CN103743769A - Method for determining the content of harmful elements in iron ore by using X-ray fluorescent spectrometry - Google Patents
Method for determining the content of harmful elements in iron ore by using X-ray fluorescent spectrometry Download PDFInfo
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Abstract
The invention relates to a method for determining the content of harmful elements in iron ore by using X-ray fluorescent spectrometry. The method comprises the following steps: firstly, selecting an iron ore standard sample and a standard substance to prepare a series of standard samples, and then transferring the standard samples, an oxidant and a release agent to a platinum yellow crucible after mixing; preparing a glass sheet after melting at high temperature, so as to obtain a calibration sample; measuring the strength of As, Pb, Zn and Cu elements in the calibration sample by using an X-ray fluorescence spectrophotometer, and making a calibration curve; putting a test sample fabricated by the same fabrication method as the calibration sample into the X-ray fluorescence spectrophotometer; and making a calibration curve of an X-ray fluorescent spectrometry by using the calibration sample for measuring, so as to obtain the content of As, Pb, Zn and Cu elements in the sample. Thus, the content of main elements of SiO2, CaO, MgO, Al2O3, TiO2, P and the like is measured when the content of As, Pb, Zn and Cu in the iron ore is measured.
Description
Technical field
The present invention relates to the chemical analysis method of metallurgical industry, a kind of particularly method that adopts x ray fluorescence spectrometry rapid and accurate determination harmful elements in iron ore content, concrete, harmful element refers to As, Pb, Zn and Cu.
Background technology
Iron ore is the important raw and processed materials of steel production enterprise, is mainly used in the blast furnace process pig iron.At present, for what smelt iron, mainly contain magnetic iron ore (Fe
3o
4), haematite (Fe
2o
3) limonite (2Fe
2o
33H
2o) and siderite (FeCO
3) etc.
In iron ore, the objectionable impurities element such as As, Pb, Zn and Cu, not only directly affects blast furnace process effect, shortens the life-span of blast furnace, also can affect follow-up steel rolling and welding performance simultaneously, thereby affect the quality of steel.Therefore,, when iron ore is smelted, must strictly control the amount of As, Pb, Zn and the Cu of feed stock for blast furnace.
In iron ore, As, Pb, Zn and Cu chemical constituents determination generally adopt chemical analysis method or atomic absorption spectrography (AAS) to measure respectively.And these two kinds of ubiquitous defects of analytical approach are: can not multielement simultaneous determination, can only individual element analysis, complex operation, molten sample formality is numerous and diverse, and analytical cycle is long.Use a large amount of chemical reagent simultaneously, environment is caused to certain pollution.Therefore, cause understanding and grasping in time the real-time working of a furnace of blast furnace, be difficult to meet the demand that blast furnace is produced.Simultaneously, because iron ore is of a great variety, often there are the accompaniments such as sulfide and sulfate to form complicated mineral structure, and iron ore place of production difference, and composition and the checking of crystal habit difference, cause the sample of preparation to have granularity effect and the mineral effect of checking, cause traditional chemical analysis or atomic absorption spectrometry to have larger analysis deviation.
X-ray fluorescence spectra (XRF) analytic approach is that a kind of important chemical composition is analysed means, it is quick, easy, accurate to have, and analytical element is many, and the content range of mensuration is wide, precision advantages of higher, simultaneously primary and secondary quantitative elements and micro impurity element in working sample.Because X-ray fluorescence spectra analysis is a kind of surface analysis method, analysis depth only has several microns, and therefore for powdery analysis, the intensity of X ray may change with the unevenness of sample granularity and sample, and this phenomenon is granularity effect.The chemical constitution phenomenons different with mineral crystal form and that change that the intensity of x ray is analyzed component are called mineral effect.These two effects can be made glass sheet by fusion method and eliminate.
Fusion method is that oxide powder sample and flux (for example lithium tetraborate) are put into platinum crucible in certain proportion, melting under certain certain fixed temperature in 1000～1300 ℃, and cooling molten mass makes the method for glass sheet, is called fusion method.
Summary of the invention
The object of the invention is to overcome above-mentioned the deficiencies in the prior art, provide a kind of by highly diluted than melting sample preparation after, by the method for the content of As, Pb, Zn and Cu in x-ray fluorescence spectrometry iron ore.
To achieve these goals, the technical solution used in the present invention is:
A kind of method of x-ray fluorescence spectrometry harmful elements in iron ore content, first choose standards for iron ore sample and primary standard substance, be mixed with by a certain percentage the series standard sample with certain gradient and content range, after again standard model being mixed with oxygenant, release agent, be transferred in platinum yellow crucible, after high-temperature fusion, make glass sheet, can obtain calibration sample; With Xray fluorescence spectrometer, carry out the intensity of As, Pb, Zn and Cu element in calibration sample to measure, according to intensity and content, determine linear relationship, make calibration curve; To put into Xray fluorescence spectrometer with the test sample made with sample making process of calibration print, and measure with the calibration curve that calibration sample is set up x ray fluorescence spectrometry, can obtain the content of As in sample, Pb, Zn and Cu element.
As the preferred version of this programme: described flux anhydrous lithium tetraborate, described oxygenant is sodium nitrate, described release agent is ammonium bromide.
As the preferred version of this programme: the ratio of described standard model and flux is 1:16.
As the preferred version of this programme: be set to 1150 ℃ during melting, duration 15min.
Beneficial effect of the present invention is: the present invention is better than traditional chemical analysis method or atomic absorption spectrometry; Simultaneously the method can be used as again ISO9516-1-2003, GB/T6730.62-2005 and SN/T0832-1999 one and supplements, at the content of measuring As, Pb, Zn and Cu simultaneously, and can be to SiO in iron ore
2, CaO, MgO, Al
2o
3, TiO
2measure with the content of the main secondary elements such as P.This method has overcome sample granularity effect and mineral effect, has reduced the absorption-enhancement effect of matrix simultaneously, and in the glass print that makes to make, element is evenly distributed, and can preserve for a long time.Meanwhile, method of operating is simple, safety, and print preparation time is short, and can preserve for a long time.Therefore, this method can be saved a large amount of test materials, greatly shortens sense cycle, and liberation labour, increases work efficiency.And except platinum yellow crucible being had small corrosion and a small amount of reagent material consumption, almost do not have other to consume, a large amount of chemical reagent waste liquid pollution on the environment while having avoided chemical analysis.Enforcement of the present invention simultaneously, while smelting for iron ore, the real-time furnace control of blast furnace and the rolling of follow-up steel provide useful help.
Embodiment
Below by the description to embodiment, the specific embodiment of the present invention is as the effect of the mutual alignment between the shape of related each member, structure, each several part and annexation, each several part and principle of work, manufacturing process and operation using method etc., be described in further detail, to help those skilled in the art to have more complete, accurate and deep understanding to inventive concept of the present invention, technical scheme.
A kind of method that adopts x-ray fluorescence spectrometry harmful elements in iron ore As, Pb, Zn and Cu content mainly comprises the following steps:
(1) selection of calibration sample:
Select standards for iron ore sample and primary standard substance, be mixed with by a certain percentage the serial calibration sample with certain gradient and content range.
(2) preparation of sample and calibration sample:
Adopt anhydrous lithium tetraborate to make flux, sodium nitrate is made oxygenant, and ammonium bromide is made release agent, and the dilution ratio of sample and flux is 1:16; Accurately take sample and flux in weighing disk, add a certain amount of oxygenant, after fully mixing, proceed in platinum-yellow crucible, and add a certain amount of release agent; Put on molten model machine, after 1150 ℃ of melting 15min, make glass sample.The demoulding, cooling after, put into exsiccator to be measured.
(3) calibration curve is made:
The serial calibration sample of preparing with table 1, by step (2), be prepared into glass print, on Xray fluorescence spectrometer, carry out condition test, select suitable crystal, collimating apparatus, voltage and current, 2 θ and pulse height distribution etc., to select the analysis condition of instrument the best.With Xray fluorescence spectrometer, measure the fluorescence intensity of 12 calibration samples, after proofreading and correct by overlap of spectral lines and matrix effect, according to intensity and content, determine linear relationship, carry out linear regression, produce calibration curve, and be kept in the quantitative analysis software of computing machine.
(4) measure:
The test sample being prepared into is put into Xray fluorescence spectrometer, and application standard print is set up the working curve of x ray fluorescence spectrometry and is measured, and after Xray fluorescence spectrometer detects, automatically calculates the content of As in sample, Pb, Zn and Cu element.
A kind of method of embodiment 1, x-ray fluorescence spectrometry harmful elements in iron ore As, Pb, Zn and Cu content: the first step, the selection of calibration sample:
Select 7 standards for iron ore samples, and add primary standard substance with standards for iron ore sample, be mixed with by a certain percentage and there is certain gradient and make 5 synthetic standard samples, composition calibration sample series.Series calibration sample is as shown in table 1 below, and the content distribution of each element is as shown in table 2 below.
Table 1 calibration sample series
| Sequence number | Numbering | Sample title |
| 1 | GSBD31004-93 | Iron ore |
| 2 | GSBH30002-97 | Iron ore |
| 3 | GSBH30003-97 | Iron ore |
| 4 | GSBH30005-97 | Iron ore |
| 5 | GSBH30006-97 | Iron ore |
| 6 | YSBC14721-98 | Magnetic iron ore |
| 7 | YSBC14722-98 | Magnetic iron ore |
| 8 | HC-1 | Synthetic standard sample 1 |
| 9 | HC-2 | Synthetic standard sample 2 |
| 10 | HC-3 | Synthetic standard sample 3 |
| 11 | HC-4 | Synthetic standard sample 4 |
| 12 | HC-5 | Synthetic standard sample 5 |
Table 2 calibration sample content range
| Element | Content range/% |
| As | 0.003-0.50 |
| Pb | 0.001-0.50 |
| Zn | 0.005-1.00 |
| Cu | 0.01-0.50 |
Second step, the preparation of sample and calibration sample:
Adopt and accurately take 0.4500g sample and 7.2000g lithium tetraborate flux in weighing disk, add 1.000g ammonium nitrate oxidizing agent, after fully mixing, proceed in platinum-yellow crucible, and add the ammonium bromide release agent of 8 20%; Put on molten model machine, after 1150 ℃ of melting 15min, make glass sample.The demoulding, cooling after, put into exsiccator to be measured.
The 3rd step, calibration curve is made:
With the calibration sample preparing, on Xray fluorescence spectrometer, carry out condition test, select suitable crystal, collimating apparatus, voltage and current, 2 θ and pulse height distribution etc., to select the analysis condition of instrument the best.Survey the fluorescence intensity of 12 calibration samples with x ray fluorescence spectrometry, after proofreading and correct by overlap of spectral lines and matrix effect, according to intensity and content, determine that linear relationship carries out linear regression, produce calibration curve, and be kept in the quantitative analysis software of computing machine.
Concrete analysis condition is as shown in table 3 below.
Table 3 instrumental analysis condition
The 4th step, test:
The test sample being prepared into is put into Xray fluorescence spectrometer, and application standard print is set up the working curve of x ray fluorescence spectrometry and is measured, and after Xray fluorescence spectrometer detects, automatically calculates the content of As in sample, Pb, Zn and Cu element.
For the accuracy of checking this method, select 4 national standard samples to verify the accuracy of this method, as shown in table 4, from chemical score and XRF, be worth contrast, the accuracy of experimental data is good, is all less than the error range that national standard allows.
Meanwhile, in order to verify the precision of this method, same sample has been carried out to identical molten sample and the melting sample preparation operation of continuous 10 times.From the precision of experimental data, investigate the stability of this method.Data by table 5 show, the relative standard deviation of As, Pb, Zn and Cu element all, within less scope, illustrates that the whole operating process of this method is reliable and stable.
Table 4 accuracy experimental data
Table 5 Precision Experiment result
Above the present invention is exemplarily described; obviously specific implementation of the present invention is not subject to the restrictions described above; as long as adopted the improvement of the various unsubstantialities that method of the present invention design and technical scheme carry out; or without improving, design of the present invention and technical scheme are directly applied to other occasion, all within protection scope of the present invention.
Claims (4)
1. the method for an x-ray fluorescence spectrometry harmful elements in iron ore content, it is characterized in that: first choose standards for iron ore sample and primary standard substance, be mixed with series standard sample, after again standard model being mixed with oxygenant, release agent, be transferred in platinum yellow crucible, after high-temperature fusion, make glass sheet, can obtain calibration sample; With Xray fluorescence spectrometer, carry out the intensity of As, Pb, Zn and Cu element in calibration sample to measure, according to intensity and content, determine linear relationship, make calibration curve; To put into Xray fluorescence spectrometer with the test sample made with sample making process of calibration print, and measure with the calibration curve that calibration sample is set up x ray fluorescence spectrometry, can obtain the content of As in sample, Pb, Zn and Cu element.
2. method according to claim 1, is characterized in that: described flux anhydrous lithium tetraborate, and described oxygenant is sodium nitrate, described release agent is ammonium bromide.
3. method according to claim 1, is characterized in that: the ratio of described standard model and flux is 1:16.
4. method according to claim 1, is characterized in that: during melting, be set to 1150 ℃, duration 15min.
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|---|---|---|---|---|
| CN104730098A (en) * | 2015-04-03 | 2015-06-24 | 甘肃酒钢集团宏兴钢铁股份有限公司 | Rapid analysis method of high-content harmful element in blast furnace iron material |
| 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 |
| CN105806865A (en) * | 2016-03-21 | 2016-07-27 | 中华人民共和国南通出入境检验检疫局 | Melting flaking method of copper concentrate for X-ray fluorescent spectrometry |
| CN106226340A (en) * | 2016-08-31 | 2016-12-14 | 广西出入境检验检疫局危险品检测技术中心 | A kind of measure the method for copper content in fireworks and firecrackers copper sulfate |
| CN106290439A (en) * | 2016-09-21 | 2017-01-04 | 海南中航特玻科技有限公司 | Quickly measure Na in Natrii Sulfas2sO4, NaCl, Fe2o3the method of content |
| CN106370686A (en) * | 2016-08-31 | 2017-02-01 | 广西出入境检验检疫局危险品检测技术中心 | Method for determining copper content in basic copper carbonate for fireworks and firecrackers |
| CN106442071A (en) * | 2016-12-21 | 2017-02-22 | 蚌埠中恒新材料科技有限责任公司 | Processing method for measuring titanium concentrate sample by X-ray fluorescent spectrometry |
| CN107179330A (en) * | 2017-06-29 | 2017-09-19 | 苏州浪声科学仪器有限公司 | The method of impurity in x-ray fluorescence spectrometry iron ore |
| CN107356618A (en) * | 2017-06-30 | 2017-11-17 | 马鞍山钢铁股份有限公司 | A kind of method of covering agent component content in x-ray fluorescence spectrometry |
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| CN108181337A (en) * | 2017-12-08 | 2018-06-19 | 芜湖新兴铸管有限责任公司 | The method for quickly measuring the content of magnesia in calcined magnesite ball using x-ray fluorescence fuse piece method |
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| CN110441340A (en) * | 2019-07-16 | 2019-11-12 | 天津钢管制造有限公司 | Measuring method based on Ta element in X-ray fluorescence spectra analysis steel alloy |
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| CN114441578A (en) * | 2022-02-11 | 2022-05-06 | 山东钢铁集团永锋临港有限公司 | Method for measuring component content in iron ore by X-ray fluorescence spectrometry |
| CN115452871A (en) * | 2022-08-08 | 2022-12-09 | 武汉科技大学 | Preparation of glass sheet for XRF analysis of iron ore and correction method of measurement result |
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| CN114441578A (en) * | 2022-02-11 | 2022-05-06 | 山东钢铁集团永锋临港有限公司 | Method for measuring component content in iron ore by X-ray fluorescence spectrometry |
| CN115452871A (en) * | 2022-08-08 | 2022-12-09 | 武汉科技大学 | Preparation of glass sheet for XRF analysis of iron ore and correction method of measurement result |
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Application publication date: 20140423 |