CN103411819B - Detect the preprocess method of boron impurity in sodium metasilicate - Google Patents
Detect the preprocess method of boron impurity in sodium metasilicate Download PDFInfo
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- CN103411819B CN103411819B CN201310343038.4A CN201310343038A CN103411819B CN 103411819 B CN103411819 B CN 103411819B CN 201310343038 A CN201310343038 A CN 201310343038A CN 103411819 B CN103411819 B CN 103411819B
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Abstract
The present invention relates to a kind of sodium metasilicate defects inspecting preprocess method, be specifically related to a kind of preprocess method detecting boron impurity in sodium metasilicate, sodium metasilicate sample is added NaOH solution to dissolve, and the adjust ph that adds water, then add sweet mellow wine, make the abundant complexing of the boron impurity in itself and sodium metasilicate, pass through extracted with diethyl ether again, be heated to volatilize completely by ether after extraction, Liquid Residue adds nitric acid and the constant volume that adds water, and finally detects.The invention has the advantages that: (1) boron element inrichment is obvious, sodion and silicate ion is not almost had in solution to be checked, largely reducing the impact of matrix effect, the recovery of boron element can be promoted to more than 95% from 80 ~ 82%, and the method detection limit of boron element is down to 0.2ppm by 1ppm; (2) pollution to sampling system is avoided: (3) method is simply easy to operation, improves accuracy in detection.
Description
Technical field
The present invention relates to a kind of sodium metasilicate defects inspecting preprocess method, be specifically related to a kind of preprocess method detecting boron impurity in sodium metasilicate.
Background technology
At present, China has become world energy sources production and consumption big country, but per capita energy's level of consumption is also very low.Along with development that is economic and society, China's energy demand is by sustainable growth, for current energy shortage situation, deep thinking is all being carried out in countries in the world, and make great efforts to improve efficiency of energy utilization, promote the development and application of regenerative resource, reduce the dependence to Imported oil, strengthen energy security.
Solar energy power generating development in recent years as one of the important development direction of regenerative resource is swift and violent, and its proportion is increasing.According to " planning of regenerative resource Long-and Medium-term Development ", to the year two thousand twenty, China strives making solar electrical energy generation installed capacity reach 1.8GW(gigawatt), will 600GW be reached to the year two thousand fifty.Expect the year two thousand fifty, the electric power installation of Chinese regenerative resource will account for 25% of national electric power installation, and wherein photovoltaic generation installation will account for 5%.Before estimating the year two thousand thirty, the compound growth rate of Chinese sun power installed capacity will up to more than 25%.
Polysilicon is as the most desirable feedstock of solar cell, impurity wherein mainly contains metallic impurity and the non-metallic impuritiess such as boron, phosphorus such as iron, aluminium, calcium, and these impurity elements can reduce the Compound Degree of silicon crystal grain interface photo-generated carrier, and the Compound Degree of photo-generated carrier determines the photoelectric transformation efficiency of solar cell, removing these impurity so effective has vital effect in the application aspect of solar cell.
Conventional metallurgy method removes the impurity in polysilicon at present, and in the process route of metallurgy method, the first step is medium smelting technology, namely adopts slag former and the slag making of silicon liquid to react, removes the boron impurity in silicon liquid.Wherein, sodium metasilicate is that slag former constituent important in boron impurity technique in polysilicon is removed in slag making, and therefore in sodium metasilicate, the content of boron impurity is most important to final refining effect.Sodium metasilicate is soluble in water, its aqueous solution can directly detect, but the existence of a large amount of sodion and silicate ion causes matrix effect serious, greatly have impact on the detection accuracy of boron impurity, and seriously polluted to sampling system, this field still belongs to blank at present.
Summary of the invention
According to above the deficiencies in the prior art, the present invention proposes a kind of preprocess method detecting boron impurity in sodium metasilicate, and method is simple, can guarantee the accuracy that in sodium metasilicate, boron impurity detects, fill up the blank of this field detection technique with this.
A kind of preprocess method detecting boron impurity in sodium metasilicate of the present invention, sodium metasilicate sample is added NaOH solution to dissolve, and the adjust ph that adds water, then sweet mellow wine is added, make the abundant complexing of the boron impurity in itself and sodium metasilicate, then by extracted with diethyl ether, the ether after extraction is heated to volatilize completely, Liquid Residue adds nitric acid and the constant volume that adds water, and finally detects.
Preferred version is for comprising the following steps:
(1) 0.5 ~ 1.0g sodium metasilicate sample is joined in PTEE beaker;
(2) in beaker, add concentration is that the NaOH solution of 5wt% makes it dissolve sodium metasilicate sample completely, then adds water and regulates solution ph to 8.0 ~ 9.0;
(3) measuring concentration is 1wt% mannitol solution 1 ~ 2ml, adds in beaker, leaves standstill after concussion;
(4) solution in beaker is poured in pp separating funnel, washing beaker 2 ~ 3 times, by cleansing solution and in pp separating funnel;
(5) in separating funnel, add 4 ~ 5ml top grade absolute ether, leave standstill after concussion after forming layering, take out ether and be placed in beaker mutually;
(6) step (5) is repeated 2 ~ 3 times, collect all ether in beaker, beaker is placed in 25 ~ 30 DEG C of water-baths, be heated to ether volatilization completely;
(7) in beaker, add 2 ~ 3ml concentration is 35wt% nitric acid, and this solution is transferred to volumetric flask, washing beaker 2 ~ 3 times, in volumetric flask, is added water and is settled to 20ml by cleansing solution, finally detect it.
Wherein, after preferably adopting ultrasonic oscillation 3 ~ 5min in step (3), leave standstill 5 ~ 10min.
After preferably adopting artificial concussion 3 ~ 5min in step (5), leave standstill 5 ~ 10min.
The boron impurity content of solution in ICP-AES or ICP-MS measurement capacity bottle is preferably adopted in step (7).
In the present invention, sodium metasilicate sample is dissolved by NaOH solution, alkaline environment is utilized to prevent the hydrolysis of silicate ion, and then add the abundant complexing of boron impurity that mannitol solution makes in itself and sodium metasilicate sample, pass through extracted with diethyl ether again, be heated to volatilize completely by ether after extraction, Liquid Residue adds nitric acid and the constant volume that adds water, and finally detects.
The invention has the advantages that: (1) boron element inrichment is obvious, sodion and silicate ion is not almost had in solution to be checked, largely reducing the impact of matrix effect, the recovery of boron element can be promoted to more than 95% from 80 ~ 82%, and the method detection limit of boron element is down to 0.2ppm by 1ppm; (2) pollution to sampling system is avoided: (3) method is simply easy to operation, improves accuracy in detection.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1:
(1) 0.5g sodium metasilicate sample is joined in PTEE beaker;
(2) in beaker, add concentration is that the NaOH solution of 5wt% makes it dissolve sodium metasilicate sample completely, then adds water and regulates solution ph to 9.0;
(3) measuring concentration is 1wt% mannitol solution 1ml, adds in beaker, after adopting ultrasonic oscillation 3min, leaves standstill 5min;
(4) solution in beaker is poured in pp separating funnel, washing beaker 2 times, by cleansing solution and in pp separating funnel;
(5) in separating funnel, add 4ml top grade absolute ether, after adopting artificial concussion 3min, leave standstill 5min, after forming layering, take out ether and be placed in beaker mutually;
(6) step (5) is repeated 2 times, collect all ether in beaker, beaker is placed in 28 DEG C of water-baths, be heated to ether volatilization completely;
(7) in beaker, add 2ml concentration is 35wt% nitric acid, and this solution is transferred to volumetric flask, washing beaker 2 times, in volumetric flask, is added water and is settled to 20ml by cleansing solution, finally adopt the boron impurity content of solution in ICP-AES measurement capacity bottle.
Embodiment 2:
(1) 1.0g sodium metasilicate sample is joined in PTEE beaker;
(2) in beaker, add concentration is that the NaOH solution of 5wt% makes it dissolve sodium metasilicate sample completely, then adds water and regulates solution ph to 8.0;
(3) measuring concentration is 1wt% mannitol solution 2ml, adds in beaker, after adopting ultrasonic oscillation 5min, leaves standstill 10min;
(4) solution in beaker is poured in pp separating funnel, washing beaker 3 times, by cleansing solution and in pp separating funnel;
(5) in separating funnel, add 5ml top grade absolute ether, after adopting artificial concussion 5min, leave standstill 10min, after forming layering, take out ether and be placed in beaker mutually;
(6) step (5) is repeated 3 times, collect all ether in beaker, beaker is placed in 30 DEG C of water-baths, be heated to ether volatilization completely;
(7) in beaker, add 3ml concentration is 35wt% nitric acid, and this solution is transferred to volumetric flask, washing beaker 3 times, in volumetric flask, is added water and is settled to 20ml by cleansing solution, finally adopt the boron impurity content of solution in ICP-MS measurement capacity bottle.
Claims (4)
1. one kind is detected the preprocess method of boron impurity in sodium metasilicate, it is characterized in that: sodium metasilicate sample is added NaOH solution and dissolve, and the adjust ph that adds water, then sweet mellow wine is added, make the abundant complexing of the boron impurity in itself and sodium metasilicate, then by extracted with diethyl ether, the ether after extraction is heated to volatilize completely, Liquid Residue adds nitric acid and the constant volume that adds water, and finally detects; Specifically comprise the following steps:
(1) 0.5 ~ 1.0g sodium metasilicate sample is joined in PTEE beaker;
(2) in beaker, add concentration is that the NaOH solution of 5wt% makes it dissolve sodium metasilicate sample completely, then adds water and regulates solution ph to 8.0 ~ 9.0;
(3) measuring concentration is 1wt% mannitol solution 1 ~ 2ml, adds in beaker, leaves standstill after concussion;
(4) solution in beaker is poured in pp separating funnel, washing beaker 2 ~ 3 times, by cleansing solution and in pp separating funnel;
(5) in separating funnel, add 4 ~ 5ml top grade absolute ether, leave standstill after concussion after forming layering, take out ether and be placed in beaker mutually;
(6) step (5) is repeated 2 ~ 3 times, collect all ether in beaker, beaker is placed in 25 ~ 30 DEG C of water-baths, be heated to ether volatilization completely;
(7) in beaker, add 2 ~ 3ml concentration is 35wt% nitric acid, and this solution is transferred to volumetric flask, washing beaker 2 ~ 3 times, in volumetric flask, is added water and is settled to 20ml by cleansing solution, finally detect it.
2. the preprocess method of boron impurity in detection sodium metasilicate according to claim 1, after it is characterized in that adopting ultrasonic oscillation 3 ~ 5min in step (3), leaves standstill 5 ~ 10min.
3. the preprocess method of boron impurity in detection sodium metasilicate according to claim 1, after it is characterized in that adopting artificial concussion 3 ~ 5min in step (5), leaves standstill 5 ~ 10min.
4. the preprocess method of boron impurity in detection sodium metasilicate according to claim 1, is characterized in that the boron impurity content adopting solution in ICP-AES or ICP-MS measurement capacity bottle in step (7).
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| CN106153419A (en) * | 2016-07-22 | 2016-11-23 | 大工（青岛）新能源材料技术研究院有限公司 | A kind of pre-treating method of impurity in ICP AES detection high purity copper |
| CN106248465A (en) * | 2016-07-22 | 2016-12-21 | 大工（青岛）新能源材料技术研究院有限公司 | ICP AES measures the preprocess method of trace B constituent content in zinc oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102928483A (en) * | 2012-10-24 | 2013-02-13 | 西安航空动力股份有限公司 | Method for measuring boron element in copper-based soldering flux |
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| WO2002012129A1 (en) * | 2000-08-07 | 2002-02-14 | Sievers Instruments, Inc. | Low-level boron detection and measurement |
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| CN102928483A (en) * | 2012-10-24 | 2013-02-13 | 西安航空动力股份有限公司 | Method for measuring boron element in copper-based soldering flux |
Non-Patent Citations (2)
| Title |
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| 《多晶硅中硼含量的密闭消解-ICP-AES法测定》;田俊等;《分析测试学报》;20100930;第29卷(第9期);第962-965页 * |
| 《无定形硼粉中的总硼测定方法研究》;姜求韬等;《矿冶》;20120930;第21卷(第3期);第96页 * |
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Effective date of registration: 20160425 Address after: 266000 Qingdao Shandong blue Silicon Valley core zone Pioneer Center (Qingdao) new energy material Technology Research Institute Co., Ltd. Patentee after: Qingdao Engineering Technology Co., Ltd. Address before: Pudong solar energy industry base in Jimo city of Shandong Province, Qingdao City, 266234 Patentee before: Qingdao Longsheng Crystalline Silicon Science & Technology Co., Ltd. |