CN107631918A - A kind of black powder and the like pre-treating method - Google Patents
A kind of black powder and the like pre-treating method Download PDFInfo
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- CN107631918A CN107631918A CN201710651074.5A CN201710651074A CN107631918A CN 107631918 A CN107631918 A CN 107631918A CN 201710651074 A CN201710651074 A CN 201710651074A CN 107631918 A CN107631918 A CN 107631918A
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Abstract
The invention discloses a kind of pre-treating method of black powder and the like, this method is to handle described black powder and the like using treatment fluid, obtain sample liquid, the sample liquid is detected for laser activated spectroscopic, the component detection case of black powder and the like is obtained by the detection of sample liquid, wherein, the occupation mode of sample liquid includes directly using, concentrate use or being added dropwise to after test piece removes solvent using.The problem of this method can not only overcome black powder and the like inflammable, and it can greatly strengthen the laser activated spectroscopic signal of black powder, to realize that the safely and fast detection of black powder provides possibility, and detected components are wide, and danger investigation and appraisal are provided convenience.
Description
Technical field
The present invention relates to spectral detection pre-treating method, more particularly to a kind of pre-treatment side of black powder and the like
Method.
Background technology
At present, the detection that laser activated spectroscopic technology is used for dark matter is always problem in industry, in particular for depth
The detection of color combustible material.The main reason for causing the technical barrier be：When laser irradiates dark matter, it is easier to absorb heat, and
Heat is not easy to shed in time and easily cause heat accumulation after heat absorption, especially as this kind of dark combustible material of black powder, uses laser
When excitation spectrum technology is directly tested, there is the danger of burning or even blast.
On the other hand, black powder and the like is more material mixing samples, and most of material is black combustible material,
Only a small amount of composition has LR laser raman, Laser induced plasma signal, and signal is weaker, is unsuitable for laser activated spectroscopic skill
Art is directly tested, and therefore, in order to meet the quick detection to black powder and the like, it is carried out using suitable means pre-
Processing, it is necessary to reuse corresponding equipment and carry out detection.
Such as in " application of the Raman spectroscopy in explosive detection " text, drawn for 12 kinds of explosives of main flow
Graceful spectral detection, remaining 11 kinds of explosive smoothly completes detection in addition to black powder, and draws corresponding collection of illustrative plates, and black powder is using
50mW, 150mW laser power fail to detect Raman collection of illustrative plates, are burnt in the detection process using 300mW laser powers.
Therefore, the problem of laser activated spectroscopic technology cannot be directly used to black powder test in the prior art is urgently to be resolved hurrily.
The content of the invention
Present invention seek to address that problem as described above.It is an object of the invention to provide one kind to be applied to black powder and its class
Like the detection pre-treating method of thing, the problem of pre-treating method can not only overcome black powder inflammable, and can isolate and have
The material of laser activated spectroscopic scattering properties, or even the laser activated spectroscopic signal of enhancing black powder, to realize the peace of black powder
Full quick detection provides may.
The invention provides a kind of pre-treating method of black powder and the like, this method is using treatment fluid processing institute
Black powder and the like is stated, obtains sample liquid, the sample liquid is detected for laser activated spectroscopic, the sample liquid makes
Include directly using, concentrate use or being added dropwise to after test piece removes solvent using with mode；Wherein, sample liquid process is made
Comprise the steps：
Blend step：Described black powder and the like is fully dissolved using treatment fluid, mixed liquor is made；
Slug removing step：The sediment in mixed liquor is removed, obtains sample liquid；
Wherein, treatment fluid includes dispersion liquid and reinforcing agent in blend step, the quality percentage of reinforcing agent in the treatment fluid
Than for 0~10%, the dispersion liquid is the polar solvent for including water.
Wherein, the reinforcing agent is ring-type ethers compound or its mixture.
Wherein, the treatment fluid also includes acidifying solution, and the acidifying solution is in hydrochloric acid solution, sulfuric acid solution and salpeter solution
One or more, the mass percent of acidifying solution described in the treatment fluid be 0~10%.
Wherein, the treatment fluid also includes acidifying solution, the acidifying solution be selected from the hydrochloric acid solution that volumetric concentration is 2~5%,
The salpeter solution that the sulfuric acid solution or volumetric concentration that volumetric concentration is 8~12% are 4~9%.
Wherein, the acidifying solution is selected from：Volumetric concentration is 2~5% hydrochloric acid solution, and addition is 4~6%；Or body
The sulfuric acid solution that product concentration is 8~12%, addition are 1~4%；Or the salpeter solution that volumetric concentration is 4~9%, add
Measure as 4~6%.
Wherein, the dispersion liquid also includes the one or more in methanol, ethanol, acetonitrile and acetone.
Wherein, the dispersion liquid is selected from water, volume ratio 1:0.1~0.5 water/alcohol mixed solution or volume ratio is 1:
0.2~0.8 water/acetone mixed solution.
Wherein, the reinforcing agent is the one or more in crown ether and crown ether derivative.
Wherein, the crown ether and crown ether derivative include 12-crown-4 and its derivative, 15- crown-s 5 and its derivative, 18-
Crown- 6 and its derivative, 21- crown-s 7 and its derivative, 24- crown-s 8 and its derivative, 30- crown-s 10 and its derivative.
Wherein, the reinforcing agent is Contrast agent A and Contrast agent B mixture, and the Contrast agent A is preced with selected from 18-
Ether -6 or derivatives thereof；The Contrast agent B is selected from 15- crown ethers -5 or derivatives thereof.
Wherein, the blend step includes one or more methods among stirring, concussion, ultrasound, heating, the slagging-off
Step includes filtering or centrifugal method.
Wherein, Contrast agent A isWherein, R1、R2、R3And R4For H or electron donating group, example
Such as-OH ,-NH2Deng R1With R2And R3With R4Cyclization can also exist jointly, such as Contrast agent A is phendioxin 8- crown-s 6.
Wherein, Contrast agent B isWherein, R1、R2、R3And R4For H or electron donating group, example
Such as-OH ,-NH2Deng R1With R2And R3With R4Cyclization can also exist jointly, such as Contrast agent B is Benzo15crown5 derivatives.
Wherein, Contrast agent A and Contrast agent B quality is than 1~4:1.
Wherein, the pre-treating method also includes preparing treatment fluid, and comprising the following steps that for the pre-treating method is shown：
Treatment fluid is prepared, the treatment fluid includes dispersion liquid, acidifying solution and reinforcing agent, and wherein dispersion liquid is water, water/ethanol
Mixed liquor or water/acetone mixture；Add acidifying solution to be acidified, the acidifying solution is hydrochloric acid solution, sulfuric acid solution or nitre
Acid solution；Reinforcing agent is eventually adding, the reinforcing agent is the one or more in crown ether and crown ether derivative；
Sample liquid is made, handles described black powder and the like using treatment fluid, obtains sample liquid；
Using sample liquid, the sample liquid is detected for laser activated spectroscopic, the occupation mode of the sample liquid includes
Directly use, concentration is used or is added dropwise to after test piece removes solvent and used.
Wherein, it is described to prepare in treatment fluid step, the crown ether and crown ether derivative include 12-crown-4 and its derivative,
15- crown-s 5 and its derivative, 18- crown-s 6 and its derivative, 21- crown-s 7 and its derivative, 24- crown-s 8 and its derivative, 30-
Crown- 10 and its derivative, the addition of the reinforcing agent is 0.001~8%.
Wherein, the test piece includes slide, sheet glass, test paper, sheet metal or plastic sheet.
Wherein, it is described remove solvent method include forced air drying, vacuum drying, freeze, heat drying, natural air drying,
Hot blast drying or cold wind drying.
Wherein, the black powder analog refers to that color to black, is easily lighted by laser in dry conditions in dark,
It is unsuitable for a kind of material of laser activated spectroscopic detection, including ignition charge, whip gunpowder, soaring gunpowder, thunder gunpowder, ignition charge.
Wherein, the laser activated spectroscopic detection includes laser excitation Raman detection or Laser induced plasma detection.
The detected components of black powder and the like include the nitrate such as potassium nitrate, ammonium nitrate, sodium nitrate in the present invention, high
One kind or more in the chlorates such as the perchlorate such as potassium chlorate, sodium perchlorate, ammonium perchlorate, potassium chlorate, sodium chlorate, ammonium chlorate
Kind.
The invention provides a kind of pre-treating method of black powder and the like, the design philosophy of the pre-treating method is
Black powder and the like is mixed with the processing solution that specialty is prepared, the processing solution can have in dissolving mixt
The material composition of laser activated spectroscopic characteristics of signals, then by the way of filtering or centrifugation, sample liquid is further obtained, should
Sample liquid is transparent or semitransparent solution, then obtains the component detection case of black powder and the like by detecting sample liquid.
Processing procedure of the present invention is used in combination with processing solution, can effectively extract the detection of black powder and the like
Component, it is easy to the quick detection of laser activated spectroscopic.Wherein, the composition of processing solution and preparation are the emphasis of the present invention, at this
Reason solution possesses the effects such as dissolving, extraction and enhancing.
Specifically, the processing solution includes dispersion liquid and reinforcing agent, in treatment fluid the mass percent of reinforcing agent for 0~
10%, the dispersion liquid is the polar solvent for including water.Polar solvent of the present invention refers to that solution has asymmetric molecular structure
Solution, the aqueous solution that the dispersion liquid can be the aqueous solution or solute is polar molecule.When dispersion liquid is the water containing polar molecule
During solution, it is preferable that the aqueous solution of the dispersion liquid also includes the one or more in methanol, ethanol, acetonitrile and acetone.It is scattered
The main function of liquid is scattered acidifying solution and reinforcing agent, and dissolves the detected components of extraction black powder and the like.
It is appreciated that when reinforcing agent addition is zero, the dispersion liquid can realize the dissolving and extraction of detected components,
Possesses basic pre-treatment effect.It is highly preferred that the dispersion liquid is selected from water, volume ratio 1:0.1~0.5 water/ethanol mixes
It is 1 to close solution or volume ratio:0.2~0.8 water/acetone mixed solution, above-mentioned three kinds of dispersion liquids possess splendid pre-treatment effect
Fruit.
As the innovative point of the present invention, treatment fluid of the present invention includes reinforcing agent, and the reinforcing agent is ring-type ethers chemical combination
Thing or its mixture.The main function of reinforcing agent strengthens the laser activated spectroscopic signal of detected components in sample liquid, real
Now more preferably pre-treatment effect.
Ring-type ethers compound finger ring ether of the present invention and the cyclic ether derivative containing substituent.Preferably, the reinforcing agent
For the one or more in crown ether and crown ether derivative；Wherein, crown ether refers to contain multiple-OCH in molecule2CH2- construction unit
Macrocyclic polyether.Preferably, the crown ether and crown ether derivative include 12-crown-4 and its derivative, 15- crown-s 5 and its derived
Thing, 18- crown-s 6 and its derivative, 21- crown-s 7 and its derivative, 24- crown-s 8 and its derivative, 30- crown-s 10 and its derivative.
The present invention has carried out numerous studies for dispersion liquid system, and the mass percent of reinforcing agent is in treatment fluid of the present invention
0~10%, preferably 0.001~8%, more preferably 0.01~5%, possesses preferably enhancing effect.
Preferably, the reinforcing agent is Contrast agent A and Contrast agent B mixture, the Contrast agent A and the increasing
Strong reagent B is different crown ether or crown ether derivative.In few examples of the present invention, most preferably, the Contrast agent A is selected from
18- crown ethers -6 or derivatives thereof, the Contrast agent B are selected from 15- crown ethers -5 or derivatives thereof.It is highly preferred that Contrast agent A with
Contrast agent B quality is than 1~4:1, the beneficial effect of reinforcing agent is more preferably.
Treatment fluid of the present invention also includes acidifying solution, and the main function of acidifying solution is dispersion liquid and reinforcing agent phase with the present invention
Coordinate, strengthen dissolving, extraction and the signal enhancing effect for the treatment of fluid, realize more preferably pre-treatment effect, while improve reinforcing agent
Stability in treatment fluid.The acidifying solution includes the one or more in hydrochloric acid solution, sulfuric acid solution and salpeter solution, processing
The mass percent of acidifying solution described in liquid is 0~10%.
Preferably, the sulfuric acid that the hydrochloric acid solution, volumetric concentration that acidifying solution is selected from that volumetric concentration is 2~5% are 8~12% is molten
Liquid or the salpeter solution that volumetric concentration is 4~9%.It is highly preferred that the acidifying solution is selected from：Volumetric concentration is 2~5% hydrochloric acid
Solution, addition are 4~6%；Or the sulfuric acid solution that volumetric concentration is 8~12%, addition are 1~4%；Or volume is dense
The salpeter solution for 4~9% is spent, addition is 4~6%.
Most preferably, the acidifying solution is selected from：Volumetric concentration be 3.6% hydrochloric acid solution, addition 5%；Or body
The sulfuric acid solution that product concentration is 10%, addition 2%；Or the salpeter solution that volumetric concentration is 6.7%, addition 5%.
Proved through lot of experiments and application data, treatment fluid provided by the invention, for example, reinforcing agent is ring-type ethers chemical combination
Thing, acidifying solution include hydrochloric acid solution, sulfuric acid solution and salpeter solution in one or more, dispersion liquid be include water polarity it is molten
Liquid, and treatment fluid pre-treatment effect made from preferable composition, preferred content are good, and laser activated spectroscopic technology can be easy to be directed to
Safe, the quick test of black powder and the like.
As the innovative point of the present invention, the pre-treating method includes the preparation process of processing, the pre-treatment side
Method comprises the steps：
Treatment fluid is prepared, situation is matched according to treatment fluid, acidifying solution and reinforcing agent are sequentially added in dispersion liquid；Use place
Manage liquid and handle described black powder and the like, obtain sample liquid；The sample liquid is detected for laser activated spectroscopic, it is described
The occupation mode of sample liquid includes directly using, concentrate use or being added dropwise to after test piece removes solvent using.
The processing procedure for the treatment of fluid and black powder and the like, which includes all, in the present invention can mix sample, dissolve
Method, such as stirring, concussion, ultrasound, heating and its method being combined etc..
Sample liquid can directly or will after solvent concentration be used for laser activated spectroscopic detect, sample drop can be also added in
Test piece, which is removed after solvent obtains solid crystal, is used for laser activated spectroscopic detection.Testing piece includes slide, sheet glass, examination
Paper, sheet metal or plastic sheet etc. can be used for the carrier of the removal process such as solvent volatilization, but not limited to this；Remove the method bag of solvent
The methods of including forced air drying, vacuum drying, lyophilized, heat drying, natural air drying, hot blast drying or cold wind drying, but be not limited to
This.
As the preferred exemplary of the present invention, the pre-treating method comprises the steps：
Treatment fluid is prepared, the treatment fluid includes dispersion liquid, acidifying solution and reinforcing agent, and wherein dispersion liquid is water, water/ethanol
Mixed liquor or water/acetone mixture；Add acidifying solution to be acidified, the acidifying solution is hydrochloric acid solution, sulfuric acid solution or nitre
Acid solution；Reinforcing agent is eventually adding, the reinforcing agent is the one or more in crown ether and crown ether derivative；
Sample liquid is made, handles described black powder and the like using treatment fluid, obtains sample liquid；
Using sample liquid, the sample liquid is detected for laser activated spectroscopic, the occupation mode of the sample liquid includes
Directly use, concentration is used or is added dropwise to after test piece removes solvent and used.
As another preferred exemplary of the present invention, the pre-treating method comprises the steps：
Treatment fluid is prepared, the treatment fluid includes dispersion liquid, acidifying solution and reinforcing agent, and wherein dispersion liquid is selected from water, volume
Than for 1:0.1~0.5 water/alcohol mixed solution or volume ratio is 1:0.2~0.8 water/acetone mixed solution；Add acid
Change liquid to be acidified, the acidifying solution is selected from：Volumetric concentration is 2~5% hydrochloric acid solution, and addition is 4~6%；Or body
The sulfuric acid solution that product concentration is 8~12%, addition are 1~4%；Or the salpeter solution that volumetric concentration is 4~9%, add
Measure as 4~6%；It is eventually adding reinforcing agent, the reinforcing agent is the one or more in crown ether and crown ether derivative, the enhancing
The addition of agent is 0~5%；
Sample liquid is made, handles described black powder and the like using treatment fluid, obtains sample liquid；
Using sample liquid, the sample liquid is detected for laser activated spectroscopic, the occupation mode of the sample liquid includes
Directly use, concentration is used or is added dropwise to after test piece removes solvent and used.
The present invention is the laser activated spectroscopic detection pre-treating method for black powder and the like.
The present invention is pre-processed for black powder and the like, overcomes that such material is inflammable and signal is weak asks
Topic, there is significant progress, compared with prior art, have the following advantages：
First, the problem of this method can not only overcome black powder inflammable, and also the laser that can greatly strengthen black powder swashs
Luminous spectrum signal, to realize that the safely and fast detection of black powder provides possibility.
Second, this method detected components include potassium nitrate, ammonium nitrate, sodium nitrate, potassium hyperchlorate, potassium chlorate, ammonium perchlorate,
One or more in potassium chlorate, sodium perchlorate, ammonium chlorate, laser activated spectroscopic technology is greatly broadened in black powder and its class
Like the application on analyte detection, danger investigation and appraisal are provided convenience.
The following description for embodiment is read with reference to the drawings, other property features of the invention and advantage will become clear
It is clear.
Brief description of the drawings
It is incorporated into specification and the accompanying drawing of a part for constitution instruction shows embodiments of the invention, and with
Description is used for the principle for explaining the present invention together, and in the drawings, similar reference is used to represent similar key element, under
Accompanying drawing in the description of face is some embodiments of the present invention, rather than whole embodiments, is come for those of ordinary skill in the art
Say, on the premise of not paying creative work, other accompanying drawings can be obtained according to these accompanying drawings.
Fig. 1 shows the pre-treating method flow chart according to a kind of black powder of the present invention and the like.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is
Part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art
The every other embodiment obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.Need
Illustrate, in the case where not conflicting, the feature in embodiment and embodiment in the application can be mutually combined.
The embodiment of the present invention 1~8 is divided into eight parts of surveys by taking the pretreatment process of black powder as an example, by 8g black powder sample
Sample, it is experimental group 1~8 to number respectively, every part of 1g.
Embodiment 1
The black powder that numbering is experimental group 1 is handled using treatment fluid, treatment fluid is the 20g aqueous solution, and black powder is added
In the beaker for filling treatment fluid, after 50 DEG C of heating stirring 2min, fully dissolving, sediment is filtered to remove while hot, obtains sample liquid 1
It is standby.
Embodiment 2
Treatment fluid is prepared, the hydrochloric acid solution that 1g concentration is 2% is added in dispersion liquid 19g water, dispersion liquid is acidified,
It is eventually adding 0.002g crown ether 18- crown-s 6；The treatment fluid processing numbering completed using preparing is the black powder of experimental group 2, will
Black powder is added in the beaker for filling treatment fluid, stirring concussion 5min, fully after dissolving, sediment is removed after centrifugation, obtains sample
Product liquid 2 is standby.
Embodiment 3~8
The preparation process of the reference implementation example 1,2 of 3~embodiment of embodiment 8, it is standby that corresponding sample liquid 1~8 is made.Its
In, treatment fluid removes with stirring in black powder mixed process, can be selected, shake, one or more methods among ultrasonic, heating
Filtering or centrifugal method can be selected in slag process, and those skilled in the art can select to use according to actual conditions.Usually, ultrasonic,
Heat effect can accelerate dissolution.
The treatment fluid quality that embodiment 1~8 uses is 20g, but the component of each treatment fluid and content are varied from, specifically
Embodiment situation is as shown in table 1：
Treatment fluid component and its content list in 1 different embodiments of table
It should be noted that the numerical value in the bracket of table 1 is mass percentage content corresponding to the component.
Above-mentioned sample liquid 1~8 is detected for Raman spectrum, in addition to the noise of sample liquid 1 is larger, sample liquid 2~8 can be entered
Row directly detects, and raman spectral signal is strong, can realize accurate detection, has beneficial technique effect；Sample liquid 1 is carried out dense
Detected after contracting, accurate detection can be achieved.Also, when reinforcing agent is the mixing composition of two kinds of different crown ethers or derivatives thereof, inspection
Survey best results.
The whole pretreatment process of embodiment 1~8 takes 5~10min, from above-described embodiment it will be seen that this hair
The pre-treating method of bright offer can not only quickly handle black powder and the like, and also overcome such material it is inflammable and
The problem of signal is weak, there is significant progress, compared with prior art, have the following advantages：
First, the problem of this method can not only overcome black powder inflammable, and also the laser that can greatly strengthen black powder swashs
Luminous spectrum signal, to realize that the safely and fast detection of black powder provides possibility.
Second, this method detected components include potassium nitrate, ammonium nitrate, sodium nitrate, potassium hyperchlorate, potassium chlorate, ammonium perchlorate,
One or more in sodium chlorate, sodium perchlorate, ammonium chlorate, laser activated spectroscopic technology is greatly broadened in black powder and its class
Like the application on analyte detection, danger investigation and appraisal are provided convenience.
Descriptions above can combine implementation individually or in a variety of ways, and these variants all exist
Within protection scope of the present invention.
Finally it should be noted that：Herein, term " comprising ", "comprising" or its any other variant are intended to non-
It is exclusive to include, so that process, method, article or equipment comprising a series of elements not only include those key elements,
But also the other element including being not expressly set out, or also include solid by this process, method, article or equipment
Some key elements.In the absence of more restrictions, the key element limited by sentence " including one ... ", it is not excluded that including institute
State in process, method, article or the equipment of key element and other identical element also be present.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations.Although with reference to the foregoing embodiments
The present invention is described in detail, it will be understood by those within the art that：It still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent substitution to which part technical characteristic；And these modification or
Replace, the essence of appropriate technical solution is departed from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (10)
- A kind of 1. pre-treating method of black powder and the like, it is characterised in that using treatment fluid handle the black powder and Its analog, obtains sample liquid；The sample liquid is detected for laser activated spectroscopic, the occupation mode of the sample liquid includes Directly use, concentration is used or is added dropwise to after test piece removes solvent and used；Wherein, sample liquid process is made includes following steps Suddenly：Blend step：Described black powder and the like is fully dissolved using treatment fluid, mixed liquor is made；Slug removing step：The sediment in mixed liquor is removed, obtains sample liquid；Wherein, treatment fluid includes dispersion liquid and reinforcing agent in blend step, and the mass percent of reinforcing agent is 0 in the treatment fluid ~10%, the dispersion liquid is the polar solvent for including water.
- 2. the pre-treating method of black powder as claimed in claim 1 and the like, it is characterised in that the reinforcing agent is ring Shape ether compound or its mixture.
- 3. the pre-treating method of black powder as claimed in claim 1 or 2 and the like, it is characterised in that the treatment fluid is also Including acidifying solution, the acidifying solution is the one or more in hydrochloric acid solution, sulfuric acid solution and salpeter solution, in the treatment fluid The mass percent of the acidifying solution is 0~10%.
- 4. black powder as claimed in claim 1 or 2 and the like pre-treating method, it is characterised in that the treatment fluid is also Including acidifying solution, the acidifying solution is selected from：Volumetric concentration is 2~5% hydrochloric acid solution, and addition is 4~6%；Or volume Concentration is 8~12% sulfuric acid solution, and addition is 1~4%；Or the salpeter solution that volumetric concentration is 4~9%, addition For 4~6%.
- 5. the pre-treating method of black powder as claimed in claim 3 and the like, it is characterised in that the dispersion liquid also wraps Include the one or more in methanol, ethanol, acetonitrile and acetone.
- 6. black powder as claimed in claim 1 and the like pre-treating method, it is characterised in that the dispersion liquid is selected from Water, volume ratio 1:0.1~0.5 water/alcohol mixed solution or volume ratio is 1:0.2~0.8 water/acetone mixed solution.
- 7. black powder as claimed in claim 1 and the like pre-treating method, it is characterised in that the reinforcing agent is enhancing The mixture of reagent A and Contrast agent B, the Contrast agent A are selected from 18- crown ethers -6 or derivatives thereof；The Contrast agent B choosings From 15- crown ethers -5 or derivatives thereof.
- 8. black powder as claimed in claim 1 and the like pre-treating method, it is characterised in that the blend step includes One or more methods among stirring, concussion, ultrasound, heating, the slug removing step include filtering or centrifugal method.
- 9. the pre-treating method of black powder as claimed in claim 1 and the like, it is characterised in that the pre-treating method Also include preparing treatment fluid, comprising the following steps that for the pre-treating method is shown：Treatment fluid is prepared, the treatment fluid includes dispersion liquid, acidifying solution and reinforcing agent, and wherein dispersion liquid is water, water/ethanol mixing Liquid or water/acetone mixture；Add acidifying solution to be acidified, the acidifying solution is that hydrochloric acid solution, sulfuric acid solution or nitric acid are molten Liquid；Reinforcing agent is eventually adding, the reinforcing agent is the one or more in crown ether and crown ether derivative；Sample liquid is made, handles described black powder and the like using treatment fluid, obtains sample liquid；Using sample liquid, the sample liquid is detected for laser activated spectroscopic, the occupation mode of the sample liquid is included directly Using, concentration use or be added dropwise to test piece remove solvent after use.
- 10. the pre-treating method of black powder as claimed in claim 9 and the like, it is characterised in that the preparation processing In liquid step, the crown ether and crown ether derivative include 12-crown-4 and its derivative, 15- crown-s 5 and its derivative, 18- crown-s 6 And its derivative, 21- crown-s 7 and its derivative, 24- crown-s 8 and its derivative, 30- crown-s 10 and its derivative, the reinforcing agent Addition be 0.001~8%.
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