CN106896007A - A kind of leach extraction method of the full lithium of soil - Google Patents
A kind of leach extraction method of the full lithium of soil Download PDFInfo
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- CN106896007A CN106896007A CN201710119424.3A CN201710119424A CN106896007A CN 106896007 A CN106896007 A CN 106896007A CN 201710119424 A CN201710119424 A CN 201710119424A CN 106896007 A CN106896007 A CN 106896007A
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- soil
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- concentrated nitric
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- 239000002689 soil Substances 0.000 title claims abstract description 40
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 30
- 238000000605 extraction Methods 0.000 title claims abstract description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 230000029087 digestion Effects 0.000 claims abstract description 18
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000428 dust Substances 0.000 claims abstract description 9
- 238000005516 engineering process Methods 0.000 claims abstract description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000007605 air drying Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 229910052783 alkali metal Inorganic materials 0.000 description 5
- 150000001340 alkali metals Chemical class 0.000 description 5
- 238000011084 recovery Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003339 best practice Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/24—Earth materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/24—Earth materials
- G01N33/248—Earth materials related to manure as a biological product
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Immunology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Remote Sensing (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
A kind of disclosure of the invention leach extraction method of the full lithium of soil, leach extraction method selection desert grey soil, 3 kinds of digestion agents are concentrated nitric acid, concentrated nitric acid and redistilled water, concentrated nitric acid and perchloric acid, respectively by volume 1:50 and 1:Under the conditions of 100, respectively it is put into 3 and disappears and boil pipe, then each plus 1ml hydrofluoric acid, stand overnight, triangular flask is placed on electric hot plate, add hydrogen peroxide, small funnel is added a cover, is cleared up at 240 DEG C of temperature 80 DEG C, cleared up for 60 DEG C every 30min ladder-elevating temperatures, continue to clear up if prepare liquid is not clarified, the prepare liquid for preparing is clarified solution, after the completion of clearing up, it is cooled to room temperature, liquid relief is reconfigured at 5 ‰ dust technologies to volumetric flask, and 50 ml are settled to the dust technology.The efficient extraction to elemental lithium in soil is the method achieve, the present invention is best suited for desert grey soil, other basic soils also have reference value.
Description
Technical field
The present invention relates to a kind of leach extraction method of the full lithium of soil.
Technical background
Lithium is biological element needed by human, and it is the side for meeting human body to lithium demand most safe and feasible that lithium is obtained from food
Method, but cereal and vegetables lithium content level are relatively low, long-term consumption is difficult to meet normal demand of the human body to lithium, can influence human body
Health and social stability.For growing for plant, lithium may be considered as a kind of unnecessary element by it, but can be all of
Plant absorption (Aral and Vecchio-Sadus, 2008).Low dosage lithium supplies (Kalinowska beneficial to plant growth
et al.,2013)(Schweigart,1962；Susan,2009；Kalinowska et al.,2013；Aral et al.,
2008；Hawrylak et al., 2012), but lithium content is too high in soil not only influences plant normal growth, can also be by food
Thing chain influences health.In recent years, the full state research both at home and abroad to alkali metal in soil is more, but relevant alkali metal lithium grinds
Study carefully less.
At present, more research has been carried out to the full state of soil alkali metal, that alkali metal in soil is extracted and be separate is most normal
It is chemical reagent extraction method with method.The extraction of the full state of soil alkali metal, with reference to full sodium and the extracting method of full potassium, and explores
Different digestion agents.
The content of the invention
It is an object of the present invention to provide a kind of leach extraction method of the full lithium of soil, the method selection desert grey soil, 3 kinds of extractions
Agent is concentrated nitric acid, concentrated nitric acid and redistilled water, concentrated nitric acid and perchloric acid, respectively by volume 1:50 and 1:Under the conditions of 100, respectively
It is put into 3 to disappear and boil pipe, then each plus 1ml hydrofluoric acid, stands overnight, triangular flask is placed on electric hot plate, adds hydrogen peroxide, plus
Cover small funnel, cleared up at 80 DEG C -240 DEG C of temperature, cleared up for 60 DEG C every 30min ladder-elevating temperatures, if prepare liquid is not clarified after
Continuous to clear up, the prepare liquid for preparing is clarified solution, after the completion of clearing up, is cooled to room temperature, and liquid relief is reconfigured at 5 ‰ dilute to volumetric flask
Nitric acid, 50ml is settled to the dust technology.The efficient extraction to elemental lithium in soil is the method achieve, the present invention is best suited for
Desert grey soil, other basic soils also have reference value.
A kind of leach extraction method of the full lithium of soil of the present invention, follow these steps to carry out：
The treatment of a, soil：Selection desert grey soil, natural air drying crosses 0.1mm sieves；
The digestion agent selection of the full lithium of b, soil：It is concentrated nitric acid, volume ratio=1 to select 3 kinds of digestion agents respectively:1 secondary steaming
Distilled water and concentrated nitric acid, volume ratio=3:1 concentrated nitric acid and perchloric acid；
C, soil full lithium is cleared up：Triangular flask, volumetric flask, dropper and the funnel that will be used use volume ratio 1:1 nitric acid
After solution soaked for 1 night, dried with redistilled water flushing stand-by；By the desert grey soil of step a and step b digestion agents by volume 1:
50 and 1:100 weigh standby respectively, and the desert grey soil that will first weigh in proportion is respectively put into 3 and disappears and boil pipe respectively, then by 3 kinds of extractions
Agent concentrated nitric acid, volume ratio=1:1 redistilled water and concentrated nitric acid, volume ratio=3:1 concentrated nitric acid and perchloric acid is separately added into
Respectively disappear in boiling pipe, it is last each plus 1ml hydrofluoric acid to stand overnight, triangular flask is placed on electric hot plate, it is 30% pair to add concentration
Oxygen water 3ml, adds a cover small funnel, is cleared up at 80 DEG C -240 DEG C of temperature, is cleared up for 60 DEG C every 30min ladder-elevating temperatures, if prepare liquid
Do not clarify, continue to clear up, the prepare liquid for preparing is clarified solution, after the completion of clearing up, is cooled to room temperature, and liquid relief is matched somebody with somebody to volumetric flask
Concentration is put for 5 ‰ dust technologies, 50ml is settled to the dust technology, while doing blank.
Brief description of the drawings
Fig. 1 is extracting effect figure of the difference digestion agent of the invention to full lithium；Whether tri- letters of abc are represented has conspicuousness
Difference, identical letter is represented does not have significant difference, and different letters is represented has significant difference；Digestion agent 1 is
10ml concentrated nitric acids；Digestion agent 2 is 5ml redistilled waters and 5ml concentrated nitric acids；Digestion agent 3 is 7.5ml concentrated nitric acids and 2.5ml chlorine high
Acid.
Specific embodiment
Embodiment
The treatment of a, soil：Selection desert grey soil natural air drying, crosses 0.1mm sieves；
The digestion agent selection of the full lithium of b, soil：It is concentrated nitric acid, volume ratio=1 to select 3 kinds of digestion agents respectively:1 secondary steaming
Distilled water and concentrated nitric acid, volume ratio=3:1 concentrated nitric acid and perchloric acid；
C, soil full lithium is cleared up：Triangular flask, volumetric flask, dropper and the funnel that will be used use volume ratio 1:1 nitric acid
After solution soaked for 1 night, dried with redistilled water flushing stand-by；By the desert grey soil of step a and step b digestion agents by volume 1:
50 and 1:100 weigh respectively it is standby, first by volume ratio 1:50 and 1:100 desert grey soil for weighing respectively are put into 3 and disappear and boil pipe respectively,
6 parts altogether, then by 3 kinds of digestion agent concentrated nitric acids, volume ratio=1:1 redistilled water and concentrated nitric acid, volume ratio=3:1 dense nitre
Acid and perchloric acid are separately added into 6 parts and respectively disappear and boil pipe, finally add 1ml hydrofluoric acid in 6 parts each disappear boils pipe, stand
At night, triangular flask is placed on electric hot plate, addition concentration is 30% hydrogen peroxide 3ml, small funnel is added a cover, at 80 DEG C -240 DEG C of temperature
Clear up, cleared up for 60 DEG C every 30min ladder-elevating temperatures, continue to clear up if prepare liquid is not clarified, the prepare liquid for preparing is clarification
Liquid, after the completion of clearing up, is cooled to room temperature, and liquid relief to volumetric flask, configuration concentration is 5 ‰ dust technologies, is settled to the dust technology
50ml, while doing blank.
As can be seen from Figure 1：The extracting effect of the full lithium of soil compares：In material ratio 1:Under conditions of 100, digestion agent
7.5ml concentrated nitric acids and 2.5ml perchloric acid best results；
Recovery of standard addition, repeatability, precision test：
Recovery of standard addition is tested：Using mark-on method, take with 6 parts of a collection of known content sample, precision adds 100% same amount mark
Quasi- sample, determines respectively；Standard sample reagent：LiCl top pure grades are, it is necessary to the content for being converted into Li determines the specific consumption of standard sample；
Repeated experiment：It is repeated 6 times with same procedure and measures result；
Precision Experiment：Take test solution continuous sample introduction 6 times, determine integrating peak areas value, survey RSD values；
The recovery of standard addition of the full lithium best practice of the soil of table 1
The recovery of standard addition of full lithium is 99.03% (n=6, RSD=0.44%), the Repeatability checking result of full lithium
1.41% (n=6), the precision testing result of full lithium is 0.14% (n=6).
Claims (1)
1. the leach extraction method of the full lithium of a kind of soil, it is characterised in that follow these steps to carry out：
The treatment of a, soil：Selection desert grey soil, natural air drying crosses 0.1mm sieves；
The digestion agent selection of the full lithium of b, soil：It is concentrated nitric acid, volume ratio=1 to select 3 kinds of digestion agents respectively:1 redistilled water and
Concentrated nitric acid, volume ratio=3:1 concentrated nitric acid and perchloric acid；
C, soil full lithium is cleared up：Triangular flask, volumetric flask, dropper and the funnel that will be used use volume ratio 1:1 salpeter solution
After soaking for 1 night, dried with redistilled water flushing stand-by；By digestion agent in the desert grey soil in step a and step b by volume 1:
50 and 1:100 difference are standby, and the desert grey soil that will first weigh in proportion is respectively put into 3 and disappears and boil pipe respectively, then 3 kinds of digestion agents are dense
Nitric acid, volume ratio=1:1 redistilled water and concentrated nitric acid, volume ratio=3:1 concentrated nitric acid and perchloric acid is separately added into respectively to disappear and boils
Guan Zhong, it is last each to add 1ml hydrofluoric acid, stand overnight, triangular flask is placed on electric hot plate, addition concentration is 30% hydrogen peroxide
3ml, adds a cover small funnel, is cleared up at 80 DEG C -240 DEG C of temperature, is cleared up for 60 DEG C every 30min ladder-elevating temperatures, if prepare liquid is not clear
Clear then continue to clear up, the prepare liquid for preparing is clarified solution, after the completion of clearing up, is cooled to room temperature, and liquid relief to volumetric flask is configured dense
It is 5 ‰ dust technologies to spend, and 50 ml are settled to the dust technology, while doing blank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710119424.3A CN106896007A (en) | 2017-03-02 | 2017-03-02 | A kind of leach extraction method of the full lithium of soil |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710119424.3A CN106896007A (en) | 2017-03-02 | 2017-03-02 | A kind of leach extraction method of the full lithium of soil |
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| CN106896007A true CN106896007A (en) | 2017-06-27 |
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| CN201710119424.3A Pending CN106896007A (en) | 2017-03-02 | 2017-03-02 | A kind of leach extraction method of the full lithium of soil |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108693016A (en) * | 2018-04-24 | 2018-10-23 | 广东省农业科学院农产品公共监测中心 | A kind of pre-treating method for the detection of batch heavy metal in soil |
| CN110333209A (en) * | 2019-07-11 | 2019-10-15 | 恩施土家族苗族自治州农业科学院(恩施土家族苗族自治州硒应用技术与产品开发研究院) | A kind of detection method of soil available Se |
| CN114252308A (en) * | 2020-09-24 | 2022-03-29 | 中国科学技术大学苏州研究院 | Method for extracting and measuring effective selenium in soil |
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2017
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108693016A (en) * | 2018-04-24 | 2018-10-23 | 广东省农业科学院农产品公共监测中心 | A kind of pre-treating method for the detection of batch heavy metal in soil |
| CN110333209A (en) * | 2019-07-11 | 2019-10-15 | 恩施土家族苗族自治州农业科学院(恩施土家族苗族自治州硒应用技术与产品开发研究院) | A kind of detection method of soil available Se |
| CN114252308A (en) * | 2020-09-24 | 2022-03-29 | 中国科学技术大学苏州研究院 | Method for extracting and measuring effective selenium in soil |
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