CN103604823A - Method for measuring contents of potassium, sodium, lead and zinc in iron ore - Google Patents
Method for measuring contents of potassium, sodium, lead and zinc in iron ore Download PDFInfo
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- CN103604823A CN103604823A CN201310567395.9A CN201310567395A CN103604823A CN 103604823 A CN103604823 A CN 103604823A CN 201310567395 A CN201310567395 A CN 201310567395A CN 103604823 A CN103604823 A CN 103604823A
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Abstract
The invention discloses a method for measuring contents of potassium, sodium, lead and zinc in an iron ore. The method comprises the following steps: selecting a series of standard samples having gradient contents of potassium, sodium, lead and zinc, fusing the standard samples and preparing samples; scanning the prepared standard sample glass sheets through a wavelength dispersive X fluorescence spectrum analyzer to measure the strength of the potassium, sodium, lead and zinc; determining a linear relation according to the strength and contents, and establishing a correction working curve of the potassium, sodium, lead and zinc; fusing an iron ore sample and preparing a sample, scanning the prepared sample glass sheet through the wavelength dispersive X fluorescence spectrum analyzer to measure the strength of the potassium, sodium, lead and zinc, and calculating according to the correction working curve to obtain the contents of the potassium, sodium, lead and zinc in the iron ore sample. The method disclosed by the invention is simple to operate, fast in analysis speed and capable of analyzing such components in the iron ore as iron, silicon, calcium, magnesium, titanium, aluminum, sulfur, phosphorus and the like while analyzing the potassium, sodium, lead and zinc elements, and the method has the advantages of good applicability, short analysis time, high accuracy, good repeatability, low detection limit, little pollution, etc.
Description
Technical field
The invention belongs to metallurgical chemistry analysis experimental technique field., the assay method of potassium sodium Pb, Zn content in especially a kind of iron ore.
Background technology
Iron ore refers to that iron-holder is quite high and can be used in the ore that refines iron in smelter, is one of primary raw material of blast furnace ironmaking.Components of iron ore is complicated, by Fe, and Si, Ca, Mg, Ti, P, Al, S, K, Na, Zn, Pb, Cu, the oxide of the multiple elements such as As and different valence state thereof, compound form.Along with the progress of the production-scale expansion of blast furnace ironmaking and smelting technique, people progressively improve the understanding of ironmaking production trace harmful elements such as K, Na, Zn, Pb in iron charge.It is generally acknowledged, in blast furnace the alkali metal vapour of potassium sodium can catalytic coke gasification reaction, the reduction degradation of aggravation sintering deposit, cause pellet abnormal expansion, destroy blast furnace lining, finally cause the ventilative liquid permeability of stock column to decline, affect blast furnace stable smooth operation.In addition alkali-metal infiltration also can cause carbon brick rotten and between pervious course and good carbon brick stress effect produce embrittlement layer, cause the breakage of furnace bottom carbon brick, cause furnace lining, cupola well to suffer erosion.Lead in blast furnace, zinc heavy metal, easily in Furnace enrichment and immerse furnace bottom carbon brick gap, destroy furnace bottom, cause burn-through of furnace hearth when serious, give the natural labor stable yields of blast furnace and long-livedly bring serious harmful effect.So control the content of K in furnace charge, Na, Zn, Pb element, become important measures of blast furnace stable smooth operation, longevity.Meanwhile, measure the needs of K, Na in iron ore, Pb, the clearing of Zn constituent content Ye Shijin factory.
Through consulting normative document data, measure K in iron ore
2o and Na
2the method of O, has flame photometry (measurement range is 0.1%-2.0%), atomic absorption spectrophotometry (measurement range is 0.005%-1.5%) and ICP plasma spectroscopy.The method of Pb and Zn in survey iron ore, there is oscilloscopic polarography (to be 0.01-0.5%,), photometry (Pb0.01-0.5%, Zn0.01-0.05%) and atomic absorption spectrography (AAS) (Zn0.01%-1.00%, Pb0.01%-1.00%) and ICP plasma spectroscopy.These methods, sample need be made solution through chemical treatment, then uses apparatus measures, and analytical procedure is complicated, and link is many, and operation easier is large, consuming time long, analysis, Fast Measurement when being not suitable for into factory's iron ore potassium, sodium, lead, zinc element.
Summary of the invention
The technical problem to be solved in the present invention is to provide the assay method of potassium sodium Pb, Zn content in a kind of analysis time of short, the iron ore that can simultaneously measure.
For solving the problems of the technologies described above, the technical solution used in the present invention is: select the standard model of a series of potassium, sodium, lead, zinc gradient content, by standard model melting sample preparation; Wavelength dispersion X-fluorescence analyser scanning for the standard specimen glass sheet of making, the intensity of mensuration potassium, sodium, lead, zinc; According to intensity and content, determine linear relationship, set up the correction work curve of potassium, sodium, lead, zinc;
By iron ore sample melting sample preparation, the sample glass sheet of making scans with wavelength dispersion X-fluorescence analyser, measures the intensity of potassium, sodium, lead, zinc, can calculate the content of potassium, sodium, lead, zinc in iron ore sample according to correction work curve.
The flux of melting sample preparation of the present invention is mark reagent in anhydrous lithium tetraborate, lithium carbonate and cobalt, and in anhydrous lithium tetraborate, lithium carbonate and cobalt, the weight ratio of mark reagent is 1:2:0.1.The weight ratio of described standard model and flux is 1:10～13; The weight ratio of described iron ore sample and flux is 1:10～13.The temperature of described melting sample preparation is 1050 ℃～1100 ℃.
The beneficial effect that adopts technique scheme to produce is: the present invention adopts the sample preparation of bead method, the method is simple to operate, analysis speed is fast, can when analyzing potassium, sodium, lead, zinc element, analyze the compositions such as iron, silicon, calcium, magnesium, titanium, aluminium, sulphur, phosphorus of iron ore kind, by confirming, the feature such as the method has science, advance, applicability, analysis time is short, accuracy is high, reproducible, detection limit is low, pollution is few; Repeatability and in linearity, be all better than traditional chemical analysis method.
The present invention is applied to, into the Fast Measurement of potassium, sodium, lead, zinc element in factory's iron ore, be better than traditional chemical analysis method; Especially when measuring iron, silicon, calcium, magnesium, titanium, aluminium, sulphur, P elements, obtain the content of potassium, sodium, lead, zinc, analysis time, precision, accuracy were better in 30 minutes, met Liao Jin factory raw material and detected demand and (require K
2o≤0.1%, Na
2o≤0.15%, K
2o+Na
2o≤0.25%; Containing zinc≤0.025%, leaded≤0.025%), there is good application value.Simultaneously the method can be used as again of GB/T 6730.62-2005 and supplements, and measures the content of potassium, sodium, lead, zinc when measuring calcium, magnesium, silicon, aluminium, titanium, manganese, phosphorus, barium.The features such as the method has science, advance, applicability, analysis time is short, accuracy is high, reproducible, detection limit is low, pollution is few, verify by preci-sion and accuracy, show that the method has high accuracy and precision.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is the correction work curve map of potassium element;
Fig. 2 is the correction work curve map of sodium element;
Fig. 3 is the correction work curve map of lead element;
Fig. 4 is the correction work curve map of zinc element.
Embodiment
The assay method X-ray fluorescence spectra assay of potassium sodium Pb, Zn content in this iron ore, comprise following processing step: the mass ratio of sample and flux is 1:10～13, in anhydrous lithium tetraborate, lithium carbonate and cobalt, mark reagent is as flux, through the melting of high frequency fusion stove, make after glass sheet, directly with X-ray fluorescence spectrometer, scan, measure the intensity of potassium, sodium, lead, zinc, according to intensity and content, determine linear relationship, set up correction work curve, then according to the intensity of potassium, sodium, lead, zinc, calculate the content of potassium, sodium, lead, zinc.
1, major equipment:
A) MXF-2400 wavelength dispersion X-ray fluorescence spectrometer; Fe, Si, Ca, Mg, Ti, P, Al, S, K, Na element passage are installed, and SCAN heavy metal scanning road; Detecting device is sweep type gas proportional counter and scintillation counter; X-ray tube peak power, 4KW.
B) sample making apparatus:
V4D high frequency fusion stove; Temperature range: 0～1300 ℃ adjustable; Blending manner: wave+spin.
2, chemical reagent:
Anhydrous lithium tetraborate (powder), top grade is pure; Lithium carbonate, analyzes pure; Cobalt sesquioxide, top grade is pure, produces mark reagent in cobalt; Ammonium iodide, analyzes purely, and making massfraction is 30% solution, as release agent.
3, other material installation:
A) platinum-gold crucible (platinum 95wt%, gold 5wt%), 70 grams of weight, bottom is circular, and diameter is greater than 35mm;
B) AUY120 electronic analytical balance, sensibility reciprocal 0.1mg;
C) iron ore national standard sample.
4, weigh sample flux:
First take 5 grams of anhydrous lithium tetraborates, then take 0.5 gram, iron ore sample, 1 gram of lithium carbonate, in cobalt sesquioxide, mark reagent is 0.5 gram, puts into successively 100ML small beaker, shakes up, and stir 50 left and right with glass bar, and transfer in platinum-gold crucible, drip 4,5 of ammonium iodide solution.
5, glass print is prepared in melting:
Platinum-gold crucible that sample and flux are housed is placed on high frequency fusion stove ceramic support piece, the condition of work of setting coreless induction furnace is, one hot time 60S, one 1050 ℃ of hot temperature degree, two hot time 60S, two 1100 ℃ of hot temperature degree, melting time 270S, 1100 ℃ of melt temperatures, from cool time 120S, wave speed 7.Press heat button, carry out sample melted, after melting completely, pour mask, print is cooled to room temperature, and crucible bottom is analysis face, and the back side is labelled standby.
6, drawing curve:
A) selection of standard model;
According to the content of routine testing sample, select the standard model of applicable a series of potassium, sodium, lead, zinc gradient content, standard model and component content thereof are in Table 1; Standard model is pressed to 4,5 molten glass sheet processed.Standard model series can be one group, and wherein the content of potassium, sodium, lead and zinc all forms gradient; Can also many groups, the content of potassium, sodium, lead and zinc forms respectively gradient in every group.
Table 1: standard model (wt%)
B) scan conventional sample, determine fluorescence analysis condition:
Select the higher conventional actual samples of chemical composition to scan, sample chamber is vacuum atmosphere, and chosen elements analysis channel, analyzing crystal are determined pipe stream, pipe pressure, analysis spectral line, PHA scope, analysis time, angular instrument 2 θ angles etc.Potassium, sodium element adopt matrix correction, and plumbous, zinc element adopts background correction pattern.When the general both sides of background are symmetrical, select single-point as a setting, when measured signal when more than 10 times, can be ignored background intensity higher than background signal by force, to shorten sweep time, analysis time when sweep signal deviation is less than 0.3% as the analysis end time.Thereby PHA obtains very accurate and stable data by eliminating the impact of the high order line of external noise and X ray, and the accurate of data depends primarily on the low mark of PHA and the setting of high standard with stablizing.When measuring micro-light element, the high order line spectrum meeting of other element or high-load light element and measurement spectral line are significantly overlapping, must determine PHA condition with actual sample or the sample that contains actual sample.The final optimum analysis condition of determining the plumbous zinc microelement analysis bank of potassium sodium is in Table 2.
Table 2: luminoscope measuring condition
C) scanning standard specimen intensity, make and optimize correction work curve:
Under fixed analysis condition, scanning standard sample, data processor is made working curve automatically, because the known component content of standard model can not be all in 95～105% scopes, therefore this experiment can only adopt fixedly a coefficient correction, sample adopts fusion method to make glass sheet, and matrix effect is little, noiseless element.Optimize post-equalization working curve as follows:
Table 3 correction work calibration curve information
The correction work curve map of potassium, sodium, lead, each element of zinc is shown in Fig. 1-Fig. 4; Fig. 1 is K
2o correction work curve, Fig. 2 is Na
2o correction work curve, Fig. 3 is Pb correction work curve, Fig. 4 is Zn correction work curve.
7, precision test:
Select an ironstone sample, according to above sample, melt method processed and analysis condition, carry out 12 replicate determinations, data are in Table 4.
Table 4: Precision Experiment measurement data
8, accuracy validation
According to above sample, melt method processed and analysis condition, part standard specimen and outer committee definite value sample are analyzed, data are in Table 5.
Table 5: accuracy validation data
Note: the definite value of entrusting outward K, Na, Zn are measured by national ferrous materials test center by ICP method; Pb ICP-MS method; River open drain fine powder, iron cage fine powder, industry slag are each institute of Gong Hu unit feeding samples of a surname's steel.
Above data show that this analytical approach has higher accuracy and precision, and Repeatability and Reproducibility is all better than traditional chemical analysis method.
9, actual samples is analyzed, by foregoing, sample is melting into glass sheet, adopt above analysis condition and correction work curve to analyze, data measured is in Table 6.
Table 6: produce sample data
Specimen coding in table 6 is the sample uniqueness sign that the sample pocket subscript in the routine testing of laboratory is noted, and comprises the information such as sample classification, date, coding.
Claims (4)
1. an assay method for potassium sodium Pb, Zn content in iron ore, is characterized in that: select the standard model of a series of potassium, sodium, lead, zinc gradient content, by standard model melting sample preparation; Wavelength dispersion X-fluorescence analyser scanning for the standard specimen glass sheet of making, the intensity of mensuration potassium, sodium, lead, zinc; According to intensity and content, determine linear relationship, set up the correction work curve of potassium, sodium, lead, zinc;
By iron ore sample melting sample preparation, the sample glass sheet of making scans with wavelength dispersion X-fluorescence analyser, measures the intensity of potassium, sodium, lead, zinc, can calculate the content of potassium, sodium, lead, zinc in iron ore sample according to correction work curve.
2. the assay method of potassium sodium Pb, Zn content in iron ore according to claim 1, it is characterized in that: the flux of described melting sample preparation is mark reagent in anhydrous lithium tetraborate, lithium carbonate and cobalt, and in anhydrous lithium tetraborate, lithium carbonate and cobalt, the weight ratio of mark reagent is 1:2:0.1.
3. the assay method of potassium sodium Pb, Zn content in iron ore according to claim 2, is characterized in that: the weight ratio of described standard model and flux is 1:10～13; The weight ratio of described iron ore sample and flux is 1:10～13.
4. according to the assay method of potassium sodium Pb, Zn content in the iron ore described in claim 1,2 or 3, it is characterized in that: the temperature of described melting sample preparation is 1050 ℃～1100 ℃.
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Cited By (10)
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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 |
| 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 |
| CN106053366A (en) * | 2016-06-17 | 2016-10-26 | 长春黄金研究院 | Efficient accurate continuous measurement method for lead and zinc in lead concentrate and gold concentrate |
| CN106168588A (en) * | 2016-08-31 | 2016-11-30 | 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 potassium content in potassium perchlorate used for fireworks and crackers |
| CN106290436A (en) * | 2016-08-31 | 2017-01-04 | 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 potassium content in fireworks and firecrackers Potassium Hydrogen Phthalate |
| CN106370687A (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 measuring potassium content in potassium hydrogen terephthalate for fireworks and crackers |
| CN108931546A (en) * | 2018-04-08 | 2018-12-04 | 中国地质科学院矿产资源研究所 | Hyperspectrum-based lithium-containing pegmatite identification method |
| CN110057852A (en) * | 2019-04-09 | 2019-07-26 | 湛江出入境检验检疫局检验检疫技术中心 | Wavelength dispersion X-ray fluorescence spectrometry measures primary and secondary amount compositions, method in zinc concentrate |
| CN110389146A (en) * | 2019-07-26 | 2019-10-29 | 新余钢铁股份有限公司 | A kind of method that the compensation of X-fluorescence cobalt internal standard-ICP cobalt detects all iron content in iron charge |
| WO2023231385A1 (en) * | 2022-06-01 | 2023-12-07 | 苏州佳谱科技有限公司 | Enrichment detection method and apparatus for trace heavy metal elements in liquid |
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Cited By (12)
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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 |
| 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 |
| CN105067651B (en) * | 2015-08-21 | 2018-04-06 | 南京市产品质量监督检验院 | Lead, cadmium, chromium, the detection method of arsenic in a kind of indoor emulsion paint metope |
| CN106053366A (en) * | 2016-06-17 | 2016-10-26 | 长春黄金研究院 | Efficient accurate continuous measurement method for lead and zinc in lead concentrate and gold concentrate |
| CN106053366B (en) * | 2016-06-17 | 2019-04-23 | 长春黄金研究院 | Lead, plant Zn content method in a kind of lead concentrate of efficiently and accurately, Gold Concentrate under Normal Pressure |
| CN106168588A (en) * | 2016-08-31 | 2016-11-30 | 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 potassium content in potassium perchlorate used for fireworks and crackers |
| CN106290436A (en) * | 2016-08-31 | 2017-01-04 | 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 potassium content in fireworks and firecrackers Potassium Hydrogen Phthalate |
| CN106370687A (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 measuring potassium content in potassium hydrogen terephthalate for fireworks and crackers |
| CN108931546A (en) * | 2018-04-08 | 2018-12-04 | 中国地质科学院矿产资源研究所 | Hyperspectrum-based lithium-containing pegmatite identification method |
| CN110057852A (en) * | 2019-04-09 | 2019-07-26 | 湛江出入境检验检疫局检验检疫技术中心 | Wavelength dispersion X-ray fluorescence spectrometry measures primary and secondary amount compositions, method in zinc concentrate |
| CN110389146A (en) * | 2019-07-26 | 2019-10-29 | 新余钢铁股份有限公司 | A kind of method that the compensation of X-fluorescence cobalt internal standard-ICP cobalt detects all iron content in iron charge |
| WO2023231385A1 (en) * | 2022-06-01 | 2023-12-07 | 苏州佳谱科技有限公司 | Enrichment detection method and apparatus for trace heavy metal elements in liquid |
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Application publication date: 20140226 |