CN102305749A - Method for quickly determining content of Fe3O4 in minerals - Google Patents

Method for quickly determining content of Fe3O4 in minerals Download PDF

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CN102305749A
CN102305749A CN201110136196A CN201110136196A CN102305749A CN 102305749 A CN102305749 A CN 102305749A CN 201110136196 A CN201110136196 A CN 201110136196A CN 201110136196 A CN201110136196 A CN 201110136196A CN 102305749 A CN102305749 A CN 102305749A
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weighing
appearance
content
magnetic field
fe3o4
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王文龙
王旭江
马春元
董勇
徐夕仁
宋占龙
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Shandong University
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Abstract

The invention relates to a method for quickly determining the content of Fe3O4 in minerals. The method comprises the following steps of: preparing a plurality of groups of Fe3O4 content calibration samples by using Fe3O4 and a weakly magnetic or nonmagnetic substance; determining the mass m1 of the calibration samples under the condition of no magnetic field; determining the mass m2 of the calibration samples under a constant magnetic field; introducing a weighing change rate factor alpha, substituting the m1 and the m2 which correspond to the calibration samples to calculate the alpha of the calibration samples, and fitting a linear relation between the Fe3O4 mass fractions of the calibration samples and the weighing change rate factor alpha; and testing m1 and m2 which correspond to a sample to be determined which contains a Fe3O4 mineral, calculating the alpha of the sample, and substituting an obtained value into the fitted linear relation to obtain the content of Fe3O4. In the method, the content of Fe3O4 in the minerals is quickly determined by using the magnetic-gravity effect; and the method is accurate, convenient, quick and pollution-free, and is particularly applicable to the determination of reduction rate of minerals such as hematite, red mud and the like which are subjected to reduction roasting.

Description

Fe in the fast measuring mineral 3O 4The method of content
Technical field
The present invention relates to Fe in a kind of mensuration mineral 3O 4The method of content, particularly a kind of based on Fe in magnetic-weight effect fast measuring mineral 3O 4The method of content.
Background technology
China's iron ore deposit is abundant, nearly 50,000,000,000 t of proven reserves, and wherein the haematite proven reserves surpass 9,500,000,000 t.Each country is to the development and use of iron ore deposit, and is general in line with principle red, easy first and difficult later behind the first magnetic because the complicated difficult choosing of haematite, cause its in the utilization factor of China less than 7%.Along with China's rapid development of economy in recent years; Steel industry develops rapidly; Supply falls short of demand for iron ore, and increasing refractory iron ore (like haematite) and iron-contained industrial discarded object (like red mud) begin to get into metallurgical process, and its development and use have been become the inexorable trend that iron resource utilizes.The development and use of haematite and red mud etc. are generally incited somebody to action weak magnetism mineral Fe wherein through reduction roasting 2O 3Be reduced into ferrimagnetism mineral Fe 3O 4Thereby, the magnetic separation rate of raising mineral.Fe 2O 3The accurate mensuration of percent reduction is for improving the reduction roasting condition, and it is extremely important to improve the commercial production economy.But at present in the metallurgical industry usually with the magnetic separation rate as the index that characterizes percent reduction because the magnetic separation process can carry out other mineral, the accuracy of this kind characteristic manner is relatively poor, accurately to measure the method for percent reduction very necessary so seek a kind of rapid and convenient.
At present, the method that might be used to measure reduction roasting product percent reduction mainly contains chemistry titration, X-ray fluorescence spectra analytical approach (XRF) and X-ray diffraction analysis method (XRD).Surveying iron content with the method for chemistry titration needs at first mineral to be cleared up, and carries out titration through the indicator change in color afterwards; But often because mineral structure is stable, clears up and be difficult for directly realizing, need strong acid or strong oxidizer usually, and in this process Fe 2+Can be oxidized to Fe 3+So the method for chemistry titration is applicable to the mensuration of all iron content usually, can not realize Fe 3+With Fe 2+Titration respectively; In addition, because mineralogical composition is complicated, the accuracy of titration results also can receive very big influence.XRF has that specimen preparation is simple, analysis speed is fast, favorable reproducibility; Cost hangs down the advantage with nondestructively measuring, and along with development in recent years, its application in the ultimate analysis field is more and more wider; But the method is mainly used in elemental composition and Determination on content, for Fe 2+With Fe 3+Differentiation powerless, therefore can't adopt the method measuring percent reduction.XRD can realize the quantitative measurement to composition in the mineral; Existing many both at home and abroad articles about the XRD quantitative test; But by contrast; This methods analyst difficult and complicated; Mathematical computations is loaded down with trivial details; Particularly mineralogical composition such as haematite is complicated, more increased XRD analysis difficulty, reduced the accuracy of its analysis.Therefore, quick, convenient, accurately measure percent reduction method obtain in metallurgical industry extremely important.
Summary of the invention
The purpose of this invention is to provide Fe in a kind of fast measuring mineral 3O 4The method of content, this kind method has quick, convenient, characteristic of accurate based on magnetic-weight effect, solves and measures the problem that the mineral reduction rate exists in the present metallurgical industry.
The technical scheme that the present invention takes is:
Fe in the fast measuring mineral 3O 4The method of content comprises that step is following:
(1) uses Fe 3O 4Demarcate with appearance with weak magnetic or the many groups of nonmagnetic material preparation, many groups are demarcated the Fe with appearance 3O 4Massfraction from 0% to 100% distributes;
(2) each group is demarcated with appearance be placed in the same sample cup, guarantee that each group demarcates with shape and the volume of appearance in cup identically, each group of weighing and record is demarcated the no field quality that uses kind and is m 1
(3), above weighing equipment, add electromagnet or permanent magnet, for weighing equipment pallet place provides an invariable magnetic field with same weighing equipment;
(4) each m of weighing once more under the stationary magnetic field 1Quality is designated as m under the corresponding magnetic field 2
(5) introduce the rate of change factor-alpha of weighing,
Figure BDA0000063564740000021
Each group is demarcated with the corresponding m of appearance 1, m 2Substitution calculates each group and demarcates the α with appearance, and the Fe that demarcates with appearance is organized in match more 3O 4The linear relation of the massfraction and the rate of change factor-alpha of weighing;
(6) will contain Fe 3O 4The testing sample of mineral is contained in the above-mentioned same sample cup; Guarantee in shape, volume and the step (2) identical; With the described identical weighing equipment of step (2) on respectively weighing its in no magnetic field and the quality under the said magnetic field of step (3); Calculate the rate of change factor-alpha of weighing; Bring α the match linear relation of step (5) calibration sample gained into, can try to achieve Fe in the testing sample 3O 4Content.
The described demarcation of step (1) is selected many groups with appearance, and preferred more than 8 groups, each is organized material and in grinding machine, mixes.
The described sample cup of step (2) is selected non magnetic materials such as corundum, plastics for use, the material compacting in the cup, and it is identical to guarantee respectively to organize the height of material in cup, promptly volume of material is identical.
The method to set up in the described invariable magnetic field of step (3) is: select for use same magnet to be fixed on sustained height directly over the balance on goods and services, can guarantee that the type in magnetic field and intensity are all constant; Or select for use an electromagnet to be fixed on same position, current stabilization in the holding circuit can guarantee that the type in magnetic field and intensity are all constant.The magnetic field that provides should guarantee on the pallet the suffered magnetic force direction of magnetic weight vertically upward.
The present invention is by magnetic-weight effect, and the magnetic power of mineral is converted into visual gravity reading, and different magnetic minerals has distinctive magnetic-weight effect result under same magnetic field.This method is applicable to removes Fe in the mineral composition 3O 4Outward, other mineral that are weak magnetic or nonmagnetic material are measured, and this method is accurate, convenient, pollution-free, are particularly useful for the mensuration of percent reduction after the mineral reduction roastings such as haematite, red mud.
Description of drawings
Fig. 1 is magnetic in the embodiment-weight effect test platform figure,
Wherein 1.PVC manages test stand, 2. magnet, 3. height adjusting screw rod nut, 4. blowing sample cup, 5. electronic balance;
Fig. 2 is magnetic-weight effect test figure as a result under the embodiment 1 bar magnet magnetic field in the embodiment;
Fig. 3 is magnetic-weight effect test figure as a result under the embodiment 2 bar magnet magnetic fields in the embodiment;
Fig. 4 is magnetic-weight effect test figure as a result under the embodiment 3 bar magnet magnetic fields in the embodiment.
Embodiment
Embodiment 1
1, test equipment
Testing used equipment has: FA2204 type electronic balance can be accurate to 0.0001g; 8ml plastic sample cup; 155mm * 50mm * 25mm ferrite bar magnet, nearly Surface field intensity can reach 1300 Gausses; The self-control testing table, wherein magnet be positioned at the electronic balance pallet directly over, on the screw rod of magnet frame in the pvc pipe test stand of both sides, can come the distance of regulating magnet through the height of setting nut screw rod, like Fig. 1 apart from balance on goods and services.
Test used chemical reagent: the Shanghai traditional Chinese medicines Fe of group 2O 3Analyze pure, SiO 2Analyze pure and mild Fe 3O 4Analyze purely, purity is all greater than 99%.
2, test procedure
Fe in the fast measuring mineral 3O 4The method of content, its concrete test procedure is:
(1) uses Fe 2O 3, SiO 2And Fe 3O 4Allocate 10 groups of materials, Fe in every group of material 3O 4Massfraction as shown in table 1:
Table 1 is respectively organized Fe in the material 3O 4The massfraction table
Figure BDA0000063564740000031
(2) respectively organize material and all in grinding machine, passed through sufficient mixing, homogeneity of ingredients is able to guarantee; Material is contained in the plastic sample cup of same size respectively and compacting, and the material surface flushes with rim of a cup, and the shape that sample is respectively organized in assurance is identical, reduces test error.
(3) on magnetic-weight effect test platform, take off magnet, after the electronic balance zero clearing charged sample cup is put in weighing on the pallet respectively, circulate three times, and record data; Load onto magnet, make magnet, once more charged sample cup is put in weighing on the electronic balance respectively after the balance zero clearing, circulate three times apart from balance on goods and services 85mm (pallet place magnetic field intensity is about 85 Gausses), and record data.
Under the test condition in no magnetic field, bar magnet magnetic field, 10 groups of charge sample cups are carried out weighing respectively, repeat Fe in the statistical study material three times 3O 4The relation of the massfraction and the rate of change factor-alpha of weighing is like table 2, Fig. 2.
Table 2Fe 3O 4The massfraction and the rate of change factor-alpha statistical form of weighing
Figure BDA0000063564740000032
Figure BDA0000063564740000041
The match formula of Fig. 2 cathetus is y=0.1879x-0.0950 (x:Fe 3O 4Massfraction; Y: α), coefficient of determination R 2=0.9993, show Fe 3O 4Massfraction and weigh and present a kind of tangible once linear relationship between the rate of change factor-alpha.
(4) use Fe 2O 3, SiO 2And Fe 3O 4Allotment 1#, 2#, three groups of materials of 3#, simulation contains Fe 3O 4Mineral.After mixing, be contained in and demarcate used identical sample cup, and compacting, the material surface flushes with rim of a cup.Respectively no magnetic field and with demarcate used identical magnetic field condition under 3 groups of charge sample cups are carried out weighing, repeat three times, calculate α, bring α into demarcation gained match linear relation y=0.1879x-0.0950, solve Fe 3O 4Massfraction, and with actual value relatively, the result shows that both deviations are less, this method can be used for Fe in the mineral 3O 4The accurate mensuration of content, like table 3:
Table 3
Embodiment 2
(1) magnet among the embodiment 1 is adjusted to 90mm (magnetic field intensity is about 79 Gausses) here apart from the balance on goods and services distance, under this magnetic field condition, 10 groups of charge sample cups is carried out weighing, repeat Fe in the statistical study material three times 3O 4The relation of the massfraction and the rate of change factor-alpha of weighing is like table 4, Fig. 3.
Table 4Fe 3O 4The massfraction and the rate of change factor-alpha statistical form of weighing
Figure BDA0000063564740000051
The match formula of Fig. 3 cathetus is y=0.1479x-0.0295 (x:Fe 3O 4Massfraction; Y: α), coefficient of determination R 2=0.9998, show Fe 3O 4Massfraction and weigh and present a kind of tangible once linear relationship between the rate of change factor-alpha.
(2) sample cup that fills 1#, 2#, three groups of materials of 3# among the embodiment 1 is placed on embodiment 2 and demarcates under the used magnetic field and carry out weighing, repeat three times, calculate α, α is brought into demarcate gained match linear relation y=0.1479x-0.0295, solve Fe 3O 4Massfraction, and with actual value relatively, the result shows that both deviations are less, this method can be used for Fe in the mineral 3O 4The accurate mensuration of content is like table 5.
Table 5
Figure BDA0000063564740000052
Embodiment 3
(1) magnet among the embodiment 1 is adjusted to 95mm (magnetic field intensity is about 75 Gausses) here apart from the balance on goods and services distance, under this magnetic field condition, 10 groups of charge sample cups is carried out weighing, repeat Fe in the statistical study material three times 3O 4The relation of the massfraction and the rate of change factor-alpha of weighing is like table 6, Fig. 4.
Table 6Fe 3O 4The massfraction and the rate of change factor-alpha statistical form of weighing
Figure BDA0000063564740000061
The match formula of Fig. 4 cathetus is y=0.1153x-0.0908 (x:Fe 3O 4Massfraction; Y: α), coefficient of determination R 2=0.9987, show Fe 3O 4Massfraction and weigh and present a kind of tangible once linear relationship between the rate of change factor-alpha.
(2) sample cup that fills 1#, 2#, three groups of materials of 3# among the embodiment 1 is placed on embodiment 3 and demarcates under the used magnetic field and carry out weighing, repeat three times, calculate α, α is brought into demarcate gained match linear relation y=0.1153x-0.0908, solve Fe 3O 4Massfraction, and with actual value relatively, the result shows that both deviations are less, this method can be used for Fe in the mineral 3O 4The accurate mensuration of content is like table 7.
Table 7
Figure BDA0000063564740000062

Claims (5)

1. Fe in the fast measuring mineral 3O 4The method of content is characterized in that, comprises that step is following:
(1) uses Fe 3O 4Demarcate with appearance with weak magnetic or the many groups of nonmagnetic material preparation, many groups are demarcated the Fe with appearance 3O 4Massfraction from 0% to 100% distributes;
(2) each group is demarcated with appearance be placed in the same sample cup, guarantee that each group demarcates with shape and the volume of appearance in cup identically, each group of weighing and record is demarcated the no field quality that uses kind and is m 1
(3), above weighing equipment, add electromagnet or permanent magnet, for weighing equipment pallet place provides an invariable magnetic field with same weighing equipment;
(4) each m of weighing once more under the stationary magnetic field 1Quality is designated as m under the corresponding magnetic field 2
(5) introduce the rate of change factor-alpha of weighing, Each group is demarcated with the corresponding m of appearance 1, m 2Substitution calculates each group and demarcates the α with appearance, and the Fe that demarcates with appearance is organized in match more 3O 4The linear relation of the massfraction and the rate of change factor-alpha of weighing;
(6) will contain Fe 3O 4The testing sample of mineral is contained in the above-mentioned same sample cup; Guarantee in shape, volume and the step (2) identical; With the described identical weighing equipment of step (2) on respectively weighing its in no magnetic field and the quality under the said magnetic field of step (3); Calculate the rate of change factor-alpha of weighing; Bring α the match linear relation of step (5) calibration sample gained into, can try to achieve Fe in the testing sample 3O 4Content.
2. Fe in the fast measuring mineral according to claim 1 3O 4The method of content is characterized in that, it is more than 8 groups that appearance is used in the described demarcation of step (1), demarcates with appearance for every group all need mix.
3. Fe in the fast measuring mineral according to claim 1 3O 4The method of content is characterized in that, the described demarcation of step (1) is with appearance Fe 3O 4Massfraction from 0% to 100% evenly distributes.
4. Fe in the fast measuring mineral according to claim 1 3O 4The method of content is characterized in that, the described sample cup of step (2) is non magnetic material.
5. Fe in the fast measuring mineral according to claim 1 3O 4The method of content is characterized in that, step (3) magnetic field that provides should guarantee on the pallet the suffered magnetic force direction of magnetic weight vertically upward.
CN201110136196A 2011-05-25 2011-05-25 Method for quickly determining content of Fe3O4 in minerals Pending CN102305749A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104090021A (en) * 2014-06-18 2014-10-08 安徽科技学院 Method for detecting iron content of quartz sand by using magnetic susceptibility
CN104614275A (en) * 2015-01-29 2015-05-13 武汉科技大学 Method for measuring ferrous content in artificial lump ore
CN107796722A (en) * 2016-08-31 2018-03-13 鞍钢股份有限公司 A kind of method that bucket amount method measures selected granulated iron Tfe contents
CN114137060A (en) * 2021-11-29 2022-03-04 安徽工业大学 Method for detecting oxidability of casting residue

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54136393A (en) * 1978-04-14 1979-10-23 Mitsubishi Heavy Ind Ltd Measuring method of magnetic substance concentration in fluid
JPH03140837A (en) * 1989-10-27 1991-06-14 Nippon Steel Corp Method for measuring iron component in soluble oil
CN101105474A (en) * 2006-07-14 2008-01-16 中南大学 Ferriferrous oxide rapid determination method
CN201096749Y (en) * 2007-11-16 2008-08-06 横店集团东磁股份有限公司 Magnetic measuring device

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54136393A (en) * 1978-04-14 1979-10-23 Mitsubishi Heavy Ind Ltd Measuring method of magnetic substance concentration in fluid
JPH03140837A (en) * 1989-10-27 1991-06-14 Nippon Steel Corp Method for measuring iron component in soluble oil
CN101105474A (en) * 2006-07-14 2008-01-16 中南大学 Ferriferrous oxide rapid determination method
CN201096749Y (en) * 2007-11-16 2008-08-06 横店集团东磁股份有限公司 Magnetic measuring device

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104090021A (en) * 2014-06-18 2014-10-08 安徽科技学院 Method for detecting iron content of quartz sand by using magnetic susceptibility
CN104090021B (en) * 2014-06-18 2017-11-17 安徽科技学院 A kind of method that iron content in quartz sand is detected using magnetic susceptibility
CN104614275A (en) * 2015-01-29 2015-05-13 武汉科技大学 Method for measuring ferrous content in artificial lump ore
CN107796722A (en) * 2016-08-31 2018-03-13 鞍钢股份有限公司 A kind of method that bucket amount method measures selected granulated iron Tfe contents
CN107796722B (en) * 2016-08-31 2020-07-17 鞍钢股份有限公司 Method for measuring Tfe content of selected granular iron by bucket weighing method
CN114137060A (en) * 2021-11-29 2022-03-04 安徽工业大学 Method for detecting oxidability of casting residue

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Application publication date: 20120104