CN106053508A - Method for energy chromatic dispersion X-ray fluorescence spectrum detection of sulfur trioxide in cement - Google Patents
Method for energy chromatic dispersion X-ray fluorescence spectrum detection of sulfur trioxide in cement Download PDFInfo
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- CN106053508A CN106053508A CN201610673483.0A CN201610673483A CN106053508A CN 106053508 A CN106053508 A CN 106053508A CN 201610673483 A CN201610673483 A CN 201610673483A CN 106053508 A CN106053508 A CN 106053508A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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Abstract
The invention relates to the technical field of detection of cement products, and in particular, relates to a method for energy chromatic dispersion X-ray fluorescence spectrum detection of sulfur trioxide in cement. The method mainly comprises the following steps: step one, determining a cement standard sample with known sulfur trioxide content by using a handheld chromatic dispersion X-ray fluorescence spectrophotometer, constructing a calibration work curve of the relationship between the X-ray fluorescence spectrum intensity and the sulfur element content, and determining sulfur element testing conditions; and step two, according to the sulfur element testing conditions determined in the step one, determining a to-be-tested cement sample by using the handheld chromatic dispersion X-ray fluorescence spectrophotometer, and thus obtaining the content of sulfur trioxide in the to-be-tested cement sample according to the relationship between the X-ray fluorescence spectrum intensity and the sulfur element content in the calibration work curve constructed in the step one. The method can detect the cement product on site, and has the advantages of convenient and sample detection process, accurate detection result and good consistency.
Description
Technical field
The present invention relates to cement products detection technique field, be specifically related to a kind of energy-dispersive X-ray fluorescence (EDXRF) spectral detection
The method of sulfur trioxide in cement, in particular by hand-held energy dispersion type X-ray fluorescence spectrophotometer in cement products three
The method that the content of sulfur oxide carries out detecting.
Background technology
Along with the quickening of Urban Construction in China speed, large construction material cement products demand is consequently increased, and cement produces
Product are as the main raw material(s) of modern building, the quality of its relationship between quality to whole building and safety, wherein comprcssive strength
It is the highly important macro property of cement products with rupture strength.
The factor affecting cement products macro property is a lot, and wherein chemical composition impact is particularly evident.Such as cement products
Middle calcium oxide content is used to weigh the parameter of Silicon in Cement acid salt cement grog, and it is the major influence factors of strength of cement.
Sulfur trioxide (SO3) intensity of excited cement can regulate again setting time of cement slurry, but content can break the most on the contrary
The intensity of bad cement, it is therefore desirable to strictly control.Simultaneously to cement products in GB 175-2007 " common portland cement " standard
Chemical composition sulfur trioxide content carried out clear and definite restriction, therefore the mensuration to its content is the important detection of cement products
Project.
The detection of national standard cement products sulfur trioxide content at present mainly uses precipitation gravimetry method to be measured, should
Method accuracy of measurement is of a relatively high, but condition requires strict, because when precipitation generates, and grain size and relative degree of supersaturation
Closely related, therefore acidity, solution addition speed, stirring etc. for solution have strict requirements, and the method is time-consuming simultaneously
Long, power consumption height.
Laboratory is to SO at present3Precipitation gravimetry is mainly used in the detection of content, and additive method such as iodimetric titration, ion are handed over
Changing method, Barium Chromate Spectrophotometry, Coulomb equation is all as alternative method, these methods either accuracy or convenience
The farthest it is inferior to precipitation gravimetry.
Wavelength dispersion type x-ray fluorescence spectrometry technology is used to carry out SO in cement products3The mensuration of content is large-scale at some
Cement plant is in popularization and application, but also faces some predicaments, and first this equipment cost puts into relatively big, a wavelength dispersion X-ray
Fluorescence spectrophotometer price is at about 1,000,000 yuan, and these equipment detector parts are crystal type, and the type equipment is to instrument work
Making environmental requirement higher, this is probably the main cause that current the method is difficult to promote.
Energy Dispersive-X-Ray fluorescent technique is fast-developing in recent years, because of its have volume little portable, be capable of in situ
The superior function such as low with fast-field evaluation, equipment cost is widely used in quality control and the quality authentication detection of product.
For these reasons, employing hand-held energy dispersion type X-ray fluorescence spectroscopy technique is researched and proposed to cement products
Middle SO3Content detects, and provides a kind of to SO in cement products3The method of content quick determination is significant.
Summary of the invention
In order to solve technical problem present in prior art, it is an object of the invention to provide a kind of Site Detection quick
Conveniently, the method for sulfur trioxide in testing result energy-dispersive X-ray fluorescence (EDXRF) spectral detection cement accurately.
For realizing above-mentioned technical purpose, the present invention uses following technical scheme:
In Energy dispersive x-ray fluorescence spectrum detection cement, the method for sulfur trioxide, mainly comprises the steps:
Step one, employing hand-held energy dispersion type X-ray fluorescence spectrophotometer measure the cement of known sulfur trioxide content
Standard specimen, builds x-ray fluorescence spectrometry intensity and the calibration operation curve of sulfur content relation, and determines element sulphur
Test condition；
Step 2, the test condition of the element sulphur determined according to step one, use hand-held energy dispersion type X-ray glimmering
Cement sample to be measured is measured by photothermal spectroscopic analyzer, strong according to x-ray fluorescence spectrometry in the calibration operation curve that step one builds
Degree and the relation of sulfur content, obtain the content of sulfur trioxide in cement sample to be measured.
As preferably, in step one, the test condition of element sulphur is: the testing time is 80s, and x-ray excited pipe pressure is
9kV, x-ray excited pipe flow is 100 μ A.
Compared with prior art, this method has following beneficial effect: use hand-held energy dispersion type X-ray
Fluorescence spectrophotometer measures the sample of self-control concentration known and builds calibration operation curve, and screens the test strip that sulfur content measures
Part, the test condition selecting element sulphur optimal detects SO in unknown sample3Content, it is possible to SO in cement products3Content enter
Row Site Detection, detection range is 0.31%-3.16%, and detection process is convenient, fast, and testing result is accurate, concordance is good.
Accompanying drawing explanation
The following drawings is only intended to, in schematically illustrating the present invention and explaining, not delimit the scope of the invention.Wherein:
Fig. 1 is the x-ray fluorescence spectrometry intensity that builds of the present invention and the calibration operation curve chart of sulfur content relation.
Detailed description of the invention
Below in conjunction with the accompanying drawings and embodiment, the present invention is expanded on further.In the following detailed description, only by explanation
Mode describes some one exemplary embodiment of the present invention.Undoubtedly, those of ordinary skill in the art will be consequently realised that,
In the case of without departing from the spirit and scope of the present invention, by various different modes, described embodiment can be repaiied
Just.Therefore, accompanying drawing and description are inherently the most illustrative rather than are used for limiting scope of the claims.
In a kind of energy-dispersive X-ray fluorescence (EDXRF) spectral detection cement, the method for sulfur trioxide, mainly comprises the steps:
Step one, take portland cement, Portland pozzolana cement, Portland fly ash cement, complex silicate respectively
Salt cement, Portland cement, portland slag cement, clinker 7 kinds have card standard sample 4.0g sample to carry out tabletting,
The pressure of every kind of sample tabletting is identical and keeps pressure time identical, is subsequently used for building x-ray fluorescence spectrometry intensity and sulfur unit
The calibration operation curve of cellulose content relation.SO in the most above-mentioned 7 kinds of standard specimens3Content be followed successively by: 3.16%, 2.59%,
2.17%, 2.30%, 2.28%, 2.02%, 0.31%.
Using hand-held energy dispersion type X-ray fluorescence spectrophotometer to above-mentioned cement standard sample test, element sulphur is
Good test condition is: the testing time is 80s, and x-ray excited pipe pressure is 9kV, and x-ray excited pipe flow is 100 μ A, test knot
Really, as shown in table 1, the different element x-ray fluorescence spectrometry intensity of result display presents incremental becoming with the content of object element
Gesture.
In table 1. cement standard sample, S is (with SO3Meter) content and x-ray fluorescence spectrometry intensity
Relevant variation diagram, the x-ray fluorescence spectrometry intensity of result display element sulphur is constructed according to table 1 test result
Presenting obvious linear dependence with the content of object element in cement products, result is as shown in Figure 1.In Fig. 1, result shows structure
The element sulphur calibration operation curve linear correlation coefficient built is more than 0.99, explores every kind of optimal test condition of element simultaneously,
Lay a good foundation for the detection of sulfur trioxide content in cement products.
Composite Portland cement, clinker, 3 kinds of cement standard samples of Portland fly ash cement are selected to carry out three oxidations
Sulfur content Accuracy Verification is tested, the SO of the cement standard sample of above-mentioned 3 types3Content is followed successively by 2.30%, 0.31%,
2.47%.Sample is carried out tabletting, then tests wherein element sulphur by hand-held energy dispersion type X-ray fluorescence spectrophotometer
Content, each sample is chosen different 7 some test and is averaged, contrasts the accuracy of this method test result.Test result
As shown in table 2.
In table 2. the inventive method 3 kinds of cement standard samples of mensuration, S is (with SO3Meter) content
The energy dispersion type X-ray fluorescence spectrum calibration operation curve that the table 2 measurement result display present invention builds can be used
The mensuration of S constituent content in cement sample, the nominal value that measurement result slightly less than precipitation gravimetry is given, this feelings occur
The reason of condition is probably energy dispersion type X-ray fluorescence spectroscopy technique and uses the mode measuring a single point to obtain element fluorescence light
Spectrum signal, the uniformity on the surface of sample and planarization may produce certain impact to measurement result.Simultaneously from statistical
Angle understands, energy dispersion type X-ray fluorescence spectroscopy technique gathers the sample number of spectral signal and takes significantly lower than precipitation gravimetry
The sample number of sample.
Step 2, according to the test condition of element sulphur in step one, use hand-held energy dispersion type X-ray fluorescence light
Spectrometer is to the SO in 6 cement sample3Content is tested, and wherein 3 samples are composite Portland cement, other 3 examinations
Sample is Portland cement.Use precipitation gravimetry to test its SO above-mentioned 6 cement sample sampling simultaneously3Content, contrast
The concordance of two kinds of method test results, test result is as shown in table 3.
Table 3. the inventive method and precipitation gravimetry measured value in prior art
Table 3 measurement result fully shows that the energy dispersion type X-ray fluorescence spectrum calibration operation curve that the present invention builds is complete
All can be enough in the mensuration of S constituent content in cement sample, measurement result is the most consistent with precipitation gravimetry measurement result.
Heretofore described hand-held energy dispersion type X-ray fluorescence spectrophotometer is prior art, and its structure is former with work
Reason is no longer described in detail.
The foregoing is only the schematic detailed description of the invention of the present invention, be not limited to the scope of the present invention.As surveyed
Strip part etc. can also the most suitably adjust or change, and any those skilled in the art, at the structure without departing from the present invention
Equivalent variations done on the premise of think of and principle and amendment, all should belong to the scope of protection of the invention.
Claims (2)
1. the method for sulfur trioxide in energy-dispersive X-ray fluorescence (EDXRF) spectral detection cement, it is characterised in that mainly include walking as follows
Rapid:
Step one, employing hand-held energy dispersion type X-ray fluorescence spectrophotometer measure the cement standard of known sulfur trioxide content
Sample, builds x-ray fluorescence spectrometry intensity and the calibration operation curve of sulfur content relation, and determines the test of element sulphur
Condition；
Step 2, the test condition of the element sulphur determined according to step one, use hand-held energy dispersion type X-ray fluorescence light
Cement sample to be measured is measured by spectrometer, according to step one build calibration operation curve in x-ray fluorescence spectrometry intensity and
The relation of sulfur content, obtains the content of sulfur trioxide in cement sample to be measured.
2. the method for sulfur trioxide in energy-dispersive X-ray fluorescence (EDXRF) spectral detection cement as claimed in claim 1, its feature exists
In, in step one, the test condition of element sulphur is: the testing time is 80s, and x-ray excited pipe pressure is 9kV, x-ray excited pipe
Stream is 100 μ A.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107703172A (en) * | 2017-09-14 | 2018-02-16 | 泰州赛宝工业技术研究院有限公司 | A kind of calibration method of energy-dispersion X-ray fluorescence spectrometer |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002082075A (en) * | 2000-09-08 | 2002-03-22 | Tdk Corp | Fluorescent x-ray analyzer and fluorescent x-ray analyzing method |
| CN103969274A (en) * | 2013-01-28 | 2014-08-06 | 东亚Dkk株式会社 | Energy dispersion type fluorescent X-ray analysis device |
| CN103969271A (en) * | 2013-01-30 | 2014-08-06 | 中国建材检验认证集团股份有限公司 | X-ray fluorescence analysis method for determining element sulphur with different valence in cement |
| CN105067651A (en) * | 2015-08-21 | 2015-11-18 | 南京市产品质量监督检验院 | Method for detecting lead, cadmium, chromium and arsenic in indoor emulsion paint wall |
| CN105241906A (en) * | 2015-10-29 | 2016-01-13 | 山东出入境检验检疫局检验检疫技术中心 | Method for determination of trace amount of sulfur in nitrogenous chemical raw material |
| CN105510369A (en) * | 2015-12-22 | 2016-04-20 | 北京安科慧生科技有限公司 | Special X-ray fluorescence energy spectrometer for high-precision cement industry |
-
2016
- 2016-08-16 CN CN201610673483.0A patent/CN106053508A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002082075A (en) * | 2000-09-08 | 2002-03-22 | Tdk Corp | Fluorescent x-ray analyzer and fluorescent x-ray analyzing method |
| CN103969274A (en) * | 2013-01-28 | 2014-08-06 | 东亚Dkk株式会社 | Energy dispersion type fluorescent X-ray analysis device |
| CN103969271A (en) * | 2013-01-30 | 2014-08-06 | 中国建材检验认证集团股份有限公司 | X-ray fluorescence analysis method for determining element sulphur with different valence in cement |
| CN105067651A (en) * | 2015-08-21 | 2015-11-18 | 南京市产品质量监督检验院 | Method for detecting lead, cadmium, chromium and arsenic in indoor emulsion paint wall |
| CN105241906A (en) * | 2015-10-29 | 2016-01-13 | 山东出入境检验检疫局检验检疫技术中心 | Method for determination of trace amount of sulfur in nitrogenous chemical raw material |
| CN105510369A (en) * | 2015-12-22 | 2016-04-20 | 北京安科慧生科技有限公司 | Special X-ray fluorescence energy spectrometer for high-precision cement industry |
Non-Patent Citations (2)
| Title |
|---|
| 周西林 等: "《原子光谱仪器操作入门》", 31 August 2015 * |
| 王益民 等: "水泥生产自动控制及能量色散X射线荧光分析技术", 《中国建材科技》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107703172A (en) * | 2017-09-14 | 2018-02-16 | 泰州赛宝工业技术研究院有限公司 | A kind of calibration method of energy-dispersion X-ray fluorescence spectrometer |
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