan, Xinjiang, on-site identification
Difficulty is big, and sample is transported to laboratory test and needs a large amount of human and material resources and financial support, thus is badly in need of establishing and is directed to lithium brightness
The fast and accurately field assay method of Li contents in stone.
Currently, in spodumene sample the assay method of Li have inductively coupled plasma emission spectrography (ICP-AES),
Atomic absorption spectrography (AAS) (FAAS), flame atomic emission pectrometry (FAES), inductively coupled plasma mass spectrometry (ICP-MS)
Deng, because these large-scale instrument and equipments are required for the flow conditions such as carrier gas, combustion gas and combustion-supporting gas, equipment instrument can not be made to minimize,
It is only limitted in experiment lab analysis.And gravimetric method, volumetric method in traditional analysis, the chromatography of ions, electrochemical method
Deng because cumbersome, it is long to measure the period, and the purpose quickly analyzed is not achieved.Portable energy dispersive x-ray fluorescence spectroscopic methodology
(ED-XRF) be field in-situ analysis one preferred technique, but limited, can not be analyzed light in spodumene sample by principle of instrument
Element Li.
Atmospheric pressure liquid cathode glow discharge emission spectrometer (SCGD-AES) is more next as a kind of novel detection instrument
More by the pro-gaze of analysis scholar, still, atmospheric pressure liquid cathode glow discharge system, which is substantially all, at present uses monochromator
The detecting system of+photoelectric multiplier, equipment instrument is larger, not readily portable, is often fixed on laboratory and irremovable,
Not as the precedent of field in-situ analysis.
Portable fluid cathode glow discharging spectrometer is easy to carry, has as lithium in field in-situ analysis spodumene
Potentiality, but the solution that its liquid cathode is overflowed by quartz capillary top is constituted with graphite electrode, and the structure is easily by containing HF's
Therefore solution corrosion needs to increase the step of catching up with HF before entering liquid cathode, process is complicated, before considerably increasing sample
Processing time is unfavorable for realizing quick analysis.
Embedded liquid cathode glow discharge spectrometry is using the corundum outer tube of resistance to HF corrosion with syringe needle cathode as embedded
Formula cathode simplifies the sample pretreatment process of spodumene, to shorten time for sample pretreatment, is suitable for field in-situ analysis
The lithium content of spodumene sample.Therefore, how to be established in spodumene sample using embedded liquid cathode glow discharge spectrometry
The rapid analysis method of lithium content realizes the lithium content in field assay spodumene, becomes the skill of prior art urgent need to resolve
Art problem.
Invention content
It is an object of the invention to propose that a kind of method of lithium content in quick analysis spodumene sample, utilization are embedded
Liquid cathode glow discharge spectrometry realizes the scene quickly analysis of hydrofluoric acid resistant.
For this purpose, the present invention uses following technical scheme：
A kind of quick method for analyzing lithium content in spodumene sample of hydrofluoric acid resistant, includes the following steps：
Micro-wave digestion step：Spodumene sample is added to high-purity HNO3And HF, it is put into microwave digestion device, is arranged
Good temperature and pressure, is cleared up, and the resolution is divided into 3-5 stage, and the temperature in each stage gradually rises, temperature range
It it is 130 DEG C -180 DEG C, each stage digestion time is 10min-40min；
Testing procedure：After counteracting tank is cooled to room temperature, counteracting tank is taken out, with ultra-pure water constant volume, shakes up spare, will wait for
It surveys solution and respectively takes identical two parts, a certain amount of lithium standard solution is added in a copy of it, and two parts of solution are diluted to certain times
Number, control solution acidity are percent by volume 1%, are then measured, are used using embedded liquid cathode glow discharge spectrometry
Standard addition method obtains the lithium content in spodumene sample.
Optionally, in the micro-wave digestion step, micro-wave digestion is 3 stages, and first stage temperature is 130 DEG C, when
Between be 10min；Second stage temperature is 150 DEG C, and the time is 10 min；Phase III temperature is 180 DEG C, time 40min.
Optionally, in the micro-wave digestion step, the ratio of sample and acid is：The spodumene sample of about 50mg is added
HNO high-purity 1mL3High-purity HF with 1mL.
Optionally, in the testing procedure, constant volume ratio is the spodumene sample pair of about 50mg in micro-wave digestion step
25mL should be settled to.
Optionally, in the testing procedure, the diluted multiple of solution is 10 times or 20 times.
The present invention shortens the molten mine time using micro-wave digestion, since Seal treatment reduces air pollution, due to embedded
Formula liquid cathode glow discharge spectrometry uses resistance to HF systems, therefore is omitted and catches up with the sour redissolution stage, improves work efficiency,
Acid is not caught up in the wild, the equipments such as electric hot plate is saved, to more environment-friendly.Point of Li elements can be carried out anywhere or anytime
Analysis test, the molten a collection of sample of mine test are less than 2 hours, have in small-size laboratory or field and be extremely widely applied foreground.
Relative to conventional method, molten mine needs three day time, and upper machine needs the Advanced Concepts Laboratory in constant temperature and humidity to carry out.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail.It is understood that tool described herein
Body embodiment is used only for explaining the present invention rather than limitation of the invention.
Applied microwave resolution of the present invention, shortens the molten mine time, and instrument uses resistance to HF systems, therefore is omitted and catches up with acid multiple
It in the molten stage, improves work efficiency, does not catch up with acid in the wild, the equipments such as electric hot plate are saved, to more environment-friendly.To make
The analysis test of Li elements can be carried out using embedded liquid cathode glow discharge spectrometry anywhere or anytime by obtaining, small-sized
Laboratory or field, which have, is extremely widely applied foreground.
The present invention is as follows：
Micro-wave digestion step：Spodumene sample is placed in counteracting tank, for example, in special polytetrafluoro counteracting tank, is added
High-purity HNO3And HF, counteracting tank is closed the lid and is mounted on fixed frame, is put into microwave digestion device, temperature is set
Degree and pressure control device, are actuated for clearing up, and the resolution is divided into 3-5 stage, and the temperature in each stage gradually rises,
Temperature range is 130 DEG C -180 DEG C, and each stage digestion time is 10min-40min；
In a preferred embodiment, micro-wave digestion is 3 stages, and first stage temperature is 130 DEG C, and the time is
10min；Second stage temperature is 150 DEG C, time 10min；Phase III temperature is 180 DEG C, time 40min.
In micro-wave digestion step, the ratio of sample and acid is：It is high-purity that 1mL is added in the spodumene sample of about 50mg
HNO3High-purity HF with 1mL.
Since, containing there are many different powder, each sample heating meeting difference carries out microwave and disappears stage by stage in ore sample
Solution, temperature gradually rises, and can enable and ensure that at maximum temperature i.e. 180 DEG C, the molten mine time of various samples is consistent, and
And compression shock caused by dissolving generates gas can be reduced in the low temperature time of molten mine.
Testing procedure：After counteracting tank is cooled to room temperature, counteracting tank is taken out, with ultra-pure water constant volume, ratio is micro-wave digestion
The spodumene sample correspondence of about 50mg is settled to 25mL in step, shakes up spare, solution to be measured is respectively taken identical two parts,
Two parts of solution are diluted to certain multiple by middle a a certain amount of lithium standard solution of addition, such as 10 times, 20 times etc., control solution
Acidity is percent by volume 1%, is then measured using embedded liquid cathode glow discharge spectrometry, using standard addition method
(only needing 2 points) obtains the lithium content in spodumene sample.
Therefore, the present invention shortens the molten mine time using micro-wave digestion, since Seal treatment reduces air pollution, by
Resistance to HF systems are used in embedded liquid cathode glow discharge spectrometry, therefore is omitted and catches up with the sour redissolution stage, improve work
Efficiency does not catch up with acid in the wild, the equipments such as electric hot plate is saved, to more environment-friendly.Li elements can be carried out anywhere or anytime
Analysis test, a collection of sample of molten mine test is less than 2 hours, before small-size laboratory or field have and be extremely widely applied
Scape.Relative to conventional method, molten mine needs three day time, and upper machine needs the Advanced Concepts Laboratory in constant temperature and humidity to carry out.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, cannot recognize
The specific implementation mode of the fixed present invention is only limitted to this, for those of ordinary skill in the art to which the present invention belongs, not
Be detached from present inventive concept under the premise of, several simple deduction or replace can also be made, all shall be regarded as belonging to the present invention by
The claims submitted determine protection domain.
Claims (5)
1. the method for lithium content, includes the following steps in a kind of quick analysis spodumene sample of hydrofluoric acid resistant：
Micro-wave digestion step：Spodumene sample is added to high-purity HNO3And HF, it is put into microwave digestion device, sets temperature
And pressure, cleared up, the resolution is divided into 3-5 stage, and the temperature in each stage gradually rises, temperature range be 130 DEG C-
180 DEG C, each stage digestion time is 10min-40min；
Testing procedure：After counteracting tank is cooled to room temperature, take out counteracting tank, with ultra-pure water constant volume, shake up it is spare, by solution to be measured
Identical two parts are respectively taken, a certain amount of lithium standard solution is added in a copy of it, two parts of solution is diluted to certain multiple, control is molten
Liquid acidity is percent by volume 1%, is then measured using embedded liquid cathode glow discharge spectrometry, using standard addition method
Obtain the lithium content in spodumene sample.
2. the method for lithium content, feature exist in the quick analysis spodumene sample of hydrofluoric acid resistant according to claim 1
In：
In the micro-wave digestion step, micro-wave digestion is 3 stages, and first stage temperature is 130 DEG C, time 10min；The
Two-stage temperature is 150 DEG C, time 10min；Phase III temperature is 180 DEG C, time 40min.
3. the method for lithium content, feature exist in the quick analysis spodumene sample of hydrofluoric acid resistant according to claim 1
In：
In the micro-wave digestion step, the ratio of sample and acid is：The high-purity HNO of 1mL are added in the spodumene sample of about 50mg3
High-purity HF with 1mL.
4. the method for lithium content, feature exist in the quick analysis spodumene sample of hydrofluoric acid resistant according to claim 1
In：
In the testing procedure, the spodumene sample correspondence that constant volume ratio is about 50mg in micro-wave digestion step is settled to
25mL。
5. the method for lithium content, feature exist in the quick analysis spodumene sample of hydrofluoric acid resistant according to claim 1
In：
In the testing procedure, the diluted multiple of solution is 10 times or 20 times.
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| CN201810554232.XA CN108732160A (en) | 2018-06-01 | 2018-06-01 | A kind of quick method for analyzing lithium content in spodumene sample of hydrofluoric acid resistant |
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| CN201810554232.XA CN108732160A (en) | 2018-06-01 | 2018-06-01 | A kind of quick method for analyzing lithium content in spodumene sample of hydrofluoric acid resistant |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105223050A (en) * | 2015-08-28 | 2016-01-06 | 中国地质科学院矿产综合利用研究所 | Method for measuring scandium in bauxite by microwave digestion inductively coupled plasma spectrometry |
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2018
- 2018-06-01 CN CN201810554232.XA patent/CN108732160A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105223050A (en) * | 2015-08-28 | 2016-01-06 | 中国地质科学院矿产综合利用研究所 | Method for measuring scandium in bauxite by microwave digestion inductively coupled plasma spectrometry |
Non-Patent Citations (1)
| Title |
|---|
| 刘晓 等: "内嵌式液体阴极辉光放电光谱仪快速测定锂辉石中的锂", 《分析实验室》 * |
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Application publication date: 20181102 |