CN108226199A - The method for quantitatively determining of tin anode mud material composition - Google Patents
The method for quantitatively determining of tin anode mud material composition Download PDFInfo
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- CN108226199A CN108226199A CN201611158437.3A CN201611158437A CN108226199A CN 108226199 A CN108226199 A CN 108226199A CN 201611158437 A CN201611158437 A CN 201611158437A CN 108226199 A CN108226199 A CN 108226199A
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N23/22—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 by measuring secondary emission from the material
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N23/22—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 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
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Abstract
The invention discloses a kind of method for quantitatively determining of tin anode mud material composition.Include the following steps：(1) appropriate tin anode mud sample is taken to carry out segmentation and rolls low temperature drying, the sample dried completely passes through division and screening, obtains gradation grade sample；(2) size fractionated sample is subjected to secondary cold edge sample preparation, rubbing down, plating conductive layer processing, obtains can be used for scanning electron microscope analysis sample；(3) using each substance standard specimen of MLA system acquisitions, the standard specimen X ray spectrograms of acquisition are added in MLA system standard specimen X ray spectrograms library, standard specimen X ray spectrograms library is arranged and is named；(4) data are handled by MLA network analyses, obtains the quantitative material composition and Elemental redistribution of each substance of tin anode mud sample.The present invention can obtain the sample for being suitble to MLA analyses by the improvement to method for making sample, by establishing tin anode mud X ray spectrogram standard specimen libraries and carrying out micro-area composition statistical analysis to tin anode mud sample, obtain the material composition and Elemental redistribution of tin anode mud relative quantification.
Description
Technical field
The present invention relates to a kind of method for quantitatively determining of tin anode mud material composition, and in particular to a kind of to utilize mineral parameter
The method of the content and distributions of metallic elements of metallics in automatically quantitative analysis system quantitative determination tin anode mud.
Background technology
The pureed plasma of cell bottom is fallen within when the earth of positive pole is electrorefining.Mainly by not dissolved in anode crude metal
The impurity of electrolyte and metal to be refined composition.Often containing valuable and metal values, can recycle as Extracting Gold,
The raw material of the precious metals such as silver.
In order to determine the essential element type and content of raw material, mainly determined using X-fluorescence semi-quantitative analysis and chemical element
Amount analysis.In order to study the chemical constitution of each substance, it is substantially carried out X-ray diffraction semi-quantitative analysis.Above method cannot provide
Quantitative material composition as a result, and the data such as the distribution in substance that can not obtain element.
Mineral parameter automatically quantitative analysis system (Mineral Liberation Analyzer, hereinafter referred to as MLA systems)
It is made of scanning electron microscope, energy disperse spectroscopy and automatic quantitative analysis of mineral software, the method that substance quantitative analysis is provided, X- can be utilized
The difference of Ray spectral peaks distinguishes and quantifies different material, and MLA systems provide automatically and manually standard specimen acquisition method.MLA systems
System is mainly used in the process mineralogy research of metallic ore, forms more mature mineral samplers database, but tin anode
The ingredient of mud and non-natural mineral, carrying out the analysis of earth of positive pole sample amounts currently with MLA systems, there has been no applications.It is based on
MLA systems provide manual standard specimen acquisition method, and the quantitative determination for the earth of positive pole provides the foundation.
In order to obtain MLA system measurement datas, sample must be made to the mating plate of suitable MLA systematic surveys first.It is in view of positive
The humidity of pole mud is big, hardness is big, heavy feature, and traditional mineral are disposably dried, the method for making sample of primary cold edge is easily made
Into mineral caking phenomenon seriously and the problem of subsidence effect is apparent, thus need to the certain improvement of method for making sample progress.
Invention content
The purpose of the present invention is to provide a kind of method for quantitatively determining of tin anode mud material composition, and tin sun is measured with analysis
The content and Elemental redistribution of substance in the mud of pole reach the result of quantitative analysis.
To achieve the above object, the present invention uses following technical scheme：
A kind of method for quantitatively determining of tin anode mud material composition, includes the following steps：
(1) appropriate tin anode mud sample is taken to carry out segmentation and rolls low temperature drying, the sample dried completely passes through division and sieve
Point, obtain gradation grade sample；
(2) size fractionated sample is subjected to secondary cold edge sample preparation, rubbing down, plating conductive layer processing, obtains can be used for scanning electricity
Mirror analyzes sample；
(3) using each substance standard specimen of MLA system acquisitions, the standard specimen X-ray spectrograms of acquisition are added to MLA system standard specimens X-
In ray spectrograms library, standard specimen X-ray spectrograms library is arranged and is named；
(4) data are handled by MLA network analyses, X-ray energy spectrum analysis systems is carried out using XBSE patterns to sample particle
Meter, measured X-Ray spectrograms with standard specimen library X-ray spectrograms are compared, measurement result is analyzed and processed to obtain tin
The quantitative material composition and Elemental redistribution of each substance of earth of positive pole sample.
Wherein, the segmentation, which rolls low temperature drying, is dried in low temperature baking oven, and sample is carried out every a period of time
It rolls, solves the caking phenomenon of sample.
The division and screening refer to using sample quarterlies 500g or so, and are sized to 4-5 grade.
The secondary cold edge sample preparation refers to use epoxy resin and coagulator V in proportionEpoxy resin∶VCoagulator=15: 2 proportionings, and
It is uniformly mixed with sample, 2-3 blocks is cut into along sample vertical section after sample solidification, rip cutting with epoxy resin and is coagulated down
Gu agent V in proportionEpoxy resin∶VCoagulator=15: 2 proportionings carry out secondary cold edge and mating plate are made.Secondary cold edge sample preparation solves sample sedimentation effect
The influence that should be brought.
The plating conductive layer processing refers to make sample surfaces conduction using spraying plating or vapor deposition means, preferably to sample surfaces into
Row plating carbon processing.
The advantage of the invention is that：
The present invention can obtain the sample for being suitble to MLA analyses, by establishing tin anode mud X- by the improvement to method for making sample
Ray spectrogram standard specimen libraries and to tin anode mud sample carry out micro-area composition statistical analysis, obtain the substance of tin anode mud relative quantification
The results such as composition and Elemental redistribution.
The present invention utilizes the standard specimen acquisition system of the offer of MLA, establishes the X-Ray spectrograms of the main matter in tin anode mud
Standard specimen database, the data obtained can provide guidance for high efficiente callback using the earth of positive pole.
Specific embodiment
With reference to embodiment, the present invention will be further described, but the present invention is not limited thereto.
The method for quantitatively determining of the tin anode mud material composition of the present invention is to utilize automatic quantitative analysis of mineral systematic quantification
The method for measuring the content and distributions of metallic elements of metallics in tin anode mud, specific steps include：
(1) sample segmentation is rolled into low temperature drying, is dried in low temperature baking oven, every a period of time (20min) to sample
Product are once rolled, until sample is dried.Segmentation is rolled to destroy intergranular bonding, while keep tin anode mud in itself
Granularity.
(2) to sample using sample quarterlies 500g or so, and it is sized to 4-5 grade.
(3) secondary cold edge sample preparation is carried out to sample, using epoxy resin and coagulator V in proportionEpoxy resin∶VCoagulator=15: 2
Proportioning, is uniformly mixed with sample, cuts into 2-3 blocks along sample vertical section after sample solidification, rip cutting is used asphalt mixtures modified by epoxy resin down
Fat and coagulator V in proportionEpoxy resin∶VCoagulator=15: 2 proportionings carry out secondary cold edge, and the secondary cold edge mating plate of 30mm diameters is made.
(4) sample surfaces are carried out with plating carbon or other spraying platings, the processing of vapor deposition means, makes sample surfaces conductive.
(5) it is measured using MLA systems, MLA system acquisitions and the X-Ray spectrograms for naming different material, by manual
Addition editor's standard specimen obtains tin anode mud X-ray spectrogram standard specimens library, and statistical measurement, measured X-Ray are carried out to sample particle
Spectrogram is compared with standard specimen library X-ray spectrograms, and measurement result handles to obtain the material composition of the sample, element point by analysis
The useful datas such as cloth.
Embodiment
Analysis of chemical elements result shows that main metal element includes tin (Sn), copper (Cu), lead in certain tin anode mud sample
(Pb), Sb (antimony), iron (Fe), nickel (Ni), containing a small amount of zinc (Zn), silver-colored (Ag) and gold (Au), wherein based on Sn and Cu, content
26.8% and 26.57% are accounted for respectively.XRD results show that the sample main matter has SnO2、CuS。
Tin anode mud is measured using automatic quantitative analysis of mineral systematic quantification, determination step is as follows：
(1) tin anode mud sample in low temperature baking oven is dried, sample is once rolled every 20min, broken
Bad intergranular bonding, while the granularity of tin anode mud in itself is kept, until sample is dried completely.
(2) sample quarterlies 500g or so is carried out to sample, and is sized to 5 grades, each grade yield is shown in Table 1.
(3) secondary cold edge sample preparation is carried out to sample, using epoxy resin and coagulator V in proportionEpoxy resin∶VCoagulator=15: 2
Proportioning, is uniformly mixed with sample, and+40 mesh and -40+100 mesh are cut into 3 pieces along sample vertical section after sample solidification carries out two
Secondary cold edge, remaining sample cut into 2 pieces and carry out secondary cold edge, wherein -100+320 mesh sample, which chooses 2 pieces, carries out secondary cold edge, -
320+500 mesh and -500 mesh samples choose 1 piece and carry out secondary cold edge.Rip cutting with epoxy resin and is coagulated down during secondary cold edge
Gu agent V in proportionEpoxy resin∶VCoagulator=15: 2 proportionings are inlayed, and the mating plate of 30mm diameters is made.
(4) mating plate surface is carried out plating carbon processing makes sample surfaces conductive.
(5) to all samples carry out MLA measure, using XBSE_STD type collections and establish different material X-Ray mark
Sample library adds and names standard specimen manually, using XBSE pattern measurement data.XBSE_STD patterns are standard specimen drainage patterns, are adopted altogether
Collect 18 standard specimens.X-Ray energy spectrum analysis is carried out to each standard specimen, obtains its composition information, some complicated alloys are taken
Multiple X-Ray constituent analyses are averaged.And after thus being classified according to follow-up measurement, existing unknown materials are adopted manually
Collection standard specimen is simultaneously added in standard specimen library.Finally establish standard specimen totally 31 in standard specimen library.
(6) measurement result is analyzed and is handled, acquired results are final material composition result.The tin anode mud sample
Material composition the results are shown in Table 2.Main matter is with impure SnO in the tin anode mud sample2Based on, wherein impurity element is main
For Sb, Cu, Pb, Ni, mainly with the SnO containing Sb, Cu impurity element2(SnO2_ SbCu), the SnO containing Sb, Pb, Cu impurity element2
(SnO2_ SbPbCu), the SnO containing Sb, Pb, Ni, Cu impurity element2(SnO2_ SbPbNiCu) three kinds of forms exist, total content
Account for about the 61.01% of mineral total amount.Secondly it is the sulfide of copper, including sulfide Cu5FeS4、Cu3S2Sn0.1, CuS and
Cu4FeS4.5, wherein with Cu5FeS4(bornite) and Cu3S2Sn0.1Based on, content accounts for 18.3% He of total material composition respectively
13.65%, CuS account for total material composition 0.89%.Separately contain a small amount of copper alloy (Cu5.6Sn1.9Ni1.7Sb0.8), elemental copper (contains Ni
And Fe) and elementary lead (Pb), content account for 4.27%, 0.39% and the 0.76% of total amount respectively.Other content of material are relatively low.+
In 40 mesh and -40+100 mesh products, SnO2Content is slightly lower compared with content for other three grades, wherein SnO in -500 mesh products2
Content highest.And content of the copper-containing substance in+40 mesh and -40+100 mesh products is slightly higher compared with other grade products, illustrates that copper exists
There are more in the larger range of grade, and stanniferous substance is more in the less range of grade.
Tin anode mud sample main metal element distribution is shown in Table 3.Tin (Sn) is mainly with oxide (SnO in the sample2)
Form exists, and is present in copper alloy and copper sulfide with Impure forms on a small quantity, copper (Cu) is mainly with sulfide (Cu5FeS4、
Cu3S2Sn0.1, CuS and Cu4FeS4.5), exist and with Impure forms in the form of copper alloy (containing Sn, Ni, Sb and Fe in Cu) on a small quantity
It is wrapped in SnO2In.Lead (Pb) is mainly contained in SnO with Impure forms2In, also a small amount of simple substance.Sb (antimony) is mainly with impurity shape
Formula is contained in SnO2In, it is wrapped in copper alloy with Impure forms on a small quantity.Iron (Fe) is mainly with Cu5FeS4Form exist, on a small quantity with
Form of iron oxide exists, and separately has and a small amount of Fe is present in high-iron sphalerite in (ZnS_Fe) or ormolu, copper alloy.Nickel
(Ni) it is mainly wrapped in copper alloy with Impure forms, fraction is contained in SnO with Impure forms2In.Zn is mainly distributed on height
(ZnS_Fe) and certain ormolu (Cu in marmatite2ZnS2_ Fe) in.Silver-colored (Ag) mainly exists with simple substance form.
Certain the tin anode mud sample screening yield table of table 1
| Granularity/mesh | +40 | -40+100 | -100+320 | -320+500 | -500 | It is total |
| Yield/% | 31.3 | 22.43 | 19.06 | 11.59 | 15.62 | 100 |
Each grade of certain tin anode mud of table 2 and total material composition
Certain the tin anode mud sample main metal element distribution table of table 3
| Substance | Sn (%) | Ag (%) | Cu (%) | Fe (%) | Ni (%) | Pb (%) | Sb (%) | Zn (%) |
| SnO2_SbCu | 12.92 | 0 | 0.32 | 0 | 0 | 0 | 15.48 | 0 |
| SnO2_SbPbCu | 41.35 | 0 | 1.01 | 0 | 0 | 33.17 | 26 | 0 |
| SnO2_SbPbNiCu | 33.38 | 0 | 1.54 | 0 | 38.32 | 65.64 | 46.98 | 0 |
| SnPO4_Cu | 0.15 | 0 | 0.01 | 0 | 0 | 0 | 0 | 0 |
| Cu3S2Sn0.1 | 3.05 | 0 | 24.84 | 0 | 0 | 0 | 0 | 0 |
| Cu5FeS4 | 0 | 0 | 60.66 | 98.84 | 0 | 0 | 0 | 0 |
| Cu4FeS4.5 | 0 | 0 | 0.2 | 0.4 | 0 | 0 | 0 | 0 |
| Cu8.4Ni1.3Fe0.3 | 0 | 0 | 2.61 | 0.76 | 9.5 | 0 | 0 | 0 |
| Cu5.6Sn1.9Ni1.7Sb0.8 | 9.15 | 0 | 7.32 | 0 | 52.18 | 0 | 11.54 | 0 |
| Cu2ZnS2_Fe | 0 | 0 | 0.01 | 0 | 0 | 0 | 0 | 82.36 |
| CuS | 0 | 0 | 1.48 | 0 | 0 | 0 | 0 | 0 |
| Pb | 0 | 0 | 0 | 0 | 0 | 1.19 | 0 | 0 |
| ZnS_Fe | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 17.64 |
| Ag | 0 | 100 | 0 | 0 | 0 | 0 | 0 | 0 |
| It is total | 100 | 100 | 100 | 100 | 100 | 100 | 100 | 100 |
Claims (4)
1. a kind of method for quantitatively determining of tin anode mud material composition, which is characterized in that include the following steps：
(1) appropriate tin anode mud sample is taken to carry out segmentation and rolls low temperature drying, the sample dried completely passes through division and screening, obtains
To gradation grade sample；
(2) size fractionated sample is subjected to secondary cold edge sample preparation, rubbing down, plating conductive layer processing, obtained available for scanning electron microscope point
Analyse sample；
(3) using each substance standard specimen of MLA system acquisitions, the standard specimen X-ray spectrograms of acquisition are added to MLA system standard specimens X-ray
In spectrogram library, standard specimen X-ray spectrograms library is arranged and is named；
(4) data are handled by MLA network analyses, statistical measurement is carried out to sample particle, by measured X-Ray spectrograms and mark
Sample library X-ray spectrograms are compared, and measurement result is analyzed and processed to obtain the quantitative material of each substance of tin anode mud sample
Composition and Elemental redistribution.
2. the method for quantitatively determining of tin anode mud material composition as described in claim 1, which is characterized in that the segmentation rolls
Low temperature drying is dried in low temperature baking oven, and interval 10-30min rolls sample, solves the caking phenomenon of sample.
3. the method for quantitatively determining of tin anode mud material composition as described in claim 1, which is characterized in that the division and sieve
Divide and refer to using sample quarterlies 500g, and be sized to 4-5 grade.
4. the method for quantitatively determining of tin anode mud material composition as described in claim 1, which is characterized in that the secondary cold edge
Sample preparation refers to use epoxy resin and coagulator V in proportionEpoxy resin∶VCoagulator=15: 2 proportionings, and be uniformly mixed with sample, treat sample
2-3 blocks are cut into along sample vertical section after product solidification, rip cutting is used to epoxy resin and coagulator V in proportion downEpoxy resin∶
VCoagulator=15: 2 proportionings carry out secondary cold edge and mating plate are made.
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Cited By (5)
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| CN108876311A (en) * | 2018-07-16 | 2018-11-23 | 河南聚合科技有限公司 | A kind of mineral selecting screening separation equipment cloud platform based on Internet of Things |
| CN112461629A (en) * | 2020-12-09 | 2021-03-09 | 金川集团股份有限公司 | Method for establishing hydrometallurgy intermediate product substance composition detection flow |
| CN112557429A (en) * | 2020-12-15 | 2021-03-26 | 广东省科学院资源综合利用研究所 | Quantitative determination method for all minerals in graphite ore and sample preparation method |
| CN112710687A (en) * | 2020-12-08 | 2021-04-27 | 长春黄金研究院有限公司 | Method for testing existence form of adsorbed fluorine element in electronic waste |
| CN114047362A (en) * | 2021-11-08 | 2022-02-15 | 广东省科学院资源利用与稀土开发研究所 | Silicate ceramic composition detection method |
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| CN108876311A (en) * | 2018-07-16 | 2018-11-23 | 河南聚合科技有限公司 | A kind of mineral selecting screening separation equipment cloud platform based on Internet of Things |
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| CN112710687B (en) * | 2020-12-08 | 2023-11-07 | 长春黄金研究院有限公司 | Method for testing existence form of adsorbed fluorine element in electronic waste |
| CN112461629A (en) * | 2020-12-09 | 2021-03-09 | 金川集团股份有限公司 | Method for establishing hydrometallurgy intermediate product substance composition detection flow |
| CN112461629B (en) * | 2020-12-09 | 2023-09-22 | 金川集团股份有限公司 | Establishment method of hydrometallurgical intermediate product substance composition detection flow |
| CN112557429A (en) * | 2020-12-15 | 2021-03-26 | 广东省科学院资源综合利用研究所 | Quantitative determination method for all minerals in graphite ore and sample preparation method |
| CN112557429B (en) * | 2020-12-15 | 2023-12-01 | 广东省科学院资源综合利用研究所 | Quantitative determination method and sample preparation method for all minerals in graphite ore |
| CN114047362A (en) * | 2021-11-08 | 2022-02-15 | 广东省科学院资源利用与稀土开发研究所 | Silicate ceramic composition detection method |
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