CN103376271A - Method for discriminating zinc concentrate from zinc-containing flue dust - Google Patents
Method for discriminating zinc concentrate from zinc-containing flue dust Download PDFInfo
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- CN103376271A CN103376271A CN2012101178163A CN201210117816A CN103376271A CN 103376271 A CN103376271 A CN 103376271A CN 2012101178163 A CN2012101178163 A CN 2012101178163A CN 201210117816 A CN201210117816 A CN 201210117816A CN 103376271 A CN103376271 A CN 103376271A
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Abstract
The invention relates to a method for discriminating zinc concentrate from zinc-containing flue dust and particularly relates to a method for discriminating zinc concentrate from zinc-containing flue dust, which is applicable to customs, inspection and quarantine laboratories and manufacture factories. According to the method, multi-means and multi-way attribute discrimination is carried out on the zinc concentrate and the zinc-containing flue dust by adopting an X-ray fluorescent spectrometry, a carbon black floatation method, an X-ray diffraction spectrometry and an electronic microscopy, and an effective method for discriminating the zinc concentrate from the zinc-containing flue dust is established, so that the behavior that overseas zinc-containing flue dust is misreported as the name of zinc concentrate products can be avoided, and a scientific, favorable and technical enforcement basis for fighting the smuggling of goods with misreported product names is provided for the customs and inspection and quarantine systems.
Description
Technical field
The present invention relates to a kind of zinc concentrate and contain the discrimination method of zinc flue dust, particularly a kind of being applicable to is customs and inspection and quarantine laboratory and manufacturer to zinc concentrate and contains the discrimination method of zinc flue dust.
Background technology
Zinc concentrate is through techniques such as fragmentation, ball milling, froth flotations and the higher ore of the zinc content that is up to state standards of producing is the primary raw material of production metallic zinc, zinc compound etc. by plumbous zinc ore or zinc-containing ores.Generally be by plumbous zinc ore or zinc-containing ores through techniques such as fragmentation, ball milling, froth flotations, produce the zinc concentrate that is up to state standards, the Main Ingredients and Appearance of zinc concentrate stipulates that according to product hierarchy zinc content is 40--55%.Contain zinc flue dust and be the smelting enterprise such as steel mill in smelting process owing to the higher flue dust of zinc content that adopts dust arrester to reclaim, also be quick ash, blast furnace gas dirt.Its chemical composition analysis satisfies or near the quality requirements of zinc concentrate.From also very nearly the same with the zinc concentrate powder in appearance.
Mineral substance solid waste is that manufacturing enterprise reduces cost, solves a kind of mode of raw mineral materials shortage, and therefore the very large market demand is arranged at home.Customs has carried out detailed classification to the import of solid waste, the utilized solid waste raw material that is divided into import prohibition, limiting inlet and permission import, contain the solid waste raw material that zinc flue dust belongs to customs's import prohibition, because outward appearance examination difficulty, normal pseudo-newspaper does not have scientific and effective attribute authentication technique at present for zinc concentrate or the immigration of zinc ore powder, therefore is difficult to implement effectively supervision, in unwitting situation, cause great threat to local environment and resident are healthy.
Summary of the invention
The present invention adopts the kinds of experiments chamber analytical technologies such as Xray fluorescence spectrometer, carbon black flotation, X-ray diffraction spectrum, electron microscope, to zinc concentrate with contain zinc flue dust and carry out the research of many means, multipath authentication technique, set up a kind of effective discriminating zinc concentrate and the method that contains zinc flue dust, avoid containing the behavior of the pseudo-newspaper of the zinc flue dust zinc concentrate name of an article overseas, the smuggled goods that hits such pseudo-newspaper name of an article for customs and inspection and quarantine system provides science favourable technology law enforcement foundation.
The present invention is achieved in that a kind of to zinc concentrate and the discrimination method that contains zinc flue dust, it is characterized in that taken separately discriminating step is as follows:
(1) draw samples quantity is no less than 100g, and is with the sample splitting that extracts, be crushed to all by 200 eye mesh screens, stand-by in 105 ℃ of oven dry;
(2) adopt x ray fluorescence spectrometry that sample is carried out the X-ray fluorescence spectra analysis: sample is pressed into the analysis print, put into XRF spectrometer sample chamber, adopt without standard specimen analysis software autoscan under the vacuum condition, deposit spectrogram and automatic analysis essential element content in, store to be checked; Essential element data and the Zinc Concentrates Quality normal data measured are compared, if it does not meet the Zinc Concentrates Quality standard, judge that tentatively this sample is not zinc concentrate, may be to contain zinc flue dust or other zinc-bearing mineral; Further adopt X-ray diffractometer to carry out the structure analysis of sample;
(3) if sample is black powder, then differentiate whether contain carbon black by following steps: get first 5-10 g sample and place in the 250 mL beakers, add water 100-200 mL, it is rear static to stir, and observes the dissolved state of sample in water; Other takes by weighing 5 g samples in the magnetic crucible, places 1000 ℃ of high temperature furnace calcinations, relatively the change color of sample before and after the calcination; If water surface floating has a large amount of black floating things, and color becomes yellow or brown by black behind 1000 ℃ of high temperature sinterings, then judges in this sample and contains carbon black, tentatively is judged as to contain zinc flue dust; Further adopt X-ray diffractometer to carry out the structure analysis of sample;
(4) adopt the X-ray diffraction spectroscopic methodology that sample is carried out the X-ray diffraction spectral analysis: dry sample is put into specimen holder, put into after the compacting on the X-ray diffraction spectrometer sample stage, scan and deposit in spectrogram, automatic analysis spectrum peak stores to be checked; If there is the feature diffracted ray of several zinc concentrates such as obvious zinc sulphide, zinc silicate in X-ray diffraction spectral analysis result, then the judgement sample attribute is zinc concentrate; If there is the feature diffracted ray of zinc paste in the X-ray diffraction analysis, and there is simultaneously the feature diffracted ray of zinc carbonate, zinc silicate, judges that then this sample is zinc concentrate; If there is the feature diffracted ray of zinc paste in the X-ray diffraction analysis, and there is simultaneously the feature diffracted ray of zinc-iron oxide, judges that then this sample contains zinc flue dust, further adopt electron microscope to carry out microexamination;
(5) adopt electron microscope method that sample is carried out microexamination: require preparation Microscopic observation sample according to the electron microscope sample, it is to be checked to put into microscope observation and document image; If scanning electron microscope result is amorphous powder, without obvious mineralogical character, then the judgement sample attribute is for containing zinc flue dust.
Description of drawings
Fig. 1 is for containing zinc flue buck flotation photo;
1-1# flue dust sample; 2-2# flue dust sample.
Fig. 2 is that 1# contains zinc flue dust sample through the photo before and after 1000 ℃ of calcinations;
3-1# flue dust former state; Sample after 1000 ℃ of calcinations of 4-1# flue dust.
Fig. 3 is that 2# contains zinc flue dust sample through the photo before and after 1000 ℃ of calcinations;
5-2# flue dust former state; Sample after 1000 ℃ of calcinations of 6-2# flue dust.
Fig. 4 is the XRD spectra of three class zinc concentrate standard models;
Fig. 5 is 2 kinds of XRD spectras that contain zinc flue dust sample;
Fig. 6 is that the 1# sample amplifies 1000 times electron micrograph;
Fig. 7 is that the 2# sample amplifies 1000 times electron micrograph;
Fig. 8 is that the zinc concentrate standard model amplifies 1000 times electron micrograph.
Embodiment
The invention will be further described by reference to the accompanying drawings.
The taken separately discriminating step of the present invention is as follows:
(1) draw samples quantity is no less than 100g, and is with the sample splitting that extracts, be crushed to all by 200 eye mesh screens, stand-by in 105 ℃ of oven dry;
(2) adopt x ray fluorescence spectrometry that sample is carried out the X-ray fluorescence spectra analysis: sample is pressed into the analysis print, put into XRF spectrometer sample chamber, adopt without standard specimen analysis software autoscan under the vacuum condition, deposit spectrogram and automatic analysis essential element content in, store to be checked; Essential element data and the Zinc Concentrates Quality normal data measured are compared, if it does not meet the Zinc Concentrates Quality standard, judge that tentatively this sample is not zinc concentrate, may be to contain zinc flue dust or other zinc-bearing mineral; Further adopt X-ray diffractometer to carry out the structure analysis of sample;
(3) if sample is black powder, then differentiate whether contain carbon black by following steps: get first 5-10 g sample and place in the 250 mL beakers, add water 100-200 mL, it is rear static to stir, and observes the dissolved state of sample in water; Other takes by weighing 5 g samples in the magnetic crucible, places 1000 ℃ of high temperature furnace calcinations, relatively the change color of sample before and after the calcination; If water surface floating has a large amount of black floating things, and color becomes yellow or brown by black behind 1000 ℃ of high temperature sinterings, then judges in this sample and contains carbon black, tentatively is judged as to contain zinc flue dust; Further adopt X-ray diffractometer to carry out the structure analysis of sample;
(4) adopt the X-ray diffraction spectroscopic methodology that sample is carried out the X-ray diffraction spectral analysis: dry sample is put into specimen holder, put into after the compacting on the X-ray diffraction spectrometer sample stage, scan and deposit in spectrogram, automatic analysis spectrum peak stores to be checked; If there is the feature diffracted ray of several zinc concentrates such as obvious zinc sulphide, zinc silicate in X-ray diffraction spectral analysis result, then the judgement sample attribute is zinc concentrate; If there is the feature diffracted ray of zinc paste in the X-ray diffraction analysis, and there is simultaneously the feature diffracted ray of zinc carbonate, zinc silicate, judges that then this sample is zinc concentrate; If there is the feature diffracted ray of zinc paste in the X-ray diffraction analysis, and there is simultaneously the feature diffracted ray of zinc-iron oxide, judges that then this sample contains zinc flue dust, further adopt electron microscope to carry out microexamination;
(5) adopt electron microscope method that sample is carried out microexamination: require preparation Microscopic observation sample according to the electron microscope sample, it is to be checked to put into microscope observation and document image; If scanning electron microscope result is amorphous powder, without obvious mineralogical character, then the judgement sample attribute is for containing zinc flue dust.
Embodiment 1:
Contain zinc flue dust sample as embodiment take 2 kinds, differentiate that step and expert's conclusion are as follows:
(1) draw samples quantity is no less than 100g, and is with the sample splitting that extracts, be crushed to all by 200 eye mesh screens, stand-by in 105 ℃ of oven dry.
(2) adopt x ray fluorescence spectrometry that sample is carried out the X-ray fluorescence spectra analysis: sample is pressed into the analysis print, put into XRF spectrometer sample chamber, adopt without standard specimen analysis software autoscan under the vacuum condition, deposit spectrogram and automatic analysis essential element content in, store to be checked; Essential element data and the Zinc Concentrates Quality normal data measured are compared, if it does not meet the Zinc Concentrates Quality standard, judge that tentatively this sample is not zinc concentrate, may be to contain zinc flue dust or other zinc-bearing mineral; Table 1 is the Zinc Concentrates Quality standard, and table 2 is 2 kinds of X-ray fluorescence spectra analysis results that contain zinc flue dust; 2 kinds of samples of preliminary judgement are not zinc concentrates, further adopt X-ray diffractometer to carry out the structure analysis of sample.
Table 1 Zinc Concentrates Quality index
| Grade | Zn(%) | Cu(%) | Pb(%) | Fe(%) |
| 1 | ≧55 | ≦0.8 | ≦1.0 | ≦6.0 |
| 2 | ≧53 | ≦0.8 | ≦1.0 | ≦6.0 |
| 3 | ≧50 | ≦1.0 | ≦1.5 | ≦8.0 |
| 4 | ≧48 | ≦1.0 | ≦1.5 | ≦12.0 |
| 5 | ≧45 | ≦1.5 | ≦2.0 | ≦12.0 |
| 6 | ≧43 | ≦1.5 | ≦2.0 | ≦12.0 |
| 7 | ≧40 | ≦2.0 | ≦2.5 | ≦14.0 |
| 8 | ≧40 | ≦2.0 | ≦2.8 | ≦18.0 |
Table 2 is 2 kinds of X-ray fluorescence spectra analysis results that contain zinc flue dust
| Sample number into spectrum | Zn(%) | Cu(%) | Pb(%) | Fe(%) |
| 1# | 21.72 | 0.68 | 1.6 | 8.18 |
| 2# | 43.31 | 0.32 | 4.76 | 18.64 |
(3) check by outward appearance, the 1# sample is black powder, the 2# sample is the tawny powder, differentiate in 2 kinds of samples whether contain carbon black by following steps: get first 5-10 g sample and place in the 250 mL beakers, add water 100-200 mL, it is rear static to stir, and observes the dissolved state of sample in water; Other takes by weighing 5 g samples in the magnetic crucible, places 1000 ℃ of high temperature furnace calcinations, relatively the change color of sample before and after the calcination; Fig. 1 is for containing zinc flue buck flotation photo, wherein, and 1-1# flue dust sample; 2-2# flue dust sample.Fig. 2 is that 1# contains zinc flue dust sample through the photo before and after 1000 ℃ of calcinations, wherein, and 3-1# flue dust former state; Sample after 1000 ℃ of calcinations of 4-1# flue dust.Fig. 3 is that 2# contains zinc flue dust sample through the photo before and after 1000 ℃ of calcinations, wherein, and 5-2# flue dust former state; Sample after 1000 ℃ of calcinations of 6-2# flue dust.Can find out in from figure that the 1# sample is through carbon black flotation experiment, water surface floating has a large amount of black floating things, may be carbon black, and color becomes yellow by black behind 1000 ℃ of high temperature sinterings, judges in the 1# sample to contain carbon black, tentatively is judged as to contain zinc flue dust; Do not contain carbon black in the 2# sample, attribute is unknown.Further adopt X-ray diffractometer to carry out the structure analysis of sample.
(4) adopt the X-ray diffraction spectroscopic methodology that sample is carried out the X-ray diffraction spectral analysis: dry sample is put into specimen holder, put into after the compacting on the X-ray diffraction spectrometer sample stage, scan and deposit in spectrogram, automatic analysis spectrum peak stores to be checked; If there is the feature diffracted ray of several zinc concentrates such as obvious zinc sulphide, zinc silicate in X-ray diffraction spectral analysis result, then the judgement sample attribute is zinc concentrate; If there is the feature diffracted ray of zinc paste in the X-ray diffraction analysis, and there is simultaneously the feature diffracted ray of zinc carbonate, zinc silicate, judges that then this sample is zinc concentrate; If there is the feature diffracted ray of zinc paste in the X-ray diffraction analysis, and there is simultaneously the feature diffracted ray of zinc-iron oxide, judges that then this sample contains zinc flue dust, further adopt electron microscope to carry out microexamination; Fig. 4 is the XRD spectra of three class zinc concentrate standard models, and Fig. 5 is 2 kinds of XRD spectras that contain zinc flue dust sample.
(5) adopt electron microscope method that sample is carried out microexamination: require preparation Microscopic observation sample according to the electron microscope sample, it is to be checked to put into microscope observation and document image; If scanning electron microscope result is amorphous powder, without obvious mineralogical character, then the judgement sample attribute is for containing zinc flue dust.Fig. 6 is that the 1# sample amplifies 1000 times electron micrograph, and Fig. 7 is that the 2# sample amplifies 1000 times electron micrograph, and Fig. 8 is that the zinc concentrate standard model amplifies 1000 times electron micrograph.Relatively can reach a conclusion, 1# and 2# flue dust sample are amorphous powder, without obvious mineralogical character.
Claims (1)
- Zinc concentrate with contain the discrimination method of zinc flue dust, it is characterized in that taken separately discriminating step is as follows:(1) draw samples quantity is no less than 100g, and is with the sample splitting that extracts, be crushed to all by 200 eye mesh screens, stand-by in 105 ℃ of oven dry;(2) adopt x ray fluorescence spectrometry that sample is carried out the X-ray fluorescence spectra analysis: sample is pressed into the analysis print, put into XRF spectrometer sample chamber, adopt without standard specimen analysis software autoscan under the vacuum condition, deposit spectrogram and automatic analysis essential element content in, store to be checked; Essential element data and the Zinc Concentrates Quality normal data measured are compared, if it does not meet the Zinc Concentrates Quality standard, judge that tentatively this sample is not zinc concentrate, may be to contain zinc flue dust or other zinc-bearing mineral; Further adopt X-ray diffractometer to carry out the structure analysis of sample;(3) if sample is black powder, then differentiate whether contain carbon black by following steps: get first 5-10 g sample and place in the 250 mL beakers, add water 100-200 mL, it is rear static to stir, and observes the dissolved state of sample in water; Other takes by weighing 5 g samples in the magnetic crucible, places 1000 ℃ of high temperature furnace calcinations, relatively the change color of sample before and after the calcination; If water surface floating has a large amount of black floating things, and color becomes yellow or brown by black behind 1000 ℃ of high temperature sinterings, then judges in this sample and contains carbon black, tentatively is judged as to contain zinc flue dust; Further adopt X-ray diffractometer to carry out the structure analysis of sample;(4) adopt the X-ray diffraction spectroscopic methodology that sample is carried out the X-ray diffraction spectral analysis: dry sample is put into specimen holder, put into after the compacting on the X-ray diffraction spectrometer sample stage, scan and deposit in spectrogram, automatic analysis spectrum peak stores to be checked; If there is the feature diffracted ray of several zinc concentrates such as obvious zinc sulphide, zinc silicate in X-ray diffraction spectral analysis result, then the judgement sample attribute is zinc concentrate; If there is the feature diffracted ray of zinc paste in the X-ray diffraction analysis, and there is simultaneously the feature diffracted ray of zinc carbonate, zinc silicate, judges that then this sample is zinc concentrate; If there is the feature diffracted ray of zinc paste in the X-ray diffraction analysis, and there is simultaneously the feature diffracted ray of zinc-iron oxide, judges that then this sample contains zinc flue dust, further adopt electron microscope to carry out microexamination;(5) adopt electron microscope method that sample is carried out microexamination: require preparation Microscopic observation sample according to the electron microscope sample, it is to be checked to put into microscope observation and document image; If scanning electron microscope result is amorphous powder, without obvious mineralogical character, then the judgement sample attribute is for containing zinc flue dust.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104198514A (en) * | 2014-09-22 | 2014-12-10 | 天津出入境检验检疫局化矿金属材料检测中心 | Method for identifying properties of manganese ore and manganese smelting slag |
| CN104237220A (en) * | 2014-08-22 | 2014-12-24 | 济南钢城矿业有限公司 | Method for detecting content of iron, sulfur, phosphorus and silicon dioxide of rolling ball for steelmaking |
| CN106885814A (en) * | 2017-03-07 | 2017-06-23 | 阿拉山口出入境检验检疫局综合技术服务中心 | Copper mine and cupric slightly refining or the discriminating of sintered material attribute |
| CN106940325A (en) * | 2017-04-12 | 2017-07-11 | 神华集团有限责任公司 | The detection method of heat transmission equipment dirt sample |
| CN107305191A (en) * | 2016-04-19 | 2017-10-31 | 中国石油天然气股份有限公司 | Determine the powder x-ray diffraction method of magnesium aluminate spinel phase content in catalyst |
| CN107462543A (en) * | 2017-10-09 | 2017-12-12 | 阿拉山口出入境检验检疫局综合技术服务中心 | A kind of detection method that copper mine and copper-contained material are detected based on infra-red sepectrometry |
| CN110376230A (en) * | 2019-08-13 | 2019-10-25 | 凉山矿业股份有限公司 | The method of X-ray fluorescence spectra analysis boiler smoke Cu, As, Pb, Zn element |
| WO2020199292A1 (en) * | 2019-04-04 | 2020-10-08 | 山东大学 | Smart lithologic characteristic recognition system and method employing image and spectroscopy technology |
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| CN104237220A (en) * | 2014-08-22 | 2014-12-24 | 济南钢城矿业有限公司 | Method for detecting content of iron, sulfur, phosphorus and silicon dioxide of rolling ball for steelmaking |
| CN104198514A (en) * | 2014-09-22 | 2014-12-10 | 天津出入境检验检疫局化矿金属材料检测中心 | Method for identifying properties of manganese ore and manganese smelting slag |
| CN104198514B (en) * | 2014-09-22 | 2016-08-24 | 天津出入境检验检疫局化矿金属材料检测中心 | Manganese ore and manganese metallurgical slag attribute discrimination method |
| CN107305191A (en) * | 2016-04-19 | 2017-10-31 | 中国石油天然气股份有限公司 | Determine the powder x-ray diffraction method of magnesium aluminate spinel phase content in catalyst |
| CN107305191B (en) * | 2016-04-19 | 2020-02-14 | 中国石油天然气股份有限公司 | Powder X-ray diffraction method for determining content of magnesium aluminate spinel phase in catalyst |
| CN106885814A (en) * | 2017-03-07 | 2017-06-23 | 阿拉山口出入境检验检疫局综合技术服务中心 | Copper mine and cupric slightly refining or the discriminating of sintered material attribute |
| CN106940325A (en) * | 2017-04-12 | 2017-07-11 | 神华集团有限责任公司 | The detection method of heat transmission equipment dirt sample |
| CN107462543A (en) * | 2017-10-09 | 2017-12-12 | 阿拉山口出入境检验检疫局综合技术服务中心 | A kind of detection method that copper mine and copper-contained material are detected based on infra-red sepectrometry |
| WO2020199292A1 (en) * | 2019-04-04 | 2020-10-08 | 山东大学 | Smart lithologic characteristic recognition system and method employing image and spectroscopy technology |
| US11536639B2 (en) | 2019-04-04 | 2022-12-27 | Shandong University | Intelligent lithology identification system and method based on images and spectrum technology |
| CN110376230A (en) * | 2019-08-13 | 2019-10-25 | 凉山矿业股份有限公司 | The method of X-ray fluorescence spectra analysis boiler smoke Cu, As, Pb, Zn element |
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Application publication date: 20131030 |