CN102539463A - X-ray fluorescent spectrometry for analyzing contents of 17 elements in organic silicon contact mass - Google Patents
X-ray fluorescent spectrometry for analyzing contents of 17 elements in organic silicon contact mass Download PDFInfo
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- CN102539463A CN102539463A CN 201110454581 CN201110454581A CN102539463A CN 102539463 A CN102539463 A CN 102539463A CN 201110454581 CN201110454581 CN 201110454581 CN 201110454581 A CN201110454581 A CN 201110454581A CN 102539463 A CN102539463 A CN 102539463A
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Abstract
The invention relates to an X-ray fluorescent spectrometry for analyzing contents of 17 elements in an organic silicon contact mass. The X-ray fluorescent spectrometry comprises the following steps of: preparing samples by using a powder pressing method, preparing standard samples by the self, establishing XRF (X-Ray Fluorescence) working curves of the elements, and showing that the relative standard deviations of the elements are less than 10% through experimental determination, wherein the degree of precision can meet the testing requirement of tracking production. Compared with an ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry), the X-ray fluorescent spectrometry has the advantage that the degree of accuracy of a determination result accurately meets the analytical error requirements of industrial silicon enterprise standards.
Description
Technical field
The present invention relates to a kind of x ray fluorescence spectrometry and analyze the content of 17 kinds of elements in the organosilicon contact.
Background technology
The ICP-AES method is mainly used in TRACE ELEMENTS ANALYSIS, and analyzable element is that most metal and silicon, phosphorus, sulphur etc. are a spot of nonmetal, totally 72 kinds.Be widely used in the ultimate analysis of quality control, the detection of ultramicro-element is especially in the water quality monitoring in environmental protection field.Can also detect macroelement, for example in the measurement of component, the element determination of principal ingredient.Use the contrast of Xray fluorescence spectrometer and ICP-AES method, the requirement of industrial silicon company standard analytical error is satisfied in accuracy.
Summary of the invention
The present invention uses Xray fluorescence spectrometer to measure the content of 17 kinds of elements in the contact.Through the powder pressing method sample preparation, the self-control standard model has been set up the XRF working curve of each element, through measuring the relative standard deviation of each element less than 10%, precision can satisfy follows the tracks of the production test requirement.
Because domestic xrf method of no use is analyzed the method for combined bed contact at present; On market, buy less than organosilicon contact standard model; We gather from ICP-AES method organosilicon contact trace analysis sample; The sample of gathering by best sample preparation article condition grinding, compressing tablet, is pressed best XRF measuring condition working sample intensity.Therefrom select to have ten to 20 in the sample of certain gradient according to the content range of 17 kinds of elements of institute's test sample article; Remove Si and adopt silicon fluoro acid potassium volumetric method (research institute and Jiangxi inspection center analysis result); Sulphur adopts outside the high frequency infrared ray carbon sulphur analyser analysis (research institute and Jiangxi inspection center analysis result), and other elements adopt the ICP-AES method to confirm its accurate concentration.Plumbous in the contact, two elements of sulphur are because concentration is too low, and change too for a short time, and it is too poor to draw the curve linear that comes out; In order to have drawn lead, sulphur working curve, we are employed in and add plumbous, sulphur national standard solution in the lower contact sample of impurity content, and flood sample with ultrapure water; Fully stir; Again on heating plate slowly the heating remove moisture to pasty state, again in baking oven fully the oven dry, confirm its accurate concentration with the ICP-AES method; Process standard model by same sample preparation condition grinding, compressing tablet again, measure intensity with XRF.With concentration is horizontal ordinate, and it is the working curve that ordinate is drawn each element that XRF measures intensity.
Advantage of the present invention significantly reduces analysis time, and a sample analysis shortened to 0.5 hour by original 4 hours, in time analyzes data-guiding production for workshop provides.
Embodiment
Embodiment 1:
From ICP-AES method organosilicon contact trace analysis sample, gather, the sample of gathering by best sample preparation article condition grinding, compressing tablet, is pressed best XRF measuring condition working sample intensity.Therefrom select to have ten to 20 in the sample of certain gradient according to the content range of 17 kinds of elements of institute's test sample article; Remove Si and adopt silicon fluoro acid potassium volumetric method (research institute and Jiangxi inspection center analysis result); Sulphur adopts outside the high frequency infrared ray carbon sulphur analyser analysis (research institute and Jiangxi inspection center analysis result), and other elements adopt the ICP-AES method to confirm its accurate concentration.Plumbous in the contact, two elements of sulphur are because concentration is too low, and change too for a short time, and it is too poor to draw the curve linear that comes out; In order to have drawn lead, sulphur working curve, we are employed in and add plumbous, sulphur national standard solution in the lower contact sample of impurity content, and flood sample with ultrapure water; Fully stir; Again on heating plate slowly the heating remove moisture to pasty state, again in baking oven fully the oven dry, confirm its accurate concentration with the ICP-AES method; Process standard model by same sample preparation condition grinding, compressing tablet again, measure intensity with XRF.With concentration is horizontal ordinate, and it is the working curve that ordinate is drawn each element that XRF measures intensity.
Claims (1)
1.X ray fluorescence spectrometry is analyzed the content of 17 kinds of elements in the organosilicon contact; It is characterized by: from ICP-AES method organosilicon contact trace analysis sample, gather; The sample of gathering by best sample preparation article condition grinding, compressing tablet, is pressed best XRF measuring condition working sample intensity.Therefrom select to have ten to 20 in the sample of certain gradient according to the content range of 17 kinds of elements of institute's test sample article; Remove Si and adopt silicon fluoro acid potassium volumetric method (research institute and Jiangxi inspection center analysis result); Sulphur adopts outside the high frequency infrared ray carbon sulphur analyser analysis (research institute and Jiangxi inspection center analysis result), and other elements adopt the ICP-AES method to confirm its accurate concentration.Plumbous in the contact, two elements of sulphur are because concentration is too low, and change too for a short time, and it is too poor to draw the curve linear that comes out; In order to have drawn lead, sulphur working curve, we are employed in and add plumbous, sulphur national standard solution in the lower contact sample of impurity content, and flood sample with ultrapure water; Fully stir; Again on heating plate slowly the heating remove moisture to pasty state, again in baking oven fully the oven dry, confirm its accurate concentration with the ICP-AES method; Process standard model by same sample preparation condition grinding, compressing tablet again, measure intensity with XRF.With concentration is horizontal ordinate, and it is the working curve that ordinate is drawn each element that XRF measures intensity.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110454581 CN102539463A (en) | 2011-12-30 | 2011-12-30 | X-ray fluorescent spectrometry for analyzing contents of 17 elements in organic silicon contact mass |
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| CN 201110454581 CN102539463A (en) | 2011-12-30 | 2011-12-30 | X-ray fluorescent spectrometry for analyzing contents of 17 elements in organic silicon contact mass |
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| CN102539463A true CN102539463A (en) | 2012-07-04 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103728328A (en) * | 2013-12-27 | 2014-04-16 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Content analyzing method of 16 elements in organic silicon powder sample |
| CN103852481A (en) * | 2014-03-12 | 2014-06-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for detecting components of elements in coated titanium dioxide |
| CN107228874A (en) * | 2017-06-29 | 2017-10-03 | 苏州浪声科学仪器有限公司 | The method of impurity in pressed powder x-ray fluorescence spectrometry metallic silicon |
| CN107656024A (en) * | 2017-11-13 | 2018-02-02 | 龙蟒佰利联集团股份有限公司 | A kind of assay method of titanium dioxide surface organosilicon stearic acid organic agent covering amount |
| CN111678935A (en) * | 2020-06-19 | 2020-09-18 | 承德金隅水泥有限责任公司 | Method for quantitatively detecting solid hazardous waste chloride ions |
-
2011
- 2011-12-30 CN CN 201110454581 patent/CN102539463A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103728328A (en) * | 2013-12-27 | 2014-04-16 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Content analyzing method of 16 elements in organic silicon powder sample |
| CN103852481A (en) * | 2014-03-12 | 2014-06-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for detecting components of elements in coated titanium dioxide |
| CN103852481B (en) * | 2014-03-12 | 2016-03-02 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method measuring elemental composition in coating titanium white |
| CN107228874A (en) * | 2017-06-29 | 2017-10-03 | 苏州浪声科学仪器有限公司 | The method of impurity in pressed powder x-ray fluorescence spectrometry metallic silicon |
| CN107656024A (en) * | 2017-11-13 | 2018-02-02 | 龙蟒佰利联集团股份有限公司 | A kind of assay method of titanium dioxide surface organosilicon stearic acid organic agent covering amount |
| CN107656024B (en) * | 2017-11-13 | 2019-11-22 | 龙蟒佰利联集团股份有限公司 | A kind of measuring method of titanium dioxide surface organosilicon stearic acid organic agent covering amount |
| CN111678935A (en) * | 2020-06-19 | 2020-09-18 | 承德金隅水泥有限责任公司 | Method for quantitatively detecting solid hazardous waste chloride ions |
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Application publication date: 20120704 |