CN108181420A - Method for rapidly determining ion adsorption type rare earth element - Google Patents
Method for rapidly determining ion adsorption type rare earth element Download PDFInfo
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- CN108181420A CN108181420A CN201611123644.5A CN201611123644A CN108181420A CN 108181420 A CN108181420 A CN 108181420A CN 201611123644 A CN201611123644 A CN 201611123644A CN 108181420 A CN108181420 A CN 108181420A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
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Abstract
the invention discloses a method for rapidly determining ion adsorption type rare earth elements, wherein an ore sample is naturally air-dried or dried, crushed to-2 mm, dried, 1.0-15.0 g of the sample is put into a 250m L triangular flask, ammonium sulfate solution 100m L with the mass concentration of 2-6% is added, the triangular flask is shaken until the ore sample is uniformly distributed in the solution, the triangular flask is fixed on an oscillator, the triangular flask is vibrated and leached for 30-150 minutes, then ore pulp is dry-filtered in a colorimetric tube by using rapid filter paper, the solutions are respectively diluted, and the rare earth element content in the solution is determined by using an inductively coupled plasma mass spectrometer.
Description
Technical field
The present invention relates to rock-mineral analysis technical field, more particularly to a kind of quick measure of ion adsorption type re element
Method.
Background technology
At present, the common method for measuring content of rare earth is oxalates-gravimetric method and chlorophosphonazo Ⅲ photometry, but oxalates
Gravimetric method is there are operating procedure is complicated, the analytic process time is long, and to deposit measurement range small, by thorium for chlorophosphonazo Ⅲ luminosity rule
The shortcomings of serious interference.Therefore it is subject to certain restrictions in the practical application that both methods is measured in content of rare earth.And this
The content of rare earth that two methods can be measured is the content of rare earth of all phases, and be not suitable for as ion adsorption type re element
Analysis method.In current analytical technology standard and patent document, there is not yet the quick analysis about ion adsorption type re
Test method, the research of the measure of relevant ions absorbent type rare earth elements is detected in the report of related journals document, however it is soaked
Ore deposit method is mostly soaked using column, and due to weathering crust type Rare Earth Mine clay content height, leaching process argillization is serious, column leaching permeance property
Difference, elution speed is slow, and analytical cycle is more common in 1 day or more, seriously affects analysis efficiency.
Invention content
In order to overcome the above-mentioned deficiencies of the prior art, the present invention provides a kind of quick surveys of ion adsorption type re element
Determine method.
The technical solution adopted in the present invention is：Ore sample is through natural air drying or drying, broken to be machined to -2mm, baking
It is dry, 1.0~15.0 grams of samples are taken in 250mL triangular flasks, and addition mass concentration is 2~6% ammonium sulfate 100mL, shakes three
Angle bottle to sample ore is uniformly distributed in solution, and triangular flask is fixed on the oscillator, concussion leaching 30~150 minutes.Then, will
Ore pulp does filtering in colorimetric cylinder with fast grade filter paper, solution is taken to be diluted respectively, is surveyed with icp ms
Determine solution Rare Earth Element Contents, the ion adsorption type re elemental analysis period of the invention is generally at 2.5 hours.
Compared with prior art, the invention has the advantages that ore grain size is thick when leaching, sample segment processing is omitted
Flow, and phase analysis can be easily separated, hence it is evident that the ion adsorption type re elemental analysis period is shortened, greatly improves rare earth elemental analysis
Efficiency.
Specific embodiment
Example 1
1mL top pure grade concentrated nitric acids is taken to be diluted in 100mL distilled water
It accurately weighs 50g analytical pure sulfuric acid ammoniums to be dissolved in 1000mL distilled water, is 4.0 with ammonium hydroxide and sulfuric acid regulation solution pH.
Prepare 15 kinds of single rare earth oxide standard solution（1000µg/mL）：It is weighed respectively through 0.1 gram through 950 DEG C of calcinations
The single rare earth oxide of one hour is respectively placed in 15 200mL beakers, is added in the dissolving of 50% nitric acid of 10mL, is added peroxidating
Hydrogen, low-temperature heat dissolving is complete, removes and is cooled to room temperature, solution is moved into respectively in the volumetric flask of 15 100mL, is diluted with water to
Scale shakes up, and single rare earth oxide concentration is 1000 μ g/mL in this solution.
Prepare mixed rare-earth oxide standard solution：Pipette respectively 15 kinds of single rare earth oxide standard solution 10mL in
In 100mL volumetric flasks, shaken up with 0.5% nitric acid dilution constant volume dilution scale.15 rare earth oxide standard solution are dense in this solution
It spends for 100 μ g/mL.
Prepare mixed rare-earth oxide standard solution：Mixed rare-earth oxide standard solution 10mL is pipetted respectively in 1000mL
In volumetric flask, shaken up with 0.5% nitric acid dilution constant volume dilution scale.15 kinds of rare earth oxide concentration of standard solution are 1 in this solution
µg/mL。
1000 μ g/mL of lithium standard solution：There is a card standard purchased from national non-ferrous metal and electronic material analysis inspection center
Solution.
1000 μ g/mL of cobalt standard solution：There is a card standard purchased from national non-ferrous metal and electronic material analysis inspection center
Solution.
What 1000 μ g/mL of indium standard solution were purchased from national non-ferrous metal and electronic material analysis inspection center has the card standard molten
Liquid.
What 1000 μ g/mL of uranium standard solution were purchased from national non-ferrous metal and electronic material analysis inspection center has the card standard molten
Liquid.
Mixing tuning liquid：Four kinds of each 1mL of solution of lithium cobalt indium uranium are pipetted respectively in 1000mL volumetric flasks, are determined with 1% nitric acid
It is dissolved in 1000mL volumetric flasks.
Rhodium standard solution：What 100 μ g/mL were purchased from national non-ferrous metal and electronic material analysis inspection center has the card standard molten
Liquid.
Rhodium inner mark solution：It pipettes rhodium standard solution in 10mL 2.9 and in 1000mL volumetric flasks, dilutes scale with 1% nitric acid,
Rhodium concentration is 1 μ g/mL in this solution.
The preparation of standard series：Pipette suitable mischmetal standard solution（1µg/mL）Be configured to standard working solution add it is suitable
Nitric acid and ammonium sulfate are measured, every standard point and prepare liquid is made to have identical nitric acid and ammonium sulfate concentrations.The standard series is shown in
Subordinate list 1
1 standard series of subordinate list（ µg/L）
Liquid is tuned with the mixing that concentration is respectively 1 μ g/ml, instrument condition is optimized, makes instrumental sensitivity, stability, oxygen
The indices such as compound ion yield reach testing requirements.Instrument working parameter sees attached list 2.
2 Instrument working parameter of subordinate list
A concentration of 0,0.1,1.0,10,100 μ g/L standard solution of 15 kinds of rare earth oxide elemental standard solutions is prepared respectively to add in
Ammonium sulfate and nitric acid make standard working solution identical with the ammonium sulfate concentrations of sample to be tested.
5.00 gram of 100 mesh sample is weighed in 250mL triangular flasks, adds 5% ammonium sulfate 100mL, stirs evenly, concussion leaching
After 90 minutes, solution does filtering in colorimetric cylinder, pipettes solution 5.00mL in 100mL volumetric flasks, with 1% nitric acid constant volume, shakes
It is even.Divide and take solution in 100mL volumetric flasks, dilute scale, mixing with 1% nitric acid.By test solution and standard series be carried out at the same time etc. from
Daughter mass spectrograph measures.
Analysis result is represented with following formula
W（RexOy）/10-6=
In formula m be sampling amount, unit g；V1 points take liquor capacity, Unit/mL；V0 leaching liquid volumes, Unit/mL, V constant volumes,
Unit/mL.
The sample analysis result is：
| Sample number into spectrum | Sample presentation number | RexOy |
| 2016XDF15972 | K mountains 5H2D | 540 |
| 2016XDF15975 | 16-K mountains 39H4D | 349 |
| 2016XDF15978 | 16-K mountains 5H7D | 525 |
Example 2
All solution are prepared, and instrument calibration, analysis calculation method and example 1 are identical.1.00 gram of 100 mesh sample is weighed in 250mL
In triangular flask, add 2% ammonium sulfate 100mL, stir evenly, after concussion leaches 30 minutes, solution does filtering in colorimetric cylinder, pipettes
Solution 5.00mL, with 1% nitric acid constant volume, shakes up in 100mL volumetric flasks.Divide and take solution in 100mL volumetric flasks, with 1% nitric acid
Dilute scale, mixing.Test solution and standard series are carried out at the same time plasma mass spectrograph to measure.
The sample analysis result is：
| Sample number into spectrum | Sample presentation number | RexOy |
| 2016XDF15972 | K mountains 5H2D | 565 |
| 2016XDF15975 | 16-K mountains 39H4D | 362 |
| 2016XDF15978 | 16-K mountains 5H7D | 544 |
Outer inspection situation：
Claims (4)
1. a kind of rapid assay methods of ion adsorption type re element
A kind of rapid assay methods of ion adsorption type re element, it is characterised in that：Include the following steps：
A, ore sample is through natural air drying, and the broken maximum particle diameter that is machined to is -2mm.
2.b, taking 1.0~15.0 grams of drying samples, addition mass concentration is 2~6% ammonium sulfates in 250mL triangular flasks
100mL shakes triangular flask to sample ore and is uniformly distributed in solution, and triangular flask is fixed on the oscillator, concussion leaching rare earth 30
~150 minutes；
C, ore pulp is done into filtering in colorimetric cylinder or other containers with fast grade filter paper, solution is taken to be diluted constant volume respectively；
D, solution Rare Earth Element Contents are measured with icp ms.
3. a kind of rapid assay methods of ion adsorption type re element according to claim 1, it is characterised in that：Step
Ore reduction is machined to grain size as -2mm in a, leaches 1.0~15.0 grams of sample size.
4. a kind of rapid assay methods of ion adsorption type re element according to claim 1, it is characterised in that：Step
The mass concentration of ammonium sulfate is 2~6% in b, and it is 5-10 to leach liquid-solid ratio (V/W), and leaching equipment is oscillator, oscillation frequency
Rate is unlimited, and the use of any equipment for having an oscillation action should all be within the scope of present claims, rare earth leaching time 30~150
Minute.
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| CN201611123644.5A CN108181420A (en) | 2016-12-08 | 2016-12-08 | Method for rapidly determining ion adsorption type rare earth element |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0579983A (en) * | 1991-09-20 | 1993-03-30 | Sumitomo Electric Ind Ltd | Analyzing method for rare earth element in glass |
| CN103076292A (en) * | 2012-12-27 | 2013-05-01 | 中国地质科学院矿产资源研究所 | System and method for quantitatively evaluating concentration of rare earth in water body based on ground reflection spectrum |
| CN105803227A (en) * | 2016-03-29 | 2016-07-27 | 江西理工大学 | Method of leaching cerium in colloid phase from ion adsorption type rare earth ores |
-
2016
- 2016-12-08 CN CN201611123644.5A patent/CN108181420A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0579983A (en) * | 1991-09-20 | 1993-03-30 | Sumitomo Electric Ind Ltd | Analyzing method for rare earth element in glass |
| CN103076292A (en) * | 2012-12-27 | 2013-05-01 | 中国地质科学院矿产资源研究所 | System and method for quantitatively evaluating concentration of rare earth in water body based on ground reflection spectrum |
| CN105803227A (en) * | 2016-03-29 | 2016-07-27 | 江西理工大学 | Method of leaching cerium in colloid phase from ion adsorption type rare earth ores |
Non-Patent Citations (2)
| Title |
|---|
| 代小吕 等: "电感耦合等离子体质谱（ICP-MS）法测定离子吸附型稀土矿中的浸出稀土元素", 《中国无机分析化学》 * |
| 胡珊玲 等: "超声波强化浸取离子型稀土矿中稀土", 《冶金分析》 * |
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Effective date of registration: 20191118 Address after: No. 82, Xinzhuang Road, Wudang District, Guiyang, Guizhou Applicant after: Guizhou Geology Mineral Center Lab Applicant after: NO.5 Geological Brigade of Guizhou Geological and Mineral Exploration and Development Bureau Address before: No. 82, Xinzhuang Road, Wudang District, Guiyang, Guizhou Applicant before: Guizhou Geology Mineral Center Lab |
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