CN107462543A - A kind of detection method that copper mine and copper-contained material are detected based on infra-red sepectrometry - Google Patents

A kind of detection method that copper mine and copper-contained material are detected based on infra-red sepectrometry Download PDF

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Publication number
CN107462543A
CN107462543A CN201710930117.3A CN201710930117A CN107462543A CN 107462543 A CN107462543 A CN 107462543A CN 201710930117 A CN201710930117 A CN 201710930117A CN 107462543 A CN107462543 A CN 107462543A
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copper
sample
contained material
detection method
infra
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Inventor
吕新明
孙春晓
田延河
王吉德
周安丽
陈伟
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COMPREHENSIVE TECHNOLOGY SERVICE CENTER ALASHANKOU ENTRY-EXIT INSPECTION AND QUARANTINE BUREAU
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COMPREHENSIVE TECHNOLOGY SERVICE CENTER ALASHANKOU ENTRY-EXIT INSPECTION AND QUARANTINE BUREAU
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Priority to CN201710930117.3A priority Critical patent/CN107462543A/en
Publication of CN107462543A publication Critical patent/CN107462543A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
    • G01N2021/3572Preparation of samples, e.g. salt matrices

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The present invention relates to ore detection technique field, and in particular to a kind of detection method that copper mine and copper-contained material are detected based on infra-red sepectrometry, comprises the following steps:S1. the testing sample of 0.5 ~ 1 parts by weight and the potassium bromide powder of 140 ~ 460 parts by weight are taken, is ground to sample particle less than 2.5 μm, and be well mixed;S2. mixed testing sample is subjected to compressing tablet process, is then placed in infrared spectrometer and is detected, obtain spectrogram;S3. spectrogram is subjected to baseline correction, smooth, mark peak analysis, then sample spectrogram is retrieved in spectrum library and binding compounds characteristic absorption peak primarily determines that main compound in sample.The present invention provides a kind of detection method of copper mine and copper-contained material, and import copper mine and copper-contained material are identified using an equipment, especially belong to the elementary step in mineral products field, infrared identification technology is applied in available metallurgical slag.

Description

A kind of detection method that copper mine and copper-contained material are detected based on infra-red sepectrometry
Technical field
The present invention relates to ore detection technique field, and in particular to one kind is based on infra-red sepectrometry detection copper mine and copper-containing substance The detection method of material.
Background technology
In recent years, with the implementation of the Belt and Road, it is continuously increased from mineral products species, the quantity of the import of Xinjiang port, Often with " copper matte regulus ", (the co-melting body of the sulfide of nonferrous heavy metal sulfide and iron is referred to as molten the Control Measure at Alataw Port of western bridgehead Sulfonium, it is the important intermediate of the sulfide concentrate pyrometallurgical smelting of the metals such as copper, nickel.The sulfonium obtained during Copper making is referred to as copper Sulfonium, practise and claim matte) the primary of copper of state of nominal import Kazakhstan production smelt or rough machined clinker mineral or smelting Slag, copper content is higher the characteristics of the commodity, reaches the raw material of Copper making, thus some Imported business melting waste slag with the trade name Claim declaration for import, or even the situation for thering is false to conceal the name of an article, to reach the purpose for the tariff that speeds passage through customs, reduces.Through preliminary search, The inspection on such " copper-contained material ", authentication method standard, pertinent literature report be not less yet both at home and abroad.Sci-tech novelty-search report Accuse retrieval conclusion:The country seen " X fluorescence spectrometer " measure " Chinese mugwort Sa Bingtong " and " sintering deposit " in Partial Elements document report, Have no any Research Literature report that copper-contained material is identified it using large scale equipment.
Because import can be had differences using copper-contained material with general Copper Ores or copper concentrate, at the same with general mineral products Melting waste slag is different, only can not differentiate, distinguish from the height of each essential element content, therefore, import be studied and defined at port The quick inspection of mineral products, authentication method, its main component is quickly determined, and find out it should to belong to classification extremely urgent, it is necessary When special picture library is established for copper-contained material, identification to approximate material from now on provides foundation.
Had determined that in addition, the quantitative analysis method of existing copper-contained material and copper concentrate can only be directed in the commodity of the name of an article Each element carries out content analysis.For the authentication method application X fluorescence spectrometer and X-ray diffractometer two of copper mine and copper-contained material Kind equipment is used in conjunction and could differentiated, part Experiment room cannot carry out appraisal when only having a wherein equipment.
Import copper mine and copper-contained material are identified merely with an equipment therefore, the present invention provides one kind, extension is red External spectrum instrument identification field application, especially belong to the elementary step in mineral products field.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide one kind based on infra-red sepectrometry detection copper mine and to contain The detection method of copper material, import copper mine and copper-contained material are identified using an equipment, especially belonged in mineral products field In the elementary step, infrared identification technology is set to be applied in available metallurgical slag.
The purpose of the present invention is achieved through the following technical solutions:
A kind of detection method that copper mine and copper-contained material are detected based on infra-red sepectrometry, is comprised the following steps:
S1. the testing sample of 0.5~1 parts by weight and the potassium bromide powder of 140~460 parts by weight are taken, is ground to sample Grain is less than 2.5 μm, and is well mixed;
S2. mixed testing sample is subjected to compressing tablet process, is then placed in infrared spectrometer and is detected, composed Figure;The testing conditions of the infrared spectrometer are part:Using blank kbr tablet as background, number of sample scan 32, resolution ratio For 4.00cm, laser frequency 15798cm-1, detector is DTGS KBr, and index glass speed is 0.6329, diaphragm 100.00, detection Scope 4000cm-1~400cm-1
S3. spectrogram is subjected to baseline correction, smooth, mark peak analysis, then sample spectrogram is retrieved and tied in spectrum library Polymerisable compounds characteristic absorption peak primarily determines that main compound in sample.
Further, in the step S1, using ten a ten thousandth balances weigh 0.5~1mg testing sample and 140~ 460mg potassium bromide powder is ground.Because sample size is very few spectral absorbance can be caused too low;Sample size excessively occurs Some bands of a spectrum hypersorptions;Bromination potassium application rate is very few, and the piece pressed out is frangible;Bromination potassium application rate is excessive, can cause the piece pressed out It is opaque;Therefore it is preferred that using 1mg testing sample and 150mg potassium bromide powder, when testing sample is highly polar group, adopt With 0.5mg testing sample and 150mg potassium bromide powder.
Further, in the step S1, sample was ground to 200~300 mesh sieves.Due in detection process, when When particle is more than optical wavelength, it may occur that scattering, mixture grinding it is not thin enough, easily there is light and dissipated in high-end in middle infrared spectrum Phenomenon is penetrated, raises spectrum high band baseline, therefore it is preferred that used the testing sample mixture of 200~300 mesh sieves.
Further, in the step S2, the tabletting is that testing sample is pushed into 50~70s in 7.5~8.5t pressure, Extrude transparent or semitransparent ingot piece.
Further, the detailed process of the tabletting is:With the small flat chisel of stainless steel by ground testing sample mixture It is transferred completely into compression mold, and is paved mixture with small flat chisel, can be also paved into middle slightly higher mound shape and so use finger The face rotary tablet compression mould of strength one depression bar, on the one hand slightly downward pressure make mixture smooth, then in 7.5~8.5t Pressure pushes 50~70s, extrudes transparent or semitransparent ingot piece.During actually detected, the pressure of application is higher, extrudes The ingot sector-meeting come is more transparent, but applies hypertonia, is easily damaged compression mold and tablet press machine;Compression mold is from tablet press machine On take off after, it should the ingot piece pressed is rushed out on tablet press machine with the subsidiary opening cylinder of compression mold, so gone out The ingot piece come is not easy fragmentation;The piece pressed should be put into infrared spectrometer and detect as early as possible, otherwise the water in ingot piece absorption air The absworption peak of water can be introduced, particularly the weak sample of some absorbances, the sample spectrogram influence of the absworption peak of water is very big;Such as can not The piece pressed is put into drier by detection in time preserves.
The beneficial effects of the invention are as follows:It is provided by the invention a kind of copper mine and copper-contained material to be detected based on infra-red sepectrometry Detection method, by analyzing the expert's conclusion of copper-contained material application infra-red sepectrometry, the existence form of each element exists in raw ore More single in infrared spectrum, the compound substantially without complexity is present;But the copper-contained material after smelting, the presence shape of each element Formula is more complicated, diversified, and the normal pictures after being scanned by infrared spectrometer with spectrum library compare, and each element is with different shapes Formula is present in copper-contained material, and suitable for inspection and quarantine, customs and research institutions are to copper mine and the thick refining of copper or clinker mineral Discriminatory analysis.
Brief description of the drawings
Fig. 1 is test example copper mine mark thing GBW07169 of the present invention detection spectrogram;
Fig. 2 is test example copper mine mark thing ZBK335 of the present invention detection spectrogram;
Fig. 3 is test example copper mine mark thing ZBK336 of the present invention detection spectrogram;
Fig. 4 is test example copper mine 7# of the present invention detection spectrogram;
Fig. 5 is test example copper mine 6# of the present invention detection spectrogram;
Fig. 6 is test example copper mine 10# of the present invention detection spectrogram;
Fig. 7 is test example copper-contained material 1# of the present invention detection spectrogram;
Fig. 8 is test example copper-contained material 0-2# of the present invention detection spectrogram;
Fig. 9 is test example copper-contained material 2518# of the present invention detection spectrogram.
Embodiment
Technical scheme, but the protection of the present invention are described in further detail with reference to specific embodiments and the drawings Scope is not limited to as described below.
Embodiment
A kind of detection method that copper mine and copper-contained material are detected based on infra-red sepectrometry, is comprised the following steps:
S1. the testing sample of 0.5~1 parts by weight and the potassium bromide powder of 140~460 parts by weight are taken, is ground to sample Grain is less than 2.5 μm, and is well mixed;
S2. mixed testing sample is subjected to compressing tablet process, is then placed in infrared spectrometer and is detected, composed Figure;The testing conditions of the infrared spectrometer are part:Using blank kbr tablet as background, number of sample scan 32, resolution ratio For 4.00cm, laser frequency 15798cm-1, detector is DTGS KBr, and index glass speed is 0.6329, diaphragm 100.00, detection Scope 4000cm-1~400cm-1
S3. spectrogram is subjected to baseline correction, smooth, mark peak analysis, then sample spectrogram is retrieved and tied in spectrum library Polymerisable compounds characteristic absorption peak primarily determines that main compound in sample.
In a preferred embodiment, in the step S1, the to be measured of 0.5~1mg is weighed using ten a ten thousandth balances The potassium bromide powder of sample and 140~460mg is ground.Because sample size is very few spectral absorbance can be caused too low;Sample Some bands of a spectrum hypersorptions excessively occur in amount;Bromination potassium application rate is very few, and the piece pressed out is frangible;Bromination potassium application rate is excessive, can make It is opaque into the piece pressed out;Therefore it is preferred that using 1mg testing sample and 150mg potassium bromide powder, it is strong in testing sample During polarity group, using 0.5mg testing sample and 150mg potassium bromide powder.
In a preferred embodiment, in the step S1, sample was ground to 200~300 mesh sieves.Due to detecting During, when particle is more than optical wavelength, it may occur that scattering, mixture is ground not thin enough, in the high-end appearance of middle infrared spectrum Easily there is light scattering phenomenon, raise spectrum high band baseline, therefore it is preferred that used the testing sample of 200~300 mesh sieves to mix Thing.
In a preferred embodiment, in the step S2, the tabletting be by testing sample under 7.5~8.5t pressure 50~70s is pressed, extrudes transparent or semitransparent ingot piece.
In a preferred embodiment, the detailed process of the tabletting is:Will be ground to be measured with the small flat chisel of stainless steel Sample mixture is transferred completely into compression mold, and is paved mixture with small flat chisel, can also be paved into middle slightly higher mound Shape so uses the depression bar of the face rotary tablet compression mould of strength one of finger, and on the one hand slightly downward pressure makes mixture smooth, then 50~70s is pushed in 7.5~8.5t pressure, extrudes transparent or semitransparent ingot piece.During actually detected, the pressure of application Higher, the ingot sector-meeting pressed out is more transparent, but applies hypertonia, is easily damaged compression mold and tablet press machine;Tabletting After mould is taken off from tablet press machine, it should gone out the ingot piece pressed on tablet press machine with the subsidiary opening cylinder of compression mold Come, the ingot piece so rushed out is not easy fragmentation;The piece pressed should be put into infrared spectrometer and detect as early as possible, and otherwise ingot piece absorbs Water in air can introduce the absworption peak of water, particularly the weak sample of some absorbances, and the sample spectrogram of the absworption peak of water influences It is very big;The piece that will be pressed can not be such as detected in time be put into drier preserve.
Test example
Copper mine standard substance, copper mine sample and copper-contained material application infra-red sepectrometry are examined using above-mentioned detection method Survey, its infrared figure such as Fig. 5-22, testing result such as table one:
The infra-red sepectrometry testing result summary sheet of table one
Analyzed by above-mentioned qualification result, the form of copper is mainly contained by infrared spectrometer copper mine and copper mine mark thing Exist in the form of chrysocolla, beaverite, faustite, zinc-copper vanadium, cyanotrichite, phosphor-copper copper mine, cupric oxide etc., part copper contains Measure relatively low can not determine its existence form in infrared spectrometer.Copper is primarily present form alkali formula carbon in copper-contained material Arsenate in sour copper, intermediate portions sample be present, arsenate mainly produces in the process such as melting waste slag, dyestuff waste liquid , the arsenic element existence form of arsenate is substantially not present in natural minerals.
Described above is only the preferred embodiment of the present invention, it should be understood that the present invention is not limited to described herein Form, the exclusion to other embodiment is not to be taken as, and can be used for various other combinations, modification and environment, and can be at this In the text contemplated scope, it is modified by the technology or knowledge of above-mentioned teaching or association area.And those skilled in the art are entered Capable change and change does not depart from the spirit and scope of the present invention, then all should be in the protection domain of appended claims of the present invention It is interior.

Claims (5)

1. a kind of detection method that copper mine and copper-contained material are detected based on infra-red sepectrometry, it is characterised in that comprise the following steps:
S1. the testing sample of 0.5 ~ 1 parts by weight and the potassium bromide powder of 140 ~ 460 parts by weight are taken, sample particle is ground to and is less than 2.5 μm, and be well mixed;
S2. mixed testing sample is subjected to compressing tablet process, is then placed in infrared spectrometer and is detected, obtain spectrogram; The testing conditions of the infrared spectrometer are part:Using blank kbr tablet as background, number of sample scan 32, resolution ratio is 4.00cm, laser frequency 15798cm-1, detector is DTGS KBr, and index glass speed is 0.6329, diaphragm 100.00, detects model Enclose 4000cm-1~400cm-1
S3. spectrogram is subjected to baseline correction, smooth, mark peak analysis, then retrieved in spectrum library sample spectrogram and combinationization Compound characteristic absorption peak primarily determines that main compound in sample.
2. a kind of detection method that copper mine and copper-contained material are detected based on infra-red sepectrometry according to claim 1, it is special Sign is, in the step S1,0.5 ~ 1mg testing sample and 140 ~ 460mg bromination are weighed using ten a ten thousandth balances Potassium powder is ground.
3. a kind of detection method that copper mine and copper-contained material are detected based on infra-red sepectrometry according to claim 1, it is special Sign is, in the step S1, sample was ground into 200 ~ 300 mesh sieves.
4. a kind of detection method that copper mine and copper-contained material are detected based on infra-red sepectrometry according to claim 1, it is special Sign is, in the step S2, the tabletting is that testing sample pushed into 50 ~ 70s in 7.5 ~ 8.5t pressure, extrudes transparent or half Transparent ingot piece.
5. a kind of detection method that copper mine and copper-contained material are detected based on infra-red sepectrometry according to claim 4, it is special Sign is that the detailed process of the tabletting is:Ground testing sample mixture is transferred completely into the small flat chisel of stainless steel In compression mold, and mixture is paved with small flat chisel, can also be paved into middle slightly higher mound shape so with the strength one side of finger The depression bar of rotary tablet compression mould, on the one hand slightly downward pressure make mixture smooth, then push 50 in 7.5 ~ 8.5t pressure ~ 70s, extrude transparent or semitransparent ingot piece.
CN201710930117.3A 2017-10-09 2017-10-09 A kind of detection method that copper mine and copper-contained material are detected based on infra-red sepectrometry Pending CN107462543A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN110779943A (en) * 2019-10-23 2020-02-11 长春黄金研究院有限公司 Identification method for dyeing natural turquoise

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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
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Publication number Priority date Publication date Assignee Title
CN110779943A (en) * 2019-10-23 2020-02-11 长春黄金研究院有限公司 Identification method for dyeing natural turquoise

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